CN204934612U - A kind of device preparing the superfine sized spherical titanium powder that 3D prints - Google Patents
A kind of device preparing the superfine sized spherical titanium powder that 3D prints Download PDFInfo
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- CN204934612U CN204934612U CN201520622223.1U CN201520622223U CN204934612U CN 204934612 U CN204934612 U CN 204934612U CN 201520622223 U CN201520622223 U CN 201520622223U CN 204934612 U CN204934612 U CN 204934612U
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Abstract
The utility model relates to a kind of device preparing the superfine sized spherical titanium powder that 3D prints, comprise auto feed system, insulation dynamic sealing device, annular aerosolization nozzle, spray chamber, arc cathode melting well, heat dissipating housing, protective cover, receive powder tank, supersonic gas pulverising mill and radio frequency plasma reactor, the utility model adopts gas atomization device to carry out elementary powder process to former titanium valve, and then utilize pulverizing, titanium valve granularity is further reduced, and then using plasma device processing titanium valve, utilize the high energy characteristic of radio frequency plasma, by titanium valve particle in irregular shape with carrying gas inject plasma torch, irregular titanium valve is heated rapidly and melts, the particle of melting forms the very high drop of sphericity under capillary effect, and under high thermograde quick solidification, form good sphericity, purity is high, hypoxic superfine sized spherical titanium powder.
Description
Technical field
The utility model relates to a kind of device preparing the superfine sized spherical titanium powder that 3D prints, and belongs to metal powder preparation technical field.
Background technology
3D printing technique is particularly suitable for developing high added value complex structure product, personalized customization and the link such as checking of design and R&D before being applied to large-scale production.Compared with current international most advanced level, in the research and development of moulding material needed for China prints at 3D, still there is a big difference, and design of material and preparation technology mainly follow the tracks of foreign progress at present.In 3D printing with in moulding material product, the almost complete dependence on import such as domestic required fine grain spherical titanium and titanium alloy powder.The shortage of high-quality 3D printing moulding material is one of bottleneck key element of restriction China 3D printing technique propagation and employment.
For 3D printing fine-grained metals titanium powder, technical process has very high requirement to dusty material, as particle size range 20-50 micron, high sphericity, low oxygen content etc.Existing titanium valve technology of preparing mainly contains: electrochemical process, mechanical attrition method, reducing process etc.The titanium that current existing preparation method goes out or titanium alloy powder pattern are difficult to control, and particle diameter is thicker and distribution is wider.Wherein, electrochemistry, reducing process cost are higher, and the solvent used and reducing agent have severe toxicity more, and easily introduce the impurity such as halogen, sulphur; Ball-milling method can only be used for fragile material, the higher and uncontrollable powder particle pattern of usual oxygen content.Therefore, the preparation method of the 3D printing metal or alloy powder of current pressing needs low cost, high-purity, size tunable.
For above-mentioned domain background, in order to solve the limitation of prior art, the utility model provides a kind of and is applicable to device of the superfine sized spherical titanium powder of 3D printing technique and preparation method thereof.
Summary of the invention
The purpose of this utility model is to provide that a kind of production efficiency is high, good sphericity, the device of the superfine sized spherical titanium powder that the low and preparation 3D of low production cost of oxygen content prints.
