CN105499589A - Method for preparing high-purity superfine low-oxygen titanium hydride powder and dehydrogenated titanium powder - Google Patents
Method for preparing high-purity superfine low-oxygen titanium hydride powder and dehydrogenated titanium powder Download PDFInfo
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Abstract
The invention relates to a method for preparing high-purity superfine low-oxygen titanium hydride powder and dehydrogenated titanium powder and belongs to the technical field of powder producing in the powder metallurgy process. The method is characterized in that hydrogenation-dehydrogenation is combined with the closed-loop airflow milling process, titanium sponge is hydrogenated and broken to obtain coarse-particle titanium hydride powder, a closed-loop airflow milling system is used to break the titanium hydride powder again, and automatic grading and vacuum packaging are performed to obtain the titanium hydride powder; the titanium hydride powder is dehydrogenated, the closed-loop airflow milling system is used for refining, and automatic grading and vacuum packaging are performed to obtain the dehydrogenated titanium powder. The method has the advantages that the whole process is free of pollution and low in oxidation, continuous production can be achieved, and the prepared titanium hydride powder and dehydrogenated titanium powder are high in purity, even in particle size and low in oxygen content.
Description
Technical field
The invention belongs to the powder-making technique field in powder metallurgical technique, be specifically related to a kind of method preparing high-purity fine hypoxemia hydride powder and dehydrogenation titanium valve.
Background technology
Titanium or titanium alloy is as a kind of high-quality light metal structural material and important functional material, little because having density, specific strength, specific stiffness are high, without magnetic, the combination property that corrosion resistance, mechanical behavior under high temperature, antifatigue and croop property and good biocompatibility etc. are excellent, has broad application prospects in fields such as Aero-Space, naval vessel, weapons, petrochemical industry, medical treatment.But due to traditional titanium smelting process there is complex process, the shortcoming such as the cycle is long, energy consumption is large and resource utilization is low, cause that titanium or titanium alloy cost is high, price, thus limit its extensive use.Therefore, the production cost reducing titanium or titanium alloy product is the important channel expanding titanium or titanium alloy application further.
The PM technique of titanium or titanium alloy part fast-developing in recent years: the technology such as isostatic pressing technology, Metal Injection Molding, Laser Rapid Prototyping Technique, warm compaction technology and 3D printing technique, because having the advantages such as near-net-shape, energy consumption is low, stock utilization is high, become the effective ways producing low cost titanium and titanium alloy product.And titanium valve and hydride powder are as the primary raw material of titanium powder metallurgy, the production of titanium valve and hydride powder is the key link of each forming technique of powder metallurgy, and its quality and production cost limit the development of titanium or titanium alloy powder metallurgy.Therefore, develop a kind of low cost, key issue that the technology of high-quality titanium valve and hydride powder of preparing becomes titanium or titanium alloy powder metallurgy.
At present, it is several that the method for producing titanium or titanium alloy powder mainly contains atomization, reducing process, electrolysis and HDH method (Hydride-Dehydrate) etc.The sized spherical titanium powder oxygen content that atomization is produced is low, good fluidity, but cost is high, and it is mainly used in the field such as national defence and Aero-Space; Reducing process mainly contains TiO
2calciothermy, Armstrong sodium reduction and metal hydride reduction method etc., but the titanium valve impurity content that this several method is produced is higher; Electrolysis mainly contains FFC Cambridge technique, OS technique, EMR/MSE technique, but applies because the problem such as technology and cost does not also reach suitability for industrialized production; Comparatively speaking, HDH method (HDH) be instantly technical maturity and industrial scale produce the main method of titanium valve, but its titanium valve oxygen content of producing is higher.First this technique be that titanium sponge hydrogenation is generated titantium hydride, then the titantium hydride of fragility carried out break process and make hydride powder, obtain titanium valve after dehydrogenation finally by vacuum dehydrogenation and classification.In above-mentioned production process, because after indivedual operation hydride powder or dehydrogenation, titanium valve can expose in atmosphere, as hydrogenation come out of the stove, grind after go out tank, dehydrogenation is come out of the stove, especially the fine powder after hydrogenation and after dehydrogenation, because its surface-active is large, so surface is very easily oxidized, causes its oxygen content to increase, thus reduce the quality of powder.Therefore, reducing oxygen content in fine powder in said process is prepare the Focal point and difficult point of high-quality titanium valve and hydride powder.So current key problem in technology is the oxygen content how controlling fine titanium valve and hydride powder, make it while not increasing, reduce the oxygen content of its powder.
