CN106378460B - Prepare the plasma atomization method and equipment of spherical pure titanium or titanium alloy powder - Google Patents

Prepare the plasma atomization method and equipment of spherical pure titanium or titanium alloy powder Download PDF

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CN106378460B
CN106378460B CN201610841237.1A CN201610841237A CN106378460B CN 106378460 B CN106378460 B CN 106378460B CN 201610841237 A CN201610841237 A CN 201610841237A CN 106378460 B CN106378460 B CN 106378460B
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titanium
atomization
plasma
titanium alloy
powder
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CN106378460A (en
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刘睿诚
吴利苹
蒋安琪
曾益伟
王强
陈玲莉
陈军
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Chengdu Excellent Technology Co Ltd
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Chengdu Excellent Technology Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making 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
    • B22F9/082Making 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 atomising using a fluid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making 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
    • B22F9/082Making 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 atomising using a fluid
    • B22F2009/0844Making 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 atomising using a fluid in controlled atmosphere
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making 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
    • B22F9/082Making 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 atomising using a fluid
    • B22F2009/086Cooling after atomisation
    • B22F2009/0876Cooling after atomisation by gas

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  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)

Abstract

The present invention relates to the plasma atomization method and equipment for preparing pure titanium or titanium alloy spherical powder, belong to the preparing technical field of titanium or titanium alloy powder.The present invention provides a kind of plasma atomization method for preparing pure titanium or titanium alloy powder, includes the following steps:A, the titanium silk or titanium alloy wire of a diameter of 3~20mm is prepared;B, in the atomization storehouse of argon atmosphere, using plasma torch by titanium silk or titanium alloy wire atomized molten, it is atomized after pure titanium or titanium alloy particle;C, the argon gas stream that temperature is 300~500 DEG C is passed through into atomization storehouse, by pure titanium or the titanium alloy particle section cooling after atomization, obtains pure titanium or titanium alloy powder.The powder good sphericity, satellite ball is few, have the advantages that particle diameter distribution uniformly, high-purity, high spherical, good fluidity, low oxygen content, be mingled with less, non-binding/agglomeration.The titanium valve prepared can be widely used in the molding modes such as metal increasing material manufacturing, powder injection-molded and high temperature insostatic pressing (HIP), for manufacturing high-precision part.

Description

Prepare the plasma atomization method and equipment of spherical pure titanium or titanium alloy powder
Technical field
The present invention relates to the plasma atomization method and equipment for preparing spherical pure titanium or titanium alloy powder, belongs to titanium or titanium closes The preparing technical field at bronze end.
Background technology
Pure titanium and titanium alloy are because density is low, and specific strength is high, corrosion resistance, good mechanical property, and biocompatibility is excellent, It is widely used in aerospace manufacture, dentistry processing and orthopaedics implantation processing and other fields.But the processability of titanium alloy Difference, machining is difficult, in hot-working, is very easy to absorb the impurity such as hydrogen-oxygen nitrogen carbon, wear resistence is poor, complex production process. Therefore the powder metallurgy mode such as metal 3D printing, powder injection-molded, high temperature insostatic pressing (HIP) is to prepare high-precision part in these fields Most popular method, but these preparation methods need high spherical titanium valve, conventional Mechanical Crushing, chemical gaseous phase the methods of system Standby titanium valve can not meet its rigors.
Pure titanium and titanium alloy are because fusing point is high, and chemism is strong under high temperature, can react, make with crucible under molten condition Chemical purity is affected;It can be aoxidized and be nitrogenized in oxygen and nitrogen environment, in addition burning, traditional aerosolization method The sized spherical titanium powder of high-purity can not be prepared.
The common preparation method of sized spherical titanium powder has water jacketed copper crucible aerosolization, electrode induction melting aerosol both at home and abroad at present Change, plasma spheroidization and plasma rotating electrode etc..Wherein water jacketed copper crucible aerosolization is relatively early to be used to prepare sized spherical titanium powder Method, although water jacketed copper crucible can largely avoid titanium from introducing chemical impurity in melting, can not avoid completely, and Smelting efficiency is low, the bad control of degree of superheat during melting.Wherein electrode induction melting aerosolization method (EIGA) is to prepare at present The hot technology of titanium valve, the technology make titanium bar-shaped, and the melting in induction coil, will not contact crucible;But electrode sense It should heat and aerosolization nozzle is flowed into after fusing, molten drop should keep steady and sustained fluidised form and uninterrupted, and actually be atomized Occur that droplet-like, or electrode are not completely melt and are broken and fall into diversion pipe in journey, so as to cause to block, therefore keep liquid The stability of stream is the difficult point of current EIGA technologies.In addition, water jacketed copper crucible aerosolization and electrode induction melting aerosolization are all Atomization is gone to cool down high temperature drop again using the high pressure argon gas of room temperature, excessive temperature differentials between drop and argon gas, causes droplet can be Solid state powder is cooled in the extremely short time, it is spherical that no time enough ensures that drop is punctured under surface tension effects, Therefore final powder sphericity is not good enough, can also produce hollow ball, internal gas-entrained.In part with such powder production Portion there are stomata, can influence the mechanical performance and fatigue behaviour of molded part.
