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Signature Redacted Signature of Author , - 61 ".lectrodeposition of Aluminum from Organic Solutions" by M.C. Sze Submitted in Partial Fulfillment of The Requirement for The Degree of Bachelor of Science in The Departmenr of Chemical Engineering from Massachusetts Instituue of Technology 1939 Signature redacted Signature of Author , - 61 Signature of Professor in Charge Signature of Head of Department I ,.I.T. Dorm., Cambridge, Mass., May 15, 1939. Professor Walter G, Whitman, Head of the Department of Chemical Engineering, Massachusetts Institute of Technology, Cambridge, Mass. Dear Sir: I am enclosing herewith my thesis on "Electrodepostion of Aluminum from Organic Solutions", submitted in partial fulfillment of the requirement for the degree of Bachelor of Science. From my laboratory results, I have Zbached the conclusion that aluminum can be successfully electrodeposited from non-aqueous solutions to give a bright and adherent film. Yours respectifully, Signature redacted (Morg n C. Sze) Acknowledgment The author wishes to express his appreciation to his supervisor, Dr. H. H. Uhlig, for his assistance and advice in the preparation of this thesis. ABLr Of CONuA\N.LS I. SUMMARY Page 1 II. INTRODUCTION 2 III. LITERATURE SURVEY 3 IV. PROCEDURE 5 V. RESULTS AND DISCUSSION 7 VI. CONCLUSIONS 20 VII. RECOMMENDATIONS 21 VIII. APPENDIX A - DETAILS OF THE PREPARATION AND DEHYDRATION O0 SOME OF THE COMPOUNDS USED 22 IX. APPENDIX B - ORIGINAL DATA 25 X. APPENDIX C - DESCRIPTION OF THE ELECTROLYTIC CELL USED 29 XI. APPENDIX D - BIBLIOGRAPHY 31 - 1 - I* SUMMARY The results of this investigation indicate that aluminum can be electrolytically deposited to give an adherent and bright plate. The electrolytes most satisfactory for this purpose are found to be the following: (1) A solution containing the reaction products formed when aluminum bromide and aluminum chloride are dissolved in ethyl bromide and benzene (2) and (2) A solution containing the reaction products of aluminum chloride and ethyl bromide in chlorobenzene. It has been found that lyophilic colloids for benzene like rubber, milled or unmilled, are capable of giving a pronouneed brightening effect to the deposit. Upon buffing, a beautiful, silvery luster is easily obtained. Low current density is also a necessary condition to obtain a satisfactory deposit. Various other solutions have been studied, but they are all unsatisfactory,for either aluminum cannot be deposited, or the cathode current efficiency is extremely low. II. INTRODUCTION The purpose of this thesis was to try to electro- plate metallic aluminum from non-aqueous solutions to give an adherent and bright film. It has been long recognized that it is impossible to electro- deposit aluminum from aqueous solutions, simply because of side reactions at the electrodes. Never- theless, it has been shown that aluminum can be obtained electrolytically from organic solutions in the absence of water, although it is not known that any entirely satisfactory deposit has been previously obtained. Aluminum plating is of considerable commercial interest-. beside possessing an ornamental appearance, aluminum can also protect the iron or steel on which it is plated against corrosion. It is resistant to concentrated nitric acid free from chlorides. Aluminum plated steel has the advantage of possessing a surface of low emissivity together with high mechanical strength. This is often very desirable, such as in refrigerator car surfaces, etc. III. LITERATURE SURVEY Evidence of aluminum being electrolytically deposited was first noticed by elotnikoff ~ 1 )during an electrolysis of aluminum bromide in ethyl bromide in 1902. This work was confirmed by Patten(13) who determined the single potential of aluminum in such a solution. These were probably the earliest work done in this field. Later in 1916 Lalbin had found that aluminum could be deposited from a 10% solution of AlCl 3 in acetonitrile. Potassium fluoride was added to in- crease the conductance. Keyes, Swann, Klabinde, and Schicktanz(6) electrolyzed a solution of aluminum diethyl iodide and aluminum ethyl di-iodide and obtained aluminum. Quintin Marino(l 4 ) used a solution of aluminum oxalate and tartrate in liquid ammonia at low temperatures. In 1933, Keyes, Phipps, and Klabinde had found that aluminum can also be deposited from a solution of AlBr3 in (Et)4 NBr. The latest electrolyte for aluminum deposition was that found by Blue and Mathers(1)(2). They used a solution containing the reaction products of aluminum bromide, aluminum chloride, and ethyl bromide in benzene and xylene. According to the investigators, this solution had a surprisingly high conductance. besides, it also gave high current efficiencies. However, satisfactory aluminum deposits had never been obtained. They were always dark and often not very adherent. IV. PROCEDURE An electrolyte consisting or aluminum bromide, aluminum chloride, and ethyl bromide in benzene and xylene 2) was first