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Tallie 1.1. Example Applications for Metal Powders.

;lPDlication example uses

abrasives metal polishing wheels, grinding-media
;'gril:ulture seed coatings. lawn und garden equipment
;1\:roSp;IC~ jet engines. heat shields, rocket nozzles
:('Chapter One· automotive
valve inserts. bushings. gears, connecting rods
colorants, filters, catalysts
Introduction to Powder Metallurgy coatings paint. hard facings, thermal spray barriers
construction asphalt roofing. r.aulking
electrical contacts, wire clamps, brazes, connectors
Frame of Reference
electronic heat sinks. inks, microelectronic packages
Among the various metalworking techno logics. powder metallurgy is the most diverse hardware locks. wrenches, cutting tools
gy manufacturing approach. One attraction of powder metallurgy (P/M) is Ihc ability to fab-
ricatc high quality, complex parts to close tolerances in an economical manner. In
heat treating
furnaces. thermocouples. conveyor trays
sound adsorption, cutting tools, diamond bonds
allurgy to essence. P/M takes a metal powderwith specific attributes of size. ~hape_ and packing, joining solders. electrodes, weld filler
111ologil:al then converts it into a strong. precise. high performance shape. Key steps Include tllc lubrication greases. abrudable seals
. shapingor compaction of the powdcr and the subse uent thermal bondi I of the articles m..gnctic relays, magnets, cores
by sintering. e pr cess effectively uses automated operations with low relative energy manufacturing dies, tools, bearing'. hurdfucing
consumption, high material utilization. and low capital costs. These characteristics make medical/dental hip implants. amalgams, forceps
P/M well aligned with current concerns about productivity. energy. and raw materials. rnctullurgical metal recovery, alloying
Consequently, the field is experiencing growth and replacing traditional rnetalforming nuclear shielding. filters. reflectors
operations. Further. powder metallurgy is a flexible manufacturing process capable of office equipment copiers. cams, gears. photocopy process carrier
delivering a wide range of new materials. microstructures. and properties. That creates ordnance fuses. ammunition, penetrarors
several unique niche applications for P/M such as wear resistant composites. personal vitamins, cosmetics. soaps. ballpoint pens
This book provides an introduction to the scientific principles behind powder metal- petrochemical catalysts, drilling bits '
lurgy. One primary audience is the student becoming acquainted with P/M as a process- plastics tools, dies. fillers. cements. wear surfaces
ing science. Additionally, the engineer involved in powder metallurgy cap also benefit printing inks. coatings, laminates
from this text. Frequently. empirical observations go unexplained and processes remain ~yrotcchnics explosives. flares, fuel. colorants.
inefficient because of an inadequate understanding. This book provides a logical presen-
tation of underlying basics without dwelling on the technological specifics covered in ponents. Funhcrruorc. metal powders find uses in such products us puint pigments, prim-
detail elsewhere. cd circuit boards, enriched [lour, explosives., welding electrodes. rocket fuels, printing
'. The P/M process relies on a different philosophical approach to component fubrica- inks. brazing compounds. ;!nd catalysts.
, . tion than is encountered in traditional metalworking. Specifically. the versatility of P/M Table 1.1 provides a collection of some common uses for metal powders in tep]'s of
gives an expanded latitude to the processing-of-materials: Material chemistry, heat treat- the industries. Although thi; diversity aids growth. it also makes the study of powder
ment, and microstructure are variable, and the distribution of phases and microcon- metallurgy as a technology difficult. Consequently, this text emphasizes the basic princi-
stituents (including porosity and. reinforcing phases) is controllable. . pies without dwelling on the specific applications.
Theapplications of P/M are quite extensive. 'Several examples will be developed.
throughout this text; however, as an introductory illustration of the diversity, consider the
u~~ of metal powders in the fabrication of tungsten lamp filaments. dental restorations.
od-Iess' beilrings, automotive transmission gears, armor piercing projectiles, electrical A few terms must he understood before beginning a discussion of powder metallurgy.
Contacts, nuclear power fuel elements. orthopedic implants. business machine parts. First. a powder is defined as a finely divided solid, smaller than 1 mm in its maximum
high-temperature fi hers, aircraft brake pads. rechargeable batteries. 'Intl jet engine COIll- dimension. In most cases, the powders will be metallic, lilt ough in many instances they

16 17
11\ IN 1111'1\\11 MUALttJlo.'t.Y
II I.:
POWDER METALLURGY SCIENCE ----------------------- -----------------------~.
I arc combined with other phases such as ceramics or lymcrs. An important charactcris-
lie of a powde.r i~ its relatively high surface area to volume ratio. The particles exhibit
behavior t~at IS intermediate between that of a 011 and a liq I • Powders will flow
under gravity to fil~ con~ainers or die cavities. so in t IS sense they behave like liquids.
They ar~ com~resslble like. a gas. But the compression of a metal powder is csxcntiilly
Irreversible. like the plastic deformation of a metal. Thus. a metal powder is casilv
shaped. with the desirable behavior of a solid after processing. .
. P?wder metall~rgy. is the study of the processing of metal powders. including the lab-
neutron. charactenzat.,on. and conversion of metal powders rnto useful engineering com- '.
ponents. The .processmg sequence involves the application of basic laws of heat. work.
powders chemistry
and defonnallon to the powder. It is the processing which changes the shape. properties
and structure of a powder into a final product. An extended list of definitions relating to
powder metallurgy is given in Appendix A.
The three main steps in the scheme of powder metallurgy are illustrated in Figure 1.1.

, Powder Metallurgy Processing

Figure 1.2. A tetrahedron illustrating the interdependence between several aspects 01
microstructure size P/M. including the alloy chemistry. powder characteristics. processing variables. and linal
chemistry shape product performance.
packing fabrication
First is the general area labeled "powder tccluiology" which is concerned with the nature
of powders. Emphasis is given to ihc Iabric.uion. classification. characterization. and
sinter handling of powders. Secondary concerns arc with the sampling. safety. packu!;ing. and
transportation. Examination of a powder for <ize and shape arc common and imponant
activiti~s in the field of powder technology. Traditional powder consolidation activities
hot press include compaction and sintering. The concerns :It this stage are with the forming and
densification of the powders. Finally, the conceptual now turns to an emphasis on the
final properties. with concomitant uucruion to product microstructure.
Students cannot separate the three activities. Decisions concerning the powder type
and its fabrication influence the case ul' compaction and sinicring. Likewise. the type of
density strength consolidation sequence applied to a powder will affect the final compact properties and . i:
ductility conductivity specific property goals require attention to the powder, processing. and chemistry. In
magnetic microstructure Figure 1.2. a tetrahedron is used to represent the interdepe¢ence of the chemistry. pow- "
der, processing. and properties. Conceptually. this book follows the flow chart in Figure
1.1. Emphasis is given to describing the effects of the many process variables. including
the relations between powder characteristics. ease of consolidation. and final compact
Agu~e 1.1. Th~ conceptual flow for powder metallurgy from the powder through the pro-
cessing to the final product. Example concerns are given for each of the three main steps. propert ies.


Brief History The initial interest in powder metallurgy grew from an expanding materials base,
forming the common elements like copper and,iron by a new. lower cost t~hnology.
The very early uses of metal powders have been traced to several parts of the world.
Sir.ce the 1940·s. several less common materials have been processed fro!" powders.
: \ .: For example. gold powder was fired 0010 jewelry by the Incas. and Egyptian uses of iron
incluJing the refractory metals and their alloys (Nb, W. Mo. Zr. TI. and Re).
powder date back to 3000 Be. Another early example is the Delhi column in India which
Additionally. the structural metals have come through a _major growth during the. ~e
dates from about 300 AD. This column is made from approximately 6.5 tons of reduced
iron powder. During the 1800's the use of powder metallurgy techniques began in time period. The majority of the structural powder-produced parts ~re .ba5ed on I~~':\.:.....
Hcwevcr, several compositions tailored for nuclear, aerospace, eicctn.clli. and magnetl~ .. ' .
earnest: The need for platinum laboratory apparatus led to the development of chemically
precipitated powder and new consolidation routes which avoided high tempe:atures. applications arc processed by P/M techniques, ., .. . . '. .'
": Such activities occurred in both Russia and England where precipitated powders were
Equally exciting has been the evolution in applications. The spint 10 DpplylO~ PIM.
'. has undergone a recent change. Initially. powder-based components were selected Simply
hot-worked to overcome the inability to obtain the high temperatures needed for casting
for .heir low costs. More recently, the basis for selecting D powder metallurgy route has
platinum. About this same time. coins were fabricated from pressed and sintcrcd copper.
been associated with improved quality, homogeneity. or properties. coupled with, an -: .
silver. and lead powders. The modern era of powder metallurgy is traced to Coolidge
attractive cost and productivity. The high temperature nickel-balled lIu~ralloys: high
who used' tungsten powder to develop a durable lamp filament for Edison. Subsequently.
specific stiffness aluminum aircraft alloys. and. cOOlroll~d thermal expansron alumlO~m-,.
cemented carbides, porous bronze bearings, and copper-grnpbue electrical Contacts were
matrix composites offer gnod examples of this evolution. Not only, can they be mad.e, i .
developed in the 1930·s. By the 1940·s. P/M was involved in the fabrication of new
with h:ller material economy hy powder approaches. but new and Improved cornpon-
tungsten alloys, ferrous structural alloys, and refractory metals.
rions arc being developed to take advaruagc of the chemistry an~ microst~cture con~rol.
The expansion or P/M prll\:e~sillg into areas requiring high quality materiuls and uruque
properties will creat~ even more opportunities in the future.

Reasons for Using Powder Metallurgy

01 Edison demonstrated his basic incandescent filament bulb system for lighting in
(i final 1879. For the technology to grow he required an inexpensive and durable filament Many auributcs contribute III the succe~s of P/M. Three overlapping categ?ries dom!~,
material resistant to repeated heating cycles. His early choice was carbonized nat- narc '1I1U nrovide an introductory concept lor the use of powder metallurgy. Figure 1.3 1\
ural fiber. These efforts built on earlier work in England that used platinum fila- a venn d'iag '1111 showing how the upplications for .P/M can be c~tegoriztd. First are the .
ments in evacuated glass containers. But by the late 1800's the efforts to find a many applications which rely on the economical production of ~omplex part~ ..
durable lamp filament 'had largely focused on carbon filaments with various treat- Components Ior the automotive industry represent good exa~ple!i of this area .and their
nature ments to increase the optical output. By 1905. Whitney had optimized metallized production is a large rIM activity. Within the area o.f economical parts. ~roductlon come
and carbon filaments with outputs of 4 lumens per watt. At this time the investigation cr nccrns with productivity. tolerances. and aurornauon. Both th~ precls~on and cOlit.nre
&.and turned to the refractory metals. first tantalum and then tungsten. The first tungsten very anracrive , while with cuxung there are problems associated with .se~regallon,
~ nant ' lilal~ent was produced from powder mixed with an organic binder that allowed machining. and maimaining final tolerances. Prealloyed powders allow fabflcat.'on bcl~w
livities s~apmg by binder-assisted extrusion. The binder.-wns.burned off and the particles the melting temperature. Thiv eliminates segregation and other defects associated With
ng and smtered to make a fragiie filament. The output was 8 lumens per wall. twice that casting. '. if .
on the of. the carbon filaments. In 1910. Coolidge developed ductile tungsten filaments As Figure 1.3 shows. there arc also unique property or micr~structu~ Just~ Icall~ns
u~mg tungs(en powder and controlled deformation processing. Tungsten allowed a Ior using P/M approaches. Some examples include porous metals. OXide d.'spemon
r type ~Igher operatin~ temperature and gave more light in contrast to the other options. strengthened alloys. ccrrncts (ceramic-metal composites). and c~mented carbl~es.9'he
ypc of n 1937. the coiled filament was developed and in 1959 halogen W;JSadded to inability [0 fabricate these unique microstructures by other techOlque.s has contributed ~
es and, . \: regenerate the coil during operation. Today. I kg of tungsten powder produces large pan to thegrowth of riM. The final cir~le sho~n on the ~enn.dlagram corresponds
stry. In 150.000 filaments for 40 W bulbs, each giving approximately 1000 h of life with to captive applications. These arc the materials which are quue difficult to
• pow- an outPUt approaching 13 lumens per watt. However. the life of the tungsten fila- other techniques. Ideal examples arc the react~ and refractory metals for which meLl1ng ,,
Figure ment may be ending: New clcctrodeless lamps that operate at 13.56 MHz using is not practical. Another emerging group of materials is amorphous or glassy met~ls. 10
quartz arcs have de . .
luding monstrated efficiencies of 135 lumens per watt. many cases. it is desirable to form a powder and develop low temperature processmg to , .~
ompact ~ avoid the microstructural damage accompanying elevated temperatures. Powder metal-


precision iron and steel
(example: automobile gears) aluminum

alloys nickel
CapUve composites
refractory (example: stainless steel tungsten
reactive filters)
stainless steel

Ideal Applications
(example: porous tantalum capacitors)
relative production
Agure 1.3. The three main reasons for using powder metallurgy are shown in the form of
a VeM diagram. The Intersection of the circles represents an ideal area for applying pow-
der metallurgy In the future. Figure 1.4. A comparison of the relative production for some common metal powders.
Note the logarithmic scaling and dominant role of iron and steel.

lurgy techniques are attractive since all of the processing can be performed in the solid fonn microstructures, 4) Economical consolid.uion of specialty alloys. typically compos-
state. .
ites containing mixed phases; these will often be fabricated by enhanced dCllsificat.ioll
Usually elements from all three categories exist in most P/M applications. Indeed. the processes. 5) Synthesis of nonequilibrium materials such as a~lOrphous. microcrystalline.
major growth and expansion will most likely come from further combinations of eco- or metastable alloys. 6) Processing of complex paris with unique ingredients or UIlCOIll,
nomic, captive, and unique aspects in. forming unique.low-cost. high quality products. man shapes.