Plasma spheroidization technology is that irregular powder is converted into spherical powder with plasma remelting, produces the grain of powder Footpath is related to original irregular powder, and the parameter of irregular powder and quality be difficult to as silk material as bar it is controllable;So The uniformity of production powder quality can be influenced be subject to raw material.And although plasma rotating electrode process can prepare sphericity Preferable titanium valve, but the rotating speed of electrode is difficult to infinitely improve, rotating speed directly affects fine powder recovery rate;And because fixture in being molded Presence, pollution risk can be brought.
Hot plasma be dense gas at atmospheric pressure or elevated pressure arc discharge or high-frequency discharge and produce, be a kind of new Emerging highly-efficient processing heat source.Plasma torch produces plasma after working gas is ionized, the gas after ionization is heated to The high temperature of more than 10000k, then residual gas is heated to 2000~10000k.Electric energy is converted into kinetic energy, produces high speed gas Body.Therefore hot plasma can by various metals instant melting and with high-speed gas atomization into powder, if being made using argon gas For working gas, hot plasma torch will be very suitable for preparing pure titanium and titanium alloy powder.
Patent US5707419 discloses a kind of plasma atomization method for preparing metal dust and ceramic powders, using pair Claim three plasma torch of distribution, form high-temperature plasma focus, the power of plasma torch is 20~40KW, and argon gas is Working gas, can produce high quality submicron metal, and the raw material being atomized can be solid (such as bar, silk material), liquid Deng having that purity is high using the superfines of this method production, size distribution is concentrated, the features such as appearance is spherical in shape.
Patent CN103769594A disclose a kind of plasma atomization prepare high pure spherical it is ultra-fine/the technique side of nanometer powder Method and equipment, establish symmetrical plasma torch, form high-temperature plasma focus, and high-temperature plasma temperature reaches 10000K, according to technological requirement, may be selected argon plasma, can use bar, silk material, powder particle as raw material, lead to Cross special former material feed device and be sent directly into plasma focus highest warm area, raw material is by instant melting or vaporization or warm Local behavior is reacted, ultra-fine/nano metal or ceramic powders are prepared in atomization.
As it can be seen that above method is to prepare metal dust using plasma atomization, the cooling for powder after atomization In-depth study is not carried out, due to the particularity of titanium valve, titanium or titanium alloy powder are prepared using above method, obtained powder Last particle diameter distribution, pattern etc. need to be further improved.
The content of the invention
For disadvantages described above, the present invention provides the plasma atomization method and equipment for preparing pure titanium or titanium alloy powder, uses In the titanium valve for preparing high spherical, high-purity, particle size range narrowly distributing and low cost.
First technical problem that the present invention solves is to provide a kind of plasma atomization for preparing pure titanium or titanium alloy powder Method.
The present invention prepares the plasma atomization method of pure titanium or titanium alloy powder, includes the following steps:
A, stock up:Prepare the titanium silk or titanium alloy wire of a diameter of 3~20mm;
B, atomized molten:In the atomization storehouse of atmosphere of inert gases, using plasma torch melts titanium silk or titanium alloy wire Melt atomization, it is atomized after pure titanium or titanium alloy particle;
C, cool down:The inert gas that temperature is 300~500 DEG C is passed through into atomization storehouse, the pure titanium or titanium after atomization are closed Gold grain section cooling, obtains pure titanium or titanium alloy powder;
Wherein, the inert gas of b step and the inert gas of step c are argon gas or helium.
Preferably, the specific method of titanium silk or titanium alloy wire atomized molten is by using plasma torch:Using Four equally distributed plasma torch, each plasma torch injection direction and silk material into silk direction be in 40 ° of angles, plasma The thermal current that body torch sprays focuses on same processing fusion zone, is 0.05~0.2m/s into silk speed, plasma torch power For 20~100kW, the air-flow spouting velocity of plasma torch mouth is 80~250L/min.
Further, in the atmosphere of inert gases described in b step, oxygen content is no more than 0.3wt%, and nitrogen content does not surpass Cross 0.3wt%.
