CN105252009B - A kind of manufacture method of micro-fine spherical titanium powder - Google Patents
A kind of manufacture method of micro-fine spherical titanium powder Download PDFInfo
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Abstract
The present invention discloses a kind of micro-fine spherical titanium powder preparation method, belongs to metal and alloy powder preparing technical field.The present invention is with titanium sponge as raw material and makes bar or silk material；In melting chamber, using tundish being poured into after the heating fusing of round trip flight pulse per second (PPS) induced with laser under vacuum condition, proceed in aerochamber under vacuum condition, titanium melt is crushed by importing the noble gases of centrifugation stem bar, further crush through Laval nozzle again, micron-sized liquid titanium is obtained；Finally insert in argon filling medium tank, solidification cooling obtains micro-fine spherical titanium powder after screening.Of the invention quick by double femtosecond lasers, efficiently, melting titanium in pure ground can form uniform, stable, continuous aluminium alloy stream, and fusing, nebulization efficiency height, improve the yield and flour extraction of metal dust atomization, and sphericity height prepared by the present invention, oxygen content are low.
Description
Technical field
The present invention relates to powder process technical field, is related to a kind of manufacture method of micro-fine spherical titanium powder.
Background technology
Titanium has density low with titanium alloy, the premium properties such as specific strength is high, anti-corrosion, heat-resist, is widely used in boat
The field such as it.For the preparation means such as relatively forging, casting, have with the complicated metallic element of powder metallurgy process shaping form
The advantages of stock utilization is high, technological process is short, becoming reduces the important channel of titanium or titanium alloy parts manufacturing cost.Titanium valve
Performance be determine titanium or titanium alloy sintered metal product quality key factor.In recent years, prepare purity height, good sphericity,
Oxygen content is low and particle diameter is little titanium or titanium alloy powder and titanium or titanium alloy powder can be become as the metal powder material of 3D printing
The developing direction and study hotspot of last field of metallurgy.
At present, preparing spherical titanium and the method for titanium alloy powder has：Gas atomization, plasma rotating electrode process, radio frequency etc.
Ion nodularization method etc..Inert gas atomizer method, titanium or titanium alloy bar of the raw material for being used for certain specification will in crucible
Fuel rod melts, the liquation high-speed gas injection that will be produced by the nozzle of crucible bottom, makes molten metal in spray form, condensation
Form sized spherical titanium powder.The powder feature prepared using the method is that particle size distribution range is wider, and fine powder recovery rate is higher, and powder
Composition is less with the composition tolerances of foundry alloy bar, and impurity element can be good at control.As gas atomization is preparing titanium valve
During, the rate of cooling of the different size granule of cooled droplet formation is different, causes sphericity poor, planet granule
It is more；Hollow powders are produced inevitably when on the other hand due to gas breaking molten metal stream, these hollow powders are rear
In the metallurgical process of continued powder end, the internal flaw of material can be caused.
The ultrasonic atomizatio method technology mainly has two kinds：One kind is high-frequency electromagnetic oscillation to be converted into liquid machine vibration,
Droplet is made to crush mist formation；Thin drop layer, thin drop are formed in radiating surface when another kind can flow through supersonic concentrator
Layer evokes capillary wave in the presence of supersonic vibration, and when the amplitude of vibration plane reaches certain peak value, droplet is from ripple
Splash on peak and go out to form mist.It is inversely proportional to supersonic frequency using the particle diameter of spherical powder obtained in ultrasonic atomizatio method, ultrasonic mist
The operating frequency of change system is higher, and obtained spherical powder granularity is less.Directly can be shaken using ultrasound using ultrasonic atomizatio method
Dynamic atomization metal, noble gases consumption are only the 1% of gas atomization, and due to restrained effectively touching between powder
Hit, make that powder Satellite granule is substantially less, any surface finish, good sphericity, technique are continuous, controllable, stable, but which is to equipment
Require higher.
Plasma rotating electrode process：Metal or alloy is made into consutrodes, electrode end surface is received electric arc heated and is molten into
Liquid, the liquid of formation are subject to the dual function of centrifugal force and surface tension of liquid, and the centrifugal force for being rotated by electrode at a high speed will
Liquid is dished out and is ground into fine drop, is finally condensed into the method for powder.Can be according to the size of arc-plasma current and electrode
The particle diameter of rotation speed regulating and controlling powder.The chemical composition of prepared powder is approximate with raw bar material composition, and composition is easily controllable, and ball
Shape degree is good, and oxygen content is low, and without hollow, particle surface is smooth, and planet granule is few, the good fluidity of powder.But due to powder particle
Refinement depend on the rotating speed of plasma rotating electrode equipment, therefore the requirement to equipment is higher, and superfines are difficult to produce, often
The stock utilization of batch is not high.
