CN109226748B - Preparation method of composite tungsten electrode material - Google Patents
Preparation method of composite tungsten electrode material Download PDFInfo
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- CN109226748B CN109226748B CN201810927265.4A CN201810927265A CN109226748B CN 109226748 B CN109226748 B CN 109226748B CN 201810927265 A CN201810927265 A CN 201810927265A CN 109226748 B CN109226748 B CN 109226748B
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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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
- 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
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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
- 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
- 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
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
Abstract
A preparation method of composite tungsten electrode material, including the following steps, oxide selection, prereduction, hydrogen reduction, high-energy mixing, shaping, medium frequency induction sintering, the preparation method of composite tungsten electrode material of the invention, adopt mono-crystalline ammonium paratungstate to prepare blue tungsten oxide of the specific phase composition through the interval reduction, blue tungsten oxide reduction produces the spheroidal tungsten powder, mix with cerium oxide, one or more than one kind of submicron grade oxides such as lanthanum oxide, yttrium oxide, zirconia, etc. high-energy powder mixer of the specific structure high-efficiently, isostatic pressing shaping, low-temperature long time medium frequency induction solid phase sintering, the second phase crystalline grain of the tungsten bar got is fine and even, segregation-free, rare earth element has high retention rate, the processability is good; the yield is more than 87%, and the processing cost is reduced by more than 20%. The tungsten rod is subjected to pressure processing and machining by adopting the conventional technology, the yield is high, and the obtained composite tungsten electrode material has the advantages of low arc starting voltage, good arc stability, low burning loss rate, long service life and environmental friendliness.
Description
Technical Field
The invention relates to a tungsten metallurgy technology, in particular to a preparation method of a composite tungsten electrode material.
Background
Tungsten has the characteristics of high melting point, good high-temperature strength, strong thermionic emission capability and the like, and cerium oxide (CeO) with high electron work function and low melting point is added2) Lanthanum oxide (L a)2O3) Yttrium oxide (Y)2O3) Zirconium oxide (ZrO)2) The tungsten-based material of (2) finds optimal application in thermionic emission materials. Is widely applied to inert gas shielded welding,Plasma welding, cutting, hot spraying, electric vacuum and other fields. The emergence and development of the argon arc welding technology drive the development of the welding technology, and the argon arc welding technology is not separated from the construction of large structural components such as skyscrapers, large-span bridges, pressure pipeline containers, ships and the like. The electrode material has the requirements of reliability and stability, and also has the requirements of material saving, low cost and no pollution.
As is known, the composite tungsten electrode material prepared by the traditional powder metallurgy method is prepared by adding nitrate into tungsten oxide, wherein the tungsten-thorium electrode material which has the best reaction in the market has lower electron work function and high emission performance, but thorium oxide in the tungsten material has serious radioactivity and causes serious harm to human bodies; secondly, most of the materials used in the market are tungsten-cerium electrode materials, and the preparation method is a method disclosed in Chinese patent application CN85100184A and is disclosed in WO3The method avoids the harm of radioactivity, and the size and uniformity of rare earth particles of the produced tungsten-cerium electrode material are considerable, but NO is difficult to eliminate2The harm of the gas to the environment and the human body is solved; in addition, in the process of preparing tungsten powder by reducing tungsten oxide doped with rare earth nitrate, a large amount of acid gas can be generated when nitrate is converted into rare earth oxide, the corrosion to hydrogen pipelines and the like of reduction equipment is serious, and the acid gas can also cause harm to human bodies and is not beneficial to industrial production; some companies use solid-solid mixing, which can eliminate the pollution to the environment, but the method can not eliminate aggregates in the powder, the dispersion degree of the rare earth oxide in the matrix is not good, the rare earth particles are distributed unevenly after mixing, and the prepared rare earth tungsten-based functional material has poor burning loss and arcing performance and can not meet the use performance; in addition, the suspension crystallization method disclosed in the Chinese patent application CN1042675A is used for producing the rare earth tungsten-based functional material, the rare earth particles of the electrode material produced by the method are uniformly distributed, and NO is solved2The production process needs 8 working procedures from material preparation, evaporative crystallization to sintering, the evaporative crystallization process is complex, the production efficiency is extremely low, and the method is not beneficial to modernization and high efficiencyAnd (4) a production mode.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a preparation method of a composite tungsten electrode material, which not only solves the environmental hazard caused in the preparation process of the composite tungsten electrode material, but also has the advantages of fine and uniform second-phase particles, low processing cost, and greatly improved processing performance, pressing performance and sintering performance.
