CN106216702B - A kind of preparation method of spherical titanium or Titanium Powder - Google Patents
A kind of preparation method of spherical titanium or Titanium Powder Download PDFInfo
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- CN106216702B CN106216702B CN201610581521.XA CN201610581521A CN106216702B CN 106216702 B CN106216702 B CN 106216702B CN 201610581521 A CN201610581521 A CN 201610581521A CN 106216702 B CN106216702 B CN 106216702B
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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
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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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention discloses a kind of spherical titanium or the preparation methods of Titanium Powder, it is characterised in that：Using titanium silk or titanium alloy wire as raw material, spherical titanium or Titanium Powder are prepared by heat source of induction plasma.The present invention, as raw material, avoids the problem that powder raw material bring purity is not high, oxygen content is higher using Filamentous titanium silk or titanium alloy wire from source；It carries out preparing titanium or Titanium Powder as the method for heat source in conjunction with using induction plasma, obtained spherical titanium and titanium alloy powder has many advantages, such as that purity is high, sphericity height, good fluidity, oxygen content be low, narrow particle size distribution, obtained spherical titanium or the average particle size of titanium alloy powder are adjustable at 10~100 μm, pollution that whole preparation process is electrodeless.
Description
Technical field
The present invention relates to metal and alloy powder preparation fields, and in particular to the preparation side of a kind of spherical titanium or Titanium Powder
Method.
Background technique
Titanium or titanium alloy is light-high-strength metal material, and has the characteristics such as highly corrosion resistant, high-fire resistance, extensive
Be applied to the fields such as Aeronautics and Astronautics, military project, medical instrument.The micron order with good fluidity is made in titanium or titanium alloy
Spherical powder, is made that structure is complicated, the irregular component of shape using means such as injection moulding, isostatic pressings.In recent years,
Completely new PM technique --- the rise of increasing material manufacturing (3D printing) technology, spherical titanium and titanium alloy powder are answered with a kind of
It is constantly expanded with field, market capacity increases increasingly.Increases material manufacturing technology can utilize high energy according to designed data model
Metal powder is successively sintered by heating device, and the component of anticipated shape is made.Increases material manufacturing technology can be made in a short period of time
For the workpiece for going out almost arbitrary shape, particularly suitable processing precious materials and complex parts can be applied to military project emergency part and add
Work and car model production etc..High energy heating device used in increases material manufacturing technology generally uses laser sintered and electron beam
Two ways is melted, wherein laser sintered heating depth is smaller, generally uses fine powder of the particle size range at 10~45 μm；And it is electric
The sintering depth of beamlet melting is larger, and particle size range can be used for 45~106 μm of coarse powder.Due to the work of increases material manufacturing technology
Skill characteristic has higher requirement to properties such as the partial size of metal powder material, mobility, purity, oxygen contents.
Domestic preparation spherical titanium or the method for titanium alloy powder mainly have following three kinds at present：
(1) inert gas atomizer method.This method is to melt rodlike raw material in crucible, then utilizes high-speed flow will
Molten metal liquid condenses in the environment of spraying from the nozzle of crucible bottom to inert gas, obtains spherical metal powder.By
Droplet size is uneven during atomization, and the spherical metal Powder Particle Size for causing this method to prepare is wide in range, and sphericity is poor, and has
The presence of hollow bead, so that the service performance of metal powder is affected.
(2) ultrasonic atomizatio method.This method is to generate molten metal liquid in liquid level under the action of supersonic concentrator
Frequency Surface tensile wave, when amplitude reaches peak value, liquid can overcome surface tension to deviate from, and form droplet, be made after cooling
Globular metallic powder.The globular metallic powder epigranular of this method preparation, good sphericity, but to the more demanding of equipment,
It is also not overripened at present.
(3) plasma rotating electrode process.The high-temperature plasma generated using direct-current arc is as heat source by raw metal
Or comsumable melt made of alloy, it casts aside molten metal liquid to form droplet by the rotation of consutrode, then
Condensation obtains globular metallic powder.The spherical metal meal component of this method preparation is easily controllable, sphericity is preferable, but to equipment
It is more demanding, and there are certain electrode foulings.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of spherical titanium or the preparation methods of Titanium Powder, by party's legal system
Spherical titanium or titanium alloy powder have the characteristics that sphericity height, good fluidity, oxygen content be low, with high purity, narrow particle size distribution.
