CN102092690A - Method for preparing tungsten diselenide nano sheets - Google Patents
Method for preparing tungsten diselenide nano sheets Download PDFInfo
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- CN102092690A CN102092690A CN2010105720157A CN201010572015A CN102092690A CN 102092690 A CN102092690 A CN 102092690A CN 2010105720157 A CN2010105720157 A CN 2010105720157A CN 201010572015 A CN201010572015 A CN 201010572015A CN 102092690 A CN102092690 A CN 102092690A
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- tungsten diselenide
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Abstract
The invention discloses a method for preparing tungsten diselenide nano sheets, comprising the following steps of: evenly mixing tungsten powder and selenium powder in a certain mol ratio; heating and reacting the mixture under protection of argon, and cooling to obtain the tungsten diselenide nano sheets. The tungsten diselenide nano sheet is of an inorganic nano sheet laminated structure; the tungsten diselenide nano sheet has excellent dispersion performance and friction performance in base oil and polymer compounds; the tungsten diselenide nano sheet is simple in preparing method, safe, environment friendly, high in production rate, low in cost and suitable for large-scale industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of inorganic nano material, more specifically, is a kind of preparation method of two selenizing tungsten nanometer sheet.
Background technology
Magnesium-yttrium-transition metal selenide MSe
2(M=Mo, W, Nb, Ta, Ti, Zr) become one of research focus of Nanotribology.Find that at present many nanometer sheet all have good antiwear and antifriction effect as lubricating oil additive, even can play repair to wear surface.With nano material as lubricating oil additive, educational circles has obtained extensive studies in friction, the aspects such as synthetic and tribological property that comprise nano material, wherein directly make between simple substance and react by solid reaction process, technical process is simple and reaction by-product is less, is a kind of synthetic method preferably.It has been found that in tribological field,, can improve its extreme pressure property, supporting capacity and frictional coefficient well when nano material is added in the base oil.At present, the explanation to nanometer additive properties of antifriction and wear resistance mechanism has: the effect of the weak Van der Waals force of the interlayer of (1) nanometer lamella; (2) friction chemical reaction; (3) provide protection of adsorption film.Especially, WSe
2Have laminate structure, two selenium atoms and tungsten atom are respectively with covalent bonds, and interlayer is used as lubricating oil additive just slip between genetic horizon easily when being subjected to shearing force with more weak Van der Waals force combination, thereby plays the effect of antifriction.But at present, less in the research of tribological field to it as lubricating oil additive, research mainly is to concentrate on anti-friction wear-resistant effect and wear surface analysis aspect, and to the research of the real-time corresponding relation of the contact resistance of friction pair oil film in process of the test and frictional coefficient still less.
Summary of the invention
The object of the invention is to provide a kind of preparation method of wear-resisting and two selenizing tungsten nanometer sheet that dispersing property is good, has characteristics such as technology is simple, production process safety and environmental protection.
The present invention realizes by following technique means: have cheap characteristics at tungsten powder and selenium powder; after mixing according to a certain percentage; under argon shield, heat; reaction generates two selenizing tungsten nanometer sheet with mineral-type nanometer sheet laminate structure; have good dispersiveness, mechanical property and wear resisting property, preparation technology is simple, cost is low and the production process safety and environmental protection.
The method of preparation two selenizing tungsten nanometer sheet of the present invention may further comprise the steps:
(1) preparation raw material mixture: the mol ratio according to Se: W～2: 1 is got tungsten powder and selenium powder, grinds and mixes the back and carry out ball milling under argon shield, is packaged in then in the vitreosil pipe, obtains raw mix;
(2) add thermal synthesis: the above-mentioned raw materials mixture is warming up to 600～700 ℃, is incubated 1 hour postcooling, obtain two selenizing tungsten nanometer sheet.
Utilize the present invention to prepare two selenizing tungsten nanometer sheet, raw material is easy to get and is cheap, effectively reduces production cost; Simple and the production process safety and environmental protection of technology is particularly suitable for large-scale commercial production; Gained two selenizing tungsten nanometer sheet have mineral-type nanometer sheet laminate structure, in base oil and polymer composite, has good dispersing property, and have good frictional behaviour, preparation method's technology is simple, safety and environmental protection, productive rate height, cost are low, be fit to large-scale industrial production.
