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You are on page 1of 52

01. November 2013

A. Trunschke

Further reading

S. Lowell, J.E. Shields, M.A. Thomas, M. Thommes, Characterization of Porous Solids and Powders:

Surface Area, Pore Size and Density, Kluwer Academic Publisher, Dordrecht, 2004, Springer 2006.

R. Brdika, Grundlagen der physikalischen Chemie, Deutscher Verlag der Wissenschaften, Berlin 1982.

P.W. Atkins, J. de Paula, Physikalische Chemie, Wiley-VCH, Weinheim 2013.

G. Wedler, H.-J. Freund, Lehrbuch der Pysikalischen Chemie, Wiley-VCH, 2012.

F. Schth, K.S.W. Sing, J. Weitkamp (Eds.), Handbook of Porous Solids, Vol. 1, Wiley-VCH, Weinheim

2002.

G. Ertl, H. Knzinger, J. Weitkamp (Eds.), Handbook of Heterogeneous Catalysis, VCH, Weinheim,

1997.

Outline

1. Introduction

2. Adsorption

3. Surface area measurements macroporous materials

4. Capillary condensation in mesopores

5. Adsorption in micropores

Modern Methods in Heterogeneous Catalysis Research; 01 Nov 2013; Surface Area and Pore Size Determination; A. Trunschke

Outline

1. Introduction

2. Adsorption

3. Surface area measurements macroporous materials

4. Capillary condensation in mesopores

5. Adsorption in micropores

Modern Methods in Heterogeneous Catalysis Research; 01 Nov 2013; Surface Area and Pore Size Determination; A. Trunschke

Heterogeneous catalysis

The number of active sites depends on the surface area

Surface area is related to

Particle size

Particle morphology

Surface texturing

Porosity

The accessibility of active sites requires pores that allow molecular transport

Porosity:

volume of the catalyst

Texture:

- pore size

- pore size distribution

- pore shape

Modern Methods in Heterogeneous Catalysis Research; 01 Nov 2013; Surface Area and Pore Size Determination; A. Trunschke

1018 particles of edge

lenght = 10-6 m

1 particle of edge

lenght = 1 m

size

Si=6x10-12 m2

Stotal=6x106 m2

S=6 m2

Wiebkes Nanocircus

shape

S=10

m2

MgO

S=100

porosity

m2

S=400 m2 Zeolite ZSM-5

Modern Methods in Heterogeneous Catalysis Research; 01 Nov 2013; Surface Area and Pore Size Determination; A. Trunschke

Dynamic light scattering

Measures Brownian motion and relates this to the size of the particles by using

a correlation function and the Stokes-Einstein equation

Non-spherical particles will be measured as equivalent spheres

D= Diffusion coefficient

k= Boltzmann constant

T= absolute temperature

= dynamic viscosity of the solvent

R= radius of the particle

Microscopy

Shape analysis

Scattering of X-rays by small domains of uniform matter (crystalline or

amorphous), for which the electron density e is different from the continuous

medium

The central peak of scattered intensity gets broader as the domain size

(particles, voids) decreases

SAXS parameters (mean size / size distribution / specific surface area) are

derived from analysis of the profile of the SAXS curve

Mercury porosimetry

Gas Adsorption

Modern Methods in Heterogeneous Catalysis Research; 01 Nov 2013; Surface Area and Pore Size Determination; A. Trunschke

Gas adsorption

Surface area

Pore volume

Texture

Pore size distribution

Pore geometry

Connectivity

Outline

1. Introduction

2. Adsorption

3. Surface area measurements macroporous materials

4. Capillary condensation in mesopores

5. Adsorption in micropores

=

Surface

energy

Adsorption

gas

chemisorption

physisorption

10

Adsorption

activated chemisorption

gas

chemisorption

Heterogeneous catalysis

physisorption

Surface area/pore size determination

11

Physisorption forces

1. Dispersion forces* (major part of the interaction potential)

The electron motion in an atom or molecule leads to a rapidly oscillating dipole moment

coupling of two neighboring moments into phase leads to a net attractive potential

2.

3.

4.

5.

Ion-induced dipole (polar solid/polarizable gas molecule)

Dipole-dipole (polar solid/polar gas molecule)

Quadrupole interactions (symmetrical molecules e.g. O-C++-O-)

12

Adsorption

Physisorption

Chemisorption

Heat of

adsorption

< 50 kJ mol-1

Coverage

Multilayer

Measurement of surface area

Titration of active sites

Interaction

happen

Kinetics

Fast

Activation required

Pores

Pore volume measurements

13

Adsorption

adsorbed molecule/atom

14

Description of adsorption

Relation between T, p, adsorbed amount (surface concentration)

= ns/sa

= ns/ma

= /Sa,sp.

