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United States Patent Office Patented Oct 3,214,355 United States Patent Office Patented Oct. 26, 1965 2 body which has already been impregnated with a metallic 3,214,355 Salt solution is polarized cathodically in an alkaline solu PROCESS FOR THE FILLING OF PORES OF METALLIC OR METALLC COATED FRAMES tion so as to obtain an evenly distributed filling of the WITH METALLIC HYDROXDES AND PROD pores with the active mass. UCTS THEREOF 5 Principal objects and features of the present invention Ludwig Kandler, Alescherstrasse 10, are the provision of novel processes for preparing elec Munich-Soln, Germany trodes and for filling their pores with active materials by No Drawing. Continuation of application Ser. No. methodic polarization treatment which provides material 837,332, Sept. 1, 1959. This application May 24, advantages over the processes heretofore known, by way 1962, Ser. No. 197,292 O of greatly speeded up production as compared with those Claims priority, application Germany, Sept. 3, 1958, processes now extant, lower energy consumption in prac K 35,669 ticing the new method as compared with known methods, 10 Claims. (Ci. 204-56) lower consumption of chemicals as compared with chemi cal pore filling processes as heretofore practiced, very This application is a continuation of my copending fine and even distribution of active masses into the pores application Serial No. 837,332, filed September 1, 1959, of the electrode frame body and as a result substantially now abandoned. 100% participation of the active masses within the elec This invention relates to galvanic elements and bat trode pores during charging and discharging of batteries teries and to process and more particularly to a process and condensers equipped with electrodes prepared accord for filling the pores of metallic or surface metallized 20 ing to the process. frames with active material with the aid of metallic Additional objects and features of the invention will oxides or metallic hydroxides. It also relates to positive become apparent from the following detailed specifica and negative electrodes for alkaline batteries, to batteries tion, it being understood that the details as set forth containing such electrodes and to electrodes for electro hereinafter are by way of example and not of limitation. lytic condensers or the like, and to condensers equipped In accordance with the procedure of this invention, the with such electrodes. It also relates to production of pores of metallic or metal-coated frames are filled with highly active catalyzers. metal-oxides or metal-hydroxides by cathodic polarization It is already known that it is of great importance for in such manner that between a soluble or non-soluble the efficiency of galvanic elements and batteries that the anode and the body of the frame acting as a cathode transformation of matter which is taking place at the 30 there is produced an electrolysis in an acid electrolyte electrodes and which is capable of supplying electric en which contains the metal ions which are to be thrown ergy, should take place with the least possible interfer off as oxides or hydroxides, and also the reducible ions ence and that the highest possible percentage of the total which have a redox potential that is more positive than available quantities of substances should participate in the cast-off potential of the metal ions. During this the electro-chemical process. These demands may be process while electrolysis takes place in the electrolyte best complied with, the more porous the active electrode space, there is maintained outside of the cathode a pH Substances are and the larger the really attainable surface value of the electrolyte which does not permit any pre of the reacting substances is in comparison with the geo cipitations of metallic hydroxide within the electrolyte. metrical dimensions of the electrodes. By making use The body of the frame is dipped as a cathode into an of porous active masses within a supporting frame it is 40 acid electrolyte solution which contains the metal to be possible, as already known, to comply more or less with exuded in the form of ions. Due to the fact that the the above demands. electrolyte contains ions having a more positive redox For instance, a suitable supporting frame may be com potential than the discharge potential of the metal ions, posed of a porous sintered layer of metal powders which there is no discharge of metal ions during the electrolysis do not react with the electrolyte and which do not exert at the cathode, but instead a reduction of the ions with any influence on the electro-chemical process. However, the more positive redox potential, using up hydrogen ions. electrically conductive porous supports made of plastic, The consumption of the hydrogen ions causes the increase glass wool, etc., may also be used. of the pH value of the electrolytic solution within the In the pores of such frames the active masses (finely pores of