US1835024A - Preparation of metal hydrides - Google Patents
Preparation of metal hydrides Download PDFInfo
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- US1835024A US1835024A US409443A US40944329A US1835024A US 1835024 A US1835024 A US 1835024A US 409443 A US409443 A US 409443A US 40944329 A US40944329 A US 40944329A US 1835024 A US1835024 A US 1835024A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
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- a ⁇ solid mass of coherent metal may be entirely converted -of the present invention I over to hydride by forming upon the metal surface metal hydride compounds, effecting thermal decomposition of these compounds with consequent corrosion of the metal surface, again forming surface hydride compounds and repeating the thermal decomposit-ion and forming of fresh hydride until the entire coherent metal body has been converted over tothe hydride.
- the metal surface is first exposed to the action of hydrogen at an elevated temperature, the hydrogen pressure being maintained above the equilibrium pressure of the metal hydride compound ⁇ at the temperature employed, promoting thereby the formation of surface metal hydride compounds.
- the temperature of the metal body is then materially increased, or the hydrogen pressure is reduced below the ,equilibrium pressure, or both factors are varied soas to effect a decomposition of the metal hydride to metal powder, which crumbles ⁇ or falls away from the coherent metal mass thereby exposing fresh metal surfaces of the mass.
- the freshly exposed. metal surface is again subjected to the. action of the hydrogen, preferably at a lower combining temperature, the hydrogen pressures being meanwhile adjusted to be in excess to the equilibrium pressure. of the metal hydride compound at that temperature. This operation is repeated as many times as is requiredto effect the entire con- Version of the coherent metal mass to metal hydride compounds, all as will be more fully hereinafter disclosed.
- Fig. 1 is a schematic diagram of the apparatus employed in the practice of the present invention.
- Fig. 2 is a graphical representation of the apparatus (not shown) such ⁇ as mercurydiffusion pumps, molecular pumps, oil immersion pumps and the like apparatus capable of giving a high vacuo in container 2 of the order of 1.0 micron pressure which is equivalent to a pressure of about .001 m. m.
- Means are provided for prevent-- ing the dispersion of oil, mercury or other deleterious vapors from the mechanical exhaust means to the container 2, such as trap 5, which may be surrounded by a suitable liquid air container, not shown.
- Means comprising a stop cock 6 are also provided for closing ofi' the exhaust appa-v ratus and means comprising a stop cock 7 are provided for introducing hydrogen gas under pressure to the evacuated container from a reservoir, not shown but indicated.
- Pressure reading means 8 are provided for determining the pressure of the hydrogen in the system 3 which in the present illustration comprises a long glass tube extension 9 of the system 3 dipping into a container 10 which is open to the atmosphere and filled with mercury 11, and means comprising stop cock 12 are provided for shutting off this lpressure reading means 8 when so desired.
- Heating means comprising a wire wound resistance furnace or oven 13 provided with temperature measuring means 14 are provided to heat the metal body 1 to the desired temperature.
- a two piece top 15 for enclosing the container 2 within the furnace 13 is also provided.
- the coherent body of metal 1 may be comprised of one of the rare refractory metals uranium, thorium, zirconium, titanium, hafnium and the like, and preferably has been prepared from substantially pure metal powder prepared in accordance with the invention set forth in U. S. Patent 1,704,257 issued March 5, 1929 to J. W. Marden et al., or by any one of the electrolytic methods set forth in my eopending applications Serial No. 275,264, filed May 4, 1928, Serial No. 277,096 led May 11, 192s, serial N0. 309.682 filed October 1, 1928, Serial No. 316,624 filed November 1, 1928, or Serial No. 351,451 filed March 30, 1929 which patent and copending applications' are all assigned to the same assignee as the present invention.
- the substantially pure rare refractory metal powder is then compacted and heattreated to a coherent body in a continuously maintained high vacuo, in accordance with the process set forth in copending application Serial No. 717,940 led June 5, 1924 by J. W. Marden, et al. which application is also assigned to the same assignee as the present invention.
