US2408116A - Selenium coated elements and method of making them - Google Patents

Selenium coated elements and method of making them Download PDF

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US2408116A
US2408116A US402103A US40210341A US2408116A US 2408116 A US2408116 A US 2408116A US 402103 A US402103 A US 402103A US 40210341 A US40210341 A US 40210341A US 2408116 A US2408116 A US 2408116A
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selenium
metal
nickel
coated
solution
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US402103A
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Hippel Arthur Von
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Federal Telephone and Radio Corp
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Federal Telephone and Radio Corp
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Priority to BE481454D priority Critical patent/BE481454A/xx
Priority to FR962190D priority patent/FR962190A/fr
Application filed by Federal Telephone and Radio Corp filed Critical Federal Telephone and Radio Corp
Priority to US402103A priority patent/US2408116A/en
Priority to GB16824/42A priority patent/GB569473A/en
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Publication of US2408116A publication Critical patent/US2408116A/en
Priority to CH283551D priority patent/CH283551A/en
Priority to DEF4300A priority patent/DE973445C/en
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/06—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising selenium or tellurium in uncombined form other than as impurities in semiconductor bodies of other materials
    • H01L21/10—Preliminary treatment of the selenium or tellurium, its application to the foundation plate, or the subsequent treatment of the combination
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/06—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising selenium or tellurium in uncombined form other than as impurities in semiconductor bodies of other materials
    • H01L21/08—Preparation of the foundation plate
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/06—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising selenium or tellurium in uncombined form other than as impurities in semiconductor bodies of other materials
    • H01L21/10—Preliminary treatment of the selenium or tellurium, its application to the foundation plate, or the subsequent treatment of the combination
    • H01L21/101—Application of the selenium or tellurium to the foundation plate

Definitions

  • This invention relates to processes of treatin metal surfaces and products thereof, and it comprises processes wherein metal surfaces are subject to the action of selenidingagents to form a film including a form of selenium, presumably a metal selenium compound on the surface; it further comprises processes wherein such coated surfaces are thereafter further coated with selenium, and it further comprises the products of such processes.
  • selenium metal is customarily applied by spreading the molten selenium on the metal surface or otherwise producing a smooth coating on one surface.
  • Selenimn has a very high tension and it is difilcult to wet the metal surface with the molten selenium. As a consequence the selenium layer is not uniformly spread on the disc and does not adhere firmly thereto.
  • the problem involves at least two factors. The first is that of so changing surface tension relationships between molten selenium and the metal to be coated that the selenium will spread evenly over the metal.
  • My invention is based upon the discovery that In the single figure of the drawing is shown. by way of example, a disc, partly broken away, which may be considered as a selenium rectifier disc or a photo-sensitive element made in accordance with my invention. The dimensions of the disc are exaggerated in order to more clearly illustrate the component parts.
  • This comprises a metal disc I coated with a film 2 of a metal selenium compound of the metal. On the upper surface of the disc is shown a selenium layer 3.
  • my invention in part can be looked upon as the formation of a metal-selenium film on the metal prior to the application of metallic selenium thereto with the metal "selenide acting as a bonding agent for bonding the metal to the overlying selenium coating.
  • This film also improves the surface tension relationship so that ent ways.
