US2926071A - Preparation of titanium nitride of high purity - Google Patents
Preparation of titanium nitride of high purity Download PDFInfo
- Publication number
- US2926071A US2926071A US667683A US66768357A US2926071A US 2926071 A US2926071 A US 2926071A US 667683 A US667683 A US 667683A US 66768357 A US66768357 A US 66768357A US 2926071 A US2926071 A US 2926071A
- Authority
- US
- United States
- Prior art keywords
- titanium
- titanium nitride
- reaction zone
- high purity
- preparation
- 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
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- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 title description 13
- 238000002360 preparation method Methods 0.000 title description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 12
- 239000010936 titanium Substances 0.000 description 12
- 229910052719 titanium Inorganic materials 0.000 description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 11
- 238000005121 nitriding Methods 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- -1 ma nganese Chemical compound 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 5
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 150000004767 nitrides Chemical class 0.000 description 4
- 229910000048 titanium hydride Inorganic materials 0.000 description 4
- 150000007513 acids Chemical class 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052790 beryllium Inorganic materials 0.000 description 2
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000004845 hydriding Methods 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 150000004681 metal hydrides Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/076—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with titanium or zirconium or hafnium
- C01B21/0768—After-treatment, e.g. grinding, purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/076—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with titanium or zirconium or hafnium
- C01B21/0761—Preparation by direct nitridation of titanium, zirconium or hafnium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Definitions
- This invention relates to the preparation of titanium nitride of high purity from titanium-containing metal scrap, such as scrap of titanium metal or scrap alloys of titanium with aluminum, vanadium, silicon, chromium, molybdenum, tungsten, ma nganese, iron, cobalt, nickel, indium, boron, copper or beryllium.
- the present invention is based upon the discovery that titanium nitride is resistant to the action of strong acids, such as aqua regia, Whereas such acids readily attack the elements present in titanium metal as alloying components or impurities and also readily attack the m trides of such elements.
- substantially pure titanium nitride from such titanium-containing materials by converting the titanium content thereof to nitride and then subjecting the nitrided material to the action of a strong acid, such as aqua regia, to convert the impurities to salts.
- the salts then may be removed in any desired manner such as by leaching the material with water or other suitable solvent.
- Bulky pieces of titanium such as pieces of sheet titanium, cannot be converted completely to titanium nitride by subjecting the pieces to the action of nitrogen or ammonia even at an elevated temperature.
- such pieces of titanium can be converted to hydride by subjecting the pieces to the action of hydrogen at an elevated temperature.
- the resulting hydrided pieces are brittle and can be broken up readily to finely divided form.
- the finely divided titanium hydride then can be converted to nitride by being subjected to the action of nitrogen or ammonia at an elevated temperature.
- a pluralityof pieces of titanium-containing metal scrap are placed in a confined reaction zone and the reaction zone is evacuated to remove air and moisture by subjecting the reaction zone to vacuum while being heated at a temperature between about 100 C. and 200 C.
- Hydrogen then is introduced into the reaction zone to maintain a small positive pressure therein, such as about five pounds per square inch, and the charge is heated to a suitable hydriding temperature, such as between about 900 C. and 1000 C.
- the reaction zone then is cooled and the hydrided pieces removed. The pieces then are broken up and converted to a finely divided form as by crushing.
- the finely divided titanium hydride-containing material I is placed in a confined reaction zone and the reaction zone is evacuated to remove air and moisture as previously described. Nitrogen or ammonia gas then is introduced into the reaction zone to maintain a small positive pressure therein, such as about five pounds per square inch, and the charge is heated to a temperature sutficiently high to start the nitriding reaction. If the nitriding gas used is ammonia, the latter is dissociated to nitrogen and hydrogen gases. Since the nitriding re action is exothermic, the reaction proceeds to completion without additional heating. If ammonia is used as the nitriding gas, the produced hydrogen may be released periodically to maintain the desired pressure in the reaction zone to prevent leakage of air into the reaction zone.
- the rate of introduction of the nitriding gas into the re action zone may be suitably controlled.
