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United States Patent (19) [11] 3,880,728 Habermann Et Al

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United States Patent (19) [11] 3,880,728 Habermann Et Al United States Patent (19) [11] 3,880,728 Habermann et al. (45) Apr. 29, 1975 54. MANUFACTURE OF LEAD 3,486,940 12/1969 Ruben................................... 36/26 DIOXIDE/TITANIUM COMPOSITE 3,499,795 3/1970 Ruben......... - - - - - - - - - - - - - - - - - - 136/26 X 3,649,485 3/1972 Chisholm..... - - - - - - - - - 204/290 F X ELECTRODES 3,770,63 l i? 1973 Chisholm..................... 204/290 F X 75) Inventors: Wolfgang Habermann, Mainz; Heinz Nohe, Meckenheim; Peter Jaeger, Primary Examiner-G. L. Kaplan Ludwigshafen, all of Germany Attorney, Agent, or Firm-Johnston, Keil, Thompson 73) Assignee: BASF Aktiengesellschaft, & Shurtleff Ludwigshafen (Rhine), Germany 22 Filed: Sept. 3, 1974 57 ABSTRACT (21) Appl. No.: 502,666 A method of producing lead dioxide/titanium compos ite electrodes by anodic deposition of lead dioxide on 52 U.S. Cl............... 204/38 A; 136/26; 204/290 F a titanium surface, in which an intermediate layer of a (51) Int. Cl. ......................... B01k 3/06; C23f 17/00 carbide or boride of an element of sub-group 4 or 5 (58) Field of Search.......... 204/38 A, 290 F, 57, 42; and/or silicide of an element of sub-group 4, 5 or 6 of 1361120 R, 26 the periodic table of the elements and/or silicon car bide, is applied to the titanium surface before deposit 56) References Cited ing the lead dioxide. UNITED STATES PATENTS 8 Claims, No Drawings 2,636,856 4/1953 Suggs et al...................... 204/290 F 3,880,728 2 MANUFACTURE OF LEAD IDIOXIEDE/TITANIUM lum carbide and tantalum boride should be singled out COMPOSITE ELECTRODES specifically. This invention relates to a process for the production Preferred silicides for use in the intermediate layers of lead dioxide/titanium composite electrodes which are titanium disilicide, zirconium disilicide, tantalum are specifically useful as anodes in electrolysis cells of disilicide, chromium disilicide and niobium disilicide, high current density. amongst which chromium disilicide, titanium disilicide Composite electrodes of a base consisting of titanium and zirconium disilicide give particularly dense inter to which lead dioxide coatings have been applied are mediate layers because of their low melting points, known. Such electrodes are manufactured by conven which are from 1,500 to 1,700°C. Silicon carbide is tional methods, through anodic deposition of the oxide also preferred. from lead-Il salt solution onto the titanium substrate. Of course, the intermediate layers can also consist of Because titanium blocks the passage of current if it is a mixture of these compounds. wired as the anode in an electrolysis system, it is how To manufacture the electrodes, the base is first ever not possible anodically to deposit an even and cleaned, preferably mechanically, for example by sand well-adhering lead dioxide coating on a titanium sur 15 blasting or corundum blasting. Thereafter, the carbides face. It is known to avoid this blockage by adding fluo and borides of the elements of sub-groups 4 and 5 of rides to the lead salt bath or by mechanically roughen the periodic system (Ti, Zr, Hf, V, Nb and Ta) and the ing, and degreasing, the titanium surface. silicides of the elements of sub-groups 4 to 6 of the per According to a known proposal, smooth, even, very iodic system (Ti, Zr, Hf, V, Nb, Ta, Cr, Mo and W) well-adhering coatings of lead dioxide on titanium sur and/or silicon carbide are applied. For this purpose, the faces, which even as thin coatings are stable to anodic plasma spraying process can be used and is advanta polarization, are attained by using oxidative treatment geously carried out under a protective atmosphere of in the presence of compounds of metals of sub-groups argon gas; in this process, the powders of the com l, 6, 7 and 8 of the periodic table and of aluminum, va pounds mentioned, of particle sizes preferably from 15 nadium and bismuth to produce a titanium dioxide to 90 pu, are fed to a plasma torch with argon plasma. coating, modified with the oxides of these metals, on The thickness of the intermediate layers produced in the titanium surface prior to depositing the lead dioxide preferably from about 60 to 200 pu, but where the layers coatings. contain more than 20 percent by weight of the silicides Finally, it is also known to manufacture lead diox mentioned, and/or of silicon carbide, a thickness down ide/titanium composite electrodes by applying seeds of to 20 u, suffices. finely divided platinum, palladium, gold, magnetite, To improve the electron conductivity, the silicides or graphite and/or lead dioxide to the titanium surface be the silicon carbide can also be modified with metals or fore the anodic deposition of lead dioxide. halides of the iron group, especially with iron itself. The The electrodes produced in accordance with the pro 3 5 proportion of metals or halides of