As titanium sponge has good ductility and moulding so that titanium sponge is difficult to carry out powder using conventional method
It is broken, in laboratory it is many using the crisp broken technology of low temperature crushing a small amount of spongy titanium powder, but this breaking method cause it is whole spherical
The preparation technology of titanium valve is relatively costly, it is difficult to carry out commercial application.Titanium sponge is in loose porous spongy, so surface area
It is very big, it is relatively more active.As surface area is bigger, bigger with the contact surface of air, so activity is higher, Yi Yushui, gas occur
, easily there is oxidation in reaction.And using the titanium valve after dehydrogenation as material powder, it is spherical to carry out for thermal source to adopt radio frequency plasma
During the preparation of titanium valve, if the granularity of material powder can meet requirement (sufficiently fine), it is possible to obtain the very thin spherical titanium of granularity
Powder.This preparation technology with fine titanium powder as raw material, the greatest problem for existing are exactly that the oxygen content of product is high, in preparation technology
Oxygen supplement cannot be avoided, it is impossible to meet the use requirement of injection molding technique, this be by fine titanium powder in dehydrogenation and shattering process grain
Degree reduces, and caused by surface area increase, is also this inevitable as the technique that raw material prepares spherical powder with fine titanium valve.Together
When, what this raw material for preparing spherical powder was obtained using hydrogenation and dehydrogenization technique, it is spherical with being prepared with titanium sponge as initiation material
The technique of titanium valve compares, and it increased hydrogenation, broken, dehydrogenation, again broken operation, and increasing operation can not only affect product
Purity, and increase can production cost, this causes this technique to be difficult to industrialized production.
The content of the invention
It is an object of the invention to provide a kind of preparation method of micro-fine spherical titanium powder.
The technical solution adopted in the present invention：The manufacture method of micro-fine spherical titanium powder, including step in detail below：
Step 1, will make the titanium sponge of bar or silk material, be sent in melting chamber, very titanium sponge by continuous feeding machine
Under empty condition, using double femtosecond pulse laser inductions, using 2ns-10ns pulse spacings, 10fs-100fs pulse widths, sea
Continuous titanium heating fusing is obtained liquation；
Step 2, obtained liquation stream in step 1 is poured in tundish, aerochamber is proceeded to by mozzle；In vacuum bar
Under part, titanium melt is crushed by the noble gases of stem bar are centrifuged, then further crushed through Laval nozzle, micron order is obtained
Liquid titanium；
Step 3, obtained liquid titanium drop in step 2 is inserted in argon filling medium tank, and solidification is cooled to room temperature, obtains titanio powder
End, recycles ultrasonic vibrating screen screening matrix powder, micro-fine spherical titanium powder is obtained.
Forvacuum process is carried out to working chamber and aerochamber, vacuum reaches 1 × 10-4Pa--1×10-2Pa。
Described feeding machine raw material feed rate is 0.2kg/min-5kg/min.
In step 3, described noble gases are argon or helium, and atomizing pressure is 0.5MPa-10MPa, atomization gas stream
Measure as 20L/S-100L/S.
The present invention has following remarkable advantage compared with prior art：1st, the present invention subtracts without the need for crushing to titanium sponge
Lack production process, it is cost-effective；2nd, using round trip flight pulse per second (PPS) induced with laser, femtosecond laser energy deposition shape is circle, shape
Into the femtosecond laser plasma of space symmetr, and axisymmetricly sprayed, resulting titanium melt fineness ratio is more uniform, can
With quick, efficiently, pure ground melting titanium；3rd, using the ultrasonic secondary-atomizing method of centrifugation, by the guide functions in vortex centrifugal chamber,
Its spiral flow trace promotes the metal liquid formation sprawled with thin liquid film circumferentially, improves which in whole vibration plane
The uniformity sprawled, makes the powder granularity of first atomization more uniform；And for the second time through Laval nozzle, due to first contracting what is expanded afterwards
Structure, keeps gas velocity not dissipate, more kinetic energy is converted into crushing energy, so as to further fully be broken to metal
It is broken, reduce the granularity of atomized metal pow der, sphericity is high, and oxygen content is low.
Description of the drawings
Fig. 1 is the equipment schematic diagram of the preparation method of micro-fine spherical titanium powder of the present invention；
Wherein, 1 is metal wire material reel；2 is continuous feeding machine；3 is femto-second laser；4 is tundish；5 is twin-stage ring
Seam close-coupled nozzle；6 is vacuum system；7 is powder collecting device.
