CN114107719A - Process for preparing tantalum-tungsten ingot by adopting carbon reduction method - Google Patents
Process for preparing tantalum-tungsten ingot by adopting carbon reduction method Download PDFInfo
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- XGZGDYQRJKMWNM-UHFFFAOYSA-N tantalum tungsten Chemical compound [Ta][W][Ta] XGZGDYQRJKMWNM-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 58
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims abstract description 70
- 229910001936 tantalum oxide Inorganic materials 0.000 claims abstract description 70
- 239000000463 material Substances 0.000 claims abstract description 69
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000006229 carbon black Substances 0.000 claims abstract description 35
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910003468 tantalcarbide Inorganic materials 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 29
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 25
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052751 metal Inorganic materials 0.000 claims abstract description 23
- 239000002184 metal Substances 0.000 claims abstract description 23
- 238000007599 discharging Methods 0.000 claims abstract description 22
- 239000000853 adhesive Substances 0.000 claims abstract description 21
- 230000001070 adhesive effect Effects 0.000 claims abstract description 21
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 18
- 239000010937 tungsten Substances 0.000 claims abstract description 18
- 238000003825 pressing Methods 0.000 claims abstract description 15
- 238000003723 Smelting Methods 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 238000000465 moulding Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- 238000003763 carbonization Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000003801 milling Methods 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 238000005259 measurement Methods 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052715 tantalum Inorganic materials 0.000 abstract description 14
- 230000007797 corrosion Effects 0.000 abstract description 6
- 238000005260 corrosion Methods 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract description 4
- 238000005245 sintering Methods 0.000 abstract description 3
- 238000010000 carbonizing Methods 0.000 abstract description 2
- 238000005070 sampling Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000003889 chemical engineering Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- CSJDCSCTVDEHRN-UHFFFAOYSA-N methane;molecular oxygen Chemical compound C.O=O CSJDCSCTVDEHRN-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
-
- 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
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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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
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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
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
The invention discloses a process for preparing tantalum-tungsten ingots by a carbon reduction method, which comprises the steps of preparing materials, wherein the prepared materials comprise tantalum oxide, carbon black, pure tungsten and a metal adhesive, then adding the carbon black into the tantalum oxide, carbonizing the mixture in a carbon tube furnace to prepare tantalum carbide, adding the tantalum oxide into the tantalum carbide, carrying out mixed material pressing and sintering to prepare tantalum strips, carrying out hydrogenation reaction on the tantalum strips to prepare powder, adding the tungsten and the metal adhesive into the tantalum powder, uniformly mixing, discharging, carrying out layering and molding, calcining the obtained product in a high-temperature furnace to prepare the tantalum-tungsten strips, and carrying out twice 3000-degree electron bombardment furnace smelting on the tantalum-tungsten strips to prepare the tantalum-tungsten 12.5 ingots. The method can prepare the high-purity tantalum tungsten 12.5 ingot, the tantalum tungsten 12.5 ingot has high-temperature strength, excellent corrosion resistance and good ductility, the carbon reduction method is less harmful to the environment, the environment is protected, and the yield is increased.
Description
Technical Field
The invention relates to the technical field of tantalum-tungsten ingot preparation, in particular to a process for preparing tantalum-tungsten ingots by a carbon reduction method.
Background
The tantalum-tungsten ingot is an alloy consisting of a base metal tantalum and an alloying element tungsten, and the tantalum is a rare metal with high melting point and high boiling point, has steel ash color, rich ductility and corrosion resistance, and has good performances such as good processability and weldability, so that the tantalum-tungsten ingot is widely applied to various industries such as electronics, chemical engineering, weapons and the like.
Tungsten is a refractory metal with the highest melting point, has the most important advantages of good high-temperature strength and good corrosion resistance to molten alkali metal and steam, can generate oxide volatilization and liquid-phase oxide only at the temperature of over 1000 ℃, but also has the defects of higher plastic-brittle transition temperature and difficulty in plastic processing at room temperature, and is widely applied to industries such as metallurgy, chemical engineering, electronics, light sources, mechanical industry and the like.
