METALLOVEDENIE I TERM. OBRABOTKA HB No.

5530
METALLOV, Dec. 1960, No. 12, pages 26-30, 35-36

E F F E C T OF A L L O T R O P I C TRANSFORMATIONS
ON T H E S I N T E R I N G OF I R O N P O W D E R

Dr. teeh. sc., Prof. A. A. SHMYKOV and Eng. V. S. SAKLINSKII

A l l - U n i o n Correspondence Institute for Machine Design and Research Institute
for A u t o m o b i l e Manufacturing Technology

Sintering of iron powder compacts is characterized chiefly by a decrease of porosity [1]. The determination
of l i n e a r shrinkage during sintering was conducted d i l a t o m e t r i c a l l y . Fig. 1 represents a typical d i l a t o m e t e r record
during sintering of an iron powder c o m p a c t with 0.05% C.

ALl0J
~ ir ' ~f-~J.lo-~
23~ X ~ ~ m~" 9
,O I1 I.I• , 1:3

70 I I I \ ..// .... !_ ~ -_# - J

l i t X oo~ 5
, I~50 ~ ~ ,aL/l .V'I 1 I/lGd "1 l_j
1 lO ~ /
o l,,'i" I..I ~. , II1t
mm 0 ~~
-2 A['lO~ | /

1000~C 1 2~ . . . . . . .
A A ref \ 875 ~ 1 .... I
\ .500 ~
b
723 ~ !700 ~ t000 ~

Fig. 1. T y p i c a l d i l a t o m e t r i c record during Fig. 2. Dilatometric curve constructed from the

sintering of a pressed iron powder sample: a c t u a l expansion of specimen, using the scale factor
A - l i n e a r expansion of reference (arbitrary of d i l a t o m e t e r (a) ; curves showing the changes of
units), Ysp - true d i l a t a t i o n of specimen. shrinkage c o e f f i c i e n t in various temperature ranges
03); A and B - theoretical curves corresponding to
theoretical d i l a t a t i o n coefficients of ferrite ( c~ = 14.5
• 10 -6) and of austenite ( a = 23.0 x 10-s); V - e x -
p e r i m e n t a l l y obtained d i l a t o m e t r i e curve of Armco
iron; G 1 and G 2 = d i l a t o m e t r i c curve of specimen of iron powder compact; G y h e a t i n g ; Gz-cooling; 1) from 25~
to r e c r y s t a l l i z a t i o n threshold; 2) from recrystallization threshold to A%; 3) Ac I to A%; 4) above A%.
Fig. 2,a shows the d i l a t o m e t r i c curve constructed from the a c t u a l d i l a t a t i o n of the specimen, taking in account
the scale factor of the d i l a t o m e t e r . It is known that

Y ~--- K L o (A -- A ): K L o AI,
spee ref

665
 for the d i l a t o m e t e r used in the experiments, its scale factor K = 318.918 and the initial length of reference and
s p e c i m e n Lo = 50 ram. It follows that

Y
hl -- ( mm/mm) or
318.918. 50

AI. 10 3 - Y
15.95

The coefficient of linear expansion is

hl mm
( X =
At mm~

The straight dash-dot lines seen in d i a g r a m Fig. 2,a in A l - t coordinates give the coefficient of linear d i l a t a -
tion which is 14.5 x 10"6 for a - i r o n and 23.0 X 10 -6 m m / m m ~ for 7 - iron [ 2 j .
It is seen in Fig. 2,a that the d i l a t o m e t r i c curves obtained during sintering of the specimens show a smaller
linear expansion than those for a fusion-made specimen; also for its coefficient of linear expansion.
The difference between dilatations of a cast and porous specimen represents the shrinkage at various t e m p e r a -
tures. The d i l a t a t i o n difference referred to a certain temperature range (local slope of curve) represents the coeffi-
c i e n t of linear shrinkage during sintering

(Mcast--Alpor) E Al
At At

The negative sign indicates contraction of the specimens.

