CN106216690B - A kind of preparation method of reunion slug type thermal spraying tungsten powder - Google Patents
A kind of preparation method of reunion slug type thermal spraying tungsten powder Download PDFInfo
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- CN106216690B CN106216690B CN201610709015.4A CN201610709015A CN106216690B CN 106216690 B CN106216690 B CN 106216690B CN 201610709015 A CN201610709015 A CN 201610709015A CN 106216690 B CN106216690 B CN 106216690B
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- tungsten powder
- agent solution
- spray drying
- thermal spraying
- ball milling
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 119
- 238000007751 thermal spraying Methods 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 47
- 239000002245 particle Substances 0.000 claims abstract description 34
- 238000001694 spray drying Methods 0.000 claims abstract description 34
- 238000005245 sintering Methods 0.000 claims abstract description 30
- 238000000498 ball milling Methods 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000008367 deionised water Substances 0.000 claims abstract description 22
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 22
- 239000000725 suspension Substances 0.000 claims abstract description 19
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 18
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 18
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 18
- 239000002002 slurry Substances 0.000 claims abstract description 18
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 16
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 16
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 16
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 16
- 238000005238 degreasing Methods 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 230000004913 activation Effects 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000000465 moulding Methods 0.000 claims abstract description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 10
- 238000005507 spraying Methods 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 238000005469 granulation Methods 0.000 abstract description 6
- 230000003179 granulation Effects 0.000 abstract description 6
- 238000009826 distribution Methods 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 37
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 229910052721 tungsten Inorganic materials 0.000 description 4
- 239000010937 tungsten Substances 0.000 description 4
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000012937 correction Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000007908 dry granulation Methods 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- -1 alkali metal salt Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000005563 spheronization Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
Classifications
-
- 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
- B22F9/026—Spray drying of solutions or suspensions
-
- B22F1/0003—
-
- 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
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
- C23C4/08—Metallic material containing only metal elements
-
- 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
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
Abstract
A kind of preparation method of reunion slug type thermal spraying tungsten powder, the following steps are included: choosing Fisher particle size first is 0.8-30 μm of tungsten powder as raw material, then polyvinyl alcohol is weighed, polyethylene glycol, polyvinylpyrrolidone and deionized water are configured to molding agent solution after mixing, by deionized water, tungsten powder is to form agent solution according to mass ratio as (10~20%): 1:(3~10%) it is put into progress ball milling activation in ball mill, after ball milling, tungsten powder suspension slurry is made, tungsten powder suspension slurry obtained is put into spray drying tower, spray drying granulation is used to obtain tungsten powder particles, tungsten powder particles obtained are put into vacuum-sintering integral furnace and successively carry out degreasing and sintering, then sintered tungsten powder is subjected to ball milling, product is made after separating treatment；Size distribution of the present invention is controllable, sphericity is high, good fluidity, impurity content is low, wear-resisting property is good, manufacturing cost is low and is suitable for industrialized production.
Description
Technical field
The present invention relates to Surface Engineering and re-manufacturing technology fields, particularly relate to a kind of reunion slug type thermal spraying
The preparation method of tungsten powder.
Background technique
Plasma spray technology is a kind of surface strengthening technology developed rapidly.It uses special equipment, will using heat source
Metal or nonmetallic materials are heated to fusing or semi-molten state, are injected into workpiece surface with high-speed flow, form coating,
Improve that workpiece is wear-resisting, the performances such as corrosion-resistant.
Tungsten has that fusing point is high, elevated temperature strength is excellent, corrosion resistance is good, thermal conductivity is good, thermal expansion coefficient is small, elasticity modulus it is high with
And the strong advantage of ray ability is absorbed, it is used widely in departments such as Aeronautics and Astronautics, war industry and electronics industries.Wherein
Thermal spraying tungsten powder high-temperature wear resistant coating, the porous tungsten part spraying of production, the spraying of nuclear fusion protecting component, wear-resistant material field,
Heat sink material of electronics industry etc. is widely applied.In spraying field, it is shape that dense spherical powder, particle size range are adjustable
At the basis of uniform coating, ball shaped thermal spray coating tungsten powder not only good fluidity, and obtained coating more evenly, it is fine and close, have more preferable
Wearability and heat resistance.