The utility model, in order to reach above-mentioned utility model object, takes following technical scheme:
A kind of device preparing the superfine sized spherical titanium powder that 3D prints, comprise auto feed system, insulation dynamic sealing device, annular aerosolization nozzle, spray chamber, arc cathode melting well, heat dissipating housing, protective cover, receive powder tank, supersonic gas pulverising mill and radio frequency plasma reactor, above described spray chamber, auto feed system is set, described auto feed system and spray chamber are provided with insulation dynamic sealing device, below described insulation dynamic sealing device, annular aerosolization nozzle is set, described annular aerosolization nozzle center is provided with arc cathode melting well, the inside of described spray chamber is provided with heat dissipating housing, heat dissipating housing top is provided with protective cover, the below of described spray chamber is provided with receives powder tank, supersonic gas pulverising mill is connected with below described receipts powder tank, this supersonic gas pulverising mill is connected with described radio frequency plasma reactor, wherein, described radio frequency plasma reactor comprises the reactor body of sealed environment, be arranged on the quartz ampoule on reactor body, be sleeved on the radio-frequency induction coil on the outer wall of quartz ampoule, and the raw meal ascending pipe to be connected with reactor body top seal, working gas input pipe and protective gas input pipe, described raw meal ascending pipe is arranged on the center of reactor body, and be tightly connected with the discharging opening of supersonic gas pulverising mill, described working gas input pipe and protective gas input pipe lay respectively at the left and right sides of raw meal ascending pipe, the bottom of described reactor body is also provided with rapid condensation room, the below of rapid condensation room is provided with titanium valve collecting region.
Further, described auto feed system, insulation dynamic sealing device and arc cathode melting well are installed on the same axis.
Further, the center of the center of described heat dissipating housing, protective cover and arc cathode melting well on the same axis.
Further, the specification of described titanium bar is φ 50mm × 500mm.
Further, the final vacuum of described device is 1 × 10
-5pa.
Further, be provided with cathode power and stabilising arc coil around the borehole wall of described arc cathode melting well, melting down-hole portion is provided with Igniting unit.
Further, described spray chamber outer wall is provided with recirculated cooling water, peep hole and vacuum interface; Described receipts powder tank is with water-cooling system.
Further, described reactor body is also provided with water-cooling system.
Further, the granularity of the spherical titanium powder of described superfine is 10 ~ 50 μm, and oxygen content is 0.05 ~ 0.2wt%.
The technological process of the preparation method that the utility model provides and principle are: adopt high pure metal titanium bar to be raw material, under the environment of inert gas, form molten metal or drip by electric arc heated, and then prepare elementary sized spherical titanium powder by high-pressure atomization nozzle; Elementary sized spherical titanium powder granularity is larger, the less secondary sized spherical titanium powder of granularity is obtained by supersonic gas pulverising mill, finally the secondary sized spherical titanium powder prepared is injected into radio frequency plasma torch reactor reaction, titanium valve larger for granularity is heated rapidly in plasmatorch and melts, the particle of melting forms the very high drop of sphericity under capillary effect, and under high thermograde quick solidification, formed good sphericity, high, the hypoxic superfine sized spherical titanium powder of purity.
Because plasma has the large characteristic of high temperature, Gao Han, high activity and thermograde, make thermal source in the spheroidising of micron-submicron and some nano-powder material with plasma, there is larger technical advantage.Simultaneously, radio frequency plasma technology and equipment due to its do not bring any impurity into, run continual and steady, material processed speed is fast, production capacity is high and equipment manufacturing cost is moderate, therefore dusty material technical field is applied more broadly in, and radio frequency plasma technology can be prepared, and component is even, defect is few, the titanium valve of good fluidity, good sphericity, therefore be a kind of technical solution approach preferably, this is also the reason that the utility model takes radio frequency plasma technology.
The beneficial effects of the utility model: electric arc melting technology and vacuum inert gas atomization technology of preparing combine by the utility model, overturn the feature of melting bottom, traditional gas-atomized powder technology middle and upper part atomization, achieve Metal Melting device below atomizer, reach the Close-Coupled Gas Atomization preparation method of titanium powder, avoid in traditional Close-Coupled Gas Atomization mode because melting kettle, flow guide system are to the pollution of metal bath; The high temperature nodularization simultaneously adopted in the utility model radio-frequency technique and rapid condensation spheronization techniques, can improve sphericity and the purity of titanium valve, decrease the problem of oxidation of titanium valve in nodularization process simultaneously, powder injects from Plasma Center top simultaneously, volume is large, and heating is abundant, electrodeless pollution; Superfine sized spherical titanium powder oxygen content prepared by the utility model is low, is no more than 0.20wt%.Powder prepared by the utility model has good sphericity, and powder property uniformity is good, cost is low, Oxygen potential is high, good fluidity, applicable industrialization promotion.