- the sintering process contemplates the heat-treatin of the metal, body in vacuo in two stages; rst, at a relatively low temperature to effect the removal of adsorbed and absorbed gases from the compacted metal powder at a temperature substantially below the combining temperature of the metal powder for the gases, and secondly at a higher temperature approximating the fusionpoint of the compacted metal powder to effect the coalescing and sintering of the degasified metal powder into a coherent metal body, the said two heat treatments being applied thereto in consecutive order without intervening exposure of the meal to deleterious gaseous absorption.
- the forming of metal hydrides from a coherent metal bodT of the rare refractory metals uranium, t orium, zirconium, hafnium and the like, is highly desirable in that the amount of deleterious impurities introduced into the resulting hydride is relatively extremely low. This is believed to be due to the fact that the two stage vacuum heat treating step to coherent form, as by the above identified copending application Serial No. 717,940, more completely eliminates the deleterious adsorbed and absorbed gases of the metal powder prior to sintering than is obtained by the practice of the relatively lower degasification heating stage of the above identified copending application filed herewith.
- Another advantage is in the relatively short period of time required to effect degaslfication or removal of the surface gases of a coherent metal body prior to the preparation of the m'etal hybride. f
- the uranium metal body 1 prepared and sintered as above disclosed in accordance with the inventions of the above identified portion 16 thereof in the manner shown, and
- the container 2 connected to the evacuating system 3 by means of the tapered stopper 4, and the entire system evacuated with stop cocks 7 and 12 closed.
- trap is surrounded by a suitable. liquid air container to preventI the back dispersion of deleterious vapors or gases.
- Container 2 and metal body 1 is then thoroughly baked and freed of surface gases by bringing the' temperature of the enclosing furnace or oven up to' temperatures just below the softening temperature of the container 2.
- the uranium metal body may also be heated to incandescence if desired by high frequency' induction means.
- the temperature of the uranium metal body is then brought up to about 225 C. at which temperature, reaction of the uranium with the hydrogen atmosphere takes place and proceeds as long as the hydrogen pressure exceeds a pressure of about 3 m. m. of mercury, as is shown in Fig. 2 and more fully set forth in copending application filed herewith.
- the absorption or reaction of the uranium with the hydrogen proceeds rapidly until the surface is completely coated and then the rate of combination slows up and eventually the further formation of metal hydride is substantially prevented.
- the metal powder product of the decomposition falls away from the surface of the coherent mass and collects in the bottom of the container 2in the manner shown.
- n alternative method would be to evacuate thc hydrogen from the system when reaction between the uranium metal surface and the hydrogen has ceased, or toreduce the pressure below the equilibrium pressure at the initial combining temperature of 225 C. effecting thereby the dissociation of the uranium hydride compound, or a still higher temperature in combination With the reduced pressures may be employed to obtain substantially the same effect as is obtained in the first illustration of the practice of my invention.
- the method of converting coherent metal bodies into metal hydride compounds which comprises converting the surface of the metal. body to hydride, effecting thermal decomposition of said hydride, and repeating the process until entire conversion of the metal body has been effected.
- the method of converting coherent meta-l bodies into metal hydride compounds which comprises repeatedly heating the metal body in hydrogen to a temperature at which the metal body reacts with the hydrogen to form metal hydride compounds at the surface maintaining the hydrogen at pressures substantially above the dissociation pressure of the formed metal hydride, intermediate each heating decomposing the surface hydride compounds.
- the method of forming metal hydride compounds from coherent metal bodies which comprises repeatedly heating the metal body in hydrogen to a temperature at which the hydride compound is formed, the pressure of the hydrogen being maintained substantially above the equilibrium pressure of the met-al hydride compound at that temperature, eecting intermediate each heating decomposition of the surface metal hydride compounds by thermal decomposition at higher temperatures at gas pressures be- 1535 lowI the equilibrium pressure at the higher temperature of heating.
