CN101664809B - Uniform macromeritic tungsten powder and method for preparing tungsten carbide powder - Google Patents
Uniform macromeritic tungsten powder and method for preparing tungsten carbide powder Download PDFInfo
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Abstract
The invention discloses a uniform macromeritic tungsten powder. During reduction, water vapor and hydrogen or a mixture thereof is sent into a reducing furnace, and tungsten oxide powder materials or mixture materials of tungsten oxide powder and tungsten powder, which are pushed into the reducing furnace, are reduced to metallic tungsten powder by controlling the partial pressure ratio (PH2O/PH2) of the water vapor and the hydrogen sent into the reducing furnace and the temperature of the furnace. By the adjustment of technological parameters, macromeritic tungsten powder of multiple grades in the range of 10-100 micrometers can be prepared. The prepared macromeritic tungsten powder has the advantages of comparatively uniform granularity, integrated crystallization, attractive appearance and high purity. After the carbonization of the macromeritic tungsten powder, uniform macromeritic tungsten carbide powder of 12-115 micrometers can be prepared. The invention can be used for producing macromeritic and super macromeritic hard alloy products of more than 4 micrometers and can be also used for the surface spray coating, the spray welding and the like of hard-surface materials.
Description
Technical field
The invention belongs to the refractory metal smelting technique, relate to a kind of preparation method of even coarse grain tungsten powder, and utilize this coarse grain tungsten powder to prepare the method for coarse grain tungsten-carbide powder.Evenly coarse grain tungsten powder and tungsten-carbide powder are mainly used in preparation coarse-grain, ultra coarse-grain carbide alloy, and production mine instrument, diel, brill pick, digging instrument also can be applicable to hard materials such as spraying, surfacing.
Background technology
The coarse grain tungsten carbide is because of its crystal property is good, fault of construction is few, the subgrain size is thick, microhardness is high, microstrain is little, have certain series of advantages such as plasticity; Be used to produce carbide alloy; Can significantly improve anti-fracture (impact) toughness of coarse-grain carbide alloy, improve service life and be able to extensive use.Therefore; Crystal grain is thick, even, the good crystallization tungsten-carbide powder is the key of preparation high-performance coarse-grain carbide alloy, and the factor of influence preparation coarse grain tungsten-carbide powder most critical is to prepare that crystal grain is thick, even, advantages of good crystallization, high-purity high-quality tungsten powder.Preparing the comparatively traditional method of coarse grain tungsten powder, tungsten carbide powder both at home and abroad is tungsten oxide high temperature reduction high temperature cabonization method; This method generally all is to adopt the dry hydrogen reduction, and reduction temperature requires 900～1200 ℃, even higher; Then with tungsten powder carbonization under the temperature more than 1600 ℃; The tungsten powder of being produced, the granularity of tungsten carbide powder can only reach 7～15 μ m, and the powder size uniformity is bad, and fine powder is more.
A kind of method that external preparation coarse grain tungsten-carbide powder is used morely is an aluminothermic process.E.N.Smith delivers on the 53rd, 54 page of " Metal Powder Report " magazine the 35th volume the 2nd (in February, 1980) is entitled as the technological principle that was described in detail aluminothermic process in " the magnanimity method of Direct Production one tungsten carbide " literary composition.U.S.'s Kennametal (Kennametal) is at its patent U.S 4; 834; A kind of method for preparing the coarse grain tungsten-carbide powder with aluminothermic process is disclosed in 963; This method is that raw material, iron oxide are that oxidant, aluminium are made reducing agent, calcium carbide is made carburization agent with the tungsten concentrate, these material balls is mixed the back prepare the coarse grain tungsten-carbide powder in reaction and fusion carbonization more than 2000 ℃.Patent 87107470 " coarse-grain---tungsten-carbide powder and production method thereof " discloses a kind of improved aluminothermic process and has been used to prepare the coarse grain tungsten-carbide powder.This method is a primary raw material with the tungsten ore washed ore, in reaction feed, adds certain iron, so that the reaction temperature of calculating is controlled in the scope of 4372～4500 ° of F.Disclosed method also is similar to aluminothermic process in the patent 200810044355.5 " a kind of production method of coarse crystal WC powder "; But be to be raw material with the tungsten oxide; Rather than use tungsten concentrate to be raw material, in tungsten oxide, add a certain proportion of C, Fe (Co, Ni), the oxide of iron, Al-Ni alloyed powder; Carry out the high-temperature fusion carbonization then, the alloy block after the carbonization gets coarse grain WC powder after fragmentation, ball milling, removal of impurities, screening.The granularity of the coarse grain tungsten carbide of above-mentioned various aluminothermic process preparation is all very thick, but the major defect that exists is that operation is longer, and impurities is on the high side, and some impurity can't be removed fully and finally influence the combination property of alloy.
