CN112846211A - High-compact-strength tungsten powder and preparation method thereof - Google Patents
High-compact-strength tungsten powder and preparation method thereof Download PDFInfo
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 40
- 239000001257 hydrogen Substances 0.000 claims abstract description 29
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 29
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 25
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910001930 tungsten oxide Inorganic materials 0.000 claims abstract description 24
- 230000009467 reduction Effects 0.000 claims description 57
- 239000007789 gas Substances 0.000 claims description 28
- 229910052721 tungsten Inorganic materials 0.000 claims description 24
- 239000010937 tungsten Substances 0.000 claims description 24
- 238000004321 preservation Methods 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 12
- 239000011362 coarse particle Substances 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 abstract description 25
- 239000002994 raw material Substances 0.000 abstract description 15
- 238000009826 distribution Methods 0.000 abstract description 14
- 230000008569 process Effects 0.000 abstract description 9
- 238000006722 reduction reaction Methods 0.000 description 46
- 239000000843 powder Substances 0.000 description 13
- 230000000694 effects Effects 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 150000002431 hydrogen Chemical class 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000011946 reduction process Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000003739 neck Anatomy 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- BPJYAXCTOHRFDQ-UHFFFAOYSA-L tetracopper;2,4,6-trioxido-1,3,5,2,4,6-trioxatriarsinane;diacetate Chemical compound [Cu+2].[Cu+2].[Cu+2].[Cu+2].CC([O-])=O.CC([O-])=O.[O-][As]1O[As]([O-])O[As]([O-])O1.[O-][As]1O[As]([O-])O[As]([O-])O1 BPJYAXCTOHRFDQ-UHFFFAOYSA-L 0.000 description 1
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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
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/20—Refractory metals
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses high-pressure blank strength tungsten powder and a preparation method thereof, wherein the preparation method of the high-pressure blank strength tungsten powder comprises the following steps: and tungsten oxide is supplied to a tubular furnace and reduced in a hydrogen atmosphere so as to obtain high-pressure blank strength tungsten powder, wherein the front end of the tubular furnace is provided with an air inlet, the rear end of the tubular furnace is provided with an air outlet, an air inlet pipe plug is arranged in the tubular furnace close to the air inlet, an air outlet pipe plug is arranged in the tubular furnace close to the air outlet, and the tungsten oxide is paved between the air inlet pipe plug and the air outlet pipe plug. The method can be suitable for various tungsten oxide raw materials, has wide application range, overcomes the limitation of the existing process by the raw materials, and can stably prepare the high-pressure blank strength tungsten powder with the particle size distribution span of more than or equal to 2.0 and the blank strength of 3.0-6.0 MPa.
Description
Technical Field
The invention belongs to the field of powder metallurgy, and particularly relates to high-pressure billet strength tungsten powder and a preparation method thereof.
Background
In recent years, tungsten products are applied to more and more fields, and the market demand is greatly increased. The continuous development and progress of science and technology make the requirements on the properties of raw materials higher and higher. The tungsten powder prepared by the conventional tungsten powder production process has the advantages of regular shape, concentrated particle size distribution, small powder particle size difference and the like, but has the defects of poor formability, low green strength and the like. When preparing pure tungsten products such as large-caliber thin-walled tubes, large-size tungsten sheets, tungsten crucibles and the like, the conventional tungsten powder cannot meet the quality requirement, so that the preparation of the tungsten powder with high green compact strength is particularly important.
At present, most production processes or research on tungsten powder with high green compact strength is carried out around raw materials, which provides higher standards for preparation processes and equipment of tungsten oxide, and meanwhile, the production limitation of tungsten powder is larger, the reduction process depends on the raw materials, and the tungsten powder with high green compact strength can be produced only by carrying out larger adjustment along with the change of the raw materials.
Therefore, the existing method for preparing tungsten powder with high green strength needs to be improved.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. Therefore, the invention aims to provide high-pressure billet strength tungsten powder and a preparation method thereof, the method can be suitable for various tungsten oxide raw materials, has wide application range, overcomes the limitation of the existing process by the raw materials, and can stably prepare the high-pressure billet strength tungsten powder with the particle size distribution span of more than or equal to 2.0 and the green compact strength of 3.0-6.0 MPa.