Currently, the thermal spraying tungsten powder that can be used for spray process has been reported.It has been reported that super using ammonium paratungstate reduction preparation
Thick globular tungsten powder although obtaining the ammonium paratungstate powder of coarse-grain by adding alkali metal salt in ammonium tungstate, and then is prepared thick
Brilliant tungsten powder (Xin Yanjun, Guo Zhimeng, Luo Ji, Wang Ruixin, Fang Zhe prepare super thick globular tungsten powder at the reduction of ammonium paratungstate), produces
The impurity content of product is few, with high purity, but its parameter is not easy to control, particle size range is not easy to control and adjusts, poor fluidity, uncomfortable
Close the industrialized production of thermal spraying tungsten powder.
There is scholar's research by carrying out Shape correction to particulate oxidation tungsten, after screening process, in reducing atmosphere
Under restored to by the tungsten oxide powder of Shape correction, sphere-like tungsten powder particle (Jia Chengchang, Wang Cong are obtained after cooling
Acute hearing, Liang Dong, Gao Peng, a kind of preparation method .CN201310042633.4 of sphere-like tungsten powder of Cui Zhaowen, Chang Yuhong), but its
The tungsten powder of preparation is spherical shape, and particle size range is single.
Also have and globular tungsten powder used for hot spraying is prepared using plasma spheroidization technology, common tungsten powder is added to plasma by the method
In jet stream, make tungsten powder particles surface or integrally fused formation molten drop, molten drop is shrunk to spherical shape due to surface tension, then by fast
Quickly cooling but, to obtain globular tungsten powder, although can prepare by this method particle surface is highly polished, density increases,
Brittleness reduces and the thermal spraying tungsten powder of good fluidity (Hou Yubai, Zeng Keli, in moonlight, Ren Guangjing, Xu Genguo, Ma Jianghong etc. from
Bulbec tungsten powder non-ferrous metal, 2008.60 (1): 41,43) (Guo Shuanquan, Ge Changchun, Feng Yunbiao, Zhou Zhangjian low cost etc. from
Sub- spheronization techniques prepare the technical study powder metallurgy industry of globular tungsten powder used for hot spraying, 2010.20 (3): Isosorbide-5-Nitrae), but should
The equipment of method is expensive, and energy consumption is high, and preparation cost is high, and nodularization process tungsten powder occurs and is oxidized phenomenon, it is difficult to realize industrialization
Production and application.
Summary of the invention
In order to solve the above-mentioned technical problem the present invention, provides a kind of preparation method of reunion slug type thermal spraying tungsten powder,
Size distribution is controllable, sphericity is high, good fluidity, impurity content is low, wear-resisting property is good, manufacturing cost is low and is suitable for industrialization
Production.
The technical scheme adopted by the invention is that: a kind of preparation method of reunion slug type thermal spraying tungsten powder, including it is following
Step:
Step 1: choosing Fisher particle size is 0.8-30 μm of tungsten powder as raw material, it is spare；
It is configured to after mixing Step 2: weighing polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and deionized water
Agent solution is formed, it is spare, wherein polyvinyl alcohol accounts for the 0~3% of the forming agent solution quality, polyethylene glycol and accounts for the forming agent
Solution quality 0~3%, polyvinylpyrrolidone account for the 10~25% of the forming agent solution quality, deionized water account for it is described at
The 75~90% of type agent solution quality；
Step 3: by deionized water and the weighed tungsten powder of step 1 and the weighed molding agent solution of step 2 according to quality
Than for (10~20%): 1:(3~10%) it is put into progress ball milling activation in ball mill, after ball milling, tungsten powder suspension slurry is made,
It is spare；
Step 4: tungsten powder suspension slurry made from step 3 is put into spray drying tower, in the import of spray drying tower
Using spraying dry under conditions of temperature is 250~350 DEG C, outlet temperature is 100~140 DEG C, feeding pressure is 0.2-3.0MPa
Dry granulation is spare to obtain sphericity and the good tungsten powder particles of consistency；
Step 5: tungsten powder particles made from step 4, which are put into vacuum-sintering integral furnace, successively carries out degreasing and sintering,
In, skimming temp is 350~650 DEG C, and the time is 2~5 hours；Sintering temperature is 1300~1600 DEG C, and the time is 1~4 hour,
Protective atmosphere during degreasing and sintering is argon gas or nitrogen；
Step 6: 1 ~ 3h of ball milling will be carried out in ball mill pulverizer through step 5 sintered tungsten powder, then in charging speed
Degree is 100~200kg/h, and air quantity is 1500~2500m3Air current classifying is carried out under conditions of/h obtains granularity in 15-120 μm of model
Interior thermal spraying tungsten powder is enclosed, product is made.
