CN112247139A - Method for reducing oxygen content of fine titanium powder - Google Patents
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- CN112247139A CN112247139A CN202011022841.4A CN202011022841A CN112247139A CN 112247139 A CN112247139 A CN 112247139A CN 202011022841 A CN202011022841 A CN 202011022841A CN 112247139 A CN112247139 A CN 112247139A
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 239000001301 oxygen Substances 0.000 title claims abstract description 76
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 76
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 42
- 239000000843 powder Substances 0.000 claims abstract description 53
- 239000002245 particle Substances 0.000 claims abstract description 34
- 238000002156 mixing Methods 0.000 claims abstract description 32
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011575 calcium Substances 0.000 claims abstract description 27
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 27
- 238000005406 washing Methods 0.000 claims abstract description 27
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 17
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000292 calcium oxide Substances 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 239000011812 mixed powder Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 229910052786 argon Inorganic materials 0.000 claims description 14
- 239000012300 argon atmosphere Substances 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 239000003638 chemical reducing agent Substances 0.000 abstract description 6
- 238000011946 reduction process Methods 0.000 abstract description 3
- 239000007769 metal material Substances 0.000 abstract description 2
- 239000010935 stainless steel Substances 0.000 description 20
- 229910001220 stainless steel Inorganic materials 0.000 description 20
- 238000010438 heat treatment Methods 0.000 description 10
- 239000000203 mixture Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000001291 vacuum drying Methods 0.000 description 8
- 229910001069 Ti alloy Inorganic materials 0.000 description 7
- 239000010936 titanium Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 238000005054 agglomeration Methods 0.000 description 5
- 230000002776 aggregation Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000004663 powder metallurgy Methods 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006392 deoxygenation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
Images
Classifications
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- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention belongs to the technical field of fine treatment of rare metal materials, and particularly relates to a method for reducing the oxygen content of fine titanium powder, which comprises the following steps: (1) uniformly mixing fine titanium powder and calcium oxide powder; (2) uniformly mixing the mixed powder obtained in the step (1) with calcium particles, and then reacting at a high temperature for 0.5-4 h; (3) and (3) after cooling, washing the product obtained in the step (2) with dilute acid, then washing with water, and drying to obtain the low-oxygen fine titanium powder. Aiming at the problems that fine titanium powder is easy to agglomerate and even sinter into blocks in the calcium oxygen reduction process, the using amount of reducing agent calcium is high and the like, the invention provides a method for reducing the oxygen content of the fine titanium powder.
Description
Technical Field
The invention belongs to the technical field of fine treatment of rare metal materials, and particularly relates to a method for reducing the oxygen content of fine titanium powder.
Background
Titanium and titanium alloy have the advantages of high specific strength, corrosion resistance, good biocompatibility and the like, and become important materials in the fields of aerospace, chemical engineering, biomedical treatment and the like. Generally, the production of titanium alloy products includes the steps of casting an alloy ingot, forging and rolling, and part fabrication. However, titanium alloys have poor machinability and high machining costs, which makes titanium alloy products expensive. As a near net shape forming technique, powder metallurgy can reduce or even eliminate machining, with obvious advantages. In addition, the titanium and the titanium alloy prepared by the powder metallurgy method can obtain fine and uniform crystal grains, and can reduce component segregation and improve component uniformity. However, titanium has a relatively high oxygen solubility and a relatively large specific surface area of the titanium powder, which results in a titanium powder metallurgy product having a relatively high oxygen concentration due to the oxygen concentration in the titanium powder. Oxygen in titanium has a great adverse effect on the physical, mechanical and electrical properties of titanium products. For example, high oxygen concentrations in the electronics industry can reduce the conductive properties of titanium sputtered films. Therefore, reducing the oxygen content in the titanium powder is of great importance for improving the performance of the titanium powder metallurgical product.