A kind of method that preparation coarse grain tungsten-carbide powder is used morely in the industry is with alkali metal compound doped tungsten oxide high temperature reduction high temperature cabonization.US4402737 has described tungsten oxide and has used alkali metal chloride, and the particularly doping of LiCl can obtain the thicker metal tungsten powder of granularity after the reduction, but its research purpose is a polycrystal powder.Form the aggregation of thin WC crystal after this tungsten powder carbonization.Patent 01815126.4 " Ultracoarse, monocrystalline tungsten carbide and its preparation method and the hard metal of preparation " thus disclosed method be with tungsten oxide and alkali carbonate (by at least two kinds in potash, lithium carbonate, the sodium carbonate mix, fusion, quenching and powdered and get) press the proper proportion mixing, at high temperature be reduced into metal tungsten powder with hydrogen then.This kind metal tungsten powder is through obtaining the coarse grain tungsten-carbide powder more than the 50 μ m behind the high temperature cabonization.Be equipped with the coarse grain tungsten-carbide powder with alkali metal compound doped tungsten oxide high temperature reduction high temperature cabonization legal system and have following shortcoming: 1) coarse grain tungsten powder defective is many, and crystallization is bad, and distortion crystal grain is many; 2) be trapped in the carbonisation on the contrary can crystal grain thinning for alkali metal, is prone to cause impurity content higher; 3) bad, the lack of homogeneity of grain morphology.
Summary of the invention
The object of the present invention is to provide a kind of new method for preparing even coarse grain tungsten powder, and utilize said coarse grain tungsten powder to prepare the method for even coarse grain tungsten-carbide powder.
The preparation method of even coarse grain tungsten powder of the present invention; Comprise successively: with the oxide powder of tungsten, or the mixture of the oxide powder of tungsten and tungsten powder reduces in reduction furnace as raw material, the coarse grain tungsten powder of reduction gained sieved to handle remove oxide skin; Promptly get described even coarse grain tungsten powder; When reduction, in reduction furnace, send into earlier the steam and the hydrogen of certain flow, the intrinsic standoff ratio P of interior steam of reduction furnace and hydrogen is sent in control
H2O/ P
H2Be 0.1～1.64, push the material boat that powder stock is housed then; The coarse grain tungsten powder particle-size of reduction gained is 10～100 μ m.
The temperature of said reduction reaction is 900～1350 ℃, and the reduction reaction time is 3～50 hours.
The oxide of described tungsten is any one in yellow tungsten oxide, blue tungsten oxide, purple tungsten oxide, the tungsten dioxide, perhaps two or more combinations.
When being raw material with the mixture of the oxide powder of tungsten and tungsten powder, the shared mass percent of tungsten powder is 0.5%-30%.
Utilize described even coarse grain tungsten powder to prepare the method for even coarse grain tungsten-carbide powder; Comprise successively: as raw material, join that the charcoal ball mixes, carbonization with said even coarse grain tungsten powder, the ball mill crushing of coming out of the stove then, sieving promptly gets described even coarse grain tungsten-carbide powder; It is characterized in that: said carburizing temperature is 1600-2500 ℃; Carbonization time 1-30 hour, carburizing atmosphere was hydrogen or argon gas, and carbonization gained coarse grain tungsten-carbide powder granularity is 12～115 μ m.
The granularity of the used tungsten oxide powder stock of the present invention is not limit, and preferred version is the powder stock that adopts 10～30 μ m.When the present invention adopts the mixture of tungsten oxide powder and tungsten powder to be initiation material; The granularity of used tungsten powder is not limit, the granularity of tungsten powder in the preferred version >=3 μ m, and the tungsten powder of adding plays the seed crystal effect; Can make the crystal grain of reduction gained tungsten powder thicker, the speeding up of reduction reaction.