The spray drying tower is one of pressure spray drying tower or Centrafugal spray drying tower.
Beneficial effects of the present invention:
(1) tungsten powder raw material needed for the present invention is general commercial tungsten powder, and raw material is cheap and easy to get；Required forming agent polyvinyl alcohol,
Polyethylene glycol, polyvinylpyrrolidone are cheap, pollution-free；
(2) tungsten powder suspension is aqueous solution, safety and operator is without actual bodily harm in the present invention；The present invention uses pressure
Formula spray drying tower or Centrafugal spray drying tower and vacuum-sintering integral furnace technique are controllable, stay in grade；
(3) tungsten powder that the present invention has been sintered ball mill crushing in crusher, particle Oxygen potential is high, surface smoothness is good；
(4) its size distribution of the reunion slug type thermal spraying tungsten powder of use invention preparation is controllable, sphericity is high, mobility
Well, impurity content is low, wear-resisting property is good, manufacturing cost is low and is suitable for industrialized production.Reunion slug type thermal spraying obtained
Tungsten powder apparent density is 3.5~8.0g/cm3, and flow velocity is 8~20s/50g, and granularity is 15-120 μm, and vacuum plasma can be used
Or low-voltage plasma spraying forms coating structure.
Detailed description of the invention
Fig. 1 is the reunion slug type thermal spraying tungsten powder surface aspect graph that the embodiment of the present invention 1 is produced.
Fig. 2 is the reunion slug type thermal spraying tungsten powder surface aspect graph that the embodiment of the present invention 2 is produced.
Fig. 3 is the coating structure figure that thermal spraying tungsten powder of the present invention is formed by vacuum plasma spray coating.
Specific embodiment
A kind of preparation method of reunion slug type thermal spraying tungsten powder, comprising the following steps:
Step 1: choosing Fisher particle size is 0.8-30 μm of tungsten powder as raw material, it is spare；
It is configured to after mixing Step 2: weighing polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and deionized water
Agent solution is formed, it is spare, wherein polyvinyl alcohol accounts for the 0~3% of the forming agent solution quality, polyethylene glycol and accounts for the forming agent
Solution quality 0~3%, polyvinylpyrrolidone account for the 10~25% of the forming agent solution quality, deionized water account for it is described at
The 75~90% of type agent solution quality；
Step 3: by deionized water and the weighed tungsten powder of step 1 and the weighed molding agent solution of step 2 according to quality
Than for (10~20%): 1:(3~10%) it is put into progress ball milling activation in ball mill, after ball milling, tungsten powder suspension slurry is made,
It is spare；
Step 4: tungsten powder suspension slurry made from step 3 is put into spray drying tower, in the import of spray drying tower
Using spraying dry under conditions of temperature is 250~350 DEG C, outlet temperature is 100~140 DEG C, feeding pressure is 0.2-3.0MPa
Dry granulation is spare to obtain sphericity and the good tungsten powder particles of consistency；
Step 5: tungsten powder particles made from step 4, which are put into vacuum-sintering integral furnace, successively carries out degreasing and sintering,
In, skimming temp is 350~650 DEG C, and the time is 2~5 hours；Sintering temperature is 1300~1600 DEG C, and the time is 1~4 hour,
Protective atmosphere during degreasing and sintering is argon gas or nitrogen；
Step 6: 1 ~ 3h of ball milling will be carried out in ball mill pulverizer through step 5 sintered tungsten powder, then in charging speed
Degree is 100~200kg/h, and air quantity is 1500~2500m3Air current classifying is carried out under conditions of/h obtains granularity in 15-120 μm of model
Interior thermal spraying tungsten powder is enclosed, product is made.
The spray drying tower is one of pressure spray drying tower or Centrafugal spray drying tower.