Ws

Vs

adsorpt (s)

adsorbent (a)

0 =1-

1

(coverage)

= / m = / m = N/Nm = W/Wm

= f (p) <eq., T = const.> adsorption isotherm

= f (T) <eq., p = const.> adsorption isobar

p = f(T) <eq., = const.> adsorption isostere

15

Adsorption isotherm

temperatures

G = H TS

Amount adsorbed

= f (p)T

T1 < T2

T1

T2

Pressure P

Adsorption is a spontaneous process: G<0

H<0 Exothermic process

Modern Methods in Heterogeneous Catalysis Research; 01 Nov 2013; Surface Area and Pore Size Determination; A. Trunschke

16

Adsorption isotherm

Planar,

nonporous,

macropores

mesoporous

microporous

17

Adsorption isotherm

= f (p)T

The shape of the isotherm of pure fluids depends on

Interplay between the strength of fluid-wall and fluid-fluid interaction

Pore space

Classification by the International Union of Pure and Applied Chemistry*

Width* [nm]

Micropores

<2

Mesopores

2 ~ 50

Macropores

> 50

Supramicropores 0.7~2nm

Width*

Diameter of a cylindrical pore

Distance between opposite walls in

case of slit pores

*

18

Adorption in micropores

molecular layers

true chemisorption

II

Nonporous or macroporous

adsorbent

B monolayer coverage

complete

Nitrogen on polyethylene

capillary condensation

Amount adsorbed

III

IV

Monolayer-multilayer

adsorption and capillary

condensation

Complete pore filling

VI

Stepwise multilayer

adsorption on a nonporous

non-uniform surface

Ar or Kr on graphitized carbon

Relative pressure

*

19

Adsorption isotherm

surface area and pore data

The models used for mathematical description are empirical models that fit

more or less to experimental data

The results are useful and required to interpret catalytic data

Please consider in the discussion of your results that the surface area or the

pore volume determined by using the various empirical models are

approximated values

20

Outline

2. Adsorption

3. Surface area measurements macroporous materials

4. Capillary condensation in mesopores

5. Adsorption in micropores

21

S = Ax Nm

Ax

Nm

Nitrogen

0.162 nm2

Argon

0.166 nm2

Krypton

0.210 nm2

with a single monolayer

Theories that give access to the monolayer capacity using

the isotherm

Langmuir

BET

22

Langmuir isotherm*

Assumptions

Monolayer adsorption

Energetically uniform surface

No interactions between adsorbed species (heat of adsorption independent of

coverage)

kinetic expression of the adsorption equilibrium

rads = rdes

dNads = dNdes

23

Langmuir isotherm

d

= kadspN(1 )

dt

N

K p

=

=

Nm 1+ K p

d

= kdesN

dt

K=

kads

kdes

Adsorption of nitrogen

on charcoal at different T

24

Langmuir isotherm

N

K p

=

=

Nm 1+ K p

Linear plot

p

1

p

=

+

N KNm Nm

N

mm

n=

=

NA Masdorptive

S = NmAx =

mmNAAx

Masdorptive

25

M. Hvecker et al., Journal of Catalysis 285 (2012) 4860.

over M1 at T=313 K

K = 0.111(6) hPa-1

Nm= 43 mol g-1

Cross-sectional area of propane: 36 2

SBET= 8.8 m2 g-1

S.J. Gregg, R. Stock, Trans. Faraday Soc. 53 (1957) 1355.

Modern Methods in Heterogeneous Catalysis Research; 01 Nov 2013; Surface Area and Pore Size Determination; A. Trunschke

26

Other isotherms

N

Type II isotherm

BET (Brunauer, Emmett, Teller) isotherm

multilayer adsorption

Nm

monolayer adsorption

Langmuir isotherm

- Chemisorption

- Physisorption isotherms of type I

p

Freundlich isotherm

(interaction of adsorbed molecules)

= c1p1/c2

Temkin isotherm

(adsorption enthalpy is a function of the pressure)

= c1ln(c2p)

Modern Methods in Heterogeneous Catalysis Research; 01 Nov 2013; Surface Area and Pore Size Determination; A. Trunschke

27

Modern Methods in Heterogeneous Catalysis Research; 01 Nov 2013; Surface Area and Pore Size Determination; A. Trunschke

28

29

30

Assumptions

Multilayer adsorption

First layer: Langmuir adsorption

Second and further layers:

condensation of gas onto liquid

Heat of adsorption:

6

5

4

3

heat of condensation

2

1

adsorbent

1

1

N

C ( p / p 0)