Preparation method of the present invention is different from the method for traditional high temperature reduction high temperature cabonization, and this method also is different from the method for alkali metal compound doped tungsten oxide high temperature reduction high temperature cabonization.The present invention is through sending into steam and hydrogen in reduction furnace, or sends into the mixture of steam and hydrogen, and steam and the intrinsic standoff ratio (P of hydrogen in the reduction furnace are sent in control
H2O/ P
H2), make process that the oxidation tungsten powder is reduced into metal tungsten powder at certain P
H2O/ P
H2Under carry out.
Tungsten oxide is by WO under the high temperature
3→ WO
2.9→ WO
2.72→ WO
2The order gradual deoxidizing of → W obtains tungsten powder, wherein WO at last
3→ WO
2.9→ WO
2.72→ WO
2The reduction reaction speed of this several links is all very fast, and WO
2The reduction reaction speed of → W comparatively speaking will be slowly many, the granularity of metal tungsten powder also mainly receives WO
2This link of → W is controlled.The present invention sends into steam and hydrogen in reduction furnace, or sends into the mixture of steam and hydrogen, and its main purpose is exactly to guarantee to make WO under the condition that reduction reaction can be carried out smoothly
2The reduction reaction process of → W has sufficiently high P
H2O/ P
H2, the quantity with control formation W nucleus is fully grown up W crystal grain.Reduction temperature is high more, P in the stove
H2O/ P
H2High more, the crystal grain of gained tungsten powder is thick more.Under the uniform temperature, P in the stove
H2O/ P
H2High more, the crystal grain of gained tungsten powder is thick more, but the required recovery time is also long more.
Through the adjustment of technological parameter, can prepare the coarse grain tungsten powder of a plurality of grades in the 10-100um scope with this method, and the tungsten powder particle crystallization is good, uniform crystal particles, purity are high.It is thick to have crystal grain equally with the coarse grain tungsten-carbide powder for preparing behind the coarse grain tungsten powder of this method preparation and the carbon black mixing high temperature cabonization, and purity height, advantages of good crystallization, fault of construction is few, the subgrain size is thick, microhardness is high, the little series of advantages of waiting until of microstrain.With this kind coarse grain tungsten-carbide powder prepare coarse-grain, ultra coarse-grain carbide alloy combination property significantly improves.
Because the similarity of molybdenum oxide hydrogen reduction reaction and tungsten oxide hydrogen reduction reaction is sent into steam and hydrogen, or sent into the mixture of steam and hydrogen in reduction furnace, the intrinsic standoff ratio (P of interior water vapour of reduction furnace and hydrogen is sent in control
H2O/ P
H2), can use molybdenum oxide powder reduction preparation coarse-grain molybdenum powder equally.Can obtain coarse-grain carbonization molybdenum powder after the carbonization of coarse-grain molybdenum powder.
The specific embodiment
Embodiment 1: adopting the blue oxide tungsten powder of the about 20 μ m of Fsss granularity (down together) is raw material, the about 6Kg raw material of every boat dress.The reduction furnace temperature is risen to 1000 ℃, in stove, send into water vapour and hydrogen, the P in the stove is sent in control
H2O/ P
H2Be 0.45.Push the material boat then, reduce about 15h, the descale that sieves after the discharging obtains the coarse grain tungsten powder, and the Fsss granularity is about 21 μ m.The pattern of gained coarse grain tungsten powder can find out that shown in accompanying drawing 1 crystal grain of tungsten powder particle is very thick, and is more even, and fine powder is few, and particle crystallization is good.
Gained coarse grain tungsten powder is joined carbon by known method, and mixed carbon comtent is 6.15%, puts into the carbide furnace carbonization then, and carburizing temperature is 2300 ℃, and carbonization time is about 2h, and carburizing atmosphere is a hydrogen.Treat that but furnace temperature reduces to discharging after the tapping temperature,, obtain the coarse grain tungsten-carbide powder after sieving the ratio of grinding media to material ball mill crushing of coarse grain tungsten carbide agglomerate by 1: 1.The granularity of gained coarse grain tungsten-carbide powder is about 23.2 μ m, and pattern can find out that shown in accompanying drawing 2 the tungsten-carbide powder particle surface is fine and close, and smooth, crystallization is fine.
Preparing alloy with above-mentioned coarse grain tungsten-carbide powder is example: with gained coarse grain tungsten-carbide powder in ball mill with 9.5% metal cobalt powder wet-milling (material: ball=1: 2 weight ratio) after 15 hours; Through 1450 ℃ of vacuum-sinterings; Obtaining hardness of alloy HRA is 86, and its porosity is pressed ISO 4505 and is A02 B00.The metallograph of alloy shown in accompanying drawing 3, the about 7 μ m of alloy grain degree, crystal grain is more even.
