CN107486560A - A kind of method that globular metallic powder is prepared in the case where malleation cools down atmosphere - Google Patents
A kind of method that globular metallic powder is prepared in the case where malleation cools down atmosphere Download PDFInfo
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- CN107486560A CN107486560A CN201710785274.XA CN201710785274A CN107486560A CN 107486560 A CN107486560 A CN 107486560A CN 201710785274 A CN201710785274 A CN 201710785274A CN 107486560 A CN107486560 A CN 107486560A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- Engineering & Computer Science (AREA)
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- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
The present invention relates to a kind of method for preparing globular metallic powder, is in particular a kind of method that globular metallic powder is prepared in the case where malleation cools down atmosphere, comprises the following steps：Step 1：Prepare plasma generator, plasma generator is placed on to the top of cavity；Step 2：Treat that nodularization powder raw material is sent into plasma generator by ready；The irregular of the plasma heating sent through plasma generator treats that nodularization occurs in the presence of surface tension for nodularization powder raw material, into positive pressure environment after can exchange heat with cooling gas rapidly and quickly solidify；Step 3：Cooling air-flow is sent into via cooling air-flow pipeline, treats that nodularization powder raw material cooled and solidified forms spherical powder in the presence of cooling air-flow, the powder after cooling passes through container collection.The metal dust sphericity for preparing is high, interior solid defect is few, good fluidity, is particularly suitable for short cycle, the small lot nodularization production of multicomponent alloy powder.
Description
Technical field
The present invention relates to a kind of method for preparing globular metallic powder, is in particular that one kind cools down atmosphere ring in malleation
The method that globular metallic powder is prepared under border.
Background technology
Metal 3D printing technique proposes very high requirement to raw material powder, it is generally recognized that sphericity is high, fine and close intact
Sunken powder helps to obtain the final products of high-quality.The preparation method of existing a variety of globular metallic powders at present：Such as disclosure
Number disclose method and apparatus using argon gas powder by atomization for EP0400659A1 and CN2855596 patent.Powder by atomization method
Be widely used in the manufacturing of titanium alloy, nickel-base alloy and Al alloy powder, yield and fine powder recovery rate compared with
It is high.But there is more satellite powder in resulting powder.Usual powder by atomization causes powder due to fusing metal liquid and crucible reaction
Deviation be present in last composition and foundry alloy.Publication No. US005707419A patent is then using 3 and the plasma gun of the above, warp
Special angle put after by metal wire material be sent into plasma flame flow joint, realize powder by atomization using high speed plasma jet,
Resulting powder sphericity is preferable.But this method method is only applicable to be prepared into the alloy material of silk material, for fragility material
Expect or be difficult to mass without the alloying component of business silk material.Publication No. JP-A-2002-180112 patent and deliver
Document " H.J.Hedger, A.R.Hall.Preparation of sphe rical powder [J] .Powder
Metallurgy,1961,8:65 ", " P.Linke, S.Zakharian, K.-H.Weiss, G.Nutsch.Manufacturing
of spherical Tungsten carbide powders with the thermal RF inductively coupled
Plasma ", " Wang Jianjun, Hao person of outstanding talent, the bright radio frequency plasmas of Guo Zhimeng, Wang Yu prepare spherical niobium powder, powdered metallurgical material section
And engineering, 2014,19 (3):361-366 " etc. realizes metal dust nodularization using radio frequency plasma, that is, utilizes high temperature radio frequency
Plasma will enter irregular powder therein heating and nodularization, but warehouse is negative pressure shape during due to radio frequency plasma nodularization
State, the powder of the high temperature melting cooling velocity in atmosphere is slower, the selective evaporation of composition be present, causes the composition of powder
Deviation.
The content of the invention
The present invention solves the technical problem of offer one kind spherical metal powder is prepared in the case where malleation cools down atmosphere
The method at end, the metal dust sphericity prepared is high, interior solid defect is few, good fluidity, is particularly suitable for polynary conjunction
The short cycle at bronze end, small lot nodularization production.
