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Iranian Journal of Hydrogen & Fuel Cell 1(2014) 1-10

Iranian Journal of Hydrogen & Fuel Cell

IJHFCJournal homepage://ijhfc.irost.ir

Determination of thermodynamic parameters of hydrogen permeation

of palladium membrane for considering the effect of stainless steel

support

Mohammadamir Saadatinasab1, Hussein Gharibi*1,2, Alireza Zolfaghari3

1Department of Chemistry, Faculty of Science, Tarbiat Modares University, P.O. Box 14115-175, Tehran, Iran

2Department of Material Science & Engineering, 122 S Campus Drive, University of Utah, Salt Lake City, Utah 84112, USA

3Department of Physical Chemistry, Chemistry and Chemical Research Center of Iran, Tehran, Iran

Article Information

Article History:

Received:

7 July 2013

Received in revised form:

14 December 2013

Accepted:

26 January 2014

Keywords

Palladium composite membrane

Enthalpy of hydrogen dissolution

Porous stainless steel support

Abstract

A palladium composite membrane was prepared by electroless plating on

through this composite membrane was measured in the temperature range

of 574-674 K and the pressure difference of two sides of membrane up to

tion behavior of hydrogen through Pd/ox-PSS membrane for calculating thecontribution of each layer in resistance against the hydrogen transport. Theamount of enthalpy of hydrogen dissolution of palladium membrane is -9.4kJ/mol.Considering a complete detailed model, this value was used for discussing theeffect of interaction of metal- support on hydrogen exiting from the palladiumlayer at the downstream side. Several composite membranes which differ in

metal-support interaction, plays an effective role in exiting activation energy.In Pd/ox-PSS composite membrane, the metal-support interaction decreaseshydrogen exiting rate from Pd membranes downstream side.

*Corresponding author. E-mail: [email protected]: +98 - (21) 8288 - 4401 (Tarbiat Modares University, Tehran, Iran)Fax: +98 - (21) 8288 - 4401 (Tarbiat Modares University, Tehran, Iran)

1. Introduction

Need to clean and healthful environment forcesthe world to the pure hydrogen production and fuelcell application. However, almost all of the ener-gy carriers are fossil fuels and hydrocarbon com-

pounds. Production of clean and green hydrogenfuel from these energy carriers is performed in rel-atively high temperature through steam reformingreaction. For hydrogen separation purposes, pal-

ladium based membranes have been studied inmany investigations owing to their suitable prop-erties at high temperature, high permeability, se-lectivity and durability.In order to construct the membrane, various sup-

anodic alumina [4], porous Hastelloy [5], and dif-ferent diffusion barriers (e.g. Cr

2O

3 2O

3

[7], ZrO2[8], TiO2[9], SiO2[10], CeO2[11]) havebeen used. Also, various palladium-based alloys

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have been used. Also, various palladium-basedalloys have been used as membrane such as Pd-Cu [12], Pd-Ag [13], Pd-Au and Pd-Au-Pt [14],Pd-Cu-Ni [15], Pd-Cu-Au [16], Pd-Cu-Ag [17],and other binary and ternary alloys [18]. In addi-tion, membranes with different micro-structures[19,20], and geometries [21,22] have been usedto evaluate the performance of them. However,the contribution of support in the permeation

process has not been concern, particularly in ex-perimental procedure.Although there are few reports. Huang et. al., by

2O

3 composite membranes,

reported hydrogen permeation activation energy,molar enthalpy and entropy of hydrogen dissolu-tion in palladium layer [23].Zhang et. al., com-

pare their data with a model and they investigatethe effects of different diffusion barriers on theactivation energy of hydrogen permeation [24].In this study, we prepared a Pd/ox-PSS mem-

brane and studied its permeation behavior. In thenext section, the background theory of permea-tion through composite palladium membrane isexplained. Then, the experimental procedure isstated. Finally, the contributions of Pd layer andsupport for hydrogen permeance are calculated.Furthermore, palladium layers permeability, hy-drogen permeation activation energy, molar en-thalpy and entropy of hydrogen dissolution in Pdlayer are investigated.

