US2750271A - Process of making pulverulent metallic titanium - Google Patents
Process of making pulverulent metallic titanium Download PDFInfo
- Publication number
- US2750271A US2750271A US342286A US34228653A US2750271A US 2750271 A US2750271 A US 2750271A US 342286 A US342286 A US 342286A US 34228653 A US34228653 A US 34228653A US 2750271 A US2750271 A US 2750271A
- Authority
- US
- United States
- Prior art keywords
- titanium
- aluminum
- solution
- alloy
- powder
- 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
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims description 25
- 239000010936 titanium Substances 0.000 title claims description 20
- 229910052719 titanium Inorganic materials 0.000 title claims description 20
- 238000000034 method Methods 0.000 title claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 17
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 17
- 229910045601 alloy Inorganic materials 0.000 claims description 11
- 239000000956 alloy Substances 0.000 claims description 11
- 239000012670 alkaline solution Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 21
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 10
- 229910000838 Al alloy Inorganic materials 0.000 description 8
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 8
- 239000001301 oxygen Substances 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000001117 sulphuric acid Substances 0.000 description 3
- 235000011149 sulphuric acid Nutrition 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- -1 for example Substances 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1236—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching
- C22B34/1254—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching using basic solutions or liquors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1295—Refining, melting, remelting, working up of titanium
Definitions
- This invention relates to a process of making pulverulent metallic titanium from titanium-aluminum alloys.
- titanium-aluminum alloys for example by alumino-thermic reduction of titanium oxide, the aluminum being employed, for instance, in the form of shot.
- lime which forms with the nascent alumina a calcium aluminate slag protecting the metal during the reaction and the cooling.
- pulverulent metallic titanium is made by treating titanium-aluminum alloy, made by any desired process, with a reagent which attacks the aluminum but does not substantially attack the titanium.
- the reagent is an aqueous alkaline solution, a particularly suitable solution being an aqueous soda solution.
- Such solution attacks the aluminum, giving a sodium aluminate solution, but leaves the titanium substantially unaltered.
- a soda solution we may use a solution of sodium hydroxide, potassium carbonate or potassium hydroxide.
- the titanium-aluminum alloys which give the best results are those containing about 40 to 65% of titanium and about 60 to 35% of aluminum. However, compositions outside of these ranges can be employed but produce less desirable results. In any case, the composition of the alloy should be such that when treated with a reagent which attacks the aluminum it does not substantially attack the titanium.
- titanium-aluminum alloy it is particularly desirable to subject the titanium-aluminum alloy to a violent cooling from its molten condition as produced. This may be done, for example, by applying an abundant supply of water to it or by quenching it in water. Such violent cooling produces a structure in the solidified alloy which makes it easier to dissolve the aluminum from the alloy by means of an alkaline solution without substantially attacking the titanium. In addition, the violent cooling causes the solidified alloy to become brittle, which promotes its pulverization.
- the strength of the aqueous alkaline solution employed is not of great importance in the results obtained. However, other conditions being equal, the higher the concentration of the alkaline solution, the more rapid is the attack of the solution on the aluminum of the alloy.
- the process can be carried out in the following manner.
- a titanium-aluminum alloy is crushed, ground, and passed through a sieve of 1296 meshes per square centimeter. It can be passed through a sieve of 117 or 324 meshes per square centimeter, but the duration of the attack by the alkaline solution is considerably longer in such case.
- the shifted alloy is treated with an aqueous solution of soda at the boiling point of the solution (a little above 100 C.).
- the duration of the treatment until almost complete elimination of aluminum is accomplished varies according to the grain size of the powder and the concentration of the soda solution. For an alloy passed through a sieve of 829 meshes per square centimeter, for example, this time is about 8 hours for a soda solution nited States atent ii 2,750,271 Patented June 12, 1956 having a concentration of 6% by weight, and about 2 hours for a soda solution having a concentration of 10%.
- the titanium powder is filtered from the solution.
- the titanium powder usually contains a small amount of aluminum and an amount of oxygen, rather variable, usually within the range of 1 to 5%.
- This oxygen is in a hydrous form of titanium oxide, believed to be fixed on the surface of the titanium particles.
- Such oxide can be largely removed, according to the invention, by washing the titanium powder with a dilute acid, for example, hydrochloric acid, sulphuric acid, nitric acid, hydrofluoric acid, or a mixture thereof, at an acid concentration of a few hundredths per cent by weight.
- a dilute acid for example, hydrochloric acid, sulphuric acid, nitric acid, hydrofluoric acid, or a mixture thereof.