Spherical titanium of the present invention or the preparation method of Titanium Powder are：Using titanium silk or titanium alloy wire as raw material, with sense
Answering plasma is that heat source prepares spherical titanium or Titanium Powder.
More specifically preparation method is：Using titanium silk or titanium alloy wire as raw material, using argon gas as carrier gas, raw material is sent
Enter and vaporize melting in plasma generator, is formed by melt and generates metal droplet in the reaction chamber, form minute spherical
Titanium or Titanium Powder, collection are formed by superfine spherical titanium or Titanium Powder, after preparation process termination, the mistake under protective atmosphere
It sieves to collect the spherical titanium or Titanium Powder of required granularity；Wherein：
Carrier gas flux is 1~6slpm, and raw material rate of feed is 10~600g/min；
The parameter of plasma generator is：Power is 1~200KW, and pressure is 13.8~130.9Kpa, central gas flow
For 5~100slpm, secondary air amount is 15~150slpm, and sheath gas is the mixed gas of argon gas and hydrogen, wherein argon flow
For 20~300slpm, hydrogen flowing quantity is 1~80slpm.
Further, preparation method of the present invention specifically includes following steps：
1) it using titanium silk or titanium alloy wire as raw material, is put into feed appliance, entire preparation system is rinsed and is hunted leak；
2) it is passed through central gas and sheath gas into plasma generator, start high frequency electric source and excites plasma, then
It is passed through secondary air, gradually regulating system pressure, power and various gas flows to predetermined value；
3) start feed appliance and be passed through carrier gas, raw material is made to be sent into plasma hair under the protection of air-flow with certain rate
Melting is vaporized in raw device, melt is formed by and is dispersed as small metal droplet through gas shock in the reaction chamber, under
It is gradually cooled into superfine spherical titanium or Titanium Powder during falling, and falls into the powder collector of reaction chamber bottom, is preparing
After process terminates, it is sieved under protective atmosphere to collect the spherical titanium or Titanium Powder of required granularity.
In above-mentioned preparation method, most of micron-sized superfine spherical titanium or Titanium Powder are directly fallen under gravity
In the powder collector for entering reaction chamber bottom, a small amount of superfine spherical titanium or Titanium Powder can be taken away when detaching gas.In order to right
The superfine spherical titanium or Titanium Powder of this part are collected, and the method for the invention further includes detaching part using gas to exist
The superfine spherical titanium or Titanium Powder formed in reaction chamber is further conducted to cyclone classified room, by the part superfine spherical titanium or
Titanium Powder is collected in the powder collector of cyclone classified room bottom；And attritive powder remaining in air-flow is pulled out in working gas
When preparation system, gas solid separation room is directed to working gas and is blocked on the filter of gas solid separation room, gas is then
It is recycled through emptying after filter or after processing.After preparation process termination, by the way that the powder in 2 powder collectors is existed
It is sieved under protective atmosphere to collect the spherical titanium or Titanium Powder of required granularity.
In above-mentioned preparation method, the central gas is preferably argon gas, and the secondary air is preferably argon gas.
In preparation method of the present invention, the diameter of the titanium silk or titanium alloy wire is 0.1~6mm.
Compared with prior art, the method have the characteristics that：
1, using Filamentous titanium silk or titanium alloy wire as raw material, powder raw material bring purity is avoided from source not
Problem high, oxygen content is higher；It carries out preparing titanium or Titanium Powder, institute as the method for heat source in conjunction with using induction plasma
Spherical titanium obtained and titanium alloy powder have purity is high, sphericity height, good fluidity, the low, narrow particle size distribution of oxygen content etc. excellent
The average particle size of point, obtained spherical titanium or titanium alloy powder is adjustable at 10~100 μm, pollution that whole preparation process is electrodeless.
2, powder collector is set to reaction chamber bottom (further comprising the bottom for being set to cyclone classified room), due to reaction chamber
(or cyclone classified room) and sieving operation later are in protective atmosphere, therefore, receive powder and sieving operation is empty in isolation
It is carried out in the environment of gas, whole process avoids surface oxidation and the moisture absorption of metal-powder.