the iron group is so cesses which have been disclosed are not equally suit chosen that the content, based on pure metal, in the sil able for all applications. Thus, for example, they suffer icide does not exceed 5 percent by weight. from the disadvantage that - if they are employed as Further suitable methods for applying the borides, anodes in electrolysis cells of high current throughput carbides or silicides and the silicon carbide are the - the lead dioxide layers flake off, especially after pro 40 flame spraying process and high vacuum vapor-coating. longed anodic polarization, and this results in the grad In these processes, as in the plasma spraying process, ual formation of a blocking layer of titanium dioxide it is important that the electrically conducting base between the titanium and the lead dioxide. If the pro should be freed from oxides on the surface which is to cess carried out uses noble metals, such electrodes can, be coated. for example when employed as anodes in electrolysis 45 A particularly suitable process for applying interme cells with cathodes of high hydrogen overvoltage, inac diate layers of silicon or silicon carbide to electrically tivate the cathodes. Furthermore, some of the conven conducting shapes has proved to be vapor phase depo tional processes are costly and time-consuming. sition by a chemical reaction with application of radi It is an object of the present invention to provide a ant energy or heat energy. Thus, for example, halides process for the production of lead dioxide/titanium 50 of elements of sub-groups 4 to 6 can be reacted with si composite electrodes which provides electrodes which lanes or silicon halides and hydrogen or base metals to do not show the said disadvantages and which can be give silicides which deposit as dense coatings on the used as anodes in electrolysis cells of high current surface of the electrically conducting bases. throughput without showing the disadvantage that the In this process it is again possible to produce interme lead dioxide layers flake off. Other objects will be ap 55 diate layers modified with metals or halides of the iron parent from the description. group, by introducing metals or halides of the iron We have found that this object is achieved by a pro group into the vapor phase. A particularly advanta cess for the production of lead dioxide/titanium com geous feature of the chemical vapor phase deposition posite electrodes by anodic deposition of lead dioxide method is that non-porous coatings can be produced on on titanium surfaces wherein an intermediate layer of 60 the base. a carbide or boride of an element of sub-group 4 or 5 in addition to this process, it is also possible to de and/or a silicide of an element of sub-group 4, 5 or 6 posit or produce the silicides or the silicon carbide by of the periodic table of the elements and/or silicon car cathodic spraying, electrophoretic deposition from sus bide, is applied to the titanium surface before deposit pensions, or chemical reduction. ing the lead dioxide. The titanium bodies pretreated in this way are then Particularly suitable carbides and borides are those provided with a PbO coating by conventional anodic of titanium and tantalum, and titanium carbide, tanta methods. 3,880,728. 3 4 For this purpose, they are anodically polarized in aqueous 1 to 25 per cent strength lead(II) nitrate or EXAMPLE 4 lead(II) perchlorate solutions which can advanta An expanded titanium metal mesh of dimensions 100 geously contain up to 0.5 percent of copper(II) nitrate X 40 mm was corundum-blasted and coated with fine and up to 0.2 percent of a wetting agent, for example 5 grained titanium disilicide, particle size from 20 to 40 based on ethoxylated alcohols. The current density is pu, to a thickness of about 100 pu, by means of a plasma torch, under a blanket of argon gas. In carrying out the advantageously from 1 to 10 A/dm and the tempera coating, the plasma torch was operated with argon con ture is advantageously from 40 to 80°C. Copper is a taining less than 0.5 percent of nitrogen. The expanded suitable cathode material. Good convection is advanta titanium metal was at a temperature of s 60°C during geously ensured by stirring or circulation. The pH value coating. of the solution, which decreases during the electrolysis, The expanded titanium metal mesh pretreated in this is preferably maintained within the range 1 < pH S way was dipped to a depth of 5 cm, along its longitudi 5 by adding basic lead carbonate. nal axis, into a solution which was prepared by dis It is an advantage of the process that the intermediate 15 solving 300 g of Pb(NO), 3 g of Cu(NO) 3 HO and layers thus produced can be re-used as a base for fresh 1 g of a wetting agent based on ethoxylated alcohols in PbO, coatings even after the PbO has detached com water to make a total of 1 liter, and was coated at a pletely, which permits the use of the electrodes in sec temperature of from 60 to 70°C for 3 hours, using a ondary batteries.
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