CN103962567A - Method and equipment for preparing spherical molybdenum powder - Google Patents

Method and equipment for preparing spherical molybdenum powder Download PDF

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Publication number
CN103962567A
CN103962567A CN201410240884.8A CN201410240884A CN103962567A CN 103962567 A CN103962567 A CN 103962567A CN 201410240884 A CN201410240884 A CN 201410240884A CN 103962567 A CN103962567 A CN 103962567A
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molybdenum
cooling
powder
reaction cavity
disk electrode
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CN201410240884.8A
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CN103962567B (en
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武洲
左羽飞
陈强
胡林
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Jinduicheng Molybdenum Co Ltd
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Jinduicheng Molybdenum Co Ltd
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Abstract

The invention discloses equipment for preparing spherical molybdenum powder. The equipment comprises a powder cooling tank, a reactor and a power collection tank, wherein an opening is formed in the middle of the upper end of the powder cooling tank, the reactor is mounted at the opening in the middle of the upper end of the powder cooling tank, and the powder collection tank is arranged below the powder cooling tank; the reactor comprises a reaction cavity, an insulating water-cooling clamp cover and a molybdenum disk electrode, an opening is formed in the lower end of the reaction cavity, the insulating water-cooling clamp cover is horizontally mounted on the reaction cavity, the molybdenum disk electrode is arranged in the reaction cavity, a blowing air pipeline communicated with the interior of the reaction cavity is arranged at the upper end of the reaction cavity, one end of the insulating water-cooling clamp cover penetrates through the reaction cavity and is located in the reaction cavity, and the other end of the insulating water-cooling clamp cover is located outside the reaction cavity. Beside, the invention further discloses a method for preparing the spherical molybdenum powder. The equipment has the advantages that the structure is simple, the design is reasonable, and the operation is simple and convenient; the spherical molybdenum powder is prepared by virtue of a discharging-melting technique, so that the nodulizing efficiency of the molybdenum powder is greatly increased, and the cost is lowered; the equipment has no specific requirement to a molybdenum powder raw material and is suitable for scale production.

Description

A kind of preparation method of spherical molybdenum powder and equipment
Technical field
The invention belongs to powder metallurgy powder spheroidizing technology field, be specifically related to a kind of preparation method and equipment of spherical molybdenum powder.
Background technology
Molybdenum goods and molybdenum group alloy material are mainly the method preparations by powder metallurgy, and the quality of molybdenum powder is a key link, and its physicochemical property becomes the key factor that affects molybdenum product quality.Common molybdenum powder granularity and apparent density be little, there is no mobility, powder microscopic appearance is irregular, is not suitable for preparing molybdenum goods and the molybdenum group alloy material of high-quality.Cannot be competent at especially at aspects such as precise electronic device, clean nearly shaping, efficient sprayings.