The preparation method of the composite tungsten electrode material comprises the following steps:
A. selecting oxides with submicron-grade spherical or irregular shape as additives, wherein the content of main components is more than or equal to 99.9 percent, the Fisher size (FSSS) is 0.50-1.5 mu m, the particle size distribution D (50) is less than or equal to 1.2 mu m, and D (100) is less than or equal to 4.0 mu m, and the oxides are cerium oxide (CeO)2) Lanthanum oxide (L a)2O3) Yttrium oxide (Y)2O3) Zirconium oxide (ZrO)2) Any one or combination of several of them;
B. pre-reducing, namely selecting single crystal ammonium paratungstate meeting APT-0 brand in GB/T10116-2007, adopting a four-zone temperature fifteen-tube reducing furnace, filling the single crystal ammonium paratungstate into a temperature-resistant alloy boat, wherein the material layer thickness is 3 cm-5 cm, and the temperature setting from a feeding hole is as follows in sequence: 320-340 ℃, 360-380 ℃, 400-420 ℃, 440-460 ℃ and hydrogen flow of 0.40m3/h~0.60m3H, boat pushing speed of 15 min/boat, Fisher's particle size of 8-12 μm, WO2.9Blue tungsten oxide with the phase component accounting for 80-90 percent;
C. reducing the obtained blue tungsten oxide by using a twelve-point temperature control reduction furnace with four-zone temperature areas, wherein the reduction temperature is 630-980 ℃, and the hydrogen flow is 20m3/h～30m3The hydrogen dew point is less than or equal to minus 60 ℃, the periodic boat pushing speed is 10min to 20min, and the boat loading amount is 700g to 1000g, so as to prepare the tungsten powder with the Fisher particle size of 1.20 mu m to 2.2 mu m;
D. high-energy mixing, adopting high-energy powder mixer, designing according to product composition, adding one or more than one oxide, adding various oxidesThe content of the powder is 0.10-4.0%, the total content is 1.0% -8.0%, the powder in the step C and the powder in the step A are sequentially fed into a vertical inverted cone high-energy powder mixer, the rotating speed of a coulter for lifting and updating the powder is 20 r/min-40 r/min, the rotating speed of a fly cutter at the lower side for depolymerization, scattering and mixing is 3000 r/min-4000 r/min, and the powder is efficiently mixed for 120 min-240 min under the protection of nitrogen and water cooling of a jacket to obtain the Fisher granularity (FSSS) of 1.0 mu m-2.0 mu m and the loose packing density of 2.0g/cm3~4.0g/cm3The homogeneous powder body of (a);
E. molding, namely filling the composite tungsten powder obtained in the step D with the single weight of 1250 +/-10 g into an elastic die sleeve with the diameter of 20 +/-0.2 mm, and pressing into a mold by using a cold isostatic press, wherein the highest pressing pressure is 160-200 MPa, so that a tungsten billet with the size of phi (17-18) mm × 500mm is obtained;
F. intermediate frequency induction sintering, the tungsten bar obtained in the step E is filled into a tungsten crucible of an intermediate frequency induction furnace, the dew point is less than or equal to minus 60 ℃, and the flow is 2.0m3/h~10m3Sintering under the protection of hydrogen for h, wherein the sintering system is three stages, the temperature is increased to 1100-1300 ℃ from the normal temperature in the first stage for 6-8 h, and the temperature is kept for 2-3 h; in the second stage, the temperature is raised from (1100-1300) DEG C to (1500-1600) DEG C for 4-6 h, and the temperature is kept for 4-6 h; in the third stage, the temperature is increased from 1500-1600 ℃ to 1900-2000 ℃ for 4-6 h, the temperature is kept for 6-10 h, the heating is stopped, the jacket is cooled to below 200 ℃ by water cooling, and the material is discharged; the section of the produced tungsten rod is crystallized finely and uniformly, the retention amount of the added oxide is more than 95 percent, the density is more than 98 percent of the theoretical density, and the grain size is more than or equal to 10000 per mm2。
The preparation method of the composite tungsten electrode material adopts single crystal ammonium paratungstate to prepare blue tungsten oxide with specific phase components through intermittent reduction, the blue tungsten oxide is reduced to generate sphere-like tungsten powder, the sphere-like tungsten powder is efficiently mixed with one or more than one submicron-grade oxides such as cerium oxide, lanthanum oxide, yttrium oxide, zirconium oxide and the like in a high-energy powder mixer with a specific structure, isostatic pressing is carried out, low-temperature long-time medium-frequency induction solid phase sintering is carried out, second-phase crystal grains of the obtained tungsten rod are fine and uniform, segregation is avoided, the retention rate of rare earth elements is high, and the processing performance is good; the yield is more than 87%, and the processing cost is reduced by more than 20%. The tungsten rod is subjected to pressure processing and machining by adopting the conventional technology, the yield is high, and the obtained composite tungsten electrode material has the advantages of low arc starting voltage, good arc stability, low burning loss rate, long service life and environmental friendliness.