  • One of the most convenient is that of selenium metal adheres much more strongly to dipping the metal, or otherwise treating its surface, with aqueous solutions of selenious acid or a. selenate, to which in some cases nitric acid has been added.
  • one suitable solution (for convenience called bath 1) consists of an aqueous nitric acid solution containing, in each liter, about 252 grams of nitric acid and about 105 grams of selenious acid expressed as $802. Such a solution is approximately 4 normal in nitric acid.
  • the metal surface on which a film of the selenide is to be formed is dipped or otherwise contacted with such a solution. The time of dipping is not important, from two to ten minutes is adequate. In such a solution the metal of the surface undergoing treatment reacts with selenium ions to form a metal-selenium compound.
  • the nickel for example, a strip or disc thereof
  • the surface of the nickel is attacked by the acid in the solution and nickel ions are formed.
  • a certain amount of nitrous oxide (NO) is also liberated and the nitrous oxide reduces selenious acid present to liberate divalent selenium ions.
  • NO nitrous oxide
  • These negative ions react with the positive nickel ions to form nickel selenide, NiSe.
  • the reactions actually occurring may be somewhat more complicated than this simple explanation would indicate.
  • the nickel selenium compound is deposited on the surfaces of the nickel strip or disc exposed to the solution. Then the treated metal is withdrawn from the aqueous solution. washed and dried. It can thereafter be coated with molten selenium and the selenium layer thus provided on the metal is uniform throughout and adheres firmly to the base metal.
  • the temperature during the selenidin8" operation is not critical although I find it advantageous to use moderately elevated temperatures of about 50 C. to 60 C. when using the nitric acid-selenious acid solution just described. With the solution at 57 C. treatment must continue for a minimum time of about 10 minutes to produce the desired result. If the treatment is continued too long, a pitting of the base metal results.
  • magnesiumaluminum alloys such as that known as Dow- Metal
  • aqueous solutions containing selenious acid can be dipped in aqueous solutions containing selenious acid, thereafter washed and dried, and finally coated with metallic selenium in any convenient way.
  • This alloy a selenium compound having a gray color is formed but the actual chemical composition of such compound is not clearly understood.
  • Dow-Metal is destroyed by acids so for this metal the nitric acid is omitted. In tests it was found that a 60% S802 solution produced a satisfactory film with a two minute treatment at 21 C. and a 10% S802 solution produced a satisfactory coating in three minutes at 21 C.
  • Tests alsoindicate that the same beneficial effects can be obtained with other metals, for example, the results of treating zinc with three types of solution to give satisfactory films are I Tempera- Bath Metal Time mm 140 Minutes C. mseori-"i norm HNOQ Zn 1 21 %%8e0
  • the metal Before seleniding the surface of the metal it is advantageous to first thoroughly clean it to free it of any solid particles, grease, rust, and the like. While this canbe accomplished in any way, I find it advantageous to first wipe the metal with a cloth to free it of any solid particles, dust, etc., then degrease the metal with any suitable solvent for oils and fats, such as trichlorethylene, ethylene dichloride, and the like, then subject the metal to an -electro-cleaning operation in ways known to the art. Finally the thus treated metal can be washed in hot and cold water and pickled in hydrochloric acid solutions, for example, to remove any rust and oxidation products.
  • any suitable solvent for oils and fats such as trichlorethylene, ethylene dichloride, and the like
  • the process of coating metal surfaces with selenium which comprises the steps of treating the surface with an aqueous solution containing nitric and selenious acid to form a metal selenium compound on the surface and thereafter coating the treated surface with selenium.
  • a selenium-coated metal plate having a selenium compound of the metal formed by sub- Jecting the surface of metal to an aqueous solu- ,tion of selenious acid underlying the selenium coating.