Granulation is that lifting molybdenum powder is physical, widens the current techique means in use field.Main molybdenum powder granulating technique has high temperature comminution granulation, atomization comminution granulation, plasma spheroidization method etc.Wherein, with the prepared molybdenum powder performance the best of plasma spheroidization method, it is of uniform size spherical that molybdenum powder particle is, and apparent density can reach 6.0g/cm 3above, below Hall stream scooter 15s/50g.Plasma spheroidization method is the high temperature utilizing more than the thousands of degree of plasma, by aspheric molybdenum powder particle send into etc. in vitro in, particle surface or entirety can be rendered as molten condition becomes molten drop, it is spherical that the surface tension of molten drop becomes particle, the in vitro rear cooling contractions such as molten drop leaves become spherical, finally obtain spherical molybdenum powder.How common molybdenum powder being sent into plasma and effectively being collected is the difficult point of plasma spheroidization method, and it is narrow as far as possible that the former grain of General Requirements molybdenum powder should have certain mobility, size distribution, otherwise cannot complete nodularization process or efficiency is very low.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, and a kind of equipment of preparing spherical molybdenum powder is provided.Device structure of the present invention is simple; reasonable in design; easy and simple to handle; by molybdenum disk electrode and molybdenum bar base are set, after energising, between molybdenum disk electrode and molybdenum bar base, discharge, make to form spherical molybdenum powder after the electric discharge melting of molybdenum bar base end; greatly improve the efficiency of molybdenum powder nodularization; reduce cost, and raw material molybdenum powder has not been had to particular/special requirement, suitability for scale production.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of equipment of preparing spherical molybdenum powder, it is characterized in that, comprise the powder cooling tank of upper center opening and be installed on the reactor of powder cooling tank upper center aperture position, and being arranged at the powder collection tank of powder cooling tank below, described reactor comprises the reaction cavity of lower ending opening, level is installed on the insulated water-cooling chuck on reaction cavity and is arranged at the molybdenum disk electrode of reaction cavity inside, the upper end of described reaction cavity is provided with the purge gas pipeline being connected with reaction cavity inside, one end of described insulated water-cooling chuck is through reaction cavity and be positioned at reaction cavity, the other end of insulated water-cooling chuck is positioned at outside reaction cavity, described molybdenum disk electrode is hollow structure, on described molybdenum disk electrode, offer and on water inlet and water inlet, be connected with the first cooling water inlet pipe, on described molybdenum disk electrode, offer and on delivery port and delivery port, be connected with the first cooling water outlet pipe, the outer end of the outer end of described the first cooling water inlet pipe and the first cooling water outlet pipe all passes reaction cavity and is supported on reaction cavity, the position that described insulated water-cooling chuck is positioned at outside reaction cavity is connected with the second cooling water inlet pipe and the second cooling water outlet pipe, described insulated water-cooling chuck inner clip is held molybdenum bar base, described molybdenum bar base passes insulated water-cooling chuck near one end of molybdenum disk electrode and is positioned at outside insulated water-cooling chuck, pass between one end of molybdenum bar base of insulated water-cooling chuck and molybdenum disk electrode and leave gap, described molybdenum bar base is provided with the propulsion plant moving horizontally for promoting molybdenum bar base away from one end of molybdenum disk electrode.
Above-mentioned a kind of equipment of preparing spherical molybdenum powder, between the inner and outer wall of described powder cooling tank, be provided with cooling cavity, the bottom of described powder cooling tank is provided with the cooling water/gas import being connected with cooling cavity, and described powder cooling tank upper end is provided with the cooling water/gas outlet being connected with cooling cavity.
Above-mentioned a kind of equipment of preparing spherical molybdenum powder, described in the gap that passes between one end and the molybdenum disk electrode of molybdenum bar base of insulated water-cooling chuck be 1mm.
Above-mentioned a kind of equipment of preparing spherical molybdenum powder, described propulsion plant is electric pushrod or Electrohydraulic push rod.
Above-mentioned a kind of equipment of preparing spherical molybdenum powder, the diameter of described molybdenum disk electrode is 5~10 times of molybdenum bar base diameter.
Above-mentioned a kind of equipment of preparing spherical molybdenum powder, described molybdenum bar base passes insulated water-cooling chuck and is positioned at outside insulated water-cooling chuck away from one end of molybdenum disk electrode.
In addition, the present invention also provides a kind of method that adopts the said equipment to prepare spherical molybdenum powder, it is characterized in that, the method comprises the following steps:
Step 1, molybdenum bar base is clamped in insulated water-cooling chuck, making molybdenum bar base is 1mm near the gap between one end and the molybdenum disk electrode of molybdenum disk electrode;
Step 2, in reaction cavity, pass into working gas by purge gas pipeline, and pass into cooling water in the first cooling water inlet pipe and the second cooling water inlet pipe;
Step 3, give the energising of molybdenum disk electrode and molybdenum bar base, boosted voltage is until molybdenum bar base and the electric discharge of molybdenum disk electrode, propulsion plant promotion molybdenum bar base is opened in electric discharge simultaneously makes molybdenum bar base and molybdenum disk electrode keep discharge condition, in discharge process, molybdenum bar base is constantly melt into spherical molybdenum powder near the end face of molybdenum disk electrode, described spherical molybdenum powder is purged into powder cooling tank cooling by the working gas passing into from purge gas pipeline, cooled spherical molybdenum powder falls into powder collection tank and collects.