Preferably, in b step, first vacuumize, then be passed through inert gas to normal pressure, make to be inert atmosphere in atomization storehouse, so Using plasma torch is by titanium silk or titanium alloy wire atomized molten afterwards.
Preferably, in step c, air pressure is 0.2~0.5Mpa at the air inlet of the inert gas.
Second technical problem that the present invention solves is to provide the plasma atomization for preparing spherical pure titanium or titanium alloy powder Equipment.
The present invention plasma atomization plant, including plasma torch, atomization storehouse, to atomization storehouse feeding feed system, The powder collection device being connected with atomization storehouse, the gas purification circulatory system being connected with powder collection device;
The gas purification circulatory system includes gas circulation power set;
Air inlet is equipped with atomization storehouse;The gas circulation power set are connected with being atomized the air inlet pipeline in storehouse; The path of gas circulation power set and air inlet is equipped with heater and controls the solenoid valve of the air inlet pressure at air inlet.
Further, atomization storehouse on be equipped with exhaust outlet, the exhaust outlet is oppositely arranged with air inlet, the exhaust outlet and Gas circulation power set pipeline connects.
Further, the exhaust outlet is positioned at the top in atomization storehouse.
Further, the inner wall in atomization storehouse is equipped with oxygen and nitrogen content detector;The oxygen and nitrogen content detector and controller Communication connection.
Further, the gas purification circulatory system further includes recycling can, and the recycling can is filled with gas circulation power Put connected, control valve is equipped with the connecting path of recycling can and gas circulation power set;It is additionally provided with and controller communication link The pressure sensor in atomization storehouse connect.
Further, the plasma torch is equipped with timer;The timer is connected with alarm.
Further, the shell of the torch spout of the plasma torch is equipped with water cooling plant.
Further, monitoring camera is installed on atomization storehouse.
Compared with prior art, the present invention has the advantages that:
The pure titanium or titanium alloy powder that the method for the present invention is prepared, good sphericity, satellite ball is few, equal with particle diameter distribution Even, high-purity, high spherical, good fluidity, low oxygen content, be mingled with less, non-binding/agglomeration the advantages that.The titanium valve prepared It can be widely used in the molding modes such as metal increasing material manufacturing, powder injection-molded and high temperature insostatic pressing (HIP), for manufacturing high accuracy Part.
The method of the present invention can be vacuumized in initial period, be circulated internal gas in atomization process, to atomized powder Cooled down;Gas is recycled after the completion of work, the reduction powder cost of high degree.
The plasma atomization plant of the present invention, is being atomized the cooling gas in atomization storehouse by gas circulation power set During circulate, produce section cooling air-flow;Heater heats the cooling gas circulated, makes cooling gas temperature It is maintained at 300~500 DEG C.The cooling gas of laminar flow, makes powder rapid dispersion in cooling procedure, prevent liquid particles reunite and Adhesion.Powder is cooled down with the section cooling air-flow higher than room temperature, extends the time that liquid particles are cooled to solid granulates, ensures liquid It is spherical that state particle has enough time to be formed under the action of surface tension in process of setting, prevents the liquid particles in atomization storehouse Cool down too fast, influence the sphericity of solid granulates, improve spherical regular degree, reduce the quantity of satellite ball.
Brief description of the drawings
Fig. 1 is schematic structural view of the invention.
Fig. 2 is plasma torch structure diagram.
In figure, plasma torch 1, torch spout 101, electrode 102, timer 110, water cooling plant 120, atomization storehouse 2, into Gas port 210, exhaust outlet 220, feed system 3, powder collection device 4, the gas purification circulatory system 5, gas circulation power set 510th, gas powder separator 520, recycling can 530, heater 6, solenoid valve 7, oxygen and nitrogen content detector 8, pressure sensor 9, control Valve 10 processed, monitoring camera 11.
Fig. 3 is the picture for the silk material melting conditions that monitoring camera photographs.
Fig. 4 is the microscopic appearance figure of pure titanium powder prepared by embodiment 1.
Fig. 5 is the microscopic appearance figure of Ti6Al4V alloy powders prepared by embodiment 2.
Embodiment
The present invention prepares the plasma atomization method of pure titanium or titanium alloy powder, includes the following steps:
A, stock up:Prepare the titanium silk or titanium alloy wire of a diameter of 3~20mm;
B, atomized molten:In the atomization storehouse of atmosphere of inert gases, using plasma torch melts titanium silk or titanium alloy wire Melt atomization, it is atomized after pure titanium or titanium alloy particle;
C, cool down:It is 300~500 DEG C of inert gas that temperature is continually fed into atomization storehouse, by the pure titanium after atomization or Titanium alloy particle section cooling, obtains pure titanium or titanium alloy powder;
Wherein, the inert gas of b step and the inert gas of step c are argon gas or helium.