- the method of forming metal hydride compounds from coherent metal bodies which comprises repeatedly heating the metal body in hydrogen to a temperature at which the hydride compound 1s formed, maintaining the pressure of the ⁇ hydrogen above the equilibrium pressure of the metal hydride compound formed, eiecting intermediate each heatin a decomposition o fthe surface metal hydride compounds by a reduction inf the hydrogen gas pressures sub ⁇ stantially below the dissociation pressure of the metal hydride compound at the tempera# ture to which it is heated.
- Y. The'method of: forming uranium' hy dride from coherent uranium metal which comprises repeatedly heatinfr the uranium metal in an atmosphere of thydrogen to a tem erature at which uranium hydride may be ormed, maintaining during the heating.
- the method of forming uranium hydride from coherent uranium metal which comprises repeatedly heatin the uranium metal in an atmosphere of ydrogen to a tem erature at which uranium hydride may be ormed, maintaining during the heating a hydrogen pressure substantially greater than the dissociation pressure ofthe uranium hydride, effecting intermediate each of the heatings a thermal decomposition of the uranium hydride.
- the method of forming uranium hydride from coherent uran-ium metal which comprises repeatedly heatin the uranium metal in an atmosphere of ydrogen to a temperature at which uranium hydride maybe formed, maintaining during the heating a hydrogen pressure substantially greater than the dissociation pressure of the uranium hydride, effecting intermediate each of the beatings a decomposition of the uranium hydride by substantially reducing the hydrogen gas pressure below the dissociation pressure of the metal hydride at the temperature to which it is heated.
- the method of forming uranium hydride from a coherent metal body which comprises alternately heating the metal in a hydrogen atmosphere to temperatures approximating 225o C. and 350o C. maintaining a gas pressure at the lirst mentioned tempera-ture substantially in excess of 3.() m. m. mercur and at the last mentioned temperature su stantially below about m. m. mercury pressure.
- the method of preparing metal ⁇ hydride compounds which comprises enclosing a coherent body of the met-al in 'a container, evacuating the container, degasifying the metal body and container, introducing an atmosphere of hydrogen in the container, heating the metal body to a temperature at which surface formation of metal hydrides is promoted maintaining at this temperature a pressure of hydrogen in excess of the dissociation pressure of the metal hydride ⁇ be ing formed, further heating the metal body to more elevated temperatures in gas pressure substantially below the dissociation pressure of the metal hydride at the higher temperature, reducing the ⁇ temperature of the metal body to the lower temperature, and repeating the steps until the entire metal body has been converted to hydride.
- the method of preparing uranium metal hydride which comprises enclosing a coherent mass of uranium in a container, evacuating the container, degasifying the metal and container, introducing an atmosphere of hydrogen into the container, and then repeatedly heating the metal body to temperatures at which the metal reacts with the hydrogen atmosphere maintaining a gas pressure substantially in excess to the decomposition pressure of the uranium hydride compound at that temperature and intermediate each of said heating operations effecting dissociation of the metal hydride formed by heating the hydride compound under gas pressure substantially below the equilibrium pressure thereof.
- the method of preparing uranium metal hydride which comprises enclosing a 4coherent body of uranium in4 a container, evacuating the container, degasiying the metal body and container, introducing a hydrogen atmosphere in the container, and then repeatedly heating the uranium first at a temperature of about 225 C. in a hydrogen gas pressure materially in excess of about 3.0
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Description
Dec. 8, 19331. F. H. DRIGGS PREPARATION OF METAL HYDRIDES Filed Nov` 25, 1929 l .200 300 TEMP. "C
0 0 M 0 0 o 0 0 7 w 5 4 3 w m 5 Patented Dec. 8, 1l
SATES FRANK H. DRIGGS, OF BLOOMFIELD, JERSEY, ASSIGNOR TO WESTINGHOUSE LAMP COMPANY; A CORPORATION OF PENNSYLVANIA.