Embodiment 2: embodiment 1 gained coarse grain tungsten powder is joined carbon by known method, and mixed carbon comtent is 6.15%, puts into the carbide furnace carbonization then, and carburizing temperature is 2300 ℃, and carbonization time is 5h, and carburizing atmosphere is Ar.Treat that but furnace temperature reduces to discharging after the tapping temperature, handle obtaining the coarse grain tungsten-carbide powder then by embodiment 1 same method.The granularity of gained coarse grain tungsten-carbide powder is about 24 μ m, shown in the also similar accompanying drawing 2 of pattern.
Embodiment 3: in the blue oxide tungsten powder of about 20 μ m, mix the tungsten powder that weight ratio is approximately 5%, granularity is about 3 μ m, mix the material boat of packing into after 1～2 hour, the above-mentioned mixed material of every boat about 6Kg of dress.The reduction furnace temperature is risen to 1000 ℃, in stove, send into water vapour and hydrogen, the P in the stove is sent in control
H2O/ P
H2Be 0.5.Push the material boat then, reduce about 10h, the descale that sieves after the discharging obtains the coarse grain tungsten powder, and the Fsss granularity is about 27 μ m.The pattern of gained coarse grain tungsten powder can find out that shown in accompanying drawing 4 crystal grain of tungsten powder particle is thicker than embodiment's 1, and is equally also very even, advantages of good crystallization.
Gained coarse grain tungsten powder is carried out carbonization treatment by embodiment 1 same method, and the coarse grain tungsten-carbide powder granularity of preparation is about 30 μ m, shown in the also similar accompanying drawing 2 of pattern.
Embodiment 4: adopting the purple tungsten oxide powder of about 15 μ m is raw material, the about 5Kg raw material of every boat dress.The reduction furnace temperature is risen to 900 ℃, in stove, send into water vapour and hydrogen, the P in the stove is sent in control
H2O/ P
H2Be 0.1.Push the material boat then, reduce about 20h, the descale that sieves after the discharging obtains the coarse grain tungsten powder, and the Fsss granularity is about 10.5 μ m, and shown in the also similar accompanying drawing 1 of pattern, the crystal grain of gained coarse grain tungsten powder is more even, and fine powder is few, and particle crystallization is good.
Gained coarse grain tungsten powder is joined carbon by known method, and mixed carbon comtent is 6.15%, puts into the carbide furnace carbonization then, and carburizing temperature is 1600 ℃, and carbonization 5h rises to 1900 ℃ again, and carbonization 2h, carburizing atmosphere are hydrogen.Treat that but furnace temperature reduces to discharging after the tapping temperature.Handle by embodiment 1 same method then and obtain the coarse grain tungsten-carbide powder.The coarse grain tungsten-carbide powder granularity of preparation is 12.1 μ m, shown in the also similar accompanying drawing 2 of pattern.
Embodiment 5: the oxide yellow tungsten powder that adopts about 23 μ m is a raw material, the about 6.5Kg raw material of every boat dress.The reduction furnace temperature is risen to 950 ℃, in stove, send into water vapour and hydrogen, the P in the stove is sent in control
H2O/ P
H2Be 0.25.Push the material boat then, reduce about 20h, the descale that sieves after the discharging obtains the coarse grain tungsten powder, and the Fsss granularity is about 15 μ m, shown in the also similar accompanying drawing 1 of looks.The crystal grain of gained coarse grain tungsten powder is more even, and fine powder is few, and particle crystallization is good.
Gained coarse grain tungsten powder is carried out carbonization treatment by embodiment 1 same method, can prepare the coarse grain tungsten-carbide powder equally.The coarse grain tungsten-carbide powder granularity of preparation is about 17.5 μ m, shown in the also similar accompanying drawing 2 of pattern.
Embodiment 6: the tungsten dioxide powder that adopts about 15 μ m is a raw material, the about 6Kg raw material of every boat dress.The reduction furnace temperature is risen to 1050 ℃, in stove, send into water vapour and hydrogen, the P in the stove is sent in control
H2O/ P
H2Be 0.7.Push the material boat then, reduce about 20h, the descale that sieves after the discharging obtains the coarse grain tungsten powder, and the Fsss granularity is about 30 μ m, shown in the also similar accompanying drawing 1 of pattern.The crystal grain of gained coarse grain tungsten powder is more even, and fine powder is few, and particle crystallization is good.