In order to solve the above technical problems, the present invention relates to a kind of method for preparing globular metallic powder, in particular it is
A kind of method that globular metallic powder is prepared in the case where malleation cools down atmosphere, comprises the following steps：
Step 1：Prepare plasma generator, plasma generator is placed on to the top of cavity, be ready to treat nodularization powder
Last raw material, the pressure in cavity is adjusted to a constant value；
Step 2：Treat that nodularization powder raw material is radially sent into plasma through carrier gas in a manner of nozzle internal powder conveying by ready
Generator；The irregular of the plasma heating sent through plasma generator treats work of the nodularization powder raw material in surface tension
With green-ball is issued, into positive pressure environment after can rapidly with cooling gas exchange heat and quickly solidify, avoid powder evaporation generation it is micro-
Moonlet powder and nano powder, while the selectivity volatilization of alloying element in powder can also drop；
Step 3：Cooling air-flow is sent into via cooling air-flow pipeline, and nodularization powder former material is treated in the presence of cooling air-flow
Expect that cooled and solidified forms spherical powder, for the powder after cooling by container collection, pressure keeps constant in cavity during this, more
Residual air body is expelled to air or access gas circulation cooling system by gas exit line.
As the further optimization of the technical program, the present invention is a kind of to prepare spherical metal in the case where malleation cools down atmosphere
The pressure in cavity described in the method for powder is malleation 0.1MPa-0.6MPa.
As the further optimization of the technical program, the present invention is a kind of to prepare spherical metal in the case where malleation cools down atmosphere
The power of ion generator described in the method for powder is 10KW-100KW.
As the further optimization of the technical program, the present invention is a kind of to prepare spherical metal in the case where malleation cools down atmosphere
Cooling air-flow described in the method for powder can be Ar, He, N2、H2One or more.
As the further optimization of the technical program, the present invention is a kind of to prepare spherical metal in the case where malleation cools down atmosphere
Cooling air-flow flow described in the method for powder is 1m3/min-10m3/min。
As the further optimization of the technical program, the present invention is a kind of to prepare spherical metal in the case where malleation cools down atmosphere
Treat that nodularization powder raw material can be the irregular powder of pre-alloyed or mechanical uniform mixing, make described in the method for powder
The loose spherical powder that grain, sintering obtain.
As the further optimization of the technical program, the present invention is a kind of to prepare spherical metal in the case where malleation cools down atmosphere
The powder feeding rate for treating nodularization powder raw material described in the method for powder is 10g/min-2000g/min.
A kind of method that globular metallic powder is prepared in the case where malleation cools down atmosphere of the present invention has the beneficial effect that：Using
This method prepares the irregular powder that globular metallic powder raw material sources are extensive, can be obtained for broken, granulation, sintering；Positive pressure gas
Powder cooling velocity is fast under atmosphere, avoids powder composition tolerances and microsatellite powder caused by gasification；Prepared powder is spherical
Degree is high, interior solid defect is few, good fluidity；It is especially applicable to the short cycle of multicomponent alloy powder, small lot nodularization
Production, it can also be used to the nodularization of other elemental powders and ceramic powders.
Brief description of the drawings
The present invention will be further described in detail with specific implementation method below in conjunction with the accompanying drawings.
Fig. 1 is the composition comparison diagram before and after TC4 spheroidizings of powder.
Fig. 2 is that a kind of device work for the method that globular metallic powder is prepared in the case where malleation cools down atmosphere of the present invention is former
Reason figure.
Fig. 3 is 5-35 μm of hydrogenation and dehydrogenization TC4 powder morphology figures.
Fig. 4 is TC4 powder morphology figures after nodularization.
Fig. 5 is shape appearance figure after the agitated mill processing of Nb-5W-2Mo-1Zr.
Fig. 6 is spherical powder shape appearance figure of the Nb-5W-2Mo-1Zr powder after granulation.
Fig. 7 is the Nb521 alloy powders shape appearance figure after plasma spheroidization is handled.
Fig. 8 Nb521 alloy powders XRD spectrograms after plasma spheroidization is handled.
Fig. 9 is shape appearance figure after the agitated mill processing of WNiFe mixed-powders.
