Sie sind auf Seite 1von 113

Particle size and pore structure of

nanomaterials
Izabella Jasiska, PhD
West Pomeranian University of Technology, Szczecin
August 10, 2011
Outline
Theory of Adsorption
Physical Adsorption
Monolayer Models
Standard Isotherms
Mesoporosity
Microporosity
Particle size
Adsorption
Physical Adsorption
3
Particle size
Why We Care About Particle Size and Surface Area ?
Flowability
Filter-ability
Viscosity-Reology
Agglomeration
Dusting tendency
Settling rate
Activity/Reactivity rate (e.g. of catalyst)
Dissolution rate (of pharmaceutical)
Gas absorption
Hydration rate (of cement)
Moisture absorption
Entry into lungs (shape dependency too)
These characteristics control many properties of materials
Particle size
Adsorption
Physical Adsorption
What is Particle Size?
Particle size
Adsorption
Physical Adsorption
What is Particle Size?
Due to symmetry, size of sphere
is completely determined by
only one parameter its
diameter (radius)
Other properties of sphere are
easily computed from its
size:
3
6
1
d V t =
2
d S t =
3
6
d m t

=
Particle size
Adsorption
Physical Adsorption
Different Equivalent Spheres
Particle size
Adsorption
Physical Adsorption
Porosity
Particle size
Adsorption
Physical Adsorption
Non-porous solid
Low specific surface area
Low specific pore volume
Porous solid
High specific surface area
High specific pore volume
F. Rouquerol, J. Rouquerol, K. S. W. Sing, Adsorption by Powders
and Porous Solids, Academic Press, 1-25, 1999
Porous materials have highly developed internal surface area that can be used to
perform specific function.
Almost all solids are porous except for ceramics fired at extremely high
temperatures
Dead end
(open)
closed
Inter-connected
(open)
Passing (open)
Particle size
Adsorption
Physical Adsorption
Porosity
F. Rouquerol, J. Rouquerol, K. S. W. Sing, Adsorption by Powders
and Porous Solids, Academic Press, 1-25, 1999
Open pores are accessible whereas closed pores are inaccessible pores.
Open pores can be inter-connected, passing or dead end.
Particle size
Adsorption
Physical Adsorption
Shapes of Pores
Conical
Interstices
Slits
Cylindrical
Spherical or
Ink Bottle
Pore
Shapes
F. Rouquerol, J. Rouquerol, K. S. W. Sing, Adsorption by Powders
and Porous Solids, Academic Press, 1-25, 1999
Particle size
Adsorption
Physical Adsorption
Measure of porosity
Pore size and
its distribution
Specific Surface Area, m
2
/g =
Porosity
Mass of the solid, g
Total surface area, m
2
Specific Pore volume, cm
3
/g
Mass of the solid, g
Total pore volume, cm
3
=
Porosity, % =
Volume of solid (including pores)
Volume of pores
X 100
Particle size
Adsorption
Physical Adsorption
Size of Pores (IUPAC Standard)
2 nm 50 nm
Micropores Mesopores Macropores
Zeolite,
Activated
carbon,
Metal organic
framework
Mesoporous silica,
Activated carbon
Sintered metals
and ceramics
Sing, K. S. W. et al. Reporting Physisorption Data for Gas/Solid Systems.
Pure & Appl. Chem. 57, 603-619 (1985).
Techniques for Porosity Analysis
Mercury
porosimetry
TEM
SEM
Small angle
X-ray
scattering
Small
Angle
Neutron
scattering
Gas
adsorption
Techniques
Particle size
Adsorption
Physical Adsorption
Mercury
porosimetry
TEM
SEM
Small angle
X-ray
scattering
Small
Angle
Neutron
scattering
Gas
adsorption
Techniques
Can measure only open pores
Pore size : 0.4 nm 50 nm
Easy
Established technique
Particle size
Adsorption
Physical Adsorption
Techniques for Porosity Analysis
Mercury
porosimetry
TEM
SEM
Small angle
X-ray
scattering
Small
Angle
Neutron
scattering
Gas
adsorption
Techniques
Particle size
Adsorption
Physical Adsorption
Similar to gas adsorption
Can measure only open
pores
Pore size >1.5 nm
Easy
Established technique
Techniques for Porosity Analysis
Mercury
porosimetry
TEM
SEM
Small angle
X-ray
scattering
Small
Angle
Neutron
scattering
Gas
adsorption
Techniques
Particle size
Adsorption
Physical Adsorption
Techniques for Porosity Analysis
Provide information
regarding pore
connectivity
Pore size > 5nm
Pore size can be
measured if the
materials contains
ordered pores
Rarely used for pore
analysis
Mercury
porosimetry
TEM
SEM
Small angle
X-ray
scattering
Small
Angle
Neutron
scattering
Gas
adsorption
Techniques
Particle size
Adsorption
Physical Adsorption
Techniques for Porosity Analysis
Any pore size
Open & Close porosity
Costly
Adsorption
Particle size
Adsorption
Physical Adsorption
surface layer at the gas-solid interface
Theory of Adsorption
Particle size
Adsorption
Physical Adsorption
Adsorbate
Adsorptive
Adsorbent
1. Diffusion to adsorbent surface
2. Migration into pores of adsorbent
3. Monolayer builds up of adsorbate
1 2 3
Gas molecules admitted under
increasing pressure to a clean, cold
surface.
Data treatment techniques find the
quantity of gas that forms the first
layer.
1 2 3
Adsorption
Particle size
Adsorption
Physical Adsorption
S. Lowell & J. E. Shields, Powder Surface Area and Porosity,
3rd Ed. Chapman & Hall, New York, 1991
Adsorption
Particle size
Adsorption
Physical Adsorption
Adsorption
Particle size
Adsorption
Physical Adsorption
Adsorption
Particle size
Adsorption
Physical Adsorption
Adsorption isotherm
adsorptive of pressure saturated
adsorbate of pressure