Accompanying drawing explanation
A kind of structural representation preparing the device of the superfine sized spherical titanium powder that 3D prints that Fig. 1 provides for the utility model;
Fig. 2 is the scanning electron microscope (SEM) photograph of 20 μm of ball-type titanium valves that the utility model obtains;
Fig. 3 is the scanning electron microscope (SEM) photograph of 50 μm of ball-type titanium valves that the utility model obtains.
Detailed description of the invention
First the utility model adopts gas atomization device to carry out elementary powder process to former titanium valve, and then utilize pulverizing, titanium valve granularity is further reduced, and then using plasma device processing titanium valve, utilize the high energy characteristic of radio frequency plasma, by titanium valve particle in irregular shape with carrying gas inject plasma torch, irregular titanium valve is heated rapidly and melts, the particle of melting forms the very high drop of sphericity under capillary effect, and under high thermograde quick solidification, form good sphericity, purity is high, hypoxic superfine sized spherical titanium powder.
The utility model mainly comprises gas atomization device, supersonic gas pulverising mill and radio frequency plasma reactor, and these equipment composition is stable, and continuous operation, what production capacity was high can suitability for industrialized production system.
The utility model adopts high temperature nodularization and rapid condensation spheronization techniques, and all employs circulating water in course of reaction, both ensure that the sealing system energy of equipment, has additionally reduced the use amount of inert gas, effectively reduce costs, ensures the purity asking shape titanium valve.
According to the nodularization of superfine titanium valve, the utility model requires that the designed system set up makes the adjusting range of every technical parameter be widened, be conducive to optimizing the parameters combination such as plasma power, density, air-flow, join with the appropriate powder meeting titanium valve treatment characteristic and the nodularization effect carrying gas and obtains the best.As shown in Figure 2,3, Oxygen potential almost reaches 100%, and spheroidal particle pattern is all good.
Below in conjunction with embodiment, the utility model is described in further detail, but the utility model is not limited to following examples.
The utility model provides a kind of device preparing the superfine sized spherical titanium powder that 3D prints, comprise auto feed system 1, insulation dynamic sealing device 2, annular aerosolization nozzle 3, spray chamber 4, arc cathode melting well 5, heat dissipating housing 6, protective cover 7, receive powder tank 8, supersonic gas pulverising mill 9 and radio frequency plasma reactor 10, on described spray chamber, 4 sides arrange auto feed system 1, described auto feed system 1 is provided with spray chamber 4 dynamic sealing device 2 that insulate, below described insulation dynamic sealing device 2, annular aerosolization nozzle 3 is set, described annular aerosolization nozzle 3 center is provided with arc cathode melting well 5, the inside of described spray chamber 4 is provided with heat dissipating housing 6, heat dissipating housing 6 top is provided with protective cover 7, the below of described spray chamber 4 is provided with receives powder tank 8, supersonic gas pulverising mill 9 is connected with below described receipts powder tank 8, this supersonic gas pulverising mill 9 is connected with described radio frequency plasma reactor 10, wherein, described radio frequency plasma reactor 10 comprises the reactor body 11 of sealed environment, be arranged on the quartz ampoule 12 on reactor body 11, be sleeved on the radio-frequency induction coil 13 on the outer wall of quartz ampoule 12, and the raw meal ascending pipe 14 to be connected with reactor body 11 top seal, working gas input pipe 15 and protective gas input pipe 16, described raw meal ascending pipe 14 is arranged on the center of reactor body 11, and be tightly connected with the discharging opening of supersonic gas pulverising mill 9, described working gas input pipe 15 and protective gas input pipe 16 lay respectively at the left and right sides of raw meal ascending pipe 14, the bottom of described reactor body 11 is also provided with rapid condensation room 17, the below of rapid condensation room 17 is provided with titanium valve collecting region 18, wherein, described auto feed system 1, insulation dynamic sealing device 2 and arc cathode melting well 5 are installed on the same axis, described heat dissipating housing 6, the center of protective cover 7 and the center of arc cathode melting well 5 are on the same axis.