The Future of POWder Metallurgy

The past successes of P/M have come from the economic benefits. evident in ••nclysis There are many industrial and consumer materials that arc available <ISpow-
of the volume of powder used for several material systems. A relative comparison of ders. They include minerals. cereals. coffee, and metal powders. On a tonnage
powder production qua~tities is given in Figure 1.4. This normalized plot shows that basis. metal powders are a relatively small activity when compared to common
common e~gineering systems constitute the largest use segment. relying on the lowest
powders such as sand andccrcnl=Tbc worldwide consumption of met~1 po.wders vol
cost matenals. More recently, the unique and difficult-to-process materials have con-
triOO.tedto the .expansion in the tech~ol~gical base. The same attributes are expected to
amounts to approximately 109 kg/ye<lr. Industrial minerals .con~umptlon IS l?8_. pp.
times larger. and even coffee. tea. and tobacco consumption tS at least 10 ....
continue merging to form new appltcattons for powder metallurgy. Six areas hold .he kg/year. Of the metal powders. thc majority are iron r~nd stee.1. As illustrated in S
nece.ssary ingredients for continued growth: I) High volume production of precise. high Figure 1.4 on logarithmic scaling. those amount to nearly 10 times thc consump- ..
quality from felTOUSalloys. 2) Consolidation of high performance rnateri- 1.1
.' tion of aluminum powder. which is. approximately twice that of copper powder,
"als. where full density and reliability are primary concerns. 3) Fabrication of difficult-to- the
which in turn is approximately twice that of nickel powder. and so on .
process materials. wbere fully dense high perfonnance alloys can be fabricated with uni-


Powder metallurgy is in a prolonged, if not steady. growth phase. The use of metal wing structures. Contrast the expected powder requirements (or these two nelda.

powders continues to expand and the field is growing faster than other metalworking
technologies. Moreover, the need for trained personnel is growing even more rapidly 1.2. ?owder metallurgy contributes to a range of automcdveeompceeau, Identify one
because of the diverse and difficult applications being developed for PIM processing. . such component and give the chief performance requlrements (check Table 1.1 and
The feedback from design engineers indicates that as knowledge about PIM expands Chapter Eleven for ideas).
there will be 'many more applications. The majority of the current uses relies on econom- 1.3. Consider the alternatives to powder metallurgy for the tabricalion of lamp filaments :"
ical net-shape processing. The future promises more challenges with the combination of from tungsten. Why are fusion techniques not applied to Ihis product? :' "
cost savings and factors such as reliability, quality. strength, dimensional control. and
unique shaping capabilities. Widespread appreciation of these advantages will provide IA. Powder metallurgy was once known as "metal ceramics." What similarities with ' '
both economic and technological growth opportunities. Research using metal powders ceramic processing does this name suggest?
offers hope for even more diverse applications, including rapidly solidified magnetic 1.5. What are some of the key differences between ceramic and metal powders and how
, alloys. new aircraft alloys. improved metal matrix composites, and ultra-high strength might these differences influence processing?
structures involving very small scale microstructures.
1.6. One of the challenges of PIM processing is to minimize tooling costs, especially din- ,
Suggested References ing product development efforts. The need is to reduce errors in the construction of pro-
duction tooling to ensure final dimensions and properties meet specifications. What steps
K. J. Anderson, "Materials for Incandescent Lighting: 110 Years for the Light Bulb." might help to minimize pre-production tool costs?
MRS Bulletin, 1990, vol. IS, no. I, pp. 52-53.
1.7. In spite of a low melting temperature (232·C). tin is widely used as a powder.
1 ,F. Clark, Advanced Experimental Techniques in Powder Metallurgy, Rowrnan and Identify some possible applications for tin powders. '
Littlefield. New York, NY. 1963, pp.I60-163.
1.8. Give <I short definition of powder metallurgy in lay terms and embellish this defini-
C. G. Goetzel, Tre~iise On Powder M~fall~i'~~~"f~ur '~~'I~;"es. Interscience Publishers. tion in engineering terms.
I powders, New York, NY. 1949.
1.9. Metal powders exhibit fluid-like behavior. Identify a common object or product that •
H.H. Hausner and M. K. Mal, Handbook of Powder Mmllurgy, second edition. relies on this attribute.
Chemical Publishing Co., New York, NY, 1982.
I)' C~111POS'
L Jenkins and J. Y. Wood (eds.), Powder Metallurgy: An Overview. The Institute of
1.10. Metal matrix composites. such as aluminum reinforced with silicon carbide
whiskers. are a new application area for PIM. Identify and explain some of the concerns •.
msli rcat lOll
Metals. London, UK. 1991.
or 1IIlCOIl1· W. D. Jones, fundamental Principles of Powder Metallurgy, Edward Amold Publishers.
associated with' the fabrication of such materials.

London, UK. 1960.

~. • ,1'

E. ~Iar (ed.), fowder Metallyrgy: Applications. Advantages, and Limitations, American

Society for Metals. Metals Park. OH, 1983. ,
us pow.
F. Y. Lenel, fowder Metallyrgy Principles and Applications, Metal Powder Industries
tonn'IIge Federation, Princeton, NJ, 1980. '
oWders K. H. Roll, "History of Powder Metallurgy," Powder Metallurgy. E. Klar (ed.),
is 300 vol. 7, ninth edition of Metals Handbook ASM International Materials Park OH 1984
pp. 14-20. '" , . r ~\ .
st 10 10,
rated in
StUdy' QUestions ,.,.
Dilsump. "
powder. ,,, 1.1. The Uses for met I d
th diff a POWers range from the very sophisticated to mundane. Consider
e I erent properties sought for aluminum powder for use in rocket fuels and aircraft

POWf)F.R MFTt'J ItJR(,y mrN(J 1\ l'NIll Il nWW:llNIIAJION'
, ,

... ,, Chapter !".!~
Powder Characterization
All powder processing starts with a powder; therefor~; one must understand the nature
of powder to understand the process. A particle is defined as the smallest unit of a pow-
der that can not be subdivided. Generally. powder metallurgy deals with particles that arc
larger than smoke (0.0 I to 1 urn), but smaller than sand (0.1 to 3 mm). Many metal pow-
ders are similar in size 10 the diameter of a human hair (25 to 200 urn). The scanning
electron microscope (SEM) is one of the best tools available for observing the discrete
characteristics of metal powders. An array of SEM micrographs for several different
powders is shown in Figure 2.1. In this series of micrographs. variations in shape from
flake to spherical and in particle size from the submicron to I mm illustrate the wide
range of possible characteristics.
Concerns beyond particle appearance require quantitative data. including the following:
I) particle size and distribution.
2) particle shape and its variation with particle size.'
3) surface area.
4) interparticle friction.
s) now and packing.
6) the internal particle structure. and
7) composition. homogeneity. and 'Contamination .
. T~ fully specify the ,nature of a powder it is also necessary .to qualitatively describe
-I "
h?w It was. fabricated. When dealing with powders. not only the properties of both indi-
Thee, partl~les but also the collective (bulk) properties of a powder lot must be studied.
", ; ~ropertles of a single particle include size. shape. chemistry. microstructure. density.
an ~ness. For a bulk lot of powder, characterization implies measurement of those
dPro~nl~s, and packing, now, and surface attributes. Both quantitative and qualitative
escnpllons are av '1 bl C' .... .
d'bed al a e. onsider the particle Image 111Figure 2.2. The Image can be
escn as a rou d db' I
value I ~ e ut irregu ar shape. However, such information is of limited FIgure 2.1: S<;~e examples of the diverse 6~ a~ Iizes of metal powde'* u seen In
of th~ n c~~~.t, dimensioning the particle is quite difficult because of the shape. Some the scanning eiectron microscope. These exMIpiea Illustrate. variety of materials, fabrl·
min t·poSSI e size. measurements are shown with the image. Widely differing size deter- cation methods, and particle shapes: a) tellurium, milled, acicular, b) Iron alloy, argon
a Ions are POSSIble d dl , atomized. spherical with aggtomerated fines, c) tungsten, gas reduced, polygonal aggre-
difficult epen mg on the Size parameter used and the shape. Shape is a
: t,,· sary tor~~:;:; t~ m~asure. Usually a simplifying assumption for the shape is neces-
e Size II1formation to a single parameter.
ga!es, d) tin. air atomized. rounded and IIgamental, e) Iron alloy, centrifugally atomized.
'. ,


POWDER MI: IN..LURGY SCllNCl 1'( 'WI '1 I . 11·\1,··\, 111.'11/\111 IN

possible size measures

A ~ projected area I:i = projected height is
S = surface area W = projected width s
V = volume M = maximum cord length o
H s
equivalent spherical diameters: a
0A= (4A/7t)112 s
0s= (S /7t)112
0v= (6V /7t)1f3

Figure 2.2. The projected image of a rounded but irregular particle. Six possible mea-
sures of the particle size are shown. three of which are based on projected dimensions
and three of which are based on equivalenl spherical diameters. .

This chapter introduces a hroad spectrum IIr tests as an armamentarium for asscssing a
powder. Such characterization of a powder is an important aspect of powder production.
research. product. development. process control. and property optimization. As a rule.
tests should be applied selectively to measure the critical powder features.

Powder Sampling and Dispersion

Collecting a representative sample of powder tor analysis can be difficult. Consider
the scope of the problem. A typical production lot may be several tons in size: a sample
of that lot will probably he on the order IIf ;1 k ilogr.un. Many modem analytical insuu- .
mcnts require sample sizes or a gram or k". Assuming a spherical shape. the particle
population in one gram depends on the ,i/e .md material density (rhcorcucal density).
Table 2.1 gives examples or the large number of panicles involved in I g samples or
small particle sizes. Only at the laq;e silL" doc the number of particles in just om: grarn
fall below the nonnal standards for stati\ticrl siguificance in a measurement. Hence, con-
cern is not with errors introduced by small \al11ple sizes: it is how well the sample repre-
sents the entire powder lot.
Sampling errors can be avoided using xomc simple rules. Powder samples should be

Table 2.1. Number of Particles in Olll\.,'c; ram .Sarnple of Munosized Powders of


Aluminum, Iron, and Tungsten

particle material (theoretical density glcm ')

diameter. um AI (2.70) Fe (7.86) _. vt(19.3)
spherical, f) tin, splat quenched, flake, g) stainless steel, water atomized. rounded and <

17 2.4. 10 17
Irregular, h) palladium, eIecttoIytIc, sponge, I) nickel. carbonyl decomposition, porous and 0.01 7.0.10 9.9·10Ih
cubic, D 'Iron-bued metallic glass, CN5hed ribbon, angular plates. k) titanium. sodium 1.0 7.0.1011 2~~. 10" 9.9·10'fl
reduced and milled, lrreguIar,and I) niobium hydride, milled, angular (photograptu cour- 2.4· 10~
1000 7.0· 10~ 9.9· 101
tesy of P. Hugo, D. KubIah. T. S. WeI, R. iaeecea, and J. Murray).


taken from a moving stream, not from stagnant lots. A major problem arises if the sam- powders, especially those below lOO..,n, will ~ibit suffICient capillary rorc:cs to.lpan-.
pleis taken after shipping or after experiencing other forms of vibration. In such cases, it raneously agglomerate with water contenu of t~ by. volume (as liule as O.l~ by':
is important to blend the lot before sampling so that settling effects are ·minimized. The weight). The capillary forcf actually increases as the meinure content decreases.
sample should be taken from maay points. Lowest sampling errors occur through the use Consequently, polar molecules are used u dis~rsant(with smaller powders.. These polar.
of a rotary riffler, which divides a flowing powder into rotating containers. If a static mo'ecules typically <Irecarbon chains with charged anwn'icor cationic terminal gtoups.·
. sampling procedure is necessary, then many small samples taken from random locations scch as hydroxyl (OH·). sulfonate (SO)'). sulfate (O~O):). andl1:Jllmonia (NH/). Shear: '
eters: avoids bias. No matter what approach is taken, it is necessary to critique the possible forces are effective in conjunction with the disPersant indeagglomenuing fine powders. ..
sampling errors and their effect on skewing the measurement of powder characteristics. The shear can be delivered using ultrasonic agitation ~ intensive mixina.
Dividers or thieves that take multiple random samples aid that task. Sample quality is
highest when it is a blend of several small specimens taken from a moving powder
The internal energy of a material is temperature' dependent, but ~tially ilis
stream, such asa conveyor belt.
Most metal particles are cohesive because of their small sizes. Thus, they are not easi-
independent of the surface area. However, ,!,he interfacial coeri)' ~CI with the .. ~:
size of a particle. Consider the size scale where ihc i~terflClal enctJ)' eqUJ:ls.thC
ly dispersed. Although van der Waals forces are small, adsorbed moisture causes particle
'.internal energy for a particle. For gold, the interfacial enc:raY is ~ product or the·
agglomeration. (Adsorbed surface films are loosely bound to a surface, in contrast with
specific surface area times the surface energy .r. At room temperature, the internal r
Ie mea-
ensicns absorbed films that are chemically attached and are difficult to remove - water forms an
energy of gold is approximately 600 MJ/m and the surface energy is approxi~
adsorbed film on stainless steel, but chromium oxide is an absorbed film.) An agglorner- '
mately 1.4 11m2. Equation 2.2 can be solved for the' particle size where the internal'
ate is defined as a cluster of particles held together by weak forces that can be overcome
ssing <J and surface energies are equal. giving
by a stress much below the intrinsic material strength. An example of an agglomerate is
dried mud, which can be crumbled by low stresses. In contrast, an aggregate can not be
a rule.
dispersed easily since it is a cluster of crystals or particles held together by strong bonds.
~ = 6 r! D.
such as cementing agents. The concern here is with dispersion of agglomerated particles.
The solution gives a particle size of 14 nrn, which corresponds to approximately'
A particle represents both internal energy (that scales with the particle volume) and
150,000 gold atoms. At this size. approximately O.3%.of the atoms I1tC on the par-
surface energy (that scales with the particle surface area). Let Er represent the total ener-
ticle surface, but the disrupted bonds as~atcd withlhose atoms contribute SO%
msider gy, V represent the particle volume, and A represent the particle surface area. Then the
cf the particle energy. In a nanoscale powder, it is ~t1mated that the first five Jay,
;ample total energy is a linear sum,
ers of atoms exhibit disrupted bonding. which corresponds to about '2~ of the
e; = YA + ~V (2.1 1 atoms for the 14 nm gold particle.
nsily). . : l.:· r
where is the surface energy (J/m2) and ~ is the internal energy (JIm"). Assuming a
rl..:s of sphere, the area will scale with the square of the particle diameter D and the volume will
t gr<J1ll scale with the cube of the diameter. Thus, the energy per unit volume is effectively a
measure of the cohesive potential per. particle, expressed as, Particle Size
. ,
EIV = ~ + 6 rID [2.21 Particle size is a determination of the dimensions of a particle. The size of a particle.
depends on the measurement technique. specific parameter being measured, and particle: "•.
~ecause the energy per particle scales inversely with. the size of the particle, the driving shape. Particle size analysis can be achieved by ~y or several instruments which USUAlly. .
~~ for agglomeration becomes larger as the particle size decreases. That creates a sig- do nOI gl~e eq~ivalenl determinations due t~di(ferences in the measured ~fllSlef5;; .
: ~cant problem in powder characterization because an agglomerated small powder will Most particle Size analyzers use one geometncpararneter and make the assumpllo~ of a,
s' Improperly assigned a larger particle size than is representative of the actual powder. spherical particle shape. The basis for analysis ca{l be any of the obvious geometric: val~: .
ince ~any processing attributes depend on particle size, improper characterization can ues, such as surface area, projected area, maximum dimension, minimum cross-sectional-
create,dlffiCulties. To characterize a powder for size or other attributes requires that it be area, or volume; Particle size is probably Orlc.p! the n:lost important characteristics to the :
prot.perly dispe~, which becomes more difficult as the particle size decreases. Surface er metallurgist. Size data are most use(ul when presented within the context of the
. ac
to rve agents can great I'y in f1uence power
d co hesi
esion or diispersion.
. Th us, th e nrst
- .
step IS irernent basis and the assumed particle shape.
pa~~ove adsorbed moisture or other agents that cause particle agglomeration. For large e example size parameters are diagrammed in Figure 2.3. For a spherical particle,
. ICes that may be sufficient for dispersion and accurate characterization. Smaller ~the s is a single parameter. the diameter. However. as the particle shape becomes more

32 33.
1'()wt)~ll MEIN.LUI~u'( ~LI~Nll I't 1\v11I1,',11!\1.:J\llllilLl\lIUN

complex, the difficulty in defininga single size parameter is obvious, Consider a plate- Table 2.2. Comparison of Particle Size Determinations for the Particle Shown in
or flake-shaped panicle (Figure 2.3b):. at least two parameters are needed to fully figure 2.2
describe the size: Diameter and width. As the shape becomes less regular. the number of
possible size parameters increases. For the rounded shape in Figure 2.3c. the size can be Measurement Value
described in terms or the projected height (random). maximum Icngth. horizontal width. linear measures
equivalent spherical volume, diameter of a sphere with an equivalent surface area. and so projected height 1.00

on. For the irregular shaped particle shown in Figure 2.3d. there is great difficulty in
defining a single panicle size. Since the size depends on the attribute measured. it is
projected width
maximum cord length
common to find disagreement between the particle size distributions obtained by many
equivalent spherical diameters
different instruments. Usually a spherical particle shape is assumed and the size is given
projected area 0.76
in terms or a single parameter, the diameter. The use 'of scanning electron microscopy
surface arca ' 1.45
provides a mechanism for demonstrating how well this assumed shape relates to the actu-
volume 0.95
al particle character.
It is important to use a particle dimension characteristic of the powder. The particle in
Figure 2.2 illustrates the approach. The size may be given in several ways. Equivalent thus.
spherical diameters are generated from values such cis the projected cross-sectional area DA = (4 At tu'" 11.41
or particle volume. Table 2.2 lists the results of various measurement tech1iques for
comparison. The maximum horizontal width W is termed Ferer's diameter.'~ similar Alternatively .. for ;1 measured volume \ ', the equivalent spherical volume diameter D, is
parameter is Mvtin's diameter. which is the particle width me~sured on the ~orizontal given as, '
bisector. The muimum cord length M and height H are. equally -viable measurements of D" = (6 V I iu'" 11.51
particle size. For nonspherical powders, these measurements aredependent on the pani-
cle orientation. ' " If the external surface area S is measured. Ihcl1, the equivalent spherical surface diameter
The equivalent spherical 'diameter can be determined from surface area. volume. pro- D, is simply.
jected area or settling rate _measurements. For example. the panicle in Figure 2.2 has a D~ = (5/n)ll.' 12.61
, projected area A. The equivalent spherical projected diameter DAis calculated by setting
the projected area equal to the equivalent area of a circle, It is possible to combine such mcasurcmcurs 10 form ratios as new coefficients for shape
and size., "
, A = rtD/14


~I For a cubic panicle with a size of I um as measured on each edge the projected

area A. surface area S. and volume V give the equivalent spherical diameters,
A = I 11m x I 11m = I (urn)? .

