CN102887512A - Method for preparing nano-tungsten carbide - Google Patents
Method for preparing nano-tungsten carbide Download PDFInfo
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- CN102887512A CN102887512A CN2012103967154A CN201210396715A CN102887512A CN 102887512 A CN102887512 A CN 102887512A CN 2012103967154 A CN2012103967154 A CN 2012103967154A CN 201210396715 A CN201210396715 A CN 201210396715A CN 102887512 A CN102887512 A CN 102887512A
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Abstract
A method for preparing nano-tungsten carbide is characterized by comprising the steps of: dissolving tungsten into distilled water for ultrasonic processing, then dissolving a carbon source into a tungsten source for ultrasonic processing, controlling the mole ratio of the tungsten source to the carbon source to 1:2-1:5, magnetically stirring to uniformly mix the tungsten source and the carbon source, and then drying a sample, performing ball-milling the sample for 5 to 15h in a ball mill, and finally sintering the sample for 1 to 10min in a microwave way, wherein the tungsten source is ammonium meta-tungstate or tungsten, and the carbon source is glucose or carbon. The method for preparing nano-tungsten carbide, provided by the invention, can quickly and effectively obtain the nano-tungsten carbide with small particle size, and the prepared nano tungsten carbide is small in particle size, high in purity and good in density, so that the method for preparing nano tungsten carbide is suitable for industrially preparing nano-tungsten carbide.
Description
Technical field
The invention belongs to technical field of material.
Background technology
In traditional nanometer tungsten carbide preparation method, such as high-energy ball milling method, high temperature solid-state method all is the preparation method who comparatively commonly uses, the general particle diameter of the wolfram varbide that adopts these methods to prepare very large (reaching micron order), purity is very low, experimental technique is complicated and power consumption is high, has had a strong impact on the intensity of wolfram varbide, the performances such as hardness and catalysis.
Because WC and Pt have a lot of similarities aspect catalysis, make wolfram varbide use very extensive in catalyst field.Therefore, the preparation of this type of small particle size nanometer tungsten carbide also seems very important day by day.
Summary of the invention
The objective of the invention is to propose a kind of preparation method of small particle size nanometer tungsten carbide.
The present invention is achieved by the following technical solutions.
At first, the tungsten source is dissolved in the distilled water, carry out supersound process, again carbon source is dissolved in and carry out supersound process in the tungsten source, the mol ratio of tungsten source and carbon source is 1:2～1:5, and magnetic agitation makes tungsten source and carbon source mixing, then sample is dried, put into ball mill ball milling 5h～15h, carry out at last microwave sintering 1min～10min.
Tungsten of the present invention source is ammonium metawolframate or tungsten.
Carbon source of the present invention is glucose or carbon.
Ball-milling Time is preferably 6h～9h in the ball mill of the present invention.
The microwave sintering time of the present invention is preferably 2min～5min.
The present invention is directed to carbon source glucose or carbon all is fabulous microwave susceptible material, they can the transient absorption microwave, and there is not waste heat in microwave, make wolfram varbide reach the effect of chilling, crystal grain is difficult for growing up, and microwave has good penetrance, makes the almost simultaneously heating of material internal, outside, so the wolfram varbide product even compact degree of microwave sintering is fine.Therefore, the present invention can prepare the nanometer tungsten carbide of small particle size fast and effectively, and the nanometer tungsten carbide particle diameter of preparing is little, and purity is high, and good compactness is applicable to industrial preparation nanometer tungsten carbide.
Description of drawings
Fig. 1 is that tungsten of the present invention source is ammonium metawolframate, and carbon source is the wolfram varbide xrd pattern that glucose is prepared.
Fig. 2 is that tungsten of the present invention source is ammonium metawolframate, and carbon source is the wolfram varbide xrd pattern that carbon is prepared.
Fig. 3 is that tungsten of the present invention source is tungsten, and carbon source is the wolfram varbide xrd pattern that glucose is prepared.
Fig. 4 is that tungsten of the present invention source is tungsten, and carbon source is the wolfram varbide xrd pattern that carbon is prepared.
Embodiment
The present invention will be described further by following examples.
Embodiment 1.
Getting the 31.7g ammonium metawolframate is dissolved in the distilled water, supersound process 5min, after the tungsten source becomes settled solution, getting 9g glucose dissolves in the settled solution, supersound process 5min, again solution magnetic agitation 15min is made that carbon source and tungsten source mix in the solution, solution dried under 80 ° of C vacuum environments put into the ball mill ball milling 12 hours, sample behind the ball milling is put into microwave oven sintering 2min, at last the resulting powder of sintering is adopted SA-3100 type specific surface tester (BET) test, the specific surface area that can get powder is 25.6 (m
2/ g), and adopt D8ADVANCE type (Cu target, the K-α radiation) x ray diffractometer x of German Bruker company that powder is carried out crystal phase analysis, see accompanying drawing 1.
Embodiment 2.
Getting the 31.7g ammonium metawolframate is dissolved in the distilled water, supersound process 5min, after the tungsten source becomes settled solution, getting 0.6g carbon dissolves in the settled solution, supersound process 5min, again solution magnetic agitation 15min is made that carbon source and tungsten source mix in the solution, solution dried under 80 ° of C vacuum environments put into the ball mill ball milling 12 hours, sample behind the ball milling is put into microwave oven sintering 2min, at last the resulting powder of sintering is adopted SA-3100 type specific surface tester (BET) test, the specific surface area that can get powder is 31.2 (m
2/ g), and adopt D8ADVANCE type (Cu target, the K-α radiation) x ray diffractometer x of German Bruker company that powder is carried out crystal phase analysis, see accompanying drawing 2.