Description of drawings
Fig. 1 is the XRD diffractogram of the embodiment of the invention 1 described two selenizing tungsten nanometer sheet 1;
Fig. 2 is the XRD diffractogram of the embodiment of the invention 2 described two selenizing tungsten nanometer sheet 2;
Fig. 3 is the transmission plot of the embodiment of the invention 1 described two selenizing tungsten nanometer sheet 1;
Fig. 4 is the transmission plot of the embodiment of the invention 2 described two selenizing tungsten nanometer sheet 2;
Fig. 5 for the embodiment of the invention 1 described two selenizing tungsten nanometer sheet 1 as the base oil additive to improving the friction curve of oil product tribological property;
To be the embodiment of the invention 1 described two selenizing tungsten nanometer sheet 1 add The friction coefficient change in rotational speed curve behind the base oil with 2% massfraction to Fig. 6.
Embodiment
Below further describe the present invention by embodiment, as known by the technical knowledge, the present invention also can describe by other the scheme that does not break away from the technology of the present invention feature, thus all within the scope of the present invention or the change that is equal in the scope of the invention all be included in the invention.
Embodiment 1:
Be prepared as follows two selenizing tungsten nanometer sheet:
(1) preparation raw material mixture: get tungsten powder and selenium powder according to 1: 2 mol ratio, and selenium powder excessive 5%, mixing the back ground 5 minutes in mortar, be that the Stainless Steel Ball of 8mm is to mix at 1: 10 to put into ball grinder by mass ratio with diameter again, sealing is also extracted air in the jar, feed and extract argon gas 5 times repeatedly, ball grinder is put into ball mill the ball grinder powder was carried out ball milling 30 minutes with 200 rev/mins rotating speed, taking out powder then, to put into the diameter that an end seals be the quartz glass tube of 15mm, obtains raw mix;
(2) add thermal synthesis: above-mentioned silica tube is heated to its opening end with the acetylene flame after molten state, seals and stay an aperture, couple together with vacuum pump and aperture and to seal again after silica tube vacuumized, the vitreosil pipe that reactant is housed that obtains sealing, put it in the tubular react furnace, speed with 7 ℃/min is heated to 600 ℃, be incubated and naturally cool to room temperature with stove after 1 hour, obtain two selenizing tungsten nanometer sheet 1.
Embodiment 2:
Be prepared as follows two selenizing tungsten nanometer sheet:
(1) preparation raw material mixture: get tungsten powder and selenium powder according to 1: 2 mol ratio, and selenium powder excessive 5%, mixing the back ground 5 minutes in mortar, be that the Stainless Steel Ball of 8mm is to mix at 1: 10 to put into ball grinder by mass ratio with diameter again, sealing is also extracted air in the jar, feed and extract argon gas 5 times repeatedly, ball grinder is put into ball mill the ball grinder powder was carried out ball milling 30 minutes with 200 rev/mins rotating speed, taking out powder then, to put into the diameter that an end seals be the quartz glass tube of 15mm, obtains raw mix;
(2) add thermal synthesis: above-mentioned silica tube is heated to its opening end with the acetylene flame after molten state, seals and stay an aperture, couple together with vacuum pump and aperture and to seal again after silica tube vacuumized, the vitreosil pipe that reactant is housed that obtains sealing, put it in the tubular react furnace, speed with 7 ℃/min is heated to 700 ℃, be incubated and naturally cool to room temperature with stove after 1 hour, obtain two selenizing tungsten nanometer sheet 2.
Facts have proved that the preparation method of two selenizing tungsten nanometer sheet of the present invention has that raw material is cheap and easy to get, technology is simple and the characteristics of safety and environmental protection.
For structure and the performance that proves products therefrom among the embodiment, at first the microscopic appearance of two selenizing tungsten nanometer sheet 1 and two selenizing tungsten nanometer sheet 1 is analyzed, earlier it is carried out X-ray diffraction analysis, the result is respectively as shown in Figure 1 and Figure 2; Again it is carried out tem analysis, the result distinguishes as shown in Figure 3, Figure 4, and as seen from the figure, products obtained therefrom does not have other assorted crystallization phases, is WSe
2Nanometer sheet.
In order further to prove embodiment of the invention gained two selenizing tungsten nanometer sheet premium properties in use, it is carried out performance test as the base oil additive, concrete testing method is as follows:
With two selenizing tungsten nanometer sheet 1 is 2% with massfraction respectively, 5%, 7% and 10% adds among the base oil HVI750, be mixed with corresponding oil product and on frictional testing machines, carry out the tribological property test, the friction contact form is ball-disc type, last sample is material mark 440C, diameter is the Stainless Steel Ball of 4mm, the 45# steel disk that following sample is Φ 20mm * 6mm, going up sample during experiment maintains static, following sample rotates, with the friction radius is 7mm, relative rotational is 400 rev/mins, loading force is respectively 0.1N, 1N, 2N, 3N, 4N, the frictional experiment time is that the condition of 30min is tested, test result as shown in Figure 5, as seen from the figure, the massfraction of two selenizing tungsten nanometer sheet 1 is 2%, friction radius is 7mm, when loading force is 2N, properties of antifriction and wear resistance the best.
