CN108237231A - A kind of manufacturing method of spherical shape molybdenum powder - Google Patents

A kind of manufacturing method of spherical shape molybdenum powder Download PDF

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Publication number
CN108237231A
CN108237231A CN201611219522.6A CN201611219522A CN108237231A CN 108237231 A CN108237231 A CN 108237231A CN 201611219522 A CN201611219522 A CN 201611219522A CN 108237231 A CN108237231 A CN 108237231A
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China
Prior art keywords
molybdenum powder
manufacturing
plasma spheroidization
method technique
powder
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CN201611219522.6A
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Chinese (zh)
Inventor
陈锐
刘志光
陈海霞
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Longyan Cercis Innovation Research Institute
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Longyan Cercis Innovation Research Institute
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Priority to CN201611219522.6A priority Critical patent/CN108237231A/en
Publication of CN108237231A publication Critical patent/CN108237231A/en
Pending legal-status Critical Current

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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
    • B22F9/14Making metallic powder or suspensions thereof using physical processes using electric discharge
    • 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
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06Metallic powder characterised by the shape of the particles
    • B22F1/065Spherical particles
    • 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
    • B22F2202/00Treatment under specific physical conditions
    • B22F2202/13Use of plasma
    • 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
    • B22F2999/00Aspects linked to processes or compositions used in powder metallurgy

Abstract

The present invention provides a kind of manufacturing method of spherical molybdenum powder, this method is to be atomized loose porous molybdenum powder that comminution granulation is prepared as raw material, molybdenum powder raw material are prepared into spherical molybdenum powder with plasma spheroidization method technique, the high spherical molybdenum powder of Oxygen potential is prepared by controlling the major parameter of radio frequency plasma powder nodularization system.The final spherical molybdenum powder for obtaining pattern rule, high Oxygen potential (≤90%), high sphericity, high-compactness, function admirable of the invention.