The tantalum-tungsten ingot can be widely applied to the fields of chemical industry, aerospace industry, atomic energy industry and the like, and is mainly used for manufacturing parts of heaters, cooling coils, heat exchangers, reactors, supersonic aircrafts, rocket engines and airship combustion chambers, high-temperature-resistant furnace parts, parts resistant to corrosion of nitric acid, sulfuric acid and hydrochloric acid and the like.
At present, when the method is actually used, the tantalum-tungsten ingots prepared by the existing method have the defects of serious environmental pollution, difficulty in preparing the tantalum-tungsten ingots with high purity and difficulty in improving the yield.
Therefore, it is necessary to invent a process for preparing tantalum-tungsten ingots by carbon reduction method to solve the above problems.
Disclosure of Invention
The invention aims to provide a process for preparing tantalum-tungsten ingots by a carbon reduction method, which comprises the steps of adding carbon black into tantalum oxide, mixing the materials in a carbon tube furnace for carbonization to prepare tantalum carbide, adding the tantalum oxide into the tantalum carbide, mixing, pressing, sintering to prepare tantalum strips, carrying out hydrogenation reaction on the tantalum strips to prepare powder, adding tungsten and a metal adhesive into tantalum powder, uniformly mixing the powder, discharging, pressing and forming the powder, calcining the powder in a high-temperature furnace to prepare the tantalum-tungsten strips, and smelting the tantalum-tungsten strips in an electron bombardment furnace at 3000 ℃ twice to prepare the tantalum-tungsten 12.5 ingots so as to solve the defects in the technology.
In order to achieve the above purpose, the invention provides the following technical scheme: a process for preparing tantalum-tungsten ingots by adopting a carbon reduction method comprises the following specific processing steps:
the method comprises the following steps: preparing materials, wherein the prepared materials comprise tantalum oxide, carbon black, pure tungsten and metal adhesive;
step two: taking 100kg of tantalum oxide, adding 19kg of carbon black into 100kg of tantalum oxide, and then uniformly mixing the tantalum oxide and the carbon black;
step three: then putting the tantalum oxide and carbon black mixed material into a carbon tube furnace for heating, carrying out carbonization reaction on the tantalum oxide and the carbon black in the carbon tube furnace, and then preparing tantalum carbide powder by using a ball mill;
step four: then taking another 100kg of tantalum oxide, adding 51kg of tantalum carbide into the 100kg of tantalum oxide, uniformly mixing the tantalum oxide and the tantalum carbide, mixing the materials, discharging and pressing into strips;
step five: after molding, calcining in a high-temperature furnace and directly heating, wherein the heating is carried out in three steps;
step six: after discharging, putting the material into a hydrogenation reaction furnace, carrying out hydrogenation reaction on the material in the hydrogenation reaction furnace, introducing hydrogen when the temperature of the hydrogenation reaction furnace is raised to a specified temperature, and cooling when the hydrogen is not absorbed any more;
step seven: after discharging, putting the material into a ball mill, milling the material by using the ball mill, filtering the powder, and sieving to obtain 200-mesh carbon reduced tantalum powder;
step eight: taking 100kg of carbon reduced tantalum powder, adding 12.7kg of tungsten powder into 100kg of carbon reduced tantalum powder, adding a metal adhesive and tantalum oxide (adding carbon and oxygen contents according to the measurement of the tantalum powder), then pouring the mixed material into a mixer, mixing for 3-9 hours, and discharging after the materials are uniformly mixed;
step nine: then putting the tantalum-tungsten powder into a press, pressing the tantalum-tungsten powder into a rectangular strip shape by using the press, thereby obtaining the tantalum-tungsten strip;
step ten: then placing the tantalum-tungsten strip into a high-temperature furnace for calcination, setting the infrared temperature in the high-temperature furnace to be 1650-1808 ℃, setting the low temperature to be 426-476 ℃, setting the standard range to be 415-505 ℃, setting the pressure value to be 1.5-1.8 pa, setting the heat preservation time to be 5-8 hours, and then cooling;
step eleven: and smelting the tantalum-tungsten bar box by a 3000-degree electron bombardment furnace for the first time, and smelting by a 3000-degree electron bombardment furnace for the second time to obtain a tantalum-tungsten 12.5 ingot.
Preferably, the temperature of the carbon tube furnace is set to 1800 degrees in step three.