Above-mentioned method, working gas described in step 2 is hydrogen and/or argon gas.
The present invention compared with prior art has the following advantages:
1, device structure of the present invention is simple, reasonable in design, easy and simple to handle.
2, equipment of the present invention is by arranging molybdenum disk electrode and molybdenum bar base; after energising, between molybdenum disk electrode and molybdenum bar base, discharge; make to form spherical molybdenum powder after the electric discharge melting of molybdenum bar base end; greatly improve the efficiency of molybdenum powder nodularization; reduce cost; and raw material molybdenum powder is not had to particular/special requirement, suitability for scale production.
3, the present invention is by adopting hollow structure and being connected with the first cooling water inlet pipe and the molybdenum disk electrode of the first cooling water outlet pipe; molybdenum disk electrode area more greatly can and molybdenum bar base electrode between form uniform and stable electric field make electric discharge carry out smoothly; in the course of work, can rapidly the heat of discharge generation be taken out of to logical cooling water in molybdenum disk electrode; protection molybdenum disk electrode, makes molybdenum disk electrode in good working state.
4, equipment of the present invention is by being held on molybdenum bar base in insulated water-cooling chuck, insulated water-cooling chuck on the one hand can be by molybdenum bar base fixed position, avoid its irregular movement, ensure that discharge stability carries out, the cooling water circulating in insulated water-cooling chuck on the other hand can be taken electric discharge heat out of, makes molybdenum bar base in good working state.
5, the present invention is directed to the shortcoming of plasma spheroidization method, adopt electric discharge fusion technology to prepare spherical molybdenum powder, raw material molybdenum powder is not had to particular/special requirement, strong adaptability, and also the ball molybdenum powder performance of preparation is suitable with plasma spheroidization method.
Below in conjunction with drawings and Examples, technical scheme of the present invention is described in further detail.
Brief description of the drawings
Fig. 1 is the structural representation of present device.
Fig. 2 is the perspective view of reactor of the present invention.
Fig. 3 is the structural representation of reactor of the present invention.
Fig. 4 is the A-A cutaway view of Fig. 3.
Fig. 5 is the B-B cutaway view of Fig. 3.
Fig. 6 adopts spherical molybdenum powder prepared by present device to amplify the scanning electron microscope (SEM) photograph of 200 times.
Fig. 7 adopts spherical molybdenum powder prepared by present device to amplify the scanning electron microscope (SEM) photograph of 500 times.
Fig. 8 is the particle size distribution figure that adopts the spherical molybdenum powder prepared of present device.
Description of reference numerals:
1-powder cooling tank; 2-reactor; 3-powder collection tank;
4-cooling cavity; 5-cooling water/gas import; 6-cooling water/gas outlet;
7-reaction cavity; 8-purge gas pipeline; The 9-the first cooling water inlet pipe;
The 10-the first cooling water outlet pipe; 11-insulated water-cooling chuck; 12-molybdenum disk electrode;
The 13-the second cooling water inlet pipe; The 14-the second cooling water outlet pipe; 15-molybdenum bar base;
16-propulsion plant.
