US3266948A - Carbide deposition on tantalum - Google Patents
Carbide deposition on tantalum Download PDFInfo
- Publication number
- US3266948A US3266948A US315413A US31541363A US3266948A US 3266948 A US3266948 A US 3266948A US 315413 A US315413 A US 315413A US 31541363 A US31541363 A US 31541363A US 3266948 A US3266948 A US 3266948A
- Authority
- US
- United States
- Prior art keywords
- tantalum
- carbide
- lampblack
- hydrogen
- mercury
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims description 32
- 229910052715 tantalum Inorganic materials 0.000 title description 13
- 230000008021 deposition Effects 0.000 title description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical class [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 15
- 239000006233 lamp black Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 claims description 11
- 229910003468 tantalcarbide Inorganic materials 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000000576 coating method Methods 0.000 description 13
- 239000011248 coating agent Substances 0.000 description 12
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 12
- 229910052753 mercury Inorganic materials 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052778 Plutonium Inorganic materials 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000001427 coherent effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- OYEHPCDNVJXUIW-UHFFFAOYSA-N plutonium atom Chemical compound [Pu] OYEHPCDNVJXUIW-UHFFFAOYSA-N 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000010943 off-gassing Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000004449 solid propellant Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/60—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using solids, e.g. powders, pastes
- C23C8/62—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using solids, e.g. powders, pastes only one element being applied
- C23C8/64—Carburising
Definitions
- the present invention relates to a method of forming a carbide coating 'on metal and, more particularly, forming a surface layer of tantalum carbide on tantalum metal.
- Liquid fuel reactors possess many advantages over solid fuel reactors such as reprocessing during operation and rapid change from a critical configuration to a non- :critical configuration. Utilization of plutonium as a reactor fuel is advantageous when utilized in a breeding cycle. Consequently, a great deal of effort has been invested in the development of a molten plutonium reactor. It has been found quite diflicult to find a material capable of containing the molten plutonium without excessive corrosion. Perhaps the most promising material is carbide coated tantalummetal. Since this coated tantalum is to be used as a structural material, it is highly desirable that the metal substrate retain its ductile characteristics.
- Tantalum powders have been coated with tantalum carbide by the intimate admixture of tantalum powder with carbon black under dry hydrogen between 1400 to 1600 C. From this prior art, it might be expected that massive tantalum could be coated with carbide at a higher temperature. Although this method forms a tantalum carbide Isolating on a tantalum powder, it has been found that the carbide diffuses into the tantalum substrate thereby causing the tantalum to assume an unwanted hardness. Carburization has also been effected by heating in a methane atmosphere. However, this method is disadvantageous in that the methane spontaneously pyrolyzes thereby depositing an interfering coat of carbon on the surface. Such a coating is spotty and incapable of protecting the tantalum metal as would a carbide coating.
- the present invention permits the formation of a very thin coherent layer of tantalum carbide on tantalum metal when it is heated in contact with lampblack in an atmosphere of hydrogen. Temperatures of 800 to 1160 C. permit the retention of the tantalum substrate softness.
- a piece of tantalum is packed in lampbl-ack and the system is evacuated to about 10 mm. of mercury.
- the system is heated to the desired temperature (between 800 and 1160 C.) and held at this temperature for between and 50 minutes in order to outgas the tantalum metal and lampblack.
- Hydrogen is then added to a pressure above 100 mm. of mercury, preferably between 200 and 300 mm. of mercury. Hydrogen is added after attaining the desired temperature in order to minimize hydride production and to permit outgassing. It is assumed, although this assumption forms no part of the invention, that methane produced at the desired temperature reacts with tantalum to form a light surface coating of carbide. This assumption is based on the fact that there is no carburization if hydrogen is not present.
- lampblack is the only carbon source presently known which is eflicacious in the above method. All sizes and purities of graphite have been utilized, but have uniformly failed to achieve a satisfactory coating. Furthermore, the lampblack packing may only be used one time effectively. This tends to indioate that the contaminants in lampblack are beneficial and permit the satisfactory coating to be obtained under the reaction conditions specified. Lampblack of average particle size angstroms, can yield a coating as thin as one micron when a temperature of 800 C. is utilized. If a less finely divided lampblack is used, e.g., less than one micron particle size and approximately A micron particle size, a coating of between 2 and 3.5 microns thickness is achieved. Temperatures of 1200 C. and above are not useful in the above-described method since these temperatures will result in hardening of the tantalum substrate.
