PALLADIUM HYDROGEN System
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1 The PALLADIUM HYDROGEN System F. A. LEWIS Department of Chemistry The Queen's University of Belfast Northern Ireland ACADEMIC PBESS 1967 LONDON NEW YORK
2 CONTENTS Preface v Chapter 1. General Introduction A. Comparison of the Properties of Palladium with Those of Other Transition Elements B. Permeation of Hydrogen Through Transition Elements "Occlusion" by Palladium C. Pressure-Composition-Temperature (p-c-t) Relationships: Non-stoichiometry D. Introduction of Hydrogen into Palladium by Electrolysis 5 E. General Comparison of the Solubility of Hydrogen in Other Transition Elements F. Solubility of Hydrogen in Other Elements of Group 8. 6 G. Absorption of Hydrogen by Transition Elements of Groups 3, 4 and H. Changes of the Electrical Resistance of Palladium as a Function of Hydrogen Content: "Hydrogenium". 10 I. The Introduction of Hydrogen into Palladium in the Course of Chemical Reactions: Palladium as an Hydrogenation Catalyst Chapter 2. Thermodynamic Factors A. Stages in the Accumulation of Pressure-Composition- Temperature (p-c-t) Relationships by Direct Equilibration with Hydrogen Gas: Non-stoichiometric Composition of the Hydrided Solids B. The Current Position Regarding Pd 2 H С Relationships at Higher Temperatures than T c. 2 0 D. The Problem of Obtaining Equilibrium Between Solid and Gaseous Phases E. Hysteresis of p-g Relationships below T c F. p-g Relationships over Purely a- or /?-phase Regions. 30
3 VUl CONTENTS G. Relationships at Very Low Temperatures H. Units of Composition I. Relationships Between Electrode Potential and Hydrogen Content and Correlations with p-c-t Relationships J. Catalytic Activity of Electrodes and the Interconversion ofe&ndp 36 K. Independence of the E against H/Pd Relationships on the Methods of Introducing or Removing Hydrogen. 36 L. The Palladium Bielectrode 37 M. Other Measurements of Hydrogen Overpotential at Palladium Cathodes N. Calorimetric Determinations of Heats of Absorption and Desorption of Hydrogen and of the Specific Heat of Hydrogen in Palladium Determinations of Partial Molar Heats and Entropies of Absorption and Desorption of Hydrogen from the Temperature Dependence of p-g Relationships.. 41 Chapter 3. Changes of the Shape and of Mechanical and Elastic Properties of Palladium Resulting from Absorption and Desorption of Hydrogen A. Changes of Elastic Constants as a Function of Hydrogen Content 43 B. Changes of Hardness and of Internal Friction.. 44 C. Microscopic Examination of Changes of the Topology of Palladium Surfaces Following Absorption of Hydrogen 47 D. Changes of Shape of Palladium Specimens Following Repeated Cycles of Absorption and Desorption of Hydrogen Chapter 4. Relationships Between Hydrogen Content and Electrical Resistance A. General Form of the Relationships between H/Pd and R/R 0 and the Problem of Hysteresis B. Hysteresis of Relationships between H/Pd and B/R 0. 54
4 CONTENTS C. Temperature Dependence of Relationships between H/Pd and R/B D. Relationships between H/Pd and B/R 0 at Very Low Temperatures E. The Use of Resistance Measurements as an Analytical Guide to Hydrogen Content During Measurements of Other Parameters F. Application of Resistance Measurements to Studies of Rates of Absorption and Desorption of Hydrogen. 59 G. Errors in Measurements of the Electrical Resistance of Specimens Immersed in Solution due to Co-conduction of the Measuring Current through the Electrolyte. 60 Chapter 5. Chemical Stability of Hydrided Palladium A. The Use of Measurements of Physical and Physicochemical Parameters for Estimations of Gain and Loss of Hydrogen B. Chemical Stability of Specimens with Highly-active Surfaces in Contact with the Gaseous Phase.. 64 С Stability of Specimens with Highly-active Surfaces Immersed in Aqueous Solutions D. Stability of Specimens with Surfaces Which are Relatively Inactive for Equilibration with Hydrogen Molecules 68 Chapter 6. Absorption of Hydrogen by Alloys of Palladium A. Some General Comments B. Crystal Structures of the Hydrogen-free Alloys.. 70 C. Absorption of Hydrogen During Electrolytic Discharge and Subsequent Comparisons of the Solubility of Hydrogen as a Function of Alloy Composition.. 72 D. Direct Derivation of p-c-t Relationships for Alloys. 73 E. Derivation oip-c-t Relationships from Measurements of Electrode Potential F. Activation of Electrodes G. Methods of Estimating Changes of Hydrogen Content. 79 H. Estimations of Changes of Hydrogen Content During Desorption JX