- An inert gas such as helium or argon, may be introduced into the reaction zone to maintain the desired pressure therein, this being especially desirable when the nitriding gas used is nitrogen.
- the charge is cooled to about room temperature while maintaining the reaction zone under a slight positive pressure of ammonia, nitrogen or inert gas.
- the impure titanium nitride powder then is removed from the reaction zone and is subjected to the action of, a strong acid, such as aqua regia, to convert the impurities to salts which are subsequently removed by leaching with water or other suitable solvent.
- the method for recovering titanium in the form of high purity titanium nitride from scrap alloy of titanium with a metal selected from the group consisting of aluminum, vanadium, silicon, chromium, molybdenum, tungsten, manganese, iron, cobalt, indium, boron, copper, beryllium and mixtures thereof which comprises subjecting the alloy to a hydriding operation to convert the titanium content of the alloy to titanium hydride, reducing the titanium hydride in the thus treated material to finely divided form,
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Description
United States Patent PREPARATION OF TITANIUM NITRIDE OF HIGH PURITY Peter P. Alexander, Beverly, Mass., assignor to Metal Hydrides Incorporated, Beverly, Mass., a company of Massachusetts No Drawing. Application June 24, 1957 Serial No. 667,683
1 Claim. (Cl. 23-191) This invention relates to the preparation of titanium nitride of high purity from titanium-containing metal scrap, such as scrap of titanium metal or scrap alloys of titanium with aluminum, vanadium, silicon, chromium, molybdenum, tungsten, ma nganese, iron, cobalt, nickel, indium, boron, copper or beryllium. The present invention is based upon the discovery that titanium nitride is resistant to the action of strong acids, such as aqua regia, Whereas such acids readily attack the elements present in titanium metal as alloying components or impurities and also readily attack the m trides of such elements. Consequently, it is possible to prepare substantially pure titanium nitride from such titanium-containing materials by converting the titanium content thereof to nitride and then subjecting the nitrided material to the action of a strong acid, such as aqua regia, to convert the impurities to salts. The salts then may be removed in any desired manner such as by leaching the material with water or other suitable solvent.
Bulky pieces of titanium, such as pieces of sheet titanium, cannot be converted completely to titanium nitride by subjecting the pieces to the action of nitrogen or ammonia even at an elevated temperature. However, such pieces of titanium can be converted to hydride by subjecting the pieces to the action of hydrogen at an elevated temperature. The resulting hydrided pieces are brittle and can be broken up readily to finely divided form. The finely divided titanium hydride then can be converted to nitride by being subjected to the action of nitrogen or ammonia at an elevated temperature.
In accordance with the present preferred practice of the invention a pluralityof pieces of titanium-containing metal scrap are placed in a confined reaction zone and the reaction zone is evacuated to remove air and moisture by subjecting the reaction zone to vacuum while being heated at a temperature between about 100 C. and 200 C. Hydrogen then is introduced into the reaction zone to maintain a small positive pressure therein, such as about five pounds per square inch, and the charge is heated to a suitable hydriding temperature, such as between about 900 C. and 1000 C. The reaction zone then is cooled and the hydrided pieces removed. The pieces then are broken up and converted to a finely divided form as by crushing.
The finely divided titanium hydride-containing material I is placed in a confined reaction zone and the reaction zone is evacuated to remove air and moisture as previously described. Nitrogen or ammonia gas then is introduced into the reaction zone to maintain a small positive pressure therein, such as about five pounds per square inch, and the charge is heated to a temperature sutficiently high to start the nitriding reaction. If the nitriding gas used is ammonia, the latter is dissociated to nitrogen and hydrogen gases. Since the nitriding re action is exothermic, the reaction proceeds to completion without additional heating. If ammonia is used as the nitriding gas, the produced hydrogen may be released periodically to maintain the desired pressure in the reaction zone to prevent leakage of air into the reaction zone. In order to prevent excessive rise in temperature, the rate of introduction of the nitriding gas into the re action zone may be suitably controlled. An inert gas, such as helium or argon, may be introduced into the reaction zone to maintain the desired pressure therein, this being especially desirable when the nitriding gas used is nitrogen. When the nitriding reaction has gone to completion, the charge is cooled to about room temperature while maintaining the reaction zone under a slight positive pressure of ammonia, nitrogen or inert gas. The impure titanium nitride powder then is removed from the reaction zone and is subjected to the action of, a strong acid, such as aqua regia, to convert the impurities to salts which are subsequently removed by leaching with water or other suitable solvent.