Gained coarse grain tungsten powder is joined carbon by known method, and mixed carbon comtent is 6.15%, puts into the carbide furnace carbonization then, and carburizing temperature is 2500 ℃, and carbonization time is 1.5h, and carburizing atmosphere is a hydrogen.Treat that but furnace temperature reduces to discharging after the tapping temperature,, obtain the coarse grain tungsten-carbide powder after sieving the ratio of grinding media to material ball mill crushing of coarse grain tungsten carbide agglomerate by 1: 2.The coarse grain tungsten-carbide powder granularity of preparation is about 34.5 μ m, shown in the also similar accompanying drawing 2 of pattern.
Embodiment 7: adopting the purple tungsten powder mixture of about 90% tungsten dioxide powder and about 10% is raw material, the about 6Kg raw material of every boat dress.The reduction furnace temperature is risen to 1050 ℃, in stove, send into water vapour and hydrogen, the P in the stove is sent in control
H2O/ P
H2Be 0.7.Push the material boat then, reduce about 25h, the descale that sieves after the discharging obtains the coarse grain tungsten powder, and the Fsss granularity is about 31 μ m, shown in the also similar accompanying drawing 1 of pattern.The crystal grain of gained coarse grain tungsten powder is more even, and fine powder is few, and particle crystallization is good.
Gained coarse grain tungsten powder is joined carbon by known method, and mixed carbon comtent is 6.15%, puts into the carbide furnace carbonization then, and carburizing temperature is 2500 ℃, and carbonization time is 1.5h, and carburizing atmosphere is a hydrogen.Treat that but furnace temperature reduces to discharging after the tapping temperature,, obtain the coarse grain tungsten-carbide powder after sieving the ratio of grinding media to material ball mill crushing of coarse grain tungsten carbide agglomerate by 1: 2.The coarse grain tungsten-carbide powder granularity of preparation is about 35.7 μ m, shown in the also similar accompanying drawing 2 of pattern.
Embodiment 8: in the tungsten dioxide powder, mix the tungsten powder that weight ratio is approximately 0.5%, granularity is about 5 μ m, mix the material boat of packing into after 1～2 hour, the about 6Kg raw material of every boat dress.The reduction furnace temperature is risen to 1050 ℃, in stove, send into water vapour and hydrogen, the P in the stove is sent in control
H2O/ P
H2Be 0.25.Push the material boat then, reduce about 10h, the descale that sieves after the discharging obtains the coarse grain tungsten powder, and the Fsss granularity is about 17 μ m, shown in the also similar accompanying drawing 1 of pattern.The crystal grain of gained coarse grain tungsten powder is more even, and fine powder is few, and particle crystallization is good.
Gained coarse grain tungsten powder is joined carbon by known method, and mixed carbon comtent is 6.15%, puts into the carbide furnace carbonization then, and carburizing temperature is 2300 ℃, and carbonization time is 1h, and carburizing atmosphere is a hydrogen.Treat that but furnace temperature reduces to discharging after the tapping temperature,, obtain the coarse grain tungsten-carbide powder after sieving the ratio of grinding media to material ball mill crushing of coarse grain tungsten carbide agglomerate by 1: 1.The coarse grain tungsten-carbide powder granularity of preparation is about 19.3 μ m, shown in the also similar accompanying drawing 2 of pattern.
Embodiment 9: in the tungsten dioxide powder, mix the tungsten powder that weight ratio is approximately 10%, granularity is about 5 μ m, mix the material boat of packing into after 1～2 hour, the about 6Kg raw material of every boat dress.The reduction furnace temperature is risen to 1050 ℃, in stove, send into water vapour and hydrogen, the P in the stove is sent in control
H2O/ P
H2Be 0.25.Push the material boat then, reduce about 3h, the descale that sieves after the discharging obtains the coarse grain tungsten powder, and the Fsss granularity is about 19 μ m, shown in the also similar accompanying drawing 1 of pattern.The crystal grain of gained coarse grain tungsten powder is more even, and a small amount of fine powder is arranged, and particle crystallization is good.
Gained coarse grain tungsten powder is joined carbon by known method, and mixed carbon comtent is 6.15%, puts into the carbide furnace carbonization then, and carburizing temperature is 2500 ℃, and carbonization 1h, carburizing atmosphere are hydrogen.Treat that but furnace temperature reduces to discharging after the tapping temperature,, obtain the coarse grain tungsten-carbide powder after sieving the ratio of grinding media to material ball mill crushing of coarse grain tungsten carbide agglomerate by 1: 2.The coarse grain tungsten-carbide powder granularity of preparation is about 22 μ m, shown in the also similar accompanying drawing 2 of pattern.
