CN105618771A - Radio frequency plasma preparation method and device for micro spherical titanium powder - Google Patents
Radio frequency plasma preparation method and device for micro spherical titanium powder Download PDFInfo
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- CN105618771A CN105618771A CN201610061951.9A CN201610061951A CN105618771A CN 105618771 A CN105618771 A CN 105618771A CN 201610061951 A CN201610061951 A CN 201610061951A CN 105618771 A CN105618771 A CN 105618771A
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- radio frequency
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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
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
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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
Abstract
The invention discloses a radio frequency plasma preparation method and device for micro spherical titanium powder. The radio frequency plasma preparation method comprises the steps that firstly, titanium wires are used as raw materials, enter a radio frequency plasma system through a wire feeder and are subjected to high-temperature heating melting treatment; then, the titanium wires are subjected to high-pressure argon atomization treatment after being processed through the radio frequency plasma technique; and finally, the micro spherical titanium powder is prepared. According to the micro spherical titanium powder, the rate of spheroidization is higher than 85%, the grain size is 10-75 [mu]m, and the oxygen content is 600-1800 ppm. The radio frequency plasma preparation method and device for the micro spherical titanium powder have the remarkable effects that the radio frequency plasma technique and the argon atomization technique are combined, the titanium wires are rapidly heated and melted to produce titanium liquid drops through radio frequency plasma, then, atomization is conducted through high-pressure gas, and finally the micro spherical titanium powder with the low oxygen content can be obtained.
Description
Technical field
The present invention relates to a kind of method adopting radio frequency plasma technology to prepare micro-sized spherical titanium powder and preparation facilities thereof.
Background technology
Titanium alloy has the high ratio good characteristic such as strong, heat-proof corrosion-resistant good, bio-compatibility is good, is widely used in the fields such as Aero-Space, automobile, medical treatment, sports goods. When preparing complex-shaped titanium alloy component, it is the most competitive method that near-net-shape technology (increases material manufacture, injection moulding), and these forming parts technology are greatly improved stock utilization, decrease part manufacturing cycle. But these technology require that raw material powder particle size is little, oxygen content is low, good fluidity. Owing to titanium is high activity refractory metal, very easily contaminated and oxidation time prepared by titanium valve, common milling method is difficult to prepare the micro-sized spherical titanium powder of low oxygen content, and it is critically important for therefore providing a kind of method preparing micro-sized spherical titanium powder.
Prepare at present the method for spherical metal titanium powder mainly have electrode induction melting aerosolization method (EIGA), plasmatorch aerosolization method, plasma rotating electrode process (PREP), be raw material with HDH powder Radio frequency plasma etc. Induction melting aerosolization method fine powder recovery rate is low, have trickle cavity in powder. It is difficult to control to the Radio frequency plasma material powder oxygen content that HDH powder is raw material. Plasma (orifice) gas atomization adopts DC arc plasmatorch, but the major defect of DC arc plasma method is its electrode erosion, introduces impurity, and electrode must be changed in timing, affects the continuous and steady operation of device systems. Plasma rotating electrode process is difficult to obtain thin sized spherical titanium powder.
Disadvantage mentioned above is overcome with radio frequency (RF) the plasma atomization rule that titanium silk is raw material. Yet there are no report.
Summary of the invention
In view of prior art exists drawbacks described above, it is an object of the invention to provide the radio frequency plasma preparation method of micro-sized spherical titanium powder and device.
The purpose of the present invention, will be achieved by the following technical programs:
The radio frequency plasma preparation method of micro-sized spherical titanium powder, comprises the steps,
S1, with titanium silk for raw material, by wire-feed motor enter plasma high-temperature region, adopt radio frequency plasma technology titanium silk is carried out high-temperature heating thawing process, described radio frequency plasma technology keep work system be evacuated to 1X10-3Carry out after pouring argon under pa; And described system maintains slip less than 1pa/h;
S2, titanium silk after radio frequency plasma technical finesse process then through high pressure argon gas atomization;
S3, finally prepared micro-sized spherical titanium powder, the Oxygen potential of described micro-sized spherical titanium powder is more than 85%, and granularity is 10��75um, and oxygen content is at 600��1800ppm.
