CN104070173B - The preparation method of globular tungsten powder - Google Patents
The preparation method of globular tungsten powder Download PDFInfo
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- CN104070173B CN104070173B CN201410280630.9A CN201410280630A CN104070173B CN 104070173 B CN104070173 B CN 104070173B CN 201410280630 A CN201410280630 A CN 201410280630A CN 104070173 B CN104070173 B CN 104070173B
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000007789 gas Substances 0.000 claims abstract description 54
- 239000000843 powder Substances 0.000 claims abstract description 36
- 229910052786 argon Inorganic materials 0.000 claims abstract description 35
- 230000001681 protective effect Effects 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 230000006698 induction Effects 0.000 claims abstract description 7
- 238000011068 loading method Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000003801 milling Methods 0.000 claims abstract description 6
- 238000009833 condensation Methods 0.000 claims abstract description 5
- 230000005494 condensation Effects 0.000 claims abstract description 5
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 5
- 239000001257 hydrogen Substances 0.000 claims description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 14
- 238000002485 combustion reaction Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000011946 reduction process Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000005266 casting Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000005563 spheronization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a kind of preparation method of globular tungsten powder, comprising: sent in airflow milling by raw material tungsten powder and grind, wherein, the granularity of tungsten powder is 5-27 μm; Set up the argon plasma torch of stable operation, during the stable operation of argon plasma torch, the input flow velocity of reacting gas argon is 20-30L/min, the pressure of reacting gas argon is 65kPa-87kPa, the flow velocity of protective gas is 85-115L/min, the pressure of protective gas is 65kPa-87kPa, and the power that induction coil loads is 75kW-90kW; Tungsten powder step one obtained is sent in the high-temperature region of argon plasma torch with loading gas and heats, and the flow velocity being loaded into gas is 4-10L/min, and tungsten powder powder feeding flow is 5-30g/min; The tungsten powder particles drop adding thermosetting enters the rapid condensation of cooling chamber and forms globular tungsten powder.Method of the present invention is improved Oxygen potential, improves the advantage of apparent density of powder and mobility.
Description
Technical field
The present invention relates to the preparation method of globular tungsten powder.
Background technology
Spherical powder has the irreplaceable property of ordinary powder, as good mobility and high apparent density, therefore obtains applying more and more widely in fields such as thermal spraying, injection moulding and gel castings.Because plasma has high temperature, Gao Han, high chemical reactivity, and to reaction atmosphere and reaction temperature, there is the features such as controllability, in the synthesis preparation and spheroidising of powder body material, show particular advantages, cause the concern of people.
At present, external plasma powder handling technology has possessed the production capacity of considerable scale.W is achieved, the spheroidising of the metal dusts such as Mo, Re, Ta, Ni, Cu as (TEKNA) company application radio frequency plasma body technique is received in Canadian Tyke.
Radio frequency plasma has that temperature is high, plasma torch volume is large, energy density is high, heat transfer and the advantage such as cooling velocity is fast, is that preparation component is even, sphericity is high, defect is few, the good approach of the spherical powder of good fluidity.Take plasma as thermal source, in refractory metal spheroidising, there is larger technical advantage.Radio frequency plasma is in the process of spheroidising powder, enough energy that its high temperature provides make powder absorb heat rapidly when passing through plasma, melting, and under surface tension effects polycondensation globulate, within the extremely short time, quenching is solidified, thus forms spherical powder.One of plasma melting spheronization techniques most effective means being considered to obtain fine and close, regular spherical powder.Although, prepare various metal dust by radio frequency plasma body technique and there is plurality of advantages, but due to the defect of technique in prior art, result in powder lower through its Oxygen potential of plasma treatment, the apparent density of powder and mobility is made all not to reach optimum state, therefore, technique of the prior art has greatly improved space.
Summary of the invention
For above-mentioned technical problem, the object of the present invention is to provide a kind of preparation method improving Oxygen potential, improve the globular tungsten powder of apparent density of powder and mobility.