Fig. 2, b contains linear contraction curves for various sintering temperatures of iron specimens with 14% ini-
t i a l porosity. Based on a number of experiments on pressed iron powder specimens with an initial porosity of 14-16%,
we obtained the following coefficients of linear contraction: in the temperature range 2 0 - 5 0 0 ~ - 1.0 x 10 -6
m m / m m ~ (relative to a curve corresponding to a coefficient of d i l a t a t i o n a = 14.5 X 10-6).

Temperature, ~ Coefficient of dilatation,

mm/mm~

5 0 0 - 723 4,5 9 10 -6 to 10 , 10 -6
723-900 19 9 10 -6 to 2 2 . 1 0 -6
Above 900 3.10 9 10 -6 to 3.80 9 10 -6

An analysis of the values and curves of the coefficient of linear contraction of porous specimens obtained dur-
ing sintering i n dilatometers (specimens wetted with alcohol to prevent oxidation) shows that the coefficient begins
to change at the recrystallization threshold,which for iron is t_ = 45 0 -500 ~C. Up to this temperature the shrinkage
coefficient is very small. Shrinkage of the specimen below 5~0~ if there is any, proceeds only on account of dis-
p l a c e m e n t of the particles of the c o m p a c t during linear expansion and an additional densification of the entire speci-
men; the shrinkage at these temperatures will evidently increase with the i n i t i a l porosity of the pressed blanks.
At temperatures above the recrystallization threshold, the shrinkage process (sintering) begins to develop v i -
gorously, Fig. 3, this being connected with the formation and growth of new grains inside each i n i t i a l l y cold-worked
m e t a l p a r t i c l e . This grain growth affects the grain boundaries by distorting and displacing them; the latter, in turn,
results in a formation of new contact surfaces, reduction of porosity and, in the final account, in a process which
could be described as the initial stage of sintering.
Due to r e l a t i v e l y low temperatures, the diffusion processes (self-diffnsion) in the newly formed grains do not
proceed to c o m p l e t i o n since an ordering of the crystal lattices has not as yet taken place. For these reasons the

666
strength of the sintered blank at the temperatures indicated is still unsatisfactory.
The highest coefficient of contraction is reached during sintering in the range of allotropic transformations
(for iron at 723-900~ where it is 2.5 to 4.4 times that at 500-723~ This is accounted for by recrystallization,
formation of new phases and the resulting redistribution of phase boundaries, formation of new contact surfaces and
liquidation of preexisting pores.

~l I0 3
Y
mm
9
140
B
120
7

190

5 ~D

#
~0
d
to
2 -
20

0 -

! -

- 20

2 -
- 40

3 -

- 60

5 - - 00

Fig. 3. Dilatometric curves obtained during sintering of iron powder compacts above
the recrystallization threshold. (Between 500 and 1000~ in 100~ intervals).

The gas pressure in closed pores increases during sintering. However, during recrystallization the gas is ex-
pelled from such pores and their internal pressure fails, this also assisting in reducing the overall porosity.
Above the upper temperature of allotropic transformation (for iron above 900~ a further shrinkage is caused
by grain growth of the newly formed anstenitic phase. Nevertheless, experiments show that the shrinkage at these
temperatures is very small; the coefficient is one-sixth to one-seventh that at 723-900~
An ordering of the crystal lattices in the austenite grains occurs above Ac3 ; the processes of self-diffusion and
diffusion of carbon within the grains terminates,and 100 qo completion of the sintering process coupled with a strength-
ening of the compacts takes place. After the sintering process is finished, the cooling curves obtained on the dilato-
meter coincide with those obtained on massive fusion-made specimens, the slope of both curves being identical.
Fig. 4 illusfrates the extent of the final shrinkage, after cooling. A graphical differentiation of the curve in
Fig. 4 shows that the change of shrinkage with temperature (slope of curve in Fig. 4) reaches a maximum near the
Ac 3 point (900~ Fig. 5.
Thus, a dilatometrie study of the sintering process in iron powder compacts leads to the following conclusions:
1. Effective sintering begins at the recrystallization threshold temperature.