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1
A kind of preparation method of reunion slug type thermal spraying tungsten powder, comprising the following steps:
Step 1: choosing Fisher particle size is 3 μm of tungsten powder as raw material, it is spare；
It is configured to after mixing Step 2: weighing polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and deionized water
Form agent solution, it is spare, wherein polyvinyl alcohol account for the 1.64% of the forming agent solution quality, polyvinylpyrrolidone account for it is described
Forming agent solution quality 16.39%, deionized water account for the 81.97% of the forming agent solution quality；
Step 3: by deionized water and the weighed tungsten powder of step 1 and the weighed molding agent solution of step 2 according to quality
Ball milling activation is carried out than being put into ball mill for 14%:1:6%, after ball milling, tungsten powder suspension slurry is made, it is spare；
Step 4: tungsten powder suspension slurry made from step 3 is put into pressure spray drying tower, in spray drying tower
Inlet temperature be 260 DEG C, outlet temperature is 105 DEG C, feeding pressure used under conditions of being 0.5MPa spray drying granulation with
Sphericity and the good tungsten powder particles of consistency are obtained, it is spare；
Step 5: tungsten powder particles made from step 4, which are put into vacuum-sintering integral furnace, successively carries out degreasing and sintering,
In, skimming temp is 400 DEG C, and the time is 2 hours；Sintering temperature is 1350 DEG C, and the time is 2 hours, and it is equal to degrease and sinter atmosphere
For argon gas or nitrogen；
Step 6: ball milling 1h will be carried out in ball mill pulverizer through step 5 sintered tungsten powder, then in charging rate
For 130kg/h, air quantity 1800m3Air current classifying is carried out under conditions of/h obtains thermal spraying tungsten of the granularity in 15-63 μ m
Powder.
The reunion slug type thermal spraying tungsten powder detection data of the present embodiment is as shown in table 1, and configuration of surface is as shown in Figure 1:
The testing result table of 1 embodiment of table, 1 reunion slug type thermal spraying tungsten powder
| W content | Oxygen content | Apparent density (g/cm3) | Flow velocity (s/50g) | Size distribution (μm) |
| W≥99.9% | 0.05% | 4.40 | 15.0 | 15~63 |
Embodiment 2
A kind of preparation method of reunion slug type thermal spraying tungsten powder, comprising the following steps:
Step 1: choosing Fisher particle size is 1 μm of tungsten powder as raw material, it is spare；
It is configured to after mixing Step 2: weighing polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and deionized water
Form agent solution, it is spare, wherein polyethylene glycol account for the 2.5% of the forming agent solution quality, polyvinylpyrrolidone account for it is described
Forming agent solution quality 12.5%, deionized water account for the 85% of the forming agent solution quality；
Step 3: by deionized water and the weighed tungsten powder of step 1 and the weighed molding agent solution of step 2 according to quality
Ball milling activation is carried out than being put into ball mill for 14%:1:6%, after ball milling, tungsten powder suspension slurry is made, it is spare；
Step 4: tungsten powder suspension slurry made from step 3 is put into Centrafugal spray drying tower, in spray drying tower
Inlet temperature be 290 DEG C, outlet temperature is 115 DEG C, feeding pressure uses spray drying granulation to obtain under conditions of being 2MPa
Sphericity and the good tungsten powder particles of consistency are obtained, it is spare；
Step 5: tungsten powder particles made from step 4, which are put into vacuum-sintering integral furnace, successively carries out degreasing and sintering,
In, skimming temp is 550 DEG C, and the time is 2 hours；Sintering temperature is 1400 DEG C, and the time is 3 hours, and it is equal to degrease and sinter atmosphere
For argon gas or nitrogen；
Step 6: ball milling 2h will be carried out in ball mill pulverizer through step 5 sintered tungsten powder, then in charging rate
For 170kg/h, air quantity 2400m3Air current classifying is carried out under conditions of/h obtains thermal spraying tungsten of the granularity in 45-75 μ m
Powder.