5 X CONTENTS I. Comparison of p-c-t Relationships for the Various Alloy Systems J. Hysteresis of p-c-t Relationships K. Critical and Supercritical Isotherms L. Changes of Partial Molar Heats and Entropies of Absorption and Desorption of Hydrogen as a Function of Alloy Composition and Hydrogen Content.. 88 M. Relationships Between Hydrogen Content and Electrical Resistance N. Changes of the Temperature Coefficient of Electrical Resistance with Changes of Hydrogen Content Chapter 7. Diffusion of Hydrogen Through Palladium and Palladium Alloys A. General Introduction and Discussion of Uses of Palladium Membranes B. General Formulation of Diffusion Equations Based on Fick's First Law С Expressing Fick's Equation in Terms of Pressure. D. Some General Comments on the Influence of Surface Processes on Permeation Rates E. Limiting Lower Temperatures for Rapid Rates Permeation: Various Methods of Pre-activation Surfaces F. Chemical Poisoning of the Diffusion Process. G. Adequate Gas Circulation: Bleed Rates H. Some Methods of Measurement of Permeation Rates I. Calculation of a-phase Diffusion Coefficients (D a ) from Studies Involving Only Gas/Solid Interfaces J. Migration of Hydrogen in a-phase Compositions in an Electric Field Gradient 103 K. General Considerations of the Diffusion of Hydrogen in Electrodes 104 L. Problems in the Determination of Diffusion Coefficients from Electrochemical Experiments M. Diffusion of Hydrogen in the ß-phase N. Electrochemical Studies of D ß О. Presence of an a-/ß-phase Boundary Within the Membrane under Steady-State Conditions ce of of
6 CO NTENTS P. Movement of the Boundary Between «- and ß-phases. 112 Q. Diffusion Processes, Nuclear Magnetic Resonance Absorption and Heat Leak Measurements R. Diffusion of Hydrogen through Alloys of Palladium, and Improved Resistance to Deformation S. Possible Correlations between Deformation and Hysteresis T. Diffusion Coefficients for Hydrogen in Pd Alloys..117 X Chapter 8. Absorption of Deuterium by Palladium and Alloys of Palladium: Separation of Hydrogen Isotopes A. Comparison of p-c-t Relationships for the Pd/H and Pd/D Systems 118 B. p-c-t Relationships Derived from Electrode Potential Measurements C. Partial Molar Heats and Entropies of Absorption and Desorption of Deuterium: Heat Capacity Measurements D. Variation of the Electrical Resistance of Palladium as a Function of Deuterium Content E. Isothermal Relationships Obtained with Mixtures of Hydrogen and Deuterium F. Comparison of Diffusion Coefficients for Hydrogen and Deuterium G. Separation of Hydrogen Isotopes by Gas Chromatographic Techniques using Column Packings Coated with Palladium 130 H. Factors Involved in the Separation of Hydrogen Isotopes During Electrolysis at Palladium Electrodes..133 Chapter 9. Investigations of Changes of Lattice Structure and of Some Other Physical and Electrical Properties as Functions of Hydrogen and Deuterium Contents A. General X-ray Crystallographic Evidence of Lattice Expansion and of the Co-existence of Two Hydride Phases over Regions of Pressure Invariance..183
7 Xll CONTENTS B. Correlation of Lattice Parameters with p-c Relationships and with Hysteresis C. Measurements of Changes of Lattice Parameters at Close to Room Temperature D. Changes of Lattice Parameters in the Palladium/ Deuterium System E. Line-broadening of X-ray Reflections F. X-ray CrystaUographic Studies of the Absorption of Hydrogen by Alloys of Palladium G. X-ray Evidence for Analogous ß-phase Hydrides of Nickel 145 H. Neutron Diffraction Studies and the Location of Hydrogen in the Crystal Lattice I. Location of the Hydrogen in a-phase Hydrides..146 J. Face-centred-cubic Symmetry and Lattice Vacancies in ß-phase Hydrides K. Changes of Magnetic Susceptibility as a Function of Hydrogen Content L. Changes of Other Electrical Properties of Palladium and Palladium Alloys as a Function of Hydrogen Content 149 Chapter 10. Theoretical Models for the Pd/H and Related Systems A. Possible Explanations of Certain Results in Terms of the Behaviour of Hydrogen Contained in "Fissures" or "Rifts" 152 B. The Pseudo-silver Hypothesis С The Possibility That the Hydrogen is Dissolved as Protons D. The Possibility of Ordering to More Covalent Molecular Units at Very Low Temperatures E. Theoretical Derivation of p-c Relationships References and Author Index Subject Index
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