CN109128207B - Superfine titanium powder and preparation method thereof - Google Patents
Superfine titanium powder and preparation method thereof Download PDFInfo
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- CN109128207B CN109128207B CN201811257670.6A CN201811257670A CN109128207B CN 109128207 B CN109128207 B CN 109128207B CN 201811257670 A CN201811257670 A CN 201811257670A CN 109128207 B CN109128207 B CN 109128207B
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
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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
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/023—Hydrogen absorption
Abstract
The invention provides superfine titanium powder and a preparation method thereof, belonging to the technical field of powder metallurgy, and the method comprises the steps of sequentially carrying out hydrogenation, dehydrogenation and plasma spheroidization on raw material titanium to obtain the superfine titanium powder; the hydrogenation temperature is 500-700 ℃; the dehydrogenation temperature is 400-600 ℃; the hydrogenation and dehydrogenation are carried out under milling conditions. The hydrogenation temperature is set to be 500-700 ℃, the diffusion coefficient of hydrogen in titanium is larger at the upper limit range of plastic deformation of titanium, and the raw material titanium is completely hydrogenated by continuous grinding, so that the hydrogenation time is shortened; the temperature in the dehydrogenation process is set to be 400-600 ℃, so that the dehydrogenation rate is ensured, and the secondary hydrogenation can be avoided. According to the invention, by carrying out hydrogenation and dehydrogenation under the grinding condition and controlling the hydrogenation and dehydrogenation temperatures, the production efficiency is improved under the condition of ensuring the product quality.
Description
Technical Field
The invention relates to the technical field of powder metallurgy, in particular to superfine titanium powder and a preparation method thereof.
Background
Powder metallurgy is a process technique for producing metal powder or metal powder (or a mixture of metal powder and nonmetal powder) as a raw material, and then forming and sintering the raw material to produce metal materials, composite materials and various products.
The metal titanium has excellent performances of small density, high specific strength, acid and alkali corrosion resistance and the like, and is widely applied to various fields of aerospace, energy and chemical industry, medical instruments, metallurgy, civil use and the like. However, titanium metal is easy to react with oxygen, nitrogen, carbon and the like at high temperature, so that the difficulty in producing high-purity titanium powder and titanium alloy with low oxygen content is increased.
At present, the production method of the metal titanium powder mainly comprises the following steps: electrolytic methods, hydrodeoxygenation methods, ultrasonic atomization methods, and plasma rotating electrode methods. The Russian Federal patent RU2631692 discloses a method for preparing spherical superfine titanium powder, which comprises the steps of periodically hydrogenating raw materials in a hydrogen environment at a temperature of not less than 815 ℃, cooling to a temperature of not more than 400 ℃, grinding titanium hydride, dehydrogenating titanium at a temperature of 580-610 ℃, grinding the dehydrogenated titanium by a rotary grinding machine under vacuum, grading powder, and feeding superfine powder into a plasma arc to perform spheroidization treatment of the superfine powder. However, the above-mentioned method in which the material is ground after hydrogenation and dehydrogenation many times results in a great reduction in the production efficiency of titanium powder.
Disclosure of Invention
In view of the above, the present invention aims to provide an ultrafine titanium powder and a preparation method thereof, and the preparation method of the ultrafine titanium powder provided by the present invention has high production efficiency, and the obtained ultrafine titanium powder has stable particle size and high sphericity.
The invention provides a preparation method of superfine titanium powder, which comprises the following steps:
sequentially hydrogenating, dehydrogenating and spheroidizing a raw material titanium by using plasma to obtain superfine titanium powder; the granularity of the raw material titanium is 3-15 mm;
the hydrogenation temperature is 500-700 ℃;
the dehydrogenation temperature is 400-600 ℃;
the hydrogenation and dehydrogenation are carried out under milling conditions.
Preferably, the raw material titanium is sponge titanium, titanium-containing alloy or titanium waste.
Preferably, the temperature of the hydrogenation is 600-650 ℃.
Preferably, the hydrogenation time is 1.5-3 h.
Preferably, the dehydrogenation temperature is 500-550 ℃.
Preferably, the dehydrogenation time is 3-8 h.
Preferably, the milling is ball milling.