Further, it is preferred to use the specific method of titanium silk or titanium alloy wire atomized molten is by plasma torch:Using Four equally distributed plasma torch, each plasma torch injection direction and silk material into silk direction be in 40 ° of angles, plasma The high temperature hot gas stream that body torch sprays focuses on same processing fusion zone, and plasma torch produces plasma after argon gas is ionized Body, the argon gas after ionization is heated to the temperature of 11000k, then residual gas is heated to 2000~10000k.Electric energy is converted For kinetic energy, high-speed gas are produced.
Raw material is entered in the form of silk material, is accurate to up to plasma torch and is processed fusion zone.Reach fusion zone silk material by etc. Gas ions moment melts, and is then atomized into spherical powder by the argon gas stream of high-speed and high-temperature.
It is to influence silk material melting conditions wherein into the flow velocity of silk speed, plasma torch power and body torch ejection working gas With the key process parameter of nebulization efficiency.It can preferably be adjusted into silk speed between 0.05~0.2m/s, plasma torch work( Rate can be adjusted between 20~100kW, and thermal current (i.e. argon gas) spouting velocity of plasma torch mouth can be in 80~250L/min Between adjust.
The method of the present invention, with the raw material thread of certain specification size, is sent into constant rate of speed, and multiple etc. in atomization the top of the warehouse Atomized molten under the focusing plasma jet that gas ions torch produces, forms liquid phase, finally by control cooldown rate, obtains spherical Powder.
Further, in order to ensure titanium valve quality, in the atmosphere of inert gases described in b step, preferably oxygen content does not surpass 0.3wt% is crossed, nitrogen content is no more than 0.3wt%.Can be using oxygen and nitrogen content detector come to oxygen and nitrogen content progress Monitoring.
Preferably, in b step, first vacuumize, then be passed through inert gas to normal pressure, make to be inert atmosphere in atomization storehouse, so Using plasma torch is by titanium silk or titanium alloy wire atomized molten afterwards.
Further, section cooling of the present invention keeps the gas in atomization storehouse to be slowly introducing inert gas Slow flow velocity, the metal dust after atomization slowly decline and cool down under gravity, prevent the collision between metal dust And with being atomized the collision of bulkhead, so as to influence sphericity.
The section cooling of the present invention can be realized by the following method:Enough gas is provided with the air inlet of cooling air-flow Pressure, air inlet and gas outlet can realize the interflow of cooling air-flow, layer realized to powder positioned at the different height in atomization storehouse Stream cooling.
In order to realize the section cooling air-flow in step c, at the air inlet of preferably described air-flow air pressure for 0.2~ 0.5Mpa。
The inert gas flows of section cooling, make powder rapid dispersion in cooling procedure, prevent powder from reuniting and adhering to. Powder is cooled down with the air-flow higher than room temperature, extends the time that liquid particles are cooled to solid granulates, ensures particle in process of setting In to have enough time to be formed under the action of surface tension spherical, prevent that the powder cooling in atomization storehouse is too fast, influence sphericity With generation satellite ball.
The present invention also provides the plasma atomization plant for preparing spherical pure titanium or titanium alloy powder.
The plasma atomization plant of the present invention, as shown in Figure 1, being sent including plasma torch 1, atomization storehouse 2, to atomization storehouse 2 The feed system 3 of material, the powder collection device 4 being connected with atomization storehouse 2, the gas purification circulation being connected with powder collection device 4 System 5;
The gas purification circulatory system 5 as shown in Figure 1 includes the gas circulation power set 510 using circulating fan; Gas circulation power set 510 circulate the cooling gas in atomization storehouse 2 in atomization process, to by plasma torch 1 The liquid particles formed after atomization carry out being cooled into solid granulates, the liquid particles, that is, drop or aerosol sprills.
To make gas circulation power set 510 can act on atomization storehouse 2, therefore, it is equipped with air inlet 210 on atomization storehouse 2; The gas circulation power set 510 are connected with being atomized 210 pipeline of air inlet in storehouse 2.And gas circulation power set 510 with The purpose that the path of air inlet 210 is equipped with the solenoid valve 7 of the air inlet pressure at control air inlet 210 is controlled by solenoid valve 7 Air inlet pressure at air inlet 210, makes the cooling gas in atomization storehouse 2 form laminar flow, and section cooling gas is formed in atomization storehouse 2 Stream, cools down the liquid particles formed after being atomized by plasma torch 1, liquid particles is quickly divided in cooling procedure Dissipate, prevent liquid particles from reuniting and adhering to.And heating is equipped with the path of gas circulation power set 510 and air inlet 210 Device 6, the purpose is to be heated to the cooling gas of circulation, makes cooling gas keep 300-500 DEG C of temperature, extends liquid Grain is cooled to time of solid granulates, prevent during sphere is cooled into, sphere caused by after the quick refrigeration of surface is loose, The defects of empty, improve spherical regular degree, reduces the quantity of satellite ball.