Figure 10 is WNiFe plasma spheroidization powder morphology figures.
Figure 11 is WNiFe plasma spheroidization powder xrd pattern spectrograms.
In figure：Plasma generator 1；Cavity 2；Powder feeding pipe 3；Cooling air-flow pipeline 4；Container 5；Gas exit line 6.
Embodiment
Fig. 2 show the device fundamental diagram that spheroidizing of powder is realized in the present invention：Plasma generator 1 is arranged on cavity
Above in the of 2, the pressure in cavity 2 is malleation 0.1-0.6MPa, treats that nodularization powder raw material is fed through plasma flame flow through powder feeding pipe 3
Heating ejection forms melted powder jet, then the cooled and solidified formation spherical powder in the presence of cooling air-flow pipeline 4, and
Collected in container 5；Pressure is kept constant in the process cavity 2, and excessive gas is expelled to air or access by gas exit line 6
Gas circulation cooling system.
Below in conjunction with the drawings and specific embodiments, the present invention will be further described：
Embodiment 1：TC4 titanium alloy spherical powders are prepared using the present invention；
1) using 5-35 μm of hydrogenation and dehydrogenization TC4 powder as raw material, powder morphology is as shown in Figure 3；
2) above-mentioned powder is fed through in plasma generator 1, plasma power 80kW, pressure is in cavity 2
0.3MPa, gases used is Ar and He gaseous mixtures (volume ratio 1：3), cooling gas flow is 8m3/ min, powder carrier gas flux
7l/min, powder sending quantity 180g/min；
3) gained spherical powder is collected, detected.Fig. 4 is obtained TC4 alloy spherical powder morphologies, powder surface
Without obvious satellite powder, Oxygen potential 98%, powder diameter is 16-45 μm.Composition contrast before and after spheroidizing of powder as shown in Figure 1
Show, significant change does not occur for the Ti after spheroidising in TC4 alloys, Al, V element content, illustrates during nodularization simultaneously
The selectivity volatilization of Al elements is not occurred, oxygen content and carbon content decrease in powder.
Embodiment 2：Spherical Nb521 alloy sphericals powder is prepared using the present invention；
1) using purity as the Nb powder that 99.9% Fisher particle size is 5 μm, purity is the W powder that 99.8% granularity is 1-2 μm, purity
For less than 99.9%5 microns of Mo powder, purity is that the Zr powder that 99.9% granularity is 3-5 μm is raw material；
2) above-mentioned raw materials are mixed and added into 1% petroleum ether as auxiliary agent according to Nb-5W-2Mo-1Zr (wt.%) ratio
Mill processing is stirred, rotating speed 500rpm, time 2h, gained powder morphology is as shown in figure 5, powder mean particle sizes after Ball-stirring mill
For 4 μm；
3) centrifugal spray granulation (PVA aqueous solvents, solid concentration 15%) is carried out through powder by above-mentioned, pattern is as shown in Figure 6；
Sieving is obtained to 35-90 μm of prilling powder degumming sintering (400 DEG C of degummings, 1280 DEG C of sintering are carried out in degumming sintering furnace
1h)；
4) above-mentioned powder is fed through in plasma generator 1, plasma power 60kW, pressure is in cavity 2
0.2MPa, gases used is Ar and H2Gaseous mixture (volume ratio 5：1), cooling gas flow is 6m3/ min, powder carrier gas flux
7l/min, powder sending quantity 60g/min；
5) gained spherical powder is collected, detected.Fig. 7 is obtained Nb521 alloy spherical powder morphologies, powder surface
It is smooth, sphericity is preferable, Fig. 8 XRD spectrum shows that powder has formd Nb521 Alloy solid solutions, powder after spheroidising
Last granularity is 15-53 μm, can meet that increasing material manufacturing requirement is melted in selective laser.