In place of aqua regia, other acids may be used for treating the impure titanium nitride to convert the impurities to salts. Thus, when the elements present in the titanium metal as alloying components or impurities are known, a particular acid may be selected for this purpose which is known to react with these elements or their corresponding nitrides to form salts. It is preferable to use for this purpose an acid which forms water soluble salts with the elements or their nitrides which are present in the impure titanium nitride.
I claim:
The method for recovering titanium in the form of high purity titanium nitride from scrap alloy of titanium with a metal selected from the group consisting of aluminum, vanadium, silicon, chromium, molybdenum, tungsten, manganese, iron, cobalt, indium, boron, copper, beryllium and mixtures thereof which comprises subjecting the alloy to a hydriding operation to convert the titanium content of the alloy to titanium hydride, reducing the titanium hydride in the thus treated material to finely divided form,
subjecting the thus reduced material to a nitriding op eration and thereby form a titanium nitride-containing mixture, subjecting said mixture to the action of aqua regia at about room temperature to form a mixture of titanium nitride and a compound of the selected metal, and removing said compound from the titanium nitride.
References Cited in the file of this patent UNITED STATES PATENTS Jacobson Mar. 16, 1952 OTHER REFERENCES
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US667683A US2926071A (en) | 1957-06-24 | 1957-06-24 | Preparation of titanium nitride of high purity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US667683A US2926071A (en) | 1957-06-24 | 1957-06-24 | Preparation of titanium nitride of high purity |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2926071A true US2926071A (en) | 1960-02-23 |
Family
ID=24679203
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US667683A Expired - Lifetime US2926071A (en) | 1957-06-24 | 1957-06-24 | Preparation of titanium nitride of high purity |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US2926071A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3228748A (en) * | 1960-12-31 | 1966-01-11 | Accary Andre | Process for the preparation of a uranium compound in powder form |
| US3427132A (en) * | 1967-04-12 | 1969-02-11 | Nat Res Corp | Tantalum nitride powder and method for its preparation |
| US5579334A (en) * | 1994-03-03 | 1996-11-26 | Baxter; Rodney C. | Method and apparatus for reacting solid particulate reagents in an electric furnace |
| US20100288316A1 (en) * | 2006-02-24 | 2010-11-18 | Bsh Bosch Und Siemens Hausgerate Gmbh | Household Device Having an Improved Shaft |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2672400A (en) * | 1952-06-02 | 1954-03-16 | Nat Lead Co | Preparation of titanium nitride |
-
1957
- 1957-06-24 US US667683A patent/US2926071A/en not_active Expired - Lifetime
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2672400A (en) * | 1952-06-02 | 1954-03-16 | Nat Lead Co | Preparation of titanium nitride |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3228748A (en) * | 1960-12-31 | 1966-01-11 | Accary Andre | Process for the preparation of a uranium compound in powder form |
| US3427132A (en) * | 1967-04-12 | 1969-02-11 | Nat Res Corp | Tantalum nitride powder and method for its preparation |
| US5579334A (en) * | 1994-03-03 | 1996-11-26 | Baxter; Rodney C. | Method and apparatus for reacting solid particulate reagents in an electric furnace |
| US20100288316A1 (en) * | 2006-02-24 | 2010-11-18 | Bsh Bosch Und Siemens Hausgerate Gmbh | Household Device Having an Improved Shaft |
| US9407119B2 (en) * | 2006-02-24 | 2016-08-02 | BSH Hausgeräte GmbH | Household device having an improved shaft |
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