This prepares the plasma atomization plant of spherical pure titanium or titanium alloy powder, is made by gas circulation power set 510 Cooling gas in atomization storehouse 2 circulates in atomization process, produces section cooling air-flow;Heater 6 is to circulating Cooling gas heats, and cooling gas temperature is maintained at 300-500 DEG C.The cooling gas of laminar flow, makes powder in cooling procedure Rapid dispersion, prevents liquid particles from reuniting and adhering to.Powder is cooled down with the section cooling air-flow higher than room temperature, extends liquid particles The time of solid granulates is cooled to, ensures that liquid particles have enough time to be formed under the action of surface tension in process of setting It is spherical, prevent that the liquid particles cooling in atomization storehouse 2 is too fast, influence the sphericity of solid granulates, improve spherical regular journey Degree, reduces the quantity of satellite ball.
Gas circulation power set 510 circulate the cooling gas in atomization storehouse 2 in atomization process, meanwhile, institute The air inlet pressure stated at the air inlet 210 in atomization storehouse 2 is 0.2-0.5Mpa.So, the gas of section cooling is formed in atomization storehouse 2 Flowing, makes liquid particles rapid dispersion in cooling procedure, prevents liquid particles from reuniting and adhering to.Protection gas was so both can guarantee that The cooled and solidified to liquid particles is realized in the flowing of body, and larger interference will not be produced to the falling motion of liquid particles, is made Into the collision between liquid particles, more satellite ball is formed, influences the quality of final products.
In the above-described embodiment, the flow export that cooling gas circulates can be doubled as by being atomized the discharge port in storehouse 2, i.e. Cooling gas in atomization storehouse 2 enters powder collection device 4 through discharge port, then enters gas by gas powder separator 520 Cycle power device 510, then entered by gas circulation power set 510 by air inlet 210 in atomization storehouse 2.However, due to liquid State particle temperature is very high, and when cooling gas is in contact with it, the rise of cooling gas temperature moment, therefore, it is necessary to timely discharge temperature Cooling gas after rise, if discharging cooling gas using discharge port, then, the cooling gas after temperature rise is in atomization storehouse 2 Holdup time length.In order to overcome the problems referred above, therefore, it is preferred that atomization storehouse 2 on be equipped with exhaust outlet 220, the exhaust outlet 220 It is oppositely arranged with air inlet 210, the exhaust outlet 220 is connected with 510 pipeline of gas circulation power set.The exhaust outlet 220 It is oppositely arranged with air inlet 210, i.e. side wall or top of the exhaust outlet 220 positioned at atomization storehouse 2, and, cooling gas is by air inlet The circulation path of 210 inflow exhaust outlets 220 passes through powder area.
Preferably, the exhaust outlet 220 is positioned at the top in atomization storehouse 2.
Exhaust outlet 220 is positioned at the top in atomization storehouse 2, then, during the work time, the cooling gas in atomization storehouse 2 flows to mist Change the top in storehouse 2, discharged by exhaust outlet 220, and the discharge port for being atomized pure titanium or titanium alloy powder to the atomization storehouse 2 in storehouse 2 moves It is dynamic, so as to play the role of certain separation argon gas and powder.
Carried out due to fusing and in atomization process in the environment of hypoxemia and low nitrogen, in order to be detected in whole work process The content of oxygen and nitrogen, therefore, the inner wall in atomization storehouse 2 is equipped with oxygen and nitrogen content detector 8;The oxygen and nitrogen content detector 8 with Controller communication connection in control cabinet.Oxygen and nitrogen content detector 8 is that containing for oxygen and nitrogen is detected in whole work process Amount, can automatic alarm and interruption of work process when oxygen and nitrogen content is exceeded.
