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Singh-IP-1968-Phd-Thesis.Pdf KINETICS OF THE HOMOGENEOUS REACTION BETWEEN PALLADIUM COMPOUNDS AND HYDRAZINE, FORMING METAL NUCLEI Thesis submitted for the degree of Doctor of Philosopy London University by Indra Pal Singh, M.Sc., D.Phil. Department of Metallurgy, Imperial College of Science December, 1967. & Technology, London, S.W.7. ABSTRACT The work discussed in this thesis comprises studies on the reduction of palladium (11) complexes by hydrazine in aqueous solutions, in order to find the causes of homogeneous nucleation in the electroless plating of palladium. This homogeneous nucleation sets in even in the absence of any third phase i.e. the article to be coated, and brings down all the palladium (11) as metallic powder, which obviously creates technical difficulties. The work has been kinetic in nature, and the mechanistic approach has remained mainly qualitative or semi-quantitative as much more thermodynamic information and data is necessary to give a more quantitative explanation. The experimental method consisted of measuring the time for the appearance of a cloud of metal precipitate for each concentration of the variable. The main variables which have been studied are palladium (11) concentration, hydrazine concentration and ammonia concentration. The rate dependence with respect to palladium was of a fractional order (1.76) at lower palladium ion concentration and higher orders (3) at higher palladium ion concentration. The rate with respect to hydrazine was found to be 2 .0 The rate dependence with respect to Palladium(11) and hydrazine in the system containing EDTA was found to be 1.5 and 2.5 respectively. The effect of ammonia concentration has been found favourable in preventing the precipitation of the metal. The evaluation of activation energy gave a value of 17.6 K. Cals/Mole at higher palladium ion concentration and 20.9 K. Cals at ordinary concentrations of palladium ion in the system containing mainly ammines. But in the system containing EDTJ the activation energy was found to be 17.3 K. Cals/Mole. The spectra of the solutions with different ranges of reactant concentration suggest that hydrazine forms complexes with palladium by displacement of ammonia and it is suggested that these substituted complexes are then reduced to the metal by a free radical mechanism, which has been discussed in detail. The spectral evidence also shows that hydrazine can displace all the four ammonia molecules of a palladous ammine in lower concentrations of ammonia. Further evidence of palladium (11) forming complexes with hydrazine has been obtained by nixing Pd(C104)2 with N2H4 2HC104, which forms bright yellow complexes with characteristic absorption peaks. The spectral data has been useful in suggesting the type of species involved in the reduction and thus giving a better picture of the mechanism. CONTENTS Pale 1. Introduction 1 2. A short review on the theories on nucleation 8 3. Review on earlier work on oxidation of hydrazine 15 4. Experimental methods and Experimental data 22 5. Interpretation of the Experimental data 42 6. Results and Discussion 46 7. Acknowledgement 61 8. References 62 9. Appendix 65 10.Figures 67 INTRODUCTION The work presented in this thesis was carried out to discover the factors responsible for the decomposition of baths in the electroless plating of palladium. The electroless plating of metals involves the reduction of complexed metal ions in solution by various reducing agents, under conditions which cause reduction at a catalytically active surface. In the case of palladium, the method of electroless plating was first developed by Rhoda and (1) Madison, who used palladous ammines and ethylene diamine tetra - acetate (ETA) complexes and reduced them with hydrazine at a suitable temperature. The optimum conditions of heterogeneous plating of palladium are given by the above authors in their paper. The electroless plating baths used for plating palladium undergo decomposition on long standing by a type of self • nucleating process and all the metal held in solution is thrown down as metallic powder. Sometimes this may happen even during the plating process if the solution has been stored for a long period. The decomposition of plating baths seems to involve two steps, in the first step the complex palladium ions react with the reducing agent at a very slow rate, producing palladium atoms and once a certain critical concentration of palladia= atoms is reached they agglomerate to form aggregats or clusters of atoms, until nuclei of a critical size are formed, creating a new heterogeneous phase. The second step is the participation of these nuclei in the further reduction of palladous ions by hydrazine by a catalytic process, The nuclei thus go on increasing in size by the deposition of palladium as a result of reaction at their surface and this leads to the precipitation of palladium as metallic powder. The second step discussed in the last paragraph is a catalysed reaction and should be quite fast. Therefore, the conditions which lead to the formation of palladium