Summary of the invention
For above-mentioned technical problem, the invention provides a kind of preparation method of high-purity fine hypoxemia hydride powder, the method comprises the steps:
1) by titanium sponge at 350 ~ 680 DEG C, hydrogenation treatment 3 ~ 8h under 0.3 ~ 0.6MPa high-purity hydrogen condition, obtain the coarse granule hydride powder that granularity is 80 ~ 500 μm;
2) grinding process by carrying out air-flow in the closed loop airflow milling of above-mentioned coarse granule hydride powder under 0.35 ~ 0.6MPa high-purity argon gas condition, obtaining high-purity fine hypoxemia hydride powder.
Wherein, the preparation method of above-mentioned high-purity fine hypoxemia hydride powder, described titanium sponge is at least 4 grades of titanium sponges, oxygen content≤0.30wt%.
Wherein, the preparation method of above-mentioned high-purity fine hypoxemia hydride powder, described high-purity hydrogen purity >=99.999%, high-purity argon gas purity >=99.99%.
Wherein, the preparation method of above-mentioned high-purity fine hypoxemia hydride powder, described hydride powder purity >=98.8wt%.
Wherein, the preparation method of above-mentioned high-purity fine hypoxemia hydride powder, the particle mean size of described hydride powder is 5 ~ 75 μm, and oxygen content is 0.1 ~ 0.2wt%.
Wherein, the preparation method of above-mentioned high-purity fine hypoxemia hydride powder, described preparation process also comprises step 3) by above-mentioned steps 2) the hydride powder Vacuum Package that obtains, obtain high-purity fine hypoxemia hydride powder product.
Present invention also offers a kind of preparation method of high-purity fine hypoxemia dehydrogenation titanium valve, preparation process is as follows:
1) with above-mentioned obtained hydride powder for raw material, dehydrogenase 12 ~ 10h under 550 ~ 850 DEG C of vacuum conditions, obtains dehydrogenation titanium valve;
2) above-mentioned dehydrogenation titanium valve is carried out under 0.35 ~ 0.6MPa high-purity argon gas condition in closed loop airflow milling air-flow and grind process, obtain high-purity fine hypoxemia dehydrogenation titanium valve;
3) above-mentioned dehydrogenation titanium valve is carried out Vacuum Package, obtain high-purity fine hypoxemia dehydrogenation titanium valve product.
Wherein, the preparation method of above-mentioned high-purity fine hypoxemia dehydrogenation titanium valve, described high-purity argon gas purity >=99.99%.
Wherein, the preparation method of above-mentioned high-purity fine hypoxemia dehydrogenation titanium valve, described dehydrogenation titanium valve purity reaches 99.7wt%.
Wherein, the preparation method of above-mentioned high-purity fine hypoxemia dehydrogenation titanium valve, the particle mean size of described dehydrogenation titanium valve is 5 ~ 75 μm, and oxygen content is 0.1 ~ 0.2wt%.
Beneficial effect of the present invention: preparation method's technique of the present invention is simple, can reduce the production cost of hydride powder and dehydrogenation titanium valve; And the purity of the hydride powder prepared and dehydrogenation titanium valve is high, oxygen content is low, even particle size distribution.