Preferably, the plasma spheroidizing comprises the following steps:
and enabling the powder obtained after dehydrogenation to flow into a downward arc of plasma in a rising powder flow mode, wherein the flow speed of the powder flow is 8-12 g/min.
The invention also provides the superfine titanium powder prepared by the preparation method, which is characterized in that the particle size of the superfine titanium powder is 10-60 mu m, and the spheroidization degree of the superfine titanium powder is 95-98%.
The beneficial technical effects are as follows: the invention provides superfine titanium powder and a preparation method thereof, wherein the titanium raw material is sequentially subjected to hydrogenation, dehydrogenation and plasma spheroidization to obtain the superfine titanium powder; the hydrogenation temperature is 500-700 ℃; the dehydrogenation temperature is 400-600 ℃; the hydrogenation and dehydrogenation are carried out under milling conditions. The hydrogenation temperature is set to be 500-700 ℃, the diffusion coefficient of hydrogen in titanium is larger at the upper limit range of plastic deformation of titanium, and the raw material titanium is completely hydrogenated by continuous grinding, so that the hydrogenation time is shortened; the temperature of the dehydrogenation process is set to be 400-600 ℃, so that the dehydrogenation rate is ensured, and the secondary hydrogenation can be avoided. According to the invention, by carrying out hydrogenation and dehydrogenation under the grinding condition and controlling the hydrogenation and dehydrogenation temperatures, the production efficiency is improved under the condition of ensuring the product quality.
Detailed Description
The invention provides a preparation method of superfine titanium powder, which comprises the following steps:
sequentially hydrogenating, dehydrogenating and spheroidizing a raw material titanium by using plasma to obtain superfine titanium powder; the granularity of the raw material titanium is 3-15 mm;
the hydrogenation temperature is 500-700 ℃;
the dehydrogenation temperature is 400-600 ℃;
the hydrogenation and dehydrogenation are carried out under milling conditions.
In the present invention, the raw material titanium is preferably titanium sponge, titanium-containing alloy, or titanium scrap.
In the invention, the titanium content in the raw material titanium is more than 95 wt%.
In the invention, the temperature of the hydrogenation is 500-700 ℃, preferably 600-650 ℃; the hydrogenation time is preferably 1.5-3 h, and more preferably 2-2.5 h. In the present invention, the hydrogenation is preferably carried out in a sealed rotating drum. The hydrogenation temperature is set to be 500-700 ℃, the diffusion coefficient of hydrogen in titanium is large in the upper limit range of plastic deformation of titanium, and the hydrogen can penetrate into titanium particles more deeply.
In the present invention, the hydrogenation is carried out under milling conditions. The milling is preferably ball milling. When the grinding is ball milling, the ball-to-material ratio of the ball milling is preferably 1: 10-20, more preferably 1: 15. in the hydrogenation process, the titanium hydride film formed on the surface of the raw material titanium in the hydrogenation process can be removed by continuously grinding the raw material titanium, and the inner layer is further hydrogenated, so that the complete hydrogenation of the raw material titanium is realized, and the hydrogenation efficiency is improved.
In the present invention, the hydrogenation step preferably further comprises selecting screens with different mesh sizes to screen the hydrogenated powder according to different applications, so as to realize final control of the powder particle size.
In the invention, the dehydrogenation temperature is 400-600 ℃, preferably 500-550 ℃; the time for dehydrogenation is preferably 3 to 8 hours, and more preferably 4 to 6 hours. In the present invention, the dehydrogenation process is preferably carried out in a sealed rotating drum. The temperature of the dehydrogenation process is set to be 400-600 ℃, so that the dehydrogenation rate is ensured, and the secondary hydrogenation can be avoided.
In the present invention, the dehydrogenation is carried out under milling conditions. The milling conditions are preferably consistent with the hydrogenation process. In the invention, the product obtained after hydrogenation is continuously ground to minimize the thickness of the surface layer, and hydrogen atoms can diffuse from the depth of particles to the surface, thereby improving the dehydrogenation efficiency.
In the present invention, the plasma spheroidizing preferably includes the steps of:
and enabling the powder obtained after dehydrogenation to flow into a downward arc of plasma in a rising powder flow mode, wherein the flow speed of the powder flow is 8-12 g/min.
In the invention, the flow speed of the powder flow is preferably 9-10 g/min. In the invention, the plasma spheroidizing device is preferably a plasma device, and the power of plasma in the plasma device is preferably 15-100 kW, more preferably 60-100 kW.
