CN116730343A - Method for preparing tantalum niobium carbide powder under carbon monoxide atmosphere condition - Google Patents
Method for preparing tantalum niobium carbide powder under carbon monoxide atmosphere condition Download PDFInfo
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- CN116730343A CN116730343A CN202310660533.1A CN202310660533A CN116730343A CN 116730343 A CN116730343 A CN 116730343A CN 202310660533 A CN202310660533 A CN 202310660533A CN 116730343 A CN116730343 A CN 116730343A
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- carbon
- boat
- niobium carbide
- tantalum
- tantalum niobium
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- RHDUVDHGVHBHCL-UHFFFAOYSA-N niobium tantalum Chemical compound [Nb].[Ta] RHDUVDHGVHBHCL-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000000843 powder Substances 0.000 title claims abstract description 34
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910002091 carbon monoxide Inorganic materials 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 61
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 61
- 238000006722 reduction reaction Methods 0.000 claims abstract description 22
- 239000006229 carbon black Substances 0.000 claims abstract description 20
- 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 17
- 229910001936 tantalum oxide Inorganic materials 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 229910000484 niobium oxide Inorganic materials 0.000 claims abstract description 16
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000012535 impurity Substances 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 238000000498 ball milling Methods 0.000 claims abstract description 10
- 238000007873 sieving Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000010000 carbonizing Methods 0.000 claims description 3
- 239000004615 ingredient Substances 0.000 claims description 3
- 239000000956 alloy Substances 0.000 abstract description 6
- 229910045601 alloy Inorganic materials 0.000 abstract description 6
- 238000003763 carbonization Methods 0.000 abstract description 4
- 239000007789 gas Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000001514 detection method Methods 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 239000011812 mixed powder Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 229910003468 tantalcarbide Inorganic materials 0.000 description 2
- 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
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 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
- 230000001681 protective effect Effects 0.000 description 1
- 230000000630 rising effect Effects 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a method for preparing tantalum niobium carbide powder under the condition of carbon monoxide atmosphere, which comprises the following steps: (1) batching and loading the materials into a boat; (2) boat feeding and carbonization reduction reaction; (3) taking out the boat for cooling; (4) ball milling and sieving; and (5) detecting the product performance. In a carbon tube furnace, the tantalum oxide, the mixture of the niobium oxide powder and the carbon black realize the combination reaction under the condition of high-temperature carbon monoxide atmosphere to generate the tantalum niobium carbide powder, and the generated tantalum niobium carbide powder has lower content of various impurities and can better meet the application requirements of the hard alloy industry.
Description
Technical Field
The invention relates to a method for preparing tantalum niobium carbide under a protective gas, in particular to a method for preparing tantalum niobium carbide powder under a carbon monoxide atmosphere condition.
Background
Niobium tantalum carbide 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.
At present, tantalum niobium 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 production of tantalum niobium carbide uses hydrogen to protect a high-temperature carbonization furnace and materials in the furnace, has the problems of high danger, easiness in influencing the purity of the hydrogen and higher impurity content in the materials in the use process, and can take away a large amount of heat energy after cold hydrogen enters the furnace from outside, so that the defects of rising electricity consumption and higher energy consumption are caused.
Disclosure of Invention
The invention aims to provide a method for preparing tantalum niobium carbide powder under the condition of carbon monoxide atmosphere so as to solve the problems in the prior art.
The technical scheme adopted for achieving the aim is that the method for preparing the tantalum niobium carbide powder under the condition of carbon monoxide atmosphere comprises the following steps:
(1) Loading ingredients into a boat: loading the tantalum oxide and niobium oxide powder and carbon black mixture into a plurality of carbon boats with the diameter of 110mm and the length of 350mm, wherein the weight of the tantalum oxide and niobium oxide powder and carbon black mixture loaded into each carbon boat is 1.8 kg-2.5 kg;
(2) Feeding into a boat and carbonizing reduction reaction: pushing the carbon boat with the mixture into a carbon tube furnace, and pushing the boat once every 20-30 minutes, wherein oxides and carbon black in the carbon boat perform reduction reaction in the carbon tube furnace under the protection of carbon monoxide gas generated by the reduction reaction, and the reduction reaction time is 20-30 minutes;
(3) And (5) cooling the ship: pushing the carbon boat after the reaction is completed out of the carbon tube furnace, and cooling the materials in the carbon boat to room temperature to obtain tantalum niobium carbide;
(4) Ball milling and sieving: ball milling is carried out on the cooled tantalum niobium carbide, and then 80-mesh sieving is carried out;
(5) And (3) detecting the product performance: and detecting main content and impurity elements of the screened tantalum niobium carbide to obtain tantalum niobium carbide powder.
Further, the working temperature of the carbon tube furnace in the step (2) is 1800-1900 ℃.
Further, the main content detected in the step (5) is as follows: ta, nb, ctotal, cfree and N, O, FSSS, and the detected impurity elements are as follows: si, P, S, al, mn, fe.
Advantageous effects
Compared with the prior art, the invention has the following advantages.