667
 2. The sintering process proceeds most vigorously between Ac, and Ac3; at these temperatures, the coefficient
of linear shrinkage is at a maximum. Above Aca the shrinkage is even less than between the recrystallization thres-
hold and At1.
3. The linear shrinkage coefficient within various temperature ranges and the method of its determination
used in this study of sintering of iron powders can be recommended for the study of sintering in other metals and
alloys.

dt

50t $00 700 ~00 _qO0 )I000"~

O 0.40

,, "N,

,l X" x
0.30
/
3
;l
0.20
"'' ~/
0.10
5 ~L

g
rO { ~-"' 0
-2Ai'iO 500 GO0 700 800 900 1000 o C
mm

Fig. 4. Values of total shrinkage of specimens obtained Fig. 5. Change of total shrinkage as function of sinter-
after sintering at various temperatures above the recrys- ing temperature (curve obtained by differentiation of
tallization threshold (values of total shrinkage inFig. 3). that in Fig. 4).
ak
~1b ,
kgm/sq.em kg/sq.mm
. . . . t I
0.4
x
o.3

o.2

0.1

/ / 72J *
/2

500 '
200 400 6oo 800 ~ooo ClOO ~

Fig. 6. Bending strength Obend and impact toughness a k of specimens

sintered at various temperatures.

The above conclusions are supported by parallel tests on determining the mechanical properties and electric
resistivity of compacts sintered at various temperatures. Fig. 6 shows the changes of bending strength and impact
toughness of iron powder specimens sintered at various temperatures. These curves also reveat that the strength be-
gins to increase only from the recrystallization threshold, around 500"C; its most spectacular rise occurs within the
723-900~ range while above 900~ these properties undergo essentially a stabilization only. If the bend strength ts
related to the various temperatures ranges, the following results are obtained.
Temperature, *C Bend strength, kg/sq.mm
20--500 ~ 0
500--723 ~ 2.24 9 10 -2
723--900 ~ 4.80 9 10 -2
Above 900 ~ i 9 10 -2

668
 The i m p a c t toughness does not change up to Ac 1. Within the allotropic transformation range, it increases rapidly.
Above 900~ i t undergoes essentially a stabilization, the rate of increase being slight and similar to that observed in
the bend strength curve.
Hence, the r e l a t i o n between the m e c h a n i c a l properties and the sintering temperature supports the conclusion
that sintering of iron powders proceeds in accordance with the F e - F % C equilibrium diagram. This correspondence
becomes most conspicuous during holding at various temperatures.
Fig. 7 contains d i l a t o m e t r i c curves of iron powder compacts with 14% initial porosity and sintemd at various
temperatures with a subsequent soaking for 5 hr. The curves were obtained on a d i l a m m e t e r without a reference,
with an a u t o m a t i c m o v e m e n t of the photographic film holder a t a rate of 18.7 m m / h r .
Curves representing the r e i a t i o n between the total shrinkage at the various temperatures and holding t i m e are
presented in Fig. 8. Their analysis indicates that m a x i m u m shrinkage is achieved during isothermal hoIding a t the
allotropic transformation temperatures and e s p e c i a l l y at 850~ After a 2 hours' soak, the following torn1 shrinkage
was obtained:

Temperature, ~ Shrinkage, m m / m m .
700 3.8 " 10 -3
750 5.1 9 I0 -3
800 6.3 9 1 0 -3
850 8,7 9 I0 "~
i000 5,7 9 i0 -~

.df.N 3

I1 i o~ 9 1,~.5"106 "1
/fl ,/% /
t .'l / ~'
9
Y
4
Z 3 * .5 hr
7

$
J
5

4
J 700 ~
2 5

1000 ~
$ 750 ~
.~ ~00 209 300 *00 540 SOO 700 800 900 ;O00~
o , 2 3 ~ ~ Shr(for700 ~
7
Duration of isothermal _ ~ 899~
-Z~d l'lO 3 I
holding

Fig. 7. D i l a t o m e t t i c curves of iron powder sintered Fig. 8. Effect of isothermal holding on shrinkage
at different temperatures with subsequent isothermal of iron powder compacts sintered at different t e m -
soaking (dashed lines). peratures,