Detailed description of the invention
The object of the invention is to solve the problem that the oxygen content of titanium sponge gained powder in hydrogenation-dehydrogenation (HDH) and broken technical process of regrinding is higher, and titanium valve and hydride powder after preparing the high-purity low-oxygen dehydrogenation of the interval narrower different stage of size distribution, for titanium or titanium alloy powder metallurgical technique provides quality raw materials.The technique adopting hydrogenation-dehydrogenation to combine with closed loop airflow milling prepares high-purity fine hypoxemia dehydrogenation titanium valve and hydride powder, utilize the ball milling that closed loop airflow milling replaces in traditional crushing process, on the one hand, closed loop airflow milling system is a closed system, and powder is pulverized by the high velocity impact between powder granule and friction in high-purity argon gas environment, so powder granule can not be contaminated, also other impurity element can not be brought into, on the other hand, closed loop airflow milling is a closed circuit system, high-purity argon gas can be recycled, thus reduce cost, and after high-purity argon gas injects grinding chamber by nozzle, the gas sharply large calorimetric of expansion absorption, the heat absorption that powder granule can be produced because of collision and friction, take away, grinding chamber is not heated up, thus be conducive to powder and reoxidize, and in closed loop airflow milling system, argon gas cool drying machine is housed, cooling can be carried out and drying to circulation argon gas, whole closed loop airflow milling system is made to be in low temperature all the time like this, in dry environment, be conducive to the refinement of powder.Finally, take out the powder in detachable storage tank in vacuum glove box, or directly take out and encapsulation process in glove box, controlled powder process body does not contact with air, and then by the Control for Oxygen Content of powder to lower limit.
This technique first titanium sponge is carried out hydrogenation treatment and coarse granule hydride powder is produced in fragmentation, then closed loop airflow milling system is utilized to carry out broken also automatic classification process, Vacuum Package to thick hydride powder again, with the high-purity low-oxygen hydride powder of obtained required grade designations; And vacuum dehydrogenation is carried out and automatic classification process to the hydride powder ground again through closed loop airflow milling, namely obtain the high-purity low-oxygen dehydrogenation titanium valve of required grade designations after Vacuum Package.
Based on above-mentioned purpose and principle, the invention provides a kind of preparation method of high-purity fine hypoxemia hydride powder, the method comprises the steps:
1) by titanium sponge at 350 ~ 680 DEG C, hydrogenation treatment 3 ~ 8h under 0.3 ~ 0.6MPa high-purity hydrogen pressure condition, obtain the coarse granule hydride powder that granularity is 80 ~ 500 μm;
2) process is ground by carrying out air-flow in the closed loop airflow milling of above-mentioned coarse granule hydride powder under 0.35 ~ 0.6MPa high-purity argon gas pressure condition, by changing grading wheel and feeding valve frequency, system oxygen content in closed loop airflow milling system, obtain the hydride powder of desired particle size and oxygen content specification;
3) above-mentioned hydride powder is carried out Vacuum Package, obtain high-purity fine hypoxemia hydride powder product.
Wherein, the preparation method of above-mentioned high-purity fine hypoxemia hydride powder, described titanium sponge is at least 4 grades of titanium sponges, oxygen content≤0.30wt%.
Wherein, the preparation method of above-mentioned high-purity fine hypoxemia hydride powder, described high-purity hydrogen purity >=99.999%, high-purity argon gas purity >=99.99%.
Wherein, the preparation method of above-mentioned high-purity fine hypoxemia hydride powder, the hydrogenation of described titanium sponge is carried out in horizontal hydrogenation furnace.
Wherein, the preparation method of above-mentioned high-purity fine hypoxemia hydride powder, described hydride powder purity >=98.8wt%.
Wherein, the preparation method of above-mentioned high-purity fine hypoxemia hydride powder, the particle mean size of described hydride powder is 5 ~ 75 μm, and oxygen content is 0.1 ~ 0.2wt%.
