CN106378460A - Plasma atomization method and apparatus for preparing pure titanium or titanium alloy powder - Google Patents

Plasma atomization method and apparatus for preparing pure titanium or titanium alloy powder Download PDF

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Publication number
CN106378460A
CN106378460A CN201610841237.1A CN201610841237A CN106378460A CN 106378460 A CN106378460 A CN 106378460A CN 201610841237 A CN201610841237 A CN 201610841237A CN 106378460 A CN106378460 A CN 106378460A
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titanium
atomization
titanium alloy
plasma
alloy powder
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CN106378460B (en
Inventor
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

Abstract

The invention relates to a plasma atomization method and apparatus for preparing spherical pure titanium or titanium alloy powder, and belongs to the technical field of preparation of titanium or titanium alloy powder. The plasma atomization method for preparing pure titanium or titanium alloy powder comprises the following steps of (1) preparing a titanium wire or titanium alloy wire with the diameter ranging from 3 millimeters to 20 millimeters, (2) using a plasma torch to fuse and atomize the titanium wire or titanium alloy wire in an atomization bin with an argon atmosphere to obtain atomized pure titanium particles or titanium alloy particles, and (3) feeding argon flow with the temperature ranging from 300 DEG C to 500 DEG C into the atomization bin, carrying out laminar cooling on the atomized pure titanium particles or titanium alloy particles to obtain pure titanium or titanium alloy powder. The obtained powder is good in degree of sphericity and low in the content of satellite balls, and has the advantages of being uniform in size distribution, high in purity and degree of sphericity, good in liquidity, low in oxygen content and impurity content, free of bond or cluster phenomenon and the like. The prepared titanium powder can be widely applied to the forming manners such as metal additive manufacturing, powder injection moulding and hot isostatic pressing for manufacturing parts with high precision.

Description

Prepare plasma atomization method and the equipment of pure titanium or titanium alloy powder
Technical field
The present invention relates to preparing plasma atomization method and the equipment of pure titanium or titanium alloy powder, belong to titanium or Titanium Powder The preparing technical field at end.
Background technology
, because density is low, specific strength is high, corrosion resistance, good mechanical property, and biocompatibility is excellent for pure titanium and titanium alloy, It is widely used in Aero-Space 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 manufacturing. The therefore 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, the method system such as conventional Mechanical Crushing, chemical gaseous phase Standby titanium valve cannot meet its rigors.
, because fusing point is high, under high temperature, chemism is strong, can react with crucible, make under molten condition for pure titanium and titanium alloy Chemical purity is affected;In oxygen and nitrogen environment can oxidized and nitridation, or even burning, traditional aerosolization method Highly purified sized spherical titanium powder cannot 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 for preparing sized spherical titanium powder Method, although water jacketed copper crucible can largely avoid titanium to introduce chemical impurity in melting, cannot avoid completely, and Smelting efficiency is low, the bad control of degree of superheat during melting.Wherein electrode induction melting aerosolization method (EIGA) is current preparation The hot technology of titanium valve, titanium is made bar-shaped, melting in induction coil by this technology, will not contact crucible;But electrode sense Should heat and flow into aerosolization nozzle after fusing, molten drop should keep stablizing lasting fluidised form and uninterrupted, and reality was atomized Droplet-like occurring in journey, or electrode is not completely melt and ruptures and fall in mozzle, thus causing to block, therefore keeping liquid The stability of stream is the difficult point of current EIGA technology.Additionally, water jacketed copper crucible aerosolization and electrode induction melting aerosolization are all Remove atomization cooling down high-temperature drop, excessive temperature differentials between drop and argon gas again using the high pressure argon gas of normal temperature, lead to the droplet can be It is cooled to solid state powder in the extremely short time, do not have time enough to ensure that drop is punctured under surface tension effects spherical, Therefore final powder sphericity is not good, also can produce hollow ball, internal gas-entrained.In part with such powder production Can there is pore, the mechanical performance of impact profiled member and fatigue behaviour in portion.
Plasma spheroidization technology is that irregular powder plasma remelting is converted into spherical powder, 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 the same with bar controlled;So The uniformity producing powder quality can be affected by raw material.And although plasma rotating electrode process can prepare sphericity Preferably titanium valve, but the rotating speed of electrode is difficult to infinitely improve, and 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 thermal source.Plasma torch produces plasma after ionizing working gas, and 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 various metals can be become powder in instant melting and with high-speed gas atomization by hot plasma, if being made using argon gas For working gas, hot plasma torch will be especially suitable for preparing pure titanium and titanium alloy powder.
