CN111421142A - Preparation method of spherical titanium powder - Google Patents
Preparation method of spherical titanium powder Download PDFInfo
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- CN111421142A CN111421142A CN202010218069.7A CN202010218069A CN111421142A CN 111421142 A CN111421142 A CN 111421142A CN 202010218069 A CN202010218069 A CN 202010218069A CN 111421142 A CN111421142 A CN 111421142A
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 63
- 238000000034 method Methods 0.000 claims abstract description 34
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 31
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052751 metal Inorganic materials 0.000 claims abstract description 22
- 239000002184 metal Substances 0.000 claims abstract description 22
- 238000005406 washing Methods 0.000 claims abstract description 20
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000007873 sieving Methods 0.000 claims abstract description 14
- 239000000292 calcium oxide Substances 0.000 claims abstract description 13
- 235000012255 calcium oxide Nutrition 0.000 claims abstract description 13
- 239000002253 acid Substances 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 11
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 10
- 239000001110 calcium chloride Substances 0.000 claims abstract description 10
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000012159 carrier gas Substances 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000012300 argon atmosphere Substances 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 10
- 239000001301 oxygen Substances 0.000 abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 6
- 239000007769 metal material Substances 0.000 abstract description 2
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 12
- 239000007788 liquid Substances 0.000 description 11
- 230000001788 irregular Effects 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- 239000010936 titanium Substances 0.000 description 9
- 229910052719 titanium Inorganic materials 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000007789 gas Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000004484 Briquette Substances 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 238000000889 atomisation Methods 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 230000003116 impacting effect Effects 0.000 description 1
- -1 powder metallurgy Chemical compound 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
-
- 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
-
- 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
- B22F1/142—Thermal or thermo-mechanical treatment
-
- 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
-
- 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
Abstract
The invention relates to a preparation method of spherical titanium powder, belonging to the technical field of metallurgy and metal material preparation. Mixing aluminum powder and quicklime uniformly, briquetting and placing at one end of a vacuum reactor; briquetting the mixture of titanium dioxide and calcium chloride, placing the briquetting at the other end of the vacuum reactor, and carrying out vacuum thermal reduction to obtain a titanium dioxide reduction product; crushing, acid washing, filtering, drying and sieving the obtained titanium dioxide reduction product to obtain metal titanium powder; and sending the obtained metal titanium powder into a plasma furnace for spheroidization to finally obtain the spherical titanium powder. The invention uses titanium dioxide as raw material, and adopts vacuum thermal reduction method and plasma spheroidizing technique to prepare spherical titanium powder, and the prepared product powder has the characteristics of high spheroidizing rate, small titanium powder granularity, low oxygen content and the like.
Description
Technical Field
The invention relates to a preparation method of spherical titanium powder, belonging to the technical field of metallurgy and metal material preparation.
Background
Titanium has the advantages of low density, high specific strength, good corrosion resistance and the like, and is widely applied to the fields of aerospace and the like. With the continuous development of the application of spherical titanium powder such as powder metallurgy, 3D printing technology and the like, the demand for the spherical titanium powder is rapidly increased, and the production technology of the spherical titanium powder with high purity, low cost and low oxygen content becomes a hot point for the research of the powder preparation technology at home and abroad. At present, the preparation method of the spherical titanium powder mainly comprises a sponge titanium mechanical crushing method, an atomization method, a plasma rotating electrode method and the like.
The mechanical crushing method is a method for crushing metal or alloy into powder by simple mechanical action, and because titanium has toughness, the shape of the powder obtained by crushing by the method is irregular, and the purity of the titanium is reduced due to pollution in the crushing process, so that the titanium does not meet the production requirement; the atomization method is a method for forming metal powder by impacting and crushing molten metal liquid flow by utilizing high-speed airflow and rapidly cooling, in the atomization process, the metal liquid is easy to deform, and most of the obtained powder is satellite balls or hollow particles; the plasma rotating electrode method is a method of making metal or alloy into consumable electrode, melting the electrode end surface into liquid by electric arc heating, throwing out the liquid by the centrifugal force of high-speed rotation of the electrode and crushing into fine liquid drops, finally condensing into powder, the powder prepared by the method has better sphericity and few hollow structure particles and planetary particles, but the method has certain defects, the particle size of the spherical titanium powder prepared by the method is mostly concentrated in the range of hundreds of microns, and the yield of the spherical titanium powder of about 50 microns is lower. In the methods, sponge titanium or titanium ingots (titanium rods) and other compact titanium are used as raw materials, and the obtained spherical titanium powder has large granularity and high production cost.