Present invention also offers a kind of preparation method of high-purity fine hypoxemia dehydrogenation titanium valve, preparation process is as follows:
1) with above-mentioned obtained hydride powder for raw material, dehydrogenase 12 ~ 10h under 550 ~ 850 DEG C of vacuum conditions, obtains dehydrogenation titanium valve;
2) above-mentioned dehydrogenation titanium valve is carried out under 0.35 ~ 0.6MPa high-purity argon gas pressure condition in closed loop airflow milling air-flow and grind process, by changing grading wheel and feeding valve frequency, system oxygen content in closed loop airflow milling system, obtain the dehydrogenation titanium valve of desired particle size and oxygen content specification;
3) above-mentioned dehydrogenation titanium valve is carried out Vacuum Package, obtain high-purity fine hypoxemia dehydrogenation titanium valve product.
Wherein, the preparation method of above-mentioned high-purity fine hypoxemia dehydrogenation titanium valve, described high-purity argon gas purity >=99.99%.
Wherein, the preparation method of above-mentioned high-purity fine hypoxemia dehydrogenation titanium valve, the dehydrogenation of described hydride powder is carried out in horizontal dehydrogenation furnace.
Wherein, the preparation method of above-mentioned high-purity fine hypoxemia dehydrogenation titanium valve, described dehydrogenation titanium valve purity reaches 99.7wt%.
Wherein, the preparation method of above-mentioned high-purity fine hypoxemia dehydrogenation titanium valve, the particle mean size of described dehydrogenation titanium valve is 5 ~ 75 μm, and oxygen content is 0.1 ~ 0.2wt%.
Above-mentioned steps 2) in, change grading wheel and feeding valve frequency in closed loop air flow system, the concrete operations of system oxygen content are: closed loop airflow milling system oxygen content is by first filling the high-purity argon gas (purity >=99.99%) of 0.35 ~ 0.6MPa to system and run closed loop airflow milling system before feeding, utilize the two ends of the circulatory system: one end is the system oxygen content detection magnetic valve located of giving vent to anger, the oxygen content of closed-loop system is detected with this, if oxygen content is higher than the setting value needed for technique, then the oxygen of discharging and exceeding setting value opened automatically by this magnetic valve; The other end is that the Electromagnetic Control of inflation place mends argon valve, by supplementing high-purity argon gas (purity >=99.99%) to closed-loop system to maintain the argon gas balance of whole closed-loop system; Closed-loop system reduces oxygen content in closed-loop system by oxygen argon filling of putting repeatedly, until open feeding valve after reaching the oxygen content of technological requirement, starts abrasive material.When closed loop airflow milling Dynamic System arranges technological parameter, according to required technological requirement, grading wheel and feeding valve frequency are set.
Compared with traditional handicraft, the invention has the advantages that:
1) hydride powder and dehydrogenation titanium valve purity high: traditional handicraft utilizes ball milling to carry out the fragmentation of powder, steel ball can increase the impurity contents such as the iron in titanium valve and hydride powder in collision process, and closed loop airflow milling utilizes high-purity argon air-flow at a high speed to make material self head-on collision pulverize, the impact force of material and grinding chamber inwall is very little, inwall is without wearing and tearing, thus foreign is brought into material, and then powder purity is high;
2) hydride powder and dehydrogenation titanium valve oxygen content low: the present invention reduces the oxygen content of powder from following several respects, one is that powder utilizes high-purity argon gas to carry out fragmentation as grinding gas in closed loop airflow milling system, do not contact with air, two is that closed loop airflow milling system constantly supplements high-purity argon gas to system by the no-load running before feeding, and then the oxygen content in closed loop airflow milling system is down to less than 0.10%, three is adopt high vacuum dehydrogenation furnace to carry out Dehydroepiandrosterone derivative when preparing titanium valve, four is that titanium valve and hydride powder all take out and encapsulate under vacuum conditions in vacuum glove box, and then the oxygen content of titanium valve and hydride powder is down to lower limit,
3) the powder process cycle is short, can be continuously produced.Closed loop airflow milling system can reinforced, the feeding of on-line continuous, and the time that grinds greatly reduces, and it is higher that powder grinds efficiency;
4) the high-purity argon gas reusable edible in closed loop airflow milling system, reduces and grinds cost.
