CN117626084A - Composite tungsten electrode material and preparation method thereof - Google Patents
Composite tungsten electrode material and preparation method thereof Download PDFInfo
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- CN117626084A CN117626084A CN202311736163.1A CN202311736163A CN117626084A CN 117626084 A CN117626084 A CN 117626084A CN 202311736163 A CN202311736163 A CN 202311736163A CN 117626084 A CN117626084 A CN 117626084A
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- 239000002131 composite material Substances 0.000 title claims abstract description 92
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 48
- 239000010937 tungsten Substances 0.000 title claims abstract description 48
- 239000007772 electrode material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 25
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 238000000748 compression moulding Methods 0.000 claims abstract description 4
- 239000002041 carbon nanotube Substances 0.000 claims description 26
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 239000011230 binding agent Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 150000002431 hydrogen Chemical class 0.000 claims description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 3
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 claims description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 230000010355 oscillation Effects 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- LLYXJBROWQDVMI-UHFFFAOYSA-N 2-chloro-4-nitrotoluene Chemical class CC1=CC=C([N+]([O-])=O)C=C1Cl LLYXJBROWQDVMI-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims 1
- 230000004927 fusion Effects 0.000 claims 1
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 5
- 150000002910 rare earth metals Chemical class 0.000 abstract description 5
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 abstract 2
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000005491 wire drawing Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
The invention is applicable to the technical field of composite tungsten electrodes, and provides a composite tungsten electrode material and a preparation method thereof, wherein the composite tungsten electrode material comprises the following components: tungsten powder, CNT/Fe3O4 composite material, WC/CNT composite material, silicon carbide and rare earth oxide; the preparation method of the composite tungsten electrode material comprises the following steps: s1, CNT/Fe 3 O 4 Preparing a composite material; s2, preparing a WC/CNT composite material; s3, doping, compression molding and sintering to obtain the composite tungsten electrode. The composite tungsten electrode material and the preparation method thereof provided by the invention have the advantages that the obtained product has good stability and excellent thermionic emission capability, and CNT/Fe is introduced 3 O 4 The composite material, WC/CNT composite material and silicon carbide greatly reduce the content of rare earth in the traditional composite tungsten electrode material and save the cost.
Description
Technical Field
The invention relates to the technical field of composite tungsten electrodes, in particular to a composite tungsten electrode material and a preparation method thereof.
Background
Tungsten has a high melting point, a high electron emission capability, a high elastic modulus and a low vapor pressure, so that the tungsten has been used as a thermionic emission material for a long time, the emission efficiency of a pure metal tungsten electrode is low, and the tungsten wire is sagged and broken due to the fact that the tungsten wire is recrystallized at a high temperature to form an equiaxed grain structure.
Most of the existing composite tungsten electrodes are only doped with rare earth oxides for modification, and the production cost of the composite tungsten electrodes is high due to the high price of rare earth.
Disclosure of Invention
The invention aims to provide a composite tungsten electrode material and a preparation method thereof, which are used for solving the problem that in the prior art, the composite tungsten electrode is mostly only doped with rare earth oxide for modification, and the production cost of the composite tungsten electrode is high due to the high price of rare earth.
In order to achieve the above purpose, the present invention provides the following technical solutions: the first aspect of the invention provides a composite tungsten electrode material, which comprises the following components:
tungsten powder, CNT/Fe 3 O 4 Composites, WC/CNT composites, silicon carbide, rare earth oxides.
Preferably, the rare earth oxide is CeO 2 、ThO 2 、La 2 O 3 、ZrO 2 And Y 2 O 3 One or more of the following.
Preferably, the content of each component in mass percent is as follows:
CNT/Fe 3 O 4 0.6 to 1.2 percent of composite material, 0.9 to 1.8 percent of WC/CNT composite material, 0.3 to 0.6 percent of silicon carbide, 0.5 to 1 percent of rare earth oxide and the balance of tungsten powder.
Preferably, the CNT/Fe 3 O 4 The content ratio of the composite material, WC/CNT composite material and silicon carbide is 2:3:1.