- Example 1 A tantalum metal piece is packed in [a -angstrom average particle size lampblack.
- the metal and lampblack are placed in a quartz tube furnace and heated to 800 C. at a pressure of about l0- mm. of mercury. These conditions are held for 45 minutes for outgassing purposes and then hydrogen is admitted bringing the pressure up to 200 mm. of mercury. These conditions are held for two hours and then cooled to room temperature.
- the tantalum carbide coating found on the tantalum metal piece is coherent and one micron thick.
- Example 2 A tantalum metal piece is packed in a less finely divided lampb lack (i.e., approximately A micron average particle size) placed in a quartz tube furnace. The system is heated to 1100 C. at a pressure of about 10 mm. of mercury and held at these conditions for about 15 minutes. Subsequently, hydrogen is admitted to bring the pressure up to 300 mm. of mercury and the 1100 C. temperature and 300 mm. hydrogen pressure is maintained for two hours and 15 minutes. A 3 micron tantalum carbide coating results.
- Example 3 Lampblack as in Example 2 is used in packing a tantalum metal in a quartz tube furnace.
- a temperature of 1100 C. at a pressure of about 10' to l0 mm. of mercury is maintained for 50 minutes, after which hydrogen is admitted bringing the pressure up to 300 mm. of mercury.
- the 1100 C. temperature is maintained for one hour and a coating of two to three micron thickness results.
- Lampblack is the only known carbon source which will permit the above described reaction and each lampblack packing may the used only once effectively.
- the method is independent of surface treatment. Some samples have been pickled in acid solution and yielded identical coatings under identical reaction conditions as those utilizing an unpick-led metal piece.
- the method of forming a tantalum carbide on tantalum metal comprising heating the tantalum metal in 3 contact with lampblack in an atmosphere of hydrogen at a temperature between 800 and 1160 C.
- reaction system is held in a vacuum of about 10 mm. of mercury before the addition of hydrogen.
- a method as in claim 4 wherein the pressure after addition of hydrogen is between 200 and 300 mm. of mercury.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Description
3,266,948 Ice Patented August 16, 1966 3,266,948 CARBIDE DEPOSITION N TANTALUM Joseph C. McGuire, White Rock, N. Mex., assignor to the United States of America as represented by the United States Atomic Energy Commission No Drawing. Filed Oct. 10, 1963, Ser. No. 315,413 6 Claims. (Cl. 14813.1)
The present invention relates to a method of forming a carbide coating 'on metal and, more particularly, forming a surface layer of tantalum carbide on tantalum metal.
Liquid fuel reactors possess many advantages over solid fuel reactors such as reprocessing during operation and rapid change from a critical configuration to a non- :critical configuration. Utilization of plutonium as a reactor fuel is advantageous when utilized in a breeding cycle. Consequently, a great deal of effort has been invested in the development of a molten plutonium reactor. It has been found quite diflicult to find a material capable of containing the molten plutonium without excessive corrosion. Perhaps the most promising material is carbide coated tantalummetal. Since this coated tantalum is to be used as a structural material, it is highly desirable that the metal substrate retain its ductile characteristics.
Tantalum powders have been coated with tantalum carbide by the intimate admixture of tantalum powder with carbon black under dry hydrogen between 1400 to 1600 C. From this prior art, it might be expected that massive tantalum could be coated with carbide at a higher temperature. Although this method forms a tantalum carbide Isolating on a tantalum powder, it has been found that the carbide diffuses into the tantalum substrate thereby causing the tantalum to assume an unwanted hardness. Carburization has also been effected by heating in a methane atmosphere. However, this method is disadvantageous in that the methane spontaneously pyrolyzes thereby depositing an interfering coat of carbon on the surface. Such a coating is spotty and incapable of protecting the tantalum metal as would a carbide coating.
The present invention permits the formation of a very thin coherent layer of tantalum carbide on tantalum metal when it is heated in contact with lampblack in an atmosphere of hydrogen. Temperatures of 800 to 1160 C. permit the retention of the tantalum substrate softness.
It is accordingly an object of the present invention to provide a tantalum carbide coated tantalum metal wherein the tantalum metal substrate retains its ductile characteristics.