Disclosure of Invention
Aiming at the problems and the defects in the prior art, the invention provides a preparation method of spherical titanium powder. The invention uses titanium dioxide as raw material, and adopts vacuum thermal reduction method and plasma spheroidizing technique to prepare spherical titanium powder, and the prepared product powder has the characteristics of high spheroidizing rate, small titanium powder granularity, low oxygen content and the like. The invention is realized by the following technical scheme.
A preparation method of spherical titanium powder comprises two main steps of thermal reduction of titanium dioxide and plasma spheroidization; the method comprises the following steps:
step 1, uniformly mixing aluminum powder and quicklime, briquetting, and placing at one end of a vacuum reactor; briquetting the mixture of titanium dioxide and calcium chloride, placing the briquetting at the other end of the vacuum reactor, and carrying out vacuum thermal reduction to obtain a titanium dioxide reduction product;
step 2, crushing, acid washing, filtering, drying and sieving the titanium dioxide reduction product obtained in the step 1 to obtain metal titanium powder;
and 3, feeding the metal titanium powder obtained in the step 2 into a plasma furnace, and carrying out spheroidization to finally obtain spherical titanium powder.
In the step 1, the mass ratio of the aluminum powder to the quick lime is 0.35: 1-0.5: 1, and the aluminum powder and the quick lime are pressed into blocks under the pressure of 2 MPa-10 MPa.
In the step 1, vacuum thermal reduction is carried out, the pressure is maintained to be less than 10Pa, the heating rate is kept to be 5-15 ℃/min, the reduction temperature is 1100-1300 ℃, and the heat preservation time is 8-20 h.
And (3) crushing, acid washing, filtering, drying and sieving in the step (2) are carried out in an argon atmosphere or in vacuum.
And 3, the plasma furnace in the step 3 is a direct current plasma or radio frequency plasma furnace.
And 3, loading the metal titanium powder into the plasma furnace through argon carrier gas, wherein the working power of the plasma furnace is 20-30 kW, the flow rate of the carrier gas is controlled to be 4-10L/min, and the feeding rate of the titanium powder is 1-10 g/min.
The step 1 is a step of thermally reducing titanium dioxide, and the step 3 is a step of plasma spheroidization.
The washing liquid in the acid washing process of the step 2 is 3wt% hydrochloric acid, the solid-to-liquid ratio ranges from 1:20 to 1:35g/m L, the stirring speed is 200 to 350r/min during washing, the filtered filtrate can be recycled, and the calcium chloride can be recycled.
The irregular metal titanium powder with the granularity of 10-40 mu m obtained after the treatment of the step 2 has the purity of more than 99.5 percent, is in a worm-like irregular shape, has the oxygen content of less than 0.3wt percent, and meets the requirement of zero-order titanium powder in the YS/T654-2007 titanium powder standard.
The invention adopts a plasma furnace to spheroidize irregular titanium powder prepared by a thermal reduction method, the raw materials are placed in a feeder, after the plasma furnace normally operates, the raw materials are fed by a feeding gun, the titanium powder enters a high-temperature area of a plasma torch through carrier gas, under the condition of protecting the gas, the spheroidization is completed through melting and condensing processes in a very short time, and the spheroidization is cooled and collected in a low-temperature area at the lower part of a furnace body.
The titanium powder treated by the plasma furnace in the step 3 is spherical, the granularity is 10-60 mu m, and the oxygen content is lower than 0.15 wt%.
Compared with the prior art, the invention has the beneficial effects that:
(1) the precursor titanium powder with smaller granularity is easily prepared by thermally reducing titanium dioxide, and the particle size is 10-40 mu m.
(2) Subsequently, spheroidizing the irregular precursor titanium powder by using a plasma spheroidizing process to obtain spherical titanium powder with the particle size of 10-60 mu m, wherein the spheroidization rate is over 95 percent, and the powder has good fluidity; in addition, the titanium powder obtained after vacuum reduction is directly transferred to plasma high-temperature spheroidization, and oxygen in titanium oxide which is not fully reduced in the titanium powder is further removed through high temperature of thousands of degrees, so that the lower oxygen content of the spherical titanium powder is ensured, and the lowest oxygen content can be 700ppm in practice.