(1) The method for preparing the tantalum niobium carbide powder has stable process technology and easy operation, and the prepared tantalum niobium carbide powder product has the main component content and the impurity contents, so that the application requirements of the hard alloy industry can be better met;
(2) According to the preparation method, the mixture of tantalum oxide, niobium oxide and carbon black is reduced in the carbonization furnace in the protection of carbon monoxide to generate tantalum niobium carbide, so that the production safety is high, the impurity content of the produced product is low, and the energy consumption is low;
(3) The tantalum niobium carbide powder product obtained by the method is applied to additives of powder metallurgy, cutting tools, fine ceramics, chemical vapor deposition, hard wear-resistant alloy cutters, tools, dies and wear-resistant and corrosion-resistant structural parts, so that the toughness of the alloy is improved, and in practical application, the tantalum niobium carbide powder product produced by the method can be reliably applied.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a flow chart of the preparation of tantalum niobium carbide powder products according to the present invention;
FIG. 2 shows the electron microscope test result of the tantalum niobium carbide product produced and prepared in example 1 of the present invention;
fig. 3 shows XRD detection results of tantalum niobium carbide products produced in example 2 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 niobium carbide powder under carbon monoxide atmosphere conditions, as shown in fig. 1, comprising the steps of:
(1) Loading ingredients into a boat: loading the tantalum oxide and niobium oxide powder and carbon black mixture into a plurality of carbon boats with the diameter of 110mm and the length of 350mm, wherein the weight of the tantalum oxide and niobium oxide powder and carbon black mixture loaded into each carbon boat is 1.8 kg-2.5 kg;
(2) Feeding into a boat and carbonizing reduction reaction: pushing the carbon boat with the mixture into a carbon tube furnace, and pushing the boat once every 20-30 minutes, wherein oxides and carbon black in the carbon boat perform reduction reaction in the carbon tube furnace under the protection of carbon monoxide gas generated by the reduction reaction, and the reduction reaction time is 20-30 minutes;
(3) And (5) cooling the ship: pushing the carbon boat after the reaction is completed out of the carbon tube furnace, and cooling the materials in the carbon boat to room temperature to obtain tantalum niobium carbide;
(4) Ball milling and sieving: ball milling is carried out on the cooled tantalum niobium carbide, and then 80-mesh sieving is carried out;
(5) And (3) detecting the product performance: and detecting main content and impurity elements of the screened tantalum niobium carbide to obtain tantalum niobium carbide powder.
The working temperature of the carbon tube furnace in the step (2) is 1800-1900 ℃.
The main content detected in the step (5) is as follows: ta, nb, ctotal, cfree and N, O, FSSS, and the detected impurity elements are as follows: si, P, S, al, mn, fe.
The invention uses the combustible carbon monoxide gas generated by the reaction of the materials 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.
During implementation, the iron pipes and the branch pipes are used for connecting the feeding end and the discharging end of the 8 carbon tube furnaces in series and parallel to form a micro-positive pressure system formed by carbon monoxide gas, the carbon tube furnaces are continuously deflated and shielded from outside air, and the carbon monoxide gas leakage detection device is installed to meet the requirements of safe production and normal production.
Example 1
Mixing 105 kg of tantalum oxide, 13 kg of niobium oxide and 23.9 kg of carbon black, and then loading into a barrel for loading, wherein 1.8 kg-2.5 kg of mixed powder of the tantalum oxide, the niobium oxide and the carbon black is loaded into a carbon boat with the diameter of 110mm and the length of 350mm;
pushing the carbon boat into a carbon tube furnace, wherein the carbon tube furnace is operated at 1800-1900 ℃ once every 30 minutes, and tantalum oxide and carbon black in the carbon boat are subjected to reduction reaction in the carbon tube furnace under the protection of carbon monoxide gas generated by reduction reaction, and the reduction reaction time is 30 minutes;
pushing the carbon boat out of the carbon tube furnace, and cooling the materials in the carbon boat to room temperature to obtain 90:10 tantalum niobium carbide;
90% after cooling: the 10 tantalum niobium carbide is subjected to ball milling and then is sieved by 80 meshes;
detecting the screened tantalum niobium carbide, wherein the main detection content is as follows: ta, nb, ctotal, cfree and N, O, FSSS, and the detected impurity elements are as follows: si, P, S, al, mn, fe, 90: 10.
The production period of the batch is about 2.0 days, and 90: 101.70kg of a 10 tantalum niobium carbide product.
The chemical composition detection results of the tantalum niobium carbide powder product of example 1 are shown in the attached table 1, and the electron microscope detection results of the tantalum niobium carbide powder product prepared by the production of example 1 are shown in fig. 2.