Patent US5707419 discloses a kind of plasma atomization method preparing metal dust and ceramic powders, using right 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 (as bar, silk material), liquid Deng having using the superfines that the method produces that purity is high, size distribution is concentrated, the feature such as outward appearance is spherical in shape.
Patent CN103769594A disclose a kind of plasma atomization prepare high pure spherical ultra-fine/the technique side of nanometer powder Method and equipment, set up symmetrical plasma torch, form high-temperature plasma focus, and high-temperature plasma temperature can reach 10000K, according to technological requirement, optional argon plasma, can be raw material using bar, silk material, powder particle, 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 Reaction local behavior, ultra-fine/nano metal or ceramic powders are prepared in atomization.
It can be seen that, above method is all to prepare metal dust using plasma atomization, for the cooling of powder after atomization Do not carry out in-depth study, due to the particularity of titanium valve, titanium or titanium alloy powder are prepared using above method, the powder obtaining Last particle diameter distribution, pattern etc. all need to be improved further.
Content of the invention
For disadvantages described above, the present invention provides the plasma atomization method preparing pure titanium or titanium alloy powder and equipment, uses In high spherical, high-purity, particle size range narrowly distributing and low cost the titanium valve of preparation.
First technical problem that the present invention solves is to provide a kind of plasma atomization preparing pure titanium or titanium alloy powder Method.
The present invention prepares the plasma atomization method of pure titanium or titanium alloy powder, comprises the steps:
A, get the raw materials ready:Prepare titanium silk or the 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 by using plasma torch Melt atomization, atomized after pure titanium or titanium alloy particle;
C, cooling:It is passed through, in atomization storehouse, the inert gas that temperature is 300~500 DEG C, the pure titanium after atomization or titanium 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 concrete grammar 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 is in 40 ° of angles with a direction of entering of silk material, plasma The thermal current that body torch sprays focuses on same processing fusion zone, and entering a speed is 0.05~0.2m/s, 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 less 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, at the air inlet of described inert gas, air pressure is 0.2~0.5Mpa.
Second technical problem that the present invention solves is the plasma atomization providing and preparing spherical pure titanium or titanium alloy powder Equipment.
The plasma atomization plant of the present invention, including plasma torch, atomization storehouse, to atomization storehouse feeding feed system, With the atomization storehouse powder collection device being connected, the gas purification circulatory system being connected with powder collection device;
The described gas purification circulatory system includes gas cycle power device;
Atomization storehouse is provided with air inlet;Described gas cycle power device is connected with the air inlet pipeline in atomization storehouse;? The magnetic valve that the path of gas cycle power device and air inlet is provided with heater and controls the air inlet pressure at air inlet.
Further, atomization storehouse on be provided with exhaust outlet, described exhaust outlet and air inlet are oppositely arranged, described exhaust outlet and Gas cycle power device pipeline connects.
Further, described exhaust outlet is located at the top in atomization storehouse.
Further, the inwall in atomization storehouse is provided with oxygen and nitrogen content detector;Described oxygen and nitrogen content detector and controller Communication connection.
Further, the described gas purification circulatory system also includes recycling can, and described recycling can is filled with gas circulation power Put connected, the connecting path with gas cycle power device for the recycling can is provided with control valve;It is additionally provided with and controller communication link The pressure sensor in atomization storehouse connecing.
Further, described plasma torch is provided with timer;Described timer is connected with alarm.
Further, the shell of the torch spout of described plasma torch is provided with water cooling plant.
Further, atomization storehouse is provided with monitoring camera.
Compared with prior art, the present invention has the advantages that:
Pure titanium or titanium alloy powder that the inventive method prepares, good sphericity, satellite ball is few, has particle diameter distribution equal Even, high-purity, high spherical, good fluidity, low oxygen content, be mingled with less, non-binding/agglomeration the advantages of.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 accuracy Part.
The inventive method can vacuumize in initial period, in atomization process is circulated internal gas, to atomized powder Cooled down;After the completion of work, gas is reclaimed, the reduction powder cost of high degree.