Calcium is often used as a deoxidizer for titanium powder due to its extremely strong oxygen affinity and high vapor pressure. Fisher et al use liquid sodium as a carrier to perform oxygen reduction (DOSS) on titanium and titanium alloy powder by using liquid calcium at high temperature, and the added sodium carrier can make calcium deoxidizer uniformly contact with metal powder (U.S. Pat. No. 4,983), but the titanium powder reduced in oxygen by the method usually agglomerates and even sinters into blocks. J.M.Oh and the like directly mix titanium powder and calcium according to the mass ratio of 2:1, and carry out oxygen reduction below the melting point of calcium, so that the problem of oxygen reduction and agglomeration of coarse titanium powder is successfully solved, the oxygen concentration of the titanium powder with the particle size of 115 mu m can be reduced to 1080ppm at 830 ℃, but the oxygen reduction temperature is low, the titanium powder with the oxygen concentration lower than 1000ppm is difficult to obtain, and the agglomeration problem of fine titanium powder still exists (Mater. Trans. 2012, 53: 1075-doped 1077). J.M. Oh et al also propose a calcium non-contact oxygen reduction method, i.e. under high vacuum environment, the mass ratio is 1: 1 and reducing agent calcium, and reducing oxygen above the melting point of calcium, wherein the oxygen concentration of the titanium Powder with the diameter of 115 mu m can be reduced to 820ppm by the method, but the method consumes more reducing agent calcium and is not beneficial to large-scale production (Powder technology. 2012, 55: 402-) -404). In addition, when the non-contact oxygen reduction is carried out on the fine titanium powder, particularly the titanium powder with the particle size less than 45 mu m, obvious agglomeration and even agglomeration can occur between the titanium powder, so that the leaching and the removal of the by-products are difficult.
Disclosure of Invention
In order to solve the problems that fine titanium powder is easy to agglomerate and even sinter into blocks in the calcium oxygen reduction process, the using amount of reducing agent calcium is high and the like, the invention provides a method for reducing the oxygen content of the fine titanium powder.
The invention is realized by adopting the following technical scheme:
a method for reducing the oxygen content of fine titanium powder comprises the following steps:
(1) uniformly mixing fine titanium powder and calcium oxide powder (the mass ratio of the fine titanium powder to the calcium oxide powder is 2-6: 1);
(2) uniformly mixing the mixed powder obtained in the step (1) with calcium particles (the mass ratio of the mixed powder to the calcium particles is 6-10: 1), and then reacting at high temperature (raising the temperature to 850-1200 ℃ in vacuum or protective atmosphere) for 0.5-4 h;
(3) and (3) after cooling, washing the product obtained in the step (2) with dilute acid, then washing with pure water, and drying to obtain the low-oxygen fine titanium powder.
According to the method for reducing the oxygen content of the fine titanium powder, the calcium oxide powder in the step (1) has the purity of 99-99.99% and the particle size of 0.1-30 mu m; the mixing is carried out in a mixer for 1-20 h, and the mixing process is carried out in an argon atmosphere.
According to the method for reducing the oxygen content of the fine titanium powder, the purity of the calcium particles in the step (2) is 99-99.99%, and the particle size is 1-10 mm; the protective atmosphere is hydrogen or argon or a mixed gas of hydrogen and argon.
According to the method for reducing the oxygen content of the fine titanium powder, the dilute acid in the step (3) is hydrochloric acid, nitric acid or sulfuric acid.
The invention has the following positive and beneficial effects:
the invention is suitable for oxygen reduction, the fine titanium powder with the granularity less than 50 mu m is used, the surface fine powder is not required to be treated in advance, the calcium oxide powder is added to prevent the fine titanium powder from directly contacting with each other so as to avoid agglomeration and even sintering of the fine titanium powder in the high-temperature oxygen reduction process, the direct contact oxygen reduction of the reducing agent calcium and the titanium powder is realized, the consumption of the reducing agent is less, the production cost is low, and the invention is suitable for large-scale production.
Drawings
FIG. 1 is an SEM morphology of titanium powder after oxygen reduction washing in example 1, in which the titanium powder is not agglomerated and is well dispersed;
FIG. 2 is a graph showing the oxygen content of titanium powder after oxygen reduction washing in example 1, the oxygen content of the titanium powder being 830 ppm;
FIG. 3 is an SEM morphology of titanium powder after deoxygenation and before washing in example 5, in which the titanium powder is not agglomerated and is well dispersed;
FIG. 4 is a diagram showing the state of the titanium powder after the high-temperature treatment in comparative example 1, in which the titanium powder after the high-temperature treatment is seriously agglomerated;
FIG. 5 is an SEM image of titanium powder before washing after oxygen reduction in comparative example 3, in which the titanium powder is sintered;
FIG. 6 is an SEM image of titanium powder before washing after oxygen reduction in comparative example 5, in which the titanium powder is slightly agglomerated.