(3) The invention takes titanium dioxide as a raw material, prepares the spherical titanium powder by thermal reduction and plasma spheroidization, shortens the process flow compared with other methods, and can control the granularity of the spherical titanium powder by changing the granularity of the irregular titanium powder of the precursor.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is an SEM photograph of spherical titanium powder prepared in example 1 of the present invention;
FIG. 3 is an SEM image of spherical titanium powder prepared in example 2 of the present invention.
Detailed Description
The invention is further described with reference to the following drawings and detailed description.
Example 1
As shown in FIG. 1, the preparation method of the spherical titanium powder comprises two main steps of thermal reduction of titanium dioxide and plasma spheroidization; the method comprises the following steps:
step 1, uniformly mixing aluminum powder and green stone (the mass ratio of the aluminum powder to the quicklime is 0.35: 1) ash, briquetting under the pressure of 2MPa, and placing at one end of a vacuum reactor; briquetting a mixture of titanium dioxide and calcium chloride (the mass ratio of the titanium dioxide to the calcium chloride is 2: 1) under the pressure of 4MPa, placing the briquette at the other end of the vacuum reactor, and starting a vacuum pump to stabilize the air pressure in the furnace to be below 10 Pa; starting the furnace, setting a program to enable the furnace to be heated to 1100 ℃ at a speed of 5 ℃/min, preserving the temperature for 20h at the reaction temperature so as to enable calcium steam generated by the reaction of the aluminum powder and the quicklime to be fully contacted with the materials, and obtaining a titanium dioxide reduction product through vacuum thermal reduction;
step 2, crushing, acid washing, filtering, drying and sieving the titanium dioxide reduction product obtained in the step 1 to obtain metal titanium powder, wherein the washing solution is 3wt% hydrochloric acid, the solid-to-liquid ratio is 1:20g/m L, the stirring speed is 200r/min during washing, the metal titanium powder is obtained after drying and sieving at 80 ℃ in a vacuum drying oven, and the crushing, acid washing, filtering, drying and sieving in the step 2 are carried out in argon atmosphere or vacuum;
and 3, turning on a power switch of the direct current plasma equipment, after arc striking, stabilizing the power at about 20kW, feeding the metal titanium powder obtained in the step 2 by a feeding gun, wherein the titanium powder is carried by carrier gas to enter a high-temperature region of the plasma torch, the carrier gas flow is 4L/min, the titanium powder loading amount is controlled to be 1.2g/min, irregular titanium powder particles are quickly melted in the high-temperature region under the protection of argon gas, the melted powder particles are quickly condensed to form liquid drops with high spherical degree under the action of surface tension under the action of great temperature gradient, and are quickly condensed to realize spheroidization in the falling process, the shield gas argon gas flow is 4L/min, and the prepared spherical titanium powder is cooled and collected in the low-temperature region at the lower part of the furnace body to be spheroidized, so that the spherical titanium powder is finally obtained.
An SEM image of the spherical titanium powder prepared by the embodiment is shown in FIG. 2, and analysis shows that the spherical titanium powder has the oxygen content of 700ppm and the particle size of 10-60 μm.
Example 2
As shown in FIG. 1, the preparation method of the spherical titanium powder comprises two main steps of thermal reduction of titanium dioxide and plasma spheroidization; the method comprises the following steps:
step 1, uniformly mixing aluminum powder and green stone (the mass ratio of the aluminum powder to the quicklime is 0.5: 1) ash, briquetting under the pressure of 6MPa, and placing at one end of a vacuum reactor; briquetting a mixture of titanium dioxide and calcium chloride (the mass ratio of titanium dioxide to calcium chloride is 4: 1) under the pressure of 8MPa, placing the briquette at the other end of the vacuum reactor, and starting a vacuum pump to stabilize the air pressure in the furnace to be below 10 Pa; then opening the furnace, setting a program to enable the temperature of the furnace to rise to 1300 ℃ at a speed of 15 ℃/min, preserving the temperature for 12h at the reaction temperature so as to enable calcium steam generated by the reaction of the aluminum powder and the quicklime to fully contact with the materials, and obtaining a titanium dioxide reduction product through vacuum thermal reduction;
step 2, crushing, acid washing, filtering, drying and sieving the titanium dioxide reduction product obtained in the step 1 to obtain metal titanium powder, wherein the washing solution is 3wt% hydrochloric acid, the solid-to-liquid ratio is 1:35g/m L, the stirring speed is 350r/min during washing, the metal titanium powder is obtained after drying and sieving at 80 ℃ in a vacuum drying oven, and the crushing, acid washing, filtering, drying and sieving in the step 2 are carried out in argon atmosphere or vacuum;
and 3, turning on a power switch of the radio frequency plasma equipment, after the equipment runs stably, enabling the working power to be about 25kW, feeding the metal titanium powder obtained in the step 2 by using a feeding gun, wherein the titanium powder is carried by carrier gas and enters a high-temperature region of the plasma torch, the carrier gas flow is 6L/min, the feeding rate of the titanium powder is about 5.8g/min, the protective gas is argon, the flow is controlled to be 10L/min, and irregular titanium powder particles are rapidly melted, fall, cooled and solidified in the high-temperature region to obtain the spherical titanium powder.