The second aspect of the invention provides a preparation method of the composite tungsten electrode material according to the first aspect of the invention, which comprises the following steps:
S1，CNT/Fe 3 O 4 preparation of the composite material:
weighing CNTs, adding the CNTs into a nitric acid solution with the mass fraction of 10%, condensing and refluxing for 12 hours at the temperature of 90 ℃, taking out the CNTs, drying, dispersing the CNTs in water, ultrasonically oscillating for 1-2 hours, then weighing a proper amount of copperas, adding a proper amount of polyethylene glycol into the dispersion, and enabling the content of the polyethylene glycol to be equalContinuously dispersing ultrasonic for 1-2 h at 50g/L, then adding a proper amount of ammonia water and a trace amount of hydrogen peroxide, wherein the content of the ammonia water is 2.5wt%, transferring into a reaction kettle, keeping the constant temperature of 150-160 ℃, carrying out hydrothermal reaction for 12h, and filtering, washing and drying after the reaction is finished to obtain the CNT/Fe 3 O 4 A composite material;
s2, preparing a WC/CNT composite material:
weighing CNTs, placing the CNTs in a nitric acid solution with the mass fraction of 10%, condensing and refluxing the CNTs for 12 hours at the temperature of 90 ℃, then placing the CNTs in a proper amount of ammonium metatungstate aqueous solution, carrying out ultrasonic oscillation for 1-2 hours, dipping for 24 hours, drying again, then placing a sample in a tubular resistance furnace, introducing nitrogen for 0.5 hour, introducing mixed gas of methane and hydrogen, heating to 750-850 ℃, keeping the constant temperature for 12 hours, and cooling to obtain the WC/CNT composite material;
s3, doping, compression molding and sintering to obtain the composite tungsten electrode:
tungsten powder, CNT/Fe 3 O 4 Mixing the composite material, WC/CNT composite material, silicon carbide and rare earth oxide according to the content to obtain a mixture, adding a binder, pressing and forming, preparing a tungsten rod by adopting a vertical melting sintering method, and preparing the composite tungsten electrode by the processes of wire drawing, straightening, cutting, polishing and the like.
Preferably, the volume ratio of methane to hydrogen in the S2 is 10:1
Preferably, the binder in the step S3 is a mixture of ethanol and glycerol, the volume ratio of the ethanol to the glycerol is 2:3, and the dosage ratio of the binder to the mixture is 10mL/kg.
The invention has at least the following beneficial effects:
the composite tungsten electrode material and the preparation method thereof provided by the invention have the advantages that the obtained product has good stability and excellent thermionic emission capability, and CNT/Fe is introduced 3 O 4 The composite material, WC/CNT composite material and silicon carbide greatly reduce the content of rare earth in the traditional composite tungsten electrode material and save the cost.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The composite tungsten electrode material comprises the following components in percentage by mass:
CNT/Fe 3 O 4 0.6% of composite material, 0.9% of WC/CNT composite material, 0.3% of silicon carbide, 0.5% of rare earth oxide and the balance of tungsten powder.
Wherein the rare earth oxide is CeO 2 。
Wherein CNT/Fe 3 O 4 The content ratio of the composite material, WC/CNT composite material and silicon carbide is 2:3:1.
Example 2
The composite tungsten electrode material comprises the following components in percentage by mass:
CNT/Fe 3 O 4 1.2% of composite material, 1.8% of WC/CNT composite material, 0.6% of silicon carbide, 1% of rare earth oxide and the balance of tungsten powder.
Wherein the rare earth oxide is CeO 2 、ThO 2 、La 2 O 3 、ZrO 2 And Y 2 O 3 And CeO 2 、ThO 2 、La 2 O 3 、ZrO 2 And Y 2 O 3 The content of (3) is the same.
Wherein CNT/Fe 3 O 4 The content ratio of the composite material, WC/CNT composite material and silicon carbide is 2:3:1.
Example 3
The composite tungsten electrode material comprises the following components in percentage by mass:
CNT/Fe 3 O 4 0.8% of composite material, 1.2% of WC/CNT composite material, 0.4% of silicon carbide, 0.7% of rare earth oxide and the balance of tungsten powder.
Wherein the rare earth oxide is ThO 2 。
Wherein CNT/Fe 3 O 4 The content ratio of the composite material, WC/CNT composite material and silicon carbide is 2:3:1.
Example 4
The content of each component of the composite tungsten electrode material in this embodiment is the same as that in embodiment 3, except that the rare earth oxide is La 2 O 3 。
Example 5
The contents of the components of the composite tungsten electrode material in this example are the same as those in example 3, except that the rare earth oxide is ZrO 2 。
Example 6
The content of each component of the composite tungsten electrode material in this embodiment is the same as that in embodiment 3, except that the rare earth oxide is Y 2 O 3 。
Example 7
The content of each component of the composite tungsten electrode material in this embodiment is the same as that in embodiment 3, except that the rare earth oxide is CeO 2 And ThO 2 And CeO 2 And ThO 2 The content of (2) is 1:3.