H 5 = 6 r\ = 6 (um)?
V = 1 urn x I prn x I urn = I (urn)!

Thus, the equivalent spherical panicle sizes are calculated as follows:

D/o, = (4 A / n)ln == 1.13 urn
~~ D~= (5/ n)lf2 = I .38 urn
W Dv = (6 V / n)lf3 = 1.44 pm
. .r"
a) sphere b) flake. c) rounded, d) Irregular Depending on the choice of measurement technique, this equiaxed panicle can
Irregular give up to a 22% variation in the apparent size. Clearly. an indication of the para-
Rgure 2.3. Atllllostratlon of the diffICUlty In measuring particle size. The number of possi- meter measured is important to convey accurate size information.
ble size meuurea Increases sa the particle shape becomes more complex. .

... ~ - ----:-- .

~ Shown in Measurement Techniques :,

A widely applied technique for particle sizing uses the ability of the eye to rapidly
size dispersed particles in a microscope. Many procedures relevant to testing metal p()\~.
dcrs are identified in Appendix B. Although microscopy is rcasonubly accurate, thc tcdi-
urn of sizing statistically significant quantities of particles has led to use of automatic
imagc analyzcrs. The image for analysis is ~el~eratcd by (either rdlectc.d or trans-
milled light). scanning electron or trans~lssion electron microscopes. The instrument
choice depends on the panicle size: however. the larger depth of field in the SEM is a
distinct advantage. especially since it shows surface topography and can provide x.ra~s
for compositional analysis. By microscopic counting of diameter. length. height or area.
a frequency distribution can be generated. The distribution will record the relative Ire- Figure 2.4. Agglomerated tungsten powder. showing a common' difficulty"In separatlno. ..
qucncy of the selected particle dimension. particles for size analysis by microscopy techniques: a) is a scanning electron micrograph" .
and b) is a transmission electron micrograph 01 the same powder.' .

12.41 A wetting liquid causes agglomeration of small panicles because of the strong
capillary force at the panicle contact. For example. the capillary force between a guish the actual particle size and shape. One technique (or dhpersing II microscopic sam-,
iamctcr D, is
panicle and a flat substrate depends on the wetting angle and quantity of liquid. pie is to mix the powderwith a 40% naphthalene and 69% camphor eutectic composi-
but approximately equals. . tion. This mixture melts at 32"C and can be easily mixed with powder (or dispersion on II
12.51 mounting slide. Subsequently. the eutectic is removed by vacuum sublimation. leaving
F" = 5 Dy the panicles dispersed for observation. .
'ace diameter
where F" is the capillary force.' D is the panicle diameter (assumed spherical). and Intelligent discrimination between single and multiple panicles is a common problem
y is the surface energy of the liquid. Consider the panicle size where that force in particle size analysis. Counting two or more small panicles as II large panicle will,
12.61 will equal the gravitational force on the particle. The panicle would adhere to the skew the distribution toward the coarse sizes. This. is significan: since processing
top of a container. The gravitational force on a panicle is given as the mass times response and final properties arc sensitive to panicle size. Improper size measurements
mx for shape
acceleration: will give false indicuticns. There are problems with measurements dependent on pOlnfde
orientation. Generally it is preferable to rely on parameters which lire orientation inde-
F = re DJ ~ P 16
.1:. • III
pendent. The equivalent spherical projected diameter D~.OlSshown in Figure 2.2. is par-
where g is the gravitational acceleration. D is the particle diameter. and P", is the ticularly useful for such measurement.
projected particle density. Combining the above two equations and solving for the particle
ers, size gives the critical condition where the capillary force equals the gravitational Screening
force. Screening is a common technique for rapidly anulyiing panicle si,le. A square grid of
evenly spaced wirescreates a mesh. The mesh size is deterrnined by' the number of wires
D = [30 yl (re g Pm)JII1
per unit length, The opening ~ii'.e varies inversely :~ith the mesh size: large mesh sizes"
If the fluid is water and the solid has a density of 10 g/cm\' then the surface imply ~Illall ~pening sil.e~ and vice v~rsa. Th~ most common convention (o~
energy is 0.07 11m2 and the critical panicle diameter is 1850 prn, indicating a large mesh size relies .a." .{he number of Wires per inch. For example, 200 mesh implies ~OO
panicle. The calculation demonstrates the difficulty in dispersing metal powders wires per inch. or '1'27 urn between wire centers. For thllt mesh. the wires are 52 11min
when they have adsorbed moisture films. diameter. thus. the remaining opening size is 75 prn, Mesh sizes cannot go to v~ry small
opening sizes. Consequently. the screening t~~£lique is usually applied to panicles
rtiele can larger than 38 urn. There arc electroformed meshes available down to 5 urn, but agglom-
the para. eration and particle adhesion to the mesh generally make the smaller electroformed
Obtaini~g a dispersed sample for image analysis is a major problem. Frequently. screens of lillie practical use. The opening sizes for the standard series of screens appears
agglomeration or coincidence OCcurs as shown in Figure 2.4. making it difficult to distin- in Table 2.3. That screen series has openings nominally spaced at a ratio of the fourth-

~---- 36 ]7
" -.


I'OWl )11:I I \i'I:AlIlIIILI\II0N i'

Tllble 2.3. Standard Sieve Sizes interval pcrccnt calcul.ucd I'm each \1/,' 11;1,·lillll.1\ fully automatic cycle is possible. The
mesh size powder passing through a mesh is designated by a - sign and that retained on a mesh is
mesh size opening. 11m opening. 11m
i • c
designated by a + sign. For example. -100/+200 mesh powder would have passed
'1 18 1000 100 150 through a toO mesh screen but nOI a 2nn mesh screen and would be between I SO and 75
20 850 120 125 pill in size. By convention. powder h<.:lllw.JS um (-325 mesh) is termed subxicve powder.
25 710 140 106 Although screening is the most widely used size analysis technique. il is not without
30 600 170 90 its problems. Screens will have from .Vir, 10 7'/()'pcnni$sible variation in average opening
II 35
size as a manufacturing tolerance. Further. individual openings can be up to 50% larger
than the prescribed mesh size. That creates a softcut point rather than a sharp division. A
45 .. 355 270 53 common problem is overloading. especially with the smaller screen openings.
50 .300 325 45 Overloading blocks the mesh openings. thereby inhibiting powder from reaching the lim-
60 Z50 400 38 iting screen size. Hence, the size dal;1 arc skewed toward the cOflrser panicle- sizes. The'
70 ... .,211 450 3? problem increases with the arnouru of powder per unit screen. area, content of fine parti-
80 180 500 25 cles." and SID'Il\cr screen openings. Another difficulty results. from the differences in
600 20 screens and techniques. In general. with any powder an R% error can be expected in a
screen analysis if the screens and techniques are not fully specified. The difference
root of two (in the ratio 1.19). between results can be. reduced 10 approximately 4%. if the.screens are the same.
Screen analysis begins with 11 !>IaCIcof screens with decreasing mesh openings. As Differencesas.small as 1.% can be achieved if full control is e.xercised over the analysis.
illustrated in Figure 2.5. the smallest opening size is at the bottom. The powder is loaded Thus. it is pointless to ascribe better than I % accuracy to a sieve analysis. Defects in
onto the top screen arid -thescreen staclc is agitated for a period of 15 minutes. For pani- screens will allow oversized panicles In pass. Also. too long a screening dural ion may
cle size analysis •• sample size of 100 g is usually sufficient when using 20 em diameter result in the panicles breaking into finer pieces. Too short.a screening duration will give
screens. After vibration. the amount of powder in each size interval is weighed and the insufficient time for fines to pass all the way through the screen stack. Because of those
difficulties. it is important to use standardized lest methodologies.

The following test results were obtained using sieve analysis with two sieve
. (1009) .'.
sets and 100 g samples from the x.unc powder 101.
f'.:~ ---.-.

. ......lI~-_

set I

mesh size ill1

.- Increasing

...-.- pan-«
·1X.4' ..
.•. t, ••., ·•.


Note that the samples may not be totally random. However. here the cumulative

* motion
particle size distributions (obtained by adding the retained weightsjare very simi-
lar except at the -20/+30 and -30/+40 mesh points. That indicates the possibility
that the 30 mesh screens were significantly differerU!~An appropriate next step
would be to inspect both 30 mesh screens for damage (rips or oversize openings)
Figure 2.5. Sieve an8.tysis relies on use of a stack of mesh screens of progressively
and to repeat the analysis with a calibrated 30 mesh screen,
smaller opening sizes (~r mesh numbers) for capture of particles based on the pro-
jected cross sectional siz.e •. "


f,,,,,,,,, The Screening is also useful in obtaining sized powders. This procedure is termed classili-
cation and is used to tailor size distributions. In several applications the ability to process buoyancy
on a mesh is force
a powder is dependent on controlling the particle size. Consequently. screening provides
ave passed
a means for removing specific size, fractions.
I 150 and 75
CV\! powder.
t ~ FV
" '.'

not without ~ vls.cous

Particle size analysis by sedimentation is most applicable to the smaller sizes.
age opening drag
Particles settling in a fluid (liquid or gas) reach a terminal velocity dependent on both the
50% larger force
particle size and the fluid viscosity. On that basis. particle size can be estimated from the kF1=O
division. A ,'.
settling velocity. Depending on the particle density and shape. sedimentation techniques
openings. at terminal
are nominally applicable to particles in the 0.02 to I00 urn range. The extension of sedi- fluid
ing the lirn- velocity
mentation to the lower particle sizes depends on the use of centrifugal forces. High fluid
sizes. The'
viscosities are needed for analysis of larger particle sizes. I
f fine parti-
Particle size analysis by sedimentation uses a predetermined settling height and places
ferences in
a dispersed powder at the top of a tube. Usually the test is performed in a fluid such as FG
cered in a
water. but air can be used for smaller particles. Measurements of the amount of powder gravitational '.
settling at the bottom. of the tube (weight or volume) versus settling time then allow cal- force
the same.
culation of the particle size distribution. Obviously. the fastest settling particles are the
e analysis.
largest while the smallest can take considerable time to settle. Automatic instrumentation FIg·m. 2.6. The force balance leading to a constant settling velocity for a spherical partie
Defects in c1e ill a viscous fluid.
for performing sedimentation analyses use light blocking. x-ray attenuation, weight or
ration may
settled cake height to determine the size distribution. Centrifugal forces can be added to
n will give nient to work with a known -culing height H while measuring the time {or settling I. In
.accelerate the test for smaller particles.
sc of those such cases. the particle size can be calculated from the settling time as fellows:
Assuming a spherical particle shape. settling at the terminal velocity in a viscous
medium is represented by a balance of forces. The buoyancy and viscous drag forces act 0= {/8 H TJt i: t (PH' - P,J/J": (2.111
to retard particle settling as diagrammed in Figure 2.6. Alternatively. the gravitational
o sieve force (or the centrifugal force if applicable) acts to cause particle sculing because of the
higher panicle density. At the terminal velocity. the forces are balanced. The gravitation-
A spherical nickel powder is to be analyzed {or particle size using sedimenta-
al settling force equals mass times acceleration.
tion. It is suspected that the particle size is near 8 urn. If the powder is dispersed
Fc=KP.,1t0·<f6 (2.71 in water at the top of a settling column 100 mm high. then what is the expected
settling lime? From Stokes law.
where 0 is the particle diameter. K is the acceleration (gravity). and Pm is the particle
density, The buoyancy force is determined by the volume of fluid displac::d by the pani- V = HIt = g D1 (P •••- PI) f (/8 TJ)
cle. .'
where H = height = 0.1 m
Fn=gPI1tD'<f6 (2.81 g = gravitational constant = 9.8 m/s1 .
D = particle size = 8. 10-6m
where PI is the density of the fluid. Finally. the viscous drag force FI' is given as.
P",;: nickel density = R.9.1()l kg/ml
Fv=.31tOVTJ 12:91 PI= water den. ity = 10l kg/rn!
7] = water viscosity = 10·l kg/m/s
where hV is the teml'lnal . vc I'ocuy an d TJ
n ISi t h e fl UIid vi
. F or a se dirmentauon. expcn-.
rneru, t e velocity is calculated from the height and time. Combining equations gives. This gives the velocity as 2.8. 10" m/s/nnd for a O.i m settling height the
corresponding time is about 360 s or 6 min. Tne Reynold number is 2.2. 10')
V =g0 1
t»; - PI) f (I (J 7]) 12.101
which is within the range assumed {or Stokes law.
for the terminal v I' '.
e ocuy, which IS known as Stokes law. It is experimentally most convc-