PREPARATION OF METAL H'YDBIDES Application led November 25, 1929. Serial No. 409,443.'
,409,442 filed November 25, 1929, entitled Preparation metal hydrides, which is assigned to the same assignee as the present invention I have disclosed a method of preparing metal hydrides from metal powders, particularly the rare refractory metal pow ders, which form compounds with atmospheric gases which -are irreducible by hydro- The method disclosed therein sets forth a degasiication of the metal powder step preliminary to the formation of the hydride compound. The degasiiication of the metal powder by the method disclosed therein is a slow and tedious process and on any commercial scale materially increases the costs of manufacture. Moreover with the more highly reactive metals, such as uranium and thorium, it. is exceedingly dicult to perform thc step without deleterious contamination of the metal with the residual gases in the evacuated system.
It is one of the objects of this invention to improve. the method of preparing metal hydrides.
It is another object to provide a method of preparing metalhydrides directly from presi ntered. substantially pure gas free coherent metal bodies.
It is another object of this invention to provide a. method. of forming metal hydrides from sintered coherent masses of rare refractorv metals.
4In accordance with the objects of the present invention I have found that a `solid mass of coherent metal may be entirely converted -of the present invention I over to hydride by forming upon the metal surface metal hydride compounds, effecting thermal decomposition of these compounds with consequent corrosion of the metal surface, again forming surface hydride compounds and repeating the thermal decomposit-ion and forming of fresh hydride until the entire coherent metal body has been converted over tothe hydride. In the practice substantially follow the practice of my copending application above identified, in that the metal surface is first exposed to the action of hydrogen at an elevated temperature, the hydrogen pressure being maintained above the equilibrium pressure of the metal hydride compound `at the temperature employed, promoting thereby the formation of surface metal hydride compounds.
The temperature of the metal body is then materially increased, or the hydrogen pressure is reduced below the ,equilibrium pressure, or both factors are varied soas to effect a decomposition of the metal hydride to metal powder, which crumbles `or falls away from the coherent metal mass thereby exposing fresh metal surfaces of the mass. The freshly exposed. metal surface is again subjected to the. action of the hydrogen, preferably at a lower combining temperature, the hydrogen pressures being meanwhile adjusted to be in excess to the equilibrium pressure. of the metal hydride compound at that temperature. This operation is repeated as many times as is requiredto effect the entire con- Version of the coherent metal mass to metal hydride compounds, all as will be more fully hereinafter disclosed.
j Before further disclosing the nature of this invention reference should be had to the accompanying drawings wherein,l
Fig. 1 is a schematic diagram of the apparatus employed in the practice of the present invention, and
Fig. 2 is a graphical representation of the apparatus (not shown) such `as mercurydiffusion pumps, molecular pumps, oil immersion pumps and the like apparatus capable of giving a high vacuo in container 2 of the order of 1.0 micron pressure which is equivalent to a pressure of about .001 m. m.
mercury. Means are provided for prevent-- ing the dispersion of oil, mercury or other deleterious vapors from the mechanical exhaust means to the container 2, such as trap 5, which may be surrounded by a suitable liquid air container, not shown.
Means comprising a stop cock 6 are also provided for closing ofi' the exhaust appa-v ratus and means comprising a stop cock 7 are provided for introducing hydrogen gas under pressure to the evacuated container from a reservoir, not shown but indicated. Pressure reading means 8 are provided for determining the pressure of the hydrogen in the system 3 which in the present illustration comprises a long glass tube extension 9 of the system 3 dipping into a container 10 which is open to the atmosphere and filled with mercury 11, and means comprising stop cock 12 are provided for shutting off this lpressure reading means 8 when so desired.
