CN106216702A - A kind of spherical titanium or the preparation method of Titanium Powder - Google Patents
A kind of spherical titanium or the preparation method of Titanium Powder Download PDFInfo
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- CN106216702A CN106216702A CN201610581521.XA CN201610581521A CN106216702A CN 106216702 A CN106216702 A CN 106216702A CN 201610581521 A CN201610581521 A CN 201610581521A CN 106216702 A CN106216702 A CN 106216702A
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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 the preparation method of a kind of spherical titanium or Titanium Powder, it is characterised in that: with titanium silk or titanium alloy wire as raw material, prepare spherical titanium or Titanium Powder with induction plasma for thermal source.The present invention uses thread titanium silk or titanium alloy wire as raw material, the problem that the purity avoiding powder raw material to bring from source is the highest, oxygen content is higher；It is prepared titanium or Titanium Powder in conjunction with using the induction plasma method as thermal source, obtained spherical titanium and titanium alloy powder have the advantages such as purity height, sphericity height, good fluidity, low, the narrow particle size distribution of oxygen content, the particle mean size of obtained spherical titanium or titanium alloy powder is adjustable in 10～100 μm, pollution that whole preparation process is electrodeless.
Description
Technical field
The present invention relates to metal and alloy powder preparation field, be specifically related to a kind of spherical titanium or the preparation side of Titanium Powder
Method.
Background technology
Titanium or titanium alloy is light-high-strength metal material, and possesses the characteristic such as highly corrosion resistant, high-fire resistance, by extensively
Be applied to the fields such as Aeronautics and Astronautics, military project, medical apparatus and instruments.Titanium or titanium alloy is made the micron order with good fluidity
Spherical powder, the available means such as injection moulding, isostatic pressing make structure complexity, the irregular component of profile.In recent years,
Answer along with a kind of brand-new PM technique increases the rise of material manufacture (3D printing) technology, spherical titanium and titanium alloy powder
Constantly expanding with field, market capacity increases increasingly.Increase material manufacturing technology and can utilize high energy according to the data model designed
Metal powder is successively sintered by heater, makes the component of anticipated shape.Increase material manufacturing technology can make in a short period of time
Standby go out almost arbitrary shape workpiece, particularly suitable processing precious materials and complex parts, can be applicable to military project part of meeting an urgent need and add
The aspects such as work and car model making.Increase the high energy heater used by material manufacturing technology and typically use laser sintered and electron beam
Melted two ways, the most laser sintered heating depth is less, generally uses the particle size range fine powder in 10～45 μm；And it is electric
The sintering depth that son bundle melts is relatively big, the coarse powder that particle size range can be used to be 45～106 μm.Owing to increasing the work of material manufacturing technology
Skill characteristic, has had higher requirement to character such as the particle diameter of metal powder material, mobility, purity, oxygen contents.
The method of current domestic preparation spherical titanium or titanium alloy powder mainly has following three kinds:
(1) inert gas atomizer method.The method is to be melted in crucible by bar-shaped raw material, then utilizes high velocity air to incite somebody to action
Melted molten metal sprays from the nozzle of crucible bottom and condenses to noble gas, obtains spherical metal dust.By
During atomization, droplet size is uneven, and the spherical metal Powder Particle Size causing the method to be prepared is wide in range, and sphericity is poor, and has
The existence of hollow bead so that the serviceability of metal dust is affected.
(2) ultrasonic atomizatio method.The method is to be produced at liquid level under the effect of supersonic concentrator by melted metal liquid
Frequency Surface tensile wave, when amplitude reaches peak value, liquid can overcome surface tension to deviate from, and forms droplet, prepares after cooling
Globular metallic powder.Globular metallic powder epigranular prepared by the method, good sphericity, but the requirement to equipment is higher,
The most overripened.
(3) plasma rotating electrode process.Utilize high-temperature plasma that direct-current arc produces as thermal source by feed metal
Or the comsumable melt that alloy is made, cast molten metal liquid aside formation droplet by the rotation of consutrode, then
Condensation obtains globular metallic powder.Spherical metal meal component prepared by the method is easily controllable, sphericity preferable, but to equipment
Require higher, and there is certain electrode fouling.