40 ~I
PO\.VDER METAlliJRGY SCIENCE 1'( )WI '11.' f "'\",''' III,VAIIC IN

A~ with all panicle sizing techniques, size analysis by sedimentation is nut without it~
error sources, First, the basic approach is limited to a narrow size range with some flexi-
To demonstrate the limiting sizcIor sedimentation analysis in air for tungsten \
bility possible through adjustment of the acceleration and fluid viscosity. However. for
powder is 17 urn. combine Stokes law with the assumed maximum allowed \
particles below I pm slow settling and turbulence (thermal gradients) can make it unrcli-
Reynolds number or 0.2. Solving I1clIl1Stokc-, law and the Reynolds number equa- \
able. The upplicuiion of centrifugal forces in thcrmalty ivol.ucd cluunbcr-, ha" been uvcd
tions for velocity and then cqu.uinj; the IWI! velocities gives.
with success in some laboratories. That has allowed extension or sedimentation tech-
niques to panicles a.~ small as 0.01 ~111. Certain particle characteristics can be qui.c trou- f) 11141\ =118RNll-'I(~p • J to -r))/"

blesome. Intemal porosity in the powder decreases the mass. thereby causing slowc.: par-
where D •• " is the maximum particle size, N,\, is the Reynolds number (assume the
ticle settling. For irregular panicles. the size parameter is somewhat difficult to visualize
lower limit of 0.1). 1) is the fluid viscosity (I,R· \O'~ kg/m/s).!: is the gravitational
-slnce settling depends on the hydraulic diameter. Furthermore, an irregular shaped pani-
constant (9.8-m/s1). p, is the fluid density (1.2 kg/m'), and POll is the metal density
cle may not take a ,tmight trajectory: hence its nonconstant velocity and uncertain path
(19.3· I O~ kg/m'). Solving the above equation with these values gives D of' 17 ,I
length hinder accurate sizing. Foreknowledge is necessary (appr?x,irrate particle size and
prn. If water is selected instead (viscosity or 10'" kg/m/s and density of I03'kg/m").
panicle density) before setting up such a test. In those cases of an unknown powder.
then the upper particle size increases to approximately 27 prn.
mixed powders of 4iffering densities (for example copper and tungsten), or newly syn-
thesized powders, those parameters may not be known.
There are mathematical limits to Stokes law. The derivation assumes that viscosity
controls settling. but this breaks down when thc Reynolds number RN increases over
approximately 0.2. In term~ of the settling parameters. the Reynolds number is given as.
Also. the panicles are assumed to reach terminal velocity rapidly. These factors usual-
Iy limit the technique to particle sizes below approximately 60 prn. For exarnpic, the
maximum"'panicle size for aluminum (density 2.7 g/cm.l) settling in air is about _'\5urn,
while for tungsten (19.3 g!cm·'). settling in air it is about 17 prn, The container walls
should not interact with the particles during settling. The particle-panicle in.eruction air __ 1 , f

must be zero: consequently; concentrations should be kept below one volume percent . flow t
with no agglomeration. Finally. the fluid and powder can not react chemically. so combi-
nations such as iron powder in water are not advised. In spite of these several ditficulties,
sedimentation techniques are in use for several powder systems. such as th~ refractory
metals. '
Elutriation applies to sedimentation techniques where the fluid flow is in the opposite II I :::: air
direction to gravity. This variation of the sedimentation technique provides a means of
generating panicle size distribution information. as well as separating a powder lot into ~ ~
.,,.. .• ~~ •.• - •.•.•. e..J
[[[[1' ••....• _ .•..•.• -;--1t ..
~ ~ flow
sized fractions. The greater the fluid flow rate. the larger the particle size carried away by
I I ~"'"
• .> ~ disk "" •••
the flow.
Another variation of the sedimentation technique is air classification. Air classifica-
tion achieves a separation of powders into selected size fractions using a cyclone or a
ifj t ::::
:::: fine't
. coarse
spiMing disle. (up to 12.000 RPM) and a cross-current air now as shown in Figure 2.7.
Tfle centrifugal forte provides a constant panicle velocity, while the .air flow achieves dll/fder
size separation by Stokes law effects. Figure 2.8 sketches how the particle trajectory is
aligned intermediate between the fluid flow and drag force vectors. Differences in the Figure 2.7. Particle size separation based on air classification of a powder using a rotat-
deceleration of panicles exiting from the disk are based on the particle diameter and ing disk and constant air flow. The smaller particle sizes are separated from the larger
sizes based on the centrifugal terce and air velocity.

powrXR ME1Al LlJJ.:tiY \ClLNC I


". "0'
~ ~I~W ~ .~','
J/owed powder . ..
. ..

. \ ~'

er cqua- feed
particle ce~~;~~gal "

~. .
" .. '
. ,',

rrne the
~ trajectory . : .....~ .
tationa! force ,':. '
• of' 17 . I
Figure 2.8. The particle trajectory in air classification depends o~ h~w the particle
Will'). responds to the combination of centrif~Qal an~ visco-us drag forces. which In turn depends
on t~e particle size and mass. . . ." ~·1··· '." . '.

mass. Consequently. lighter or smaller particles are deflected by th\! air flow and separat- . ,',.

ed from the larger particles. Control of the disk rotational speed ana air flow velocity. sample
provides the means of altering the particle size separation. Air classifiers are generally cell
applicable to the size range from I to 150 prn, although the actual behavior varies with
the inverse square-root of the material density.

Light Scattering Figure 2.9. The principte of particle siie analysis using. forward laser light scattering~'Th~:~: /.,
",' In streaming techniques for size analysis. particles are dispersed in a moving fluid. powder is dispersed and fed into the sample cell wherescatte,ring takes place, The defec.:; <,.'
Size determination based on a discontinuity in the fluid strearridue to the presence of tor system measures the angular'intensity tor subsequent computer calculation 01 !hElper-.· .
the particles. With careful instrument calibration, the discontinuity size can be related to ticle size distribution. . . . . '.:. . .'
particle size. Most devices are highly automated. so particle size analysis by streaming is ')'

popular, but expensive. Streaming methods provide a large dynamic ratio; the ratio of the
largest to smallest particles that can be measured simultaneously. In modem instruments 'detector
"Iens array

relying on multiple detectors. the dynamic ratio can be as large as8000. There is. howev-
er, a minimum particle size that can be detected. _ .
A versatile streaming technique available for analysis of particle size is based on light incident
scattering. Low angle Fraunhofer light scattering using monochromatic (laser) light and
laser beam
••• -----; .' .,.-
----- ..
..".,:. ----
dispersed particles is widely used for automatic size analysis. Particle size affects both
the intensity and ungular extent of scattering. A fluid stream with dispersed particles is
--. ----
large .........
passed in front of a detector system, such as diagrammed in Figure 2.9. The data particle particle
t~ panicle size are collected using a photodiode detector array. With coherent (laser)
h~ht the angle of scattering varies inversely with the particle diameter. as illustrated in
Figure 2.10. The intensity of the scattered signal varies with t~e square of the particle Figure 2.1 oj Small particles provide a wider scattering angle than large particles, giving a
basis for particle size analysis based on laser light scattering.
diamete-, Computer analysis of the intensity versus angle data will determine the particle
SI2.edistribution. Depending on instrument design, the dynamic ratio can range from 30 *(. '. .

~o 5~. far in excess of most other automatic instruments. Fraunhofer forward scattering tion is difficult, but can be: mi~imi2.ed by proper dispersion and ultrasonic deagglomera-
a rotat_ IS typically applied to the I to 200 urn size range. The smallest particles should be at tion. The technique is in widespread use because data 'collection is easy:
e larger leas~ twi~e the wavelength of the laser light for detection. As with other approaches to Mie scattering is applicable to particles generally below 3 11m and overlaps with
particle Size analysis, the particle shape is assumed to be spherical. Detecting agglornera- Fraunhofer techniques. Here. the detector is located at 90" with respect to an incident

-- ------------,--.:..-_---_._.
44 4~ .

light beam. Consequently, both detectors can be incorporated into one instrument to
expand the dynamic ratio during. an analysis. Modern laser light scancring inxtnuncrus combine 'various light sources and
Another light scattering technique uses the Doppler frequency shift. associated with detection techniques to give dynamic ratios of 7000 (0.1 to 700 urn) or more.
moving particles. For huge particles. the sample is dispersed in air' and accelerated Consider this range in terms of the number or particles, The mass of one spherical
through u nozzle into a partial vacuum, initially propelling the panicles at nearly sonic panicle at 700 um equals the m;I~' or 3.4 . 10s particles at 0,1 !lm.'ln terms or
velocities. As the particles slow. two-laser Doppler shift readings are made to extract the familiar size scales. a ratio or 7()()() Icngth, to I is the same as i4 ntm out of I km
time of flight and estimate the particle size. The approach can size panicles between 0,5 or <} inches out or r mile. The nonual ruler has an accurate dynamic ratio of 300 .
.and 200 JIm at count rates of I()~per second. that is I nun increments in a total length or JOO nun.
For smaller particles, the thermally induced random motion. known as Brownian
motion, provides sufficient velocity for sizing the particles. The Stokes-Einstein equation
gives the relation between the particle diameter D and, the translational diffusivity DT as
Electrical Zone Sensing
follows: '
The electrical conductivity or ;1 fluid p;I""1g through ;1 small aperture in all iusul.uor
provides a method of measuring the number alld size or part ides suspended in the fluid.
Conductivity mcasurcmcut is achieved I", 111;lkillgthe fluid conductive and applying ;1
small voltage across the opening. A COIlIIIlOIltechnique for measuring blood cells. it call
where k is Boltzmann's constant, T is the absolute temperature. and 1] is the fluid viscosi-
he applied to sizing powders, The main katllrl'~ or the d~vicc arc shown in Figure ~,12,
,ty. In a size lUUIly~istechnique termed photocorrclationspcctroscopy. laser light is used
to detect the Doppler frequency shift of particles in a fluid. The approach uses an internal
beam splitter for calibration as sketched in Figure 2,1'1. Over the panicle size range from
I approximatety 0.00510 ~ .prn, the reflections from the particles 'give frequency ,hif:s
(rom 1000 to I Hz, depending on the inverse of the panicle 'size. TIle,' intensity versus ire-
.quency information is collected over a period of minutes. The output is analyzed to
deconvolute the particle slze distribution from the signals. To use that approach one must
: know the optical properties of the fluid and panicles, fluid viscosity, and temperature. to pump
... The advantage is it's applicability to very small panicles with few assumptions about the
tttt '
inherent particle size distribution.

• . '; '-"-"e.

~ . ::::0f" ~
scatterIng • !.----. • aperture
r--+---sampl~ cell ~./



., .: electrode


'-"-" electrolyte

photo reflection '-"--' ,

FIgure 2.11. Very ~ particles undergo Brownian motion in a fluId, the velocity c'! the Figure 2.12. The principle of partictesize analysis using electrical conductivily changes in
motion provides Infonnatlon on particle size as measured by the Doppler shift of .:I laser a small aperture zone due to the streaming 01 particles dispersed in an electrolyte flowing
OO~. . through the insulating aperture.

46 47

higher dcusity materials xuch ~IS iron and tungsten. For tungsten powder. the technique is
)un:es and limited to particles below 6 urn. Another difficulty is maintaining 11 low powder coneen-
, or more. tr••tion to avoid coincidence (multiple particles) in the aperture. Experience has shown
sphcri<.:al lIuld the instruments are susceptible' to electrical noise and aperiure 'plugging by agglomerates ~.
1 terms or flow or large particles. Generally. better results are obtained.fer low density materials (such u.~
III of I kill ceramics and polymers).·
io or 300.
Light Blocking .; ..
Particle size analysis based on light blocking iOimilJir to electrical conductivity and'.
is another variation of streaming analysis, A light beam is' interrupted by a now or dis-
persed particles a~ shown in Figure 2.14. As a particle passes in front or the window. it ..
partially blocks the light reaching the photocell. Assuming a spherical particle shape. the
an insulator amount of-light blockage is equated to an equivalent circular cross-sectional area. The
time (expanded scale)
in the fluid. dynamic ratio for the technique is 45. The lower particle size is determined by the optical
cI "pplying a resolution. with I urn being typical. Particle dlspersion in the fluid is important to avoid- .
~ cells. it can inf coincidence. Measurements are similar to those obtained using electrical zone sens-
Figure ~.I~. current ing techniques in terms of both problems and ·Iimitations.

X·Ray Techniques .. .
time Two x-ray techniques call be applied 10 size analysis of very small particles. .'
Diffraction line broadening for crystalline materials. has several causes, including. strain .
Figure 2.13. An expanded view of the aperture from Figure 2.12. The streaming fluid car-
and small crystal size. The destructive interference from the crystal is not complete at ,
ries a particle through the aperture. During passage, the particle reduces Ihe current in
proportion to its volume and provides a basis for counting and sizing. angles slightly off the Bragg condition. .·1

A narrow aperture in a nonconductive glass tube carries a flow of electrolyte (I % sail

water) under a small pressure differential. An electrical current is' maintained between
the electrodes inside and outside of the tube. As shown in Figure 2.13. dispersed particles
in the electrolyte are carried by the fluid flow into the aperture anq cause a decrease in
conductivity. The decrease in the aperture conductivity is proportional to the. particle vol- light
ume and thereby generates pulses related to particle size. Through calibration procedures
a~d selection of the appropriate aperture diameter (about 1.6 times the largest particle
Size) the technique can be applied to several size ranges. The dynamic ratio is approxi-
mately 30 with a lower particle size capability of 0.5 urn. . .
The wide range of applicable particle sizes is an advantage of the technique.
Approp~iate aperture selection avoids plugging problems while ensuring goad resolution ,

of the distribution. Particle settling in the outer chamber during analysis causes the data
to be .skewed to the finer particle sizes. As an empirical rule, the electrical zone sensing wlndows . ~
techOlque is only valid when, . . .. .~••(j

,·r· .'.

if changes in
D (p~ . P,Y'} < 500 . 12.141 time . J.,

olyte flowing ~~:~ D is ih.e particl~ diam~ter in }l~, P., is the theo~etical d~nsity of the. powder in FigL're 2.14. Particle size analysis based on. light blocking, where the Interrupted light
.: .and P,IS the fluid density, also In g/cnr'. The particle settling problem IS acute for beam is used to size and count particles based on their proJected area,
¥ll ~ lUI~t', Y \( IL Nt I
.. -
1"'\\,1111., 'I I"l 1111."\111" J

12.1.'i 1 IIll' hroa!it-lIill!! due 10 I'arlil'k ~i/l', a ,1;11111:11.1 :1 dilll'l'l'l1t

