CN110722172A - Production method of high-pressure billet strength tungsten powder with wide particle size distribution - Google Patents
Production method of high-pressure billet strength tungsten powder with wide particle size distribution Download PDFInfo
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- CN110722172A CN110722172A CN201911062852.2A CN201911062852A CN110722172A CN 110722172 A CN110722172 A CN 110722172A CN 201911062852 A CN201911062852 A CN 201911062852A CN 110722172 A CN110722172 A CN 110722172A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
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Abstract
The invention discloses a production method of high-pressure billet strength tungsten powder with wide particle size distribution, which comprises the following steps: (1) placing ammonium paratungstate in a calcining furnace for calcining to obtain WO3In an amount of 5-25%, WO2.9In an amount of 60-75%, WO2.72The content of blue tungsten is 10-30% of phase component; (2) and (3) feeding the blue tungsten into a reduction furnace for reduction to obtain the tungsten powder with wide particle size distribution and high green compact strength. In the invention, because of the fixed content of tungsten oxide and the adoption of the inconsistent reduction principle, the particle size distribution of the generated tungsten powder is wider, the reaction temperature is controlled in the reduction stage, the particle size distribution width span value of the tungsten powder reaches more than 2.5, the formability is good, and the green strength can reach 2.5-3.5 Mpa.
Description
Technical Field
The invention belongs to the technical field of powder metallurgy, and particularly relates to a production method of high-pressure billet strength tungsten powder with wide particle size distribution.
Background
The refractory material metal tungsten has the characteristics of high melting point, large elastic modulus, good wear resistance and the like, and is widely applied to the fields of high temperature resistance, radiation resistance, wear resistance and the like. The metal tungsten powder is an important raw material for powder metallurgy, and the particle size distribution control requirements of the tungsten powder are not completely the same according to the requirements of different products.
The large product like a tungsten crucible is mainly dependent on higher high green strength for improving the density of a sintered blank, but the particle size distribution of common tungsten powder is narrower, and the green strength is improved by improving the pressing pressure due to the large elastic modulus and poor formability of the tungsten powder, so that cracks and delamination are easy to generate. And reasonable particle size distribution or tungsten powder with wider particle size can realize higher green strength by filling small particles in gaps of large particles.
The traditional method mainly comprises the steps of realizing high-pressure blank strength by powder preparation, grading tungsten powder by using a multistage screen, mixing 3-5 tungsten powders with narrow particle size distribution according to the requirement of a sintered product, and adopting the technical scheme disclosed by CN 103817342B, wherein blue tungsten is reduced at 850-950 ℃, tungsten powders with different particle sizes are obtained by screening, the screened tungsten powders are mixed according to a certain particle size ratio, and the green blank strength is controlled to be 1.8-2.4 MPa. The method is simple to operate, but has complex procedures and low cost advantage.
The technical scheme disclosed by CN 103240421A is that ammonium paratungstate and purple tungsten oxide are used as raw materials and are mixed according to a certain proportion, after uniform mixing, the mixture is placed in a hydrogen reduction furnace to be reduced to obtain high-pressure blank strength tungsten powder, and the blank strength can reach 3.0-5.0 MPa. The technical scheme has the defects that the process of mixing ammonium paratungstate and purple tungsten oxide is added, the process is complex, and the cost advantage is low. The technical scheme disclosed in CN 101318223B is similar to that of CN 103240421A, and the mixture of ammonium paratungstate and ammonium metatungstate in a fixed proportion is subjected to primary reduction to obtain 2.8-4.0 MPa high-pressure green tungsten powder.
The technical scheme disclosed by CN 1730208A adopts ammonium paratungstate to directly reduce and produce tungsten powder with high green compact strength of 2.0-3.6 MPa. The method has the defects that ammonium paratungstate is used as a raw material, and the risk of product stability is high in industrial production.
The compaction strength of the tungsten powder for high compaction is mainly related to the particle size distribution and the morphology of the tungsten powder. Most of the prior art focuses on how to develop a reasonable tungsten powder particle size distribution, that is, the green strength can be higher than 1.8MPa under the condition that the proportion of coarse particles, medium particles and fine particles is appropriate.
The research on the preparation of blue tungsten and tungsten powder from ammonium tungstate, which is reported in the university of south-central industry and national science and technology fruit net, adopts ammonium paratungstate as a raw material, and the raw material is calcined to generate tungsten oxide (WO)3、WO2.9) And then, performing hydrogen reduction treatment on the tungsten oxide to generate tungsten powder, wherein the tungsten powder has complete particle development and concentrated particle size, but the strength value of a pressed compact is only 1.3-2.0 Mpa. In the prior art, most of tungsten powder obtained by reduction of yellow tungsten, blue tungsten and purple tungsten is concentrated in particle size distribution and good in particle uniformity, and the span value of powder particles is generally 1.0-1.8.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a production method of high-pressure billet strength tungsten powder with wide particle size distribution.