Summary of the invention
The technical problem to be solved in the present invention is to provide the preparation method of a kind of spherical titanium or Titanium Powder, by the party's legal system
The spherical titanium or the titanium alloy powder that obtain have the features such as sphericity height, good fluidity, oxygen content is low, purity is high, narrow particle size distribution.
The preparation method of spherical titanium of the present invention or Titanium Powder is: with titanium silk or titanium alloy wire as raw material, with sense
Answering plasma is that thermal source prepares spherical titanium or Titanium Powder.
More specifically preparation method is: with titanium silk or titanium alloy wire as raw material, uses argon as carrier gas, is sent by raw material
Entering vaporization melting in plasma generator, the melt formed generates metal droplet in the reaction chamber, forms minute spherical
Titanium or Titanium Powder, collect the superfine spherical titanium or Titanium Powder formed, after preparation process terminates, mistake under protective atmosphere
Sieve the spherical titanium to collect desired particle size 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 1～200KW, and pressure is 13.8～130.9Kpa, central gas flow
Being 5～100slpm, secondary air amount is 15～150slpm, and sheath gas is the mixed gas of argon and hydrogen, wherein argon flow amount
Being 20～300slpm, hydrogen flowing quantity is 1～80slpm.
Further, preparation method of the present invention specifically includes following steps:
1) with titanium silk or titanium alloy wire as raw material, put in feed appliance, whole preparation system is rinsed and hunts leak；
2) in plasma generator, it is passed through central gas and sheath gas, starts high frequency electric source and excite plasma, then
It is passed through secondary air, progressively regulates system pressure, power and various gas flow to predetermined value；
3) start feed appliance and be passed through carrier gas, making raw material send into plasma with certain speed under the protection of air-flow and send out
Vaporizing melting in raw device, the melt formed is dispersed as small metal droplet through gas shock in the reaction chamber, under
Gradually it is cooled into superfine spherical titanium or Titanium Powder during falling, and falls in the powder collector bottom reative cell, in preparation
After process terminates, sieve to collect the spherical titanium of desired particle size or Titanium Powder under protective atmosphere.
In above-mentioned preparation method, most of micron-sized superfine spherical titanium or Titanium Powder the most directly fall
Enter in the powder collector bottom reative cell, a small amount of superfine spherical titanium or Titanium Powder can be taken away when being detached by gas.In order to right
Superfine spherical titanium or the Titanium Powder of this part are collected, and the method for the invention also includes that utilizing gas to detach part exists
The superfine spherical titanium or the Titanium Powder that are formed in reative cell are further conducted to cyclone classified room, by this part superfine spherical titanium or
Titanium Powder is collected in the powder collector bottom cyclone classified room；And attritive powder remaining in air-flow is pulled out at working gas
During preparation system, being directed to gas solid separation room with working gas and be blocked on the filter of gas solid separation room, gas is then
Through emptying after filter or recycle after treatment.After preparation process terminates, by the powder in 2 powder collectors is existed
Sieve to collect spherical titanium or the Titanium Powder of desired particle size under protective atmosphere.
In above-mentioned preparation method, described central gas is preferably argon, and described secondary air is preferably argon.
In preparation method of the present invention, described titanium silk or a diameter of the 0.1 of titanium alloy wire～6mm.
Compared with prior art, present invention is characterized in that
1, use thread titanium silk or titanium alloy wire as raw material, from source, avoid the purity that powder raw material brings not
Problem high, that oxygen content is higher；It is prepared titanium or Titanium Powder, institute in conjunction with using the induction plasma method as thermal source
It is excellent that the spherical titanium prepared and titanium alloy powder have purity height, sphericity height, good fluidity, low, the narrow particle size distribution of oxygen content etc.