Detailed Description
A preparation method of a composite tungsten electrode material comprises the following steps:
A. selecting oxides with submicron-grade spherical or irregular shape as additives, wherein the content of main components is more than or equal to 99.9 percent, the Fisher size (FSSS) is 0.50-1.5 mu m, the particle size distribution D (50) is less than or equal to 1.2 mu m, and D (100) is less than or equal to 4.0 mu m, and the oxides are cerium oxide (CeO)2) Lanthanum oxide (L a)2O3) Yttrium oxide (Y)2O3) Zirconium oxide (ZrO)2) Any one or combination of several of them;
B. pre-reducing, namely selecting single crystal ammonium paratungstate meeting APT-0 brand in GB/T10116-2007, adopting a four-zone temperature fifteen-tube reducing furnace, filling the single crystal ammonium paratungstate into a temperature-resistant alloy boat, wherein the material layer thickness is 3 cm-5 cm, and the temperature setting from a feeding hole is as follows in sequence: 320-340 ℃, 360-380 ℃, 400-420 ℃, 440-460 ℃ and hydrogen flow of 0.40m3/h~0.60m3H, boat pushing speed of 15 min/boat, Fisher's particle size of 8-12 μm, WO2.9Blue tungsten oxide with the phase component accounting for 80-90 percent;
C. reducing the obtained blue tungsten oxide by using a twelve-point temperature control reduction furnace with four-zone temperature areas, wherein the reduction temperature is 630-980 ℃, and the hydrogen flow is 20m3/h～30m3The hydrogen dew point is less than or equal to minus 60 ℃, the periodic boat pushing speed is 10min to 20min, and the boat loading amount is 700g to 1000g, so as to prepare the tungsten powder with the Fisher particle size of 1.20 mu m to 2.2 mu m;
D. high-energy mixing, namely adopting a high-energy powder mixer, designing according to product components, adding one or more oxides, wherein the content of each added oxide is 0.10-4.0%, the total content is 1.0% -8.0%, sequentially feeding the powder of the step C and the powder of the step A into the vertical inverted cone high-energy powder mixer, the rotating speed of a coulter for lifting and updating the powder is 20 r/min-40 r/min, the rotating speed of a fly cutter at the lower side for depolymerization, scattering and mixing is 3000 r/min-4000 r/min, and under the protection of nitrogen and water cooling of a jacket, high-energy mixing is carried outThe mixture is mixed for 120-240 min to obtain the Fischer-Tropsch particle size (FSSS) of 1.0-2.0 μm and the apparent density of 2.0g/cm3~4.0g/cm3The homogeneous powder body of (a);
E. molding, namely filling the composite tungsten powder obtained in the step D with the single weight of 1250 +/-10 g into an elastic die sleeve with the diameter of 20 +/-0.2 mm, and pressing into a mold by using a cold isostatic press, wherein the highest pressing pressure is 160-200 MPa, so that a tungsten billet with the size of phi (17-18) mm × 500mm is obtained;
F. intermediate frequency induction sintering, the tungsten bar obtained in the step E is filled into a tungsten crucible of an intermediate frequency induction furnace, the dew point is less than or equal to minus 60 ℃, and the flow is 2.0m3/h~10m3Sintering under the protection of hydrogen for h, wherein the sintering system is three stages, the temperature is increased to 1100-1300 ℃ from the normal temperature in the first stage for 6-8 h, and the temperature is kept for 2-3 h; in the second stage, the temperature is raised from (1100-1300) DEG C to (1500-1600) DEG C for 4-6 h, and the temperature is kept for 4-6 h; in the third stage, the temperature is increased from 1500-1600 ℃ to 1900-2000 ℃ for 4-6 h, the temperature is kept for 6-10 h, the heating is stopped, the jacket is cooled to below 200 ℃ by water cooling, and the material is discharged; the section of the produced tungsten rod is crystallized finely and uniformly, the retention amount of the added oxide is more than 95 percent, the density is more than 98 percent of the theoretical density, and the grain size is more than or equal to 10000 per mm2。
Claims (1)
1. A preparation method of a composite tungsten electrode material is characterized by comprising the following steps: it comprises the following steps:
A. selecting oxides, selecting the oxides with submicron-grade spherical or irregular shape as additives, wherein the content of main components is more than or equal to 99.9 percent, the Fisher particle size is 0.50-1.5 mu m, the particle size distribution D50 is less than or equal to 1.2 mu m, and D100 is less than or equal to 4.0 mu m, and the oxides are cerium oxide (CeO)2) Lanthanum oxide (L a)2O3) Yttrium oxide (Y)2O3) Zirconium oxide (ZrO)2) Any one or combination of several of them;