where
=
|
|
.
|

\
|
=
p
p
p
p
f
o
o
V
a
V
a
Desorption isotherm
p
p
o
Gas sorption - Isotherm
Particle size
Adsorption
Physical Adsorption
S. Lowell & J. E. Shields, Powder Surface Area and Porosity,
3rd Ed. Chapman & Hall, New York, 1991
Adsorption
Particle size
Adsorption
Physical Adsorption
Adsorption
Particle size
Adsorption
Physical Adsorption
Adsorption
Particle size
Adsorption
Physical Adsorption
Particle size
Adsorption
Physical Adsorption
SURFACE AREA
Adsorption
Particle size
Adsorption
Physical Adsorption
Interpretation
Adsorption Analysis
Sample Preparation
Steps for Measurement
Particle size
Adsorption
Physical Adsorption
Vacuum
Analysis
station
Adsorbate
Helium
P
o
Outgassing
station
Sample
Cell
Sample preparation (outgassing)
Particle size
Adsorption
Physical Adsorption
Adsorbate
Helium
Vacuum
P
o
Outgassing
station
Analysis station
Sample
Cell
Adsorption analysis
Particle size
Adsorption
Physical Adsorption
(N
2
, Ar, CO
2
, Kr)
(1 mg sample is sufficient)
Analysis temperature (liquid nitrogen,
liquid argon, 0