Heating means comprising a wire wound resistance furnace or oven 13 provided with temperature measuring means 14 are provided to heat the metal body 1 to the desired temperature. A two piece top 15 for enclosing the container 2 within the furnace 13 is also provided.
In accordance with the present invention the coherent body of metal 1 may be comprised of one of the rare refractory metals uranium, thorium, zirconium, titanium, hafnium and the like, and preferably has been prepared from substantially pure metal powder prepared in accordance with the invention set forth in U. S. Patent 1,704,257 issued March 5, 1929 to J. W. Marden et al., or by any one of the electrolytic methods set forth in my eopending applications Serial No. 275,264, filed May 4, 1928, Serial No. 277,096 led May 11, 192s, serial N0. 309.682 filed October 1, 1928, Serial No. 316,624 filed November 1, 1928, or Serial No. 351,451 filed March 30, 1929 which patent and copending applications' are all assigned to the same assignee as the present invention.
The substantially pure rare refractory metal powder is then compacted and heattreated to a coherent body in a continuously maintained high vacuo, in accordance with the process set forth in copending application Serial No. 717,940 led June 5, 1924 by J. W. Marden, et al. which application is also assigned to the same assignee as the present invention.
Briefly the sintering process contemplates the heat-treatin of the metal, body in vacuo in two stages; rst, at a relatively low temperature to effect the removal of adsorbed and absorbed gases from the compacted metal powder at a temperature substantially below the combining temperature of the metal powder for the gases, and secondly at a higher temperature approximating the fusionpoint of the compacted metal powder to effect the coalescing and sintering of the degasified metal powder into a coherent metal body, the said two heat treatments being applied thereto in consecutive order without intervening exposure of the meal to deleterious gaseous absorption.
By this method of sintering the metal powders of the more highly reactive rare refractory metals into a coherent metal body a metal mass is obtained which is substantially free of deleterious impurities of oxides, nitrides, hydrides and the like compounds.
The forming of metal hydrides from a coherent metal bodT of the rare refractory metals uranium, t orium, zirconium, hafnium and the like, is highly desirable in that the amount of deleterious impurities introduced into the resulting hydride is relatively extremely low. This is believed to be due to the fact that the two stage vacuum heat treating step to coherent form, as by the above identified copending application Serial No. 717,940, more completely eliminates the deleterious adsorbed and absorbed gases of the metal powder prior to sintering than is obtained by the practice of the relatively lower degasification heating stage of the above identified copending application filed herewith.
Another advantage is in the relatively short period of time required to effect degaslfication or removal of the surface gases of a coherent metal body prior to the preparation of the m'etal hybride. f
In the practice of the present invention and as a specific `embodiment thereof I will disclose the method I employ in the forming of uranium hydride from a coherent body of uranium.
The uranium metal body 1 prepared and sintered as above disclosed in accordance with the inventions of the above identified portion 16 thereof in the manner shown, and
.the container 2 connected to the evacuating system 3 by means of the tapered stopper 4, and the entire system evacuated with stop cocks 7 and 12 closed. When a relatively high vacuo has been obtained by mechanical exhaust means, trap is surrounded by a suitable. liquid air container to preventI the back dispersion of deleterious vapors or gases. Container 2 and metal body 1 is then thoroughly baked and freed of surface gases by bringing the' temperature of the enclosing furnace or oven up to' temperatures just below the softening temperature of the container 2. The uranium metal body may also be heated to incandescence if desired by high frequency' induction means.
When a pressure of about 1.0 micron.. (.001 m. 1n. mercury) has been obtained in .the system the evacuating system is closed by means of stop cock 6, the uranium metal button allowed to cool to about room temperature and the system then filled with pure dry hydrogen from the hydrogen reservoir (not shown but indicated)` by opening stop cock 7, and the pressure of the gas adjusted to about 150 m. m. as determined by means of the pressure reading device 8.