Preferably, the gas purification circulatory system 5 further includes recycling can 530, and the recycling can 530 is moved with gas circulation Power apparatus 510 is connected, and control valve 10, the control are equipped with the connecting path of recycling can 530 and gas circulation power set 510 Valve 10 processed is electrically connected with the controller in control cabinet;It is additionally provided with and is passed with the pressure in atomization storehouse 2 of controller communication connection Sensor 9.In fusing and in atomization process, plasma torch 1 can input the working gas such as certain argon gas, shadow to atomization storehouse 2 The air pressure in atomization storehouse 2 is rung, so as to influence the shape of solid granulates after cooling, pressure sensor 9 is then used to detect atomization storehouse 2 Interior air pressure, when air pressure exceedes setting value, controller instruction control valve 10 is opened, and the gas being atomized in storehouse 2 is pumped into back Closed cans 530 recycles.Control cabinet is existing structure, is not represented in the example shown.
Since 102 service life of electrode of plasma torch 1 is limited, the operating time of the electrode 102 of plasma torch 1 arrives Up to during critical value, it is necessary to replace electrode 102.Therefore, it is preferred that as shown in Fig. 2, the plasma torch 1 is equipped with timer 110, the timer 110 is connected with alarm.When timer 110 is used to record the work of electrode 102 of plasma torch 1 Long, when operating during long arrival critical value, the meeting warning reminding operator of timer 110 replaces electrode 102 in advance, prevents from working During electrode 102 break down influence production.
In order to which plasma torch 1 carries out anti-carbonization and the processing of anti-tungsten, the torch spout 101 of the plasma torch 1 Shell be equipped with water cooling plant 120.Water cooling plant 120 is existing apparatus, it circulates the spout of plasma torch 1 using water Shell carries out cooling treatment, to reduce the skin temperature of spout, so as to play the role of anti-carbonization and anti-tungsten to a certain extent. Meanwhile the torch spout 101 of the plasma torch 1 is high-temperature ceramic materials product.Replaced using high-temperature ceramic materials product Torch spout 101 made of traditional metal material, overcome metal material because high temperature occur carbonization and tungsten will bring it is miscellaneous Matter, the defects of influencing the purity of pure titanium and titanium alloy powder.
Preferably, monitoring camera 11 is installed on atomization storehouse 2.Monitoring camera 11 can monitor wire in real time Melting conditions, monitoring camera 11 record the picture that plasma torch 1 is acted on Metal wire material, are converted into fusing shape Condition.If there is situations such as not being completely melt or superfusing when monitoring wire fusing, the work of powder by atomization can be adjusted in time Skill parameter, it is ensured that wire is reasonably melted, and ensures the quality of production powder and has high consistency.
The embodiment of the present invention is further described with reference to embodiment, is not therefore limited the present invention System is among the embodiment described scope.Plasma atomization plant using the present invention in embodiment.
Embodiment 1
First, the raw material preparation stage
Select the circular pure titanium silk material of a diameter of 8mm to be used as powder raw material processed, there is detection material book per a collection of raw material, it is all full Requirements of the sufficient American society for testing and materials ASTM to chemical composition.
2nd, atomization storehouse 2 vacuumizes and the applying argon gas stage
Before fusing and atomization, take the air in atomization storehouse 2 away with vaccum-pumping equipment, make the internal vacuum for reaching 40kPa Degree and then past the inside are filled with argon gas to normal pressure, the primary oxygen inside atomization storehouse 2 and initial nitrogen content is less than 0.1%. The content of oxygen and nitrogen is all detected in whole work process using oxygen and nitrogen content detector 8, makes fusing and atomization process low Carried out in the environment of oxygen and low nitrogen, can automatic alarm and interruption of work process when oxygen and nitrogen content is more than 0.3%.
3rd, fusing and atomization step
This patent selects four equally distributed plasma torch 1, wherein the injection direction and silk of each plasma torch 1 The vertical of material into silk direction is in 40 ° of angles, and the high temperature hot gas stream that four plasma torch spray focuses on same processing fusion zone.
Raw material is flowed into the form of pure titanium silk material, and straightening metal wire device ensure that the straightness of silk material, wire is hung down It is straight downward, it is accurate to up to plasma torch and processes fusion zone.Reach fusion zone silk material melted by plasma moment, then by The argon gas stream of high-speed and high-temperature is atomized into spherical powder.
It is 0.1m/s wherein into silk speed, plasma torch power is 30kW, and the thermal current spouting velocity of body torch mouth is 15L/min.Melting with atomization process, monitoring camera 11 can monitor fusing and the atomization situation of wire in real time, will etc. The picture that gas ions torch is acted on Metal wire material is recorded, and is converted into melting conditions.If occur when monitoring silk material fusing Situations such as not being completely melt or superfusing, whole equipment can adjust the technological parameter of powder by atomization in time, it is ensured that silk material obtains Rational fusing, the quality for ensureing to produce pure titanium powder have high consistency.