Specific embodiment
Below in conjunction with the accompanying drawings the present invention is further described：
Step 1, with titanium sponge as raw material, is made into bar or silk material.Titanium sponge on metal wire material reel 1 is passed through
Continuous feeding machine 2 is fed in melting chamber, carries out evacuation using vacuum system 6, and two big work(are arranged in melting chamber
The femto-second laser 3 of rate.Using round trip flight pulse per second (PPS) induced with laser, the pulse spacing is 2-10ns.In femto-second laser 3, pass through
The birefringece crystal and prism insertion loss of fs-laser system are adjusted, changes the output wavelength of laser, so as to by pulse width
In 10-100fs, laser focusing punctures air in atmosphere and produces plasma, and femtosecond laser energy deposition shape is circle for control
Shape, result in formation of the femtosecond laser plasma of space symmetr, and plasma is then sprayed into axial symmetry in melting chamber
Penetrate, titanium sponge bar or silk material heat fusing in the presence of plasma, as plasma is axisymmetricly to be sprayed
, resulting titanium melt fineness ratio is more uniform.
Step 2, liquation stream is poured in the tundish 4 of powder by atomization equipment, is then proceeded in aerochamber by mozzle.
It is indoor in atomization, evacuation is carried out using vacuum system 6, then using twin-stage circumferential weld close-coupled nozzle 5, ground floor is using centrifugation
Stem bar, when melt flows through centrifugation stem bar with certain flow, by the guide functions in vortex centrifugal chamber, makes the molten metal bodily form of outflow
Into hollow wimble structure, its spiral flow trace accelerates metal liquid sprawling on vibration plane, promotes liquid along week
To the formation sprawled with thin liquid film, improve the uniformity that metal liquid is sprawled in whole vibration plane, when the amplitude of vibration plane
When reaching certain peak value, thin liquid layer is crashed to pieces in the presence of supersonic vibration, and the droplet for evoking splashes from crest and goes out
Mist is formed, primary atomization is realized.High frequency, powerful piezoelectric transducer are adopted simultaneously, can be substantially reduced atomized metal pow der
Granularity.And for the second time through Laval nozzle, the spouting velocity of gas is considerably increased, simultaneously because the structure for expanding afterwards that first contracts
Design, is made air-flow hardly be contacted with duct wall, maintains not dissipating for gas velocity, more kinetic energy are converted into broken
Can, so as to further sufficiently be crushed to metal.
Granular liquid titanium drop is inserted powder collecting device 7, in argon filling medium tank is cooled to its solidification by step 3
Room temperature, obtains matrix powder, recycles ultrasonic vibrating screen screening matrix powder, screens out desired spherical powder.
Embodiment 1
With titanium sponge as raw material, bar or silk material are made into, melting chamber is fed into by continuous feeding machine, raw material enters
It is 0.2kg/min to speed, using round trip flight pulse per second (PPS) induced with laser, the pulse spacing is 2ns, pulse width 10fs, laser focusing
Puncture air in atmosphere and produce plasma, titanium sponge bar or silk material heat fusing in the presence of plasma.By liquation
Stream is poured in the tundish of powder by atomization equipment, is then proceeded in aerochamber by mozzle, and water conservancy diversion bore is 4mm.To mist
Changing room and melting chamber carries out evacuation process, and vacuum reaches 1 × 10-4Pa.Then titanium melt flows through centrifugation stream with certain flow
Mouth, thin liquid layer are crashed to pieces in the presence of supersonic vibration, and the droplet for evoking splashes from crest and goes out to be formed that mist evokes is little
Drop splashes from crest and goes out to form mist, realizes primary atomization.The nozzle second layer adopts Laval nozzle structure, primary atomization
After the completion of, atomizing medium forms the ultrasound wave that high frequency is agitated in the exit of Laval nozzle, and ultrasound wave is completed with primary atomization
Fused solution metal afterwards meets, and starts secondary-atomizing so as to be atomized as more small drop.Atomizing pressure is controlled in 2-
4MPa, atomization gas flow are 20L/S.Granular liquid titanium drop is inserted makes its solidification be cooled to room temperature in argon filling medium tank,
Matrix powder is obtained, ultrasonic vibrating screen screening matrix powder is recycled.Screen out desired spherical powder.