The plasma atomization plant of the present invention, makes the cooling gas in atomization storehouse in atomization by gas cycle power device During circulate, produce section cooling air-flow;Heater, to the cooling gas heating circulating, makes cooling gas temperature It is maintained at 300~500 DEG C.The cooling gas of laminar flow, make powder rapid dispersion in cooling procedure, prevent liquid particles reunite and Adhesion.Cool down powder with the section cooling air-flow higher than room temperature, extend liquid particles and be cooled to the time of solid granulates it is ensured that liquid It is spherical that state particle has enough time to be formed in the presence of surface tension in process of setting, prevents the liquid particles being atomized in storehouse Cooling is too fast, the sphericity of impact solid granulates, improves spherical regular degree, decreases the quantity of satellite ball.
Brief description
Fig. 1 is present configuration schematic diagram.
Fig. 2 is plasma torch structural representation.
In figure, plasma torch 1, torch spout 101, electrode 102, timer 110, water cooling plant 120, atomization storehouse 2, enter Gas port 210, exhaust outlet 220, feed system 3, powder collection device 4, the gas purification circulatory system 5, gas cycle power device 510th, gas powder separator 520, recycling can 530, heater 6, magnetic valve 7, oxygen and nitrogen content detector 8, pressure sensor 9, control Valve 10 processed, monitoring camera 11.
The picture of the silk material melting conditions that Fig. 3 photographs for monitoring camera.
Fig. 4 is the microscopic appearance figure of the pure titanium powder of embodiment 1 preparation.
Fig. 5 be embodiment 2 preparation Ti6Al4V alloy powder microscopic appearance figure.
Specific embodiment
The present invention prepares the plasma atomization method of pure titanium or titanium alloy powder, comprises the steps:
A, get the raw materials ready:Prepare titanium silk or the 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 by using plasma torch Melt atomization, atomized after pure titanium or titanium alloy particle;
C, cooling:To atomization storehouse in be continually fed into the inert gas that temperature is 300~500 DEG C, by atomization after pure titanium 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 concrete grammar of titanium silk or titanium alloy wire atomized molten is by plasma torch:Using Four equally distributed plasma torch, each plasma torch injection direction is in 40 ° of angles with a direction of entering of silk material, plasma The high temperature hot gas stream that body torch sprays focuses on same processing fusion zone, and plasma torch produces plasma after ionizing argon gas 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, produce high-speed gas.
Raw material is entered with silk material form, accurately reaches plasma torch processing 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.
The flow velocity wherein entering a speed, plasma torch power and body torch ejection working gas is impact silk material melting conditions Key process parameter with nebulization efficiency.Preferably enter a speed to adjust 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 inventive method, with the raw material thread of certain specification size, is sent into constant rate of speed, and multiple etc. in atomization silo roof portion Atomized molten under the focusing plasma jet that gas ions torch produces, forms liquid phase, finally by controlling 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 Cross 0.3wt%, nitrogen content is less than 0.3wt%.Can oxygen and nitrogen content are carried out using oxygen and nitrogen content detector 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 is to be slowly introducing inert gas, so that the gas in atomization storehouse is kept Slow flow velocity, the metal dust after atomization slowly declines under gravity and cools down, and prevents the collision between metal dust And the collision with atomization bulkhead, thus affecting sphericity.
The section cooling of the present invention can be realized by the following method:It is provided with enough gas in the air inlet of cooling air-flow Pressure, air inlet and gas outlet are located at the different height in atomization storehouse, are capable of the interflow of cooling air-flow, realize layer to powder 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 be 0.2~ 0.5Mpa.
The inert gas flows of section cooling, make powder rapid dispersion in cooling procedure, prevent powder from reuniting and adhere to. Cool down powder with the air-flow higher than room temperature, extend liquid particles and be cooled to the time of solid granulates it is ensured that particle is in process of setting In to have enough time to be formed in the presence of surface tension spherical, prevent the powder cooling being atomized in storehouse too fast, affect sphericity With generation satellite ball.
The present invention also provides the plasma atomization plant preparing spherical pure titanium or titanium alloy powder.
The plasma atomization plant of the present invention, as shown in figure 1, including plasma torch 1, atomization storehouse 2, sending 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 includes the gas cycle power device 510 using circulating fan as shown in Figure 1; Gas cycle power device 510, in atomization process, makes the cooling gas in atomization storehouse 2 circulate, to by plasma torch 1 The liquid particles being formed after atomization carry out being cooled into solid granulates, and described liquid particles are drop or aerosol sprills.
