CN116947047A - Preparation method of tantalum carbide powder - Google Patents
Preparation method of tantalum carbide powder Download PDFInfo
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- CN116947047A CN116947047A CN202310646914.4A CN202310646914A CN116947047A CN 116947047 A CN116947047 A CN 116947047A CN 202310646914 A CN202310646914 A CN 202310646914A CN 116947047 A CN116947047 A CN 116947047A
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- carbon
- tantalum carbide
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- powder
- tantalum
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- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229910003468 tantalcarbide Inorganic materials 0.000 title claims abstract description 65
- 239000000843 powder Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 66
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 65
- 239000006229 carbon black Substances 0.000 claims abstract description 21
- 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 21
- 229910001936 tantalum oxide Inorganic materials 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 238000006722 reduction reaction Methods 0.000 claims abstract description 16
- 239000012535 impurity Substances 0.000 claims abstract description 12
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910002091 carbon monoxide Inorganic materials 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000000498 ball milling Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000012216 screening Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 9
- 230000035484 reaction time Effects 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 3
- 239000000956 alloy Substances 0.000 abstract description 8
- 229910045601 alloy Inorganic materials 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 7
- 238000001514 detection method Methods 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000003763 carbonization Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- KAQHZJVQFBJKCK-UHFFFAOYSA-L potassium pyrosulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OS([O-])(=O)=O KAQHZJVQFBJKCK-UHFFFAOYSA-L 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method of tantalum carbide powder, which comprises the following steps: (1) Loading tantalum oxide powder and carbon black powder mixture into a carbon boat; (2) Pushing the carbon boat filled with the mixed materials into a carbon tube furnace, and carrying out reduction reaction on tantalum oxide and carbon black in the carbon boat; (3) pushing the carbon boat out of the carbon tube furnace, and cooling to obtain tantalum carbide; (4) ball milling and screening; and (5) detecting the performance to obtain tantalum carbide powder. In the carbon tube furnace, the invention realizes the combination reaction of the mixture of the tantalum oxide and the carbon black under the condition of high-temperature carbon monoxide atmosphere to generate the tantalum carbide powder, and the tantalum carbide powder has lower content of various impurities, can meet the application requirements of the hard alloy industry, and is simple in operation and easy for industrial production.
Description
Technical Field
The invention belongs to the field of preparation of tantalum and hard alloy thereof, and particularly relates to a preparation method of tantalum carbide powder.
Background
At present, the national standard of tantalum carbide powder products is GB/T20508-2019. Tantalum carbide molecular weight 192.956, light brown metal-like cubic crystal powder, belongs to sodium chloride-like cubic crystal. Is insoluble in water, poorly soluble in inorganic acids, soluble in mixed acids of hydrofluoric acid and nitric acid, and decomposable. Has strong oxidation resistance and is easy to be melted and decomposed by potassium pyrosulfate. The conductivity is large, the resistance is 30 ohms at room temperature, and the superconducting property is shown.
The tantalum carbide is mainly used as an additive for powder metallurgy, cutting tools, fine ceramics, chemical vapor deposition, hard wear-resistant alloy cutters, tools, dies and wear-resistant and corrosion-resistant structural components, and improves the toughness of the alloy. The traditional tantalum carbide production uses hydrogen to protect a high-temperature carbonization furnace and materials in the furnace, the use process is high in danger, the materials are easy to be influenced by the purity of the hydrogen, the impurity content is higher, a large amount of heat energy can be taken away after cold hydrogen enters the furnace from the outside of the furnace, and the power consumption is increased and the energy consumption is higher.
Disclosure of Invention
The invention aims to provide a preparation method of tantalum carbide powder, which aims to solve the problems in the background.
The technical scheme adopted for achieving the purpose is that the preparation method of the tantalum carbide powder comprises the following steps:
(1) Loading tantalum oxide powder and carbon black powder mixture into a carbon boat;
(2) Pushing the carbon boat filled with the mixed materials into a carbon tube furnace with the working temperature of 1800-1900 ℃ for once every 20-30 minutes, so that tantalum oxide and carbon black in the carbon boat undergo a reduction reaction in the carbon tube furnace under the protection of carbon monoxide gas generated by the reduction reaction to generate tantalum carbide;
(3) Pushing the carbon boat out of the carbon tube furnace, and cooling to room temperature to obtain tantalum carbide;
(4) Ball milling the cooled tantalum carbide and screening;
(5) And detecting main content and impurity elements of the screened tantalum carbide to obtain tantalum carbide powder.
Further, the tantalum oxide powder and carbon black powder mixture of each carbon boat is filled in the step (1), the weight of the mixture is 1.8 kg-2.5 kg, the diameter of the carbon boat is 110mm, and the length of the carbon boat is 350mm.