Example 8
The content of each component of the composite tungsten electrode material in this embodiment is the same as that in embodiment 3, except that the rare earth oxide is La 2 O 3 、ZrO 2 And Y 2 O 3 And La (La) 2 O 3 、ZrO 2 And Y 2 O 3 The content of (2) is 2:2:1.
Example 9
The content of each component of the composite tungsten electrode material in this embodiment is the same as that in embodiment 3, except that the rare earth oxide is CeO 2 、ZrO 2 And Y 2 O 3 And CeO 2 、ZrO 2 And Y 2 O 3 The content of (2) is 1:2:3.
It should be noted that the technical solutions provided in the above embodiments 1 to 9 are some embodiments of the present invention, but not all embodiments, especially the components and content ratios of rare earth oxides.
The preparation method of the composite tungsten electrode material provided in the above embodiments 1 to 9 comprises the following steps:
S1，CNT/Fe 3 O 4 preparation of the composite material:
weighing CNTs, adding the CNTs into a nitric acid solution with the mass fraction of 10%, condensing and refluxing for 12 hours at the temperature of 90 ℃, taking out the CNTs, drying, dispersing the CNTs in water, ultrasonically oscillating for 1-2 hours, then weighing a proper amount of copperas, adding a proper amount of polyethylene glycol into the dispersion, enabling the content of the polyethylene glycol to be 50g/L, continuously dispersing ultrasonic for 1-2 hours, then adding a proper amount of ammonia water and trace hydrogen peroxide, enabling the content of the ammonia water to be 2.5wt%, transferring the ammonia water into a reaction kettle, keeping the constant temperature of 150-160 ℃, performing hydrothermal reaction for 12 hours, and filtering, washing and drying after the reaction is finished to obtain CNTs/Fe 3 O 4 A composite material;
s2, preparing a WC/CNT composite material:
weighing CNTs, placing the CNTs in a nitric acid solution with the mass fraction of 10%, condensing and refluxing the CNTs for 12 hours at the temperature of 90 ℃, then placing the CNTs in a proper amount of ammonium metatungstate aqueous solution, carrying out ultrasonic oscillation for 1-2 hours, dipping for 24 hours, then drying, placing the sample in a tubular resistance furnace, introducing nitrogen for 0.5 hour, introducing mixed gas of methane and hydrogen, wherein the volume ratio of the methane to the hydrogen is 10:1, heating the mixture to 750-850 ℃, keeping the constant temperature for 12 hours, and cooling the mixture to obtain the WC/CNT composite material;
s3, doping, compression molding and sintering to obtain the composite tungsten electrode:
tungsten powder, CNT/Fe 3 O 4 The composite material, WC/CNT composite material, silicon carbide and rare earth oxide are mixed according to the content to obtain a mixture, a binder is added, the binder is a mixture of ethanol and glycerol, the volume ratio of the ethanol to the glycerol is 2:3, the dosage ratio of the binder to the mixture is 10mL/kg, the mixture is pressed and molded, a tungsten rod is prepared by adopting a vertical melting sintering method, and then the composite tungsten electrode is prepared by the processes of wire drawing, straightening, cutting, polishing and the like.
The composite tungsten electrode material and the preparation method thereof provided by the invention have the advantages that the obtained product has good stability, the effective work function at 1300 ℃ is 2.81 eV-3.12 eV, and the product has excellent thermionic emission capabilityBy introducing CNT/Fe 3 O 4 The composite material, WC/CNT composite material and silicon carbide greatly reduce the content of rare earth in the traditional composite tungsten electrode material and save the cost.
While the fundamental and principal features of the invention and advantages of the invention have been shown and described, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. The composite tungsten electrode material is characterized by comprising the following components:
tungsten powder, CNT/Fe 3 O 4 Composites, WC/CNT composites, silicon carbide, rare earth oxides.
2. A composite tungsten electrode material according to claim 1, wherein: the rare earth oxide is CeO 2 、ThO 2 、La 2 O 3 、ZrO 2 And Y 2 O 3 One or more of the following.
3. The composite tungsten electrode material according to claim 1, wherein the contents of the components in mass percent are as follows:
CNT/Fe 3 O 4 composite 0.61.2 percent, WC/CNT composite material 0.9 to 1.8 percent, silicon carbide 0.3 to 0.6 percent, rare earth oxide 0.5 to 1 percent, and the balance being tungsten powder.
