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PROPERTIES of PLATINIZED PLATINUM a Thesis Submitted For

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PROPERTIES of PLATINIZED PLATINUM a Thesis Submitted For PROPERTIES OF PLATINIZED PLATINUM A thesis submitted for the degree of Doctor of Philosophy of the University of London by Alan Martin Feltham Department of Chemistry Imperial College of Science and Technology London S.W.7. October, 1971 2 ABSTRACT This thesis deals with three distinct aspects of the properties of platinized platinum. In the preparation of platinized platinum electrodes a small amount of lead acetate is commonly added to the plating solution. The lead is partly incorporated into the platinum deposit. Its subsequent rate of leaching out has been studied, and was found to require the presence of both acid and oxygen. The results indicate that only the lead in the top 2 or 3 atomic layers of the deposit dissolves and that it is largely present there as PbO; most of the dissolution occurs within an hour. The potentials of lead-containing platinized platinum electrodes behave in a non-Nernstian manner in the presence of lead nitrate. The major aim of platinizing platinum is to obtain a large surface area. To this end optimum plating conditions must be sought. Yet there is extensive disagreement in the literature, which is reviewed, on the way in which the area of platinized platinum electrodes varies with current density or potential of deposition. The variation of the mass specific area of platinized platinum with deposition potential from -56 to +594- mV(NHE) was tnerefore studied at constant mass degrees -2 of platinization (10 and 5 mg cm ). Maximum mass specific area was obtained at a deposition potential of approximately 150 mV(NHE) where the average current density of platinization was about 27 mA cm-2 At deposition potentials more cathodic than about 140 mV(NHE) a coupled reduction reaction led to the simultaneous evolution of hydrogen. The coulombic efficiency of the deposition process passed through a maximum at about 120 mV(NHE). Platinum catalyses the disappearance of bromopentamminecobalt(III) bromide in acid solution. The kinetics of the corresponding catalysis by platinized platinum have been studied by means of a rotating disc system. The main catalysed reaction was found to be reduction to cobalt(II), and the presence of bromide ions seems to be essential. 3 ACKNOWLEDGEMENTS I should like to thank Dr M. Spiro for his help and guidance throughout this work and his genuine interest in my welfare, and Professor R.M. Barrer, F.R.S., for providing research facilities. My thanks are due also to the Science Research Council for the award of a Research Studentship. I am grateful to Roger D. Jee for the use of his a.c. polaro- graph and for helpful discussions on analytical chemistry. CONTENTS Page PART I INTRODUCTION 7 Chapter 1 Preamble. 8 1.1 Preparation of Finely Divided Platinum. 8 1.2 Historical Origins of Platinized Platinum. 8 Chapter 2 Electrode Kinetics and Mechanism of Platinization. 10 2.1 In the Absence of Lead. 12 2.2 In the Presence of Lead. 18 2.3 Substrate Pretreatment. 19 Chapter 3 Electrodeposition. 21 3.1 Deposit Appearance. 21 3.1.1 In the Absence of Lead. 21 3.1.2 In the Presence of Lead and Other Additives 22 3.2 Deposit Growth. 26 3.2.1 In the Absence of Lead. 27 3.2.2 In the Presence of Lead. 27 3.2.3 Occlusion of Reagents. 28 3.3 Deposit Structure. 28 3.4 The Effect of Alternating Current. 29 PART II THE STABILITY OF LEAD IN PLATINIZED PLATINUM DEPOSITS 31 Chapter 4 Composition of Lead Containing Deposits. 32 Chapter 5 The Leaching of Lead from Platinized Platinum Electrodes in Acid Solution. 35 5.1 Polarography. 36 5.2 Experimental Procedure. 38 5.3 Results. 50 5.4 Discussion. 54 5 Page PART III THE SURFACE AREA OF PLATINIZED PLATINUM ELECTRODES .57 Chapter 6 The Measurement of Electrode Surface Area. 58 6.1 Definition of Useful Parameters. 58 6.2 Electrochemical Determination. 59 6.2.1 The Three Potential Regions of Platinum. 60 6.2.2 Empirical Details of Area Determination. 64 Chapter 7 Co-ordination of Past Area Work. 71 7.1 Dependence on Plating Conditions. 71 7.1.1 Degree of Platinization. 71 7.1.2 Lead Acetate Concentration. 80 7.1.3 Current Density of Deposition. 85 7.1.4 Potential of Deposition. 89 7.1.5 Temperature. 94 7.2 Reproducibility \ 94 7.3 Decrease with Time. 95 Chapter 8 The Variation of Area and Coulombic Efficiency of Platinized Platinum Electrodes with Deposition Potential at Constant Mass Degree of Platinization. 100 8.1 Experimental Procedure. 100 8.2 Results. 109 8.3 Discussion. 111 8.3.1 Mass Specific Area. 111 8.3.2 Coulombic Efficiency and Current Density. 115 8.3.3 Deposition from Different Plating Solutions. 117 8.3.4 Coulombic Specific Area. 119 8.3.5 Variation of the Parameters with Current Density of Platinization. 119 8.3.6 Hydrogen Evolution. 