Detailed description of the invention
Embodiment 1
A kind of equipment of preparing spherical molybdenum powder shown in Fig. 3, Fig. 4 and Fig. 5 as shown in Figure 1, Figure 2,, comprise the powder cooling tank 1 of upper center opening and be installed on the reactor 2 of powder cooling tank 1 upper center aperture position, and being arranged at the powder collection tank 3 of powder cooling tank 1 below; described reactor 2 comprises the reaction cavity 7 of lower ending opening, level is installed on the insulated water-cooling chuck 11 on reaction cavity 7 and is arranged at the molybdenum disk electrode 12 of reaction cavity 7 inside, the upper end of described reaction cavity 7 is provided with the purge gas pipeline 8 being connected with reaction cavity 7 inside, one end of described insulated water-cooling chuck 11 is through reaction cavity 7 and be positioned at reaction cavity 7, the other end of insulated water-cooling chuck 11 is positioned at outside reaction cavity 7, described molybdenum disk electrode 12 is hollow structure, on described molybdenum disk electrode 12, offer and on water inlet and water inlet, be connected with the first cooling water inlet pipe 9, on described molybdenum disk electrode 12, offer and on delivery port and delivery port, be connected with the first cooling water outlet pipe 10, the outer end of the outer end of described the first cooling water inlet pipe 9 and the first cooling water outlet pipe 10 all passes reaction cavity 7 and is supported on reaction cavity 7, the position that described insulated water-cooling chuck 11 is positioned at outside reaction cavity 7 is connected with the second cooling water inlet pipe 13 and the second cooling water outlet pipe 14, described insulated water-cooling chuck 11 inner clips are held molybdenum bar base 15, described molybdenum bar base 15 passes insulated water-cooling chuck 11 near one end of molybdenum disk electrode 12 and is positioned at outside insulated water-cooling chuck 11, pass between one end of molybdenum bar base 15 of insulated water-cooling chuck 11 and molybdenum disk electrode 12 and leave gap, described molybdenum bar base 15 is provided with the propulsion plant 16 moving horizontally for promoting molybdenum bar base 15 away from one end of molybdenum disk electrode 12.
As shown in Figure 1, between the inner and outer wall of described powder cooling tank 1, be provided with cooling cavity 4, the bottom of described powder cooling tank 1 is provided with the cooling water/gas import 5 being connected with cooling cavity 4, and described powder cooling tank 1 upper end is provided with the cooling water/gas outlet 6 being connected with cooling cavity 4.
As shown in Figure 2, Figure 3 and Figure 4, the gap passing described between one end and the molybdenum disk electrode 12 of molybdenum bar base 15 of insulated water-cooling chuck 11 is 1mm.
As shown in Figure 1, described propulsion plant 16 is electric pushrod or Electrohydraulic push rod.
As shown in Fig. 2, Fig. 3, Fig. 4 and Fig. 5, the diameter of described molybdenum disk electrode 12 is 5~10 times (preferably 5 times, 6 times, 7 times, 8 times, 9 times and 10 times) of molybdenum bar base 15 diameters.
As shown in Fig. 2, Fig. 3, Fig. 4 and Fig. 5, described molybdenum bar base 15 passes insulated water-cooling chuck 11 and is positioned at outside insulated water-cooling chuck 11 away from one end of molybdenum disk electrode 12.
The method that adopts present device to prepare spherical molybdenum powder comprises the following steps:
Step 1, molybdenum bar base 15 is clamped in insulated water-cooling chuck 11, making molybdenum bar base 15 is 1mm near the gap between one end and the molybdenum disk electrode 12 of molybdenum disk electrode 12;
Step 2, in reaction cavity 7, pass into working gas (hydrogen or argon gas, or the mist of argon gas and hydrogen) by purge gas pipeline 8, and pass into cooling water in the first cooling water inlet pipe 9 and the second cooling water inlet pipe 13;
Step 3, switch on to molybdenum disk electrode 12 and molybdenum bar base 15, boosted voltage until molybdenum bar base 15 discharge with molybdenum disk electrode 12, electric discharge is opened propulsion plant 16 simultaneously and is promoted molybdenum bar base 15 and make molybdenum bar base 15 and molybdenum disk electrode 12 keep discharge condition, in discharge process, molybdenum bar base 15 is constantly melt into spherical molybdenum powder near the end face of molybdenum disk electrode 12, described spherical molybdenum powder is by the working gas (hydrogen or the argon gas that pass into from purge gas pipeline 8, or the mist of argon gas and hydrogen) be purged in powder cooling tank 1 cooling, cooled spherical molybdenum powder falls into powder collection tank 3 and collects.