The invention also aims to provide the high-pressure billet strength tungsten powder with wide grain size distribution.
The invention prepares tungsten oxide with specific phase components by calcining ammonium paratungstate with a specific calcining process, wherein the tungsten oxide comprises three phases of yellow tungsten phase, blue tungsten phase and purple tungsten phase which are stored together according to a certain proportion, and the tungsten oxide multiphase components are utilized to obtain high-pressure blank tungsten powder in a specific reduction process, the span value of the tungsten powder is more than 2.5, and the blank strength is 2.5-3.5 MPa.
Ammonium paratungstate is used as a raw material, the Fsss particle size is about 30-50 mu m, and the bulk ratio is about 1.8-2.5 g/cm3. The ammonium paratungstate is generated into tungsten oxide by strictly controlling a calcination process, wherein the phase components of the tungsten oxide are mainly WO3、WO2.9、WO2.72The reaction process is as follows:
loss of water from Ammonium Paratungstate (APT):
(NH4)10(H2W12O42)·4H2O→(NH4)10(H2W12O42)+4H2O
ammonium Paratungstate (APT) -metatungstate (AMT):
(NH4)10(H2W12O42)→(NH4)6H4(H2W12O42)+4NH3
ammonium Metatungstate (AMT) -Ammonium Tungsten Bronze (ATB):
(NH4)6H4(H2W12O42)+4NH3→(NH4)212WO3+3.6NH3+5.6H2O+0.4NO
aminotungsten bronze (ATB) -tungsten trioxide (WO)3)：
(NH4)212WO3→12WO3+2NH3+H2
Tungsten Trioxide (TYO) -blue Tungsten (TBO):
WO3+0.1H2→WO2.9+0.1H2O
blue Tungsten (TBO) -purple Tungsten (TVO):
WO2.9+0.18H2→WO2.72+0.18H2O
ammonia Tungsten Bronze (ATB), tungsten trioxide (WO)3) The difference in reaction rates between blue Tungsten (TBO) and purple Tungsten (TVO) in the converter is tungsten trioxide (WO)3) Blue Tungsten (TBO) and purple Tungsten (TVO). According to the process temperature of the front four bands of the converter of 650-800 ℃, the temperature of the last band is +/-25 ℃ higher than that of the last band, the phase component of the tungsten oxide can be obtained, WO3In an amount of 5-25%, WO2.9In an amount of 60-75%, WO2.72The content of (A) is 10-30%.
Tungsten oxide with specific phase components is subjected to hydrogen reduction treatment to generate high-pressure blank strength tungsten powder with wide particle size distribution, and the reduction process is as follows.
WO3+0.1H2→WO2.9+0.1H2O
WO2.9++0.18H2→WO2.72+0.18H2O
WO2.72+0.72H2→2WO2+0.72H2O
WO2.72+2H2→W+2H2O
WO2+2H2→W+2H2O
Due to the difference of phase compositions, the nucleation speed and the volatilization degree of the particles are different under certain reduction conditions.
Under the same partial pressure of water, WO3、WO2.9、WO2.72The temperature at which the next reduction is carried out varies, for example, the higher the O content, the lower the reduction temperature. In the actual reduction process, the reduction temperature and the water partial pressure in the same area are the same, so that the inconsistent characteristic of the three-phase tungsten oxide reduction is particularly remarkable; nucleation of tungsten powder with WO2(OH)2The vapor deposition time is greatly prolonged, the granularity of the tungsten powder is widened, wherein the content of a yellow tungsten phase influences the proportion of coarse-particle tungsten powder, the content of a blue tungsten phase influences the proportion of medium-particle tungsten powder, and the content of a purple tungsten phase influences the proportion of fine-particle tungsten powder. In the phase composition range, the particle size distribution width span value of the prepared tungsten powder reaches more than 2.5, the proportion of coarse powder and medium powder is reasonable, the formability is good, and the green strength can reach 2.5-3.5 Mpa.
The specific technical scheme of the invention is as follows:
a production method of tungsten powder with wide particle size distribution comprises the following steps:
(1) placing ammonium paratungstate in a calciner for calcination to obtain blue tungsten, wherein the calcination temperature of the last temperature zone of the calciner is 5-25 ℃ lower than that of the penultimate temperature zone;
(2) and (3) feeding the blue tungsten into a reduction furnace for reduction to obtain the tungsten powder with wide particle size distribution and high green compact strength.