For making gas cycle power device 510 can act on atomization storehouse 2, therefore, atomization storehouse 2 is provided with air inlet 210; Described gas cycle power device 510 is connected with air inlet 210 pipeline in atomization storehouse 2.And gas cycle power device 510 with The purpose that the path of air inlet 210 is provided with the magnetic valve 7 of air inlet pressure at control air inlet 210 is to be controlled by magnetic valve 7 Air inlet pressure at air inlet 210, makes the cooling gas in atomization storehouse 2 form laminar flow, forms section cooling gas in atomization storehouse 2 The liquid particles being formed after being atomized by plasma torch 1 are cooled down, so that liquid particles is quickly divided in cooling procedure by stream Dissipate, prevent liquid particles from reuniting and adhere to.And, the path with air inlet 210 for the gas cycle power device 510 is provided with heating Device 6, its objective is the cooling gas of circulation are heated, makes the temperature that cooling gas keep 300-500 DEG C, extend liquid Grain is cooled to time of solid granulates, prevent during being cooled into spheroid, the spheroid causing after the quick refrigeration of surface is loose, The defects such as cavity, improve spherical regular degree, decrease the quantity of satellite ball.
This prepares the plasma atomization plant of spherical pure titanium or titanium alloy powder, is made by gas cycle power device 510 Cooling gas in atomization storehouse 2 circulate in atomization process, produce section cooling air-flow;Heater 6 is to circulating Cooling gas heat, and make cooling gas temperature be maintained at 300-500 DEG C.The cooling gas of laminar flow, make powder in cooling procedure Rapid dispersion, prevents liquid particles from reuniting and adheres to.Cool down powder with the section cooling air-flow higher than room temperature, extend liquid particles It is cooled to the time of solid granulates it is ensured that liquid particles have enough time to be formed in the presence of surface tension in process of setting Spherical, prevent the liquid particles cooling being atomized in storehouse 2 too fast, the sphericity of impact solid granulates, improve spherical regular journey Degree, decreases the quantity of satellite ball.
Gas cycle power device 510, in atomization process, makes the cooling gas in atomization storehouse 2 circulate, meanwhile, institute Stating the air inlet pressure at the air inlet 210 in atomization storehouse 2 is 0.2-0.5Mpa.So, form the gas of section cooling in atomization storehouse 2 Flowing, makes liquid particles rapid dispersion in cooling procedure, prevents liquid particles from reuniting and adheres to.So both can guarantee that shielding gas The cooled and solidified to liquid particles is realized in the flowing of body, will not produce larger interference to the falling motion of liquid particles again, make Become the collision between liquid particles, form more satellite ball, the quality of impact final products.
In the above-described embodiment, the flow export that the discharging opening in atomization storehouse 2 can circulate as cooling gas, i.e. Cooling gas in atomization storehouse 2 enter powder collection device 4 through discharging opening, are then passed through gas powder separator 520 and enter gas Cycle power device 510, then entered by air inlet 210 in atomization storehouse 2 through gas cycle power device 510.However, due to liquid State particle temperature is very high, and when cooling gas are in contact with it, cooling gas temperature moment raises, accordingly, it would be desirable to timely discharge temperature Cooling gas after rising, if discharge cooling gas using discharging opening, then, the cooling gas after temperature raises are being atomized storehouse 2 Holdup time long.For overcoming the problems referred to above, therefore it is preferred that it is provided with exhaust outlet 220, described exhaust outlet 220 on atomization storehouse 2 It is oppositely arranged with air inlet 210, described exhaust outlet 220 is connected with gas cycle power device 510 pipeline.Described exhaust outlet 220 It is oppositely arranged with air inlet 210, i.e. exhaust outlet 220 is located at side wall or the top in atomization storehouse 2, and, cooling gas are by air inlet The circulation path of 210 inflow exhaust outlets 220 passes through powder area.
Preferably, described exhaust outlet 220 is located at the top in atomization storehouse 2.
Exhaust outlet 220 is located at the top in atomization storehouse 2, then, in the course of the work, the cooling gas in atomization storehouse 2 flow to mist Change the top in storehouse 2, discharge through exhaust outlet 220, and the discharging opening being atomized the pure titanium in storehouse 2 or titanium alloy powder to atomization storehouse 2 moves Dynamic, thus playing certain separation argon gas and powder effect.