It is a further object of this invention to provide a thin coherent coating of tantalum carbide on tantalum metal thereby protecting the tantalum from oxidation.
According to the present invention a piece of tantalum is packed in lampbl-ack and the system is evacuated to about 10 mm. of mercury. The system is heated to the desired temperature (between 800 and 1160 C.) and held at this temperature for between and 50 minutes in order to outgas the tantalum metal and lampblack. Hydrogen is then added to a pressure above 100 mm. of mercury, preferably between 200 and 300 mm. of mercury. Hydrogen is added after attaining the desired temperature in order to minimize hydride production and to permit outgassing. It is assumed, although this assumption forms no part of the invention, that methane produced at the desired temperature reacts with tantalum to form a light surface coating of carbide. This assumption is based on the fact that there is no carburization if hydrogen is not present.
It should be noted that lampblack is the only carbon source presently known which is eflicacious in the above method. All sizes and purities of graphite have been utilized, but have uniformly failed to achieve a satisfactory coating. Furthermore, the lampblack packing may only be used one time effectively. This tends to indioate that the contaminants in lampblack are beneficial and permit the satisfactory coating to be obtained under the reaction conditions specified. Lampblack of average particle size angstroms, can yield a coating as thin as one micron when a temperature of 800 C. is utilized. If a less finely divided lampblack is used, e.g., less than one micron particle size and approximately A micron particle size, a coating of between 2 and 3.5 microns thickness is achieved. Temperatures of 1200 C. and above are not useful in the above-described method since these temperatures will result in hardening of the tantalum substrate.
The method of the invention can best be illustrated by the following examples which are \given for this purpose only and not for the purpose of limiting the spirit and scope of the present invention.
Example 1 A tantalum metal piece is packed in [a -angstrom average particle size lampblack. The metal and lampblack are placed in a quartz tube furnace and heated to 800 C. at a pressure of about l0- mm. of mercury. These conditions are held for 45 minutes for outgassing purposes and then hydrogen is admitted bringing the pressure up to 200 mm. of mercury. These conditions are held for two hours and then cooled to room temperature. The tantalum carbide coating found on the tantalum metal piece is coherent and one micron thick.
Example 2 A tantalum metal piece is packed in a less finely divided lampb lack (i.e., approximately A micron average particle size) placed in a quartz tube furnace. The system is heated to 1100 C. at a pressure of about 10 mm. of mercury and held at these conditions for about 15 minutes. Subsequently, hydrogen is admitted to bring the pressure up to 300 mm. of mercury and the 1100 C. temperature and 300 mm. hydrogen pressure is maintained for two hours and 15 minutes. A 3 micron tantalum carbide coating results.
Example 3 Lampblack as in Example 2 is used in packing a tantalum metal in a quartz tube furnace. A temperature of 1100 C. at a pressure of about 10' to l0 mm. of mercury is maintained for 50 minutes, after which hydrogen is admitted bringing the pressure up to 300 mm. of mercury. The 1100 C. temperature is maintained for one hour and a coating of two to three micron thickness results.
It will be seen from the above discussion that a method is described which coats tantalum metal with tantalum carbide at unexpectedly low temperatures, thereby yielding a beneficial high ductility tantalum substrate. Lampblack is the only known carbon source which will permit the above described reaction and each lampblack packing may the used only once effectively. The method is independent of surface treatment. Some samples have been pickled in acid solution and yielded identical coatings under identical reaction conditions as those utilizing an unpick-led metal piece.
What is claimed is:
1. The method of forming a tantalum carbide on tantalum metal comprising heating the tantalum metal in 3 contact with lampblack in an atmosphere of hydrogen at a temperature between 800 and 1160 C.
2. A method as in claim 1 wherein the hydrogen is added after the desired temperature is maintained for a period between 15 and 50 minutes.
3. A method as in claim 2 wherein the reaction system is held in a vacuum of about 10 mm. of mercury before the addition of hydrogen.
4. A method as in claim 3 wherein a sufficient quantity of hydrogen is added to bring the reaction system pressure to above 100 mm. of mercury.
5. A method as in claim 4 wherein the pressure after addition of hydrogen is between 200 and 300 mm. of mercury.
6. A method as in claim 1 wherein the lampblack is of less than one micron average particle size.
References Cited by the Examiner DAVID L. RECK, Primary Examiner.