In one aspect of the invention, a method of preparing a high green strength tungsten powder is provided. According to an embodiment of the present invention, the method of preparing a high green strength tungsten powder includes: tungsten oxide is supplied to a tube furnace to be reduced in hydrogen atmosphere so as to obtain high-pressure blank strength tungsten powder,
the device comprises a tubular furnace, wherein the front end of the tubular furnace is provided with an air inlet, the rear end of the tubular furnace is provided with an air outlet, an air inlet pipe plug is arranged in the tubular furnace close to the air inlet, an air outlet pipe plug is arranged in the tubular furnace close to the air outlet, and tungsten oxide is paved between the air inlet pipe plug and the air outlet pipe plug.
According to the method for preparing the high-green-compact-strength tungsten powder, the gas inlet pipe plug is arranged at a position close to a gas inlet in the tubular furnace, the gas outlet pipe plug is arranged at a position close to a gas outlet, tungsten oxide is laid between the gas inlet pipe plug and the gas outlet pipe plug, and the tungsten oxide is reduced in a hydrogen atmosphere. Compared with the conventional tungsten powder preparation process in the prior art, the hydrogen flows smoothly, water vapor generated by reaction is taken away by the flowing hydrogen, so that the volatilization-deposition effect is relatively weaker and mainly caused by sintering growth, the particle size difference of the upper layer tungsten powder and the lower layer tungsten powder in the tube furnace is small, the product uniformity is good, the powder is in a sphere-like shape, and the green compact strength is low due to poor meshing effect in the green compact process. Therefore, the method can be suitable for various tungsten oxide raw materials, has wide application range, overcomes the limitation of the existing process by the raw materials, and can stably prepare the high-pressure blank strength tungsten powder with the particle size distribution span of more than or equal to 2.0 and the compact strength of 3.0-6.0 MPa.
In addition, the method for preparing the high green strength tungsten powder according to the above embodiment of the present invention may also have the following additional technical features:
in some embodiments of the invention, the tungsten oxide comprises at least one of yellow tungsten, blue tungsten, and purple tungsten.
In some embodiments of the present invention, the tubular furnace includes a first reduction zone, a second reduction zone and a third reduction zone in sequence, and the temperatures of the first reduction zone, the second reduction zone and the third reduction zone are gradually increased.
In some embodiments of the invention, the temperature of the first reduction zone is 600-780 ℃, the heat preservation time is 1-2 h, the temperature of the second reduction zone is 750-900 ℃, the heat preservation time is 1-2 h, the temperature of the third reduction zone is 920-990 ℃, and the heat preservation time is 1-2 h. Therefore, the high-pressure blank strength tungsten powder with the blank strength of 3.0-6.0 MPa can be prepared.
In some embodiments of the present invention, the temperature increase rate of the first reduction zone to the second reduction zone and the second reduction zone to the third reduction zone is 5 to 10 ℃/min respectively and independently. Therefore, the high-pressure blank strength tungsten powder with the blank strength of 3.0-6.0 MPa can be prepared.
In some embodiments of the present invention, the flow rate of the hydrogen supplied through the gas inlet is 250 to 650L/h. Therefore, the high-pressure blank strength tungsten powder with the blank strength of 3.0-6.0 MPa can be prepared.
In some embodiments of the invention, the tungsten oxide is laid on a boat and then is supplied into the tube furnace for reduction, wherein the thickness of the material layer in the boat is 5-12 mm. Therefore, the high-pressure blank strength tungsten powder with the blank strength of 3.0-6.0 MPa can be prepared.
In some embodiments of the invention, further comprising: and (3) sieving the high-pressure blank strength tungsten powder by a 200-mesh sieve to remove coarse particles and mechanical impurities. Therefore, the high-pressure blank strength tungsten powder with the blank strength of 3.0-6.0 MPa can be prepared.