The technical scheme solved the problems of the technologies described above is as follows:
The preparation method of globular tungsten powder, comprises the following steps:
Step one, sends into raw material tungsten powder in airflow milling and grinds, obtain good dispersion, even particle size distribution one-tenth individual particle powder after and carry out abundant drying, wherein, the granularity of tungsten powder is 5-27 μm;
Step 2, set up the argon plasma torch of stable operation, during the stable operation of argon plasma torch, the input flow velocity of reacting gas argon is 20-30L/min, the pressure of reacting gas argon is 65kPa-87kPa, the flow velocity of protective gas is 85-115L/min, the pressure of protective gas is 65kPa-87kPa, and the power that induction coil loads is 75kW-90kW;
Step 3, tungsten powder step one obtained is sent in the high-temperature region of argon plasma torch with loading gas and heats, and the flow velocity being loaded into gas is 4-10L/min, and tungsten powder powder feeding flow is 5-30g/min;
Step 4, the tungsten powder particles drop adding thermosetting enters the rapid condensation of cooling chamber and forms globular tungsten powder, puts into drying box and carry out drying after being collected by globular tungsten powder;
Step 5, globular tungsten powder step 4 obtained carries out slight reduction treatment.
Have employed such scheme, the present invention first grinds raw material tungsten powder, obtain good dispersion, carry out abundant drying after the powder of the one-tenth individual particle of even particle size distribution, the erose corner angle of raw material tungsten powder are eliminated, improving under dispersed and that water content is very low prerequisite, prevent raw material tungsten powder from occurring reuniting, reunion powder is integrally fused in spheroidizing process to avoid postorder to occur in the plasma, nodularization, the situation causing powder size to increase occurs, also avoid the disorder of raw material tungsten powder amount of powder running orbit in nodularization process simultaneously, the tungsten powder of melting collides mutually when passing through plasma, form oarse-grained tungsten powder, therefore by grinding and the dry granularity contributing to guarantee raw material tungsten powder.In addition, running parameter and the powder feed rate of plasma of the present invention are optimized, when raw material tungsten powder is when passing through the high-temperature region of plasma, tungsten powder can fully absorb heat, obtain melting and nodularization, after plasma spheroidization process, obtain the powder of smooth surface, good sphericity, its Oxygen potential reaches 100%, and is still single-phase tungsten powder after nodularization.Due to good sphericity, when these spheric granules are piled up, contact surface is little, and arch formation reduces, and interparticle space is few, improves bulk density.Powder sphericity is higher, and apparent density is larger, and therefore, globular tungsten powder has high apparent density and the feature of high fluidity.Draw through detecting and analyzing, the globular tungsten powder obtained with technique of the present invention, the apparent density after tungsten powder nodularization is by the 6.5g/cm before nodularization
3bring up to 11.5g/cm
3, powder flowbility also significantly improves.
The reduction of described step 5 is using hydrogen plasma as heat source and be loaded into gas, hydrogen plasma heating thermal source enters reduction furnace from the bottom of reduction furnace, the top of globular tungsten powder from reduction furnace under hydrogen plasma current-carrying enters, fall into the high-temperature region of hydrogen plasma heating, globular tungsten powder carries out deoxidation in hydrogen plasma heating district.Although the effect that the tungsten powder obtained through the process of argon plasma torch can not be oxidized, put into after drying box carries out drying after being collected by tungsten powder, tungsten powder more or less can be oxidized, therefore, by the mode of reduction to improve the quality of tungsten powder.Reduction mode of the present invention utilizes the high temperature of hydrogen plasma and high reproducibility, and from top to bottom, heating source from bottom to top, makes tungsten powder reduction process be in suspended state, carries out moment deoxidation to tungsten powder tungsten powder.While adopting hydrogen plasma to carry out reducing, also avoid high temperature sintering and product re-oxidation, and whole process is pollution-free.