Preferably, in the fifth step, the temperature rise is divided into three steps, wherein the temperature rise in the first step is 1750 ℃, the temperature is preserved for 3 hours and then the temperature rise in the second step is carried out, the temperature rise in the second step is 1850 ℃, the temperature is preserved for 5 hours and then the temperature rise in the third step is carried out, the temperature rise in the third step is carried out to 1950 ℃, and the temperature is preserved until the pressure in the high-temperature furnace is 5pa and then the temperature is reduced.
Preferably, in the fifth step, the designated temperature of the hydrogenation reaction furnace is set to 800 degrees.
In the technical scheme, the invention provides the following technical effects and advantages:
the method comprises the steps of adding carbon black into tantalum oxide, carbonizing the mixed material in a carbon tube furnace to prepare tantalum carbide, adding tantalum oxide into the tantalum carbide, pressing and sintering the mixed material to prepare a tantalum strip, then carrying out hydrogenation reaction on the tantalum strip to prepare powder, adding tungsten and a metal adhesive into the tantalum powder, uniformly mixing the tungsten and the metal adhesive, discharging, pressing and molding the mixture, calcining the mixture in a high-temperature furnace to prepare the tantalum tungsten strip, and smelting the tantalum tungsten strip in an electron bombardment furnace at 3000 ℃ twice to prepare a tantalum tungsten 12.5 ingot.
Drawings
In order to more clearly illustrate the embodiments of the present application or technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments described in the present invention, and other drawings can be obtained by those skilled in the art according to the drawings.
FIG. 1 is an overall production flow diagram of the present invention.
Detailed Description
In order to make the technical solutions of the present invention better understood, those skilled in the art will now describe the present invention in further detail with reference to the accompanying drawings.
Example 1
The invention provides a process for preparing a tantalum-tungsten ingot by adopting a carbon reduction method as shown in figure 1, wherein the used raw materials comprise: tantalum oxide, carbon black, pure tungsten and a metal adhesive, wherein the carbon black is added into the tantalum oxide, the tantalum oxide is carbonized in a carbon tube furnace to prepare tantalum carbide, the tantalum oxide is added into the tantalum carbide, the tantalum carbide is pressed and sintered to prepare a tantalum strip, the tantalum strip is hydrogenated to prepare powder, the tungsten and the metal adhesive are added into tantalum powder and then uniformly mixed, the tantalum powder is discharged and pressed into strips, the strips are pressed and molded after molding, the strips are calcined in a high-temperature furnace to prepare tantalum tungsten strips, and the tantalum tungsten strips are smelted into tantalum tungsten 12.5 ingots by two 3000-degree electron bombardment furnaces.
The specific processing steps are as follows:
the method comprises the following steps: preparing materials, wherein the prepared materials comprise tantalum oxide, carbon black, pure tungsten and metal adhesive;
step two: taking 100kg of tantalum oxide, adding 19kg of carbon black into 100kg of tantalum oxide, and then uniformly mixing the tantalum oxide and the carbon black;
step three: then putting the tantalum oxide and carbon black mixed material into a carbon tube furnace for heating, carrying out carbonization reaction on the tantalum oxide and the carbon black in the carbon tube furnace, and then preparing tantalum carbide powder by using a ball mill;
step four: then taking another 100kg of tantalum oxide, adding 51kg of tantalum carbide into the 100kg of tantalum oxide, uniformly mixing the tantalum oxide and the tantalum carbide, mixing the materials, discharging and pressing into strips;
step five: after molding, calcining in a high-temperature furnace and directly heating, wherein the heating is carried out in three steps;
step six: after discharging, putting the material into a hydrogenation reaction furnace, carrying out hydrogenation reaction on the material in the hydrogenation reaction furnace, introducing hydrogen when the temperature of the hydrogenation reaction furnace is raised to a specified temperature, and cooling when the hydrogen is not absorbed any more;
step seven: after discharging, putting the material into a ball mill, milling the material by using the ball mill, filtering the powder, and sieving to obtain 200-mesh carbon reduced tantalum powder;
step eight: taking 100kg of carbon reduced tantalum powder, adding 12.7kg of tungsten powder into 100kg of carbon reduced tantalum powder, adding a metal adhesive and tantalum oxide (adding carbon and oxygen contents according to the measurement of the tantalum powder), then pouring the mixed material into a mixer, sampling 4 materials after 3 hours of mixing, and discharging after the materials are uniformly mixed;