In a preferred embodiment of the invention, the reduction temperature of the first-stage temperature zone of the reduction furnace is 700-900 ℃, and the reduction temperature of the second-stage temperature zone is 80-100 ℃ higher than the reduction temperature of the first-stage temperature zone.
In a preferred embodiment of the invention, the blue tungstenThe phase components are as follows: WO3In an amount of 5-25%, WO2.9In an amount of 60-75%, WO2.72The content of (A) is 10-30%.
The other technical scheme of the invention is as follows:
the wide-granularity distribution tungsten powder is prepared by using ammonium paratungstate as a raw material, calcining the raw material in a calcining furnace to form blue tungsten, and reducing the blue tungsten by a reducing furnace, wherein the calcining temperature of the last temperature zone of the calcining furnace is 5-25 ℃ lower than that of the penultimate temperature zone.
In a preferred embodiment of the invention, the reduction temperature of the first-stage temperature zone of the reduction furnace is 700-900 ℃, and the reduction temperature of the second-stage temperature zone is 80-100 ℃ higher than the reduction temperature of the first-stage temperature zone.
In a preferred embodiment of the present invention, the phase composition of the blue tungsten is specifically: WO3In an amount of 5-25%, WO2.9In an amount of 60-75%, WO2.72The content of (A) is 10-30%.
The invention has the beneficial effects that:
1. the invention adopts ammonium paratungstate as a raw material, and generates tungsten oxide by a specific and strictly controlled calcination process, wherein the phase components of the tungsten oxide mainly comprise WO3、WO2.9And WO2.72Then, the tungsten oxide containing different phase components is subjected to hydrogen reduction treatment to generate high-pressure blank strength tungsten powder with wide particle size distribution.
2. The tungsten powder generated by the inconsistent reduction of tungsten oxide phase components has wider particle size distribution, the reaction temperature, the boat loading flow and the hydrogen flow are properly controlled in the reduction stage, so that the particle size distribution width of the tungsten powder can reach more than 2.5, the formability is good, and the green strength can reach 2.0-3.5 Mpa.
Detailed Description
The technical solution of the present invention is further illustrated and described by the following detailed description.
Example 1
(1) Placing ammonium paratungstate (mainly comprising complete-crystal square crystals, and less developed arc crystals) in a calciner, and calcining in five temperature zones to obtain blue tungsten; the five temperature zones are sequentially divided into a first temperature zone, a second temperature zone, a third temperature zone, a fourth temperature zone, a fifth temperature zone, a sixth temperature zone, a fifth temperature zone, a;
the specific parameters of the ammonium paratungstate are as follows: the grain size of the Fsss is 30-40 μm; the bulk density is 1.6-2.1 g/cm3(ii) a Screening parameters: 1% or less of +70 meshes, 0-4.0% of-70 +100 meshes, 55-5% of-100 +200 meshes, 15-30% of-200 +325 meshes and 15% or less of-325 meshes; the water content is less than or equal to 1 percent;
the specific parameters of the obtained blue tungsten are as follows: the particle size of the Fsss is 12-18 mu m; the bulk density is 2.1-2.7 g/cm3(ii) a Screening parameters: 100 meshes is less than or equal to 1 percent, 100+200 meshes is more than or equal to 30 percent, 200+325 meshes is more than or equal to 35 percent, 325 meshes is less than or equal to 30 percent; phase composition: WO315-25%, WO2.9In an amount of 65 to 75%, WO2.72The content of (A) is 10-25%;
(2) feeding the blue tungsten into a reducing furnace to be reduced in three temperature areas, wherein the three temperature areas are sequentially divided into a first reducing temperature area, a second reducing temperature area and a third reducing temperature area, the reducing temperatures are 740-750 ℃, 850-860 ℃ and 850-860 ℃, and the tungsten powder (1.5 mu m tungsten powder) with wide particle size distribution and high green compact strength is obtained;
the flow of the reducing furnace is 38-42 m3H, the pushing speed is 8-11 min, and the boat loading amount is 0.4-0.6 kg per boat;
the laser particle size distribution of the 1.5-micron tungsten powder is as follows: d10 (1.0-1.2 μm), D50 (2.7-2.9 μm), and D90 (6.5-7.0 μm); the particle size distribution width of the 1.5 mu m tungsten powder is more than 2.7, and the green compact strength can reach 2.0-3.0 MPa.