Further, the reduction reaction time in the step (2) is 20 minutes to 30 minutes. 0008 further, the tantalum carbide in the step (4) is subjected to ball milling and then is sieved by a sieve of 80 meshes.
Advantageous effects
Compared with the prior art, the invention has the following advantages.
(1) The preparation method disclosed by the invention has the advantages that the process technology is stable and easy to operate, and the chemical components of the prepared tantalum carbide powder product, whether the main component content or the impurity content, can meet the application requirements of the hard alloy industry;
(2) The invention produces tantalum carbide by reducing a mixture of tantalum oxide and carbon black in a carbonization furnace under carbon monoxide protection, wherein: the mass percent of C is 6.2% +/-0.1%, the mass percent of Ta is 93.8% +/-0.1%, the mass percent of FSSS is 1.0 micrometer+/-0.2 oxygen and the mass percent of impurities is as follows: oxygen is less than or equal to 0.20 percent, the impurity content Si is less than or equal to 0.005 percent, P is less than or equal to 0.005 percent, S is less than or equal to 0.005 percent, mo is less than or equal to 0.01 percent, na is less than or equal to 0.01 percent, fe is less than or equal to 0.01 percent, cf is less than or equal to 0.15 percent, and N is less than or equal to 0.02 percent;
(3) The tantalum carbide powder product prepared by the method is applied to powder metallurgy, cutting tools, fine ceramics, chemical vapor deposition, hard wear-resistant alloy cutters, tools, dies and wear-resistant and corrosion-resistant structural component additives, and can improve the toughness of the alloy; in practical application, the tantalum carbide powder product prepared by the method can be reliably applied.
Drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 is a graph showing the result of electron microscopy of a tantalum carbide powder product prepared in accordance with example 1 of the present invention;
FIG. 2 is a graph showing XRD detection results of tantalum carbide powder products produced and prepared in example 2 of the present invention;
FIG. 3 is a diagram of an apparatus for carrying out the production method of the present invention.
Detailed Description
The invention will now be described in further detail by reference to the drawings and examples.
A method for preparing tantalum carbide powder, comprising the following steps:
(1) Loading tantalum oxide powder and carbon black powder mixture into a carbon boat;
(2) Pushing the carbon boat filled with the mixed materials into a carbon tube furnace with the working temperature of 1800-1900 ℃ for once every 20-30 minutes, so that tantalum oxide and carbon black in the carbon boat undergo a reduction reaction in the carbon tube furnace under the protection of carbon monoxide gas generated by the reduction reaction to generate tantalum carbide;
(3) Pushing the carbon boat out of the carbon tube furnace, and cooling to room temperature to obtain tantalum carbide;
(4) Ball milling the cooled tantalum carbide and screening;
(5) And detecting main content and impurity elements of the screened tantalum carbide to obtain tantalum carbide powder.
And (3) loading 1.8 kg-2.5 kg of the mixture of tantalum oxide powder and carbon black powder of each carbon boat in the step (1), wherein the diameter of the carbon boat is 110mm, and the length of the carbon boat is 350mm. The reduction reaction time in the step (2) is 20-30 minutes.
And (3) ball milling the tantalum carbide in the step (4), and sieving the tantalum carbide through 80 meshes.
The invention uses the combustible reducing gas (carbon monoxide) generated by the reaction of the tantalum oxide powder and the carbon black powder mixture in the carbonization furnace to replace the hydrogen in the traditional process as the medium for isolating the air, thereby achieving the purposes of eliminating the danger of the hydrogen and reducing the use cost of the hydrogen. When the preparation method is implemented, as shown in fig. 3, the feeding end and the discharging end of the 8 carbon tube furnaces are connected in series and parallel by using the iron pipes with the diameters of 50mm and the branch pipes to form a micro-positive pressure system formed by carbon monoxide gas, so that the carbon tube furnaces continuously deflate and shield the outside air, and a carbon monoxide gas leakage detection device is arranged in the iron pipes to meet the requirements of safe production and normal production.
Example 1
Mixing 120 kg of tantalum oxide powder with 22.82 kg of carbon black powder, and loading into a plurality of carbon boats; the weight of the mixture of tantalum oxide powder and carbon black powder in each carbon boat is 1.8 kg-2.5 kg, the diameter of the carbon boat is 110mm, and the length of the carbon boat is 350mm; pushing the carbon boat filled with the mixed materials into a carbon tube furnace, wherein the boat is pushed once every 20 minutes, and the working temperature of the carbon tube furnace is 1800-1900 ℃; tantalum oxide and carbon black in the carbon boat are subjected to reduction reaction in a carbon tube furnace under the protection of carbon monoxide gas generated by the reduction reaction to generate carbonization talks, and the reduction reaction time is 20 minutes; pushing the reacted carbon boat out of the carbon tube furnace, and cooling the carbon boat and materials in the carbon boat to room temperature to obtain tantalum carbide; the cooled tantalum carbide is subjected to ball milling and then is sieved by 80 meshes; the tantalum carbide after screening is detected, and the main content is detected as follows: ctotal, cstream, N, O, FSSS, the detected impurity elements are: si, P, S, al, mn, fe, etc., to obtain tantalum carbide powder products.