Fig. 6 and Fig. 7 are the scanning electron microscope (SEM) photograph that adopts the spherical molybdenum powder prepared of present device.Fig. 8 is the particle size distribution figure that adopts the spherical molybdenum powder prepared of present device.From Fig. 6 and Fig. 7, can find out that spherical molybdenum powder size prepared by logical present device is inhomogeneous, the basic granular size keeping from raw material molybdenum powder, has embodied present device to the loose adaptive capacity of raw material molybdenum powder.From Fig. 8 particle size distribution figure, also can clearly find out that its particle size distribution and raw material molybdenum powder are substantially close, but the composition of powder major part become spherical.
The above; it is only preferred embodiment of the present invention; not the present invention is done to any restriction, every any simple modification of above embodiment being done according to invention technical spirit, change and equivalent structure change, and all still belong in the protection domain of technical solution of the present invention.

Claims (8)

1. prepare the equipment of spherical molybdenum powder for one kind, it is characterized in that, comprise the powder cooling tank (1) of upper center opening and be installed on the reactor (2) of powder cooling tank (1) upper center aperture position, and be arranged at the powder collection tank (3) of powder cooling tank (1) below; described reactor (2) comprises the reaction cavity (7) of lower ending opening, level is installed on the insulated water-cooling chuck (11) on reaction cavity (7) and is arranged at the inner molybdenum disk electrode (12) of reaction cavity (7), the upper end of described reaction cavity (7) is provided with the purge gas pipeline (8) being connected with reaction cavity (7) inside, one end of described insulated water-cooling chuck (11) is through reaction cavity (7) and be positioned at reaction cavity (7), the other end of insulated water-cooling chuck (11) is positioned at outside reaction cavity (7), described molybdenum disk electrode (12) is hollow structure, on described molybdenum disk electrode (12), offer and on water inlet and water inlet, be connected with the first cooling water inlet pipe (9), on described molybdenum disk electrode (12), offer and on delivery port and delivery port, be connected with the first cooling water outlet pipe (10), the outer end of the outer end of described the first cooling water inlet pipe (9) and the first cooling water outlet pipe (10) all passes reaction cavity (7) and is supported on reaction cavity (7), described insulated water-cooling chuck (11) is positioned at the outer position of reaction cavity (7) and is connected with the second cooling water inlet pipe (13) and the second cooling water outlet pipe (14), described insulated water-cooling chuck (11) inner clip is held molybdenum bar base (15), described molybdenum bar base (15) passes insulated water-cooling chuck (11) and is positioned at outside insulated water-cooling chuck (11) near one end of molybdenum disk electrode (12), pass between one end of molybdenum bar base (15) of insulated water-cooling chuck (11) and molybdenum disk electrode (12) and leave gap, described molybdenum bar base (15) is provided with the propulsion plant (16) moving horizontally for promoting molybdenum bar base (15) away from one end of molybdenum disk electrode (12).
2. a kind of equipment of preparing spherical molybdenum powder according to claim 1, it is characterized in that, between the inner and outer wall of described powder cooling tank (1), be provided with cooling cavity (4), the bottom of described powder cooling tank (1) is provided with the cooling water/gas import (5) being connected with cooling cavity (4), and described powder cooling tank (1) upper end is provided with the cooling water/gas outlet (6) being connected with cooling cavity (4).
3. a kind of equipment of preparing spherical molybdenum powder according to claim 1, is characterized in that, described in the gap that passes between one end and the molybdenum disk electrode (12) of molybdenum bar base (15) of insulated water-cooling chuck (11) be 1mm.
4. a kind of equipment of preparing spherical molybdenum powder according to claim 1, is characterized in that, described propulsion plant (16) is electric pushrod or Electrohydraulic push rod.