Detailed Description
The technical solution of the present invention is further described in detail with reference to the following examples, but the scope of the present invention is not limited thereto.
Example 1
A method for reducing the oxygen content of fine titanium powder specifically comprises the following steps:
(1) uniformly mixing titanium powder with oxygen content of 5500ppm and particle size of 10 mu m and calcium oxide powder with purity of 99.99% and particle size of 1 mu m in a mixer according to the mass ratio of 4:1, wherein the mixing time is 16h, and the mixing process is carried out in argon atmosphere;
(2) uniformly mixing the mixed powder obtained in the step (1) with calcium particles with the purity of 99.9% and the particle size of 5mm according to the mass ratio of 7:1, then placing the mixture into a stainless steel crucible, then placing the stainless steel crucible into a high-temperature furnace, heating to 1000 ℃ at the speed of 10 ℃/min under the protection of argon, reacting for 2 hours, and cooling to room temperature along with the furnace;
(3) and (3) taking out the powder obtained in the step (2), washing the powder with 10% hydrochloric acid, washing the powder with pure water, then placing the powder in a vacuum drying oven for drying to obtain low-oxygen fine titanium powder, carrying out SEM observation, as shown in figure 1, and carrying out oxygen content measurement by using an NCS-3000 oxygen-nitrogen-hydrogen tester, as shown in figure 2.
Example 2
A method for reducing the oxygen content of fine titanium powder specifically comprises the following steps:
(1) uniformly mixing 4500ppm of titanium powder with the granularity of 15 mu m and calcium oxide powder with the purity of 99.9% and the granularity of 5 mu m in a mixer according to the mass ratio of 3:1, wherein the mixing time is 8 hours, and the mixing process is carried out in an argon atmosphere;
(2) uniformly mixing the mixed powder obtained in the step (1) with calcium particles with the purity of 99.9% and the particle size of 5mm according to the mass ratio of 9:1, then placing the mixture into a stainless steel crucible, then placing the stainless steel crucible into a high-temperature furnace, heating to 1000 ℃ at the speed of 5 ℃/min under the protection of argon, reacting for 3 hours, and then cooling to room temperature along with the furnace;
(3) and (3) taking out the powder obtained in the step (2), washing the powder with 10% hydrochloric acid, washing the powder with pure water, and then drying the powder in a vacuum drying oven to obtain the low-oxygen fine titanium powder.
Example 3
A method for reducing the oxygen content of fine titanium powder specifically comprises the following steps:
(1) uniformly mixing titanium powder with the oxygen content of 4000ppm and the granularity of 20 mu m and calcium oxide powder with the purity of 99.99 percent and the granularity of 8 mu m in a mixer according to the mass ratio of 5:1 for 10 hours, wherein the mixing process is carried out in an argon atmosphere;
(2) uniformly mixing the mixed powder obtained in the step (1) with calcium particles with the purity of 99.9% and the particle size of 3mm according to the mass ratio of 6:1, then placing the mixture into a stainless steel crucible, then placing the stainless steel crucible into a high-temperature furnace, heating to 1050 ℃ at the speed of 5 ℃/min under the protection of argon, reacting for 1h, and cooling to room temperature along with the furnace;
(3) and (3) taking out the powder obtained in the step (2), washing the powder with 10% hydrochloric acid, washing the powder with pure water, and then drying the powder in a vacuum drying oven to obtain the low-oxygen fine titanium powder.