C)
Porosity Analyzer
Outgassing
station
Analysis station
Liquid nitrogen
bath
Physisorption Analyzer
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
www.micromeritics.com
Porosity Analyzer
Outgassing
station
Analysis station
Physisorption Analyzer
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
www.micromeritics.com
Physisorption Dynamic Adsorption Hardware
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
FlowSorb III
www.micromeritics.com
Physisorption Dynamic Adsorption
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Points P/P
o
Volume adsorbed
1
2
3
Weight of sample
Pore shape
Specific
surface area
Pore volume
Pore size
&
distribution
Results
Interpretation
Particle size
Adsorption
Physical Adsorption
Adsorption
Particle size
Adsorption
Physical Adsorption
Langmuir method BET method
Multipoint BET Single point BET
Type I - Isotherm
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Adsorbate
Adsorbent
adsorbate. of pressure
and constant; empirical
monolayer; form to required gas of volume
; pressure at adsorbed gas of volume
where
1
=
=
=
=
+ =
P
b
V
P V
V
P
b V V
P
m
a
m m a
Langmuir
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
I. Langmuir, J. Am. Chem. Soc., 1916, 38, 2221-2295
Assumptions
homogeneous surface (all adsorption sites energetically identical)
monolayer adsorption (no multilayer adsorption)
no interaction between adsorbed molecules
Langmuir
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Langmuir
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
N
2
Adsorption on 13x Zeolite
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
N
2
Adsorption on 13x Zeolite
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
N
2
Adsorption on 13x Zeolite
Type II - Isotherm
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Brunauer, Emmett i Teller
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
S. Brunauer, P. Emmett, E. Teller,
J. Am. Chem. Soc., 1938, 60, 309319
BET Assumptions
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
S.Brunauer, P.Emmett, E.Teller, J. Am. Chem. Soc.,
1938, 60 (2), pp 309319
BET Model
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
S.Brunauer, P.Emmett, E.Teller, J. Am. Chem. Soc.,
1938, 60 (2), pp 309319
BET Model
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
S.Brunauer, P.Emmett, E.Teller, J. Am. Chem. Soc.,
1938, 60 (2), pp 309319
Brunauer, Emmett i Teller
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
S.Brunauer, P.Emmett, E.Teller, J. Am. Chem. Soc.,
1938, 60 (2), pp 309319
Brunauer, Emmett i Teller
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
S.Brunauer, P.Emmett, E.Teller, J. Am. Chem. Soc.,
1938, 60 (2), pp 309319
N
2
Adsorption on Macro-porous Silica
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
N
2
BET Transformation 25.7 m
2
/g
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption

=
M
A
N
n
M
A N n
S
cs
A
m
cs A m
monolayer capacity
cross-sectional area
of adsorbate
Avogadro number
molecular weight
of adsorbate
Specific surface area:
Special Case Single Point Surface Area