Preferably, in described S1, the wire feed rate of wire-feed motor is 25cm/min��200cm/min.
Preferably, in described S1, radio frequency plasma technological parameter is: power 30��100KW, and work argon flow amount 1��5m3/ h, pressure 0.1��0.5MPa, shield gas flow rate 3��10m3/ h, pressure 0.1��0.5MPa; System pressure 50��80KPa.
Preferably, in described S2 step, the argon pressure of atomization is 1��50MPa, and flow is 30��500m3/h��
Preferably, the diameter of described titanium silk is 0.5��10mm, and described titanium silk carried out removing ultrasonic oil removing before entering wire-feed motor and cleans.
Preferably, device prepared by the described radio frequency plasma for micro-sized spherical titanium powder, including,
Wire-feed motor, for being sent into next program by titanium silk raw material;
Radio frequency plasma system, for titanium silk is carried out plasma high-temperature heating thawing, the described arrival end of radio frequency plasma system is connected with the discharge end of wire-feed motor;
Reative cell, for the nodularization of titanium silk, the arrival end of described reative cell is provided with atomization system, and the arrival end of described atomization system is connected with the port of export of radio frequency plasma system; It is provided with gas powder filter in described reative cell, and described reative cell is provided with the gas pipeline for discharging gas.
Preferably, being provided with plasma gun in described plasma system, described plasma gun top is provided with dynamic sealing device.
Preferably, described device also includes the powder collecting tank that is arranged at reative cell lower end for collecting titanium valve.
The prominent effect of the present invention is: combined by gentle for radio frequency plasma technology atomization technique, utilizes the quick heating and melting titanium silk of radio frequency plasma to produce titanium drop, recycling gases at high pressure atomization, finally can obtain low oxygen content micro-sized spherical titanium powder.
Hereinafter just accompanying drawing in conjunction with the embodiments, is described in further detail the specific embodiment of the present invention, so that technical solution of the present invention is more readily understood, grasps.
Accompanying drawing explanation
Fig. 1 is the structural representation of the present invention.
Detailed description of the invention
Present invention is disclosed a kind of device prepared for the radio frequency plasma of micro-sized spherical titanium powder, as it is shown in figure 1, include,
Wire-feed motor 2, for being sent into next program by raw material titanium silk 1; The diameter of general described titanium silk is 0.5-10mm.
Radio frequency plasma system 3, for carrying out plasma high-temperature heating thawing by titanium silk 1; The arrival end of described radio frequency plasma system is connected with the discharge end of wire-feed motor 2; Being provided with plasma gun in described plasma system, described plasma gun top is provided with dynamic sealing device.
Reative cell 5, for the nodularization of titanium silk, the arrival end of described reative cell 5 is provided with atomization system 4, and the arrival end of described atomization system 4 is connected with the port of export of radio frequency plasma system 3; It is provided with gas powder filter in described reative cell 5, and described reative cell 5 is provided with the gas pipeline 6 for discharging gas. Ring-type aerosolization nozzle it is provided with in described atomization system 4.
Described reative cell 5 lower end is additionally provided with the powder collecting tank (meaning not shown in the figures) for collecting titanium valve.
Apparatus above can be used for the preparation of the refractory metal powder such as tungsten, molybdenum, tantalum, niobium.
The method adopting apparatus above to prepare micro-sized spherical titanium powder, comprises the steps,
S1, with titanium silk for raw material, by wire-feed motor enter plasma high-temperature region, adopt radio frequency plasma technology titanium silk is carried out high-temperature heating thawing process, described radio frequency plasma technology keep work system be evacuated to 1X10-3Carry out after pouring argon under pa; And described system maintains slip less than 1pa/h;
S2, titanium silk after radio frequency plasma technical finesse process then through high pressure argon gas atomization;
S3, finally prepared micro-sized spherical titanium powder, the Oxygen potential of described micro-sized spherical titanium powder is more than 85%, and granularity is 10-75um, and oxygen content is at 600-1800ppm.