The specification of the titanium bar that the utility model is chosen is φ 50mm × 500mm, and the final vacuum of device is 1 × 10
-5pa; Be provided with cathode power and stabilising arc coil around the borehole wall of arc cathode melting well, melting down-hole portion is provided with Igniting unit; Spray chamber outer wall is provided with recirculated cooling water, peep hole and vacuum interface; Described receipts powder tank is with water-cooling system; Reactor body is also provided with water-cooling system.
Meanwhile, the utility model additionally provides a kind of method preparing the superfine sized spherical titanium powder that 3D prints, and comprises the following steps:
(1) vacuumize whole device, vacuum reaches 1 × 10
-5pa, is then full of whole device by inert gas argon gas;
(2) the arc cathode melting well sent in spray chamber by dynamic sealing device by auto feed system by titanium bar is inner, using highly purified titanium bulk as anode, using melting well as negative electrode, under the environment of inert gas argon gas, high intensity electric arc is formed by discharge process, striking current is 1000A, and arc voltage is 50V;
(3) under the effect of high intensity electric arc, titanium bar carries out elementary fusing and forms continuous print metal liquid stream or drop;
(4) free-falling under gravity of the metal liquid stream obtained or drop, after leaving the high intensity electric arc thermal treatment zone, be ground into tiny molten drop by the inert gas that annular aerosolization nozzle produces, the pressure of atomization gas is 5 ~ 10MPa, and atomization gas flow is 50-150L/S;
(5) molten drop is in descent, becomes titanium powder through nodularization, cooled and solidified, and fall into the elementary titanium powder of the interior formation of receipts powder tank of spray chamber lower end, now, the granularity of titanium valve is 50-100 μm;
(6) the elementary titanium valve received in powder tank is imported in supersonic gas pulverising mill, pulverize, pulverize and obtain the secondary titanium powder that particle mean size is 30 μm;
(7) using above-mentioned secondary titanium powder as raw material, adopt radio frequency plasma carry out spheroidising, specifically adopt following steps: adopt argon gas as plasma gas, i.e. working gas, radio frequency plasma power output is 30kw-80kw; Protective gas and working gas use argon gas, and shielding gas flow amount is selected at 0.8m
3/ h-1.9m
3/ h, working gas flow is selected at 0.5m
3/ h-1.5m
3/ h, makes the plasmatorch that formation is stable; Then adopt argon gas, as carrier gas, secondary titanium powder is delivered to plasmatorch central authorities; the speed of conveying powder is selected at 40g/min-200g/min; secondary titanium powder is heated rapidly through plasmatorch and melts in dropping process; the particle of melting forms the very high drop of sphericity under capillary effect; then under the protection of argon gas, enter condensation chamber fast carry out rapid cooled and solidified; form the spherical titanium powder of superfine that sphericity is very high; the granularity of the spherical titanium powder of superfine of preparation is 10 ~ 50 μm, and oxygen content is 0.05 ~ 0.2wt%.