Accompanying drawing explanation
Fig. 1 is the enlarged diagram of 1,000 times of tungsten powder before nodularization;
Fig. 2 is the enlarged diagram of 2,000 times of tungsten powder before nodularization;
Fig. 3 is the enlarged diagram of 1,000 times of tungsten powder after nodularization;
Fig. 4 is the enlarged diagram of 2,000 times of tungsten powder after nodularization;
Detailed description of the invention
Referring to figs. 1 through Fig. 4, the preparation method of globular tungsten powder of the present invention, comprises the following steps:
Step one, sends into raw material tungsten powder (as Fig. 1 and Fig. 2) in airflow milling and grinds, obtain good dispersion, even particle size distribution one-tenth individual particle powder after and carry out abundant drying, wherein, the granularity of tungsten powder is 5-27 μm;
Step 2, set up the argon plasma torch of stable operation, during the stable operation of argon plasma torch, the input flow velocity of reacting gas argon is 20-30L/min, the pressure of reacting gas argon is 65kPa-87kPa, the flow velocity of protective gas is 85-115L/min, the pressure of protective gas is 65kPa-87kPa, and the power that induction coil loads is 75kW-90kW;
Step 3, tungsten powder step one obtained is sent in the high-temperature region of argon plasma torch with loading gas and heats, and the flow velocity being loaded into gas is 4-10L/min, and tungsten powder powder feeding flow is 5-30g/min;
Step 4, the tungsten powder particles drop adding thermosetting enters the rapid condensation of cooling chamber and forms globular tungsten powder (as Fig. 3 and Fig. 4), puts into drying box and carry out drying after being collected by globular tungsten powder;
Step 5, globular tungsten powder step 4 obtained carries out slight reduction treatment.The reduction of described step 5 is using hydrogen plasma as heat source and be loaded into gas, hydrogen plasma heating thermal source enters reduction furnace from the bottom of reduction furnace, the top of globular tungsten powder from reduction furnace under hydrogen plasma current-carrying enters, fall into the high-temperature region of hydrogen plasma heating, globular tungsten powder carries out deoxidation in hydrogen plasma heating district.Described protective gas is nitrogen.Combustion chamber and reduction room are set in reduction furnace, a dividing plate is provided with between combustion chamber and reduction room, dividing plate is provided with the through hole that logical combustion flame passes through, heat source burns after entering reduction furnace from the bottom of reduction furnace in a combustion chamber, and combustion flame enters into reduction room by through hole and reduces to tungsten powder.In reduction process, in reduction furnace, pass into protective gas, the flow velocity of described protective gas is 150-400ml/min.Protective gas is arranged in reduction room, protects the tungsten powder of reduction.
Embodiment 1:
Material powder is selected to be tungsten powder in irregular shape, sieve 200 orders, purity > 99.9%, material powder is sent in airflow milling and grinds, obtain the powder of one-tenth individual particle of good dispersion, even particle size distribution, the separation wheel rotating speed of airflow milling is 2500-7000 rev/min, and grinding chamber pressure is 0.1MPa-1MPa, powder feeding rate 1-15kg/ hour.Load for powder room, with atmospheric isolation after deaeration after raw material tungsten powder is fully dry.RF plasma generator first vacuumizes, then working gas argon (Ar) is passed into, start RF plasma generator, set up stable argon plasma torch, during the stable operation of argon plasma torch, the input flow velocity of reacting gas argon is 20L/min, and the pressure of reacting gas argon is 65kPa, and the flow velocity of protective gas is 85L/min, the pressure of protective gas is 65kPa, and the power that induction coil loads is 75kW; Tungsten powder is with loading gas hydrogen (H
2) be sent in the high-temperature region of argon plasma torch and heat, the flow velocity being loaded into gas is 4L/min, and tungsten powder powder feeding flow is 5g/min.The tungsten powder particles drop adding thermosetting enters the rapid condensation of cooling chamber and forms globular tungsten powder, puts into after drying box carries out drying, then carry out slight reduction treatment after being collected by globular tungsten powder.