In described S1, the wire feed rate of wire-feed motor is 25cm/min 200cm/min.
In described S1, radio frequency plasma technological parameter is: power 30-100KW, and work argon flow amount 1-5m3/ h, pressure 0.1��0.5MPa, shield gas flow rate 3-10m3/ h, pressure 0.1��0.5MPa, system pressure 50-80KPa.
In described S2 step, the argon pressure of atomization is 1-50MPa, and flow is 30-500m3/h��
It is the enforcement step that example describes the present invention in detail below in conjunction with specifically preparing the oxygen content spherical TC4 titanium valve less than 1000ppm, particle mean size 30um:
Selecting oxygen content 800ppm, string diameter 2mm's to coil TC4 titanium silk, for ensureing the cleaning of last titanium valve, described raw material titanium silk requires that doing ultrasonic oil removing cleans. Generally, raw material titanium silk oxygen content is lower than the requirement of finished product oxygen content in power all can realize final requirement.
Charging tray is loaded in fuse mechanism, draws silk in plasma gun by wire feeder. Whole system is evacuated to 1X10-3Pa, is re-filled with high-purity argon gas.
Open water ring pump and be evacuated to 30KP; igniting, regulates and sets up stable radio frequency plasma, and its main technologic parameters is: power 60KW; work argon flow amount 2 side/hour; pressure 0.2Pa, shield gas flow rate 5 side/hour, pressure 0.2Pa; keep system pressure 70KPa; unlatching high pressure argon gas is atomized, and the pressure of atomization is 40bar, and flow is 20m3/h��
Starting wire feed, wire feed rate is 100cm/min, and being obtained by reacting titanium or titanium alloy sphere of powder rate is 90%, and titanium valve granularity D50 is 38um, and oxygen content is at 1200ppm.
Owing to the titanium silk raw material of low oxygen content is easier to obtain; radio frequency plasma heating is quick and clean pollution-free; titanium silk can obtain little initial liquid drop after melting; the micro-sized spherical titanium powder that granularity is controlled can be obtained again through high pressure argon gas atomization; the control of described granularity can pass through plasma work parameter (power, work argon flow amount and pressure, shield gas flow rate and pressure, system pressure), atomization parameter (pressure and flow) and wire feed rate, and string diameter specifically controls. Method cost is low, oxygen content is low for this, Oxygen potential is high, good sphericity, and the sized spherical titanium powder of production can meet the requirement increasing material manufacture and injection molding technology.
Apparatus and method of the present invention produces titanium or titanium alloy powder when can realize fine vacuum, continuous industry, meets the field market demands to high-performance titanium and titanium alloy powder such as 3D printing technique, MIM, hot isostatic pressing technique, plasma spray technology and conventional powder metallurgy.
The present invention still has numerous embodiments, all employing equivalents or equivalent transformation and all technical schemes of being formed, all falls within protection scope of the present invention.
Claims (8)
1. the radio frequency plasma preparation method of micro-sized spherical titanium powder, it is characterised in that: comprise the steps,
S1, with titanium silk for raw material, by wire-feed motor enter plasma high-temperature region, adopt radio frequency plasma technology titanium silk is carried out high-temperature heating thawing process, described radio frequency plasma technology keep work system be evacuated to 1X10-3Carry out after pouring argon under pa; And described system maintains slip less than 1pa/h;
S2, titanium silk after radio frequency plasma technical finesse process then through high pressure argon gas atomization;
S3, finally prepared micro-sized spherical titanium powder, the Oxygen potential of described micro-sized spherical titanium powder is more than 85%, and granularity is 10��75um, and oxygen content is at 600��1800ppm.