Example 4
A method for reducing the oxygen content of fine titanium powder specifically comprises the following steps:
(1) uniformly mixing 4800ppm of titanium powder with the granularity of 10 mu m and calcium oxide powder with the purity of 99.9% and the granularity of 5 mu m in a mixer according to the mass ratio of 4:1 for 10 hours, wherein the mixing process is carried out in an argon atmosphere;
(2) uniformly mixing the mixed powder obtained in the step (1) with calcium particles with the purity of 99.9% and the particle size of 6mm according to the mass ratio of 7:1, then placing the mixture into a stainless steel crucible, then placing the stainless steel crucible into a high-temperature furnace, heating to 960 ℃ at the speed of 6 ℃/min under the protection of argon, reacting for 4 hours, and cooling to room temperature along with the furnace;
(3) and (3) taking out the powder obtained in the step (2), washing the powder with 10% hydrochloric acid, washing the powder with pure water, and then drying the powder in a vacuum drying oven to obtain the low-oxygen fine titanium powder.
Example 5
A method for reducing the oxygen content of fine titanium powder specifically comprises the following steps:
(1) uniformly mixing 6500ppm of titanium powder with the granularity of 8 mu m and calcium oxide powder with the purity of 99.9 percent and the granularity of 2 mu m in a mixer according to the mass ratio of 3:1 for 12 hours, wherein the mixing process is carried out in an argon atmosphere;
(2) uniformly mixing the mixed powder obtained in the step (1) with calcium particles with the purity of 99.9% and the particle size of 5mm according to the mass ratio of 6:1, then placing the mixture into a stainless steel crucible, then placing the stainless steel crucible into a high-temperature furnace, heating to 950 ℃ at the speed of 5 ℃/min under the protection of argon, reacting for 3 hours, and then cooling to room temperature along with the furnace;
(3) and (3) taking out the powder obtained in the step (2), washing the powder with 10% hydrochloric acid, washing the powder with pure water, and then drying the powder in a vacuum drying oven to obtain the low-oxygen fine titanium powder.
Comparative example 1
A method for reducing the oxygen content of fine titanium powder specifically comprises the following steps:
(1) placing titanium powder with oxygen content of 5500ppm and particle size of 10 μm in a stainless steel crucible, then placing the stainless steel crucible in a high temperature furnace, heating to 1000 ℃ at a speed of 5 ℃/min under the protection of argon, preserving heat for 2h, and cooling to room temperature along with the furnace;
(2) taking out the powder obtained in the step (1).
Comparative example 2
A method for reducing the oxygen content of fine titanium powder specifically comprises the following steps:
(1) uniformly mixing titanium powder with oxygen content of 5500ppm and particle size of 10 mu m and calcium oxide powder with purity of 99.9% and particle size of 2 mu m in a mixer according to the mass ratio of 6:1 for 12 hours;
(2) placing the mixed powder obtained in the step (1) in a stainless steel crucible, then placing the stainless steel crucible in a high-temperature furnace, heating to 1000 ℃ at the speed of 5 ℃/min under the protection of argon, preserving heat for 2h, and then cooling to room temperature along with the furnace;
(3) and (3) taking out the powder obtained in the step (2).
Comparative example 3
A method for reducing the oxygen content of fine titanium powder specifically comprises the following steps:
(1) uniformly mixing titanium powder with oxygen content of 5500ppm and particle size of 10 mu m and calcium particles with purity of 99.9% and particle size of 5mm according to a mass ratio of 5:1, placing the mixture in a stainless steel crucible, then placing the stainless steel crucible in a high-temperature furnace, heating to 1000 ℃ at a speed of 5 ℃/min under the protection of argon, reacting for 2 hours, and cooling to room temperature along with the furnace;
(2) and (2) taking out the powder obtained in the step (1), washing the powder with 10% hydrochloric acid, washing the powder with pure water, and then drying the powder in a vacuum drying oven to obtain the low-oxygen fine titanium powder.
Comparative example 4
A method for reducing the oxygen content of fine titanium powder specifically comprises the following steps:
(1) uniformly mixing titanium powder with oxygen content of 2500ppm and granularity of 115 mu m and calcium particles with purity of 99.9% and granularity of 5mm according to the mass ratio of 6:1, placing the mixture in a stainless steel crucible, then placing the stainless steel crucible in a high-temperature furnace, heating to 1000 ℃ at the speed of 8 ℃/min under the protection of argon, reacting for 2h, and cooling to room temperature along with the furnace;
(2) and (2) taking out the powder obtained in the step (1), washing the powder with 10% hydrochloric acid, washing the powder with pure water, and then drying the powder in a vacuum drying oven to obtain the low-oxygen fine titanium powder.