=

=

N m (1 p / p 0 ) [1 p / p 0 + C ( p / p 0)]

p0 ...vapor pressure of liquid N2

*

31

BET plot

1

1

C 1 p

=

+

W [ p / p 0 1] WmC WmC p 0

W ... mass of adsorbed N

1

Wm =

s+i

s

C = +1

i

1

WmNAAx

S i=

S=

Ssp. =

WmC

Madsorptive

m

2

C 1

s=

WmC

Assumption: For high values of C the intercept may be taken as zero

p

Wm = W 1

p 0

p NA

S = W 1

Ax

p 0 Madsorptive

32

completed monolayers (0.05<p/p0<0.3)

experiment and theory agree well powerful

method of surface area determination

(desH-evH)/RT

C=e

33

Limitations

BET theory ignores inhomogeneities of the surface and lateral adsorbateadsorbate interactions

High energy sites will be occupied at lower relative pressures

Reason for the nonlinearity of BET plots at p/p0 <0.05

Polarization forces would induce a higher heat of adsorption in the second layer than

in the third and so forth

Reason for the failure of the BET equation at p/p0 >0.3

The BET equation is applicable for surface area analysis of nonporous materials

Difficulties to separate mono-multilayer adsorption from pore filling

Filling of micropores is completed at p/p0 <0.1, however, linear BET plot are found at

even lower relative pressures

measured surface area reflects not a real internal surface, but a characteristic BET

surface area

For mesoporous materials exhibiting pore diameters between 2 and 4 nm (MCM-41,

MCM-48) pore filling is observed at pressures close to mono-multilayer formation

overestimation of monolayer capacity

34

Cross-sectional area

Krypton established

for low surface area

measurements

(0.5-0.05 m2) due

to ist low saturation

pressure at 77K

For most of the adsorbents the C constant lies in the range from about

50 to 300 (no weak interaction, no chemisorption)

Its permanent quadrupole moment is responsible for the formation of

well-defined monolayers on most of the surfaces

Overestimation of surface areas of hydroxylated silica surfaces by 20%

due to specific interactions with the polar surface groups (use 13.5 2)

*

Literatur IUPAC.

35

Outline

2. Adsorption

3. Surface area measurements macroporous materials

4. Capillary condensation in mesopores

5. Adsorption in micropores

36

Capillary condensation

Phenomenon whereby a gas

condenses to a liquid-like

phase in a pore at a pressure

p less than saturation

pressure p0 of the bulk liquid

A Monolayer formation

B Multilayer

adsorption

D Capillary

condensation

E Pore evaporation

C Critical film

thickness reached

MCM-41

F multilayer film

37

The wider the pore size distribution the less sharper is the pore condensation step

H1 well defined cylyndrical pore channels

H2 disordered pores

(pore blocking, percolation phenomena)

(slit-shaped pores)

H4 narrow slit pores including pores in the

micropore region

Low pressure hysteresis

no accurate pore size analysis possible!

Changes in the volume of the adsorbent

Swelling of non-rigid pores

Irreversible uptake of molecules in the pores

Chemisorption

*

38

Kelvin equation

The relative pressure where the pore condensation occurs depends on the pore radius

The Kelvin equation provides a correlation between pore diameter and pore condesation

pressure

surface tension of liquid nitrogen

p 2 Vl Vl liquid molar volume

Assumptions

rp pore radius

ln =

Pores of cylindrical shape

p 0 rpRT rk critical radius

No fluid-wall interactions

R universal gas constant

t statistical thickness

4.15

rk =

(N2, 77 K)

rp = rk + t

5

t = 3.54

ln( p / p 0)

Modern Methods in Heterogeneous Catalysis Research; 01 Nov 2013; Surface Area and Pore Size Determination; A. Trunschke

39

40

The shape of the isotherm does not depend only on the texture of the porous material, but also

on the differences of the thermodynamic states between the confined fluid and the bulk fluid

H1 - independent cylindrical pores (MCM-41, SBA-15)

Independent pore model

Pore condensation is associated with metastable states of the pore fluid in ordered

materials

The desorption branch of the hysteresis loop reflects the equilibrium phase transition

Methods, which describe the equilibrium phase transition (BJH) have to be applied to

the desorption branch

(Applicable also to three-dimensional network of pores)

H2, H3 disordered, connected pores

Origin of hysteresis not yet completely understood

Pore blocking (inkbottle pores) associated with the desorption process

Analysis of the adsorption branch (NLDFT-spinodal condensation method, Kelvin

equation based approach calibrated for the adsorption branch)

41

Outline

2. Adsorption

3. Surface area measurements macroporous materials

4. Capillary condensation in mesopores

5. Adsorption in micropores

42

Adsorption in Micropores

Micropores

Width* [nm]

Supermicropores

0.7 ~ 2

Ultramicropores

< 0.7

Gas-solid interactions

Cooperative mechanism

Bilayer thickness of the N2

molecule!