4th, powder cooling stage
After molten metal after fusing is atomized into tiny particle, gas circulation power set 510 are started to work, and are kept Air pressure at air inlet 210 is 0.2Mpa, circulates the argon gas in atomization storehouse 2, produces section cooling argon gas stream;Circulate argon Hot-air heater 6 can will heat the argon gas circulated, and the cooling gas temperature for making to be passed through is maintained at 320~330 DEG C.
5th, argon gas recovery stage
In powder cooling procedure processed, argon gas is recycling always, and keeps being passed through temperature at 320~330 DEG C;Powder processed terminates Afterwards, it is recovered to by gas circulation power set 510 by argon gas unnecessary in storehouse is atomized in recycling can 530, makes argon gas in next time It can also be reused during work, reduce powder cost processed.Pure titanium powder is cooled to after solid spherical, the argon that can be circulated Air-flow is brought into Powder Recovery storehouse 4 and stores.
The pure titanium powder prepared be illustrated in figure 4 it is high it is spherical, particle is uniform, and satellite ball particle is few.
In addition the pure titanium powder component prepared meets standards of the ASTM F67 to pure 1 grade of titanium material, its component is shown in Table 1, Powder property is shown in Table 3.
The pure titanium powder component list of table 1
Component (%) O Fe C N H OET Ti
Pure titanium powder 0.12 0.05 0.08 0.03 0.012 < 0.4 Bal.
Embodiment 2
The circular Ti6Al4V silk materials of a diameter of 8mm are selected to be used as powder raw material processed, using the method for embodiment 1, only change portion Divide parameter, titanium alloy powder is prepared.Wherein, the parameter of change is:
Vacuumized in atomization storehouse 2 with applying argon gas stage, primary oxygen and initial nitrogen content less than 0.08%, when oxygen nitrogen contains Can automatic alarm and interruption of work process when amount is more than 0.2%.
It is 0.08m/s into silk speed in melting and atomization step, plasma torch power is 40kW, the hot gas of torch mouth Stream spouting velocity is 20L/min.
Air pressure at powder cooling stage, air inlet 210 is 0.5Mpa, and the cooling gas temperature being passed through is maintained at 300 ~320 DEG C.
The Ti6Al4V alloy powders prepared are as shown in figure 5, be that height is spherical, particle is uniform, and satellite ball particle is few.Separately The Ti6Al4V alloy powder components prepared outside meet standards of the ASTM F136 to 23 grades of Ti6Al4V materials, its component is shown in Table 2, powder property is shown in Table 3.
2 Ti6Al4V alloy powder component lists of table
Component (%) Al V Fe C N H O Ti
Ti6Al4V alloy powders 6.0 4.1 0.24 0.02 0.01 0.012 0.09 Bal.
Comparative example 1
The circular pure titanium silk material of a diameter of 8mm is selected to be used as powder raw material processed, using the method for embodiment 1, only changing section Parameter, is prepared titanium alloy powder.Wherein, the parameter of change is:Air pressure at powder cooling stage, air inlet 210 is 0.8Mpa.Since inlet pressure is excessive, powder can be directly blown onto on atomization storehouse side wall in cooling procedure, shorten powder The time of particle collapses balling-up, influences powder sphericity.
The titanium valve obtained using the above method, sphericity are deteriorated, and the increase of satellite ball particle, influences final flow of powder Property, its powder property is shown in Table 3.
Comparative example 2
The circular pure titanium silk material of a diameter of 8mm is selected to be used as powder raw material processed, using the method for embodiment 1, only changing section Parameter, is prepared titanium alloy powder.Wherein, the parameter of change is:Air pressure at powder cooling stage, air inlet 210 is 0.1Mpa.Since inlet pressure is too small, powder can not be dispelled, the effect unobvious of section cooling, can be sent out in cooling procedure Green powder adheres to, and influences powder sphericity.
The titanium valve obtained using the above method, sphericity are deteriorated, the increase of satellite ball particle, the increase of fine powder recovery rate, its powder Last performance is shown in Table 3.
Comparative example 3
The circular pure titanium silk material of a diameter of 8mm is selected to be used as powder raw material processed, using the method for embodiment 1, only changing section Parameter, is prepared titanium alloy powder.Wherein, the parameter of change is:In powder cooling stage, the cooling gas temperature being passed through is Room temperature.Due to going to cool down using room temperature argon gas, liquid particles, which will be cooled to the solid time, to be greatly shortened, and most particle will There is no enough time to be formed under the action of surface tension spherical.
The titanium valve obtained using the above method, powder sphericity are deteriorated it is obvious that influencing the final mobility of powder, its powder Last performance is shown in Table 3.
