CN102557029A - Synthetic method of fibrous nano-tungsten carbide - Google Patents
Synthetic method of fibrous nano-tungsten carbide Download PDFInfo
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- CN102557029A CN102557029A CN2012100002027A CN201210000202A CN102557029A CN 102557029 A CN102557029 A CN 102557029A CN 2012100002027 A CN2012100002027 A CN 2012100002027A CN 201210000202 A CN201210000202 A CN 201210000202A CN 102557029 A CN102557029 A CN 102557029A
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- carbon nanotube
- carbon nano
- tungsten
- nano tube
- tungsten carbide
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Abstract
A synthetic method of fibrous nano-tungsten carbide is characterized by comprising the following steps: (1), a carbon nano tube and tungsten oxide powder are added into an ethanol solution according to the weight ratio of 1 to 3-50, and dispersed through ball milling in a ball grinder, and then evenly mixed; (2), after being filtered, the dispersed solution of the carbon nano tube and the tungsten oxide powder is subjected to filtering and then vacuum drying, the powder dried is put into a high-temperature carbonization furnace, is heated at the temperature of 500 DEG C to 700 DEG C in a hydrogen reducing atmosphere, kept for 2 to 10 hours, heated in the reducing atmosphere at the temperature of more than 1,000 DEG C to 1,500 DEG C, and then in thermal insulation under the protection of argon gas for 3 to 20 hours. According to the invention, the carbon nano tube and the tungsten oxide powder are in reaction so as to form a tungsten carbide layer with the thickness of a plurality of atom layers on the surface of the carbon nano tube, an inner layer still keeps the original fibrous carbon nano tube structure, the diameter can be controlled within a range of 10 to 100 nm, and the prepared nano tungsten carbide not only keeps the high hardness of tungsten carbide, but also keeps the high strength and the high ductility of the carbon nano tube. Therefore, the contradiction that both the strength and the rigidity of hard alloy products can not be achieved at the same time can be overcome.
Description
Technical field
The invention belongs to field of nanometer material technology.
Background technology
Wolfram varbide be make hart metal product main raw material, its particulate size has decisive influence to the hart metal product performance.The preparation of nanometer tungsten carbide becomes the main path that improves the hart metal product obdurability, and wimet is a hard brittle material, exists contradiction between its hardness and the intensity, and hardness height then intensity is on the low side, and intensity height then hardness is on the low side.Comprehensive contradiction between the two, both are effectively combined is directions of people's effort always.Since nanometer tungsten carbide in building-up process, be easy to reunite cause particle grow up and in sintering process grain growth, can't obtain at present less than carbide particle below 100 nanometers and hart metal product with nanometer particle tungsten carbide.
Summary of the invention
The present invention provides a kind of compound method of nanometer tungsten carbide.
The present invention realizes through following technical scheme.
(1) carbon nanotube and oxidation tungsten powder are pressed in the 1:3-50 weight ratio adding ethanolic soln, and Ball milling in ball mill makes carbon nanotube and oxidation tungsten powder uniform mixing.
(2) dispersion soln with carbon nanotube and tungsten powder filters the final vacuum drying, dried powder is put into the high temperature carbonization stove; In hydrogen reducing atmosphere,, be incubated 2-10 hour, Tungsten oxide 99.999 is reduced with 500 ℃-700 ℃ temperature heating; Then in reducing atmosphere, heat more than-1500 ℃ with 1000 ℃; Insulation is 3-20 hour under argon shield, and carbon nanotube top layer atom and tungsten reaction generate wolfram varbide, and internal layer keeps the carbon nanotube original structure.Forming the top layer is the microcosmic matrix material of carbon nanotube for the wolfram varbide internal layer.
Carbon nanotube of the present invention and tungsten are reflected at the carbon nanotube top layer and form several carbide layers to the dozens of atomic layer level thickness; Internal layer still keeps the fibrous of original carbon nanotube structure; Controllable diameter is built in 10-100nm; The nanometer tungsten carbide of its preparation had both kept the high firmness of wolfram varbide, had kept HS, the H.T. of carbon nanotube again, and this microcosmic nano silicon carbide composite tungsten material has solved the contradiction that hart metal product intensity and hardness can not have concurrently fully.
Main application of the present invention is following: be used to make high-strong toughness, the high firmness hart metal product 1..2. the catalyzer as fuel cell substitutes noble metal platinum.3. as the wear-resistant coating of making various materials and equipment.
Embodiment
The present invention will be described further through following examples.
Embodiment 1.
(1) 1 gram carbon nanotube and 6.3 gram oxidation tungsten powders add in the ethanolic soln, and Ball milling is 8 hours in ball mill, makes carbon nanotube and oxidation tungsten powder uniform mixing.
(2) dispersion soln with carbon nanotube and tungsten powder filters the final vacuum drying, dried powder is put into the high temperature carbonization stove; In hydrogen reducing atmosphere with 500 ℃ temperature heat tracing 2 hours; Tungsten oxide 99.999 is reduced to tungsten, then in reducing atmosphere with 1200 ℃ of ℃ of heating, under argon shield, be incubated 3 hours; Carbon nanotube top layer atom and tungsten reaction generate wolfram varbide, and internal layer keeps the carbon nanotube original structure.Forming the top layer is the microcosmic matrix material of carbon nanotube for the wolfram varbide internal layer.
Embodiment 2.
(1) 1 gram carbon nanotube and 50 gram oxidation tungsten powders add in the ethanolic soln, and Ball milling is 6 hours in ball mill, makes carbon nanotube and oxidation tungsten powder uniform mixing.