2. Theory

A composite palladium membrane consists ofa porous support and a thin layer of palladium.Although in many researches, the support effectis disregarded but it affects on the characteristics

of permeation through the composite palladiummembrane. To differentiate the contributions ofporous support and palladium layer in the perme-ation resistance, we used the resistance model.This model was developed by Henis and Tripodifor gas permeation in a composite membrane[25]. The permeation resistance of a layer is de-

to this model, the permeation behaviour of gasthrough a composite membrane is analogous to

resistors.

ure 1 shows the schematic of composite mem-brane resistance model for a dense palladiumcomposite membrane. The transport resistances


in the support and palladium layer have beensymbolized by R

sand R

Pd, respectively.

The total resistance of the composite membraneR

tot, is the sum of resistances in the palladium

layer and the support layer:

(1)

Where

Ftot

is the composite membrane permeance, andP

h, P

iand P

l are feed side pressure (high pres-

sure side), pressure (high pressure side), pressurein the palladium-support interface and permeateside pressure (low pressure side), respectively.

The permeance through porous support

In pressure-driven gas permeation processthrough a bare porous support, the transportmechanism mainly follows Knudsen diffusion

through a bare porous disk vs. trans-membraneaverage pressure is correlated by a straight line:

(2)

(3)

The slope and intercept of the latter equation rep-and Knud-

sen diffusion, respectively.Fk,s

andFv,s

(4)

(5)

Figure 1. Schematic representation of H2

permeation through Pd composite membrane.

1tot s Pd

tot

R R RF

,i ls

P PR

J

h i

Pd

P PR

J

( )h l

J F P P

, ,.

k s v s avF F F P

,

4 2 1

3

kk s

rF

L R MT

2

,

1

8k

v s

rF

RL T

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Iranian Journal of Hydrogen & Fuel Cell 1(2014) 1-10 3

Fk,s

and Fv,s

for a given porous media, and the second itemsare functions of gas molecular mass and temper-ature.

The permeation through Palladium layer

by the solution-diffusion mechanism can be ex-pressed as follows:

(6)

If adsorption and desorption of hydrogen mole-cules (surface process) are done quickly, then thediffusion of hydrogen in the bulk palladium layer

is described by:

(7)

Where

The temperature dependence of permeabilityFpl

D, can be expressed by

an exponential form as the below equations:

(8)

(9)

The molar values for the enthalpy of hydrogen

dissolution,H

H and the entropy of hydrogen dis-solution in palladium layer HS , could be calcu-lated by:

(10)

The contribution of palladium layer in permea-tion resistance

In a composite membrane, to obtain hydrogenpermeance through Pd layer only and the con-tribution of this layer in the transport resistance,

hydrogen pressure at palladium-support interfaceP

i, should be calculated by the resistances in se-

ries model as below:

n n

h lJ F P P

0.5 0.5

h lpl

P PJ F

L

bpl

s

NF DS D

K

,0exp a

pl pl

EF F

RT

0exp d

ED D

RT

expH H

s

H SK

RT R

(11)

This equation easily can be derived by consider-ing the resistance model and solving Eq. (3) forcalculating pressure at the interface.

3. Experimental procedure

3.1. Membrane preparation

PSS 316L disk with nominal particle retention

chased from Mott metallurgical corporation.According to the manufacturer, the disk has a

porosity of roughly 2023%. Such a plate madeby metal powders has been widely used as thesubstrate to provide mechanical strength for pal-ladium membrane. The PSS support was cleanedin an ultrasonic bath with a mixture of an alka-line sodium solution and an organic detergent at333K for 30 min. The cleaning procedure wasfollowed by rinsing in deionised water and iso-

propanol, respectively.

port at 393K for 3h.Then it was oxidized in the stagnant air at 1173Kfor 12h to form an oxide intermetallic diffusion

barrier at the intermediate of the support and thehydrogen selective Pd layer. Before electroless

plating, the disk was sensitized and activated ac-cording to a conventional SnCl

2/PdCl

2 method

[26]. Pd membrane was prepared using electro-less plating over the ox-PSS disk support. Thechemicals and conditions required for electroless

The volume/area ratio between the plating solu-tion and the plated area was kept about 3cm3/cm2.