3 pure titanium of table or Ti6Al4V alloy powder performance tables

Claims (12)

1. prepare the plasma atomization method of spherical pure titanium or titanium alloy powder, it is characterised in that include the following steps:
A, stock up:Prepare the titanium silk or titanium alloy wire of a diameter of 3~20mm;
B, atomized molten:In the atomization storehouse of atmosphere of inert gases, titanium silk or titanium alloy wire are melted mist by using plasma torch Change, it is atomized after pure titanium or titanium alloy particle;
C, cool down:The inert gas that temperature is 300~500 DEG C is passed through into atomization storehouse, by the pure titanium or titanium alloy after atomization Grain section cooling, obtains pure titanium or titanium alloy powder;
Wherein, the inert gas of b step and the inert gas of step c are argon gas or helium.
2. the plasma atomization method according to claim 1 for preparing spherical pure titanium or titanium alloy powder, it is characterised in that: The specific method of titanium silk or titanium alloy wire atomized molten is by using plasma torch:Using four equally distributed plasmas Torch, each plasma torch injection direction and silk material are in 40 ° of angles into silk direction, and the thermal current that plasma torch sprays focuses on Same processing fusion zone, is 0.05~0.2m/s into silk speed, and plasma torch power is 20~100kW, plasma torch The air-flow spouting velocity of mouth is 80~250L/min.
3. the plasma atomization method according to claim 1 or 2 for preparing spherical pure titanium or titanium alloy powder, its feature exist In:In atmosphere of inert gases described in b step, oxygen content is no more than 0.3wt%, and nitrogen content is no more than 0.3wt%.
4. the plasma atomization method according to claim 3 for preparing spherical pure titanium or titanium alloy powder, it is characterised in that: In b step, first vacuumize, then be passed through inert gas to normal pressure, make to be inert atmosphere in atomization storehouse, then using plasma torch By titanium silk or titanium alloy wire atomized molten.
5. the plasma atomization method according to claim 1 or 2 for preparing spherical pure titanium or titanium alloy powder, its feature exist In:In step c, air pressure is 0.2~0.5MPa at the air inlet of the inert gas.
6. implementation 5 any one of them of Claims 1 to 5 prepares the plasma atomization method of spherical pure titanium or titanium alloy powder Plasma atomization plant, including plasma torch (1), atomization storehouse (2), feed system (3) and mist to atomization storehouse (2) feeding The gas purification circulatory system (5) for change storehouse (2) connected powder collection device (4), being connected with powder collection device (4);It is special Sign is:
The gas purification circulatory system (5) includes gas circulation power set (510);
Air inlet (210) is equipped with atomization storehouse (2);The gas circulation power set (510) and the air inlet of atomization storehouse (2) (210) pipeline connects;Heater (6) and control are equipped with the path of gas circulation power set (510) and air inlet (210) The solenoid valve (7) of the air inlet pressure at air inlet (210) place;Exhaust outlet (220), the exhaust outlet (220) are equipped with atomization storehouse (2) It is oppositely arranged with air inlet (210), the exhaust outlet (220) is connected with gas circulation power set (510) pipeline;Air inlet (210) place's air pressure is 0.2~0.5MPa;The air inlet pressure at air inlet (210) place is controlled by solenoid valve (7), is made in atomization storehouse (2) Cooling gas formed laminar flow;Heater (6) heats the cooling gas circulated, cooling gas temperature is maintained at 300 ~500 DEG C.
7. plasma atomization plant according to claim 6, it is characterised in that:The exhaust outlet (220) is positioned at atomization storehouse (2) top.
8. plasma atomization plant according to claim 7, it is characterised in that:Oxygen nitrogen is equipped with the inner wall of atomization storehouse (2) Content detection instrument (8);The oxygen and nitrogen content detector (8) communicates to connect with controller.
9. plasma atomization plant according to claim 8, it is characterised in that:The gas purification circulatory system (5) is also Including recycling can (530), the recycling can (530) is connected with gas circulation power set (510), in recycling can (530) and gas The connecting path of body circulation power set (510) is equipped with control valve (10);It is additionally provided with and is located at mist with what controller communicated to connect Change the pressure sensor (9) in storehouse (2).
10. plasma atomization plant according to claim 6, it is characterised in that:The plasma torch (1) is equipped with meter When device (110);The timer (110) is connected with alarm.
11. plasma atomization plant according to claim 10, it is characterised in that:The torch of the plasma torch (1) The shell of spout (101) is equipped with water cooling plant (120).
12. plasma atomization plant according to claim 11, it is characterised in that:Monitoring is installed in atomization storehouse (2) Camera (11).
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