2. the radio frequency plasma preparation method of micro-sized spherical titanium powder according to claim 1, it is characterised in that: in described S1, the wire feed rate of wire-feed motor is 25cm/min��200cm/min.
3. the radio frequency plasma preparation method of micro-sized spherical titanium powder according to claim 1, it is characterised in that: in described S1, radio frequency plasma technological parameter is: power 30��100KW, and work argon flow amount 1��5m3/ h, pressure 0.1��0.5MPa; Shield gas flow rate 3��10m3/ h, pressure 0.1��0.5MPa; System pressure 50��80KPa.
4. the radio frequency plasma preparation method of micro-sized spherical titanium powder according to claim 1, it is characterised in that: in described S2 step, the argon pressure of atomization is 1��50MPa, and flow is 30��500m3/h��
5. the radio frequency plasma preparation method of micro-sized spherical titanium powder according to claim 1, it is characterised in that: the diameter of described titanium silk is 0.5��10mm, and described titanium silk carried out removing ultrasonic oil removing before entering wire-feed motor and cleans.
6. the device prepared for the radio frequency plasma of micro-sized spherical titanium powder as claimed in claim 1, it is characterised in that: include,
Wire-feed motor, for being sent into next program by titanium silk raw material;
Radio frequency plasma system, for titanium silk is carried out plasma high-temperature heating thawing, the described arrival end of radio frequency plasma system is connected with the discharge end of wire-feed motor;
Reative cell, for the nodularization of titanium silk, the arrival end of described reative cell is provided with atomization system, and the arrival end of described atomization system is connected with the port of export of radio frequency plasma system; It is provided with gas powder filter in described reative cell, and described reative cell is provided with the gas pipeline for discharging gas.
7. the device prepared for the radio frequency plasma of micro-sized spherical titanium powder as claimed in claim 6, it is characterised in that: being provided with plasma gun in described plasma system, described plasma gun top is provided with dynamic sealing device.
8. the device prepared for the radio frequency plasma of micro-sized spherical titanium powder as claimed in claim 6, it is characterised in that: described device also includes the powder collecting tank being arranged at reative cell lower end for collecting titanium valve.
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Cited By (13)
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CN106166617A (en) * | 2016-09-27 | 2016-11-30 | 中航迈特粉冶科技(北京)有限公司 | A kind of preparation method of 3D printing titanium alloy powder |
CN106363187A (en) * | 2016-09-27 | 2017-02-01 | 中航迈特粉冶科技(北京)有限公司 | Preparation method of high-temperature alloy powder for 3D printing |
CN107030291A (en) * | 2017-06-02 | 2017-08-11 | 徐东山 | A kind of device for being used to manufacture 3D metal powder materials |
CN107150125A (en) * | 2017-06-02 | 2017-09-12 | 徐东山 | A kind of method of manufacture 3D metal powder materials |
CN107199345A (en) * | 2017-05-22 | 2017-09-26 | 加拿大艾浦莱斯有限公司 | A kind of high-purity superfine spherical titanium powder, preparation method thereof and its device |
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CN107030291A (en) * | 2017-06-02 | 2017-08-11 | 徐东山 | A kind of device for being used to manufacture 3D metal powder materials |
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CN107790735A (en) * | 2017-11-01 | 2018-03-13 | 攀钢集团攀枝花钢铁研究院有限公司 | The method that radio frequency plasma smelting system prepares the spherical Titanium Powder of 3D printing |
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CN108580913A (en) * | 2018-07-10 | 2018-09-28 | 深圳微纳增材技术有限公司 | A kind of 3D printing noble metal powder preparation method |
CN109482894A (en) * | 2019-01-08 | 2019-03-19 | 成都先进金属材料产业技术研究院有限公司 | The method of direct current plasma atomization preparation 3D printing spherical titanium and Titanium Powder |
CN113880463A (en) * | 2021-11-04 | 2022-01-04 | 福州大学 | Method for producing magnesium oxide for magnesium phosphate cement by radio frequency plasma technology |
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