3, preparation method of the present invention is raw materials used and gas is nontoxic, and preparation process is being greater than an atmospheric pressure
In the environment of carry out, there is no cause the danger of explosion due to leaking into air.
Detailed description of the invention
Fig. 1 is high-frequency plasma equipment schematic diagram used in preparation method of the present invention；
Fig. 2 is the scanning electron microscope (SEM) photograph of sized spherical titanium powder made from the embodiment of the present invention 1；
Fig. 3 is the scanning electron microscope (SEM) photograph of spherical shape Titanium Powder made from the embodiment of the present invention 2；
Fig. 4 is the scanning electron microscope (SEM) photograph of sized spherical titanium powder made from the embodiment of the present invention 3.
Figure label is：
1 feed appliance；2 raw materials；3 central gas；4 sheath gas；5 plasma generators；6 secondary airs；7 reaction chambers；8 receive powder
Device；9 cyclone classified rooms；10 filters；11 gas outlets；12 gas solid separation rooms.
Specific embodiment
The present invention is described in further detail combined with specific embodiments below, content to better understand the invention, but
The present invention is not limited to following embodiments.
Preparation system used in the method for the invention is as shown in Figure 1, mainly include feed appliance 1, plasma generation
Device 5, reaction chamber 7, cyclone classified room 9 and gas-solid separation chamber 12 are respectively arranged with band in reaction chamber 7 and 9 bottom of cyclone classified room
The powder collector 8 of ultrasonic wave high-frequency vibration device realizes sized spherical titanium powder or Titanium Powder and collection by the two powder collectors 8.Tool
Raw material 2 is first fitted into feed appliance 1 by body when using the preparation system, and in flushing, the leak detection for completing preparation system, (operation is equal
It is same as the prior art), and be passed through central gas 3, sheath gas 4 and secondary air 6 etc. and make system debug stablize (operation with existing skill
Art is identical) after, 2 wire of raw material is sent into plasma generator 5 under the protection of carrier gas by the way of centre charging
Melting is vaporized, the plasma high-temperature area in reaction chamber 7 melts rapidly, is formed by melt and rushes in reaction chamber 7 through air-flow
Hit and be dispersed as small metal droplet, these droplets be gradually cooled into during the falling process micro-sized spherical titanium powder or
Titanium Powder, the sized spherical titanium powder or Titanium Powder of formation are fallen into the powder collector 8 of 7 bottom of reaction chamber, a small amount of sized spherical titanium powder or titanium
Alloyed powder can export to cyclone classified room 9 from reaction chamber 7 with the gas for being passed through preparation system, and whirlwind is fallen into after cyclone classified
In the powder collector 8 of 9 bottom of grading room, and attritive powder remaining in air-flow is when working gas is pulled out preparation system, with work
Gas solid separation room 12 is directed to as gas and is blocked on the filter 10 of gas solid separation room 12, and gas then penetrates filter
It empties after 10 through gas outlet 11 or is recycled after processing.After preparation process termination, by by the powder in 2 powder collectors 8
It is sieved under protective atmosphere (usually argon gas) to collect the spherical titanium or Titanium Powder of required granularity at end.
Embodiment 1
1) taking diameter is that the titanium silk of 0.2mm is fitted into feed appliance, and then preparation system is rinsed and is hunted leak with argon gas；
2) sheath gas (argon flow 30slpm, hydrogen flowing quantity 2slpm) and center are passed through into plasma generator
Gas (argon gas 8slpm), adjustment system air pressure are 27.6Kpa, open high frequency electric source and excite plasma, then pass to auxiliary gas
Flowing and adjusting uninterrupted is 25slpm, and system air pressure is gradually adjusted to 103.4Kpa, system power is adjusted to 15KW；
3) feed appliance is opened after the system stabilizes to start feed with the rate of 12g/min and be passed through carrier gas in feed appliance
(argon gas, flow 2slpm), titanium silk is sent into plasma generator under the protection of carrier gas and vaporizes melting, in plasma height
Temperature area melts rapidly, is formed by melt and is dispersed as small metal droplet through gas shock in the reaction chamber, under
Micro-sized spherical titanium powder is gradually cooled into during falling；Most of micron-sized globular metallic powder is fallen under gravity
In the powder collector for entering reaction chamber bottom, a small amount of micron particles export to whirlwind from reaction chamber with the gas for being passed through preparation system
Grading room is fallen into after cyclone classified in the powder collector of cyclone classified room bottom, and attritive powder remaining in air-flow is working
When gas is pulled out preparation system, gas solid separation room is directed to working gas and is blocked in the filter of gas solid separation room
In, gas is emptied through gas outlet after then penetrating filter or is recycled after processing；
4) after preparation process terminates, the high frequency ultrasound vibration generated using the vibration device carried in powder collector keeps powder sliding
It falls, the powder in reaction chamber bottom and cyclone classified room bottom powder collector is collected in the environment of completely cutting off air, obtains spherical titanium
Powder.Successively -325 mesh of mistake and+1340 mesh screens, acquisition main particle size range are 10~45 to gained powder under the protection of argon gas
μm sized spherical titanium powder, the average grain diameter of sized spherical titanium powder is 24.1 μm.