TABLE 1 Effect of oxygen reduction treatment and caking behavior in the respective embodiments
Comparative example 5
A method for reducing the oxygen content of fine titanium powder specifically comprises the following steps:
(1) uniformly mixing titanium powder with the oxygen content of 4000ppm and the granularity of 10 mu m and calcium oxide powder with the purity of 99.9 percent and the granularity of 2 mu m in a mixer according to the mass ratio of 4:1 for 12 hours;
(2) uniformly mixing the mixed powder obtained in the step (1) with calcium particles with the purity of 99.9% and the particle size of 5mm according to the mass ratio of 4:1, then placing the mixture into a stainless steel crucible, then placing the stainless steel crucible into a high-temperature furnace, heating to 1000 ℃ at the speed of 6 ℃/min under the protection of argon, reacting for 1h, and cooling to room temperature along with the furnace;
(3) and (3) taking out the powder obtained in the step (2), washing the powder with 10% hydrochloric acid, washing the powder with pure water, and then drying the powder in a vacuum drying oven to obtain the low-oxygen fine titanium powder.
Claims (9)
1. A method for reducing the oxygen content of fine titanium powder is characterized by comprising the following steps:
(1) uniformly mixing fine titanium powder and calcium oxide powder;
(2) uniformly mixing the mixed powder obtained in the step (1) with calcium particles, and then reacting at a high temperature for 0.5-4 h;
(3) and (3) after cooling, washing the product obtained in the step (2) with dilute acid, then washing with water, and drying to obtain the low-oxygen fine titanium powder.
2. The method of reducing the oxygen content of fine titanium powder according to claim 1, wherein: the calcium oxide powder in the step (1) has the purity of 99-99.99% and the particle size of 0.1-30 μm.
3. The method of reducing the oxygen content of fine titanium powder according to claim 1, wherein: and (2) mixing in the step (1) is carried out in a mixer for 1-20 h, and the mixing process is carried out in an argon atmosphere.
4. The method of reducing the oxygen content of fine titanium powder according to claim 1, wherein: the mass ratio of the fine titanium powder to the calcium oxide powder used in the step (1) is 2-6: 1.
5. The method of reducing the oxygen content of fine titanium powder according to claim 1, wherein: the purity of the calcium particles in the step (2) is 99-99.99%, and the particle size is 1-10 mm.
6. The method of reducing the oxygen content of fine titanium powder according to claim 1, wherein: the mass ratio of the mixed powder used in the step (2) to the calcium particles is 6-10: 1.
7. The method of reducing the oxygen content of fine titanium powder according to claim 1, wherein: the high-temperature reaction in the step (2) is carried out at 850-1200 ℃ in vacuum or protective atmosphere.
8. The method of reducing the oxygen content of fine titanium powder according to claim 7, wherein: the protective atmosphere is hydrogen or argon or a mixed gas of hydrogen and argon.
9. The method of reducing the oxygen content of fine titanium powder according to claim 1, wherein: the dilute acid in the step (3) is hydrochloric acid, nitric acid or sulfuric acid.
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| JPH11140513A (en) * | 1997-08-26 | 1999-05-25 | Sumitomo Metal Mining Co Ltd | Manufacture of spherical nickel powder |
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| CN111644610A (en) * | 2020-05-13 | 2020-09-11 | 西南科技大学 | Method for reducing oxygen content in titanium powder |
-
2020
- 2020-09-25 CN CN202011022841.4A patent/CN112247139A/en active Pending
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| JPH11140513A (en) * | 1997-08-26 | 1999-05-25 | Sumitomo Metal Mining Co Ltd | Manufacture of spherical nickel powder |
| US20130125706A1 (en) * | 2011-11-18 | 2013-05-23 | Jae-Won Lim | Method for preparing titanium powder with low oxygen concentration |
| US20160074942A1 (en) * | 2014-05-13 | 2016-03-17 | University Of Utah Research Foundation | Production of substantially spherical metal powders |
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Non-Patent Citations (1)
| Title |
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