3.2. Membrane permeation testing

A conventional homemade disk type setup wasused to measure the permeation of gas throughthe prepared membrane. The composite mem-

brane was assembled in the compact testing cell,and the perimeter of that, was sealed fully witha high temperature resistant silver paste. Thevalid membrane diameter for the permeation test was

measured by introducing into the palladium mem-brane disk. Measurement of hydrogen permeation

1 22

, , ,2

, , , ,

22

k s k s k s

i l l

v s v s v s v s

F F FJP P P

F F F F

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Table 1. Palladium plating bath composition and

conditions

sures. Before testing, the membrane was heatedin nitrogen atmosphere up to 674K at 1K/min.Then the nitrogen introducing gas substituted

urements at 674K and different pressures up to90kPa, the temperature was lowered, and the ex-

periment was repeated at the next point. At each

ment continues some time to ensure of reach-ing to stability and equilibrium conditions. The

subsequent calculations. The pressure at the per-meate side was always ambient (87.7kPa) with-out purging gas in any of the experiments. The

of its pressure at the membrane feed side by soap

3.3. CharacterizationMicrostructural images of PSS and the mem-

brane were taken by scanning electron micro-scope (SEM TESCAN/VEGA xmu). Pd layerthickness was measured by SEM, too.

4. Results and discussion

In the composite palladium membrane, the plat-ing substrate should be neither too coarse to pre-

2a and 2b show SEM micrographs of the cleanedPSS surface before and after oxidation, respec-tively. Although the surface of PSS is smooth,the morphology of the ox-PSS, presented in Fig-ure 2b, shows homogenous nanoscale coarsensurface, which increases the metal-support inter-action surface area. Figure 3 shows the morphol-ogy of the prepared membrane.As can be seen,the membrane has a compacted coating which

According to the permeation test, the compositepalladium membrane showed zero nitrogen per-

meation lux at room temperature and the pressuredifference of 1 bar.

Figure 2. SEM micrographs of: a) the PSS disk surfacebefore and b) after surface oxidation.

It means that at this condition, nitrogen permea--5 mol/m2.s, based on

the permeation test equipment limit. SEM mi-crograph of the membranes cross-section shows

In order to calculate the amounts of viscose

Figure 3. SEM micrograph of electrolessly plated

palladium membrane.

and Knudsen constants for the ox-PSS support,we placed it in the permeation test cell and fedwith hydrogen. Figure 4 shows the hydrogen

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permeances at various trans-membrane averagepressures at room-temperature for ox-PSS sup-port. The regressed values for the constants ofF

k,s(mol/ m2.s.Pa) and F

v,s (mol/ m2.s.Pa2) at

room temperature are 1.3510-5 and 1.6210-10,respectively. By measuring F

k,sand F

v,s in one

temperature, their values can be calculated for

(4) & (5)].

Figure 4. Hydrogen permeance of the support as a

function of average pressure.

By using Eq. (11) the pressure at the interfacewas obtained. Then the permeance and resistanceof each layer was calculated. Figure 5 shows the

percentage of the palladium layer permeationresistance to composite membrane permeationresistance at different temperatures, where thefeed side pressure of the membrane is adoptedas the abscissa. It is shown that the support hasaveragely a contribution of 5% in hydrogen

permeation resistance that is large enoughto consider it in calculating thermodynamic

properties of hydrogen permeation throughpalladium layer.

Figure 5. The ratio ofRPd

/Rtot

(%) vs. feed side pressure

at different temperatures: 674K, 624K, 574K.

It can be seen that by rising of temperature, thepalladium layers resistance decreased. It is dueto the enhancement of palladium bulk permeanceinduced by temperature rise. In addition, more

pressure in the feed side, leads to more palladiumlayer contribution in composite membrane per-meation resistance.Considering the Pd layer separately, the depend-

ence, is shown in Figure 6.

the palladium layer at different temperatures: 674K,624K, 574K.