The testing result table of 2 embodiment of table, 2 reunion slug type thermal spraying tungsten powder
Embodiment 3
A kind of preparation method of reunion slug type thermal spraying tungsten powder, comprising the following steps:
Step 1: choosing Fisher particle size is 0.8 μm of tungsten powder as raw material, it is spare；
It is configured to after mixing Step 2: weighing polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and deionized water
Form agent solution, it is spare, wherein polyvinyl alcohol account for the 3% of the forming agent solution quality, polyvinylpyrrolidone account for it is described at
Type agent solution quality 10%, deionized water account for the 87% of the forming agent solution quality；
Step 3: by deionized water and the weighed tungsten powder of step 1 and the weighed molding agent solution of step 2 according to quality
Ball milling activation is carried out than being put into ball mill for 10%:1:3%, after ball milling, tungsten powder suspension slurry is made, it is spare；
Step 4: tungsten powder suspension slurry made from step 3 is put into pressure spray drying tower, in spray drying tower
Inlet temperature be 250 DEG C, outlet temperature is 100 DEG C, feeding pressure used under conditions of being 0.2MPa spray drying granulation with
Sphericity and the good tungsten powder particles of consistency are obtained, it is spare；
Step 5: tungsten powder particles made from step 4, which are put into vacuum-sintering integral furnace, successively carries out degreasing and sintering,
In, skimming temp is 350 DEG C, and the time is 2 hours；Sintering temperature is 1300 DEG C, and the time is 1 hour, and it is equal to degrease and sinter atmosphere
For argon gas or nitrogen；
Step 6: ball milling 1h will be carried out in ball mill pulverizer through step 5 sintered tungsten powder, then in charging rate
For 100kg/h, air quantity 1500m3Air current classifying is carried out under conditions of/h obtains thermal spraying of the granularity in 15-120 μ m
Tungsten powder.
Embodiment 4
A kind of preparation method of reunion slug type thermal spraying tungsten powder, comprising the following steps:
Step 1: choosing Fisher particle size is 30 μm of tungsten powder as raw material, it is spare；
It is configured to after mixing Step 2: weighing polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and deionized water
Form agent solution, it is spare, wherein polyethylene glycol account for the 3% of the forming agent solution quality, polyvinylpyrrolidone account for it is described at
Type agent solution quality 22%, deionized water account for the 75% of the forming agent solution quality；
Step 3: by deionized water and the weighed tungsten powder of step 1 and the weighed molding agent solution of step 2 according to quality
Ball milling activation is carried out than being put into ball mill for 20%:1:10%, after ball milling, tungsten powder suspension slurry is made, it is spare；
Step 4: tungsten powder suspension slurry made from step 3 is put into Centrafugal spray drying tower, in spray drying tower
Inlet temperature be 350 DEG C, outlet temperature is 140 DEG C, feeding pressure used under conditions of being 3.0MPa spray drying granulation with
Sphericity and the good tungsten powder particles of consistency are obtained, it is spare；
Step 5: tungsten powder particles made from step 4, which are put into vacuum-sintering integral furnace, successively carries out degreasing and sintering,
In, skimming temp is 650 DEG C, and the time is 5 hours；Sintering temperature is 1600 DEG C, and the time is 4 hours, and it is equal to degrease and sinter atmosphere
For argon gas or nitrogen；
Step 6: ball milling 3h will be carried out in ball mill pulverizer through step 5 sintered tungsten powder, then in charging rate
For 200kg/h, air quantity 2500m3Air current classifying is carried out under conditions of/h obtains thermal spraying of the granularity in 15-120 μ m
Tungsten powder.