In a second aspect of the invention, the invention provides a high green strength tungsten powder prepared by the method according to the embodiment of the invention. Therefore, the high-pressure blank strength tungsten powder obtained by the method contains more fine powder, the particle size distribution span is more than or equal to 2.0, and the blank strength is 3.0-6.0 MPa, so that a foundation is provided for producing high-performance tungsten products and high-tungsten content alloy products, and the requirements of the market on preparing large-size tungsten sheets and large-diameter thin-walled tubes difficult to form are met.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
fig. 1 is a schematic view of the structure of a tube furnace in a method for preparing high green strength tungsten powder according to an embodiment of the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The following detailed description of embodiments of the invention is intended to be illustrative, and is not to be construed as limiting the invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In one aspect of the invention, a method of preparing a high green strength tungsten powder is provided. According to an embodiment of the present invention, the method for preparing high green strength tungsten powder comprises: tungsten oxide is supplied to a tube furnace to be reduced under hydrogen atmosphere so as to obtain high-pressure blank strength tungsten powder, wherein, referring to figure 1, the front end of the tube furnace 100 is provided with a gas inlet 101, the rear end of the tube furnace 100 is provided with a gas outlet 102, a gas inlet pipe plug 11 is arranged in the tube furnace 100 and close to the gas inlet 101, a gas outlet pipe plug 12 is arranged in the tube furnace 100 and close to the gas outlet 102, tungsten oxide is laid between the gas inlet pipe plug 11 and the gas outlet pipe plug 12, namely, hydrogen enters the tube furnace 100 through the gas inlet 101 and contacts with tungsten oxide laid between the gas inlet pipe plug 11 and the gas outlet pipe plug 12 to carry out reduction reaction, wherein, in the process that the hydrogen flows to the gas outlet 102, the gas inlet pipe plug 11 and the gas outlet pipe plug 12 obstruct the normal circulation of the hydrogen, so that water vapor generated by the reduction reaction can not be smoothly and timely brought out by the hydrogen, which causes the high water content in the tube furnace 100, therefore, the powder particles have obvious growth steps, the crystal growth plane is obvious and is in a smooth polyhedral shape, and the meshing effect is strong in the blank pressing process, so that the high-pressure blank strength tungsten powder with high blank pressing strength is prepared.
According to an embodiment of the present invention, the tungsten oxide includes at least one of yellow tungsten, blue tungsten, and purple tungsten, and the tungsten oxide is spread on a boat 13, and then the boat 13 is supplied into the tube furnace 100 and reduced in a hydrogen atmosphere, wherein a thickness of a material layer in the boat 13 is 5 to 12 mm. The inventor finds that if the thickness of the material layer is too high, the reaction is incomplete, and the product quality is influenced; if the thickness of the material layer is too low, the yield is low and the powder particle size is fine. Specifically, in the hydrogen reduction process, hydrogen enters the inside of the particles and reacts with the inside and the surface of the particles, so that the particle size of the prepared tungsten powder is finer, the requirement on the particle size of the powder can be met by increasing the thickness of a material layer under the same process condition, and meanwhile, the yield is effectively improved. Therefore, the material layer thickness can ensure the optimal reaction rate and yield, and the high-pressure blank strength tungsten powder with the particle size distribution span of more than or equal to 2.0 and the green compact strength of 3.0-6.0 MPa is prepared.
Further, the tube furnace 100 sequentially comprises a plurality of reducing zones, for example, three reducing zones, namely, a first reducing zone, a second reducing zone and a third reducing zone, wherein the temperatures of the first reducing zone, the second reducing zone and the third reducing zone are gradually increased, the temperature of the first reducing zone is 600-780 ℃, the heat preservation time is 1-2 hours, the temperature of the second reducing zone is 750-900 ℃, the heat preservation time is 1-2 hours, the temperature of the third reducing zone is 920-990 ℃, and the heat preservation time is 1-2 hours. The inventor finds that in a reasonable temperature range, if the reduction temperature span is larger, the tungsten powder has wider particle size distribution, which is beneficial to improving the green compact strength of the powder; if the reduction temperature span is smaller, the powder particle size distribution is relatively narrower and the powder green compact strength is lower. Meanwhile, the longer the heat preservation time is, the longer tungsten powder particles are sintered to form sintering necks, which is not beneficial to improving the strength of a pressed compact and reduces the production efficiency, thereby causing high production cost; and if the time is too short, the powder reduction reaction is incomplete, thereby affecting the product quality. Therefore, the reduction temperature and the heat preservation time can ensure the optimal reaction rate and yield, the cost is reduced, and the high-pressure blank strength tungsten powder with the blank strength of 3.0-6.0 MPa is prepared.