The temperature of the uranium metal body is then brought up to about 225 C. at which temperature, reaction of the uranium with the hydrogen atmosphere takes place and proceeds as long as the hydrogen pressure exceeds a pressure of about 3 m. m. of mercury, as is shown in Fig. 2 and more fully set forth in copending application filed herewith. The absorption or reaction of the uranium with the hydrogen proceeds rapidly until the surface is completely coated and then the rate of combination slows up and eventually the further formation of metal hydride is substantially prevented.-
By the next step of my invention I raise the temperature of the metal body to about 350 to 400o C. at which temperature the equilibrium pressure for hydrogen and uranium hydride is between Labout 80 and 320 m. m. mercury and effect thereby a decomposition or dissociation of the uranium hydride compound formed in the first step, the metal powder product of the decomposition falls away from the surface of the coherent mass and collects in the bottom of the container 2in the manner shown. I then reduce the temperature of the container 2 to about 225 (l again, form more hydride upon the uranium metal body and repeat the decomposition of the hydride by again increasing the temperature to 350 to 400 C. This is repeated as many times as is required to entirely convert the uranium body over to the hydride compound which is eventually collected as a loose powder in the bottom of the container 2.
From the weight of the uranium metal body 1 the approximate amount of hydrogen required to effect entire conversion may be readily calculated, and the capacity of the system 3 adjusted by means of suitable res- 05 ervoirs 17 to hold the same, and suitable pre- 'body it is apparent that there may be many cautions must be taken so that the system will safel carry the higher pressures of gases re uired by this method.
n alternative method would be to evacuate thc hydrogen from the system when reaction between the uranium metal surface and the hydrogen has ceased, or toreduce the pressure below the equilibrium pressure at the initial combining temperature of 225 C. effecting thereby the dissociation of the uranium hydride compound, or a still higher temperature in combination With the reduced pressures may be employed to obtain substantially the same effect as is obtained in the first illustration of the practice of my invention.
While I have disclosed herein the specific method I employ in producing uranium hydride from a coherent uranium metal modifications made therein in both the process and apparatus Without substantially departing from the nature of the invention, and that the invention is adaptable to be employed in the manufacture of other metal hydrides'than uranium,.and that such modications, departures and applications thereof are anticipated as may fall within the kscope of the following claims.
What is claimed is:
1. The method of converting coherent metal bodies into metal hydride compounds which comprises converting the surface of the metal. body to hydride, effecting thermal decomposition of said hydride, and repeating the process until entire conversion of the metal body has been effected.
2. The method of converting coherent meta-l bodies into metal hydride compounds which comprises repeatedly heating the metal body in hydrogen to a temperature at which the metal body reacts with the hydrogen to form metal hydride compounds at the surface maintaining the hydrogen at pressures substantially above the dissociation pressure of the formed metal hydride, intermediate each heating decomposing the surface hydride compounds. l
3. The method of forming metal hydride compounds from coherent metal bodies which comprises repeatedly heating the metal body in hydrogen to a temperature at which the hydride compound is formed, the pressure of the hydrogen being maintained substantially above the equilibrium pressure of the met-al hydride compound at that temperature, eecting intermediate each heating decomposition of the surface metal hydride compounds by thermal decomposition at higher temperatures at gas pressures be- 1535 lowI the equilibrium pressure at the higher temperature of heating.
4. The method of forming metal hydride compounds from coherent metal bodies which comprises repeatedly heating the metal body in hydrogen to a temperature at which the hydride compound 1s formed, maintaining the pressure of the `hydrogen above the equilibrium pressure of the metal hydride compound formed, eiecting intermediate each heatin a decomposition o fthe surface metal hydride compounds by a reduction inf the hydrogen gas pressures sub` stantially below the dissociation pressure of the metal hydride compound at the tempera# ture to which it is heated.