Description

A kind of manufacturing method of spherical shape molybdenum powder
Technical field
The present invention relates to technical field of material, especially relate to a kind of manufacturing method of spherical molybdenum powder.
Background technology
Globular metallic powder is widely used in material increasing field, and compared with other kinds of material, powder Class material has many advantages, such as, for example, prepare and be easier to, stock utilization is high, classification is extensive, building course is simple etc..Increase material system It is globular metallic powder material melts accumulation molding to make used in SLM, LENS, EBM in technique etc..
It is either domestic or external, all there are more research and development units to spherical metal powder powder material and technique into Go relevant research-and-development activity, it is more famous to have the EOS of Germany, the Optomec in the U.S. etc. in foreign countries;There is Zhuzhou in the country Pu Linte, Beijing friend are emerging etc..
The production method for being presently used for preparing metal powder mainly has electrolysis, water/gas atomization, atomization comminution granulation etc.. In dendroid, in powder particle, there are larger internal stress, poor fluidity to be not suitable for straight for the powder morphology that wherein prepared by electrolysis It connects for increasing material manufacturing;Metal powder Oxygen potential and sphericity are all relatively low made from water/gas atomization, generally also not direct For increasing material manufacturing;Powder made from comminution granulation is atomized in loose and porous structure, consistency is low with apparent density, uncomfortable directly to use In increasing material manufacturing.
Invention content
It is above-mentioned technical problem to solve, the invention is realized in this way:
A kind of manufacturing method of spherical shape molybdenum powder, this method is to be atomized loose porous molybdenum powder that comminution granulation is prepared to be former Molybdenum powder raw material are prepared into spherical molybdenum powder by material with plasma spheroidization method technique.
It is atomized comminution granulation:Molybdenum powder is subjected to grain composition first;Then in proportion with water-based solvent, binding agent, dispersant It is mixed with antifoaming agent, ground dispersion, obtains the uniform slurry of dispersion mixing;Then slurry is pumped into spray dryer It is dried;It finally moves in Equipment for Heating Processing, is heat-treated, be cooled to room temperature, you can obtain required product.
Using atomization comminution granulation obtained by loose porous molybdenum powder by carrier gas carry by feeding gun be passed into grade from It is molten by heating in very short time under radiation, convection current, conduction and the effect of these four chemical heat transfer mechanisms after daughter torch Change, under the effect of the smelt surface tension of molybdenum powder particle melted immediately, form the very high molybdenum powder drop of sphericity, and in pole Quick solidification under high temperature gradient forms spherical molybdenum powder particle.
Device used in the processing method receives the SY129 radio frequency plasma powder that (TEKNA) company produces by Tyke Body nodularization system, SY129 radio frequency plasma powder nodularizations system are module management, are mainly included:(1) plasma torch:Easily In maintenance, can be operated under oxidation, reduction or inert environments, electrodeless pollution.(2) treatment reactor and powder collector: Line acquisition system, filter automatic cleaning system.(3) operation interface:Real-time data acquisition, alarm indication and management, sequencing Operation and operation.(4) plasma exhaust gas recycles:90% waste gas circulation uses, argon, helium and hydrogen economical operation.(5) defeated powder Device:Special design, for conveying lazy flow powder, runs, online bulking system under controllable air pressure, transfer rate prison Control.
The operation principle of SY129 radio frequency plasma powder nodularization systems is:Metal powder granulates pass through charging by carrier gas After rifle is injected to plasma torch, under four kinds of radiation, convection current, conduction and chemistry heat transfer mechanism effects, it is heated rapidly and melts Change.The particle of melting forms the very high drop of sphericity under the action of surface tension, and rapid under high temperature gradient Solidification forms spherical particle.
SY129 radio frequency plasma powder nodularizations system work when protective gas be purity be 99.99% nitrogen with 99.99% hydrogen.
Loose porous molybdenum powder of the raw material used in the present invention obtained by using atomization comminution granulation, the raw material is through SY129 After the spheroidising of radio frequency plasma powder nodularization system, pattern rule, high Oxygen potential (≤90%), high spherical shape can be obtained Degree, high-compactness, function admirable spherical molybdenum powder.
It should be clear that the particle size distribution range of the spherical molybdenum powder obtained by the method, related with the particle size distribution range of raw material, if It is the epigranular of the epigranular of raw material, then products obtained therefrom, vice versa.
The control parameter of SY129 radio frequency plasma powder nodularization systems mainly includes several following:End reaction container Interior air pressure, grid current, plate voltage, plate electric current, rate of feeding, argon inlet mouth pressure are (including sheath stream pressure, central fluidizing gas Pressure with for powder stream pressure), hydrogen inlet pressure.
Nodularization equipment used in plasma spheroidization method technique receives the SY129 radio frequencies that (TEKNA) company produces by Tyke Plasma powder nodularization system.
Preferably, it is 14.0psia to 15.0psia that air pressure in container is answered in plasma spheroidization method technique.
Preferably, the grid current set by plasma spheroidization method technique is 0.40A to 0.46A.
Preferably, the plate voltage set by plasma spheroidization method technique is 7.4KV to 8.8KV.
Preferably, the plate electric current of plasma spheroidization method technique initialization is 3.7A to 4.4A.
Preferably, the rate of feeding set by plasma spheroidization method technique is 1rpm to 2rpm.
Preferably, the argon gas sheath stream pressure set by plasma spheroidization method technique is 50psig to 60psig.
Preferably, the argon gas central fluidizing gas pressure of plasma spheroidization method technique initialization is 12psig to 16psig.
Preferably, the argon gas set by plasma spheroidization method technique is 5psig to 8psig for powder stream pressure.
Preferably, the hydrogen inlet pressure set by plasma spheroidization method technique is 6psig to 9psig.
The invention has the advantages that:The present invention intends solving to be the loose porous molybdenum powder as obtained by atomization comminution granulation The problem of cannot be used directly for increasing material manufacturing provides a kind of processing method, using radio frequency plasma powder nodularization system to mist Change the loose porous molybdenum powder obtained by comminution granulation further to be processed, it is final obtain pattern is regular, high Oxygen potential (≤ 90%), the spherical molybdenum powder of high sphericity, high-compactness, function admirable.