Point, the particle mean size of obtained spherical titanium or titanium alloy powder is adjustable in 10～100 μm, pollution that whole preparation process is electrodeless.
2, powder collector is arranged at bottom reative cell and (farther includes to be arranged at the bottom of cyclone classified room), due to reative cell
(or cyclone classified room) and operation of sieving afterwards are in protective atmosphere, therefore, receive powder and operation of sieving all at isolation sky
Carrying 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 more than an atmospheric pressure
In the environment of carry out, there is not the danger causing blast owing to leaking into air.
Accompanying drawing explanation
Fig. 1 is the high-frequency plasma equipment schematic diagram used in preparation method of the present invention；
Fig. 2 is the scanning electron microscope (SEM) photograph of the sized spherical titanium powder that the embodiment of the present invention 1 prepares；
Fig. 3 is the scanning electron microscope (SEM) photograph of the spherical titanium alloyed powder that the embodiment of the present invention 2 prepares；
Fig. 4 is the scanning electron microscope (SEM) photograph of the sized spherical titanium powder that the embodiment of the present invention 3 prepares.
Figure is numbered:
1 feed appliance；2 raw materials；3 central gas；4 sheath gas；5 plasma generators；6 secondary airs；7 reative cells；8 receive powder
Device；9 cyclone classified rooms；10 filters；11 gas outlets；12 gas solid separation rooms.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, to be more fully understood that present disclosure, but
The present invention is not limited to following example.
The preparation system used in the method for the invention is as it is shown in figure 1, mainly include that feed appliance 1, plasma occur
Device 5, reative cell 7, cyclone classified room 9 and gas-solid separation chamber 12, be respectively arranged with band bottom reative cell 7 and cyclone classified room 9
The powder collector 8 of ultrasound wave high-frequency vibration device, realizes sized spherical titanium powder or Titanium Powder and collection by the two powder collector 8.Tool
Raw material 2, when using this preparation system, is first loaded in feed appliance 1 by body, and completing the flushing of preparation system, (operation is all in leak detection
Same as the prior art), and be passed through central gas 3, sheath gas 4 and secondary air 6 etc. make system debug stable (operation all with existing skill
Art is identical) after, use the mode of centre charging to be sent in plasma generator 5 under the protection of carrier gas by raw material 2 tinsel
Vaporization melting, the plasma high-temperature area in reative cell 7 melts rapidly, and the melt formed rushes through air-flow in reative cell 7
Hit and be dispersed as small metal droplet, these droplets fall during be gradually cooled into micro-sized spherical titanium powder or
Titanium Powder, the sized spherical titanium powder of formation or Titanium Powder fall in the powder collector 8 bottom reative cell 7, a small amount of sized spherical titanium powder or titanium
Alloyed powder can export to cyclone classified room 9 along with the gas being passed through preparation system from reative cell 7, falls into whirlwind after cyclone classified
In powder collector 8 bottom grading room 9, and attritive powder remaining in air-flow is when working gas is pulled out preparation system, with work
Being directed to gas solid separation room 12 as gas and be blocked on the filter 10 of gas solid separation room 12, gas is then through filter
Empty through gas outlet 11 or recycle after treatment after 10.After preparation process terminates, by by the powder in 2 powder collectors 8
End sieves to collect the spherical titanium of desired particle size or Titanium Powder under protective atmosphere (usually argon).