Below in conjunction with embodiment, the invention will be further described, but it should be understood that and protection scope of the present invention should be limited in following examples.
Embodiment 1
Prepare the hydride powder of 500 orders, oxygen content 0.20wt%
1, by oxygen content be 0.30wt% 4 grades of titanium sponges 580 DEG C, carry out hydrogenation treatment 6h under 0.55MPa high-purity hydrogen pressure condition, obtain the coarse granule titantium hydride of particle mean size 80 μm;
2, carry out airflow milling process by the closed loop airflow milling of above-mentioned hydride powder under 0.6MPa high-purity argon gas pressure condition, obtain that purity is greater than 98.8wt%, particle mean size is 25 μm (500 orders), oxygen content is the hydride powder of 0.20wt%;
3, above-mentioned hydride powder is carried out vacuum packing, namely obtain high-purity fine hypoxemia hydride powder product.
Prepare the dehydrogenation titanium valve of 500 orders, oxygen content 0.19wt%
1, by oxygen content be 0.30wt% 4 grades of titanium sponges 580 DEG C, carry out hydrogenation treatment 6h under 0.55MPa high-purity hydrogen pressure condition, obtain the coarse granule titantium hydride of particle mean size 80 μm;
2, carry out airflow milling process by the closed loop airflow milling of above-mentioned hydride powder under 0.6MPa high-purity argon gas pressure condition, obtain the titantium hydride that particle mean size is 28 μm;
3, namely the titantium hydride vacuum dehydrogenation 5h under 750 DEG C of conditions after closed loop airflow milling being ground obtains dehydrogenation titanium valve;
4, carry out levigate process by the closed loop airflow milling system of dehydrogenation titanium valve under 0.6MPa high-purity argon gas pressure condition, obtain the dehydrogenation titanium valve that purity reaches 99.7wt%, particle mean size is 25 μm (500 orders), oxygen content is 0.19wt%.
5, above-mentioned dehydrogenation titanium valve is carried out vacuum packing, namely obtain high-purity fine hypoxemia dehydrogenation titanium valve product.
Embodiment 2
Prepare the hydride powder of 400 orders, oxygen content 0.18wt%
1, by oxygen content be 0.30wt% 4 grades of titanium sponges 680 DEG C, carry out hydrogenation treatment 4h under 0.55MPa high-purity hydrogen pressure condition, obtain the coarse granule titantium hydride of particle mean size 100 μm;
2, carry out airflow milling process by the closed loop airflow milling of above-mentioned hydride powder under 0.6MPa high-purity argon gas pressure condition, obtain that purity is greater than 98.8wt%, particle mean size is 38 μm (400 orders), oxygen content is the hydride powder of 0.18wt%;
3, above-mentioned hydride powder is carried out vacuum packing, namely obtain high-purity fine hypoxemia hydride powder product.
Prepare the dehydrogenation titanium valve of 400 orders, oxygen content 0.17wt%
1, by oxygen content be 0.30wt% 4 grades of titanium sponges 680 DEG C, carry out hydrogenation treatment 4h under 0.55MPa high-purity hydrogen pressure condition, obtain the coarse granule titantium hydride of particle mean size 100 μm;
2, carry out airflow milling process by the closed loop airflow milling of above-mentioned hydride powder under 0.6MPa high-purity argon gas pressure condition, obtain the titantium hydride that particle mean size is 40 μm;
3, namely the titantium hydride vacuum dehydrogenation 5h under 600 DEG C of conditions after closed loop airflow milling being ground obtains dehydrogenation titanium valve;
4, carry out airflow milling process by the closed loop airflow milling of dehydrogenation titanium valve under 0.6MPa high-purity argon gas pressure condition, obtain the dehydrogenation titanium valve that purity reaches 99.7wt%, particle mean size is 38 μm (400 orders), oxygen content is 0.17wt%.
5, above-mentioned dehydrogenation titanium valve is carried out vacuum packing, namely obtain high-purity fine hypoxemia dehydrogenation titanium valve product.