the results for the sampling tests are as follows:
| C | O | Ta | |
| first sample tantalum tungsten material | 0.194 | 0.578 | 87.68 |
| Second sample tantalum tungsten material | 0.194 | 0.567 | 87.12 |
| Third sample tantalum tungsten material | 0.193 | 0.557 | 87.61 |
| Fourth sample tantalum tungsten material | 0.197 | 0.560 | 87.57 |
Step nine: then putting the tantalum-tungsten powder into a press, pressing the tantalum-tungsten powder into a rectangular strip shape by using the press, thereby obtaining the tantalum-tungsten strip;
step ten: then placing the tantalum-tungsten strip into a high-temperature furnace for calcination, setting the infrared temperature in the high-temperature furnace to 1650 ℃, setting the low temperature to 426 ℃, setting the infrared temperature to 415 ℃ for a standard table, setting the pressure value to 1.8pa in vacuum, preserving the heat for 5 hours, and then cooling;
step eleven: and smelting the tantalum-tungsten bar box by a 3000-degree electron bombardment furnace for the first time, and smelting by a 3000-degree electron bombardment furnace for the second time to obtain a tantalum-tungsten 12.5 ingot.
Further, in the above technical solution, the temperature of the carbon tube furnace in the third step is set to 1800 ℃.
Further, in the technical scheme, in the fifth step, the temperature rise is divided into three steps, the temperature rise in the first step is 1750 ℃, the temperature is preserved for 3 hours, then the temperature rise in the second step is carried out, the temperature rise in the second step is 1850 ℃, the temperature is preserved for 5 hours, then the temperature rise in the third step is carried out, the temperature rise in the third step is 1950 ℃, and the temperature is reduced when the pressure in the high-temperature furnace is preserved to be 5pa in vacuum.
Further, in the above technical solution, in the fifth step, the specified temperature of the hydrogenation reaction furnace is set to 800 ℃.
Example 2
The invention provides a process for preparing a tantalum-tungsten ingot by adopting a carbon reduction method as shown in figure 1, wherein the used raw materials comprise: tantalum oxide, carbon black, pure tungsten and a metal adhesive, wherein the carbon black is added into the tantalum oxide, the tantalum oxide is carbonized in a carbon tube furnace to prepare tantalum carbide, the tantalum oxide is added into the tantalum carbide, the tantalum carbide is pressed and sintered to prepare a tantalum strip, the tantalum strip is hydrogenated to prepare powder, the tungsten and the metal adhesive are added into tantalum powder and then uniformly mixed, the tantalum powder is discharged and pressed into strips, the strips are pressed and molded after molding, the strips are calcined in a high-temperature furnace to prepare tantalum tungsten strips, and the tantalum tungsten strips are smelted into tantalum tungsten 12.5 ingots by two 3000-degree electron bombardment furnaces.
The specific processing steps are as follows:
the method comprises the following steps: preparing materials, wherein the prepared materials comprise tantalum oxide, carbon black, pure tungsten and metal adhesive;
step two: taking 100kg of tantalum oxide, adding 19kg of carbon black into 100kg of tantalum oxide, and then uniformly mixing the tantalum oxide and the carbon black;
step three: then putting the tantalum oxide and carbon black mixed material into a carbon tube furnace for heating, carrying out carbonization reaction on the tantalum oxide and the carbon black in the carbon tube furnace, and then preparing tantalum carbide powder by using a ball mill;
step four: then taking another 100kg of tantalum oxide, adding 51kg of tantalum carbide into the 100kg of tantalum oxide, uniformly mixing the tantalum oxide and the tantalum carbide, mixing the materials, discharging and pressing into strips;
step five: after molding, calcining in a high-temperature furnace and directly heating, wherein the heating is carried out in three steps;
step six: after discharging, putting the material into a hydrogenation reaction furnace, carrying out hydrogenation reaction on the material in the hydrogenation reaction furnace, introducing hydrogen when the temperature of the hydrogenation reaction furnace is raised to a specified temperature, and cooling when the hydrogen is not absorbed any more;
step seven: after discharging, putting the material into a ball mill, milling the material by using the ball mill, filtering the powder, and sieving to obtain 200-mesh carbon reduced tantalum powder;
step eight: 100kg of carbon reduced tantalum powder is taken, 12.7kg of tungsten powder is added into 100kg of carbon reduced tantalum powder, then metal adhesive and tantalum oxide (added according to the carbon-oxygen content measured by the tantalum powder) are added, then the mixture is poured into a mixer, 4 samples are taken after 6 hours of mixing, and the material can be discharged after being uniformly mixed.