Embodiment 1
1) the titanium silk taking a diameter of 0.2mm loads in feed appliance, is then rinsed preparation system with argon and hunts leak；
2) in plasma generator, it is passed through sheath gas (argon flow amount is 30slpm, and hydrogen flowing quantity is 2slpm) and center
Gas (argon 8slpm), adjusting system air pressure is 27.6Kpa, opens high frequency electric source and excites plasma, then passes to assist gas
Flowing and adjusting uninterrupted is 25slpm, progressively by system air pressure adjustment to 103.4Kpa, system power is adjusted to 15KW；
3) after system stability, open feed appliance start feed with the speed of 12g/min and in feed appliance, be passed through carrier gas
(argon, flow is 2slpm), vaporization melting in plasma generator sent under the protection of carrier gas by titanium silk, high at plasma
Temperature area melts rapidly, and the melt formed is dispersed as small metal droplet through gas shock in the reaction chamber, under
Micro-sized spherical titanium powder gradually it is cooled into during falling；The micron-sized globular metallic powder of major part falls under gravity
Entering in the powder collector bottom reative cell, a small amount of micron particles exports to whirlwind along with the gas being passed through preparation system from reative cell
Grading room, falls in the powder collector bottom cyclone classified room after cyclone classified, and attritive powder remaining in air-flow is in work
When gas is pulled out preparation system, it is directed to gas solid separation room with working gas and is blocked in the filter of gas solid separation room
In, gas then or recycles through gas outlet emptying after treatment through after filter；
4), after preparation process terminates, the high frequency ultrasound vibration utilizing the vibrating device carried in powder collector to produce makes powder sliding
Fall, the powder collected bottom bottom reative cell and cyclone classified room in powder collector in the environment of isolation air, obtain spherical titanium
Powder.Gained powder mistake-325 mesh and+1340 eye mesh screens successively under the protection of argon, it is thus achieved that main particle size scope is 10～45
The sized spherical titanium powder of μm, the mean diameter of sized spherical titanium powder is 24.1 μm.
Being analyzed the microstructure of the sized spherical titanium powder that the present embodiment prepares, its 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, result as described in Table 1:
Table 1:
Embodiment 2
1) titanium alloy wire (component is Ti+6wt.%Al+4wt.%V) taking a diameter of 2mm loads in feed appliance, then uses
Preparation system is rinsed and hunts leak by argon；
2) in plasma generator, it is passed through sheath gas (argon flow amount is 75slpm, and hydrogen flowing quantity is 6slpm) and center
Gas (argon 25slpm), adjusting system air pressure is 34.5Kpa, opens high frequency electric source and excites plasma, then passes to auxiliary
Air-flow to adjust uninterrupted be 45slpm, progressively by system air pressure adjustment to 110.2Kpa, is adjusted to 60KW by system power；
3) after system stability, open feed appliance start feed with the speed of 50g/min and in feed appliance, be passed through carrier gas
(argon, flow is 4slpm), titanium alloy wire sends in plasma generator vaporization melting under the protection of carrier gas, wait from
Sub-high-temperature area melts rapidly, and the melt formed is dispersed as small metal droplet through gas shock in the reaction chamber,
Minute spherical Titanium Powder gradually it is cooled into during falling；The micron-sized globular metallic powder of major part is at gravity
Effect falls in the powder collector bottom reative cell, and a small amount of micron particles is led from reative cell along with the gas being passed through preparation system
Go out to cyclone classified room, fall into after cyclone classified in powder collector bottom cyclone classified room, and fine powder remaining in air-flow
End, when working gas is pulled out preparation system, is directed to gas solid separation room with working gas and is blocked in gas solid separation room
Filter in, gas then through emptying after filter or recycles after treatment；
4), after preparation process terminates, the high frequency ultrasound vibration utilizing the vibrating device carried in powder collector to produce makes powder sliding
Fall, the powder collected bottom bottom reative cell and cyclone classified room in powder collector in the environment of isolation air, obtain spherical titanium
Alloy powder.Gained powder mistake-150 mesh and+325 eye mesh screens successively under the protection of argon, it is thus achieved that main particle size scope is 45
～106 spherical titanium alloyed powders of μm, the mean diameter of sized spherical titanium powder is 71.3 μm.
Being analyzed the microstructure of the spherical titanium alloyed powder that the present embodiment prepares, its scanning electron microscope (SEM) photograph is as shown in Figure 3；
And its sphericity, tap density, mobility and oxygen content are tested, result is as shown in Table 1 above.