Embodiment 1
First choose the titanium bar that specification is φ 50mm × 500mm, titanium bar is delivered to arc cathode melting well by auto feed system inner, then vacuumize whole device, vacuum reaches 1 × 10
-5pa, is then full of whole device by inert gas argon gas; Then using highly purified titanium bulk as anode, using melting well as negative electrode, under the environment of inert gas argon gas, form high intensity electric arc by discharge process, striking current is 1000A, and arc voltage is 50V; Under the effect of high intensity electric arc, titanium bar carries out elementary fusing and forms continuous print metal liquid stream or drop; The metal liquid stream obtained or drop free-falling under gravity, after leaving the high intensity electric arc thermal treatment zone, be ground into tiny molten drop by the inert gas that annular aerosolization nozzle produces, the pressure of atomization gas is 5MPa, and atomization gas flow is 50L/S; Molten drop, in descent, becomes titanium powder through nodularization, cooled and solidified, and fall into the elementary titanium powder of the interior formation of receipts powder tank of spray chamber lower end, now, the granularity of titanium valve is 100 μm; The elementary titanium valve received in powder tank is imported in supersonic gas pulverising mill, pulverizes, pulverize and obtain the secondary titanium powder that particle mean size is 30 μm; Using above-mentioned secondary titanium powder as raw material, adopt radio frequency plasma to carry out spheroidising, specifically adopt following steps: adopt argon gas as plasma gas, i.e. working gas, radio frequency plasma power output is 80kw; Protective gas and working gas use argon gas, and shielding gas flow amount is selected at 1.9m
3/ h, working gas flow is selected at 1.5m
3/ h, makes the plasmatorch that formation is stable; Then adopt argon gas, as carrier gas, secondary titanium powder is delivered to plasmatorch central authorities; the speed of conveying powder is selected at 200g/min; secondary titanium powder is heated rapidly through plasmatorch and melts in dropping process; the particle of melting forms the very high drop of sphericity under capillary effect; then under the protection of argon gas, enter condensation chamber fast carry out rapid cooled and solidified, form the spherical titanium powder of superfine that sphericity is very high.
The spherical powder analysis result prepared is: spherical rate 99%, oxygen content 0.07wt%, average grain diameter is 10 μm.
Embodiment 2
First choose the titanium bar that specification is φ 50mm × 500mm, titanium bar is delivered to arc cathode melting well by auto feed system inner, then vacuumize whole device, vacuum reaches 1 × 10
-5pa, is then full of whole device by inert gas argon gas; Then using highly purified titanium bulk as anode, using melting well as negative electrode, under the environment of inert gas argon gas, form high intensity electric arc by discharge process, striking current is 1000A, and arc voltage is 50V; Under the effect of high intensity electric arc, titanium bar carries out elementary fusing and forms continuous print metal liquid stream or drop; The metal liquid stream obtained or drop free-falling under gravity, after leaving the high intensity electric arc thermal treatment zone, be ground into tiny molten drop by the inert gas that annular aerosolization nozzle produces, the pressure of atomization gas is 10MPa, and atomization gas flow is 150L/S; Molten drop, in descent, becomes titanium powder through nodularization, cooled and solidified, and fall into the elementary titanium powder of the interior formation of receipts powder tank of spray chamber lower end, now, the particle mean size of titanium valve is 50 μm; The elementary titanium valve received in powder tank is imported in supersonic gas pulverising mill, pulverizes, pulverize and obtain the secondary titanium powder that particle mean size is 30 μm; Using above-mentioned secondary titanium powder as raw material, adopt radio frequency plasma to carry out spheroidising, specifically adopt following steps: adopt argon gas as plasma gas, i.e. working gas, radio frequency plasma power output is 30kw; Protective gas and working gas use argon gas, and shielding gas flow amount is selected at 0.8m
3/ h, working gas flow is selected at 0.5m
3/ h, makes the plasmatorch that formation is stable; Then adopt argon gas, as carrier gas, secondary titanium powder is delivered to plasmatorch central authorities; the speed of conveying powder is selected at 40g/min; secondary titanium powder is heated rapidly through plasmatorch and melts in dropping process; the particle of melting forms the very high drop of sphericity under capillary effect; then under the protection of argon gas, enter condensation chamber fast carry out rapid cooled and solidified, form the spherical titanium powder of superfine that sphericity is very high.
The spherical powder analysis result prepared is: spherical rate 99%, oxygen content 0.12wt%, average grain diameter is 10 μm.
As can be seen from Fig. 2,3, the shape of the titanium valve after shaping is spherical, and the surface of each particle is extremely smooth.
Draw through overtesting, the apparent density of the titanium valve after plasma spheroidization processing process increases.The increase of apparent density and the change of grain shape are conducive to improving titanium valve mobility.
In a word, the good fluidity of superfine sized spherical titanium powder prepared by the utility model, Oxygen potential is high, sphericity is high, oxygen content is low.