Description

Sept. 24; 1946. VQN 2,408,116,.
SELENIUN comma ELEMENTS AND METHOD or MAKING THE! Filed July 12, 1941 sag/W0 2 J'LE/V/DE 1744/ IN VENTOR ATTORNEY PalentedWMlHB' SELENIUM COATED ELEMENTS AND METHOD OF MAKING THEM Arthur von Hippel, Weston, Mass., assignor to Federal Telephone & Radio Corporation, a corporation of Delaware Application July 12, 1941, Serial No. 402,103
Claims. 1
This invention relates to processes of treatin metal surfaces and products thereof, and it comprises processes wherein metal surfaces are subiect to the action of selenidingagents to form a film including a form of selenium, presumably a metal selenium compound on the surface; it further comprises processes wherein such coated surfaces are thereafter further coated with selenium, and it further comprises the products of such processes.
The application of selenium to metals, such as iron, nickel. and others, for the purpose of preparing photoelectric cells, rectifiers, and the like, has hitherto presented many problems. Selenium metal is customarily applied by spreading the molten selenium on the metal surface or otherwise producing a smooth coating on one surface. Selenimn, however, has a very high tension and it is difilcult to wet the metal surface with the molten selenium. As a consequence the selenium layer is not uniformly spread on the disc and does not adhere firmly thereto. The problem involves at least two factors. The first is that of so changing surface tension relationships between molten selenium and the metal to be coated that the selenium will spread evenly over the metal. This can be realized by thoroughly cleaning the metal surface prior to applying the selenium. The second factor has to do with establishing a firm bond of adhesion between the selenium and the metal. The adherence of the film to the metal is of great importance in plates or discs to be used as rectifiers or light sensitive cells, and hithertothere has been no satisfactory way of improving the "bond" between the metal and the selenium film.
It has been previously found that an improved bond could be obtained by roughing the surface of discs before applying selenium thereto. However, even this rougheni'n'g does not secure a sufilciently close or firm bond. Moreover. it cannot be satisfactorily applied to base metal discs such as iron or aluminum discs which have been plated with another metal, such as nickel'or zinc, because the roughening treatment will cut through the plating exposing the plated metalto corrosion.
I have now discovered ways by which selenium matings on metal surfaces can be made to adhere tenaciously thereto and thus I am able to prepare selenium-coated metals which resist ro'ugh handling, abrasion, and the like, so that the selenium plates are not readily damaged in use.
My invention is based upon the discovery that In the single figure of the drawing is shown. by way of example, a disc, partly broken away, which may be considered as a selenium rectifier disc or a photo-sensitive element made in accordance with my invention. The dimensions of the disc are exaggerated in order to more clearly illustrate the component parts.
This comprises a metal disc I coated with a film 2 of a metal selenium compound of the metal. On the upper surface of the disc is shown a selenium layer 3.
Thus my invention in part can be looked upon as the formation of a metal-selenium film on the metal prior to the application of metallic selenium thereto with the metal "selenide acting as a bonding agent for bonding the metal to the overlying selenium coating. This film also improves the surface tension relationship so that ent ways. One of the most convenient is that of selenium metal adheres much more strongly to dipping the metal, or otherwise treating its surface, with aqueous solutions of selenious acid or a. selenate, to which in some cases nitric acid has been added. For example, one suitable solution (for convenience called bath 1) consists of an aqueous nitric acid solution containing, in each liter, about 252 grams of nitric acid and about 105 grams of selenious acid expressed as $802. Such a solution is approximately 4 normal in nitric acid. The metal surface on which a film of the selenide is to be formed is dipped or otherwise contacted with such a solution. The time of dipping is not important, from two to ten minutes is adequate. In such a solution the metal of the surface undergoing treatment reacts with selenium ions to form a metal-selenium compound.
Theoretically, the reactions occurring are probably as follows, using nickel as an example.
When the nickel, for example, a strip or disc thereof, is immersed in the solution, the surface of the nickel is attacked by the acid in the solution and nickel ions are formed. A certain amount of nitrous oxide (NO) is also liberated and the nitrous oxide reduces selenious acid present to liberate divalent selenium ions. These negative ions react with the positive nickel ions to form nickel selenide, NiSe. However, the reactions actually occurring may be somewhat more complicated than this simple explanation would indicate. In any event, the nickel selenium compound is deposited on the surfaces of the nickel strip or disc exposed to the solution. Then the treated metal is withdrawn from the aqueous solution. washed and dried. It can thereafter be coated with molten selenium and the selenium layer thus provided on the metal is uniform throughout and adheres firmly to the base metal.