Embodiment 3
Repeat embodiment 1, except for the difference that:
Step 1) in, a diameter of 6mm of titanium silk；
Step 2) in, the sheath gas being passed through is: argon flow amount is 300slpm, and hydrogen flowing quantity is 80slpm；Central gas argon stream
Amount for 100slpm, is passed through secondary air and to adjust uninterrupted is 100slpm, progressively by system air pressure adjustment to 130.9Kpa,
System power is adjusted to 200KW；
Step 3) in, feed appliance is with the speed feed of 200g/min and be passed through carrier gas in feed appliance (argon, flow is
6slpm。
Step 4) in, powder mistake-150 mesh and+325 eye mesh screens successively under the protection of argon, it is thus achieved that main particle size scope
Being the sized spherical titanium powder of 45～106 μm, the mean diameter of sized spherical titanium powder is 72.5 μm.
Being analyzed the microstructure of the spherical titanium alloyed powder that the present embodiment prepares, its scanning electron microscope (SEM) photograph is as shown in Figure 4；
And to its sphericity, tap density, mobility and oxygen content characterization result as shown in Table 1 above.
Claims (7)
1. a spherical titanium or the preparation method of Titanium Powder, it is characterised in that: with titanium silk or titanium alloy wire as raw material, with sensing
Plasma is that thermal source prepares spherical titanium or Titanium Powder.
Preparation method the most according to claim 1, it is characterised in that: with titanium silk or titanium alloy wire as raw material, use argon
Or nitrogen is as carrier gas, raw material being sent into vaporization melting in plasma generator, the melt formed generates in the reaction chamber
Metal droplet, forms superfine spherical titanium or Titanium Powder, collects the superfine spherical titanium or Titanium Powder formed, was preparing
After journey terminates, sieve to collect the spherical titanium of desired particle size or Titanium Powder under protective atmosphere；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, and central gas flow is 5
～100slpm, secondary air amount is 15～150slpm, and sheath gas is the mixed gas of argon and hydrogen, and wherein argon flow amount is 20
～300slpm, hydrogen flowing quantity is 1～80slpm.
Preparation method the most according to claim 2, it is characterised in that: comprise the following steps:
1) with titanium silk or titanium alloy wire as raw material, put in feed appliance, whole preparation system is rinsed and hunts leak；
2) in plasma generator, it is passed through central gas and sheath gas, starts high frequency electric source and excite plasma, then passing to
Secondary air, progressively regulates system pressure, power and various gas flow to predetermined value；
3) start feed appliance and be passed through carrier gas, making raw material send into plasma generator with certain speed under the protection of air-flow
Middle vaporization melting, the melt formed is dispersed as small metal droplet through gas shock in the reaction chamber, fall
During be gradually cooled into superfine spherical titanium or Titanium Powder, and fall in the powder collector bottom reative cell, in preparation process
After termination, sieve to collect the spherical titanium of desired particle size or Titanium Powder under protective atmosphere.
4. according to the preparation method described in Claims 2 or 3, it is characterised in that: the superfine spherical titanium of formation or Titanium Powder portion
Divide and be imported into cyclone classified room, to collect pressed powder.
5. according to the preparation method described in Claims 2 or 3, it is characterised in that: described central gas is argon.
6. according to the preparation method described in Claims 2 or 3, it is characterised in that: described secondary air is argon.
7. according to the preparation method according to any one of claims 1 to 3, it is characterised in that: described titanium silk or titanium alloy wire
A diameter of 0.1～6mm.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN108237220A (en) * | 2016-12-27 | 2018-07-03 | 中国科学院宁波材料技术与工程研究所 | A kind of composite powder and its preparation method and application |
| CN108296489A (en) * | 2018-04-25 | 2018-07-20 | 张格梅 | A method of it is brilliant to prepare high temperature compound block |
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| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108237220A (en) * | 2016-12-27 | 2018-07-03 | 中国科学院宁波材料技术与工程研究所 | A kind of composite powder and its preparation method and application |
| 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 |
| 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 |
| CN108296489A (en) * | 2018-04-25 | 2018-07-20 | 张格梅 | A method of it is brilliant to prepare high temperature compound block |
| 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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