(2) dispersion soln with carbon nanotube and tungsten powder filters the final vacuum drying, dried powder is put into the high temperature carbonization stove; In hydrogen reducing atmosphere with 700 ℃ temperature heat tracing 10 hours; Tungsten oxide 99.999 is reduced to tungsten, then in reducing atmosphere with 1400 ℃ of heating, under argon shield, be incubated 20 hours; Carbon nanotube top layer atom and tungsten reaction generate wolfram varbide, and internal layer keeps the carbon nanotube original structure.Forming the top layer is the microcosmic matrix material of carbon nanotube for the wolfram varbide internal layer.
Embodiment 3.
(1) 1 gram carbon nanotube and 30 gram oxidation tungsten powders add in the ethanolic soln, and Ball milling is 8 hours in ball mill, makes carbon nanotube and oxidation tungsten powder uniform mixing.
(2) dispersion soln with carbon nanotube and tungsten powder filters the final vacuum drying, dried powder is put into the high temperature carbonization stove; In hydrogen reducing atmosphere with 600 ℃ temperature heat tracing 5 hours; Tungsten oxide 99.999 is reduced to tungsten, then in reducing atmosphere with 1200 ℃ of heating, under argon shield, be incubated 5 hours; Carbon nanotube top layer atom and tungsten reaction generate wolfram varbide, and internal layer keeps the carbon nanotube original structure.Forming the top layer is the microcosmic matrix material of carbon nanotube for the wolfram varbide internal layer.
Embodiment 4.
(1) 1 gram carbon nanotube and 3 gram oxidation tungsten powders add in the ethanolic soln, and Ball milling is 6 hours in ball mill, makes carbon nanotube and oxidation tungsten powder uniform mixing.
(2) dispersion soln with carbon nanotube and tungsten powder filters the final vacuum drying, dried powder is put into the high temperature carbonization stove; In hydrogen reducing atmosphere with 550 ℃ temperature heat tracing 8 hours; Tungsten oxide 99.999 is reduced to tungsten, then in reducing atmosphere with 1500 ℃ of heating, under argon shield, be incubated 3 hours; Carbon nanotube top layer atom and tungsten reaction generate wolfram varbide, and internal layer keeps the carbon nanotube original structure.Forming the top layer is the microcosmic matrix material of carbon nanotube for the wolfram varbide internal layer.
Claims (1)
1. the compound method of a fibrous nano wolfram varbide is characterized in that as follows:
(1) carbon nanotube and oxidation tungsten powder are pressed in the 1:3-50 weight ratio adding ethanolic soln, and Ball milling in ball mill makes carbon nanotube and oxidation tungsten powder uniform mixing;
(2) dispersion soln with carbon nanotube and tungsten powder filters the final vacuum drying, dried powder is put into the high temperature carbonization stove; Temperature with 500 ℃-700 ℃ in hydrogen reducing atmosphere heats; Be incubated 2-10 hour; Then in reducing atmosphere, heat more than-1500 ℃ with 1000 ℃, insulation is 3-20 hour under argon shield.
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| CN2012100002027A CN102557029A (en) | 2012-01-04 | 2012-01-04 | Synthetic method of fibrous nano-tungsten carbide |
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| CN2012100002027A CN102557029A (en) | 2012-01-04 | 2012-01-04 | Synthetic method of fibrous nano-tungsten carbide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105597801A (en) * | 2015-09-23 | 2016-05-25 | 厦门理工学院 | Tungsten carbide/carbon nanotube composite particle and preparation method thereof |
| CN115094432A (en) * | 2022-05-12 | 2022-09-23 | 中国科学院金属研究所 | Preparation method of structure function integrated transition metal carbide/single-walled carbon nanotube composite film |
Citations (3)
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| CN1122768A (en) * | 1995-09-29 | 1996-05-22 | 中国科学院固体物理研究所 | Dimension controllable method for prepn. of Nanometre grade tungsten carbide |
| CN1396112A (en) * | 1995-06-07 | 2003-02-12 | 国际卡比泰克工业公司 | Method for generating tungsten carbide |
| CN101985356A (en) * | 2010-12-10 | 2011-03-16 | 中国科学院上海硅酸盐研究所 | Method for preparing tungsten carbide nano-powder |
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2012
- 2012-01-04 CN CN2012100002027A patent/CN102557029A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1396112A (en) * | 1995-06-07 | 2003-02-12 | 国际卡比泰克工业公司 | Method for generating tungsten carbide |
| CN1122768A (en) * | 1995-09-29 | 1996-05-22 | 中国科学院固体物理研究所 | Dimension controllable method for prepn. of Nanometre grade tungsten carbide |
| CN101985356A (en) * | 2010-12-10 | 2011-03-16 | 中国科学院上海硅酸盐研究所 | Method for preparing tungsten carbide nano-powder |
Non-Patent Citations (2)
| Title |
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| NICOLAS KELLER ET AL.: "A new one-dimensional tungsten carbide nanostructured material", 《MATERIALS LETTERS》, vol. 60, 27 December 2005 (2005-12-27), pages 1774 - 1777 * |
| 张秋和等: "超细碳化钨粉工业生产实践", 《中国钨业》, vol. 24, no. 6, 31 December 2009 (2009-12-31), pages 32 - 33 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105597801A (en) * | 2015-09-23 | 2016-05-25 | 厦门理工学院 | Tungsten carbide/carbon nanotube composite particle and preparation method thereof |
| CN115094432A (en) * | 2022-05-12 | 2022-09-23 | 中国科学院金属研究所 | Preparation method of structure function integrated transition metal carbide/single-walled carbon nanotube composite film |
| CN115094432B (en) * | 2022-05-12 | 2024-03-08 | 中国科学院金属研究所 | Preparation method of transition metal carbide/single-walled carbon nanotube composite film with integrated structure and function |
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Application publication date: 20120711 |