123 Chapter 9 Survey of Platinizing Procedures. 126 PART IV HETEROGENEOUS CATALYSIS IN SOLUTION 129 Chapter 10 Survey of Past Work. 130 10.1 Electron Transfer Reactions. 130 10.2 Isomerization Reactions. 131 10.3 Substitution Reactions. 131 6 Page Chapter 11 Theory of the Rotating Disc and Its Application to Catalysis. 134 11.1 Mass Transport in the Rotating Disc System. 135 11.1.1 Hydrodynamics. 135 11.1.2 Solute Transport. 138 11.1.3 Further Analysis. 140 11.1.4 Practical Factors. 141 11.2 Kinetic Analysis. 143 11.2.1 Surface Control. 143 11.2.2 Intermediate Kinetics. 146 Chapter 12 The Heterogeneous Catalysis of the Aquation of Bromopentamminecobalt(III) Bromide by Platinized Platinum. 150 12.1 Aims of the Present Work. 151 12.2 Preliminary Experiments. 152 12.2.1 Preparation and Analysis of Bromopentamminecobalt(III) Bromide. 152 12.2.2 The Homogeneous Rate. 153 12.2.3 Kinetic Runs with a Foil Catalyst. 154 12.3 Rotating Disc Experiments. 157. 12.3.1 Platinization. 160 12.3.2 Area Determination. 161 12.3.3 Catalysis Runs. 165 12.3.4 Production of Cobalt(II) 170 12.4 Discussion. 172 12.5 Conclusion. 175 REFERENCES 176 PART I INTRODUCTION 8 CHAPTER I PREAMBLE 1.1 PREPARATION OF FINELY DIVIDED PLATINUM Platinum is a good catalyst for numerous reactions. Since the catalytic activity of a heterogeneous catalyst depends greatly on its surface area, it is clearly desirable to have the platinum in as finely divided a form as possible. This can be achieved by the reduction of a platinum compound in solution to form "platinum black", and there are three ways of performing this reduction. One is chemical, e.g. the reduction of chloroplatinic acid with formaldehyde 1 in alkaline solution. Another is electrochemical, e.g. the cathodic reduction of chloroplatinic acid on platinum.2 The last method is radiolytic, e.g. the irradiation of an alkaline saturated solution of . sodium hexahydroxoplatinate(IV) with electrons .3 This thesis is concerned with the physical and chemical properties of platinum that has been electrodeposited on a platinum substrate, known as platinized platinum. 1.2 HISTORICAL ORIGINS OF PLATINIZED PLATINUM It is an accident of history that the original recipes for platinum black electrodeposition were devised, not for electrochemical purposes, but in connection with the measurement of radiation. When radiation falls on a black metallic strip its temperature rises, and the resulting increase in resistance can be determined with a Wheatstone bridge arrangement. Early models of such devices, known as bolometersi 4 made use of platinum strips blackened with soot by means of a petroleum flame. The irreproducibility of this method of blackening led Lummer 2 and Kurlbaum to try instead the electrodeposition of platinum black, since composition of the plating solution, current, voltage, and time can be exactly defined and controlled. But there was one drawback: platinum black electrodeposited from pure chloroplatinic acid solutions did not adhere properly to the electrode. In attempting to overcome 9 this difficulty, Kurlbaum and Lummer5 recalled that platinum black can easily be precipitated from chloroplatinic acid solution by adding copper or lead, so that such chemically prepared platinum black always contains some copper or lead as well. Accordingly, they tried adding a small amount of copper sulphate, to the extent of about r% of the chloroplatinic acid present, to the plating solution, and found that tnis regularly produced very good platinum black deposits. Even better and more rapid results were attained by adding a small quantity of lead acetate. Their final recipe5 was 1 part of chloroplatinic acid and 0.008 parts of lead acetate to 30 parts of water, the electrolysis being -2 carried out at a current density of 30 mA cm at the cathode and with a potential difference of 4 volts between the (platinum) working electrodes. It is this recipe which was shortly afterwards adopted by Kohlrauschb for makingplatinum black electrodes for electrochemical purposes. Kohlrausch, to whom this preparation has at times been incorrectly attributed,7 stated clearly, but without quoting any litera- ture sources, that the method was that of Lummer and Kurlbaum. Only 8 in a later book is reference (51 specifically referred to. That this historic recipe is quite sound is shown by the results of more modern research which is discussed in the following sections. In the original bolometric study the platinum compound was referred 2,5 10,11 to as Tlatinchlorid", but both Kohlrausch9 and more recent books have pointed out that this term was commonly applied to chloroplatinic acid. This loose nomenclature has caused some confusion in the later literature and in many present day undergraduate laboratory manuals. 12,13 Even PtCl4 may mean chloroplatinic acid unless a special preparation9 of platinic chloride is given.
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