Specific embodiment
In order to describe the technical content, the structural feature, the achieved object and the effect of this invention in detail, below in conjunction with embodiment It is explained in detail.
Embodiment 1
A kind of manufacturing method of spherical shape molybdenum powder, this method is to be atomized loose porous molybdenum powder that comminution granulation is prepared to be former Molybdenum powder raw material are prepared into spherical molybdenum powder by material with plasma spheroidization method technique,
The major parameter of SY129 radio frequency plasma powder nodularization systems is controlled including as follows:
It is 14.0psia that air pressure in container is answered in plasma spheroidization method technique;
Grid current set by plasma spheroidization method technique is 0.40A;
Plate voltage set by plasma spheroidization method technique is 7.4KV;
The plate electric current of plasma spheroidization method technique initialization is 3.7A;
Rate of feeding set by plasma spheroidization method technique is 1rpm;
Argon gas sheath stream pressure set by plasma spheroidization method technique is 50psi;
The argon gas central fluidizing gas pressure of plasma spheroidization method technique initialization is 12psig;
It is 5psig that argon gas set by plasma spheroidization method technique, which supplies powder stream pressure,;
Hydrogen inlet pressure set by plasma spheroidization method technique is 6psig.
The Oxygen potential of spherical molybdenum powder after nodularization is not less than 90%.
Embodiment 2
A kind of manufacturing method of spherical shape molybdenum powder, this method is to be atomized loose porous molybdenum powder that comminution granulation is prepared to be former Molybdenum powder raw material are prepared into spherical molybdenum powder by material with plasma spheroidization method technique,
The major parameter of SY129 radio frequency plasma powder nodularization systems is controlled including as follows:
It is 15.0psia that air pressure in container is answered in plasma spheroidization method technique;
Grid current set by plasma spheroidization method technique is 0.46A;
Plate voltage set by plasma spheroidization method technique is 8.8KV;
The plate electric current of plasma spheroidization method technique initialization is 4.4A;
Rate of feeding set by plasma spheroidization method technique is 2rpm;
Argon gas sheath stream pressure set by plasma spheroidization method technique is 60psig;
The argon gas central fluidizing gas pressure of plasma spheroidization method technique initialization is 16psig;
It is 8psig that argon gas set by plasma spheroidization method technique, which supplies powder stream pressure,;
Hydrogen inlet pressure set by plasma spheroidization method technique is 9psig.
The Oxygen potential of spherical molybdenum powder after nodularization is not less than 90%.
Embodiment 3
A kind of manufacturing method of spherical shape molybdenum powder, this method is to be atomized loose porous molybdenum powder that comminution granulation is prepared to be former Molybdenum powder raw material are prepared into spherical molybdenum powder by material with plasma spheroidization method technique,
The major parameter of SY129 radio frequency plasma powder nodularization systems is controlled including as follows:
It is 14.5psia that air pressure in container is answered in plasma spheroidization method technique;
Grid current set by plasma spheroidization method technique is 0.42A;
Plate voltage set by plasma spheroidization method technique is 7.8KV;
The plate electric current of plasma spheroidization method technique initialization is 3.9A;
Rate of feeding set by plasma spheroidization method technique is 1.3rpm;
Argon gas sheath stream pressure set by plasma spheroidization method technique is 53psig;
The argon gas central fluidizing gas pressure of plasma spheroidization method technique initialization is 13psig;
It is 6psig that argon gas set by plasma spheroidization method technique, which supplies powder stream pressure,;
Hydrogen inlet pressure set by plasma spheroidization method technique is 7psig.
The Oxygen potential of spherical molybdenum powder after nodularization is not less than 90%.
Embodiment 4
A kind of manufacturing method of spherical shape molybdenum powder, this method is to be atomized loose porous molybdenum powder that comminution granulation is prepared to be former Molybdenum powder raw material are prepared into spherical molybdenum powder by material with plasma spheroidization method technique,
The major parameter of SY129 radio frequency plasma powder nodularization systems is controlled including as follows:
It is 14.7psia that air pressure in container is answered in plasma spheroidization method technique;
Grid current set by plasma spheroidization method technique is 0.44A;
Plate voltage set by plasma spheroidization method technique is 8.0KV;
The plate electric current of plasma spheroidization method technique initialization is 4.0A;
Rate of feeding set by plasma spheroidization method technique is 1.6rpm;
Argon gas sheath stream pressure set by plasma spheroidization method technique is 55psig;
The argon gas central fluidizing gas pressure of plasma spheroidization method technique initialization is 13psig;
It is 7psig that argon gas set by plasma spheroidization method technique, which supplies powder stream pressure,;
Hydrogen inlet pressure set by plasma spheroidization method technique is 8psig.
The Oxygen potential of spherical molybdenum powder after nodularization is not less than 90%.
Embodiment 5
A kind of manufacturing method of spherical shape molybdenum powder, this method is to be atomized loose porous molybdenum powder that comminution granulation is prepared to be former Molybdenum powder raw material are prepared into spherical molybdenum powder by material with plasma spheroidization method technique,
The major parameter of SY129 radio frequency plasma powder nodularization systems is controlled including as follows:
It is 14.8psia that air pressure in container is answered in plasma spheroidization method technique;
Grid current set by plasma spheroidization method technique is 0.45A;
Plate voltage set by plasma spheroidization method technique is 8.4KV;
The plate electric current of plasma spheroidization method technique initialization is 4.2A;
Rate of feeding set by plasma spheroidization method technique is 1.8rpm;
Argon gas sheath stream pressure set by plasma spheroidization method technique is 58psig;
The argon gas central fluidizing gas pressure of plasma spheroidization method technique initialization is 15psig;
It is 7psig that argon gas set by plasma spheroidization method technique, which supplies powder stream pressure,;
Hydrogen inlet pressure set by plasma spheroidization method technique is 8psig.
The Oxygen potential of spherical molybdenum powder after nodularization is not less than 90%.
The foregoing is merely the embodiment of the present invention, not thereby limit the scope of patent protection of the present invention, every utilization The equivalent structure or equivalent flow shift that present specification is made directly or indirectly is used in other relevant technologies Field is included within the scope of the present invention.