Carry out in the environment of hypoxemia and low nitrogen due to fusing with atomization process, in order to detect in whole work process Oxygen and the content of nitrogen, therefore, the inwall in atomization storehouse 2 is provided with oxygen and nitrogen content detector 8;Described oxygen and nitrogen content detector 8 with Controller communication connection in control cabinet.Oxygen and nitrogen content detector 8 be in whole work process detection oxygen and the containing of nitrogen Amount, can automatic alarm interruption of work process when oxygen and nitrogen content is exceeded.
Preferably, the described gas purification circulatory system 5 also includes recycling can 530, and described recycling can 530 is dynamic with gas circulation Power apparatus 510 are connected, and are provided with control valve 10, described control on the connecting path with gas cycle power device 510 for the recycling can 530 Valve 10 processed is electrically connected with the controller in control cabinet;It is additionally provided with the pressure in atomization storehouse 2 with controller communication connection to pass Sensor 9.In fusing with atomization process, plasma torch 1 can input the working gas such as certain argon gas, shadow to atomization storehouse 2 Ring the air pressure in atomization storehouse 2, thus the shape of the solid granulates after affecting to cool down, pressure sensor 9 is then for detection atomization storehouse 2 Interior air pressure, when air pressure exceedes setting value, controller instruction control valve 10 is opened, and the gas in atomization storehouse 2 is pumped into back Closed cans 530 recycles.Control cabinet is existing structure, does not represent in the example shown.
Because electrode 102 service life of plasma torch 1 is limited, the operating time of the electrode 102 of plasma torch 1 arrives When reaching critical value, need to change electrode 102.Therefore it is preferred that as shown in Fig. 2 described plasma torch 1 is provided with timer 110, described timer 110 is connected with alarm.When timer 110 is used for the work of electrode 102 recording plasma torch 1 Long, when operating during long arrival critical value, timer 110 warning reminding operator can change electrode 102 in advance, prevents in work During electrode 102 break down impact produce.
In order to plasma torch 1 carries out anti-carbonization and the process of anti-tungsten, the torch spout 101 of described plasma torch 1 Shell be provided with water cooling plant 120.Water cooling plant 120 is existing apparatus, and it utilizes the spout of water circulation plasma torch 1 Shell carries out cooling treatment, to reduce the skin temperature of spout, thus playing anti-carbonization and the effect of anti-tungsten to a certain extent. Meanwhile, the torch spout 101 of described plasma torch 1 is high-temperature ceramic materials product.Replaced using high-temperature ceramic materials product The torch spout 101 that traditional metal material is made, overcomes metal material and will bring miscellaneous because of high temperature generation carbonization and tungsten Matter, affects the defect of the purity of pure titanium and titanium alloy powder.
Preferably, atomization storehouse 2 is provided with monitoring camera 11.Monitoring camera 11 can monitor in real time wiry Melting conditions, the picture that plasma torch 1 is acted on Metal wire material is recorded by monitoring camera 11, is converted into fusing shape Condition.If situations such as be not completely melt or superfuse occurs when monitoring wire fusing, the work of powder by atomization can be adjusted in time Skill parameter is it is ensured that wire is reasonably melted it is ensured that the quality producing powder has the uniformity of height.
With reference to embodiment, the specific embodiment of the present invention is further described, therefore the present invention is not limited System is among described scope of embodiments.All using the plasma atomization plant of the present invention in embodiment.
Embodiment 1
First, the raw material preparatory stage
From a diameter of 8mm circle pure titanium silk material as powder raw material processed, often a collection of raw material has detection material book, all full The requirement to chemical composition for sufficient American society for testing and materials ASTM.
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 inside reach the vacuum of 40kPa After degree, then it is filled with argon gas to normal pressure toward the inside, make the primary oxygen within atomization storehouse 2 and initial nitrogen content be less than 0.1%. All adopt oxygen and nitrogen content detector 8 to detect the content of oxygen and nitrogen in whole work process, make fusing and atomization process low Carry out in the environment of oxygen and low nitrogen, can automatic alarm 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, the wherein injection direction of each plasma torch 1 and silk A direction of vertically entering of material is in 40 ° of angles, and the high temperature hot gas stream of four plasma torch ejections focuses on same processing fusion zone.
Raw material is flowed into pure titanium silk material form, and straightening metal wire device ensure that the linearity of silk material, so that wire is hung down Directly downward, accurately reach plasma torch processing 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.