The spherical powder analysis result for preparing is：Spherical rate is 99%, and oxygen content is 0.09wt%, and particle mean size is
22μm。
Embodiment 2
With titanium sponge as raw material, bar or silk material are made into, melting chamber is fed into by continuous feeding machine, raw material enters
It is 5kg/min to speed, using round trip flight pulse per second (PPS) induced with laser, the pulse spacing is 10ns, pulse width 100fs, laser focusing
Puncture air in atmosphere and produce plasma, titanium sponge bar or silk material heat fusing in the presence of plasma.By liquation
Stream is poured in the tundish of powder by atomization equipment, is then proceeded in aerochamber by mozzle, and water conservancy diversion bore is 5mm.To mist
Changing room and melting chamber carries out evacuation process, and vacuum reaches 1 × 10-2Pa.Then titanium melt flows through centrifugation stream with certain flow
Mouth, thin liquid layer are crashed to pieces in the presence of supersonic vibration, and the droplet for evoking splashes from crest and goes out to form mist, realize primary
Atomization.The nozzle second layer adopts Laval nozzle structure, after the completion of primary atomization, outlet of the atomizing medium in Laval nozzle
Place, forms the ultrasound wave that high frequency is agitated, and ultrasound wave is met with the fused solution metal after the completion of primary atomization, starts secondary mist
Change so as to be atomized as more small drop.Atomizing pressure is controlled in 2.5-5MPa, and atomization gas flow is 100L/S.By granule
The liquid titanium drop of change is inserted and makes its solidification be cooled to room temperature in argon filling medium tank, obtains matrix powder, recycles ultrasonic vibrating screen sieve
Divide matrix powder.Screen out desired spherical powder.
The spherical powder analysis result for preparing is：Spherical rate is 99%, and oxygen content is 0.10wt%, and particle mean size is
14μm。
Embodiment 3
With titanium sponge as raw material, bar or silk material are made into, melting chamber is fed into by continuous feeding machine, raw material enters
It is 1.5kg/min to speed, using round trip flight pulse per second (PPS) induced with laser, the pulse spacing is 4ns, pulse width 100fs, laser focusing
Puncture air in atmosphere and produce plasma, titanium sponge bar or silk material heat fusing in the presence of plasma.By liquation
Stream is poured in the tundish of powder by atomization equipment, is then proceeded in aerochamber by mozzle, and water conservancy diversion bore is 4mm.To mist
Changing room and melting chamber carries out evacuation process, and vacuum reaches 1 × 10-3Pa.Then titanium melt flows through centrifugation stream with certain flow
Mouth, thin liquid layer are crashed to pieces in the presence of supersonic vibration, and the droplet for evoking splashes from crest and goes out to form mist, realize primary
Atomization.The nozzle second layer adopts Laval nozzle structure, after the completion of primary atomization, outlet of the atomizing medium in Laval nozzle
Place, forms the ultrasound wave that high frequency is agitated, and ultrasound wave is met with the fused solution metal after the completion of primary atomization, starts secondary mist
Change so as to be atomized as more small drop.Atomizing pressure is controlled in 6.5-10MPa, and atomization gas flow is 40L/S.By granule
The liquid titanium drop of change is inserted and makes its solidification be cooled to room temperature in argon filling medium tank, obtains matrix powder, recycles ultrasonic vibrating screen sieve
Divide matrix powder.Screen out desired spherical powder.
The spherical powder analysis result for preparing is：Spherical rate is 99%, and oxygen content is 0.08wt%, and particle mean size is
7μm。
Embodiment 4
With titanium sponge as raw material, bar or silk material are made into, melting chamber is fed into by continuous feeding machine, raw material enters
It is 3kg/min to speed, using round trip flight pulse per second (PPS) induced with laser, the pulse spacing is 6ns, and pulse width 85fs, laser focusing exist
Puncture air in air and produce plasma, titanium sponge bar or silk material heat fusing in the presence of plasma.By liquation stream
Pour in the tundish of powder by atomization equipment, then proceeded in aerochamber by mozzle, water conservancy diversion bore is 5mm.To atomization
Room and melting chamber carry out evacuation process, and vacuum reaches 1 × 10-4Pa.Then titanium melt flows through centrifugation stem bar with certain flow,
Thin liquid layer is crashed to pieces in the presence of supersonic vibration, and the droplet for evoking splashes from crest and goes out to form mist, realizes primary mist
Change.The nozzle second layer adopt Laval nozzle structure, after the completion of primary atomization, atomizing medium in the exit of Laval nozzle,
The ultrasound wave that high frequency is agitated is formed, ultrasound wave is met with the fused solution metal after the completion of primary atomization, start secondary-atomizing, make
Its atomization is more small drop.Atomizing pressure is controlled in 3.5-7MPa, and atomization gas flow is 60L/S.By granular liquid
Titanium drop is inserted and makes its solidification be cooled to room temperature in argon filling medium tank, obtains matrix powder, recycles ultrasonic vibrating screen screening titanio
Powder.Screen out desired spherical powder.