Y. The'method of: forming uranium' hy dride from coherent uranium metal which comprises repeatedly heatinfr the uranium metal in an atmosphere of thydrogen to a tem erature at which uranium hydride may be ormed, maintaining during the heating.
a hydrogen pressure substantially greater than the dissociation pressure of the uranium hydride, intermediate each of the heatings decomposing the uranium hydride formed.
6. The method of forming uranium hydride from coherent uranium metal which comprises repeatedly heatin the uranium metal in an atmosphere of ydrogen to a tem erature at which uranium hydride may be ormed, maintaining during the heating a hydrogen pressure substantially greater than the dissociation pressure ofthe uranium hydride, effecting intermediate each of the heatings a thermal decomposition of the uranium hydride.
7. The method of forming uranium hydride from coherent uran-ium metal which comprises repeatedly heatin the uranium metal in an atmosphere of ydrogen to a temperature at which uranium hydride maybe formed, maintaining during the heating a hydrogen pressure substantially greater than the dissociation pressure of the uranium hydride, effecting intermediate each of the beatings a decomposition of the uranium hydride by substantially reducing the hydrogen gas pressure below the dissociation pressure of the metal hydride at the temperature to which it is heated. u
8. The method of forming uranium hydride from a coherent metal body which comprises alternately heating the metal in a hydrogen atmosphere to temperatures approximating 225o C. and 350o C. maintaining a gas pressure at the lirst mentioned tempera-ture substantially in excess of 3.() m. m. mercur and at the last mentioned temperature su stantially below about m. m. mercury pressure.
9. The method of preparing metal `hydride compounds which comprises enclosing a coherent body of the met-al in 'a container, evacuating the container, degasifying the metal body and container, introducing an atmosphere of hydrogen in the container, heating the metal body to a temperature at which surface formation of metal hydrides is promoted maintaining at this temperature a pressure of hydrogen in excess of the dissociation pressure of the metal hydride `be ing formed, further heating the metal body to more elevated temperatures in gas pressure substantially below the dissociation pressure of the metal hydride at the higher temperature, reducing the `temperature of the metal body to the lower temperature, and repeating the steps until the entire metal body has been converted to hydride.
10. The method of preparing uranium metal hydride which comprises enclosing'aY coherent mass of uranium in a container,
evacuating the container, degasifying the metal and container, introducing. an atmosphere ofhydrogen into the container, and then repeatedly heating the metal body to temperatures at which the metal reacts with composition pressure of the uranium hydride` compound at that temperature and intermediate each of said heating operations effecting thermal decomposition of the metal hydride formed.
12. The method of preparing uranium metal hydride which comprises enclosing a coherent mass of uranium in a container, evacuating the container, degasifying the metal and container, introducing an atmosphere of hydrogen into the container, and then repeatedly heating the metal body to temperatures at which the metal reacts with the hydrogen atmosphere maintaining a gas pressure substantially in excess to the decomposition pressure of the uranium hydride compound at that temperature and intermediate each of said heating operations effecting dissociation of the metal hydride formed by heating the hydride compound under gas pressure substantially below the equilibrium pressure thereof.
13. The method of preparing uranium metal hydride which comprises enclosing a 4coherent body of uranium in4 a container, evacuating the container, degasiying the metal body and container, introducing a hydrogen atmosphere in the container, and then repeatedly heating the uranium first at a temperature of about 225 C. in a hydrogen gas pressure materially in excess of about 3.0
m. m. mercury and then to a, temperature of about 350 in a hydrogen gas pressure materially less than about 80 m. m. of mercury until the mass of uranium metal has been en- 5 tirely converted to hydrde.
In testimony whereof, I have hereunto subscribed my name this 22nd day of November, 1929.
FRANK H. DRIGGS.