Embodiment 3.
Getting 9.2g tungsten is dissolved in the distilled water, supersound process 5min, after the tungsten source becomes settled solution, getting 45 g glucose dissolves in the settled solution, supersound process 5min, again solution magnetic agitation 15min is made that carbon source and tungsten source mix in the solution, solution dried under 80 ° of C vacuum environments put into the ball mill ball milling 12 hours, sample behind the ball milling is put into microwave oven sintering 2min, at last the resulting powder of sintering is adopted SA-3100 type specific surface tester (BET) test, the specific surface area that can get powder is 26.4 (m
2/ g),, and adopt D8ADVANCE type (Cu target, the K-α radiation) x ray diffractometer x of German Bruker company that powder is carried out crystal phase analysis, see accompanying drawing 3.
Embodiment 4.
Getting 18.4 g tungsten is dissolved in the distilled water, supersound process 5min, after the tungsten source becomes settled solution, getting 6 g carbon dissolves in the settled solution, supersound process 5min, again solution magnetic agitation 15min is made that carbon source and tungsten source mix in the solution, solution dried under 80 ° of C vacuum environments put into the ball mill ball milling 12 hours, sample behind the ball milling is put into microwave oven sintering 2min, at last the resulting powder of sintering is adopted SA-3100 type specific surface tester (BET) test, the specific surface area that can get powder is 35.6 (m
2/ g), and adopt D8ADVANCE type (Cu target, the K-α radiation) x ray diffractometer x of German Bruker company that powder is carried out crystal phase analysis, see accompanying drawing 4.
Claims (3)
1. the preparation method of a nanometer tungsten carbide, it is characterized in that at first, the tungsten source is dissolved in the distilled water, carry out supersound process, carbon source is dissolved in carry out supersound process in the tungsten source again, the mol ratio of tungsten source and carbon source is 1:2～1:5, magnetic agitation makes tungsten source and carbon source mixing, then with the sample oven dry, put into ball mill ball milling 5h～15h, carry out at last microwave sintering 1min～10min;
Described tungsten source is ammonium metawolframate or tungsten;
Described carbon source is glucose or carbon.
2. the preparation method of nanometer tungsten carbide according to claim 1 is characterized in that Ball-milling Time is 6h～9h in the ball mill.
3. the preparation method of nanometer tungsten carbide according to claim 1 is characterized in that the microwave sintering time is 2min～5min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103302309A (en) * | 2013-06-17 | 2013-09-18 | 南昌大学 | Preparation method of nano tungsten carbide |
| CN103302308A (en) * | 2013-06-17 | 2013-09-18 | 南昌大学 | Preparation method of nano tungsten powder |
| CN104556038A (en) * | 2015-01-23 | 2015-04-29 | 南昌硬质合金有限责任公司 | Synthetic method of spherical tungsten carbide powder |
| CN106350721A (en) * | 2016-09-05 | 2017-01-25 | 中南大学 | Preparation method of high-performance WC-Co cemented carbide of plate-like grain structure |
| CN112777597A (en) * | 2021-03-23 | 2021-05-11 | 上海简巨医学生物工程有限公司 | Niobium carbide nano material and preparation method thereof |
Citations (1)
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| CN101181690A (en) * | 2007-12-14 | 2008-05-21 | 中山大学 | Microwave induction catalytic preparation method of nano tungsten carbide |
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2012
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101181690A (en) * | 2007-12-14 | 2008-05-21 | 中山大学 | Microwave induction catalytic preparation method of nano tungsten carbide |
Non-Patent Citations (3)
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| Z.-G.BAN ET AL.: "Synthesis and processing of nanostructured WC-Co materials", 《JOURNAL OF MATERIALS SCIENCE》 * |
| 傅小明: "纳米碳化钨的制备技术及研究现状", 《稀有金属与硬质合金》 * |
| 赵学华等: "纳米WC粉体的制备及其催化应用", 《粉末冶金技术》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103302309A (en) * | 2013-06-17 | 2013-09-18 | 南昌大学 | Preparation method of nano tungsten carbide |
| CN103302308A (en) * | 2013-06-17 | 2013-09-18 | 南昌大学 | Preparation method of nano tungsten powder |
| CN103302309B (en) * | 2013-06-17 | 2016-04-20 | 南昌大学 | A kind of preparation method of nanometer tungsten carbide |
| CN104556038A (en) * | 2015-01-23 | 2015-04-29 | 南昌硬质合金有限责任公司 | Synthetic method of spherical tungsten carbide powder |
| CN104556038B (en) * | 2015-01-23 | 2016-08-31 | 南昌硬质合金有限责任公司 | A kind of synthetic method of spherical carbide tungsten powder |
| CN106350721A (en) * | 2016-09-05 | 2017-01-25 | 中南大学 | Preparation method of high-performance WC-Co cemented carbide of plate-like grain structure |
| CN106350721B (en) * | 2016-09-05 | 2018-06-29 | 中南大学 | A kind of preparation method of plate crystal structure high-performance WC-Co hard alloy |
| CN112777597A (en) * | 2021-03-23 | 2021-05-11 | 上海简巨医学生物工程有限公司 | Niobium carbide nano material and preparation method thereof |
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