The spherical powder analysis result for preparing is：Spherical rate is 99%, and oxygen content is 0.09wt%, and particle mean size is
11μm。
Embodiment 5
With titanium sponge as raw material, bar or silk material are made into, melting chamber is fed into by continuous feeding machine, raw material enters
It is 4kg/min to speed, using round trip flight pulse per second (PPS) induced with laser, the pulse spacing is 8ns, and pulse width 65fs, laser focusing exist
Puncture air in air and produce plasma, titanium sponge bar or silk material heat fusing in the presence of plasma.By liquation stream
Pour in the tundish of powder by atomization equipment, then proceeded in aerochamber by mozzle, water conservancy diversion bore is 4mm.To atomization
Room and melting chamber carry out evacuation process, and vacuum reaches 1 × 10-3Pa.Then titanium melt flows through centrifugation stem bar with certain flow,
Thin liquid layer is crashed to pieces in the presence of supersonic vibration, and the droplet for evoking splashes from crest and goes out to form mist, realizes primary mist
Change.The nozzle second layer adopt Laval nozzle structure, after the completion of primary atomization, atomizing medium in the exit of Laval nozzle,
The ultrasound wave that high frequency is agitated is formed, ultrasound wave is met with the fused solution metal after the completion of primary atomization, start secondary-atomizing, make
Its atomization is more small drop.Atomizing pressure is controlled in 4-8.5MPa, and atomization gas flow is 80L/S.By granular liquid
Titanium drop is inserted and makes its solidification be cooled to room temperature in argon filling medium tank, obtains matrix powder, recycles ultrasonic vibrating screen screening titanio
Powder.Screen out desired spherical powder.
The spherical powder analysis result for preparing is：Spherical rate is 99%, and oxygen content is 0.09wt%, and particle mean size is
25μm。
Claims (4)
1. a kind of manufacture method of micro-fine spherical titanium powder, it is characterised in that including comprising the following steps that：
Step 1, will make the titanium sponge of bar or silk material, titanium sponge is sent in melting chamber by continuous feeding machine, vacuum bar
Under part, using double femtosecond pulse laser inductions, using 2ns-10ns pulse spacings, 10fs-100fs pulse widths, titanium sponge
Heating fusing is obtained liquation；
Step 2, obtained liquation stream in step 1 is poured in tundish, aerochamber is proceeded to by mozzle；In vacuum condition
Under, titanium melt is crushed by the noble gases of stem bar are centrifuged, then further crushed through Laval nozzle, be obtained micron-sized
Liquid titanium；
Step 3, obtained liquid titanium drop in step 2 is inserted in argon filling medium tank, and solidification is cooled to room temperature, obtains matrix powder,
Ultrasonic vibrating screen screening matrix powder is recycled, micro-fine spherical titanium powder is obtained.
2. the manufacture method of micro-fine spherical titanium powder according to claim 1, it is characterised in that in step 1 and step 2,
Working chamber and aerochamber carry out forvacuum process, and vacuum reaches 1 × 10-4Pa--1×10-2Pa。
3. the manufacture method of micro-fine spherical titanium powder according to claim 1, it is characterised in that in step 2, feeding machine are former
Material feed rate is 0.2kg/min-5kg/min.
4. the manufacture method of micro-fine spherical titanium powder according to claim 1, it is characterised in that in step 3, described is lazy
Property gas be argon or helium, atomizing pressure is 0.5MPa-10MPa, and atomization gas flow is 20L/S-100L/S.
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| CN106914626B (en) * | 2017-04-10 | 2020-02-21 | 西安铂力特增材技术股份有限公司 | Preparation device and preparation method of superfine metal powder |
| CN107584128A (en) * | 2017-08-24 | 2018-01-16 | 龙岩紫荆创新研究院 | Sized spherical titanium powder prepared by the preparation method and this method of a kind of micron order increasing material manufacturing sized spherical titanium powder |
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| CN108480653A (en) * | 2018-06-29 | 2018-09-04 | 中国科学院上海光学精密机械研究所 | The device and method of hollow over spherical powder is prepared based on femtosecond laser |
| CN108580913A (en) * | 2018-07-10 | 2018-09-28 | 深圳微纳增材技术有限公司 | A kind of 3D printing noble metal powder preparation method |
| CN109967755B (en) * | 2019-05-14 | 2023-08-18 | 湖州恒合科技有限公司 | Spherical fine metal powder production system and method thereof |
| CN113547126A (en) * | 2021-06-29 | 2021-10-26 | 鞍钢股份有限公司 | Method for preparing fine powder by tight coupling gas atomization for preventing guide pipe from being blocked |
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