An SEM image of the spherical titanium powder prepared by the embodiment is shown in FIG. 3, and analysis shows that the spherical titanium powder has an oxygen content of 1500ppm and a particle size of 10-60 μm.
Example 3
As shown in FIG. 1, the preparation method of the spherical titanium powder comprises two main steps of thermal reduction of titanium dioxide and plasma spheroidization; the method comprises the following steps:
step 1, uniformly mixing aluminum powder and green stone (the mass ratio of the aluminum powder to the quicklime is 0.4: 1) ash, briquetting under the pressure of 10MPa, and placing at one end of a vacuum reactor; briquetting a mixture of titanium dioxide and calcium chloride (the mass ratio of the titanium dioxide to the calcium chloride is 4: 1) under the pressure of 12MPa, placing the briquette at the other end of the vacuum reactor, and starting a vacuum pump to stabilize the air pressure in the furnace to be below 10 Pa; then opening the furnace, setting a program to enable the temperature of the furnace to rise to 1200 ℃ at a speed of 10 ℃/min, preserving the temperature for 18h at the reaction temperature so as to enable calcium steam generated by the reaction of the aluminum powder and the quicklime to fully contact with the materials, and obtaining a titanium dioxide reduction product through vacuum thermal reduction;
step 2, crushing, acid washing, filtering, drying and sieving the titanium dioxide reduction product obtained in the step 1 to obtain metal titanium powder, wherein the washing solution is 3wt% hydrochloric acid, the solid-to-liquid ratio is 1:32g/m L, the stirring speed is 300r/min during washing, the metal titanium powder is obtained after drying and sieving at 80 ℃ in a vacuum drying oven, and the crushing, acid washing, filtering, drying and sieving in the step 2 are carried out in argon atmosphere or vacuum;
and 3, turning on a power switch of the radio frequency plasma equipment, after the equipment runs stably, enabling the working power to be about 30kW, feeding the metal titanium powder obtained in the step 2 by using a feeding gun, wherein the titanium powder is carried by carrier gas and enters a high-temperature region of the plasma torch, the carrier gas flow is 10L/min, the feeding rate of the titanium powder is about 9.2g/min, the protective gas is argon, the flow is controlled to be 6L/min, and irregular titanium powder particles are rapidly melted, fall, cooled and solidified in the high-temperature region to obtain the spherical titanium powder.
While the present invention has been described in detail with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit and scope of the present invention.
Claims (6)
1. A preparation method of spherical titanium powder is characterized by comprising the following steps: comprises two main steps of thermal reduction of titanium dioxide and plasma spheroidization; the method comprises the following steps:
step 1, uniformly mixing aluminum powder and quicklime, briquetting, and placing at one end of a vacuum reactor; briquetting the mixture of titanium dioxide and calcium chloride, placing the briquetting at the other end of the vacuum reactor, and carrying out vacuum thermal reduction to obtain a titanium dioxide reduction product;
step 2, crushing, acid washing, filtering, drying and sieving the titanium dioxide reduction product obtained in the step 1 to obtain metal titanium powder;
and 3, feeding the metal titanium powder obtained in the step 2 into a plasma furnace, and carrying out spheroidization to finally obtain spherical titanium powder.
2. The method for preparing spherical titanium powder according to claim 1, characterized in that: in the step 1, the mass ratio of the aluminum powder to the quick lime is 0.35: 1-0.5: 1, and the aluminum powder and the quick lime are pressed into blocks under the pressure of 2 MPa-10 MPa.
3. The method for preparing spherical titanium powder according to claim 1, characterized in that: and (3) performing vacuum thermal reduction in the step (1), wherein the pressure is maintained to be less than 10Pa, the reduction temperature is 1100-1300 ℃, and the heat preservation time is 8-20 h.
4. The method for preparing spherical titanium powder according to claim 1, characterized in that: and (3) crushing, acid washing, filtering, drying and sieving in the step (2) are carried out in an argon atmosphere or in vacuum.