- Example 1 Titanium-aluminum alloy containing:
- the titanium powder after separating it from the solution, was deoxidized by washing it for 5 minutes in a sulphuric acid solution at a concentration of 5 by weight or in a mixture of equal parts of sulphuric acid having a concentration of 10% and hydrofluoric acid having a concentration of 1%. In each case the powder was washed with water after the acid washing. The proportion of oxygen was lowered in this manner to about 0.3%.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR304809X | 1952-03-19 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2750271A true US2750271A (en) | 1956-06-12 |
Family
ID=8888823
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US342286A Expired - Lifetime US2750271A (en) | 1952-03-19 | 1953-03-13 | Process of making pulverulent metallic titanium |
Country Status (5)
| Country | Link |
|---|---|
| US (1) | US2750271A (en(2012)) |
| BE (1) | BE517104A (en(2012)) |
| CH (1) | CH304809A (en(2012)) |
| GB (1) | GB733712A (en(2012)) |
| LU (1) | LU31972A1 (en(2012)) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2903350A (en) * | 1957-03-14 | 1959-09-08 | Ici Ltd | Method of manufacturing titanium |
| US2927854A (en) * | 1957-12-31 | 1960-03-08 | Nat Res Corp | Separation of tantalum |
| US2948687A (en) * | 1955-12-13 | 1960-08-09 | Gen Electric | Hydrogenation catalyst |
| US3021562A (en) * | 1957-04-01 | 1962-02-20 | Dow Chemical Co | Production of group iv, subgroup a, metal prills |
| US3091526A (en) * | 1957-01-08 | 1963-05-28 | Union Carbide Corp | High-purity titanium production |
| US3442641A (en) * | 1965-03-04 | 1969-05-06 | Gen Electric | Metallic brazing mixture |
| US4891184A (en) * | 1988-12-23 | 1990-01-02 | Mikkola Donald E | Low density heat resistant intermetallic alloys of the Al3 Ti type |
| US5006054A (en) * | 1988-12-23 | 1991-04-09 | Technology Development Corporation | Low density heat resistant intermetallic alloys of the Al3 Ti type |
| US5368660A (en) * | 1992-10-30 | 1994-11-29 | New Mexico Tech Research Foundation | High temperature TiAl2 -based ternary alloys |
| US5685924A (en) * | 1995-07-24 | 1997-11-11 | Howmet Research Corporation | Creep resistant gamma titanium aluminide |
| CN113894281A (zh) * | 2021-10-12 | 2022-01-07 | 中国科学院福建物质结构研究所 | 一种表面均匀纳米多孔结构的钛铝合金微球及其制备方法和应用 |
| CN115365506A (zh) * | 2021-05-17 | 2022-11-22 | 康永红 | 一种高产能氢化脱氢一体炉钛粉生产技术 |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1067601B (de) * | 1955-07-29 | 1959-10-22 | Vaw Ver Aluminium Werke Ag | Verfahren zur Herstellung einer hochprozentigen eisenfreien Titan-Aluminium-Legierung aus titanhaltigen Rohstoffen |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1628190A (en) * | 1926-05-14 | 1927-05-10 | Raney Murray | Method of producing finely-divided nickel |
| US2299228A (en) * | 1938-01-12 | 1942-10-20 | Radio Patents Corp | Electric condenser |
-
0
- LU LU31972D patent/LU31972A1/xx unknown
- BE BE517104D patent/BE517104A/xx unknown
-
1953
- 1953-02-03 CH CH304809D patent/CH304809A/fr unknown
- 1953-02-26 GB GB5457/53A patent/GB733712A/en not_active Expired
- 1953-03-13 US US342286A patent/US2750271A/en not_active Expired - Lifetime
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1628190A (en) * | 1926-05-14 | 1927-05-10 | Raney Murray | Method of producing finely-divided nickel |
| US2299228A (en) * | 1938-01-12 | 1942-10-20 | Radio Patents Corp | Electric condenser |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2948687A (en) * | 1955-12-13 | 1960-08-09 | Gen Electric | Hydrogenation catalyst |
| US3091526A (en) * | 1957-01-08 | 1963-05-28 | Union Carbide Corp | High-purity titanium production |
| US2903350A (en) * | 1957-03-14 | 1959-09-08 | Ici Ltd | Method of manufacturing titanium |
| US3021562A (en) * | 1957-04-01 | 1962-02-20 | Dow Chemical Co | Production of group iv, subgroup a, metal prills |
| US2927854A (en) * | 1957-12-31 | 1960-03-08 | Nat Res Corp | Separation of tantalum |
| US3442641A (en) * | 1965-03-04 | 1969-05-06 | Gen Electric | Metallic brazing mixture |
| US4891184A (en) * | 1988-12-23 | 1990-01-02 | Mikkola Donald E | Low density heat resistant intermetallic alloys of the Al3 Ti type |
| US5006054A (en) * | 1988-12-23 | 1991-04-09 | Technology Development Corporation | Low density heat resistant intermetallic alloys of the Al3 Ti type |
| US5368660A (en) * | 1992-10-30 | 1994-11-29 | New Mexico Tech Research Foundation | High temperature TiAl2 -based ternary alloys |
| US5685924A (en) * | 1995-07-24 | 1997-11-11 | Howmet Research Corporation | Creep resistant gamma titanium aluminide |
| CN115365506A (zh) * | 2021-05-17 | 2022-11-22 | 康永红 | 一种高产能氢化脱氢一体炉钛粉生产技术 |
| CN113894281A (zh) * | 2021-10-12 | 2022-01-07 | 中国科学院福建物质结构研究所 | 一种表面均匀纳米多孔结构的钛铝合金微球及其制备方法和应用 |
| CN113894281B (zh) * | 2021-10-12 | 2022-10-11 | 中国科学院福建物质结构研究所 | 一种表面均匀纳米多孔结构的钛铝合金微球及其制备方法和应用 |
Also Published As
| Publication number | Publication date |
|---|---|
| GB733712A (en) | 1955-07-20 |
| LU31972A1 (en(2012)) | |
| CH304809A (fr) | 1955-01-31 |
| BE517104A (en(2012)) |
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