Embodiment 10: in the tungsten dioxide powder, mix the tungsten powder that weight ratio is approximately 10%, granularity is about 30 μ m, mix the material boat of packing into after 1～2 hour, the about 7Kg raw material of every boat dress.The reduction furnace temperature is risen to 1100 ℃, in stove, send into water vapour and hydrogen, the P in the stove is sent in control
H2O/ P
H2Be 0.8.Push the material boat then, reduce about 30h, the descale that sieves after the discharging obtains the coarse grain tungsten powder, and the Fsss granularity is about 50 μ m, shown in the also similar accompanying drawing 1 of pattern.The crystal grain of gained coarse grain tungsten powder is more even, and fine powder is few, and particle crystallization is good.
Gained coarse grain tungsten powder is joined carbon by known method, and mixed carbon comtent is 6.15%, puts into the carbide furnace carbonization then, and carburizing temperature is 2000 ℃, and carbonization time is 5h, rises to 2500 ℃ again, and carbonization 5h, carburizing atmosphere are hydrogen.Treat that but furnace temperature reduces to discharging after the tapping temperature,, obtain the coarse grain tungsten-carbide powder after sieving the ratio of grinding media to material ball mill crushing of coarse grain tungsten carbide agglomerate by 1: 4.The coarse grain tungsten-carbide powder granularity of preparation is about 59.2 μ m, shown in the also similar accompanying drawing 2 of pattern.
Embodiment 11: in the tungsten dioxide powder, mix the tungsten powder that weight ratio is approximately 30%, granularity is about 30 μ m, mix the material boat of packing into after 1～2 hour, the about 8Kg raw material of every boat dress.The reduction furnace temperature is risen to 1350 ℃, in stove, send into water vapour and hydrogen, the P in the stove is sent in control
H2O/ P
H2Be 1.64.Push the material boat then, reduce about 50h, the descale that sieves after the discharging obtains the coarse grain tungsten powder, and the Fsss granularity is about 100 μ m, shown in the also similar accompanying drawing 1 of pattern.The crystallization of gained coarse grain tungsten powder is better, and fine powder is few.
Gained coarse grain tungsten powder is joined carbon by known method, and mixed carbon comtent is 6.15%, puts into the carbide furnace carbonization then, and carburizing temperature is 1600 ℃; Carbonization 10h rises to 2000 ℃, carbonization 10h; Rise to 2200 ℃, carbonization 5h rises to 2500 ℃ again; Carbonization 5h, wherein carburizing atmosphere below 2000 ℃ is a hydrogen, carburizing atmosphere is an argon gas more than 2000 ℃.Treat that but furnace temperature reduces to discharging after the tapping temperature,, obtain the coarse grain tungsten-carbide powder after sieving the ratio of grinding media to material ball mill crushing of coarse grain tungsten carbide agglomerate by 1: 4.The coarse grain tungsten-carbide powder granularity of preparation is about 115 μ m, shown in the also similar accompanying drawing 2 of pattern.
Claims (3)
1. the preparation method of an even coarse grain tungsten powder; Comprise successively: with the oxide powder of tungsten, or the mixture of the oxide powder of tungsten and tungsten powder reduces in reduction furnace as raw material, with the processing of sieving of the coarse grain tungsten powder of reduction gained; Promptly get described even coarse grain tungsten powder; It is characterized in that: when reduction, in reduction furnace, send into earlier the steam and the hydrogen of certain flow, the intrinsic standoff ratio P of interior steam of reduction furnace and hydrogen is sent in control
H2O/ P
H2Be 0.1～1.64, push the material boat that powder stock is housed then; The coarse grain tungsten powder particle-size of reduction gained is 10～100 μ m.
2. the preparation method of even coarse grain tungsten powder according to claim 1 is characterized in that: the temperature of reduction reaction is 900～1350 ℃, and the reduction reaction time is 3～50 hours.
3. the preparation method of even coarse grain tungsten powder according to claim 1 is characterized in that: the oxide of described tungsten is any one in yellow tungsten oxide, blue tungsten oxide, purple tungsten oxide, the tungsten dioxide, perhaps two or more combinations.
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