Embodiment 2:
Difference from Example 1 is: during the stable operation of argon plasma torch, the input flow velocity of reacting gas argon is 25L/min, the pressure of reacting gas argon is 75kPa, the flow velocity of protective gas is 100L/min, and the pressure of protective gas is 75kPa, and the power that induction coil loads is 80kW; Tungsten powder is with loading gas hydrogen (H
2) be sent in the high-temperature region of argon plasma torch and heat, the flow velocity being loaded into gas is 7L/min, and tungsten powder powder feeding flow is 15g/min.
Embodiment 3:
Difference from Example 1 is: during the stable operation of argon plasma torch, the input flow velocity of reacting gas argon is 30L/min, the pressure of reacting gas argon is 87kPa, the flow velocity of protective gas is 115L/min, and the pressure of protective gas is 87kPa, and the power that induction coil loads is 90kW; Tungsten powder is with loading gas hydrogen (H
2) be sent in the high-temperature region of argon plasma torch and heat, the flow velocity being loaded into gas is 10L/min, and tungsten powder powder feeding flow is 30g/min.
Claims (1)
1. the preparation method of globular tungsten powder, comprises the following steps:
Step one, sends into raw material tungsten powder in airflow milling and grinds, obtain good dispersion, even particle size distribution one-tenth individual particle powder after and carry out abundant drying, wherein, the granularity of tungsten powder is 5-27 μm;
Step 2, set up the argon plasma torch of stable operation, during the stable operation of argon plasma torch, the input flow velocity of reacting gas argon is 20-30L/min, the pressure of reacting gas argon is 65kPa-87kPa, the flow velocity of protective gas is 85-115L/min, the pressure of protective gas is 65kPa-87kPa, and the power that induction coil loads is 75kW-90kW;
Step 3, tungsten powder step one obtained is sent in the high-temperature region of argon plasma torch with loading gas and heats, and the flow velocity being loaded into gas is 4-10L/min, and tungsten powder powder feeding flow is 5-30g/min;
Step 4, the tungsten powder particles drop adding thermosetting enters the rapid condensation of cooling chamber and forms globular tungsten powder, puts into drying box and carry out drying after being collected by globular tungsten powder;
Step 5, globular tungsten powder step 4 obtained carries out slight reduction treatment; The reduction of described step 5 is using hydrogen plasma as heat source and be loaded into gas, hydrogen plasma heating thermal source enters reduction furnace from the bottom of reduction furnace, the top of globular tungsten powder from reduction furnace under hydrogen plasma current-carrying enters, fall into the high-temperature region of hydrogen plasma heating, globular tungsten powder carries out deoxidation in hydrogen plasma heating district; Described protective gas is nitrogen; Combustion chamber and reduction room are set in reduction furnace, a dividing plate is provided with between combustion chamber and reduction room, dividing plate is provided with the through hole that logical combustion flame passes through, heat source burns after entering reduction furnace from the bottom of reduction furnace in a combustion chamber, and combustion flame enters into reduction room by through hole and reduces to tungsten powder; In reduction process, in reduction furnace, pass into protective gas, the flow velocity of described protective gas is 150-400ml/min; Protective gas is arranged in reduction room, protects the tungsten powder of reduction.
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| CN105798317B (en) * | 2016-03-31 | 2017-08-25 | 宇辰新能源材料科技无锡有限公司 | A kind of preparation method of polyhedron Sub-micron Tungsten Powder |
| CN106001594B (en) * | 2016-07-15 | 2017-12-22 | 北京科技大学 | A kind of preparation method of super thick globular tungsten powder |
| CN107470639B (en) * | 2017-09-18 | 2019-10-18 | 北京科技大学 | A kind of preparation method of narrow size distribution globular tungsten powder |
| CN111250723A (en) * | 2018-12-03 | 2020-06-09 | 上海大境海洋新材料有限公司 | Method for producing spherical tungsten alloy powder by radio frequency plasma |
| CN114289722B (en) * | 2021-12-08 | 2023-08-29 | 北京科技大学 | Preparation method of fine-grained spherical tungsten powder |
| CN114751450A (en) * | 2022-03-30 | 2022-07-15 | 合肥中航纳米技术发展有限公司 | Method for preparing gas-phase nano titanium dioxide by high-temperature plasma combustion method |
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