nuclei in the first step by a slow homogeneous reaction can be delayed by the control of chemical concentration of reactants. Although it is unlikely to be possible to keep the baths for indefinitely long times, it is not difficult to prolong their life by controlling the various factors involved in the reduction of metal ions to metallic powder. Though both physical and chemical factors are responsible for the decomposition of the plating baths, under normal conditions the control of chemical factors alone could produce quite effective results. This is not to say that physical factors are totally insignificant, but the physical factors are not easy to control under normal working conditions. The chemical factors on the contrary are easy to control and are sufficiently effective alone. -2 - In addition to the chemical and physical factors responsible for the formation of palladium nuclei, there are certain other factors, which can create a great deal of trouble in the storing of the plating baths. These are certain catalytically active particles introduced into the solution from the external atmosphere which bring about a heterogeneous decomposition of the solution before any homogeneous reduction has taken place. Thane external particles could be largely avoided by the use of scrupulously clean solutions and by keeping them in sealed vessels, which do not come in direct contact with the atmosphere. Sometimes a material contaminating the vessels may itself help in the decomposition of the solution, due to the participation of the unclean surface, which may be catalytically active. This may happen if the baths are not cleaned properly after the decomposition of the solution and all the metal sticking on the walls is not dissolved off properly by the use of acids such as aqua regia. In the present work it was found necessary to clean the flasks with fresh aqua regia as the re-used aqua regia did not dissolve all the palladium on the walls of the flasks and this -wands after lead to the rapid deoomposition of experimental solutions in subsequent runs. Though particles from the atmosphere and other 3 .00 sources may be responsible for the rapid decomposition of the plating baths, the main precipitation of metal in the form of powder is due to a homogendomschemical reduction and external impurities only accelerate the process if they are present. The reproducibility of results and the effects of concentration, temperature, etc. on the time before nucleation occurs suggest that spontaneous formation of fresh nuclei does occur. As discussed earlier, palladium atoms are formed by a slow homogeneous chemical reaction between palladium ions and hydrazine. The reaction obviously is a redox reaction, where palladium is reduced and hydrazine is oxidized by some type of electron transfer mechanism. For the reaction to take place it is necessary that the two reactants come close together by forming an intermediate complex, which can be a stable or a short lived species. This subj at will be discussed later in subsequent chapters. Palladium forms fairly stable ammines and ohlora- mmines, but the palladous ammines are more labile than their platinum anologues. Therefore, it is quite safe to assume that hydrazine may replace an ammonia molecule from a molecule of palladous ammine to form a monosubstituted hydrazine complex of palladium. The further replacement of - 4 ammonia by hydrazine depends purely on the relative concentration of the two ligands and will be discussed later. The possibility of palladium hydrazine complexes cannot be ruled out as a large number of metal hydrazine complexes are known and many metal hydrazine systems have been studied from structural and thermodynamic view points. (2) L. Sacconi and A. Sabatini have studied the I.R. Spectra of the hydrazine complexes of some bivalent metal ions. P. Abmad and S.M. Fazlur Rahman have reported some hydrazine (4) complexes of cobalt, nickel and copper. Banerjea and Singh have determined the formation constants of copper, nickel, cobalt, man;•anese and zinc complexes of hydrazine in aqueous (5) solutions. Swarzenbach and Zobrist found that four hydrazine molecules are co-ordinated to a zinc ion and six to a nickel ion in a manner comparable with ammonia. Robertus, (6) Laitinen and Bailar have found that zinc ion will co-ordinate with four hydrazine molecules with only slight differences in successive formation constants. All these studies confirm the fact that hydrazine acts as a monodentate ligand and quickly exchanges with ammonia in the palladous ammines, before any reduction of bivalent palladium ions takes place. (7) Audrieth and Ogg have pointed out that in most casts the number of hydrazine groups coordinated to a metal ion is one half of the normal co-ordination number of the -5- metal. Since no structural determinationhhave been made, it seems quite reasonable to predict the formation of three membered rings, but the low solubility of most of these comp- ounds suggest polynuclear structures involving hydrazine bridges rather than chelate structures.
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