Embodiment 5
A kind of preparation method of reunion slug type thermal spraying tungsten powder, comprising the following steps:
Step 1: choosing Fisher particle size is 15 μm of tungsten powder as raw material, it is spare；
It is configured to after mixing Step 2: weighing polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and deionized water
Agent solution is formed, it is spare, wherein polyvinyl alcohol accounts for the 1.5% of the forming agent solution quality, polyethylene glycol and accounts for the forming agent
Solution quality 1.5%, polyvinylpyrrolidone account for that the 10% of the forming agent solution quality, that deionized water accounts for the forming agent is molten
The 87% of liquid quality；
Step 3: by deionized water and the weighed tungsten powder of step 1 and the weighed molding agent solution of step 2 according to quality
Ball milling activation is carried out than being put into ball mill for 15%:1:7%, after ball milling, tungsten powder suspension slurry is made, it is spare；
Step 4: tungsten powder suspension slurry made from step 3 is put into pressure spray drying tower, in spray drying tower
Inlet temperature be 300 DEG C, outlet temperature is 120 DEG C, feeding pressure used under conditions of being 1.7MPa spray drying granulation with
Sphericity and the good tungsten powder particles of consistency are obtained, it is spare；
Step 5: tungsten powder particles made from step 4, which are put into vacuum-sintering integral furnace, successively carries out degreasing and sintering,
In, skimming temp is 500 DEG C, and the time is 3 hours；Sintering temperature is 1450 DEG C, and the time is 3 hours, and it is equal to degrease and sinter atmosphere
For argon gas or nitrogen；
Step 6: ball milling 2h will be carried out in ball mill pulverizer through step 5 sintered tungsten powder, then in charging rate
For 150kg/h, air quantity 2000m3Air current classifying is carried out under conditions of/h obtains thermal spraying of the granularity in 15-120 μ m
Tungsten powder.
Claims (2)
1. a kind of preparation method of reunion slug type thermal spraying tungsten powder, it is characterised in that: the following steps are included:
Step 1: choosing Fisher particle size is 0.8-30 μm of tungsten powder as raw material, it is spare；
It is configured to form after mixing Step 2: weighing polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and deionized water
Agent solution, it is spare, wherein polyvinyl alcohol accounts for the 0~1.64% of the forming agent solution quality, polyethylene glycol and accounts for the forming agent
Solution quality 0~2.5%, polyvinylpyrrolidone accounts for the 12.5~16.39% of the forming agent solution quality, deionized water and accounts for
The 81.97~85% of the forming agent solution quality；
Step 3: being according to mass ratio with the weighed tungsten powder of step 1 and the weighed molding agent solution of step 2 by deionized water
(10~20%): 1:(3~10%) it is put into ball mill progress ball milling activation, after ball milling, tungsten powder suspension slurry is made, it is standby
With；
Step 4: tungsten powder suspension slurry made from step 3 is put into spray drying tower, in the inlet temperature of spray drying tower
It is made under conditions of for 250~350 DEG C, outlet temperature be 100~140 DEG C, feeding pressure is 0.2-3.0MPa using spray drying
Grain is spare to obtain sphericity and the good tungsten powder particles of consistency；
Step 5: tungsten powder particles made from step 4, which are put into vacuum-sintering integral furnace, successively carries out degreasing and sintering, wherein de-
Rouge temperature is 350~650 DEG C, and the time is 2~5 hours；Sintering temperature is 1300~1600 DEG C, and the time is 1~4 hour, degreasing
It is argon gas or nitrogen with the protective atmosphere in sintering process；
Step 6: 1 ~ 3h of ball milling will be carried out in ball mill pulverizer through step 5 sintered tungsten powder, then it is in charging rate
100~200kg/h, air quantity are 1500~2500m3Air current classifying is carried out under conditions of/h obtains granularity in 15-120 μ m
Thermal spraying tungsten powder, be made product.
2. a kind of preparation method of reunion slug type thermal spraying tungsten powder as described in claim 1, it is characterised in that: described spraying
Drying tower is one of pressure spray drying tower or Centrafugal spray drying tower.
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| CN109047781B (en) * | 2018-08-16 | 2021-11-30 | 北京科技大学 | Method for preparing large-size tungsten product |
| CN111922330B (en) * | 2020-06-17 | 2022-04-22 | 广东省科学院新材料研究所 | Metal tungsten powder for laser additive manufacturing of tungsten product, tungsten product and preparation method of tungsten product |
| CN111644612A (en) * | 2020-06-19 | 2020-09-11 | 安徽省春谷3D打印智能装备产业技术研究院有限公司 | Preparation method of plasma sintering agglomerated metal ceramic thermal spraying composite powder |
| CN115401195A (en) * | 2022-09-13 | 2022-11-29 | 中国化学工程第十一建设有限公司 | A particle-reinforced high-entropy alloy powder and its preparation method and application |
| CN116422876B (en) * | 2023-02-25 | 2024-11-26 | 湖南顶立科技股份有限公司 | Spherical tungsten powder for additive manufacturing, preparation method and application |
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