Gas-solid interaction

condensation in mesopores

Adsorption potential theories (0.4 nm ~ )

Classical methods based on macroscopic,

thermodynamic assumptions

Polanyi

Dubinin (DR method)

Stoeckli

Horvath-Kawazoe

Density Functional Theory

Monto Carlo simulations

Empirical methods (0.7~2nm)

t-method

MP-method

s-method

*

43

Assumption

The thickness of the absorbed film on pore walls is uniform statistical thickness t

Wa

Vliq

t = 3.54

=

10 4

Wm

S

It has been shown for type II

isotherms that a plot of the volume

adsorbed versus t gives a staight

line throug the origin

(N2, 77 K)

V-t curve

areas calculated from the slope

comparable to BET values

Modern Methods in Heterogeneous Catalysis Research; 01 Nov 2013; Surface Area and Pore Size Determination; A. Trunschke

44

The t-method

Principle

Comparing an isotherm of a microporous material with a standard type II isotherm of a

nonporous absorbent with BET C constants similar to that of the microporous sample

Plot of the reference isotherm as a t-curve: Vads=f(t)

The t values are in practice calculated with the help of thickness equations that desribe the

particular standard reference curve

Siliceous materials

1

2

13.99

t =

log( p / p 0) + 0.034

C-like materials

45

The t-method

Vmicro= i x 0.001547 cm3

Vliq

t=

10 4

S

St = s x 15.47 m2/g

nonporous material: St = SBET

microporous material: St = Sext

no micropores

with micropores

Modern Methods in Heterogeneous Catalysis Research; 01 Nov 2013; Surface Area and Pore Size Determination; A. Trunschke

46

800

700

600

#8233

#8261

#8434

#8457

700

SBA-15 (#8233)

400

600

300

200

500

cal. AS/SBA-15(#8456)

100

0

0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0

P/P0

V (ml STP/g)

V (ml/g)

500

Acquire HAADF

400

13%Mo/SBA-15 (#8441)

300

200

100

10 nm

0

0

10

statistical thickness t ()

Modern Methods in Heterogeneous Catalysis

Research; 01 Nov 2013; Surface Area and Pore Size Determination; A. Trunschke

10

10 nm

nm

12

14

47

Properties of MoOx/SBA-15

Mo#loading#a#

Surface#Mo##density#

A s#

A e#

(m2/g)#

(m2/g)#

Vp#g#

dp#h#

(%)f#

(ml/g)#

(nm)#

(nm52)#

(wt%)#

Mo#

(nm52)#

b#

Isolated##

SiOH# c,#

(nm52)#

d#

0#

0#

1.6#c#

859#

261#

36#

1#

7.5#

2.1#

0.21#

1.1#d#

637#

164#

31#

0.79#

7.1#

5.1#

0.58#

0.88d#

554#

127#

28#

0.71#

7.1#

6.6#

0.85#

0.68#d#

490#

135#

28#

0.61#

7.1#

9.7#

1.09#

0.39#d#

556#

96#

21#

0.78#

7.2#

13.3#

2.51#

0.07#d#

332#

36#

13#

0.55#

7.4#

heights#of#the#silanol#peak#at#3745cm51,# e#micropore#(<#~0.9#nm#of#width)#surface#estimated#by#t5plot#

method,#f#A#divided#by#AS,#g#at#P/P0#=#0.95,#g#at#the#dehydrated#state;#h#estimated#by#NLDFT#approach.##

#

Modern Methods in Heterogeneous Catalysis Research; 01 Nov 2013; Surface Area and Pore Size Determination; A. Trunschke

48

Experimental

Sample preparation:

1. Homogenization

2. Weighing

3. Outgassing adapted to

the chemical nature of

the sample in vacuum

or under flow (repetitive

cycling)

Maximun residual pressure:

1 Pa (7.5x10-3 Torr)

Micropore analysis: p<0.01 Pa

49

Vd volume of adsorptive dosed

Vm volume of manifold

Vv volume of the sample cell, which is

not occupied by the adsorbent

peq equilibrium pressure after the dose

Vd =

Teq pStd

Tm

Problems

Void volume determination

He is not adsorbed

He does not penetrate into regions

inaccessible for the adsorptive (He removal

procedure for micropore measurements!)

Coolant level and temperature control

p0 determination

pVv 77 K

Vs = Vd

pStd

Tstd = 273.15 K, pstd = 760 torr

Vstp[cm 3 ] / 22414 cm 3 = ns

50

Experimental

equilibrium vapor pressure

exhibited by the pure adsorptive

contained in the sample cell when

immersed in the coolant

The saturation pressure

increases exponentially with T

Due to dissolved water vapor,

oxygen or other gases the T is

slightly elevated:

0.1-0.2 K ~ p = 10-20 torr

BET plot not very sensitive to p0

Broad pressure range for

micropore analysis:

10-7 p/p0 1

51

Acknowledgements

52

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