III dillrarti(ll1 p.nrcrn is 111i~l'd
with the lest powder. Ily lIsil1!! a slal1d:lld \\'1111;1 uruch lar!!er rryxta] size Inver I )1111) thl'
'where ,t is the x-ray wavelength, is the interplanar spacing. and () is the diffraction hroadcning :JI a similar diffraction angle call be measured. If B.,. is the 101a1 measured
angle. The width of the diffraction peak increases as the thickness of the diffracting crys- hroadening. then the particle size broadcninp /I i~ calculated from the total using the dif-
1:11 decreases. The most useflil approach to particle size analysis using x-rays relic: 011 the fl'rem:e 01" the squarc«,
peak width a! half of the maximum intensity us diugrummed ill Figure 2.15. Peak hro.ul-
yning ut thai intensity depends. in pUf!;on the number of diffraclillg planes ill the ny~tul. lJ: = B,.-' - H/ 12.'171
:.;J11e Scherrer formula gives (he crystal size D in terms of the broadening B. diffraction
r angle 9. and x-ray wQveleng(h ). ~s foJ.lows:' where B.\ is the IX:ak broadening for the ~lal1dard. Thetechnique is best applied 10 parti-
~ '. . . ' ~. ..'
Fk~ in the 50 lillj size range. Under careful cxpcrimcntul conditions, x-ray peak broaden-
,. .D = 0.9 ).J(8 cos(O}) 12,101 ing can be used for panicles up 10 0.2 pill eOO nm) in size. However, the technique gives
.. ,,' , , ' , "',, , ' " ; I .
only a mean crystal (panicle) size with 110 disuiluuion or shape information.
: t ,:'
Jt is easier to measure the crystal size at large diffraction unglcs (high index planes) and Thc second x-ray technique is sm;dl :ll1gk ~catlerill!!, which can determine the size
with larger incident wavelengths, The wider the diffraction peak. (he smaller the panicle distribution if tilt:' particle share is known. The inl~n;'il)' of x-ruys scattered by a small
"" 'size. panicle varies with the particle volume. Small ;l11gh: x-ray scuncring is most useful for
For accurate size analysis by peak broadening. the effect of strain mus: be subtracted. particles below $0 run in size. The technique a"lImes the particles to be dispersed with-
<, That can be accomplished' by analyzing for the amount of broadening versus the diffrac- out iutcrparticlc interference. The x-ruy illlL'n,ity versus angle is measured within the () to
, tion angle. Additionally. broadening due to machine sources. beam diverucncc and sum- .'. range III estimate either the panicle ~ilL'di~lrihlllioll l1I' the particle sh:'1ie.
, pie size must be subtracted. Typically. the peak broadening is best applied 10 annealed or
briitle materials where strain,'is not aconcern. Milled metal powders will usually exhibit Comparison ,!Jf Particle Size Analysis Techniques
rion-unifpnn strains and CDn ,not be analyzed accurately by x-ray broadening. To .solatc Analysis otpanictc size depends upon ml';I~uring,lilc response of a particle 10 some
physical icst.vlngcncral. a spherical partirit' ,Ilape is' assumed: difficulties often can be

x-ray traced directly 10 Ihal assumption. Because (If the differing physical attributes tested hy
Intensity each technique and the assumption of a~phl'ril'al particle.shape. the various size analysis
techniques will yield very different rc-ulr-, Oil '<line powders. Table 2.4 and Figure 2.10
provide comparisons of the several technique available for panicle size analysis and
give the approximate size range of upplicabilitv. dynamic ratio. approximate sample size,
B = broadening approximate analysis lime. and basis for the distribution (population or weight). The fig-

ure and table generally reflect the best posxihle measurement range obtainable
powders. Often . larger panicle size ranges or dynamic ratios are claimed. bUI nOI demon-
for metal

strutcd with the denser metallic panicles and the courser panicle sizes. With respect 10
relative cost, automated instruments arc expensive. In the simplest sense, an accurate
panicle size analysis is possible uxing simple instrumentation and basic physical princi-
ples (for example with a watch and water filled graduated cylinder). The selection of a
technique depends on several factors including availability and approximate particle size

Particle Size Data

Once particle size data are collected, concern turns 10 an analysis of the distribution, .....
dlHraction angle, 29 The distribution is given in terms of a histogram or frequency plot showing the amount
of powder in each size increment. On such plots, the m6'de is the peak particle size.
Figure 2.15. X-Ray peak, broadening Is measured in terms of the width 8 at an intsnsltv Consider the sieving data in Table 2.5, which ~ivc the weight of powder retained on each
one half of the maximum. ' .
screen after sieving. The firs: task ill Ihe analysis is 10 convert the data into incremental

" .. so '>1
"I .,:
. .' ;..
rn i~ rnixvd
r I )1111) lilL' ..
by dividing each increment by "ilie: .toti.I.~ple

Table 2.4. Comparison or Particle Size Analysis Approaches ~ntages weight. The histogram (or
I measured
these data is generated b.y plotting the incremental percenta~ venus the screen opening
,ing the dif- size dynamic sample relative
technique size. Sucha plot ;s given in Figure 2.17 for the- data frdm 'Table 2.5. Notice (or chis plot'
range. jim ratio size. g speed· basis"
e., the particle size is converted to a log scale. thereby. miXing the increment widths equal.
12.'171 optical In most instances. metal powders are found to ~xhibit a bell shaped curve (Gausshln or ' ..
0.1l and up 30 <I 'S P
electron 0.001-400 30 <I S P
icd 10 pari i· sieving (wet and dry) Table 2.5. Example Particle ~ile Dlstrlbutlon Data
uk broaden- wire mesh 38 and up 20 100 I w mesh opening weight' '. interval cumulative
niquc givcs electroform 5'- 120 20 >5 S w size ~m retained. g percent percent
IlC the size gravity 0.2· 100 50 5 I w 70 212 0-,0' . 0.0 0.0
by a small
centrifugal 0.02-10 50 I s w 80 180 1.1 0.9 '. 0.9 ..
light scattering
.. . 2.5, '

I useful tor 100 I~O 3.0' ':'~'

3.3 , '.
.rscd with-
Fraunhofer 1-800 <200 <5 F w 120 125 8.7 7.1 10.4
Mie . 0.1 - 3 30 I F w . 21.2·
hin thc () 10 velocity
140 J06 13.2 10.8
0.5 - 200 400 I F P
Brownian 170 9{) 16.5 13.5 34.7 .
0.005 - 5 1000 <I P
electrical zone 200 75 20.8 17.0 51.7
230 63 18.0 14.7 ~, 66.4:
sensing 0.4 - 1000 30 5 w
llc 10 some light blocking 1-600 45 3 p 270 53 16.9 '.1'3.8 80.2
Itcn Gill he x-ray 325 45 13.6 11.1 91.3. ,
s icsrcd hy broadening 0.0 I - 0.2 S P 400 38 10.8 8:8 100.0. -.
ze analyxi» small angle 0.00 I - 0.05 I' S P 500 25. 0.0 0.0 100.0
igure 2.16 = =
··S slow (I hour or more). I intermediate (-1/2 hour). F = fast (:t/4 hour or less) total weight = 122.6 g e: ,.
alysis and • P = population basis. W = weight basis
umrle size.
I). The rig.

c for metal ___ ----------~x·ray small. angle

x·ray broadening
weight percent
20 .I
101 demon. ~modeslze
light blocking

••••• Il:=j
electrical zone lensing
Brownian light scattering
15 '- ,.. -
ical princi- • velocity ilgh! scattering
,mick size
of a

•••• II1Mle light scattering
Fraunhofer light scattering
10 '- . screen -
__ -I centrifugal sedimentation analysl1
r--_-Igravlty sedlmantatlon
electrofcrm sieves
5 '- - ,,

wire mesH sieves
electron. microscopy o
10 100
rh 1000
0.001 ' optical microscopy
rhe amounl 0.01 0.11 1 :i'fO ""'''100 ····1000
nlclc size.
particle size, um
particle 8Ize,~m
led on each
neremellIul Figure 2.16 A co . Figure 2.17. A histogram plot of the screening data from.TabIe 2.5 with the particleSIze
ful size ranges
. formpara!' I of particle
'. size.anatysls techniques and the nominal use- .

-- each. Ive pot

axis en a logarithmic basis. The most populous size Is termed the mode, her& It Is
between 75 and 90 urn,
_____ ...:.- .__ '_'1 _JW_'_" r,.• II,W,\, _'_"_"_/A_'_'I_IN _

size intervals), Finally, the standard deviation a is calculated from thc arithmetic mean as
cumulative percent finer. follows:
100r----------.~wt~~~ 12.201'
a= II /IN)!: n,: \.,. l) .....: I"!
75 Basis lur Plots
An analysis determined by micr\l~(lIp) techniques giws the pupulution of p.miclc-,
versus their size. However. an analysis taken by sieving techniques provides a weight
distribution. It is important to state the hasis for plotting particle size information.
Consider the difficulties ill comparing tW(I ~ets of data on differing bases. The weight
2S distrihution is skewed to the coarser particle sizes in comparison to the population based
. distribution. The particle size data from Figure 2.1 X have been replotted in Figure 2.19
.0.L--_......c::J1:::.-..L-...l- ....J -t- ••. ,
along with i1i~'population bused distribution for the same powder. The obvious differ-
cncc in placement of the two distr!I)\I~~o'.l~c;.~,.lhe seen in comparison of the median sizes
10 1000
(72 IIIll VcTSUS' -12 um). For any partil'ic Sill'. ';I~suming a spherical shape allows calcula-,
tion of the number (If particles 1/ kunwin;; till' weight \I' and thcuretic,tlllletallit:llsity I~",:'

Figure 2.18. The cumulative particle size distribution plot lor the data in Table 2.5. The 1/ = (I \II I (P .., IT IJ') 12.211
arrows Indicate the standard deviations lor the distr;ibution.
where D is tll'e diameter. Direct comparison llf weight ,II1dpopulation based particle size
distributions is invalid.
-normal distribution) when plotted on a log size scale. termed log-normal. A cumulaiivc
. particle size distribution is generated by adding the interval percentages and plotting the
result versus the lower incremental panicle size. An analogous distribution could te gen-
. crated by plotting the cumulative percent larger than a given size. The raw data trcrtrncnt
cumulative % finer
. is outlined in Table 2.5 while the resulting plot is shown in Figure 2.1 X. The information
100 -1
. given in a screening analysis is with respect to the weight of powder larger than the spe- I

cific screen sizes. In Figure 2.18. a smooth curve h~s been used to connect the known I

points. population,'
75 I
On the smooth cumulative. particle size distribution. the median size corresponds to I

the 50% value, The mode. particle size corresponds to the most frequent particle size. I

which ill the highest peak on the histogram distribution. The standard deviation and mean 50 I
size can both be calculated by usual procedures. The standard deviation sizes (+ or· one I
standard deviation) correspond to the particle sizes at roughly 84% and 16% (more pre- I
cisely 84.13% and 15.87%). , 25 I
For histogram data; the ari.lhmet'ic mean size D ",., and the geometric mean size. D x'" arc I

calculated as follows: . . ,. I
0 '"
10 100 1000
particle size, IlITI

log (D,..I = (lINlEy/log (01) 12.191 '"

Figure 2.19.A comparison 01 the cumulative particle size distributions as determined 011
where D/ is the midpoint size for each interval. y/ is the frequency of occurrence in the basis of weight (e.g. screening) and population (e.g. microscopy). The population drs-
the size interval. and N is the total number of occurrences (N is the sum of .,
v. over all tribution is,displaced toward the liner particle sizes.

S4 55
. -;.
ithmctic mean as
. Common Distributions (rilonn<iispcrse). The t"ypi\'al pnxluc: is polydispcrsc, ~iih II wide rall~~:uf:Jlartich: lIii'.cs. -.
It is useful 10 review some of the shapes of panicle size distributions encountered in Vr;ry special efforts a(\' lll'l'Ik'd tll achieve amonesizcd powder. rllh~.lluently. II median
P/M. TIle typical bell curve' which occurs when 'the interval panicle si·,.e data are ploucd or mean size and the dispersion in particle srze.arene<i:e$S~:tyinform;lIio!l. The disPeisioq-,
on a log basis is shown in Figu'ie 2.17. In contrast, the plots in Figure 2.20 show varia- is effectively the standard deviation. A common pr3c~ice'in P/Mh io·distillthepart;icle ..
tions including broad and narrow distributions as well as a bimodal distribution (two si:·.e distribution information into three points c!esi~~'icci /)vii D.I!;: and DIU' corres- .
iion or p:trltck,
peaks). Normal powder fabrication practices can not form a single sized powder pOmling III the pari ides sizes at the 90. SO. ~and' 10 petceru, paints on the cumulative
'ovides a weight
distribution. . ' ".' , , : / , .',' . , ... . ', ::..
zc information. .:
scs. The weight
Dopulation based cumulative Log-Normal SizeDistributions ',' ., ;. z . ..' '~'. ':.
frequency frequency Most powders follow the log-normal form in th~ir .nril.ur.&I.unscreened state. A log! ' '
d in Figure 2.19
obvious differ- GaussIan 100 normal size distribution gives a bell curve when die fr~quen~y is plotted on a linear scale-, .
he median sizes (log-normal) against the log of the panicle size. This distribution !=ant>edeseribedmathematically .by,·· .',•
: allows culculn-, a modified form of the Gaussian probability function,;Let P(x) be the probabilit~ of
% observing a part iclc size described by .r=!I/(si:r ),~iving " , ' .. ':.' "'.
ctal dcnsirv •. /),'/1 :'

12.~II o~~-....,....:--- 12.211

log size log size
poiydisperse 100 -
when' U is the natural 'Io\!:,rithlll of the mean':. particle size
. and .'
.. is the standard devia- .. '
(broad) tion of the distribution (on a logarithmic scale).

% 12.231 -.

Figure 2.21 gives a xchcm.u ic comparison of a panicle size distribution ploued on S/:ver: -,
o •....•~--.....,..;...-- al lJa:c:s. The linear scaling shows a skewed particle size distribution while the log seal.:, '
log size log size ing gives the expected bell curve. The cumulative particle size distribution Fix) c!n be
monodlsperse expressed in tenus of the iutcgr.rl or P(.I'} over the. interval (rom 0 to r,

: Ft.r)= t: Ptxtdx

which i~ uw:III}' given on :, pcrccnrage basis.