The results for the sampling tests are as follows:
| C | O | Ta | |
| first sample tantalum tungsten material | 0.197 | 0.560 | 87.57 |
| Second sample tantalum tungsten material | 0.194 | 0.567 | 87.12 |
| Third sample tantalum tungsten material | 0.193 | 0.557 | 87.61 |
| Fourth sample tantalum tungsten material | 0.194 | 0.578 | 87.68 |
Step nine: then putting the tantalum-tungsten powder into a press, pressing the tantalum-tungsten powder into a rectangular strip shape by using the press, thereby obtaining the tantalum-tungsten strip;
step ten: then placing the tantalum-tungsten strip into a high-temperature furnace for calcination, setting the infrared temperature in the high-temperature furnace to be 1728 ℃, setting the low temperature to be 457 ℃, setting the infrared temperature to be 471 ℃ for a standard table, setting the pressure value to be vacuum 1.5pa, preserving heat for 5 hours, and then cooling;
step eleven: and smelting the tantalum-tungsten bar box by a 3000-degree electron bombardment furnace for the first time, and smelting by a 3000-degree electron bombardment furnace for the second time to obtain a tantalum-tungsten 12.5 ingot.
Further, in the above technical solution, the temperature of the carbon tube furnace in the third step is set to 1800 ℃.
Further, in the technical scheme, in the fifth step, the temperature rise is divided into three steps, the temperature rise in the first step is 1750 ℃, the temperature is preserved for 3 hours, then the temperature rise in the second step is carried out, the temperature rise in the second step is 1850 ℃, the temperature is preserved for 5 hours, then the temperature rise in the third step is carried out, the temperature rise in the third step is 1950 ℃, and the temperature is reduced when the pressure in the high-temperature furnace is preserved to be 5pa in vacuum.
Further, in the above technical solution, in the fifth step, the specified temperature of the hydrogenation reaction furnace is set to 800 ℃.
Example 3
The invention provides a process for preparing a tantalum-tungsten ingot by adopting a carbon reduction method as shown in figure 1, wherein the used raw materials comprise: tantalum oxide, carbon black, pure tungsten and a metal adhesive, wherein the carbon black is added into the tantalum oxide, the tantalum oxide is carbonized in a carbon tube furnace to prepare tantalum carbide, the tantalum oxide is added into the tantalum carbide, the tantalum carbide is pressed and sintered to prepare a tantalum strip, the tantalum strip is hydrogenated to prepare powder, the tungsten and the metal adhesive are added into tantalum powder and then uniformly mixed, the tantalum powder is discharged and pressed into strips, the strips are pressed and molded after molding, the strips are calcined in a high-temperature furnace to prepare tantalum tungsten strips, and the tantalum tungsten strips are smelted into tantalum tungsten 12.5 ingots by two 3000-degree electron bombardment furnaces.