Embodiment 3
Prepare the hydride powder of 300 orders, oxygen content 0.16wt%
1, by oxygen content be 0.30wt% 4 grades of titanium sponges 480 DEG C, carry out hydrogenation treatment 7h under 0.3MPa high-purity hydrogen pressure condition, obtain the coarse granule titantium hydride of particle mean size 150 μm;
2, carry out airflow milling process by the closed loop airflow milling of above-mentioned hydride powder under 0.58MPa high-purity argon gas pressure condition, obtain that purity is greater than 98.8wt%, particle mean size is 48 μm (300 orders), oxygen content is the hydride powder of 0.16wt%;
3, above-mentioned hydride powder is carried out vacuum packing, namely obtain high-purity fine hypoxemia hydride powder product.
Prepare the dehydrogenation titanium valve of 300 orders, oxygen content 0.15wt%
1, by oxygen content be 0.30wt% 4 grades of titanium sponges 480 DEG C, carry out hydrogenation treatment 7h under 0.3MPa high-purity hydrogen pressure condition, obtain the coarse granule titantium hydride of particle mean size 150 μm;
2, carry out airflow milling process by the closed loop airflow milling of above-mentioned hydride powder under 0.58MPa high-purity argon gas pressure condition, obtain the titantium hydride that particle mean size is 50 μm;
3, namely the titantium hydride vacuum dehydrogenation 8h under 650 DEG C of conditions after closed loop airflow milling being ground obtains dehydrogenation titanium valve;
4, carry out airflow milling process by the closed loop airflow milling of dehydrogenation titanium valve under 0.58MPa high-purity argon gas pressure condition, obtain the dehydrogenation titanium valve that purity reaches 99.7wt%, particle mean size is 48 μm (300 orders), oxygen content is 0.15wt%.
5, above-mentioned dehydrogenation titanium valve is carried out vacuum packing, namely obtain high-purity fine hypoxemia dehydrogenation titanium valve product.
Embodiment 4
Prepare the hydride powder of 200 orders, oxygen content 0.15wt%
1, by oxygen content be 0.30wt% 4 grades of titanium sponges 580 DEG C, carry out hydrogenation treatment 5h under 0.4MPa high-purity hydrogen pressure condition, obtain the coarse granule titantium hydride of particle mean size 250 μm;
2, carry out airflow milling process by the closed loop airflow milling of above-mentioned hydride powder under 0.55MPa high-purity argon gas pressure condition, obtain that purity is greater than 98.8wt%, particle mean size is 74 μm (200 orders), oxygen content is the hydride powder of 0.15wt%;
3, above-mentioned hydride powder is carried out vacuum packing, namely obtain high-purity fine hypoxemia hydride powder product.
Prepare the dehydrogenation titanium valve of 200 orders, oxygen content 0.14wt%
1, by oxygen content be 0.30wt% 4 grades of titanium sponges 580 DEG C, carry out hydrogenation treatment 5h under 0.4MPa high-purity hydrogen pressure condition, obtain the coarse granule titantium hydride of particle mean size 250 μm;
2, carry out airflow milling process by the closed loop airflow milling of above-mentioned hydride powder under 0.55MPa high-purity argon gas pressure condition, obtain the hydride powder that particle mean size is 75 μm;
3, namely the hydride powder vacuum dehydrogenation 6h under 700 DEG C of conditions after closed loop airflow milling being ground obtains dehydrogenation titanium valve;
4, carry out airflow milling process by the closed loop airflow milling of dehydrogenation titanium valve under 0.55MPa high-purity argon gas pressure condition, obtain the dehydrogenation titanium valve that purity reaches 99.7wt%, particle mean size is 74 μm (200 orders), oxygen content is 0.14wt%.
5, above-mentioned dehydrogenation titanium valve is carried out vacuum packing, namely obtain high-purity fine hypoxemia dehydrogenation titanium valve product.