Consider a plot of standard deviations instead of percentage . The standard devlmions
o '-----'-~---- correspond to specific percentage points. For example a standard deviation of zero from' .
log size log size
the mean corresponds III the average size. The 'standard deviations and corresponding'
blmodlai '. '11'
~ "" .~ •••
;--- cumulative percentage points arc listed in Table 2.6. , '.
The log-normal particle size distribution is created by replouing the percentage P91nls '
from a cumulative distribution in terms of deviations. Such a plot is shown in the bottom
of FiJure 2.21':' Many powders exhibit straight line behavior on the log-normal plot.
Hence, the particle size distribution can be reduced to juS! two parameters. the slope and ,.
OL-~------ ir.rcrccpt or slope and mean size. An advantage-in doing such a fit becomes evident when
s determined all log size log slze particle size distributions are compared by d(ffering measurement techniques. In Figure
e Population dis- 2.22. the particle size dat;, from Table 2.5 have been plotted on a cumulative log-normal
~~~~:: ;"~-hA comparison of Ihe common types of particle size distr~butions. showing the basi. The standard deviation points indicated in Figure 2_) 8 have been used to make this

-- I the frequency and cumulative plots. plot. giving a straight line for the distribution.
/., '1'.'/./ f'. ""f"\' "/.'1/'1/1, f1l
I'OWDl~ M.lllII.tUh'l,n( II NIt


standard deviations cumulative percent

IIn~ar 80
frequency a 50
percent plot 40
log -1 20
cumulative -2
percent··· plot
20 50 100 200

. ,
' plot

log-normal ;i,. ,
particle size, ~ m

Figure 2.22.'-The Ioq-norrnal particle size orstnbution plot of the data from Table 2.5 using
the standard deviation points from Figure 2.18. . .

that such comparisons (or data transfurm.uionx) are relatively simple. If tl~e slope and
~~----------~Iog intercept ofa distribution are known. then the other distribution can be estimated by a
translation. In 'transfonnarions. the slope remains constant on a log-normal basis.
FJgure 2.21. The particle size distribution shown on four different bases; a) the frequency Transformation ~f the data requires culcul.u iun of the displacement parameter 8 shown in
versus particle size .on a linear scale. 'b) the frequency versus particle size on a log scale, Figure 2.23. To convert from a weight distribution to a population distribution. the dis- .
c) the cul'!'lulative frequency versus log particle size. and d) the log-normal distribution
showing the standard deviations as a function· of the log particle size..
J',' : standard deviations
Table 2.6. The Percentage Points and Stan~ard Deviations on a Cumulative Particle
Siu Distribution POPUlatiOn//!
, ,
deviations percentage
-2.0 2.28 median /'
-1.5 6.68 a ······················>l················
-1.9. 15.87 ,
-0.5 31.85
0.0 50.00 /\ s =6.908/m
0.5 .. 69.15
, ,,
1.0 84.13 ,,
1.5 93.32
.2.0 97.72 x=log,o (particle size) "

Reali the problem of comparing analyses taken from screening and microscopic Figure 2.23. The use of the log-normal particle size distribution to transform from a
'measurements. Screening gives size data on a weight basis while microscopy gi les it on weight to a population basis. The vertical translation distance 0 depends on the slope of
the distributi~n. .
• population buis. One of the fundamental attractions of the log-normal distribution is

.•. c'-- _H~" -.. i_


I placement is upward and the magnitude is dependent on the slope m where D,. is the largest particle size. A similar distribution is the Dinger-Funk distribb-.
1. tion which uses both th~ smallest size Ds and largest size DL•
1) = 6,908'1 m 12,251
j F(D) = (0" - D")
~ 1(;) ··0, \
") 12.lll
whcn the panicle size is expressed on a base-l 0 logarithmic scale. I ore, 6.90R equals :I ...
times the loge I O. where e is the basis for the natural logarithm and :I represents the size 'Problems in Particle Size A'"a'Y~is
exponent in Equation 2.21. To convert from a population to a weight distribution. the
There arc several problems with particle siz~ is quit~. difficult to resolve a:
displacement is negative (downward) with equal magnitude. Once the transformation is
'~id.e ran~c of particle sizes simultaneously during an analysis. Almost all devices·hav~·;i
completed. determination of the median size is straightforward (zero standard deviations
. lir.iitcd size range they can accurately resolve and .l.anatyze at one time. Often thnt Hmiia.,
on the new distribution). On the other hand. mathematical detcrmination of the median
tion results in a realistic dynamic ratio less thap th:e advertised runge. If the particle. size:
size is possible. For a weight distribution the median size D., •. is given as.
distribution is broader than that, the methods are noi.accuraie. Additionally. each tech •. '
nique has a range of optimal -uirability, For sieves .. it i~ generally above 38 jJm.,Optical.'
microscopy is restricted l\l purticlcs aboveupproxlmutely lum. Techniques such a:~scdi-.'
mentation arc only applicable l\l a narrow size r.ll}ge :~cause of limltations imPosed'by -
and then the median population size 0 is g~'~:~'as
/1111 •
the fundamental physic». - . .
The particle shape problem was emphasized earlier in this chapter; more on shaPe >
D = /O'lh+oYm 12.271
"'I' . analysis follows in the next section. The more irregular the particle shape.rhe more parol"
meters necessary to size a particle. Most rncasurement techniques assume a srhcri~oll
Ie 2,5using where" is the intercept (the standard de'viation corresponding to the I prn panicle size)
sl.apc, Accurate description of shape and its variation with size is tedious. It is notewor- '.'
and 11/ is the slope, The steeper the particle size distribution. the smal!er 1) will be or.
tll:' rh,u shape. like size. is a distributed property or" pOwder.· . ..: ,," ,
alternatively. the closer the median sizes by the two techniques.
e slope and ; In general. the finer particle sizes arc poorly-characterized .by sieving techniques. Tli~·.
atcd by a limited ;m;t1ysi~ range coupled with a bias toward weight based dimibutions results'ii\:,
Other Size Distributions
rmal basis, disregard for the filler particle sizes. In many instances; the disregard is not \\Iarr~ied.
Generally. the log-normal distribution is the most useful when dealing with metal
1) shown in powders. Others arc sometimes applied to panicle size data. One is the Rosiu-Rammler
sin~e t~e fil~er particle, Il(l'~':'~ the greater su'rface .~rea and kinetic activity. Ai. a ~i~e::
on. the dis~ ' rauo '11 25. It takes 15625 Ill' the smallest particles 10 equal the malls of just one' ontlc':'
distribution. given as follows:
largest pan icles. . .
There arc common problems with automatic size analyzers. The finn is COincidence;"
F(D) = I - exp!-D"ID/)
: When more than one particle i~ in the detection zone of IU1 analyzer. they are si~(fas one
large particle. Conscqucurly. the particle size distribution becomes artificially skewet1' .
where F(D) is the cumulative particle size distrib~tion and 0 is a characteristic size cor-
toward the coarse particle sizes. To minimize the problem. lower the ccncerurationof
respo~ding to D,l~' the 'panicle size a(::n%' ~;;"ihe di'stributio~.' The exponent 1/ indicates
powders inthe detector wile. For the streaming devices. that requires dilute conceritrl!~:
the W.ldth of thc distribution. A plotting basis takes the double logarithm to give a lincir
equation. . tions of the powder in the carrier tluid. Secondly. agglomeration causes firie particles to'
appear as coarser particles. Dcagglornenuion requires agitation. milling. and chemica)
treatments to maintain particle dispersion. Another problem results from the relativCiy .
log,ofll/!I - F(D))) ;" 1/ log (D) - 1/ 10" (0 ) 12.291 <'
'U "'II II h IJn SpeCI'fiIC gravity
. 01. most metal powders. Streaming techniques assume a uniform ~
where 1/ is the s'1ope 0 f t h e p If'ot 0 the left hand Side versus 10gio(D).
, random dispersion of particles in the feedstock for the detector. The measurements-can'
The Andreasen . I . di 'b' . . become qi~~d because of preferential settling of the coarse particles. To aS5u~e mini-
. . panic e size istn unon has been linked to optimized packing proper-
ties mum error from sell ling. it is good practice to pass the entire sample through the detec-
. and IS sorn e t'imes . use fl'u m working. with .. high packing
, density. metul powders. It is
tor. ;t~ .
given as follows: '
Many examinations of particle size analyzers have been performed. Under critical
F(D)=AD"ID" assessment. it appears that the particle size distribution can be reproduced with.a 2 per-
L 12.301
cent to 3 percent variation. Figure 2.24 illustrates the cumulative particle size distribution ..
m from a of a coarse spherical iron powder. Between instruments it is common to see at least a
e Slope of
._-_ .. _- /01
1\)\V()1 II MllAllUI;C,y \(11 Nll . 1'( 1\v1 II ,.', '1'\1"\' II 1I11A III IN'

-----------------------------------------~----------------. •.

cumulative mass percent "

100 r----~----_;:==_=~:;:iiI""'_, ~ ~angUlar
t .,

80 Iron spheres
c!) tear drop'
60 urn
. ~CUblc ~/'
:.\t· sponge or

" ;.''''



20 . -. . :",;

'();iPOlygOnal . .:':
. :":
" .
'. rffI:? ~ggregate
10 100
particle slze,llm
V dendritic .: . .~':
. "
FIgure 2.24. A demonstration of scatter for particle sizes analysis results using Ihe same Figure 2.25. A cotlccuon of possible particle shapes and the suggested qualitative
powder and seven measurements of the size distribution with four laser scattering descriptors. .
devices. The powder was nominally a 60 101m spherical iron. Note the variation at thp. 0'0
and 010 particle sizes. '

descriptor is th~ aspect ratio. defined as the maximum particle dimensio~ divided by the
10% difference in the median particle size. and many instruments will disagree by 30 minimum particle dimension. For a sphere. the aspect ratio is unity, while for a ligament I.

percent to SO percent. It is inappropriate to assign high accuracy to panicle size distribu- a value near 3 to 5 is more likely. A flake particle can have an aspect ratio in excess of
10. and in some instances can be as high as 2()(). Generally, microscopy techniques are , .
. tions. "'" "
most appropriate for quantifying shape.
Consider the irregular shaped particle diagrammed in Figure 2.26. Various shape l..

: :Partlcle Shape parameters result from the projected image. Particle shape can also be expressed by the
I •• '''~'.: ;

Particle shape inf1uence~ packing. flow. and compressibility, provides information on ratio DjD A' where Do is the diameter or the .outer embracing circle and DAis the equiva-
the powder fabrication route, and help~ explain many processing characteristics. Because lent spherical diameter based on the projected area. By far. the microscopy based shape
,iUs difficult to quantify panicle shape, qualitative descriptors are frequently used to con- descriptors are the. easiest to understand and arc relatively easy to obtain from projected
. vey a sense of the shape. Figure,t.2S gives a collection of particle shapes and shows the images. , ,
.appropriate qualitative descriptors. A more complex shape parameter can be generated from a profile analysis of a parti-
Particle shape varies with size and manufacturing technique, A panicle size analysis cle. If a radial coordinate system were centered inside a panicle. such as in Figure 2.27,
which assumes I constant shape Could potentially have a large error. For many analyses, then a plot of the surface profile could be constructed. The plot might look as shown on ..'0
~ . .a'simple quantitative shape desc~iptor proves adequate. The most straightforward the right in Figure 2.27. The tracing of the surface position becomes a contour in terms

:..... •. ,-
" ,
,. ,

" particles. Useful because, it often correiates' with ,various ~;and ~etric chara~te'r~
istics. surface area provides. insight into the. powderbc:ha ••• ior·durinl chemical activity.
,I , .J', ' catalysis. friction. adsorption. contamination', P.l'eSS~1 i9d Iintuina. However, the sui-
, ," t;Dol' , \
~--- ,
Do = diameterof "c;wl~r
face of a powder lot tells nothing about the dlsttlbut10n In propcrtiea. pqwdcr texture
or :n~ernal structure. So, it is combined with. C)thti'·paramerers as part or an overall
I' , \
embracing circle
description' of the powder. Two main analysis techniquei ror measuring lurface area an:
DA = diameter of ctrcle with gas adsorption and s= permeability. ',' '. ' j,

equal projected area

Gas Adsorpt~ltSurface Area Analysis .. .
,, The gas adsorption approach starts with a clean powder surface achieved through vac-
;,' ,

_--_ ..• uum or inert gas~Jkeout. The clean powder surface Is cxpolCd CO VlI)'inl partial pres-

'•...... ',' sures of known a!sl)roing vapors. A measurement Is made or the amounl or IU adsorbed
on tho powder surface versus the panial pressure. The mcuUrcmcnl Is often referred to .
Figure 2.26. The projected Image of an Irregular particle and two forms of measuring the as the BET specific surface area, after Brunauer, Emmett ancs Teller who developed the'
size 11'1 terms of the clrcular diameters. concept in 1938. -
,. Under equilibrium. the rate of adsorption equals the rate or evaporation. As illustrated
in Figure 2.28. the BET technique measures the qUJl\llty of iU needed CO saturate the
R powder surface. By assuming each gas molecule occupies a pRelsc area. the surface area
of the powder can be calculated from the adsorptlon behavior. Leuinl P equal tbe panial

::': .... ', ,


nlilalive ~'.

Figure 2.27. A two dimensional particle profile showing one appioach to particle shape .'
tJ by the
ana/yala. The outer particle contour Is used to create a tunctlonal ralation between the
radial length R and the angle e.
~ce~s of
ues are or the lWOcoordinates. Such an approach to conveying particle shape is a specialized
. /.

.: ... ,'.: ....

al~lve 10 the microscopy techniques. While the qualitative and simple quantitati:ve
S shape leclulIques mlly provide too little detail. the profile based techniques have the opposite
hy the
~roblem - each particle is fully analyzed for shape such that with a large number of par-
1I7les there is too much information. Recent efforts have examined the use of fractal
. <;'
shape dlmen.sions as part of the shape characterization. where the apparent perimeter length of
ojected ,a. panicle increases in an inverse relation to the stepsize used to' circuit the particle. A
Simple qualitative description coupled with a SEM micrograph is the most efficient parti-
a pani- cle shape ind'~x in routine
. use. .;-
c 2.27. unsafurated
own on Surface Area Analysis
I tenns '" Figure 2.28. lIiustration of molecular adsorption ona surface and the usa of a monolayer'
1bc .surface area is in average measure of the external condition of a large number of coating at saturation to assess the surface area.
I', 1111111'.11'\1' I' II 1,'1/" II! IN
I'OWDFR Mf1A1IIJl~(iY \( " Nt I --.------ ---_.

pressure of adsqrbale, f" equal the saturation pressure of adsorbate (which depends Oil

the gu and temperature), X equal the amount ofgas adsorbed at a pressure P. X •• equal OUIpUI
the monolayer capacity of the powder (the amount of gas necessary to form a saturated
surface coating one atomic layer thick), and C equal a constant relating 10 the adsorption
enthalpy. give~
time \

P ,. _1- [1+ L- (C.I)] 12.:\21

X(P,;P] X.C P" valves

Note the linear relation between the term on the left of the equal sign and the par.ial pres·
sure ratio PIP". The BET equatlon is generally valid for powders in the: pressure range
PIP" from O.OS to 0.30. Equation 2.32 can be rewritten in a general form as. flowmeter
stabilizer \ I
P IIX (PH' P)/. 8 + A PIP" ID:\I '-- ...J powder I
where .
Figure 2.29. A schematic drawing 01 a nitrogen BET specific surface area analyzer. A
X:''' (A + 8}'1 ID41 clean powder sample is chilled to a tempera lure where adsorption will occur (liquid nitro-
gen temperature in this case). The helium and nitrogen flows are adjusted for a specific
partial pressure .ratio. The gas sample is exposed to the gas mixture. resulting in a
with A as the slope and 8 as the intercept of the linear Equation 2.:\:\. Finally. the specific change in gas thermal conductivity as nitrogen is selectively adsorbed. The area 01 the
surface area is calculated as adsorption peak provides a means of measuring the surface area.

S •• X.N ••A•.'( .••·M] 12.:\51 ,

x[{P 0 IP)-']
using M IlS the molecular weight. of adsorbate, An as the average occupational area of an
ud~orbule molecule, N••u Avogadro's number, and I<' as the sample weight.
A schematlc example or a surface area measurement device is shown in Figure 2.2lJ. tantalum
A glass holder immersed into a chilling fluid holds the sample. which has a gas inlet con-
trolled for panial pressure. .Oases used for adsorption include nitrogen. krypton. carbon 600
specific surface
monoxide, carbon dioxide, water, and benzene. The sample temperature is adjusted to areaec.assrn 2/g
the gu condensation temperature through external cooling. Measurement, are made via
a detector such lis a thennal conductivity bridge. In most instances. multiple partial pres- 400
sures are used to extrac't both the slope and intercept for Equation 2.:\4. However. in
some instances, single point detenninations are made with the assumption of a zero inter-
cept, That approach is quick but less accurate. An example plot of the adsorption versus 200
panlal pressure 'is shown in Figure 2.30. Those data were taken on a fine tantalum ;Ylw.
der using nitrogen. u the ad$orbate. The boiling temperature for liquid nitrogen i~ -196'C lntercepteso
where it hu a molecular occupational area of 1.62. \0.19 m!. By immersing l'le powder O~----~------~----~
o O~
(in its holder) in liquid nitrogen, adsorption can be induced. The partial pressure of nitro-
gen in equilibrium·with the powder can be controlled by pressure regulators or gas mix-
'ing (midn, nitrogen wilh an inert gas such as helium). When the nitrogen is exposed to Figure 2.30. Example of data for 'the spccitic surface area of a fine irregular tantalum
the cold powder. the amount adsorbed is detennined by the pressure drop, the weight powder (mean size of 4.1 urn). The adsorption data have been plotted according to'
increase of the powder. or the change in the thennal conductivity through the gas. Using Equation 2.33. resulting in a specific surface area of 0.399 m2/g.


the partial pressure and adsorption data, a least squarl's analysis gives the slope ;IIHIinter- drop is IIII'aslln.'1I III d,'t\'rlllill,' Ilk' pcnlll.'ahility. llsin~ powder pIIRlllily an,llhcuMi~'al
cept. which .gives• X .11'.. densily. Ihl' specific xurt.u'c area is calculated using Equation 2•.l1(. vCllcrnlly. the tech-
I~ niquc is restricted 10 p,'.rtic.:1l:sill the 0,5 to 50 um range. Often the measured surface otrea
Gas Permeability Surface Area Analysis is converted into an equivalent spherical surface diameler and expressed in' Ihis mlUlllCr
Ison The pcnncability of a gas:'passing through a porous structure is dependent on (he sur- rather than as a surface area. This is commonly reported as lhe subsieve size. Either wuy.
face area. assuming viscous flow of the gas, The Darcy equation for flow in a porous. it i~ \1111)'an approximate measurement 1601 since it docs nol IL~SCSS the dead ended sur,
material gives the tlow rate Q in m,l/s based on the pressur~l~rop M = Pu . PL and the f;ll'~ connected 'poruxity which contributes to the 'BET surface area, However. because
gas viscosity T) as follows: u.e permeability measurement is relatively simple ~n(hhe devices are widely available. ~
:] the subsievc si~es arc used frequently to detail the properties of fine powders, " ;,';
Q=MK"A/(LT)) 12,361
l Surface Area as a Shape Index , '
where the sample length Land cross-sectional area A are as shown in Figure 2.3 I, The The specific surface area is expressed in terms of the area per unit mau (ml/g), Fo;.,.
parameter K" is known as the perrneability.cocfflcienr. The gas velocity exiting from the monoxizcd spheres, the area per sphere A and the volume per sphere \I arc:,given as. :
low pressure side is given as.

\I = n 1)'/,6 12.401
! area analyzer, A with V equal to the flow rate per unit area (Q/A). Based on an analysis b), Kozeny and
Cannan. the surface area of-the compact is related to the permeability through the porosi- Note the area per unit solid volume is 6/D, The weight W of a solid particle is calculated
occur (liquid nitro-
Isted lor a specific from the particle volume and theoretical metallic density P",
ty e as.
ura, resulting in a
d. The area of the IV = P., V 12.411
s= _[I ' E,I
]1/2 12J!l1
P"' 5K( "E)2
Consequently. the area per unit weight (S = A/W) is given as
with PHI equal tothe theoretical density of the material. In Equat-ion 2.38 the porosity E is
.J=o/(DP.,J " 12.421, ..
the fractional void' space out of the total volume:
Surface area measurements based on the permeability of the powder use a subsieve
sizer.·A preweighed amount of powder is exposed to a known ,f1?W rate and the pressure where S i~ the specific surface area, For a polydisperse powder (a powder with a wide'
..' . . . size range). the mean particle size on a population basis provides a first estimate for the'
di ••meter in Equations 2.39 through 2.42, Convenient units for size. surface area. and
density are 11m. m2/g, and g/cnr'. respectively, When these units arc used. the conversion
factors cancel in Equation 2.42.
If a different particle shape is assumed'in Equation 2.42. then the relation between
particle size and surface area would be different, A general fonn would be as follows:",:

--- PI,.!)o PL
toP = Pu- PL S = k.' (D p ••J
--- , .' .. .':." ",

where kJ is termed a particle shape factor, lr is possible to make a rough determination

panicle shape by comparing independent measurements of particle size (on a populatlon ;
,'.. j\":

A powder tube basis) and specific surface area through theplculated proportionality constantk'. Use"
simple shape models to determine the shape 1:onstant for a monosized powder, ' ',
Figure 2.31. The deterrnt r
measuring the flow rat I~a Ion 01 powder surface area by gas permeability is possible by
regular tantalurTl ferential. e a a gas through a packed powder bed at a known pressure dit- : -.:

ted according 10'

68 69
"OW""." : 1"1'". " III/Allr)N

A shape factor Ie, tllat Iinkri panicle size and specific surface area can be calcu-
lated for most geometric shapes. It is influenced by the parameter selected to mea-
sure the particle size. Consider a cylinder shaped particle with a length twice the I,
diameter D. Using the diameter as the size parameter measured by screening. thc
~urface area A is given as: ' a = angle of
A = 2 1t [)1 + Tt D112 = 512 1t D!
and the volume is tan(a) = hlr
V. (1t [)114)(2 D) = 1[/2 [)1

and the weight is the density times the volume P. V. Thui the specific surface
area S. is
S -, A I (V P.) = (512) 1t D11/(//2) P,. D' Tt/ = 51 (D P••i
"Figure 2.32, Theang:e of repose is a measure of the interparticle friction, It can be deter.
For screening, the particle will orient to pass through a mesh that is equal to or mined from the height and radius of a powder pile passed thr?ugh a funnel.
larger:than the particle diameter. Thus, the average particle size will be measured ••• ~ ••••
" II,

as the cylinder diameter D and the value of 1:,is 5,0.

Aliernatively, If the particle size is obtained by measuring the equivalent
spherical volume diameter DV' then,
Tt D/ 16 = Tt D' I 2
Vfunnel "
or D" =3 11
,1 D
Thus. combining equations gives baffles

S =A I (V P••) = 5 / (Pm D,.) = 5 3 11 1

• I (P•••D,.) density
which gives a Ie, value of 7.21.

Half Scott

Interparticle Friction
\ #
Under the general heading or interparticle friction come two main concerns: powder
flow and packing. The friction between particles is dominated by the surface area, sur-
Figure 2.33. The basic components of the Hall flowmeter and seen volumeter for mea.
suring the flow and packing of powders.

face roughness, and surface chemistry. As the surface area increases. the amount of fric-
book density for a powder: the density when there is no porosity present. The angle of
tion in a powder mass increases. Consequently, the particles exhibit less efficient flow
repose is another friction index, It is the angle a formed by pouring a powder into a pile"
and packing. Those concerns are important to automatic die filling during powde! com-
as shown in Figure 2.32, where the tangent of a equals the height divided by the radius
paction, as well as packaging, transportation, blending. and mixing, '
of the loose powder pile. The angle of repose is also observed by tilting or rotating pow-
Resistance to now il a main feature of friction. The density or packing properties
der to the angle 'where it naturally flows. Finally, the [low. rate is a measure of the rate a
decrease because of poor now past neighboring particles, Consequently, attention is
powder will feed under gravity through a small opening. Mos!.small, subsieve powders
given to measures of the interparticle friction. Apparent density. or bulk density. of a will not flow due to high interparticle friction. Such powderxarc termed non-free flow-
powder is the density (mus/volume) when the powder is in the loose state without agita- ing and arc difficult to fonn,
tion. Tap density il the highest density that can be achieved by vibration or a pcwdcr
Various devices can measure apparent density, Examples of both the Hall flowmeter
without the application of extemiJ pressure. 'Theoretical density corresponds to the hand-
and the Scott volurnercr are given in Figure 2,:n, The Hall flowmeter is used for the
, ,.
70 ", .

coarser particles measuring both the flow rate and the apparent density. The Scott device Thus. as the only unknown. the powder volume can'be calculated.
is applied to smaller powders which do not freely flow because of a high interparticle
friction, The Arnold meter minimizes powder flow by using a ring containing powder to VI' = VJ'"+ V (I - PIP :
)./ (2.45)
directly fill a 20 ern? cylindrical volume. That technique best correlates with the filling. of
die cavities in powder compaction operations., ' , The powder mass divided hy the volume gives the pycnometer density. Since sealed
The flow rate is usually expressed as the time for 50 g of powder to flow through the pores in the particles can not be accessed by the test gas, the pycnometer density can be
, Hall flowmeter. Short flow times indicate free flowing powders while long times indicate lower than the theoretical density. The typical accuracy is 1%.
high interparticle friction. The apparent density and flow times are easily obtained with , In most all applications involving powders, high packing densities are desired.
the Hall flowmeter by combining a precision volume cup with the funnel. The apparent Improved packing densities arc possible by adjustment of the particle size.. shape, and
density is the weight of powder divided by the cup volume. The precision falls between I size distribution. The higher the packing coordination, the higher the observed powder
percent and 5 per~ent and .the, typical apparent density is between 30 percent to 60 per- oensity. The f.o;ordination number is the number of touching neighbors that any p~icle
cent of the theoretical density. ' has in a po~tr ensemble. and is synonymous, with the number of nearest neighbors.
Another simple test for interparticle friction is the tap density. Powder is vibrated in a Small particles will have more interparticle friction, giving a lower number of nearest
cylinder for IOOOto 3000 cycles at 284 cycles per minute using '1 3.2 m~ throw from ~n neighbors. Everything else being equal, the smaller the mean panicle size, the lower the
eccentric cam. Usually the initial powder volume is 25 rnl. The occupied volume Will apparent density. For a coarse spherical powder, the packing fraction for loose p~cking'
decrease rapidly with initial vibration and eventually reach a plateau value. giving the tap (corresponding to the apparent density) is usually near 60% of theoretical and the tap
r can be deter- density as the weight divided by the final volume, It is higher than the apparent density, density is near 64* of theoretical. The cocrdinatlonnumber exhibits a distribution
Both the tap and apparent densities can be expressed as fractions of theoretical density. around a mean value. For louse packed, monosized spheres, the mean coordination is..'
The pycnometer density is sometimes given to assess the theoretical density of an between six and seven. Generally. in random packing, spheres pack more efficiently than
unknown powder or the amount of closed-off (internal) porosity. A pressurized gas (usu- any other shape. .
ally helium) is used to measure the volume of pores in a powder of known mass. in a It is possible to assess particle shape and friction characterization through the apparent
sample chamber of known volume V, but unknown powder volume VI" Initially. the and tap densities. The ratio of the tap to apparent densities gives a signature characteris-
chamber is at a pressure PI" As shown in Figure 2.34. there is a calibration chamber with tic of the interparticle friction. and is called the Hausner ratio. useful in categorizing rela-
volume V" connected to the sample volume. It is initially evacuated. After the connecting rive interparticle friction. For a spherical powder. the tap to apparent ratio will be slightly
valve is opened. the pressure decreases to Pr Applying the ideal gas law gives. above unity. More irregular particle shapes undergo a larger density increase with vibra-
'ion. resulting in a higher Hausner ratio. .
P, (V - V ) = P, (V - V + V) \2.441
J t • J " "

"," -,,' ' .••·1··· One of the main uses for metal powders is for fabricating complex shapes by com-
paction. Accordingly. the compaction behavior is an important characteristic.
, pre!jsure
sensor calibration Compressibility. or compactability, measures the ability to densify a powder under an
~ chamber applied load. The typical test geometry is a sjmple cylinder or rectangle. The die is
ter for mea- /'" (volume = V e) loaded with powder and the density is measured after compaction at a predetermined
~~~vacuum pressure. often near 414 MPa (corresponding to 30 ton/in1 or 60,000 psi). That is termed
valve the green density and is the basis for expressing the compressibility. For a com~tion
h~ allg'le of sample grade of iron or steel powders the green density might be 85 to 90% of theoretical. A
Illto a pile, powder chamber parameter used in tool design is the compression ratio C/I'
the radius (volume = V p) (volume = V 5)
tating pow- ,·r· 12.46}
f the rurc a Figure 2.34. A schemSitic d' '
using a p cno t lag ram of the true volume measurement for a loose powder
e POwders pressure ~ea:~eer. The powder of known weight is placed into the sample chamber. and where \lL is the volume of the! loose powder, Vc' is the' volume of the compacted powder,
-free now- ed calibration VOluments are made before and after equilibration with an initially evacuat- p. is the green density. and P" is the apparent density. A high interparticle friction will
me. give a low initial density. but other factors such 3S panicle size, chemistry, lubrication.
ed for the 72 73
---------------------------------------------------------- 1'0 vt)1 I; (