Embodiment 3：Spherical WNiFe alloy sphericals powder is prepared using the present invention；
1) the W powder for being 1-2 μm as 99.8% granularity using purity, granularity are 5-8 μm of Ni powder, and granularity is 3-5 μm of carbonyl
Fe powder is raw material；
2) stirred according to the stearic acid of W-7Ni-3Fe (wt.%) ratio mixed material powder and addition 1% as auxiliary agent
Mill processing is mixed, rotating speed 500rpm, time 2h, gained powder morphology is as shown in figure 9, powder mean particle sizes are 3 μm after Ball-stirring mill；
3) centrifugal spray granulation (PVA alcohol solvents, solid concentration 10%) is carried out through powder by above-mentioned；Sieving is obtained
50-150 μm of prilling powder carries out degumming sintering (400 DEG C of degummings, 1300 DEG C of sintering 1h) in degumming sintering furnace；
4) above-mentioned powder is fed through in plasma generator 1, plasma power 40kW, pressure is in cavity 2
0.3MPa, gases used is Ar and H2Gaseous mixture (volume ratio 5：2), cooling gas flow is 4m3/ min, powder carrier gas flux
7l/min, powder sending quantity 50g/min；
Gained spherical powder is collected, detected.Figure 10 is obtained WNiFe alloy spherical powder morphologies, powder surface
Smooth, spherical degree is preferable, and XRD spectrum (Figure 11) shows that powder has synthesized WNiFe Alloy solid solutions, mistake after spheroidising
Powder size is 45-105 μm after sieve, can meet electron beam selective melting increasing material manufacturing requirement.
Certainly, described above is not limitation of the present invention, and the present invention is also not limited to the example above, the art
The variations, modifications, additions or substitutions that those of ordinary skill is made in the essential scope of the present invention, fall within the guarantor of the present invention
Protect scope.
Claims (7)
1. a kind of method that globular metallic powder is prepared in the case where malleation cools down atmosphere, comprises the following steps：
Step 1：Prepare plasma generator, plasma generator is placed on to the top of cavity, be ready to treat nodularization powder original
Material, the pressure in cavity is adjusted to a constant value；
Step 2：Treat that the radial direction in a manner of nozzle internal powder conveying is sent into plasma to nodularization powder raw material through carrier gas by ready
Device；The irregular of the plasma heating sent through plasma generator treats nodularization powder raw material in the presence of surface tension
Generation nodularization, into positive pressure environment after can exchange heat with cooling gas rapidly and quickly solidify, avoid powder evaporation generation from small defending
Star powder and nano powder, while the selectivity volatilization of alloying element in powder can also drop；
Step 3：Cooling air-flow is sent into via cooling air-flow pipeline, treats that nodularization powder raw material is cold in the presence of cooling air-flow
But solidification forms spherical powder, and the powder after cooling is by container collection, and pressure keeps constant, more residual air in cavity during this
Body is expelled to air or access gas circulation cooling system by gas exit line.
2. a kind of method that globular metallic powder is prepared in the case where malleation cools down atmosphere according to claim 1, it is special
Sign is：Pressure in described cavity is malleation 0.1MPa-0.6MPa.
3. a kind of method that globular metallic powder is prepared in the case where malleation cools down atmosphere according to claim 1, it is special
Sign is：The power of described ion generator is 10KW-100KW.
4. a kind of method that globular metallic powder is prepared in the case where malleation cools down atmosphere according to claim 1, it is special
Sign is：Described cooling air-flow can be Ar, He, N2、H2One or more.
5. a kind of method that globular metallic powder is prepared in the case where malleation cools down atmosphere according to claim 1, it is special
Sign is：Described cooling air-flow flow is 1m3/min-10m3/min。
6. a kind of method that globular metallic powder is prepared in the case where malleation cools down atmosphere according to claim 1, it is special
Sign is：Described treats that nodularization powder raw material can be the irregular powder of pre-alloyed or mechanical uniform mixing, granulation, burning
Tie obtained loose spherical powder.