The microstructure of sized spherical titanium powder made from the present embodiment is analyzed, scanning electron microscope (SEM) photograph is as shown in Figure 2；And it is right
Its sphericity, tap density, mobility and oxygen content are tested, as a result as described in Table 1：
Table 1：
Embodiment 2
1) taking diameter is that the titanium alloy wire (group is divided into Ti+6wt.%Al+4wt.%V) of 2mm is fitted into feed appliance, is then used
Argon gas is rinsed and hunts leak to preparation system；
2) sheath gas (argon flow 75slpm, hydrogen flowing quantity 6slpm) and center are passed through into plasma generator
Gas (argon gas 25slpm), adjustment system air pressure are 34.5Kpa, open high frequency electric source and excite plasma, then pass to auxiliary
Air-flow simultaneously adjusts uninterrupted as 45slpm, and system air pressure is gradually adjusted to 110.2Kpa, system power is adjusted to 60KW；
3) feed appliance is opened after the system stabilizes to start feed with the rate of 50g/min and be passed through carrier gas in feed appliance
(argon gas, flow 4slpm), titanium alloy wire are sent into plasma generator under the protection of carrier gas and vaporize melting, wait from
Sub- high-temperature area melts rapidly, is formed by melt and is dispersed as small metal droplet through gas shock in the reaction chamber,
It is gradually cooled into minute spherical Titanium Powder during the falling process；Most of micron-sized globular metallic powder is in gravity
It is fallen under effect in the powder collector of reaction chamber bottom, a small amount of micron particles are led with the gas for being passed through preparation system from reaction chamber
Cyclone classified room is arrived out, is fallen into the powder collector of cyclone classified room bottom after cyclone classified, and fine powder remaining in air-flow
End is directed to gas solid separation room with working gas and is blocked in gas solid separation room when working gas is pulled out preparation system
Filter in, gas, which then penetrates, to be emptied after filter or is recycled after processing；
4) after preparation process terminates, the high frequency ultrasound vibration generated using the vibration device carried in powder collector keeps powder sliding
It falls, the powder in reaction chamber bottom and cyclone classified room bottom powder collector is collected in the environment of completely cutting off air, obtains spherical titanium
Alloy powder.Successively -150 mesh of mistake and+325 mesh screens, acquisition main particle size range are 45 to gained powder under the protection of argon gas
~106 μm of spherical Titanium Powder, the average grain diameter of sized spherical titanium powder are 71.3 μm.
The microstructure of spherical shape Titanium Powder made from the present embodiment is analyzed, scanning electron microscope (SEM) photograph is as shown in Figure 3；
And its sphericity, tap density, mobility and oxygen content are tested, as a result as shown in Table 1 above.
Embodiment 3
Embodiment 1 is repeated, unlike：
In step 1), the diameter of titanium silk is 6mm；
In step 2), the sheath gas being passed through is：Argon flow is 300slpm, hydrogen flowing quantity 80slpm；Central gas argon gas stream
Amount is 100slpm, and being passed through secondary air and adjusting uninterrupted is 100slpm, and system air pressure is gradually adjusted to 130.9Kpa,
System power is adjusted to 200KW；
In step 3), feed appliance is passed through carrier gas with the rate feed of 200g/min and into feed appliance, and (argon gas, flow are
6slpm。
In step 4), powder successively -150 mesh of mistake and+325 mesh screens under the protection of argon gas obtain main particle size range
For 45~106 μm of sized spherical titanium powder, the average grain diameter of sized spherical titanium powder is 72.5 μm.