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Special considerations
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Gas Temperature Cross
sectional
area (nm
2
)
N
2
-195.8
o
C (liquid nitrogen)
-183
o
C (liquid argon)
0.162
Ar -183
o
C (liquid argon)
-195.8
o
C (liquid nitrogen)
0.142
CO
2
-78
o
C, -25
o
C, 0
o
C 0.195
CO -183
o
C (liquid argon) 0.163
Kr -195.8
o
C (liquid nitrogen) 0.205
O
2
-183
o
C (liquid argon) 0.141
C
4
H
10
0
o
C, 25
o
C 0.469
Common Adsorbates
Particle size
Adsorption
Physical Adsorption
Physisorption Special Considerations
Particle size
Adsorption
Physical Adsorption
Limitations of BET Surface Area Method
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
This may or may not be accompanied by a short linear region at lower
relative pressures, If there is no truly linear region, then it can be said
that the BET equation is invalid for that particular sample
The BET method depends on the cross-sectional area of adsorbate.
Monolayer structure is same on all the surface.
Localized monolayer coverage.
K. S. W. Sing, Colloids and Surfaces, 187 188, 2001, 3-9
Particle size
Adsorption
Physical Adsorption
POROSITY,
PORE SIZE
Adsorption
Particle size
Adsorption
Physical Adsorption
V
a
1
P/P
o
Type I
or
Langmuir
Concave to the P/P
o
axis
Exhibited by microporous solids (<2nm)
1
P/P
o
Type II
Exhibited by nonporous or
macroporous solids (>50nm)
Unrestricted monolayer-multilayer
adsorption
Point B indicates the relative pressure
at which monolayer coverage is
complete
B
V
a
Particle size
Adsorption
Physical Adsorption
V
a
1
P/P
o
Type
III
Convex to the P/Po axis
Exhibited by nonporous solids
V
a
1
P/P
o
Type IV
Exhibited by mesoporous solids
Initial part of the type IV follows
the same path as the type II
Particle size
Adsorption
Physical Adsorption
V
a
1
P/P
o
Type V
Highly uncommon
Exhibited by mesoporous solids
Particle size
Adsorption
Physical Adsorption
Hysteresis indicates the presence of mesopores.
Hysteresis gives information regarding pore shapes .
Types I, II and III isotherms are generally reversible but type
I can have a hysteresis. Types IV and V exhibit hysteresis.
1
P/P
o
Hysteresis
V
a
Particle size
Adsorption
Physical Adsorption
Histeresis
V
a
1
P/P
o
TypeA
Cylindrical Slits
Type B
1
P/P
o
1
P/P
o
Type C Type D
1
P/P
o
Type E
1
P/P
o
Conical
Ink bottle
Particle size
Adsorption
Physical Adsorption
Total Pore Volume and Average Pore Radius
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
RT
V V P
V
m ads a
liq
=
V
ads
is the volume of nitrogen adsorbed; V
liq
is the volume of liquid nitrogen
P
a
and T are ambient pressure and temperature, respectively,
V
m
is the molar volume of the liquid adsorbate (34.7 cm
3
/mol for nitrogen).
S
V
r
liq
p
2
=
The average pore radius r
p
assuming cylindrical pore geometry (type A hysteresis)
Total Pore Volume
Particle size
Adsorption
Physical Adsorption
STANDARD
ISOTHERMS
Standard Isotherms
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
The t-plot Method
Resembles a type II
Relative Pressure (P/Po)
S
t
a
t
i
s
t
i
c
a
l