Claims (8)
1. prepare the device of the superfine sized spherical titanium powder that 3D prints for one kind, comprise auto feed system, insulation dynamic sealing device, annular aerosolization nozzle, spray chamber, arc cathode melting well, heat dissipating housing, protective cover, receive powder tank, supersonic gas pulverising mill and radio frequency plasma reactor, it is characterized in that, above described spray chamber, auto feed system is set, described auto feed system and spray chamber are provided with insulation dynamic sealing device, below described insulation dynamic sealing device, annular aerosolization nozzle is set, described annular aerosolization nozzle center is provided with arc cathode melting well, the inside of described spray chamber is provided with heat dissipating housing, heat dissipating housing top is provided with protective cover, the below of described spray chamber is provided with receives powder tank, supersonic gas pulverising mill is connected with below described receipts powder tank, this supersonic gas pulverising mill is connected with described radio frequency plasma reactor, wherein, described radio frequency plasma reactor comprises the reactor body of sealed environment, be arranged on the quartz ampoule on reactor body, be sleeved on the radio-frequency induction coil on the outer wall of quartz ampoule, and the raw meal ascending pipe to be connected with reactor body top seal, working gas input pipe and protective gas input pipe, described raw meal ascending pipe is arranged on the center of reactor body, and be tightly connected with the discharging opening of supersonic gas pulverising mill, described working gas input pipe and protective gas input pipe lay respectively at the left and right sides of raw meal ascending pipe, the bottom of described reactor body is also provided with rapid condensation room, the below of rapid condensation room is provided with titanium valve collecting region.
2. a kind of device preparing the superfine sized spherical titanium powder that 3D prints according to claim 1, is characterized in that, described auto feed system, insulation dynamic sealing device and arc cathode melting well are installed on the same axis.
3. a kind of device preparing the superfine sized spherical titanium powder that 3D prints according to claim 1, it is characterized in that, the center of described heat dissipating housing, protective cover and the center of arc cathode melting well are on the same axis.
4. a kind of device preparing the superfine sized spherical titanium powder that 3D prints according to claim 1, it is characterized in that, the specification of described titanium bar is φ 50mm × 500mm.
5. a kind of device preparing the superfine sized spherical titanium powder that 3D prints according to claim 1, it is characterized in that, the final vacuum of described device is 1 × 10
-5pa.
6. a kind of device preparing the superfine sized spherical titanium powder that 3D prints according to claim 1, it is characterized in that, be provided with cathode power and stabilising arc coil around the borehole wall of described arc cathode melting well, melting down-hole portion is provided with Igniting unit.
7. a kind of device preparing the superfine sized spherical titanium powder that 3D prints according to claim 1, it is characterized in that, described spray chamber outer wall is provided with recirculated cooling water, peep hole and vacuum interface; Described receipts powder tank is with water-cooling system.
8. a kind of device preparing the superfine sized spherical titanium powder that 3D prints according to claim 1, is characterized in that, described reactor body is also provided with water-cooling system.
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| CN107199345A (en) * | 2017-05-22 | 2017-09-26 | 加拿大艾浦莱斯有限公司 | A kind of high-purity superfine spherical titanium powder, preparation method thereof and its device |
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| CN107199345A (en) * | 2017-05-22 | 2017-09-26 | 加拿大艾浦莱斯有限公司 | A kind of high-purity superfine spherical titanium powder, preparation method thereof and its device |
| CN107199345B (en) * | 2017-05-22 | 2019-09-13 | 加拿大艾浦莱斯有限公司 | A kind of high-purity superfine spherical titanium powder, preparation method thereof and its device |
| CN107470610A (en) * | 2017-09-07 | 2017-12-15 | 王明江 | A kind of titanium alloy powder body material for 3D printing |
| CN108296489A (en) * | 2018-04-25 | 2018-07-20 | 张格梅 | A method of it is brilliant to prepare high temperature compound block |
| CN108296489B (en) * | 2018-04-25 | 2021-04-09 | 张格梅 | Method for preparing high-temperature compound bulk crystal |
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