The specific processing steps are as follows:
the method comprises the following steps: preparing materials, wherein the prepared materials comprise tantalum oxide, carbon black, pure tungsten and metal adhesive;
step two: taking 100kg of tantalum oxide, adding 19kg of carbon black into 100kg of tantalum oxide, and then uniformly mixing the tantalum oxide and the carbon black;
step three: then putting the tantalum oxide and carbon black mixed material into a carbon tube furnace for heating, carrying out carbonization reaction on the tantalum oxide and the carbon black in the carbon tube furnace, and then preparing tantalum carbide powder by using a ball mill;
step four: then taking another 100kg of tantalum oxide, adding 51kg of tantalum carbide into the 100kg of tantalum oxide, uniformly mixing the tantalum oxide and the tantalum carbide, mixing the materials, discharging and pressing into strips;
step five: after molding, calcining in a high-temperature furnace and directly heating, wherein the heating is carried out in three steps;
step six: after discharging, putting the material into a hydrogenation reaction furnace, carrying out hydrogenation reaction on the material in the hydrogenation reaction furnace, introducing hydrogen when the temperature of the hydrogenation reaction furnace is raised to a specified temperature, and cooling when the hydrogen is not absorbed any more;
step seven: after discharging, putting the material into a ball mill, milling the material by using the ball mill, filtering the powder, and sieving to obtain 200-mesh carbon reduced tantalum powder;
step eight: taking 100kg of carbon reduced tantalum powder, adding 12.7kg of tungsten powder into 100kg of carbon reduced tantalum powder, adding a metal adhesive and tantalum oxide (adding carbon and oxygen contents according to the measurement of the tantalum powder), then pouring the mixed material into a mixer, sampling 4 materials for 9 hours, and discharging after the materials are uniformly mixed;
the results for the sampling tests are as follows:
| C | O | Ta | |
| first sample tantalum tungsten material | 0.193 | 0.557 | 87.61 |
| Second sample tantalum tungsten material | 0.194 | 0.567 | 87.12 |
| Third sample tantalum tungsten material | 0.194 | 0.578 | 87.68 |
| Fourth sample tantalum tungsten material | 0.197 | 0.560 | 87.57 |
Step nine: then putting the tantalum-tungsten powder into a press, pressing the tantalum-tungsten powder into a rectangular strip shape by using the press, thereby obtaining the tantalum-tungsten strip;
step ten: then placing the tantalum-tungsten strip into a high-temperature furnace for calcination, setting the infrared temperature in the high-temperature furnace to be 1808 ℃, setting the low temperature to be 476 ℃, setting the infrared temperature to be 505 ℃ for a standard table, setting the pressure value to be vacuum 1.5pa, preserving the heat for 8 hours, and then cooling;
step eleven: and smelting the tantalum-tungsten bar box by a 3000-degree electron bombardment furnace for the first time, and smelting by a 3000-degree electron bombardment furnace for the second time to obtain a tantalum-tungsten 12.5 ingot.
Further, in the above technical solution, the temperature of the carbon tube furnace in the third step is set to 1800 ℃.
Further, in the technical scheme, in the fifth step, the temperature rise is divided into three steps, the temperature rise in the first step is 1750 ℃, the temperature is preserved for 3 hours, then the temperature rise in the second step is carried out, the temperature rise in the second step is 1850 ℃, the temperature is preserved for 5 hours, then the temperature rise in the third step is carried out, the temperature rise in the third step is 1950 ℃, and the temperature is reduced when the pressure in the high-temperature furnace is preserved to be 5pa in vacuum.
Further, in the above technical solution, in the fifth step, the specified temperature of the hydrogenation reaction furnace is set to 800 ℃.
Example 4:
the seventh step of examples 1-3 was performed with different stirring times for carbon-reduced tantalum powder, tungsten powder, metal binder and tantalum oxide (the carbon-oxygen content was determined from the tantalum powder), but the results of the data obtained with different stirring times were not substantially changed, and thus the stirring time was within 3-9 hours.
The tantalum tungsten bar burn-out results are as follows: the 10 tantalum-tungsten bars obtained in the above examples 1 to 3 were taken, and the content of C, O, N in the tantalum-tungsten bars was detected, so as to obtain the following data:
| C | O | N | |
| tantalum tungsten bar in example 1 | 0.0055 | 0.290 | 0.031 |
| Tantalum tungsten bar in example 2 | 0.0049 | 0.305 | 0.038 |
| Tantalum tungsten bar in example 3 | 0.0053 | 0.224 | 0.035 |
As can be seen from the above table, in example 3, the raw material mixing ratio is moderate, each parameter in the processing technology is moderate, and the heating condition of the tantalum-tungsten bar is moderate, so that the tantalum-tungsten 12.5 ingot can be obtained, which has the highest purity, higher high-temperature strength, excellent corrosion resistance and good ductility, and is suitable for working environments such as high temperature, high pressure and corrosion resistance, and the carbon reduction method is less harmful to the environment, so that the environment-friendly effect can be achieved, and the yield can be increased.