5. The method for preparing spherical titanium powder according to claim 1, characterized in that: and 3, the plasma furnace in the step 3 is a direct current plasma or radio frequency plasma furnace.
6. The method for preparing spherical titanium powder according to claim 1, wherein in the step 3, the metallic titanium powder is loaded into a plasma furnace through argon carrier gas, the working power of the plasma furnace is 20-30 kW, the flow rate of the carrier gas is controlled to be 4-10L/min, and the feeding rate of the titanium powder is 1-10 g/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113000833A (en) * | 2021-02-23 | 2021-06-22 | 郑州大学 | Ti-6Al-4V alloy spherical powder for additive manufacturing and preparation method thereof |
| CN115961151A (en) * | 2023-01-13 | 2023-04-14 | 山东建筑大学 | Zero-carbon-emission one-step process for simultaneously preparing magnesium metal and titanium metal |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009287105A (en) * | 2008-05-30 | 2009-12-10 | Hitachi Metals Ltd | Method for producing spherical titanium based powder |
| CN101628337A (en) * | 2009-08-06 | 2010-01-20 | 昆明理工大学 | Method for preparing metallic titanium powder by reducing titanium dioxide with magnesium |
| CN101716686A (en) * | 2010-01-05 | 2010-06-02 | 北京科技大学 | Short-flow preparation method of micro-sized spherical titanium powder |
| CN102921953A (en) * | 2012-10-31 | 2013-02-13 | 昆明理工大学 | Method of preparing metal titanium powder through TiO2 |
| CN106334791A (en) * | 2016-10-24 | 2017-01-18 | 贵州省钛材料研发中心有限公司 | Production method for spherical titanium powder for 3D printing |
| CN107639234A (en) * | 2017-10-10 | 2018-01-30 | 安徽工业大学 | A kind of magnesiothermic reduction TiO2The method for preparing metallic titanium powder |
| RU2681022C1 (en) * | 2018-06-26 | 2019-03-01 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский технологический университет "МИСиС" | Method for producing narrow fractional spherical powders from heat-resisting alloys based on nickel aluminide |
| CN109877343A (en) * | 2019-04-04 | 2019-06-14 | 北京工业大学 | A kind of preparation method of the high-quality sized spherical titanium powder suitable for 3D printing |
-
2020
- 2020-03-25 CN CN202010218069.7A patent/CN111421142A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009287105A (en) * | 2008-05-30 | 2009-12-10 | Hitachi Metals Ltd | Method for producing spherical titanium based powder |
| CN101628337A (en) * | 2009-08-06 | 2010-01-20 | 昆明理工大学 | Method for preparing metallic titanium powder by reducing titanium dioxide with magnesium |
| CN101716686A (en) * | 2010-01-05 | 2010-06-02 | 北京科技大学 | Short-flow preparation method of micro-sized spherical titanium powder |
| CN102921953A (en) * | 2012-10-31 | 2013-02-13 | 昆明理工大学 | Method of preparing metal titanium powder through TiO2 |
| CN106334791A (en) * | 2016-10-24 | 2017-01-18 | 贵州省钛材料研发中心有限公司 | Production method for spherical titanium powder for 3D printing |
| CN107639234A (en) * | 2017-10-10 | 2018-01-30 | 安徽工业大学 | A kind of magnesiothermic reduction TiO2The method for preparing metallic titanium powder |
| RU2681022C1 (en) * | 2018-06-26 | 2019-03-01 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский технологический университет "МИСиС" | Method for producing narrow fractional spherical powders from heat-resisting alloys based on nickel aluminide |
| CN109877343A (en) * | 2019-04-04 | 2019-06-14 | 北京工业大学 | A kind of preparation method of the high-quality sized spherical titanium powder suitable for 3D printing |
Non-Patent Citations (1)
| Title |
|---|
| 万贺利等: "钙热还原法制备钛粉过程的研究", 《功能材料》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113000833A (en) * | 2021-02-23 | 2021-06-22 | 郑州大学 | Ti-6Al-4V alloy spherical powder for additive manufacturing and preparation method thereof |
| CN115961151A (en) * | 2023-01-13 | 2023-04-14 | 山东建筑大学 | Zero-carbon-emission one-step process for simultaneously preparing magnesium metal and titanium metal |
| CN115961151B (en) * | 2023-01-13 | 2024-01-23 | 山东建筑大学 | Process for simultaneously preparing magnesium metal and titanium by one-step method with zero carbon emission |
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