5. a kind of equipment of preparing spherical molybdenum powder according to claim 1, is characterized in that, the diameter of described molybdenum disk electrode (12) is 5~10 times of molybdenum bar base (15) diameter.
6. a kind of equipment of preparing spherical molybdenum powder according to claim 1, it is characterized in that, described molybdenum bar base (15) passes insulated water-cooling chuck (11) and is positioned at outside insulated water-cooling chuck (11) away from one end of molybdenum disk electrode (12).
7. adopt equipment as claimed in claim 1 to prepare a method for spherical molybdenum powder, it is characterized in that, the method comprises the following steps:
Step 1, molybdenum bar base (15) is clamped in insulated water-cooling chuck (11), making molybdenum bar base (15) is 1mm near the gap between one end and the molybdenum disk electrode (12) of molybdenum disk electrode (12);
Step 2, in reaction cavity (7), pass into working gas by purge gas pipeline (8), and pass into cooling water in the first cooling water inlet pipe (9) and the second cooling water inlet pipe (13);
Step 3, give molybdenum disk electrode (12) and molybdenum bar base (15) energising, boosted voltage is until molybdenum bar base (15) and molybdenum disk electrode (12) electric discharge, propulsion plant (16) promotion molybdenum bar base (15) is opened in electric discharge simultaneously makes molybdenum bar base (15) and molybdenum disk electrode (12) keep discharge condition, in discharge process, molybdenum bar base (15) is constantly melt into spherical molybdenum powder near the end face of molybdenum disk electrode (12), described spherical molybdenum powder is purged into powder cooling tank (1) cooling by the working gas passing into from purge gas pipeline (8), cooled spherical molybdenum powder falls into powder collection tank (3) and collects.
8. method according to claim 7, is characterized in that, working gas described in step 2 is hydrogen and/or argon gas.
CN201410240884.8A 2014-05-31 2014-05-31 A kind of preparation method of spherical molybdenum powder and equipment Active CN103962567B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106839815A (en) * 2017-03-25 2017-06-13 泰州市万鑫钨钼制品有限公司 A kind of molybdenum powder cooling tube
CN107824120A (en) * 2017-11-29 2018-03-23 郑州大学 It is a kind of that there is the superhigh temperature reactor for extending plasma arcs area
CN108115147A (en) * 2017-12-04 2018-06-05 中国兵器科学研究院宁波分院 A kind of complete closely knit, the spherical molybdenum powder of high apparent density the preparation method of cold spraying

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CN102581293A (en) * 2012-03-16 2012-07-18 河海大学常州校区 Synchronous rotation electrode flour mill
CN103157801A (en) * 2013-04-12 2013-06-19 金堆城钼业股份有限公司 Equipment of restraining spheroidized molybdenum powder of direct current plasma temperature field and method
CN203853547U (en) * 2014-05-31 2014-10-01 金堆城钼业股份有限公司 Equipment for manufacturing spherical molybdenum powder

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JPS56136635A (en) * 1980-03-29 1981-10-26 Res Dev Corp Of Japan Production of ultra-fine powder and particle utilizing arc plasma sputtering and its device
JP2004091843A (en) * 2002-08-30 2004-03-25 Hitachi Metals Ltd Manufacturing method of high purity high melting point metal powder
CN2587554Y (en) * 2002-09-30 2003-11-26 王飚 Apparatus for producing high melting point alloy or ceramic powder by electric-are evaporation method
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106839815A (en) * 2017-03-25 2017-06-13 泰州市万鑫钨钼制品有限公司 A kind of molybdenum powder cooling tube
CN107824120A (en) * 2017-11-29 2018-03-23 郑州大学 It is a kind of that there is the superhigh temperature reactor for extending plasma arcs area
CN108115147A (en) * 2017-12-04 2018-06-05 中国兵器科学研究院宁波分院 A kind of complete closely knit, the spherical molybdenum powder of high apparent density the preparation method of cold spraying

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