and metallurgical properties will determine the pressed density. ofth
. A'typic;!1 atomized iron powder has ,10 apparent density of 2.9 glcm \ and com-
pacts to a density of 6.71( gjcm" at 414 MPa pressure. The compaction ratio is redu

c, = P, / p. = 6.7H /2.9 = 23-1

If the powder was compressed to a height of 18 rnrn, then the initial powder fill
depth for uniaxial compaction would have to be 42.1 mm (18 times 2.34).

Figure 2.36. The scanning electron microscope is a polent tool in characterizing metal

powders. In example a) three layers are evident in the fractured particle. The picture also
Powder Structure shows satellite formation and agglomeration In this gas atomized alloy powder, In exam- beo
ple b) the fractured centrifugally atomized particle shows clear evidence of the solidifica- diffr'
A magnified cross-section through 'a powder reveals artifucts that indicate 1';lbriCltion tion events (photo courtesy of.J. Hawers). . :.

conditions and possible processing problem's. Cro,ss-~ectional analysis provides inlonna-
• appr
tion orliftlternol pores, segregation and can he Lsefu{ in detecting inclusions and oxidcv, production. III Ih;11c.r-c. rhc pll\\li.:r i-, cuu.uucd ill ;1 nickel ekt:troplatill!! d.:pn,il where Adv
. Figure 2,:l~ shows Ihe internal structure of two powders. TIle first powder i~ a ~pheric;d il is ~uhst:qu.:nlly 'l'Clil1l1.:d .IIHI illil nul lvd rill' electron truuxparcncy. However. -uch Mici
_ .-.!!!l.oy pow.der,_1]le, ~Ich~d ~_r:os.s~~,C!!ol1
show~ a large gas-fjlle.(LW.fe and radial crack-, efforts arc uvuallyrc-u'ictcd to the 'l'c'CI;dl\ powder», such as supcralloys .. sitio
. ' ~ The second powder i••irregular in shape with con ••ider ••ble porosity in the panicles which In xumc ill~talln·'. uuportanr micro-uucuu c iuform.uion can he gained hy SEM analy· sine,
inhibit!! packing. compaction. nnd attainment of high final properties. Such' microxtruc- ~is. Fieurc 2..~6 illll'lr;IIl', one ilhlal1c·,· 1\ here the particle fractured to reveal I\VO vhclls usin
lures indicate subsequent processing problems since internal pores arc difficult to climi- around a ~mall p;Ir\lck core. '\ddllilll1;dl~, uuclc.uion ~il':~. cout.uuination. t:lllllill~ rail'. near
nate. To observe the internal powder structure, mix loose powder wit~l a metallurgical !!r••ill size. ;1I1d,..:!!rl·!!;lIi'"1call he' a",'",11 Irom SEM examinations. Further information pre.
mounting epoxy resin. The particles seule during curing of the resin. Subsequent polish- on the powder C;l;l I~' ~;Iin,d hy ,urran' ;l1l;dy,i~ tonlx. These arc appropriate 111the char-
ing and etching of the mount brings out the panicle microstructure. Tranxmiscion clcc- al'leri/alilln 111'1'"I\(kr, -cnxitivv 111,'lIlll;lIl1il1;l!io1\,Thermal analysi •• providc-, another
Iron mi~mscopy ha.•• also been u~d to observe the solidification events during powder A
imponan: mcan-, 111'a"c'"ing Iii..: I'",,,kr, Included in these techniques arc ditfcrcnriul
thermal analvsi-, for detection or pha-c u'au-Ioruuuiou» and melting events. dirrt;r':lltial
scanning c;Ii;lriml'lry ror quantific.uion of endothermic and exothermic events. and thcr- teri
mogravimctric analy,i, for determination I\l'ight loss due to desorption and evaporation
:1 pro
during hearing. mir
Chemica. Characterization pol
When di~cussillg their chemistries. powders must be subdivided into three groups, pol
The elemental powders arc rel.uivc ly high·purity materials where chemical analysis
focuses on the impurity concentration. Premixed powders arc combinations or two or to
more distinct powders that will diffusionally alloy in sintering. An example would be the bu:
use of mixed 'copper and tin powders 10 Iorrn a bronze a1l9)1.Impurity levels and proper we
'. Ty
compounding of the mixture arc chcmicul conccrns with tile premixed powders, The pre-
Agure 2.35. Two example micrographs of cross-sectioned metal powders showirg how alloyed powders constitute micro-castingx with multiple elements in a predetermined
Internal mlc:roauctutal details can help In characterization of,the powders; a) cp.ntrifugally ratio. For the preulloycd powders. uucntion is given to the alloy composition as well as
atomized steel alloy powder. and b) water atomized Iron poWd8[1(photos courtesy of J. the impurity concentrations. Normal analYlical chemistry techniques are appropriate for
O\napandJ ..~), . ,f',,,-
all powders.