Preferably, the temperature rise rates of the first to second reduction zones and the second to third reduction zones are respectively and independently 5 to 10 ℃/min. The inventor finds that if the temperature rise rate is too high, the volatilization-deposition effect is obvious, and the granularity of the tungsten powder is coarser; if the temperature rise rate is too low, the time of the powder in a low-temperature zone is longer, the granularity of the tungsten powder is finer, and the production efficiency is reduced. Further, the flow rate of the hydrogen supplied through the inlet 101 is 250 to 650L/h. The inventor finds that if the hydrogen flow is too high, the moisture generated by the reaction is discharged quickly, the volatilization-deposition effect is weakened, and the tungsten powder has finer granularity; if the hydrogen flow is too low, the water produced by the reaction is slowly discharged, the volatilization-deposition effect is enhanced, and the tungsten powder has coarser granularity. Therefore, the high-pressure blank strength tungsten powder with the particle size distribution span of more than or equal to 2.0 and the green compact strength of 3.0-6.0 MPa can be prepared by adopting the heating rate and the hydrogen flow rate.
Further, the method also comprises the step of screening the high-pressure blank strength tungsten powder obtained by reduction through a 200-mesh screen to remove coarse particles and mechanical impurities, wherein the undersize is the high-pressure blank strength tungsten powder which contains more fine powder, has the particle size distribution span of more than or equal to 2.0 and has the blank strength of 3.0-6.0 MPa.
The inventor finds that the high-pressure blank strength tungsten powder with high green compact strength is prepared by arranging the gas inlet pipe plug at a position close to the gas inlet in the tubular furnace and arranging the gas outlet pipe plug at a position close to the gas outlet, laying tungsten oxide between the gas inlet pipe plug and the gas outlet pipe plug, and reducing the tungsten oxide in a hydrogen atmosphere. Compared with the conventional tungsten powder preparation process in the prior art, the hydrogen flows smoothly, water vapor generated by reaction is taken away by the flowing hydrogen, so that the volatilization-deposition effect is relatively weaker and mainly caused by sintering growth, the particle size difference of the upper layer tungsten powder and the lower layer tungsten powder in the tube furnace is small, the product uniformity is good, the powder is in a sphere-like shape, and the green compact strength is low due to poor meshing effect in the green compact process. Therefore, the method can be suitable for various tungsten oxide raw materials, has wide application range, overcomes the limitation of the existing process by the raw materials, and can stably prepare the high-pressure blank strength tungsten powder with the particle size distribution span of more than or equal to 2.0 and the compact strength of 3.0-6.0 MPa.
In a second aspect of the invention, a high green strength tungsten powder is provided. According to the embodiment of the invention, the high green strength tungsten powder is prepared by the method. Therefore, the high-pressure blank strength tungsten powder obtained by the method contains more fine powder, the particle size distribution span is more than or equal to 2.0, and the blank strength is 3.0-6.0 MPa, so that a foundation is provided for producing high-performance tungsten products and high-tungsten content alloy products, and the requirements of the market on preparing large-size tungsten sheets and large-diameter thin-walled tubes difficult to form are met. It should be noted that the features and advantages described above for the method of preparing high green strength tungsten powder are also applicable to the high green strength tungsten powder, and are not described herein again.
The invention will now be described with reference to specific examples, which are intended to be illustrative only and not to be limiting in any way.
Example 1
The method for preparing the high green strength tungsten powder comprises the following steps:
1. taking yellow tungsten as a raw material, flatly paving the yellow tungsten in a boat, controlling the thickness of a material layer to be 6mm, then supplying the boat to a tubular furnace shown in figure 1 for reduction in a hydrogen atmosphere, controlling the flow of hydrogen supplied through an air inlet to be 300L/h, wherein the tubular furnace comprises three reduction zones (namely a first reduction zone, a second reduction zone and a third reduction zone which are sequentially included), the temperature of the first reduction zone is controlled to be 700 ℃, the heat preservation time is 1h, the temperature of the second reduction zone is controlled to be 820 ℃, the heat preservation time is 1h, the temperature of the third reduction zone is controlled to be 950 ℃, the heat preservation time is 1h, and the heating rates of the first reduction zone to the second reduction zone and the second reduction zone to the third reduction zone are respectively and independently 8 ℃/min;
2. and (3) sieving the reduced high-pressure blank strength tungsten powder with a 200-mesh sieve to remove coarse particles and mechanical impurities.