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| US409443A US1835024A (en) | 1929-11-25 | 1929-11-25 | Preparation of metal hydrides |
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| US409443A US1835024A (en) | 1929-11-25 | 1929-11-25 | Preparation of metal hydrides |
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Cited By (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2446780A (en) * | 1944-07-22 | 1948-08-10 | Atomic Energy Commission | Method of preparing uranium hydride |
| US2452139A (en) * | 1944-07-22 | 1948-10-26 | Amos S Newton | Method of preparing uranium deuteride |
| US2521937A (en) * | 1945-05-18 | 1950-09-12 | Amos S Newton | Method of purifying inert gases |
| US2534676A (en) * | 1945-02-16 | 1950-12-19 | Amos S Newton | Preparation of compounds of uranium and nonmetals |
| US2534677A (en) * | 1945-02-17 | 1950-12-19 | Amos S Newton | Production of uranium halides |
| US2536616A (en) * | 1945-05-22 | 1951-01-02 | James C Warf | Preparation of uranium hydride |
| US2544277A (en) * | 1945-06-12 | 1951-03-06 | Amos S Newton | Preparation of uranium nitride |
| US2558377A (en) * | 1944-11-13 | 1951-06-26 | Morris L Perlman | Preparation of compacts of highdensity uranium hydride |
| US2588153A (en) * | 1947-03-04 | 1952-03-04 | Atomic Energy Commission | Method of making metal hydride |
| US2635956A (en) * | 1950-01-27 | 1953-04-21 | Harley A Wilhelm | Preparation of powdered thorium |
| US2678870A (en) * | 1950-06-21 | 1954-05-18 | Walter M Weil | Manufacture of refractory metal borides |
| US2778725A (en) * | 1952-07-18 | 1957-01-22 | Union Carbide & Carbon Corp | Method for making powdered vanadium metal |
| US2784054A (en) * | 1944-12-05 | 1957-03-05 | James H Carter | Separation of uranium from other metals by hydriding and extraction with oxidizing reagents |
| US2851338A (en) * | 1944-05-01 | 1958-09-09 | Iral B Johns | Method for testing coatings |
| DE1039499B (en) * | 1955-10-20 | 1958-09-25 | Bayer Ag | Process for cleaning alkaline earth hydrides |
| DE1059414B (en) * | 1956-01-12 | 1959-06-18 | Bayer Ag | Process for cleaning alkaline earth hydrides |
| US2905547A (en) * | 1955-03-28 | 1959-09-22 | Titanium Metals Corp | Dehydrogenating titanium metal powder |
| US2915362A (en) * | 1946-08-16 | 1959-12-01 | Fried Sherman | Plutonium-hydrogen reaction product, method of preparing same and plutonium powder therefrom |
| US3152868A (en) * | 1961-03-09 | 1964-10-13 | Charles P Kempter | Preparation of scandium hydrides |
| US3461040A (en) * | 1966-03-29 | 1969-08-12 | Lepetit Spa | Apparatus for automatic reduced pressure semi-micro distillation of liquid decomposing at boiling point under atmospheric pressure |
| US4296074A (en) * | 1978-04-10 | 1981-10-20 | Rockwell International Corporation | Method of decladding |
| WO2017081160A1 (en) | 2015-11-10 | 2017-05-18 | Stichting Energieonderzoek Centrum Nederland | Additive manufacturing of metal objects |
| WO2018208155A1 (en) | 2017-05-10 | 2018-11-15 | Admatec Europe B.V. | Additive manufacturing of metal objects |
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1929
- 1929-11-25 US US409443A patent/US1835024A/en not_active Expired - Lifetime
Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2851338A (en) * | 1944-05-01 | 1958-09-09 | Iral B Johns | Method for testing coatings |
| US2452139A (en) * | 1944-07-22 | 1948-10-26 | Amos S Newton | Method of preparing uranium deuteride |
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| WO2017081160A1 (en) | 2015-11-10 | 2017-05-18 | Stichting Energieonderzoek Centrum Nederland | Additive manufacturing of metal objects |
| WO2018208155A1 (en) | 2017-05-10 | 2018-11-15 | Admatec Europe B.V. | Additive manufacturing of metal objects |
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