The temperature during the selenidin8" operation is not critical although I find it advantageous to use moderately elevated temperatures of about 50 C. to 60 C. when using the nitric acid-selenious acid solution just described. With the solution at 57 C. treatment must continue for a minimum time of about 10 minutes to produce the desired result. If the treatment is continued too long, a pitting of the base metal results.
If the above selenious acid solution is made up with normal nitric acid (bath 2) instead of 4 normal then the temperature, for "seleniding nickel, can be reduced to about 45 C. for the same time of treatment.
These solutions are somewhat unstable due to the formation of nitrous acid. This can be overcome by the addition of sodium nitrite, in an amount of about 30 grams per liter, to the solution to form (bath 3). At the same time the temperature during the seleniding operation can be reduced to about 29 C. for the ten minutes of treatment.
If instead of 30 grams 60 grams of sodium nitrite is added to the 4 normal HNOa solution (bath 3A) two minutes treatment at about 29 C. is sufllcient for producing a film to which the selenium will firmly adhere.
In the foregoing example I have illustrated ways of practicing my invention for "selenidin8 nickel prior to the application of metallic selenium coatings thereto. The same process is used when iron is to be pretreated prior to coating with selenium. Iron surfaces ordinarily require a shorter dipping time than do nickel surfaces. As examples, it was found that iron when treated with (bath 1) required only two minutes at 29 C. and with (bath 2) only three minutes at 22 C.
Many other metals can be provided with a coating of a metal-selenium compound in exactly the same way. For example, magnesiumaluminum alloys, such as that known as Dow- Metal, can be dipped in aqueous solutions containing selenious acid, thereafter washed and dried, and finally coated with metallic selenium in any convenient way. With this alloy a selenium compound having a gray color is formed but the actual chemical composition of such compound is not clearly understood. Dow-Metal is destroyed by acids so for this metal the nitric acid is omitted. In tests it was found that a 60% S802 solution produced a satisfactory film with a two minute treatment at 21 C. and a 10% S802 solution produced a satisfactory coating in three minutes at 21 C.
Tests alsoindicate that the same beneficial effects can be obtained with other metals, for example, the results of treating zinc with three types of solution to give satisfactory films are I Tempera- Bath Metal Time mm 140 Minutes C. mseori-"i norm HNOQ Zn 1 21 %%8e0|+2 norm BNO; Zn 5 21 %NaSe04+2 norm BN0. Zn 2 21 It was found that while selenious acid (SeOa) constituents which will react with the metal to form metal ions thereof so that these positive ions can react with divalent negative selenium ions to form a metal selenium compound. Copper, nickel, iron, zinc, tin, magnesium-aluminum alloys, steels of various kinds, and other metals can be selenided as described above.
Before seleniding the surface of the metal it is advantageous to first thoroughly clean it to free it of any solid particles, grease, rust, and the like. While this canbe accomplished in any way, I find it advantageous to first wipe the metal with a cloth to free it of any solid particles, dust, etc., then degrease the metal with any suitable solvent for oils and fats, such as trichlorethylene, ethylene dichloride, and the like, then subject the metal to an -electro-cleaning operation in ways known to the art. Finally the thus treated metal can be washed in hot and cold water and pickled in hydrochloric acid solutions, for example, to remove any rust and oxidation products. Metal surfaces so treated and finally washed free of acid are quite readily wetted by selenium so that homogeneous films of metallic selenium can be applied thereto but the selenium does not adhere very strongly. But by selenium treating the surface of the metal prior to the application of the selenium, as described above, I am able to obtain selenium-coated surfaces wherein the selenium metal has greatly improved adherences.
Having thus described my invention, what I claim is:
1. In the coating of metal surfaces for the production of selenium coated plates the steps which comprise treating the metal surface with a solution containing a form of selenium to form a metal-selenium compound thereon and thereafter coating the treated surface with selenium.
2. The process as in claim 1 wherein the surface to be coated is nickel.
3. The process as in claim 1 wherein the surface to be coated is zinc.
4. The process as in claim 1 wherein the surface to be treated is a magnesium-aluminum alloy.
5. The process of coating metal surfaces with selenium which comprises the steps of treating the surface with an aqueous solution containing nitric and selenious acid to form a metal selenium compound on the surface and thereafter coating the treated surface with selenium.
6. The process as in claim 5 wherein the surface to be coated 1s nickel.
7. The process as in claim 5 wherein the surface to be coated is zinc.
8. A selenium-coated metal plate having a selenium compound of the metal formed by sub- Jecting the surface of metal to an aqueous solu- ,tion of selenious acid underlying the selenium coating.
9. Selenium-coated nickel having a nickel-selenium compound formed by subjecting the surface of the nickel to an aqueous solution of selenious acid underlying the selenium coating.
10. A process of treating galvanized iron surfaces with selenious acid to form a zinc selenium compound thereon.
ARTHUR VON I-IIPPEL.
US402103A 1941-07-12 1941-07-12 Selenium coated elements and method of making them Expired - Lifetime US2408116A (en)