Example 2
The method for preparing the high green strength tungsten powder comprises the following steps:
1. blue tungsten is taken as a raw material, the blue tungsten is flatly paved in a boat, the thickness of a material layer is controlled to be 8mm, then the boat is supplied to a tubular furnace shown in figure 1 to be reduced under the hydrogen atmosphere, the flow of the hydrogen supplied through an air inlet is controlled to be 400L/h, the tubular furnace comprises three reducing zones (namely a first reducing zone, a second reducing zone and a third reducing zone are sequentially included), the temperature of the first reducing zone is controlled to be 740 ℃, the heat preservation time is 1h, the temperature of the second reducing zone is controlled to be 860 ℃, the heat preservation time is 1h, the temperature of the third reducing zone is controlled to be 970 ℃, the heat preservation time is 1h, and the heating rates of the first reducing zone to the second reducing zone and the second reducing zone to the third reducing zone are respectively and independently 9 ℃/min;
2. and (3) sieving the reduced high-pressure blank strength tungsten powder with a 200-mesh sieve to remove coarse particles and mechanical impurities.
Example 3
The method for preparing the high green strength tungsten powder comprises the following steps:
1. the method comprises the following steps of (1) flatly paving purple tungsten serving as a raw material in a boat, controlling the thickness of a material layer to be 11mm, then supplying the boat to a tubular furnace shown in figure 1 to perform reduction in a hydrogen atmosphere, controlling the flow rate of hydrogen supplied through an air inlet to be 450L/h, controlling the temperature of a first reduction zone to be 760 ℃, the temperature of a second reduction zone to be 2h, the temperature of a second reduction zone to be 880 ℃, the temperature of a third reduction zone to be 2h, controlling the temperature of the third reduction zone to be 990 ℃, and the temperature of the third reduction zone to be 1h, wherein the temperature rising rates of the first reduction zone to the second reduction zone and the second reduction zone to the third reduction zone are respectively and independently 10 ℃/min;
2. and (3) sieving the reduced high-pressure blank strength tungsten powder with a 200-mesh sieve to remove coarse particles and mechanical impurities.
The results of measuring the particle size distribution and green strength of the high-pressure green strength tungsten powder obtained in examples 1 to 3 are shown in Table 1.
TABLE 1
| Particle size distribution particle size | Green compact strength (MPa) | |
| Example 1 | 2.1 | 4.5 |
| Example 2 | 2.05 | 4.0 |
| Example 3 | 2.02 | 3.8 |
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (9)
1. A method of preparing high green strength tungsten powder comprising: tungsten oxide is supplied to a tube furnace to be reduced in hydrogen atmosphere so as to obtain high-pressure blank strength tungsten powder,
the device comprises a tubular furnace, wherein the front end of the tubular furnace is provided with an air inlet, the rear end of the tubular furnace is provided with an air outlet, an air inlet pipe plug is arranged in the tubular furnace close to the air inlet, an air outlet pipe plug is arranged in the tubular furnace close to the air outlet, and tungsten oxide is paved between the air inlet pipe plug and the air outlet pipe plug.
2. The method of claim 1, wherein the tungsten oxide comprises at least one of yellow tungsten, blue tungsten, and purple tungsten.
3. The method according to claim 1, characterized in that the tube furnace comprises a first reduction zone, a second reduction zone and a third reduction zone in sequence, and the temperatures of the first reduction zone, the second reduction zone and the third reduction zone are increased in a gradient manner.
4. The method according to claim 3, wherein the temperature of the first reduction zone is 600 to 780 ℃ and the holding time is 1 to 2 hours,
the temperature of the second reduction zone is 750-900 ℃, the heat preservation time is 1-2 h,
the temperature of the third reduction zone is 920-990 ℃, and the heat preservation time is 1-2 hours.
5. The method according to claim 3 or 4, wherein the temperature increase rate of the first reduction zone to the second reduction zone and the temperature increase rate of the second reduction zone to the third reduction zone are each independently 5 to 10 ℃/min.
6. The method according to claim 1, wherein the flow rate of the hydrogen supplied through the gas inlet is 250 to 650L/h.
7. The method according to claim 1, wherein the tungsten oxide is spread on a boat in which a thickness of a material layer is 5 to 12mm, and then supplied into the tube furnace for reduction.
8. The method of claim 1, further comprising: and (3) sieving the high-pressure blank strength tungsten powder by a 200-mesh sieve to remove coarse particles and mechanical impurities.
9. A high green strength tungsten powder prepared by the method of any one of claims 1 to 8.
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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 |
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| CN114472913B (en) * | 2022-02-14 | 2023-10-03 | 崇义章源钨业股份有限公司 | Preparation method of high-pressure blank strength tungsten powder |
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