7. a kind of method that globular metallic powder is prepared in the case where malleation cools down atmosphere according to claim 1, it is special
Sign is：The described powder feeding rate for treating nodularization powder raw material is 10g/min-2000g/min.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108188389A (en) * | 2018-04-02 | 2018-06-22 | 湖南工业大学 | A kind of plasma powder spheroidization device and its methods and applications |
| CN109128207A (en) * | 2018-10-26 | 2019-01-04 | 四川恒珲新材料科技有限公司 | A kind of purification ultrafine titanium powder and preparation method thereof |
| CN111360275A (en) * | 2018-12-26 | 2020-07-03 | 中国科学院宁波材料技术与工程研究所 | Intelligent control adjusting device for powder spheroidizing control |
| CN111515408A (en) * | 2020-05-12 | 2020-08-11 | 广东省材料与加工研究所 | NiTi alloy powder and preparation method and application thereof |
| CN111842875A (en) * | 2020-07-06 | 2020-10-30 | 北京科技大学 | Method for preparing high-performance Nb521 product by low-cost printing |
| CN113000833A (en) * | 2021-02-23 | 2021-06-22 | 郑州大学 | Ti-6Al-4V alloy spherical powder for additive manufacturing and preparation method thereof |
| RU2782498C1 (en) * | 2021-12-28 | 2022-11-01 | федеральное государственное автономное образовательное учреждение высшего образования "Санкт-Петербургский политехнический университет Петра Великого" (ФГАОУ ВО "СПбПУ") | Method for obtaining a wear-resistant coating from a high-entropy alloy with a surface-carbonized layer |
| CN115401207A (en) * | 2022-07-23 | 2022-11-29 | 杭州新川新材料有限公司 | Apparatus for producing mixed metal powder |
| WO2023015613A1 (en) * | 2021-08-12 | 2023-02-16 | 江苏天楹等离子体科技有限公司 | Device and method for producing metal powder by means of plasma atomization |
| CN118477996A (en) * | 2024-07-10 | 2024-08-13 | 西安赛隆增材技术股份有限公司 | Method and device for processing irregular metal powder |
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| CN108188389B (en) * | 2018-04-02 | 2023-08-15 | 湖南工业大学 | Plasma powder spheroidizing device and method and application thereof |
| CN109128207B (en) * | 2018-10-26 | 2022-03-04 | 四川恒珲新材料科技有限公司 | Superfine titanium powder and preparation method thereof |
| CN109128207A (en) * | 2018-10-26 | 2019-01-04 | 四川恒珲新材料科技有限公司 | A kind of purification ultrafine titanium powder and preparation method thereof |
| CN111360275A (en) * | 2018-12-26 | 2020-07-03 | 中国科学院宁波材料技术与工程研究所 | Intelligent control adjusting device for powder spheroidizing control |
| CN111515408A (en) * | 2020-05-12 | 2020-08-11 | 广东省材料与加工研究所 | NiTi alloy powder and preparation method and application thereof |
| CN111515408B (en) * | 2020-05-12 | 2022-12-06 | 广东省材料与加工研究所 | NiTi alloy powder and preparation method and application thereof |
| CN111842875A (en) * | 2020-07-06 | 2020-10-30 | 北京科技大学 | Method for preparing high-performance Nb521 product by low-cost printing |
| CN113000833A (en) * | 2021-02-23 | 2021-06-22 | 郑州大学 | Ti-6Al-4V alloy spherical powder for additive manufacturing and preparation method thereof |
| WO2023015613A1 (en) * | 2021-08-12 | 2023-02-16 | 江苏天楹等离子体科技有限公司 | Device and method for producing metal powder by means of plasma atomization |
| RU2782498C1 (en) * | 2021-12-28 | 2022-11-01 | федеральное государственное автономное образовательное учреждение высшего образования "Санкт-Петербургский политехнический университет Петра Великого" (ФГАОУ ВО "СПбПУ") | Method for obtaining a wear-resistant coating from a high-entropy alloy with a surface-carbonized layer |
| CN115401207A (en) * | 2022-07-23 | 2022-11-29 | 杭州新川新材料有限公司 | Apparatus for producing mixed metal powder |
| CN115401207B (en) * | 2022-07-23 | 2024-05-14 | 杭州新川新材料有限公司 | Production device for mixed metal powder |
| CN118477996A (en) * | 2024-07-10 | 2024-08-13 | 西安赛隆增材技术股份有限公司 | Method and device for processing irregular metal powder |
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