Priority Applications (6)

Application Number Priority Date Filing Date Title
BE481454D BE481454A (en) 1941-07-12
FR962190D FR962190A (en) 1941-07-12
US402103A US2408116A (en) 1941-07-12 1941-07-12 Selenium coated elements and method of making them
GB16824/42A GB569473A (en) 1941-07-12 1942-11-26 Selenium coated elements and method of making them
CH283551D CH283551A (en) 1941-07-12 1948-02-24 Process for applying a selenium coating to a metal surface.
DEF4300A DE973445C (en) 1941-07-12 1950-10-01 Process for the production of metal plates covered with selenium for rectifiers, photo elements and the like. like

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CH (1) CH283551A (en)
DE (1) DE973445C (en)
FR (1) FR962190A (en)
GB (1) GB569473A (en)

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2522474A (en) * 1942-07-02 1950-09-12 Battelle Memorial Institute Treatment of zinc surfaces
US2527232A (en) * 1948-11-04 1950-10-24 Wright G Scroxton Bluing metals
US2575388A (en) * 1947-01-06 1951-11-20 Vickers Inc Electrical rectifiers
US2649409A (en) * 1943-07-30 1953-08-18 Standard Telephones Cables Ltd Electrodeposition of selenium
DE926987C (en) * 1952-06-10 1955-04-28 Falkenthal Process for the production of thin, cohesive, homogeneous, hexagonal selenium layers on a smooth, translucent base, e.g. B. on glass or quartz glass
US2822299A (en) * 1955-11-28 1958-02-04 Philips Corp Method of making a cadmium-telluride semi-conductive device
DE971697C (en) * 1948-10-01 1959-03-12 Siemens Ag Process for the manufacture of selenium rectifiers
US2937594A (en) * 1955-05-03 1960-05-24 Harris Intertype Corp Lithographic printing
US2997409A (en) * 1959-11-04 1961-08-22 Santa Barbara Res Ct Method of production of lead selenide photodetector cells
US3130137A (en) * 1959-10-14 1964-04-21 Nippon Electric Co Manufacture of selenium rectifier cell
US3178312A (en) * 1959-01-02 1965-04-13 Santa Barbara Res Ct Solutions and methods for depositing lead selenide
DE1207508B (en) * 1957-08-01 1965-12-23 Siemens Ag Semiconductor component with non-blocking contact electrodes and method for manufacturing
DE1229192B (en) * 1956-10-11 1966-11-24 Standard Elektrik Lorenz Ag Process for the manufacture of selenium rectifiers
US5089349A (en) * 1989-06-05 1992-02-18 Calgon Corporation Compositions and method for applying coatings to metallic surfaces

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1133471B (en) * 1961-08-30 1962-07-19 Licentia Gmbh Process for the production of selenium dry rectifiers
DE1141028B (en) * 1961-09-05 1962-12-13 Licentia Gmbh Process for the manufacture of selenium rectifiers
DE1185727B (en) * 1962-03-15 1965-01-21 Licentia Gmbh Process for the manufacture of selenium rectifiers

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT117386B (en) * 1927-12-06 1930-04-25 Sueddeutsche Telefon App Kabel Electric AC rectifier.
AT131780B (en) * 1930-08-07 1933-02-10 Erwin Falkenthal Photoelectric cell and method of making the same.
DE922896C (en) * 1938-08-16 1955-01-27 Siemens Ag Method of manufacturing a selenium rectifier

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2522474A (en) * 1942-07-02 1950-09-12 Battelle Memorial Institute Treatment of zinc surfaces
US2649409A (en) * 1943-07-30 1953-08-18 Standard Telephones Cables Ltd Electrodeposition of selenium
US2575388A (en) * 1947-01-06 1951-11-20 Vickers Inc Electrical rectifiers
DE971697C (en) * 1948-10-01 1959-03-12 Siemens Ag Process for the manufacture of selenium rectifiers
US2527232A (en) * 1948-11-04 1950-10-24 Wright G Scroxton Bluing metals
DE926987C (en) * 1952-06-10 1955-04-28 Falkenthal Process for the production of thin, cohesive, homogeneous, hexagonal selenium layers on a smooth, translucent base, e.g. B. on glass or quartz glass
US2937594A (en) * 1955-05-03 1960-05-24 Harris Intertype Corp Lithographic printing
US2822299A (en) * 1955-11-28 1958-02-04 Philips Corp Method of making a cadmium-telluride semi-conductive device
DE1229192B (en) * 1956-10-11 1966-11-24 Standard Elektrik Lorenz Ag Process for the manufacture of selenium rectifiers
DE1207508B (en) * 1957-08-01 1965-12-23 Siemens Ag Semiconductor component with non-blocking contact electrodes and method for manufacturing
US3178312A (en) * 1959-01-02 1965-04-13 Santa Barbara Res Ct Solutions and methods for depositing lead selenide
US3130137A (en) * 1959-10-14 1964-04-21 Nippon Electric Co Manufacture of selenium rectifier cell
US2997409A (en) * 1959-11-04 1961-08-22 Santa Barbara Res Ct Method of production of lead selenide photodetector cells
US5089349A (en) * 1989-06-05 1992-02-18 Calgon Corporation Compositions and method for applying coatings to metallic surfaces

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DE973445C (en) 1960-02-18
FR962190A (en) 1950-06-02
BE481454A (en)
CH283551A (en) 1952-06-15
GB569473A (en) 1945-05-25

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