The production cycle of the batch is about 24 hours, and 104.70kg of tantalum carbide products are produced. The chemical composition detection results of the tantalum carbide powder product of the example 1 are shown in the attached table 1, and the electron microscope detection results of the tantalum carbide powder product produced and prepared in the example 1 are shown in fig. 1.
Example 2
Mixing 120 kg of tantalum oxide powder with 22.82 kg of carbon black powder, and then feeding into a barrel to fill a plurality of carbon boats; the mixture of tantalum oxide and carbon black contained in each carbon boat is 1.8 kg-2.5 kg by weight, the diameter of the carbon boat is 110mm, and the length of the carbon boat is 350mm; pushing the carbon boat filled with the mixed materials into a carbon tube furnace, wherein the boat is pushed once every 30 minutes, and the working temperature of the carbon tube furnace is 1800-1900 ℃; tantalum oxide and carbon black in the carbon boat are subjected to reduction reaction in a carbon tube furnace under the protection of carbon monoxide gas generated by the reduction reaction to generate tantalum carbide, wherein the reduction reaction time is 30 minutes; pushing the reacted carbon boat out of the carbon tube furnace; cooling the carbon boat material to room temperature to obtain tantalum carbide; ball milling the cooled tantalum carbide and sieving the tantalum carbide through 80 meshes; the tantalum carbide after screening is detected, and the main content is detected as follows: ctotal, cstream, N, O, FSSS, the detected impurity elements are: si, P, S, al, mn, fe, etc., to obtain tantalum carbide powder products.
The production cycle of the batch is about 36 hours, and 104.70kg of tantalum carbide products are produced. The chemical composition detection results of the tantalum carbide powder product of example 2 are shown in the attached table 1, and the electron microscope and XRD detection results of the tantalum carbide powder product produced and obtained in example 2 are shown in fig. 2.
Table 1 test results of tantalum carbide powder products prepared in example 1 and example 2;
from the data in table 1, it can be seen that the main component of the tantalum carbide powder product prepared by the preparation method of the invention can meet the customer requirements, and the impurity content is better.
The preparation method of the invention is that in a carbon tube furnace, the mixture of tantalum oxide powder and carbon black powder is subjected to chemical combination reaction under the condition of high-temperature carbon monoxide atmosphere to generate a tantalum carbide powder product, and the product has lower content of various impurities, can meet the application requirements of the hard alloy industry, and meets the national standard of 'tantalum carbide powder' GB/T20508-2019. The preparation method of the tantalum carbide powder is simple to operate and easy for industrial production.
Claims (4)
1. The preparation method of the tantalum carbide powder is characterized by comprising the following steps:
(1) Loading tantalum oxide powder and carbon black powder mixture into a carbon boat;
(2) Pushing a carbon boat filled with mixed materials into a carbon tube furnace with the working temperature of 1800-1900 ℃ for once every 20-30 minutes, so that tantalum oxide and carbon black in the carbon boat undergo a reduction reaction in the carbon tube furnace under the protection of carbon monoxide gas generated by the reduction reaction to generate tantalum carbide;
(3) Pushing the carbon boat out of the carbon tube furnace, and cooling to room temperature to obtain tantalum carbide;
(4) Ball milling the cooled tantalum carbide and screening;
(5) And detecting main content and impurity elements of the screened tantalum carbide to obtain tantalum carbide powder.
2. The method for preparing tantalum carbide powder according to claim 1, wherein the mixture of tantalum oxide powder and carbon black powder loaded into the carbon boat in the step (1) is 1.8 kg-2.5 kg by weight, the diameter of the carbon boat is 110mm, and the length of the carbon boat is 350mm.
3. The method for preparing tantalum carbide powder according to claim 1, wherein the reduction reaction time in the step (2) is 20 minutes to 30 minutes.
4. The method for preparing tantalum carbide powder according to claim 1, wherein the tantalum carbide powder obtained in the step (4) is subjected to ball milling and then sieving through 80 mesh sieve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310646914.4A CN116947047A (en) | 2023-06-02 | 2023-06-02 | Preparation method of tantalum carbide powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310646914.4A CN116947047A (en) | 2023-06-02 | 2023-06-02 | Preparation method of tantalum carbide powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116947047A true CN116947047A (en) | 2023-10-27 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310646914.4A Pending CN116947047A (en) | 2023-06-02 | 2023-06-02 | Preparation method of tantalum carbide powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116947047A (en) |
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2023
- 2023-06-02 CN CN202310646914.4A patent/CN116947047A/en active Pending
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