In the present invention, when the flow rate of the powder stream is less than 8.0g/min, the powder particles agglomerate into larger particles, which results in a change in the particle composition of the product and reduces the production efficiency for obtaining an acceptable product, and when the powder feed rate is higher than 12g/min, it results in more than 15% of non-spherical particles in the product.
The invention also provides the superfine titanium powder prepared by the preparation method, wherein the particle size of the superfine titanium powder is 10-60 mu m, and the spheroidization degree of the superfine titanium powder is 95-98%.
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
Example 1
The hydrogenation and dehydrogenation processes are carried out in a reactor with an external heating source and a heat-insulated seal, and a vacuum system with a mechanical vacuum pump and a diffusion pump. The hydrogen used was gaseous hydrogen purified on a special apparatus, and the starting material used was ground titanium sponge, model TA 0.
The hydrogenation process is carried out in a heat insulation sealed rotary drum with an external heating source, the drum body and the grinding ball are made of hard alloy, the ball-material ratio is 1:10, the hydrogenation temperature is 550 ℃, the hydrogenation time is 2 hours, hydride is obtained, the hydride is screened by selecting screens with different meshes according to different purposes and then is added into a reactor for dehydrogenation, the dehydrogenation process is also carried out in the heat insulation sealed rotary drum with the same ball-material ratio, the dehydrogenation temperature is 500 ℃, and the formation of sintering blocks is not observed in the dehydrogenation process, so that the continuity and high productivity of the process for manufacturing high-quality titanium powder are ensured. Spheroidizing the dehydrogenated powder in a plasma device, wherein the plasma power is 100kW, and the dehydrogenated powder enters a downward arc of plasma in a rising powder flow mode to be spheroidized to obtain superfine titanium powder; the conveying speed of the powder flow is 10.0g/min, the spheroidization degree of the titanium powder is 98%, the size range of the powder is 10-60 micrometers, and the yield of the whole process reaches 92%.
Examples 2 to 4
The parameters for examples 2 to 4 are shown in Table 1, and the other conditions were exactly the same as in example 1.
Comparative examples 1 to 2
Relevant parameters of comparative examples 1 to 2 are shown in Table 1, and other conditions were exactly the same as those of example 1.
TABLE 1 comparison of relevant parameters and effects of examples 1-4 and comparative examples 1-2
As shown in Table 1, the preparation method of the ultrafine titanium powder provided by the invention shortens the hydrogenation and dehydrogenation time, and has high spheroidization degree and high yield.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (4)
1. A preparation method of ultrafine titanium powder comprises the following steps:
sequentially hydrogenating, dehydrogenating and spheroidizing a raw material titanium by using plasma to obtain superfine titanium powder; the granularity of the raw material titanium is 3-15 mm;
the temperature of the hydrogenation is 700 ℃; the hydrogenation time is 2 h;
the temperature of the dehydrogenation is 600 ℃;
the hydrogenation and dehydrogenation are carried out under milling conditions;
the grinding is ball milling, and the ball-to-material ratio of the ball milling is 1: 10;
the size of the superfine titanium powder is within the range of 10-60 mu m;
the plasma spheroidizing method comprises the following steps:
the powder obtained after dehydrogenation flows into a downward arc of plasma in the form of ascending powder flow, and the flow rate of the powder flow is 6 g/min; the plasma power was 100 kW.
2. The method according to claim 1, wherein the raw material titanium is titanium sponge, titanium-containing alloy, or titanium scrap.
3. The preparation method according to claim 1, wherein the dehydrogenation time is 3-8 h.
4. The ultrafine titanium powder prepared by the preparation method according to any one of claims 1 to 3, wherein the particle size of the ultrafine titanium powder is 10 to 60 μm, and the spheroidization degree of the ultrafine titanium powder is 98%.
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| CN109622943B (en) * | 2019-01-08 | 2021-04-06 | 成都先进金属材料产业技术研究院有限公司 | Superfine titanium powder and preparation method thereof |
| CN110560696A (en) * | 2019-10-15 | 2019-12-13 | 江苏思睿迪快速制造科技有限公司 | method for preparing titanium alloy spherical powder by recycling titanium material |
| 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 |
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