While certain exemplary embodiments of the present invention have been described above by way of illustration only, it will be apparent to those of ordinary skill in the art that the described embodiments may be modified in various different ways without departing from the spirit and scope of the invention. Accordingly, the drawings and description are illustrative in nature and should not be construed as limiting the scope of the invention.
Claims (4)
1. The process for preparing tantalum-tungsten ingots by a carbon reduction method according to claim 1, which is characterized in that: the specific processing steps are as follows:
the method comprises the following steps: preparing materials, wherein the prepared materials comprise tantalum oxide, carbon black, pure tungsten and metal adhesive;
step two: taking 100kg of tantalum oxide, adding 19kg of carbon black into 100kg of tantalum oxide, and then uniformly mixing the tantalum oxide and the carbon black;
step three: then putting the tantalum oxide and carbon black mixed material into a carbon tube furnace for heating, carrying out carbonization reaction on the tantalum oxide and the carbon black in the carbon tube furnace, and then preparing tantalum carbide powder by using a ball mill;
step four: then taking another 100kg of tantalum oxide, adding 51kg of tantalum carbide into the 100kg of tantalum oxide, uniformly mixing the tantalum oxide and the tantalum carbide, mixing the materials, discharging and pressing into strips;
step five: after molding, calcining in a high-temperature furnace and directly heating, wherein the heating is carried out in three steps;
step six: after discharging, putting the material into a hydrogenation reaction furnace, carrying out hydrogenation reaction on the material in the hydrogenation reaction furnace, introducing hydrogen when the temperature of the hydrogenation reaction furnace is raised to a specified temperature, and cooling when the hydrogen is not absorbed any more;
step seven: after discharging, putting the material into a ball mill, milling the material by using the ball mill, filtering the powder, and sieving to obtain 200-mesh carbon reduced tantalum powder;
step eight: taking 100kg of carbon reduced tantalum powder, adding 12.7kg of tungsten powder into 100kg of carbon reduced tantalum powder, adding a metal adhesive and tantalum oxide (adding carbon and oxygen contents according to the measurement of the tantalum powder), then pouring the mixed material into a mixer, mixing for 3-9 hours, and discharging after the materials are uniformly mixed;
step nine: then putting the tantalum-tungsten powder into a press, pressing the tantalum-tungsten powder into a rectangular strip shape by using the press, thereby obtaining the tantalum-tungsten strip;
step ten: then placing the tantalum-tungsten strip into a high-temperature furnace for calcination, setting the infrared temperature in the high-temperature furnace to be 1650-1808 ℃, setting the low temperature to be 426-476 ℃, setting the standard range to be 415-505 ℃, setting the pressure value to be 1.5-1.8 pa, setting the heat preservation time to be 5-8 hours, and then cooling;
step eleven: and smelting the tantalum-tungsten bar box by a 3000-degree electron bombardment furnace for the first time, and smelting by a 3000-degree electron bombardment furnace for the second time to obtain a tantalum-tungsten 12.5 ingot.
2. The process for preparing tantalum-tungsten ingots by a carbon reduction method according to claim 1, which is characterized in that: the temperature of the carbon tube furnace was set to 1800 degrees in step three.
3. The process for preparing tantalum-tungsten ingots by a carbon reduction method according to claim 1, which is characterized in that: in the fifth step, the temperature rise is divided into three steps, the temperature rise of the first step is 1750 ℃, the second step of temperature rise is carried out after the heat preservation is carried out for 3 hours, the temperature rise of the second step of temperature rise is 1850 ℃, the third step of temperature rise is carried out after the heat preservation is carried out for 5 hours, the temperature rise of the third step of temperature rise is 1950 ℃, and the temperature rise is carried out when the heat preservation is carried out until the pressure in the high-temperature furnace is 5pa in vacuum.
4. The process for preparing tantalum-tungsten ingots by a carbon reduction method according to claim 1, which is characterized in that: in step five, the specified temperature of the hydrogenation reactor was set at 800 degrees.
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| CN118143261B (en) * | 2024-05-09 | 2024-07-05 | 江苏镕耀新材料有限公司 | Method for preparing high-purity tantalum ingot with low loss |
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