R. O. DEAN, Assistant Examiner.
Claims (1)
1. THE METHOD OF FORMING A TANTALUM CARBIDE ON TANTALUM METAL COMPRISING HEATING THE TANTALUM METAL IN CONTACT WITH LAMPBLACK IN AN ATMOSPHERE OF HYDROGEN AT A TEMPERATURE BETWEEN 800 AND 1160*C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US315413A US3266948A (en) | 1963-10-10 | 1963-10-10 | Carbide deposition on tantalum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US315413A US3266948A (en) | 1963-10-10 | 1963-10-10 | Carbide deposition on tantalum |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3266948A true US3266948A (en) | 1966-08-16 |
Family
ID=23224309
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US315413A Expired - Lifetime US3266948A (en) | 1963-10-10 | 1963-10-10 | Carbide deposition on tantalum |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US3266948A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3362842A (en) * | 1963-10-31 | 1968-01-09 | Navy Usa | Method of providing refractory metals with protective coatings and resulting article |
| US3411959A (en) * | 1966-03-21 | 1968-11-19 | Westinghouse Electric Corp | Method for producing tantalum carbide and tantalum-alloy carbide filaments |
| US3964981A (en) * | 1972-04-14 | 1976-06-22 | Iowa State University Research Foundation, Inc. | Method for polarographic analysis using an electrode of tantalum/carbon material |
| US5383981A (en) * | 1993-06-14 | 1995-01-24 | The United States Of America As Represented By The United States Department Of Energy | Reusable crucible for containing corrosive liquids |
| US5580397A (en) * | 1995-01-26 | 1996-12-03 | The United States Of America As Represented By The Department Of Energy | Carbide and carbonitride surface treatment method for refractory metals |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2181094A (en) * | 1937-05-19 | 1939-11-21 | Nesaloy Products Inc | Metallurgical process |
| US2720474A (en) * | 1952-09-13 | 1955-10-11 | Raytheon Mfg Co | Coated electrodes for electron discharge devices |
| US2778757A (en) * | 1953-08-28 | 1957-01-22 | Firth Sterling Inc | Carburized tungsten alloy article |
| US2832710A (en) * | 1956-03-01 | 1958-04-29 | Heraeus Gmbh W C | Method for carburizing spinning nozzles composed of tantalum and alloys thereof |
| US2962388A (en) * | 1954-03-12 | 1960-11-29 | Metallgesellschaft Ag | Process for the production of titanium carbide coatings |
-
1963
- 1963-10-10 US US315413A patent/US3266948A/en not_active Expired - Lifetime
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2181094A (en) * | 1937-05-19 | 1939-11-21 | Nesaloy Products Inc | Metallurgical process |
| US2720474A (en) * | 1952-09-13 | 1955-10-11 | Raytheon Mfg Co | Coated electrodes for electron discharge devices |
| US2778757A (en) * | 1953-08-28 | 1957-01-22 | Firth Sterling Inc | Carburized tungsten alloy article |
| US2962388A (en) * | 1954-03-12 | 1960-11-29 | Metallgesellschaft Ag | Process for the production of titanium carbide coatings |
| US2832710A (en) * | 1956-03-01 | 1958-04-29 | Heraeus Gmbh W C | Method for carburizing spinning nozzles composed of tantalum and alloys thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3362842A (en) * | 1963-10-31 | 1968-01-09 | Navy Usa | Method of providing refractory metals with protective coatings and resulting article |
| US3411959A (en) * | 1966-03-21 | 1968-11-19 | Westinghouse Electric Corp | Method for producing tantalum carbide and tantalum-alloy carbide filaments |
| US3964981A (en) * | 1972-04-14 | 1976-06-22 | Iowa State University Research Foundation, Inc. | Method for polarographic analysis using an electrode of tantalum/carbon material |
| US5383981A (en) * | 1993-06-14 | 1995-01-24 | The United States Of America As Represented By The United States Department Of Energy | Reusable crucible for containing corrosive liquids |
| US5580397A (en) * | 1995-01-26 | 1996-12-03 | The United States Of America As Represented By The Department Of Energy | Carbide and carbonitride surface treatment method for refractory metals |
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