the frame body. On the outer surface of the distributed metals or metal alloys) are inserted. Up to frame body the increase of the pH value is reduced by now the insertion was achieved by a chemical impregna the subsequent diffusion of the hydrogen ions which are tion process, as for instance the preferred method in the contained in an excessive amount within the acid elec manufacture of electrodes for alkaline batteries whereby trolyte. However, within the pores the rate of consump the porous electrode frames were dipped into a solution tion of hydrogen ions is considerably larger than rate of cadmium or nickel salts, then dried and subsequently of diffusion and therefore the eletrolyte becomes alka dipped into an alkali. During that process cadmium or line. This provides, as a consequence, a precipitation nickel hydroxides are precipitated into the pores of the of metallic hydroxide. electrode frame. By repeating this process a few times Due to the increase in diffusion resistance the hydrox the pores are filled to a considerable extent with cadmium ide precipitation starts at the most inapproachable or in or nickel hydroxide. By an electro-chemical process of 60 accessible portions of the frame support, meaning that electrolytic reduction in the alkaline electrolytes the cad the pores of the frame or base are filled in the most ad mium hydroxide is transformed into finely distributed vantageous manner from inside-out with metallic hydrox porous cadmium metal, or by means of an electrolytic ide. It is therefore possible by electro-chemical means oxidation the bivalent nickel hydroxide is transformed to fill all accessible pores with a very finely distributed into the trivalent nickel hydroxide. Such already known porous active mass, even in the case of frames of sev processes for filling of pores of the electrode frames with eral millimeters thickness, such as for instance 2 to 5 mm. the aid of electro-chemical active substances are very thickness. tedious and require, because of the repeated drying steps The metal hydroxides which have been deposited ac during the repetition of the filling, a considerable amount cording to the invention into the pores may then, accord of energy. ing to the already know methods, be reduced by electrol There is also already known a process for the filling 70 ysis into finely divided metals or may by electrolytic of the pores of the electrode body whereby the electrode oxidation be transformed into oxides of a higher value. 3,214,355 3 4. It is, for instance, possible to build very effective solution the empty spaces created by the drying, resulting in the anodes or depolarization cathodes for galvanic elements desired capacity increase. and batteries. The process of the invention of filling by When constructing a cadmium electrode the pores of electro-chemical means the pores of body frames with the frame body are filled according to the invention very thinly divided porous active masses can be used, 5 with cadmium hydroxide and the frame body is subse aside from the manufacture of cadmium or nickel elec quently electrically connected in an alkaline electrolyte trodes for batteries, in a quite general manner for the solution bath as a cathode. This results in the reduc precipitation of metallic oxides or hydroxides in porous tion of the previously formed cadmium hydroxide into frame materials. The essential requirement is the pres finely dispersed cadmium metal. Inasmuch as the dis ence of ions which are reduced with the aid of cathodic O placement of the metal is lower than the volume of the polarization with simultaneous consumption of hydrogen hydroxide, the reduction furnishes additional space or ions whereby the electrolyte dissolution takes place with volume in the space or void of the pores which is filled in the pores and the electrolyte becomes alkaline within with additional cadmium hydroxide during a new cathodic the pores of the frame and causes the hydroxides to pre polarization of the partly filled frame body. cipitate in the pores. In the electrolyte outside of the Consequently, it is possible by using the above de body frame there is maintained a pH value which does scribed features of the invention to obtain a maximum not permit a precipitation of metal hydroxides. active material retaining capacity of the thus processed Especially suitable ions for this purpose are nitrate frame body whereby a result of importance is that dur ions. However, also all other ions with a high redox ing the use of electrodes prepared according to the in potential, as chromium acid ions, chlorate ions and per vention, the active masses that have been introduced manganate ions may be used. It is therefore possible, into the pores participate to practically 100% in the for instance, to manufatcure, aside from electrodes of delivery of current of galvanic element or battery equipped galvanic elements and batteries, active layers of electrodes with such electrodes.
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