Example 2
(1) Placing ammonium paratungstate (mainly comprising complete-crystal square crystals, and less developed arc crystals) in a calciner, and calcining in five temperature zones to obtain blue tungsten; the five temperature zones are sequentially divided into a first temperature zone, a second temperature zone, a third temperature zone, a fourth temperature zone, a fifth temperature zone, a sixth temperature zone, a fifth temperature zone;
the specific parameters of the ammonium paratungstate are as follows: the grain size of the Fsss is 30-40 μm; the bulk density is 1.6-2.1 g/cm3(ii) a Screening parameters: 1% or less of +70 meshes, 0-4.0% of-70 +100 meshes, 55-75% of-100 +200 meshes, 15-30% of-200 +325 meshes and 15% or less of-325 meshes; the water content is less than or equal to 1 percent;
the specific parameters of the obtained blue tungsten are as follows: the particle size of the Fsss is 12-18 mu m; the bulk density is 2.1-2.7 g/cm3(ii) a Screening parameters: 100 meshes is less than or equal to 1 percent, 100+200 meshes is more than or equal to 30 percent, 200+325 meshes is more than or equal to 35 percent, 325 meshes is less than or equal to 30 percent; phase composition: WO3The content of (A) is 15-30%, WO2.9In an amount of 65-75%, WO2.72The content of (A) is 10-15%;
(2) feeding the blue tungsten into a reducing furnace to be reduced in three temperature areas, wherein the three temperature areas are sequentially divided into a first reducing temperature area, a second reducing temperature area and a third reducing temperature area, the reducing temperatures are 790-810 ℃, 895-910 ℃ and 950-960 ℃, and the tungsten powder (5.0 mu m tungsten powder) with wide particle size distribution and high green compact strength is obtained;
the flow of the reducing furnace is 18-23 m3H, the pushing speed is 13-16 min, and the boat loading amount is 0.9-1.1 kg per boat;
the laser particle size distribution of the 5.0 mu m tungsten powder is as follows: d10 (4.0-4.5 μm), D50 (7.9-10.0 μm), and D90 (20.0-25.0 μm); the particle size distribution width of the 5.0 mu m tungsten powder is more than 2.5, and the green compact strength can reach 2.6-3.5 MPa.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (6)
1. A production method of tungsten powder with wide particle size distribution is characterized in that: the method comprises the following steps:
(1) placing ammonium paratungstate in a calciner for calcination to obtain blue tungsten, wherein the calcination temperature of the last temperature zone of the calciner is 5-25 ℃ lower than that of the penultimate temperature zone;
(2) and (3) feeding the blue tungsten into a reduction furnace for reduction to obtain the tungsten powder with wide particle size distribution and high green compact strength.
2. The method of claim 1, wherein: the reduction temperature of the first-stage temperature zone of the reduction furnace is 700-900 ℃, and the reduction temperature of the second-stage temperature zone is 80-100 ℃ higher than that of the first-stage temperature zone.
3. The method of claim 1 or 2, wherein: the phase components of the blue tungsten are as follows: WO3In an amount of 5-25%, WO2.9In an amount of 60-75%, WO2.72The content of (A) is 10-30%.
4. A tungsten powder with wide particle size distribution is characterized in that: the method is characterized in that ammonium paratungstate is used as a raw material and is placed in a calcining furnace to be calcined to form blue tungsten, and then the blue tungsten is reduced by the reducing furnace to prepare the magnesium tungstate, wherein the calcining temperature of the last temperature zone of the calcining furnace is 5-25 ℃ lower than that of the penultimate temperature zone.
5. The wide particle size distribution tungsten powder of claim 4, wherein: the reduction temperature of the first-stage temperature zone of the reduction furnace is 700-900 ℃, and the reduction temperature of the second-stage temperature zone is 80-100 ℃ higher than that of the first-stage temperature zone.
6. The wide particle size distribution tungsten powder according to claim 4 or 5, wherein: the phase components of the blue tungsten are as follows: WO3In an amount of 5-25%, WO2.9In an amount of 60-75%, WO2.72The content of (A) is 10-30%.
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| CN114472913A (en) * | 2022-02-14 | 2022-05-13 | 崇义章源钨业股份有限公司 | Preparation method of high-pressure billet strength tungsten powder |
| CN115464144A (en) * | 2022-09-13 | 2022-12-13 | 长沙升华微电子材料有限公司 | Preparation method of heat sink material injection molding slurry |
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| CN115464144A (en) * | 2022-09-13 | 2022-12-13 | 长沙升华微电子材料有限公司 | Preparation method of heat sink material injection molding slurry |
| CN115464144B (en) * | 2022-09-13 | 2024-01-09 | 长沙升华微电子材料有限公司 | Preparation method of injection molding slurry of heat sink material |
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