The microstructure of spherical shape Titanium Powder made from the present embodiment is analyzed, scanning electron microscope (SEM) photograph is as shown in Figure 4；
And it is as shown in Table 1 above to its sphericity, tap density, mobility and oxygen content characterization result.
Claims (5)
1. the preparation method of a kind of spherical titanium or Titanium Powder, it is characterised in that：Using titanium silk or titanium alloy wire as raw material, with induction
Plasma is that heat source prepares spherical titanium or Titanium Powder, specific preparation method are：
Using titanium silk or titanium alloy wire as raw material, using argon gas or nitrogen as carrier gas, raw material is sent into plasma generator
Melting is vaporized, melt is formed by and generates metal droplet in the reaction chamber, form superfine spherical titanium or Titanium Powder, collect institute
The superfine spherical titanium or Titanium Powder of formation, after preparation process termination, sieving is under protective atmosphere to collect required granularity
Spherical titanium or Titanium Powder；Wherein：
Carrier gas flux is 1 ~ 6slpm, and raw material rate of feed is 10 ~ 600g/min；
The parameter of plasma generator is：
Power is 15KW, and pressure 103.4Kpa, central gas flow is 8slpm, and secondary air amount 25slpm, sheath gas is argon gas
With the mixed gas of hydrogen, wherein argon flow is 30slpm, hydrogen flowing quantity 2slpm；Either
Power is 60KW, and pressure 110.2Kpa, central gas flow is 25slpm, and secondary air amount 45slpm, sheath gas is argon
The mixed gas of gas and hydrogen, wherein argon flow is 75slpm, hydrogen flowing quantity 6slpm；Either
Power is 200KW, pressure 130.9Kpa, and central gas flow is 100slpm, secondary air amount 100slpm, and sheath gas is
The mixed gas of argon gas and hydrogen, wherein argon flow is 300slpm, hydrogen flowing quantity 80slpm.
2. preparation method according to claim 1, it is characterised in that：Include the following steps：
1）It using titanium silk or titanium alloy wire as raw material, is put into feed appliance, entire preparation system is rinsed and is hunted leak；
2）It is passed through central gas and sheath gas into plasma generator, start high frequency electric source and excites plasma, then passes to
Gas is assisted, gradually regulating system pressure, power and various gas flows to predetermined value；
3）Starting feed appliance is simultaneously passed through carrier gas, and raw material is made to be sent into plasma generator under the protection of air-flow with certain rate
Middle vaporization melting is formed by melt and is dispersed as small metal droplet through gas shock in the reaction chamber, in whereabouts
It is gradually cooled into superfine spherical titanium or Titanium Powder in the process, and falls into the powder collector of reaction chamber bottom, in preparation process
After termination, it is sieved under protective atmosphere to collect the spherical titanium or Titanium Powder of required granularity.
3. preparation method according to claim 1 or 2, it is characterised in that：The central gas is argon gas.
4. preparation method according to claim 1 or 2, it is characterised in that：The auxiliary gas is argon gas.
5. preparation method according to claim 1 or 2, it is characterised in that：The diameter of the titanium silk or titanium alloy wire is 0.1
~6mm。
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| CN108237220B (en) * | 2016-12-27 | 2020-01-14 | 中国科学院宁波材料技术与工程研究所 | Composite powder and preparation method and application thereof |
| CN107199345B (en) * | 2017-05-22 | 2019-09-13 | 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 |
| CN107150125A (en) * | 2017-06-02 | 2017-09-12 | 徐东山 | A kind of method of manufacture 3D metal powder materials |
| CN107321997A (en) * | 2017-06-29 | 2017-11-07 | 成都磁动势科技有限公司 | The processing method of magnetic |
| 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 |
| CN108436095A (en) * | 2018-03-14 | 2018-08-24 | 张格梅 | A method of preparing metal powder using high-temperature evaporation, spheroidization processing |
| CN108296489B (en) * | 2018-04-25 | 2021-04-09 | 张格梅 | Method for preparing high-temperature compound bulk crystal |
| CN111545766A (en) * | 2020-06-23 | 2020-08-18 | 柯良节 | Equipment and method for preparing high-purity spherical metal powder |
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