~'I' "'"'''i'~'


Beyond the bulk chemical information, the surface condition is an important property Tablr 2.7, Puwdt'r Cha"'oIrh'ri1~lliclIIfur Ihr TunJ:.<ilen Powder Shown In "i~ur~2.-'7
of the powder. Hence, there is concern with oxides, adsorbed organic films, and the prcs-,
encc of surface coatings like silica to determine appropriate cleaning treatments. A loss Material = Tungsten
on reduction is reported to show the weight loss when heated in hydrogen at a low tern- Designation = -325 mesh
perature. This measures the surface oxidation as well as volatile organic content and Metallic Chemistry =
99.99% W •

reducible compounds and is less sophisticated as compared to thermogravimetric analy- Impurities (ppm) = C (10), Cu (I I. Fe '(2), K (15), Mg (4), Mo (10). N (100), Nu (6), .•

sis. Likewise, the inclusion concentration is measured by acid dissolution. For some 0(740), Si (2)
materials, the powder hardness provides a gross gauge of the impurity level and assures Apparent Density = 4.37 g/cnr' (23%)
that the powder has been annealed. Often the elemental iron powders are derived either Tap Density =8.05 g/cm' (42%)
from ores or metal scrap. The ore based elemental powders will usually have less lot-to- Flow Time for 50 g = not free flowing
lot chemistry variations than the scrap based powders. On the other hand, the ore based =
BET Specific Surface Area 0.12 m!/g
powders tend to have higher inert or oxide inclusion contents. Powders fabricated by =
Gas Permeability Surface Area O.02X m!/g
melting techniques provide greater opportunity for chemical refining. and can be expect- Particle Size by Sedimentation
·terizing metal ed to have higher purity. .
Depending on the desired sensitivity. bulk chemical characterization 01 a powder (an
DII.= 3.0 prn
e picture also D". = 6.4 ~1l1
der. In exam-
the soiiditlca- .'
be obtained from wet analysis. emission or name spectroscopy. atomic absorption. x-ray
diffraction, x-ray fluorescence, or neutron activation analysis. Emission spectroscopy
DVI.= 12~m

.. and x-ray fluorescence are typically used for routine analysis. with lower sensitivities of Particle Size by Electrical Zone Scnving
approximately 10 ppm (pprn is the standard abbreviation for parts per million or l O'"), D." = 3.5 pm
ep("il where Advanced techniques arc capable of extending analytical accuracy to the 0.0 I ppm level. 0.".= 6.2 ~1l1'
1Wl·\,er. such Microanalysis by electron or ion beams is useful for characterizing the chemical compo- D",. = X.9 ~1l1

sition in small volumes. The microanalysis techniques are not useful for routine analysis
• SEM analy· since they are typically semi-quantitative and slow. Finally. surface analysis is possible

al 1\\'1I ,Ilells using Auger or other research techniques. Here low energy electrons arc stimulated from
(llolin~ rate. near-surface regions. These electrons convey infonnation related to the chemical species
informalion present on the powder surface. •
! 10 Illl' char-
ide, annllll'!'
, dil'kreillial A Minimum Characterization Battery
. dil'i't;rl:llIi'al
.It is rare that a full battery of measurements is either needed or warranted to charuc-
IS. and thcr-
: ('d tenze a metal powd er, Th' e typical goal 111 . powder metallurgy is to control the process to
eVaporalion provi e a standardiz d ad
. . e pr uct. Powder characterization is geared toward performing the
m1l11mum amount of t . .
research dd estll1g necessary to ensure consistent feedstock to the process. In
and und an evelopment
a I" h ... ..
pp icanons, c aractenzauon IS necessary for future repetition
powder to
ersran 1I1gof the I F
resu ts. or that purpose. a few tests should be performed on a ,

ensure control Oft h .

irce groups. powder cha .. . en t ey are relegated to the manufacturer who certifies the
t:11 an;lIysis In the characterizati f
Sol' Iwo or to perform and I' on 0 a powder, the test should be meaningful. accurate, and easy
rep icare E h .
ould be the bulk chemistry th d . mp am should be given to the powder chemistry. Beyond
and proper weight loss me~sur: egree o.f ~ontamination should be determined using hydrogen
rs, The pre. Typically, a scannin mC~ts. 11 IS I.mponant to obtain a reliable particre size distribution.
parison to some S\angdedectroh micrograph will provide sufficient shape detail for com- Figure 2.37. A scanning electron micrograph of the tungsien powder as characterized In
ar S Add' . Table 2.7.
as well as . uionahy, one or more of the simple tests for interparticle
ropriate for
---.-- ------ II
-------------------------_. ---~~---------------------------
friction should be given to provide a relative assessment of now, mixing, and fnction International. Materials Park. OH. Il}X4.
behavior. Finally. in some materials. it may be necessary to examine the internal ~truc-
H. D. Lewis. "Sm;J1I Panicle Statistics: The Analysis of Particle 'Size' Data." TesliD.!:
ture via metallography techniques for pores. inclusions or second phases.
Characterization of Powders and Fin~ Particles, 1. K. Bit and T. Meloy (cds.).
In most instances, not all of these characteristics need be measured: however. in
Heyden. London. England. 1980. pro 1.t5-175.
research situation!! a broad test battery is reasonable. Table 2.7 gives an example charae.
terizatlon of the tungsten powder shown in Figure 2.:n. It is a high purity elemental pow- S. Lowell and J. E. Shields. Introduction III Powder Surf;tce Arca·and P(lrosily. john
der with a specific surface area indicating an irregular panicle shape. as seen in t!"lescan- Wiley and Sons. New York. NY. IlJX4.
ning electron micrograph. The particle size distribution by two techniques gives a medi-
G. Matei. N. Claussen and H. H. Hausner, "Influencc of Relative Humidity on Flow of
an size near 6 11m.while the SEM shows individual crystals from 0.5 to 311m. The low
Metal and Ceramic Powders." Modem Dcvelopments in Powder Metallur~y. vol. K. H.
packing densities. lack of flow, fine size. and irregular particle shape are consistent with
H. Hausner and W. E. Smith (eds.), Metal Powder Industries Federation. Princeton. NJ,
one another and indicale an agglomerated. snail powder. Generally. the goal of such an
1974. pp. 5-11.
analysis Is 10 obtain specific information of the panicle size. shape. friction and structure
as well as lhe chemistry. The appropriate combination of tests will. of course. be modi- T. P. Meloy. "Particulate Shape Characterization." J. Powder Bulk Solids Tech .. 1978.
fied for the Iype o~ powder under consideration. vol. 2. no. 2. pp. 13-23.
R. Meyer. '''Standardizing Test Method» fill' Characterizing Powders." ), Powder Rulk
Suggested References Solids Tech,. 1979. vol. 3. no. 2. pro 21-27.
A. Adler. "Flow Properties of Metal Powders." IDler: J. Powder Met" 1969. vol. 5. no. I. M. J. Rhodes (editor). Principles of f>mnkr T.:chnology. John Wiley and Sons. New
York. NY. 1990.
T. Allen. Particle Size Measurement. fourth edition. Chapman and Hall. London. UK. 2.1
L. M. Sheppard. "Automation of Particle Analysis." Ceramic Rull .. 1988. vol. 67. pp. pial
87R-883. an;
J. K. Beddow. Particulate Science and TechnQlo~y. Chemical Publishing. New York. J. D. Stockham and E. G. Fochtman (elk l. Parlit:1e Size Analysis. Ann Arbor Science 2.1
NY. 1980.
Publishers. Ann Arbor. Michigan. 1977. in
J. K. Beddow and T. P. Meloy. Advanced Particulale Momholo~y, CRC Press. Boca siz
L. Svarovsky. Powder Testing Guide. Elsevier Applied Science. London. UK. 19K7.
Raton. FL. 1980.
J. F. Waus and T. J. Carney, "Surface ChclI~ical Characterization of Powders," P()\:dcr
R. O. Grey and J. K. Bit, "On the Hausner Ratio and its Relationship to Some Properties mi
Metallurgy - An Overview. I. Jenkins and 1. V. Wood (eds.), The Institute of Materials.
of Metal Powders." Powder Tech •• 1969. vol. 2. pp. 323-326. me
.. London. UK. 1991. pp. 76·91. m(
M. Ghadiri, F. A. Farhadpour. R. Clift and J. P. K. Seville. "Particle Characterization:
Size and Morphology." Powder Metallurgy - An Overvjew. I. Jenkins and J. V. 'Wood Study Ouestions
(eds.), The Institute of Materials. London. UK. 19<)): pp. 56-75.
2.1. A 200 s sample is used to measure Ihe panicle size .of spherical nick~1 pO\~.dcr.TIt~
A. Guinier, G. Founet. B. Walker and K. L. Yudowitch, Small Angle Scanerjng. John average size is 120 11m.roughly how many particles arc IIIthe sample? (NI density IS X.1
Wiley and Sons. New York. NY. 1955. g/crrr')
H. H. Hausner and M. K. Mal. Handbook of Powder Metallurgy. second edition. 2.2. A powder with an ellipsoid shape (lcnglh = 120 11mand diameter. = 60 11m)is sized 2.
OlCmical Publishing. New York. NY. 1982. by screening. What panicle dimension will best correl~te to the mesh size? m

2.3. For a cubic panicle of sides 3 urn. a) what is the equivalent spherical surface diame- gJ
W. I. Huppmann and K. -Dalal, Meta!J0CC30hic Atlas of Powder Metallurgy. Verlag
Schmid. Frieburg. Gennany. 1986. ter. and b) the equivalent spherical volume diameter? ;.. , 2
B. H. Kaye, "Review' of New Methods for Characterizing the Shape and Texture of Fine 2.4. Iron powder is screened into -'I &)/~2(i() m'~sh and -325 m~sh fractions. The apparent P
Particles." I. Powder Bylk Solids Tech., 1982. vol, 6. no. 2. pp. 1-4. density of the coarse fraction is 2.6 g!cm \ and the line fraction has an apparent dc~slty of
2.3 g/cm'. When a blend is prepared using. 20% fine panicles in the coarse Iruction, the
Eo K1ar (editor). Powder MetaJltu:EY, vol. 7, ninth edition of Metals Handbook. ASM , .

1\ "VIII /( U ~nRllATION

nt density is measured as 2.8 g/crn'. Explain the effect. prn. However. the other properties are quite different as noted below:
5 Air is penneated through a tube of I cm2 cross sectional area by I em lone contain- I. [l9wder A powder B
specific surface area. m~/g 0.26 0.12
Dara." Testin~ ~.. Iybdenum powder with an apparent density of 4.5 g/crn'. At one atmosphere pres-
apparent densuy, g/cm' :U 4.5
. Meloy (cds.), . rno
mg differential (2 atmospheres to I atmosphere) the measure d fl ow ve I"ocuy IS 0 " I 'i tap density. g/cm
sur/c. What is the equivalent spherical diameter'! (air viscosity = 1.8· 10'· gicm/s. Mo ~,6 8.1
em s. . , .
1 Porosity. John theoretical density = 10.2 g/cm ) a) Explain why there might he a difference in surface areas.
2 .,6 Exp lain why the flow time (in the Hall flowmeter) is observed to increase with the b) What equivalent sp~erical dial.Heler woul~ give the same surface area.~ for each powder'!
ratio of the tap density to apparent density? c) What differences might explain the packing propenies?
d) What addiuonat information would be useful?
2.7. The' oxide on the surface of aluminum powder can be used to form a dispersion :or
strengthening the consolida~ed powder. For. a 10 11mparticle di.amet~r and ~ ;5 nm thick 2.17. ~alculate th: upward gas Ilo~"'.velocit~ for air so that a 10 urn panicle of le'l2 will
oxide surface layer. what will be the consolidated percent of OXIde dispersoid? be levlt~ted (held III a constant posinon) against gravjty, (air viscosity =
1.8.10-1 giS/em.
arr density = 1(;··1g/cm', Pb theoretical density = 11.4 g/cm')
2.8. What powder characteristics might cause the surface areas to differ when measured
by permeability and by gas adsorption? 2.1 It Data arc collected by sedimentation for an aluminum powder (theoretical density =
2.7 g/crn:') as follows:
I. Powde'r Rulk 2.9. The Reynolds number must be below approximately 1.0 for Stokes law to be valid in
siz-: r;J.nge. pm weit:hl,:,:
performing a sedimentation analysis for particle size. For aluminum spheres settling in o to I (1.O
lnd Sons. New water, what is the maximum particle diameter for which sedimentation is valid? (density I to 2 0.4
of AI = 2.7 g/cm', density of water = 1.0 g/crrr'. viscosity of water = I0 ~ gis/cm)
.. 2 to 4 5.5
2.10. Set up a quality control flow chart for testing incoming powders at a P/M parts 4 tu X ., 2.l4
8. vol. 67. pp.
plant. The flow chart should include the minimum. but necessary. steps needed to ensure 8 to 12 IlJ.O
, an acceptable and repeatable powder. Nominally. the powder is -I ()() mesh iron. 12 to 20 17.6
Arbor Science 20 to 32 5.lJ
2.11. The ratio of the tap to apparent densities has been proposed as a particle shape
32 to 44 1.1
index. Discuss such a ratio and the possible combined influence of particle shape and
size. 44 to XX 0 ..1
over XX 0.0
!luers." Powder 2 '.12. A polydisperse powder sample is analyzed for particle size using optical a) Give a particle size distribution plot showing the cumulative weight percent versus the
te of Materials. microscopy, giving a mean size of 13 urn. A second analysis is performed using scdi- 10glOof the particle size. .
mentat~on. giving a mean size of 28 11m.Give some possible reasons for the difference in b) What is the mean panicle size 1111 a weight basis?
mean sizes.
c) Estimate the mean panicle size on a population basis.
2..13 ·Calc~late the shape index k in Equation 2.43 for a regular parallelepiped panicle d) What techniques could be applied tll the size analysls of this powder?
wit han axial ratio of 1:2:8.
('I powder. The
. '2.14. Two laborator' d
J •

2.19 ':A spheri~al .20 11m part ide lIf ~itallium (theoretical density 4.5 glcm·1) has a ~ urn
Ii density is X.lJ laborat res con uct sieve analyses of an irregular shaped powder. The first
spherical VOId 111 ItS center. What will be the terminal settling velocity for this particle in < I
a few ;~i~I~;s the mean size as 54 11m,while the second claims it to be 75 urn. Offer water? .How d.oes that com.pare to the terminal velocity for a pore-free particle of the '
)0 urn) is sized ypotheses Why the values differ. same diameter? (water density = I g/cm:', viscosity = 10.2 glcm/s)
» 2.15. Approximatel h . 2.20. How might mixed P'~~;ides of copper and tin be separated from one another?
mesh iron powd y ow ma~y panIcles are contained in a 10 g sample of +325/-270
surface diarne- g/cml)
er and what IS th
. ..
e estimated surface area? (theoretical density = 7.86 , (.

2.16. Two different tun rste

>. The apparent panicle size using g ~ powders (theoretical density = 19.3 g/crrr') arc analyzed for
a stream IIlg t h .
ircm density of cc ruque and found to have an equivalent mean size of 5
se fraction. the