Wherein entering a speed is 0.1m/s, and plasma torch power is 30kW, and the thermal current spouting velocity of body torch mouth is 15L/min.In fusing and atomization process, monitoring camera 11 meeting monitor in real time is wiry to melt and atomization situation, will etc. The picture that gas ions torch is acted on Metal wire material is recorded, and is converted into melting conditions.If occurring when monitoring silk material fusing Situations such as be not completely melt or superfuse, whole equipment can adjust the technological parameter of powder by atomization in time it is ensured that silk material obtains Rational fusing is it is ensured that the quality producing pure titanium powder has the uniformity of height.
4th, powder cooling stage
After molten metal after fusing is atomized into tiny particle, gas cycle power device 510 is started working, and keeps Air pressure at air inlet 210 is 0.2Mpa, so that the argon gas in atomization storehouse 2 is circulated, and produces section cooling argon gas stream;Circulation argon Hot-air heater 6 can make the cooling gas temperature being passed through be maintained at 320~330 DEG C by the argon gas heating circulating.
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 being atomized unnecessary argon gas in storehouse in recycling can 530 by gas cycle power device 510, make argon gas in next time Can also reuse during work, reduce powder cost processed.After pure titanium powder is cooled to solid spherical, the argon that meeting be circulated Air-flow is brought into storage in Powder Recovery storehouse 4.
The pure titanium powder prepared is illustrated in figure 4 high spherical, particle uniformly, and satellite ball particle is few.
In addition the pure titanium powder composition prepared meets the standard to 1 grade of pure titanium material for the ASTM F67, and its composition is shown in Table 1, Powder property is shown in Table 3.
The pure titanium powder component list of table 1
Composition (%) 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
From a diameter of 8mm circular Ti6Al4V silk material as powder raw material processed, using the method for embodiment 1, only change portion Divide parameter, prepare titanium alloy powder.Wherein, the parameter of change is:
Vacuumize and the applying argon gas stage in atomization storehouse 2, primary oxygen and initial nitrogen content are less than 0.08%, when oxygen nitrogen contains Can automatic alarm interruption of work process when amount is more than 0.2%.
In melting and atomization step, entering a speed is 0.08m/s, and 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 powder prepared is as shown in figure 5, for high spherical, particle uniformly, and satellite ball particle is few.Separately The Ti6Al4V alloy powder composition prepared outward meets the standard to 23 grades of Ti6Al4V material for the ASTM F136, and its composition is shown in Table 2, powder property is shown in Table 3.
Table 2 Ti6Al4V alloy powder component list
Composition (%) Al V Fe C N H O Ti
Ti6Al4V alloy powder 6.0 4.1 0.24 0.02 0.01 0.012 0.09 Bal.
Comparative example 1
From a diameter of 8mm circle pure titanium silk material as powder raw material processed, using the method for embodiment 1, only changing section Parameter, prepares titanium alloy powder.Wherein, the parameter of change is:Air pressure at powder cooling stage, air inlet 210 is 0.8Mpa.Because inlet pressure is excessive, in cooling procedure, powder can be directly blown onto on atomization Cang Cebi, shorten powder The time of particle collapses balling-up, affect powder sphericity.
The titanium valve being obtained using said method, sphericity is deteriorated, and satellite ball particle increases, and affects final flow of powder Property, its powder property is shown in Table 3.
Comparative example 2
From a diameter of 8mm circle pure titanium silk material as powder raw material processed, using the method for embodiment 1, only changing section Parameter, prepares titanium alloy powder.Wherein, the parameter of change is:Air pressure at powder cooling stage, air inlet 210 is 0.1Mpa.Due to inlet pressure too small it is impossible to powder is dispelled, the DeGrain of section cooling, can send out in cooling procedure Green powder adheres to, and affects powder sphericity.
The titanium valve being obtained using said method, sphericity is deteriorated, and satellite ball particle increases, and fine powder recovery rate increases, its powder Last performance is shown in Table 3.
Comparative example 3
From a diameter of 8mm circle pure titanium silk material as powder raw material processed, using the method for embodiment 1, only changing section Parameter, prepares titanium alloy powder.Wherein, the parameter of change is:In powder cooling stage, the cooling gas temperature being passed through is Normal temperature.Due to going to cool down using normal temperature argon gas, the time that liquid particles are cooled to solid-state will greatly shorten, and most particle will Enough time is not had to be formed in the presence of surface tension spherical.