By graphical differentiation of the curves in Fig. 8, the sintering rates, W r a m / r a m , hr were obtained. They
showed, in line with the previous conclusions, a m a x i m u m shrinkage rate at the allotropic change temperature
around Ac 3. The shrinkage rate above this point was very s m a l l . This was also confirmed by experiments conducted
elsewhere, where "the densifieation rate at 982~ was only 1/1000th of the rate at 816~ and where" no visible con-
traction was observed at the higher temperature even after two months;" Hence, the heating time above Ac 3 need
not e x c e e d one hour.
As a result of the findings reported here, the following procedure for making parts with improved strength from
iron powder is r e c o m m e n d e d : pressing, sintering at 875~ with a 1.5-2.5 hr soak, finish pressing to final shape, sin-
tering at 1000-1050~ with a holding t i m e of not more than 1 hr.

REFERENCES
1. G . A . Geach, Sintering Theory, (Teoriya Spekaniya).Uspekhi Fiziki Metallov, Vol. 1 [Russian Translation]
M e t a l l u r g i z d a t Press, 1956.

669
 P o w d e r Metallurgy-- of I r o n . [Available HB Translations]

P o r o u s a n d N o n - p o r o u s S t r i p f r o m I r o n P o w d e r . A. N. N i k o l a e v .
M e t a l l o v e d . T e r m . O b r a b . M e t . , J a n . 1960, #1, 2 8 - 3 1 . HB
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the R e s u l t s of S i n t e r i n g . W. R u t k o w s k i . N e u e H ~ t t e , v. 6, 1961,
#1Z, 7 8 8 - 7 9 0 . HB T r a n s l a t i o n #5559. $4.80

S u r f a c e T r e a t m e n t of I r o n P o w d e r P r o d u c t s . P . Szeki. M e t a l l -
o b e r f l ~ c h e , v. 14, 1960, #9, 2 6 6 - 2 6 9 . FIB T r a n s l a t i o n No.
5071. $4.90

S e l f - D i f f u s i o n a n d V i s c o u s F l o w of C o m p a c t e d M e t a l ( i n c l u d i n g
Iron) Powders. Ya. E. G e g u z i n et al. D o k l a d y A k a d . N a u k
SSSR, v. 87, 195Z, #4, 5 7 7 - 5 8 0 . HB T r a n s l a t i o n No. 3362.
$z. 90
S o m e P r o p e r t i e s of I r o n P o w d e r s P r o d u c e d b y A t o m i z a t i o n .
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A r c h l y E i s e n h . , v. 24, 1953, # 5 / 6 , 2 5 1 - 5 5 . FIB T r a n s l a t i o n
No. 3273. $7.80

New P r o c e s s f o r the R e d u c t i o n of I r o n P o w d e r s . H. S i e p m a n n .
Stab/ und E i s e n , v. 73, 1953, #6, 3 6 0 - 4 . HB T r a n s l a t i o n
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C r y s t a l L a t t i c e D i s t o r t i o n s a n d S i n t e r i n g of M e t a l [ I r o n ] P o w -
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S t u d i e d b y t h e i r E l e c t r i c a l C o n d u c t i v i t y . V. I. L i k h t m a n a n d
L. T. N a z a r o v . Z h u r n a l T e k h n . F i z i k i , v. Z2, 195Z, #4, 6 9 6 -
70Z. HB T r a n s l a t i o n No. 3065. $6.40

Corrosion-Resistant Iron-Base Metal Powder Products. N.I.

M o s k v i n . V e s t n i k M a s h . , v. 32, 195Z, #3, 7 3 - 7 6 . HB T r a n s -
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I n f l u e n c e of b ~ , r f a c e - A c t i v e L u b r i c a n t s u p o n the P r o c e s s e s of
C o m p r e s s i o n a n d S i n t e r i n g of M e t a l [ I n c l . E d d y - M i l l e d a n d
R e d u c e d I r o n ] P o w d e r s . V. I. L i k h t m a n a n d P . A. R e b i n d e r .
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SSSR, O T N , M a r c h 1951, No. 3, 4 1 1 - 8 . HB T r . # Z 7 6 6 . $ 6 . 4 0 .

6qo