B. pre-reducing, namely selecting single crystal ammonium paratungstate meeting APT-0 brand in GB/T10116-2007, adopting a four-zone temperature fifteen-tube reducing furnace, filling the single crystal ammonium paratungstate into a temperature-resistant alloy boat, wherein the material layer thickness is 3 cm-5 cm, and the temperature setting from a feeding hole is as follows in sequence: 320-340 ℃, 360-380 ℃ and 400 DEG C440-460 ℃ at 420 ℃, and the hydrogen flow is 0.40m3/h~0.60m3H, boat pushing speed of 15 min/boat, Fisher's particle size of 8-12 μm, WO2.9Blue tungsten oxide with the phase component accounting for 80-90 percent;
C. reducing the obtained blue tungsten oxide by using a twelve-point temperature control reduction furnace with four-zone temperature areas, wherein the reduction temperature is 630-980 ℃, and the hydrogen flow is 20m3/h～30m3The hydrogen dew point is less than or equal to minus 60 ℃, the periodic boat pushing speed is 10min to 20min, and the boat loading amount is 700g to 1000g, so as to prepare the tungsten powder with the Fisher particle size of 1.20 mu m to 2.2 mu m;
D. high-energy mixing, adopting a high-energy powder mixer, designing according to product components, adding one or more than one oxide in the step A, wherein the content of each added oxide is 0.10-4.0%, the total content is 1.0% -8.0%, sequentially feeding the powder in the step C and the powder in the step A into a vertical inverted cone high-energy powder mixer, the rotating speed of a colter for lifting and updating the powder is 20 r/min-40 r/min, the rotating speed of a fly cutter at the lower side for depolymerization, scattering and mixing is 3000 r/min-4000 r/min, mixing is carried out for 120 min-240 min under the protection of nitrogen and water cooling of a jacket, and the Fisher particle size is 1.0-2.0 mu m, and the apparent density is 2.0g/cm3~4.0g/cm3The homogeneous powder body of (a);
E. molding, namely filling the composite tungsten powder obtained in the step D with the single weight of 1250 +/-10 g into an elastic die sleeve with the diameter of 20 +/-0.2 mm, and pressing into a mold by using a cold isostatic press, wherein the highest pressing pressure is 160-200 MPa, so that a tungsten billet with the size of phi 17-18 mm × 500mm is obtained;
F. intermediate frequency induction sintering, the tungsten blank bar obtained in the step E is put into a tungsten crucible of an intermediate frequency induction furnace, the dew point is less than or equal to minus 60 ℃, and the flow is 2.0m3/h~10m3Sintering under the protection of hydrogen for h, wherein the sintering system is three stages, the temperature is increased to 1100-1300 ℃ from the normal temperature in the first stage, the time is 6-8 h, and the temperature is kept for 2-3 h; in the second stage, the temperature is increased from 1100-1300 ℃ to 1500-1600 ℃, the time is 4-6 h, and the temperature is kept for 4-6 h; and in the third stage, the temperature is increased from 1500-1600 ℃ to 1900-2000 ℃, the time is 4-6 h, the temperature is kept for 6-10 h, the heating is stopped, the jacket is cooled to below 200 ℃ by water cooling, and the material is discharged.
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| CN110045428B (en) * | 2019-03-26 | 2021-01-05 | 中国地质大学（武汉） | Deep sea pressure resistant solid nonpolarized electrode and preparation method thereof |
| CN110788318B (en) * | 2019-10-29 | 2022-08-12 | 安泰天龙（宝鸡）钨钼科技有限公司 | Preparation method of high-density rare earth tungsten electrode |
| CN111041315A (en) * | 2019-11-27 | 2020-04-21 | 洛阳爱科麦钨钼科技股份有限公司 | Quaternary composite rare earth tungsten alloy electrode material and preparation method thereof |
| CN111850331B (en) * | 2020-06-09 | 2022-01-07 | 厦门虹鹭钨钼工业有限公司 | Hydride-doped rare earth tungsten electrode material and preparation method thereof |
| CN113186438B (en) * | 2021-01-20 | 2022-09-13 | 厦门虹鹭钨钼工业有限公司 | Alloy wire and preparation method and application thereof |
| CN115992329B (en) * | 2023-03-22 | 2023-06-06 | 中钨稀有金属新材料(湖南)有限公司 | Tungsten rod blank and application thereof |
| CN117604307B (en) * | 2024-01-24 | 2024-03-26 | 崇义章源钨业股份有限公司 | Rare earth tungsten rod and preparation method thereof |
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| CN1060709C (en) * | 1998-06-25 | 2001-01-17 | 北京工业大学 | Ternary compound rare-earth tungsten electrode material and its preparing process |
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