The titanium valve being obtained using said method, powder sphericity is deteriorated it is obvious that affecting the final mobility of powder, its powder Last performance is shown in Table 3.
The pure titanium of table 3 or Ti6Al4V alloy powder performance table

Claims (13)

1. the plasma atomization method preparing pure titanium or titanium alloy powder is it is characterised in that comprise the steps:
A, get the raw materials ready:Prepare titanium silk or the 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, atomized after pure titanium or titanium alloy particle;
C, cooling:It is passed through, in atomization storehouse, the inert gas that temperature is 300~500 DEG C, by the pure titanium after atomization or titanium alloy 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 preparing pure titanium or titanium alloy powder according to claim 1 it is characterised in that:Using The concrete grammar of titanium silk or titanium alloy wire atomized molten is by plasma torch:Using four equally distributed plasma torch, Each plasma torch injection direction is in 40 ° of angles with a direction of entering of silk material, and the thermal current that plasma torch sprays focuses on same One processing fusion zone, entering a speed is 0.05~0.2m/s, and plasma torch power is 20~100kW, plasma torch mouth Air-flow spouting velocity be 80~250L/min.
3. the plasma atomization method preparing pure titanium or titanium alloy powder according to claim 1 and 2 it is characterised in that:b In atmosphere of inert gases described in step, oxygen content is less than 0.3wt%, and nitrogen content is less than 0.3wt%.
4. the plasma atomization method preparing pure titanium or titanium alloy powder according to claim 3 it is characterised in that:B walks In rapid, first vacuumize, then be passed through inert gas to normal pressure, make to be inert atmosphere in atomization storehouse, then using plasma torch will Titanium silk or titanium alloy wire atomized molten.
5. the plasma atomization method preparing pure titanium or titanium alloy powder according to claim 1 and 2 it is characterised in that:c In step, at the air inlet of described inert gas, air pressure is 0.2~0.5Mpa.
6. prepare the plasma atomization plant of pure titanium or titanium alloy powder, including plasma torch (1), atomization storehouse (2), to atomization The powder collection device (4) that the feed system (3) of storehouse (2) feeding is connected with atomization storehouse (2) is connected with powder collection device (4) The gas purification circulatory system (5);It is characterized in that:
The described gas purification circulatory system (5) includes gas cycle power device (510);
Atomization storehouse (2) is provided with air inlet (210);Described gas cycle power device (510) and the air inlet being atomized storehouse (2) (210) pipeline connects;Heater (6) is provided with the path with air inlet (210) for the gas cycle power device (510) and controls The magnetic valve (7) of the air inlet pressure at air inlet (210) place.
7. the plasma atomization plant preparing pure titanium or titanium alloy powder according to claim 6 it is characterised in that:In mist Change storehouse (2) and be provided with exhaust outlet (220), described exhaust outlet (220) and air inlet (210) are oppositely arranged, described exhaust outlet (220) It is connected with gas cycle power device (510) pipeline.
8. the plasma atomization plant preparing pure titanium or titanium alloy powder according to claim 7 it is characterised in that:Described Exhaust outlet (220) is located at the top of atomization storehouse (2).
9. the plasma atomization plant preparing pure titanium or titanium alloy powder according to claim 8 it is characterised in that:In mist The inwall changing storehouse (2) is provided with oxygen and nitrogen content detector (8);Described oxygen and nitrogen content detector (8) is communicated to connect with controller.
10. the plasma atomization plant preparing pure titanium or titanium alloy powder according to claim 9 it is characterised in that:Institute State the gas purification circulatory system (5) and also include recycling can (530), described recycling can (530) and gas cycle power device (510) It is connected, the connecting path with gas cycle power device (510) for the recycling can (530) is provided with control valve (10);Be additionally provided with The pressure sensor (9) in atomization storehouse (2) of controller communication connection.
The 11. plasma atomization plants preparing pure titanium or titanium alloy powder according to claim 6 it is characterised in that:Institute State plasma torch (1) and be provided with timer (110);Described timer (110) is connected with alarm.
The 12. plasma atomization plants preparing pure titanium or titanium alloy powder according to claim 11 it is characterised in that:Institute The shell stating the torch spout (101) of plasma torch (1) is provided with water cooling plant (120).
The 13. plasma atomization plants preparing pure titanium or titanium alloy powder according to claim 12 it is characterised in that:? In atomization storehouse (2), monitoring camera (11) is installed.
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