4. A composite tungsten electrode material according to claim 3, wherein said CNT/Fe is 3 O 4 The content ratio of the composite material, WC/CNT composite material and silicon carbide is 2:3:1.
5. A method of producing a composite tungsten electrode material according to any one of claims 1 to 4, comprising the steps of:
S1，CNT/Fe 3 O 4 preparation of the composite material:
weighing CNTs, adding the CNTs into a nitric acid solution with the mass fraction of 10%, condensing and refluxing for 12 hours at the temperature of 90 ℃, taking out the CNTs, drying, dispersing the CNTs in water, ultrasonically oscillating for 1-2 hours, then weighing a proper amount of copperas, adding a proper amount of polyethylene glycol into the dispersion, enabling the content of the polyethylene glycol to be 50g/L, continuously dispersing ultrasonic for 1-2 hours, then adding a proper amount of ammonia water and trace hydrogen peroxide, enabling the content of the ammonia water to be 2.5wt%, transferring the ammonia water into a reaction kettle, keeping the constant temperature of 150-160 ℃, performing hydrothermal reaction for 12 hours, and filtering, washing and drying after the reaction is finished to obtain CNTs/Fe 3 O 4 A composite material;
s2, preparing a WC/CNT composite material:
weighing CNTs, placing the CNTs in a nitric acid solution with the mass fraction of 10%, condensing and refluxing the CNTs for 12 hours at the temperature of 90 ℃, then placing the CNTs in a proper amount of ammonium metatungstate aqueous solution, carrying out ultrasonic oscillation for 1-2 hours, dipping for 24 hours, drying again, then placing a sample in a tubular resistance furnace, introducing nitrogen for 0.5 hour, introducing mixed gas of methane and hydrogen, heating to 750-850 ℃, keeping the constant temperature for 12 hours, and cooling to obtain the WC/CNT composite material;
s3, doping, compression molding and sintering to obtain the composite tungsten electrode:
tungsten powder, CNT/Fe 3 O 4 Mixing the composite material, WC/CNT composite material, silicon carbide and rare earth oxide according to the content to obtain a mixtureAdding binder, press forming, preparing tungsten rod by vertical fusion sintering, drawing, straightening, cutting off and polishing to obtain the final product.
6. The method of manufacturing according to claim 5, wherein: and the volume ratio of methane to hydrogen in the S2 is 10:1.
7. The method of manufacturing according to claim 5, wherein: the binder in the step S3 is a mixture of ethanol and glycerol, the volume ratio of the ethanol to the glycerol is 2:3, and the dosage ratio of the binder to the mixture is 10mL/kg.
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| CN104630532A (en) * | 2015-02-10 | 2015-05-20 | 中南大学 | Preparation method of carbide/rare-earth oxide composite reinforced fine-grain tungsten material |
| CN106602088A (en) * | 2016-12-07 | 2017-04-26 | 浙江工业大学 | Nano sheet-like ammonium metatungstate, CNT supported nano sheet-like tungsten oxide palladium-loaded composite material and application thereof |
| CN107604186A (en) * | 2017-09-15 | 2018-01-19 | 江西理工大学 | A kind of composite rare-earth oxide strengthens tungsten base high-specific-gravity alloy composite and preparation method thereof |
| US20220325380A1 (en) * | 2019-08-12 | 2022-10-13 | Henan University Of Science And Technology | Tungsten-base alloy material and preparation method therefor |
| CN115341125A (en) * | 2022-08-12 | 2022-11-15 | 广州市华司特合金制品有限公司 | Tungsten alloy medical shielding plate and preparation method thereof |
| CN117004857A (en) * | 2023-08-15 | 2023-11-07 | 中南大学 | High-strength and high-toughness tungsten alloy and preparation method thereof |
-
2023
- 2023-12-18 CN CN202311736163.1A patent/CN117626084A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62149841A (en) * | 1985-12-24 | 1987-07-03 | Toshiba Corp | Tungsten material |
| WO2015054974A1 (en) * | 2013-10-16 | 2015-04-23 | 苏州汉瀚储能科技有限公司 | Tungsten-based material super battery and supercapacitor |
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| US20220325380A1 (en) * | 2019-08-12 | 2022-10-13 | Henan University Of Science And Technology | Tungsten-base alloy material and preparation method therefor |
| CN115341125A (en) * | 2022-08-12 | 2022-11-15 | 广州市华司特合金制品有限公司 | Tungsten alloy medical shielding plate and preparation method thereof |
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