t
h
i
c
k
n
e
s
s
A statistical monolayer
A statistical multilayer
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
The t-plot method
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
t t t
The t-plot shapes of adsorption isotherm usually found by nitrogen adsorption
The t-plot Method
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Statistical thickness t
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Statistical thickness t
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
The t-Method microporoos sample 13x
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
The t-Method mesoporous sample MCM 41
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
The t-Method mesoporous sample MCM 41
Standard Isotherms
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
The o
s
-Method
Particle size
Adsorption
Physical Adsorption
PORE SIZE
DISTRIBUTION
Adsorption =
multilayer formation,
then
Desorption =
meniscus control
Kapilary condensation
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
From: M Thommes, Physical
adsorption characterization of
ordered and amorphous mesoporous
materials, Nanoporous Materials-
Science and Engineering (edited by
Max Lu, X.S Zhao), Imperial College
Press, Chapter 11, 317-364 (2004)
Sorption, Pore Condensation and Hysteresis Behavior of a Fluid in a Single Cylindrical Mesopore
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Kapilary condensation
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Capillary Condensation
is the "process by which multilayer adsorption from the vapor into a
porous medium proceeds to the point at which pore spaces become
filled with condensed liquid from the vapor
Calculation methods
Gas Sorption Calculation Methods
P/Po range Mechanism Calculation model
1x10-7 to 0.02 micropore filling DFT, GCMC, HK, SF, DA, DR
0.01 to 0.1 sub-monolayer formation DR
0.05 to 0.3 monolayer complete BET, Langmuir
> 0.1 multilayer formation t-plot (de-Boer,FHH),
> 0.35 capillary condensation BJH, DH
0.1 to 0.5 capillary filling DFT, BJH
in M41S-type materials
Particle size
Adsorption
Physical Adsorption
PORE SIZE
DISTRIBUTION
(MEZOPOROSITY)
2 nm 50 nm
Micropores
Mesopores Macropores
Methods Assumption
Pore Shape Based on ..
BJH (Barrett, Joyner and
Halenda) method
Cylindrical, Slit-shaped Kelvin equation
DH (Dollimore Heal) method
Cylindrical t-method
Choice of Method
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
P. A. Webb, C. Orr, Analytical Methods in Fine Particle Technology,
Micromeritics, 53 152, 1997
BJH (Barrett, Joyner, Halenda) Calculations
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
BJH Calculations
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Pore volume requires assumption of liquid density!
u
t k
r
Adsorbed layer
F. Rouquerol, J. Rouquerol, K. S. W. Sing, Adsorption by Powders
and Porous Solids, Academic Press, 203, 1999
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
u
k
r
BJH Calculations
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
BJH Calculations
BJH Example Data
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
BJH Example Data
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
BJH Example Data
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
BJH Example Data
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
BJH Example Data
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
BJH Example Data
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
DH (Dollimore Heal) method
DH
Extremely similar calculation to BJH, which gives
very similar results. Essentially differs only in minor
mathematical details.
Particle size
Adsorption
Physical Adsorption
PORE SIZE
DISTRIBUTION
(MICROPOROSITY)
V
a
1
P/Po
Type I
or
Langmuir
Type I isotherms dont have
hysteresis.
Pore shape cannot be determined
by isotherm.
As various methods for pore size
calculation are based on shape of
pores, reliability of pore size
calculation is questionable.
Shape of Microporous Materials
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
F. Rouquerol, J. Rouquerol, K. S. W. Sing, Adsorption by Powders
and Porous Solids, Academic Press, 1-25, 1999
2 nm
50 nm
Micropores
Mesopores Macropores
Methods Assumption
Pore Shape Based on ..
Brunauer MP method Cylindrical or Slit shaped de Boers t-method
Dubinin-Astakhov method - Polanyi potential
theory
Independent of
Kelvin equation
HK (Horvath-Kawazoe)
method
Slit Everett and Powl
method
Independent of
Kelvin equation
Saito-Foley method Cylindrical HK method
P. A. Webb, C. Orr, Analytical Methods in Fine Particle Technology,
Micromeritics, 53 152, 1997
Choice of Method
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
2 nm
50 nm
Micropores
Mesopores Macropores
Methods Assumption
Pore Shape Based on ..
NLDFT (Non Local Density
Functional Theory) and
Monte Carlo simulation
method
Cylindrical and slit Statistical
thermodynamics
Choice of Method
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
P. A. Webb, C. Orr, Analytical Methods in Fine Particle Technology,
Micromeritics, 53 152, 1997
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Microporosity
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Microporosity
The DA Method pore size distribution
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Microporosity
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Microporosity
The HK Method pore size distribution
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Microporosity
Microporosity
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Microporous carbon
BET Method poor fitting
Microporosity - BET Method
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Tag all adsorption
points
Analyze behavior
Note knee
transition from
micropore filling to
limited multilayering
(plateau).
Microporosity t-Method
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Langmuir (Monolayer model) /
DR for Surface Area, Micropore
Volume
Langmuir in
P/P
0
range 0.05 - 0.2
(monolayer)
Microporosity - Langmuir
Particle size
Adsorption
Physical Adsorption
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
DR Method for surface
area, micropore volume
Choose low relative
pressure points
(up to P/P0 = 0.2)
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Microporosity DR Method
Langmuir
Reports micropore surface area, and micropore volume.
Note Langmuir, DR surface areas very close (1430 m
2
/g vs. 1424 m
2
/g)
DR
Monolayer Models
Standard Isotherms
Meso-porosity
Micro-porosity
Particle size
Adsorption
Physical Adsorption
Microporosity Langmuir and DR Method
Particle size
Adsorption
Physical Adsorption
Characterization of Porous Solids and Powders: Surface Area,
Pore Size and Density by S. Lowell, J.E Shields, M.A. Thomas & M.
Thommes (2004) Springer ISBN:1402023022
Adsorption, Surface Area and Porosity by S.J. Gregg and K.S.W.
Sing 2nd Edition (1982) Academic Press ISBN: 0123009561
Gas Adsorption and Characterization of Powders
and Porous Materials, J. Kenvin, Micromeritics Instrument
Corporation (2007)
Bibliography
Thank you for your attention

Das könnte Ihnen auch gefallen