Claims (10)

1. it is a kind of spherical shape molybdenum powder manufacturing method, which is characterized in that this method be atomized comminution granulation be prepared it is loose porous Molybdenum powder for raw material, molybdenum powder raw material are prepared into spherical molybdenum powder with plasma spheroidization method technique.
2. the manufacturing method of spherical shape molybdenum powder as described in claim 1, which is characterized in that answer container in plasma spheroidization method technique Interior air pressure is 14.0psia to 15.0psia.
3. the manufacturing method of spherical shape molybdenum powder as claimed in claim 2, which is characterized in that set by plasma spheroidization method technique Grid current is 0.40A to 0.46A.
4. the manufacturing method of spherical shape molybdenum powder as claimed in claim 3, which is characterized in that set by plasma spheroidization method technique Plate voltage is 7.4KV to 8.8KV.
5. the manufacturing method of spherical shape molybdenum powder as claimed in claim 4, which is characterized in that the plate of plasma spheroidization method technique initialization Electric current is 3.7A to 4.4A.
6. the manufacturing method of spherical shape molybdenum powder as claimed in claim 5, which is characterized in that set by plasma spheroidization method technique Rate of feeding is 1rpm to 2rpm.
7. the manufacturing method of spherical shape molybdenum powder as claimed in claim 6, which is characterized in that set by plasma spheroidization method technique Argon gas sheath stream pressure is 50psig to 60psig.
8. the manufacturing method of spherical shape molybdenum powder as claimed in claim 7, which is characterized in that the argon of plasma spheroidization method technique initialization Gas central fluidizing gas pressure is 12psig to 16psig.
9. the manufacturing method of spherical shape molybdenum powder as claimed in claim 8, which is characterized in that set by plasma spheroidization method technique Argon gas is 5psig to 8psig for powder stream pressure.
10. the manufacturing method of spherical shape molybdenum powder as claimed in claim 9, which is characterized in that set by plasma spheroidization method technique Hydrogen inlet pressure be 6psig to 9psig.
CN201611219522.6A 2016-12-26 2016-12-26 A kind of manufacturing method of spherical shape molybdenum powder Pending CN108237231A (en)

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Publication number Priority date Publication date Assignee Title
CN109570521A (en) * 2018-12-24 2019-04-05 南通金源智能技术有限公司 The method that plasma spheroidization prepares metal powder
CN109692965A (en) * 2019-02-27 2019-04-30 北京工业大学 A kind of preparation method of the spherical tungsten-molybdenum alloy powder of 3D printing
CN111318715A (en) * 2018-12-14 2020-06-23 上海大境海洋新材料有限公司 Production method of 3D printing spherical titanium alloy powder

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111318715A (en) * 2018-12-14 2020-06-23 上海大境海洋新材料有限公司 Production method of 3D printing spherical titanium alloy powder
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CN109692965A (en) * 2019-02-27 2019-04-30 北京工业大学 A kind of preparation method of the spherical tungsten-molybdenum alloy powder of 3D printing

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Application publication date: 20180703