vs. pressure difference obtains with pressure ex-ponent of 0.5. This means that the determiningstep of permeation rate is bulk diffusion process.Figure 7 shows the effect of temperature on thehydrogen permeance through the Pd layer. Fromthe Arrhenius plot, the activation energy of hy-drogen permeation through Pd layer in this mem-

brane was evaluated to be 12.83kJ/mol.Generally, hydrogen permeation through dense

palladium layer involves several steps in series.These are in order from the feed side to the per-meate side as:(1) molecular hydrogen transportfrom the bulk gas to the gas layer near the surface(2) dissociative adsorption (chemisorption) (3)atomic hydrogen absorption into the bulk metal(surface to bulk transition) (4) diffusion of theatomic hydrogen through the membrane via thelattice structure (5) transition of atomic (bulk tosurface transition) (6) re-associative desorptionof the hydrogen atoms into molecular hydrogen

(7) movement of the resulting hydrogen mol-ecules away from the downstream surface of themembrane [22]. At equilibrium, the adsorptionand desorption rates (steps 2 and 6), are equal, as

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are the transition rates between the surface andthe bulk metal, i.e. surface-to-bulk metal transi-tion (step 3) and bulk metal-to-surface transition(step 5). Each of these steps is characterized by arate equation. Equating and combining these ex-

pressions as formulated by Ward and Dao, andusing the ideal gas law, leads to the following re-lationship [27]:

(12)

EA, E

B and E

d are activation energies for H at-

oms surface-to-bulk metal transition, activationenergy for H atoms bulk metal-to-surface tran-sition, and activation energy for hydrogen des-orption, respectively. This equation shows thatmolar enthalpy of dissolution is proportional to

EA-(E

B+E

d). It means that less activated H atoms

transiting from upstream surface to bulk of thepalladium layer (less E

A) and/or more activated

hydrogen exiting from the downstream surfaceof the palladium layer (moreE

BandE

d) make the

molar enthalpy of dissolution to be more nega-tive and vice versa.Enthalpy of hydrogen dissolution in palladiumlayer can be calculated considering Eqs. (7)-(10).Data for hydrogen diffusion in palladium layerhave been reported by a number of researchers[28-30]. There is some variation, but most valuesare reasonably consistent. We have chosen to use

parameters based on thosereported by Holleck[28]. They have been determined in the tempera-ture range of 533-913K for a thick palladium foilthat hydrogen diffuses through palladium bulk.In this electroless plated palladium layer, as can

be seen in Figure 3, the grain sizes appear to be

diffusion through the grain boundaries is not ex-

data ofD0=2.9410-7m2/s andE

d=22.2kJ/mol ac-

hydrogen at different temperatures were calculat-ed. Then, the solubility constants were evaluated

by Eq.(7). By calculating the Sieverts constants

at different temperatures (Ks), thermodynamicparameters have been obtained [Eq. (10)]. Basedon this calculation, the enthalpy and entropy ofhydrogen dissolution in the palladium layer ob-

0.50.25 20.5

0 0

0.5

0 0

2 1exp

exp exp

s A B d

H H

k N MRT F E E E

S G RT

S H

R RT

tained as -9.4kJ/mol and -55.3J/mol.K, respec-tively. Few researchers report the molar enthalpyof hydrogen dissolution in palladium membrane[23, 28]. We used enthalpy of hydrogen dissolu-tion in palladium layer of different membranesin order to compare their behaviour in hydrogen

permeation steps. These values have been com-pared with each other in Table 2.

Table 2. A comparison of interdiffusion parameters of

hydrogen through the Pd layer.

aprepared by electroless plating method

bThese amounts extracted from reference data.

Note that all of them have been measured byconsidering only palladium layer contribution in

permeance using the same diffusion parameters

as Holleck. The value of HH reported by Hol-leck [28] is -8.4kJ/mol. Comparison between ourmembrane and the Pd/Al

2O

3 composite mem-

brane prepared by Huang, shows good accord-ance with each other in the value of HH but ismore negative than the value reported by Hol-leck. Since Holleck used self supported mem-

brane, this difference should be attributed tometal-support interaction. This is the main dif-ference.of Hollecks membrane with fabricatedmembrane in our lab and Huangs membrane[23]. In contrast to Pd/ox-PSS and Pd/Al

2O

3, the

value of HH in palladium layer of Pd/YSZ-Al2

O3

composite membrane prepared by Zhang et. al. issimilar to this value of Hollecks self supported

palladium layer [24].Given that all four membranes are made of pure

palladium and considering the main differencebetween these palladium membranes i.e. supportmaterial and based on the direct proportion be-tween HH andE