Claims (10)
1. the preparation method of high-purity fine hypoxemia hydride powder, is characterized in that, preparation process is as follows:
1) by titanium sponge at 350 ~ 680 DEG C, hydrogenation treatment 3 ~ 8h under 0.3 ~ 0.6MPa high-purity hydrogen condition, obtain the coarse granule hydride powder that granularity is 80 ~ 500 μm;
2) grinding process by carrying out air-flow in the closed loop airflow milling of above-mentioned coarse granule hydride powder under 0.35 ~ 0.6MPa high-purity argon gas condition, obtaining high-purity fine hypoxemia hydride powder.
2. the preparation method of high-purity fine hypoxemia hydride powder according to claim 1, is characterized in that, described titanium sponge is at least 4 grades of titanium sponges, oxygen content≤0.30wt%.
3. the preparation method of high-purity fine hypoxemia hydride powder according to claim 1, is characterized in that, described high-purity hydrogen purity >=99.999%, high-purity argon gas purity >=99.99%.
4. the preparation method of high-purity fine hypoxemia hydride powder according to claim 1, is characterized in that, described hydride powder purity >=98.8wt%.
5. the preparation method of high-purity fine hypoxemia hydride powder according to claim 1, is characterized in that, the particle mean size of described hydride powder is 5 ~ 75 μm, and oxygen content is 0.1 ~ 0.2wt%.
6. the preparation method of high-purity fine hypoxemia hydride powder according to claim 1, it is characterized in that, described preparation process also comprises step 3) by above-mentioned steps 2) the hydride powder Vacuum Package that obtains, obtain high-purity fine hypoxemia hydride powder product.
7. the preparation method of high-purity fine hypoxemia dehydrogenation titanium valve, it is characterized in that, preparation process is as follows:
1) with the obtained hydride powder of any one of Claims 1 to 5 for raw material, dehydrogenase 12 ~ 10h under 550 ~ 850 DEG C of vacuum conditions, obtains dehydrogenation titanium valve;
2) by above-mentioned dehydrogenation titanium valve under 0.35 ~ 0.6MPa high-purity argon gas condition, in closed loop airflow milling, carry out air-flow grind process, obtain high-purity fine hypoxemia dehydrogenation titanium valve;
3) by above-mentioned dehydrogenation titanium valve Vacuum Package, high-purity fine hypoxemia dehydrogenation titanium valve product is obtained.
8. the preparation method of high-purity fine hypoxemia dehydrogenation titanium valve according to claim 7, is characterized in that, described high-purity argon gas purity >=99.99%.
9. the preparation method of high-purity fine hypoxemia dehydrogenation titanium valve according to claim 7, is characterized in that, described dehydrogenation titanium valve purity is 99.7wt%.
10. the preparation method of high-purity fine hypoxemia dehydrogenation titanium valve according to claim 7, is characterized in that, the particle mean size of described dehydrogenation titanium valve is 5 ~ 75 μm, and oxygen content is 0.1 ~ 0.2wt%.
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CN109202090A (en) * | 2018-10-23 | 2019-01-15 | 朝阳金达钛业股份有限公司 | A kind of production method of hypoxemia hydrogenation dehydrogenation titanium powder |
WO2019124325A1 (en) * | 2017-12-20 | 2019-06-27 | トーホーテック株式会社 | Titanium powder and method for producing same |
CN110756813A (en) * | 2019-11-01 | 2020-02-07 | 宁波江丰电子材料股份有限公司 | Preparation method of high-purity titanium powder |
CN111151762A (en) * | 2020-01-15 | 2020-05-15 | 北京科技大学 | Preparation method of low-cost fine-grained low-oxygen titanium and titanium alloy powder |
WO2020211402A1 (en) * | 2019-04-16 | 2020-10-22 | 北京科技大学 | Preparation, based on fluidized bed jet milling technique, of titanium and titanium alloy powders for 3d printing |
CN113976894A (en) * | 2021-09-14 | 2022-01-28 | 北京七弟科技有限公司 | Preparation method of spherical or spheroidal metal powder for low-oxygen MIM |
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