prepared by dissolving AlBr 3 and AlCl 3 in benzene and xylene and adding to the mixture some ethyl bromide. The dark red reaction products were electrolyzed with an aluminum anode and a copper cathode. The bath was investigated to determine the effects of various additional agents, current density and temperature. The purpose was to find the optimum conditions whereat an adherent and bright deposit could be obtained. Copper cathodes and aluminum anodes were used exclusively throughout the investigation. ihe cathodes used were always pickled first with acid, washed with distilled water, and then distilled benzene. After electrolysis they were washed with benzene again. Simultaneously a search was made to find some other electrolyte from which aluminum could be deposited. Various anhydrous aluminum salts were dissolved in organic solvents and the solutions were tested to see whether they were conducting. In the cases where the solutions were found to be highly - (1- conducting, they were electrolyzed to see if aluminum could be deposited or not. Attempts were made to form some organo-aluminum complexes which would give high conductances and serve as electrolytic baths. The electric circuit employed for electrolysis was as follows: (Rhest-t cei coulaometer A,",-"Ceter The copper coulometer was used whenever the current efficiencies of the electrolyzing bath were determined. In the determination of influence or temperature on the nature of the aluminum deposit, the cell was immersed in a constant temperature oil bath regulated by mercury contact control. In all the above experimental work, great care was exercised in dehydrating the various solvents and salts used, as minute quantities of water may effect the results enormously. Details for the preparation and dehydration of some of the compounds used are given in the appendix. - I - V. RESULTS AND DISCUSSION The results of this thesis can be classified under two main headings; namely, (1) Solutions from which aluminum is deposited, and (2) Solutions from which aluminum is not deposited. A. Solutions from Which Aluminum Is Deposited. 1. AlBr3 , AlCl3 , and EtBr in Benzene and Xylene (2) This is the electrolyte suggested by Blue and Mathers for aluminum deposition. AlBr3 was first prepared reacting 6.0 g. of Al with 44.0 g. of bromine. The product was fused with 30.0 g. of AlCl 3 ' To this mixture were added 70.0 cc of xylene and 110.0 cc of benzene. A dark colored solution was obtained, to which o5.0 cc of ethyl bromide was added. -UCl gas was given off and two immiscible layers were formed. The bottom layer containing the red reaction products gradually increased in volume as the reaction proceeded. a. rffect of Additional Agents. Various additional agents were added to the electrolyte to see whether bright and adherent deposits could be odtained. The results are given in Table I. This work was all done at room temperature which was about 25'C. -8 - Table I Run Current Time Addition Nature of The Deposit No. Density (Hrs.) Agents 1 .125amp/i 20.0 None Laposit spongy, dark and coarsely crystal- line. 2 *074 " 20.b Added P2 05 Better throwing power; deposit still dark; loose Al particles were found on cathode; the layer of Al under- neath was more adher- ent. 3 .052 " -- Added 40cc Deposit dark, but chloroben- smoother, easily rub- zene; used bed off. N atmos- p.ere. 4 .071 " -- Added a Deposit adherent, less few parti- dark. cles of CaCl and 5cc 9f a colloidal soln. of rubber in benzene (lg.rubber per 100cc benzene). N2 used. 5 .112 " 17.6 bc more Deposit on the side of of the cathode facing the rubber anode was still dark soln. and not very adherent; but back side was bright and adherent; upon buffing, became very shiny. - C - The results in Table I indicate that rubber, a lyophilic colloid for benzene, has a pronounced brightening effect on the deposit. The reason that only the back side of the cathode has a bright deposit is obviously due to the fact that the current density in the front side is too high. By reducing the current density, satisfactory deposits can be obtained. The function of the minute quantity of rubber in this solution can be considered the same as that of glue in copper plating solutions. b. Effect of Current Density. From Table I we can already see that lower current density ought to give better deposits. Several runs were made at different current densities and the results are given in Table II. This work was also done at room temperature. The results in Table II confirm the fact that lower current density will give a much better deposit. Deposits at a current density below .025 amp./in.2 are very satisfactory. The reason that some of the deposits peel off upon buffing is probably that there are occluded electrolytes in the deposits. This electrolyte if in contact with moisture of if suddenly heated as by buffing will evolve a gas. The last sample, which is very - 10 - Table II Run Current Time Other Conditions Nature of The No.
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