A-(E

B+E

d), more negative value

of HH implies to higher EB+E

d. It means acti-

vated hydrogen exiting from downstream side ofpalladium layer, might be related to metal-sup-port interaction in these membranes. It is known

that the oxides are reduced to metallic state underH2 atmosphere. After that, supports metal ele-

ments and palladium could migrate and diffuse toopposite layer. More chemical activity of support

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causes to more diffusion and alloying with pal-ladium layer. The investigation and comparisonbetween Fe

2O

3, Al

2O

3 and YSZ, indicates high

chemical activity of Fe2O

3and Al

2O

3 and inert-

ness of YSZ [24,32,33]. Using cross sectionalSEM and EDS of palladium supported mem-

branes, Akis and Okazaki, showed that in com-posite palladium membranes Fe and Al are al-loyed with palladium while no alloying occurs

between Palladium and Yttrium or Zirconium ofYSZ [32,33]. The formation of Pd-Fe and Pd-Alalloys lower the hydrogen solubility and diffu-sivity and increase the activation energy for hy-

drogen exiting [34,35]. In the case of Pd/YSZ-Al2O

3 composite membrane, since Yttrium and

Zirconium is more inert and stable as the support,no alloy layer might form in the palladium-sup-

port interface of Pd/YSZ-Al2O

3membrane [32].

In fact, in the Holecks and Zhangs membranes,H exiting is less activated step and the value ofobtains more positive.This analysis shows that the support has an im-

portant role in permeation characteristics. In ad-dition, it is reasonable to say that the molar en-thalpy of hydrogen dissolution can be used tocompare chemical activity of support surface in

different composite membranes.

5. Conclusion

A palladium membrane was prepared on ox-PSS support by electroless plating method. Itwas shown that the support layer has averagelya contribution of 5% in hydrogen permeation re-sistance of the composited membrane. The per-meation data of palladium layer was evaluatedand the activation energy of hydrogen permea-

tion and the molar enthalpy of hydrogen disso-lution were calculated. The molar enthalpy ofhydrogen dissolution in palladium layer depos-ited on ox-PSS obtained as -9.4kJ/mol whichis similar to the value of HH palladium layerdeposited on Al

2O

3and more negative than this

value of self supported palladium layer and thepalladium layer deposited on YSZ. Using a com-plete model, it was deduced that molar enthalpyof hydrogen dissolution is directly proportionalwithE

A-(E

d+E

B). By comparing several compos-

ite membranes which differ in support material,

tion, plays an effective role in exiting activationenergy. In Pd/ox-PSS composite membrane, themetal-support interaction decreases hydrogen ex-iting rate from Pd membranes downstream side.

Nomenclature

in Pd (m2/s)

D0 Pre-exponential factor for

D(m2/s)

S Solubility constant

F Permeance (mol/m2.s.Pa)

Fpl Permeability (mol.m/m2.s.Pa-n)

Fpl0

Pre-exponential factor for Fpl

(mol.m/m2.s.Pa-n)

EA Activation energy for H atoms

surface-to-bulk metal transition(kJ/mol H)

EB Activation energy for H atoms

bulk metal-to-surface transition(kJ/mol H)

Ed Hydrogen desorption activation

energy (kJ/mol H)

F( ), G( ) Functions of coverage factor

HH Molar enthalpy of hydrogen dis

(kJ/mol H)

HS Molar entropy of hydrogen

(kJ/mol K H)

J Flux through composite membrane(mol/m2s)

Ks Sievert's law constant

Nb Bulk metal Pd atom concentration

(mol Pd/m3)

S0

(at zerocoverage)

T Absolute temperature (K)

r Pore radius (m)

M Molecular mass (kg/mol)

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R Universal gas constant(8.314 J/molK)

L Membrane thickness (m)

k0 Desorption rate constant pre-

exponential factor

Greek letters

(Pa s)

(atomic H/Pdratio on surface)

(cm3/mol H s)

(cm3/mol H s)

Subscripts/Superscripts

av average

s support

p pinhole

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