Example 2
Mixing 93.4 kg of tantalum oxide, 25.8 kg of niobium oxide and 25.7 kg of carbon black, and then loading into a barrel for loading, wherein each of the barrels is filled with 1.8 kg-2.5 kg of mixed powder, based on the mixture of tantalum oxide, niobium oxide and carbon black, of which the diameter is 110mm and the length is 350mm;
pushing the carbon boat materials into a carbon tube furnace, wherein the boat pushing is carried out once every 30 minutes, and the working temperature of the carbon tube furnace is 1800-1900 ℃; tantalum oxide, niobium 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, and the reduction reaction time is 30 minutes;
pushing the carbon boat material out of the carbon tube furnace, and cooling the carbon boat material to room temperature to obtain 80:20 tantalum niobium carbide;
for 80% after cooling: ball milling 20 tantalum niobium carbide, and sieving with 80 mesh sieve;
the performance of tantalum niobium carbide after screening is detected, and the main content is detected as follows: ta, nb, ctotal, cfree and N, O, FSSS, and the detected impurity elements are as follows: si, P, S, al, mn, fe, 80:20 tantalum niobium carbide powder product.
The production period of the batch is about 2.0 days, and 104.70kg of tantalum niobium carbide products are produced.
The chemical composition detection results of the tantalum niobium carbide product of example 2 are shown in the attached table 1, and the XRD detection results of the tantalum niobium carbide product prepared by the production of example 2 are shown in fig. 3.
Example 3
70.1 kg of tantalum oxide, 51.7 kg of niobium oxide and 29.2 kg of carbon black are mixed and then fed into a barrel for loading, and 1.8 kg-2.5 kg of mixed powder with the weight of 1.8 kg-2.5 kg of the mixture of tantalum oxide, niobium oxide and carbon black is loaded into a carbon boat, wherein the diameter of the carbon boat is 110mm, and the length of the carbon boat is 350mm;
pushing the carbon boat materials into a carbon tube furnace, wherein the boat pushing is carried out once every 30 minutes, and the working temperature of the carbon tube furnace is 1800-1900 ℃; tantalum oxide, niobium 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, and the reduction reaction time is 30 minutes;
pushing the carbon boat material out of the carbon tube furnace, and cooling the carbon boat material to room temperature to obtain 60:40 tantalum niobium carbide;
for 60 after cooling: ball milling the 40 tantalum niobium carbide, and sieving the 40 tantalum niobium carbide by 80 meshes;
the performance of tantalum niobium carbide after screening is detected, and the main content is detected as follows: ta, nb, ctotal, cfree and N, O, FSSS, and the detected impurity elements are as follows: si, P, S, al, mn, fe, yield 60:40 tantalum niobium carbide powder product.
The production period of the batch is about 2.0 days, and 101.60kg of tantalum niobium carbide products are produced.
The chemical composition detection results of the tantalum carbide powder niobium product of example 3 are shown in the attached table 1.
Table 1 test results for tantalum niobium carbide products prepared in example 1, example 2 and example 3
From the data in Table 1, it is clear that the main component of the tantalum niobium carbide powder product prepared by the method can meet the customer requirements, and the impurity content is better.
Claims (3)
1. A method for preparing tantalum niobium carbide powder under carbon monoxide atmosphere conditions, which is characterized by comprising the following steps:
(1) Loading ingredients into a boat: loading the tantalum oxide and niobium oxide powder and carbon black mixture into a plurality of carbon boats with the diameter of 110mm and the length of 350mm, wherein the weight of the tantalum oxide and niobium oxide powder and carbon black mixture loaded into each carbon boat is 1.8 kg-2.5 kg;
(2) Feeding into a boat and carbonizing reduction reaction: pushing the carbon boat with the mixture into a carbon tube furnace, and pushing the boat once every 20-30 minutes, wherein oxides and carbon black in the carbon boat perform reduction reaction in the carbon tube furnace under the protection of carbon monoxide gas generated by the reduction reaction, and the reduction reaction time is 20-30 minutes;
(3) And (5) cooling the ship: pushing the carbon boat after the reaction is completed out of the carbon tube furnace, and cooling the materials in the carbon boat to room temperature to obtain tantalum niobium carbide;
(4) Ball milling and sieving: ball milling is carried out on the cooled tantalum niobium carbide, and then 80-mesh sieving is carried out;
(5) And (3) detecting the product performance: and detecting main content and impurity elements of the screened tantalum niobium carbide to obtain tantalum niobium carbide powder.
2. The method for preparing tantalum niobium carbide powder according to claim 1, wherein the operating temperature of the carbon tube furnace in the step (2) is 1800 ℃ to 1900 ℃.
3. The method for preparing tantalum niobium carbide powder according to claim 1, wherein the main content of the powder in the step (5) is: ta, nb, ctotal, cfree and N, O, FSSS, and the detected impurity elements are as follows: si, P, S, al, mn, fe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310660533.1A CN116730343A (en) | 2023-06-06 | 2023-06-06 | Method for preparing tantalum niobium carbide powder under carbon monoxide atmosphere condition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310660533.1A CN116730343A (en) | 2023-06-06 | 2023-06-06 | Method for preparing tantalum niobium carbide powder under carbon monoxide atmosphere condition |
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| Publication Number | Publication Date |
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| CN116730343A true CN116730343A (en) | 2023-09-12 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202310660533.1A Pending CN116730343A (en) | 2023-06-06 | 2023-06-06 | Method for preparing tantalum niobium carbide powder under carbon monoxide atmosphere condition |
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| Country | Link |
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| CN (1) | CN116730343A (en) |
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- 2023-06-06 CN CN202310660533.1A patent/CN116730343A/en active Pending
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