For the massfraction that illustrates further above-mentioned two selenizing tungsten nanometer sheet 1 tribological property of 2% oil product and the relation of rotating speed, this oil product is carried out the speed change experiment, described oil product and pure base oil HVI750 are respectively 100 rev/mins, 200 rev/mins, 300 rev/mins, 400 rev/mins, 500 rev/mins in load 2N, friction speed of rotation, friction radius is 7mm, experimental period is to test under the condition of 30min, test result as shown in Figure 6, antifriction performance the best when as seen from the figure, rotating speed is 400 rev/mins.
The tribological property of embodiment 2 gained two selenizing tungsten nanometer sheet 2 and embodiment 1 gained two selenizing tungsten nanometer sheet 1 show similar result.
In sum, the two selenizing tungsten nanometer sheet of utilizing the present invention to prepare have mineral-type nanometer sheet laminate structure, in base oil, has good dispersing property, and have good frictional behaviour, preparation method's technology is simple, safety and environmental protection, productive rate height, cost are low, be fit to large-scale industrial production.
Claims (1)
1. the preparation method of a selenizing tungsten nanometer sheet is characterized in that, may further comprise the steps:
(1) preparation raw material mixture: the mol ratio according to Se: W～2: 1 is got tungsten powder and selenium powder, grinds and mixes the back and carry out ball milling under argon shield, is packaged in then in the vitreosil pipe, obtains raw mix;
(2) add thermal synthesis: the above-mentioned raw materials mixture is warming up to 600～700 ℃, is incubated 1 hour postcooling, obtain two selenizing tungsten nanometer sheet.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010105720157A CN102092690A (en) | 2010-12-03 | 2010-12-03 | Method for preparing tungsten diselenide nano sheets |
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| CN2010105720157A CN102092690A (en) | 2010-12-03 | 2010-12-03 | Method for preparing tungsten diselenide nano sheets |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102504910A (en) * | 2011-11-28 | 2012-06-20 | 镇江中孚复合材料有限公司 | Molybdenum-doped tungsten diselenide nanosheet serving as anti-fraction additive and preparation method thereof |
| CN103373714A (en) * | 2012-04-24 | 2013-10-30 | 长沙联恒科技有限公司 | Production method of tungsten selenide and production equipment thereof |
| CN103613080A (en) * | 2013-12-02 | 2014-03-05 | 镇江市高等专科学校 | Method for synthesizing ultrathin niobium diselenide nanosheet by pressureless sintering |
| CN105776154A (en) * | 2016-05-10 | 2016-07-20 | 电子科技大学 | Preparation method of tungsten diselenide nanosheet |
| CN105967155A (en) * | 2016-05-10 | 2016-09-28 | 电子科技大学 | Method for preparing tungsten diselenide nanoflower |
| CN107601443A (en) * | 2017-11-09 | 2018-01-19 | 安徽大学 | A kind of preparation method of ultra-thin tungsten selenide nanometer sheet |
| CN107662906A (en) * | 2017-11-10 | 2018-02-06 | 福州大学 | A kind of preparation method of two selenizings W film and the application of photocatalytic reduction of carbon oxide |
| CN110282975A (en) * | 2019-07-08 | 2019-09-27 | 先导薄膜材料（广东）有限公司 | A kind of Germanium selenide target and preparation method thereof |
| CN113501505A (en) * | 2021-08-19 | 2021-10-15 | 河北大学 | Two-dimensional tungsten selenide nano material and preparation method thereof |
-
2010
- 2010-12-03 CN CN2010105720157A patent/CN102092690A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| VILAS GANPAT POL, ET AL: "One Pot, Environmentally Benign, Thermal Reaction to Fabricate WSe2 and mose2 nanoplates", 《JOURNAL OF NANO RESEARCH》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102504910A (en) * | 2011-11-28 | 2012-06-20 | 镇江中孚复合材料有限公司 | Molybdenum-doped tungsten diselenide nanosheet serving as anti-fraction additive and preparation method thereof |
| CN103373714A (en) * | 2012-04-24 | 2013-10-30 | 长沙联恒科技有限公司 | Production method of tungsten selenide and production equipment thereof |
| CN103613080A (en) * | 2013-12-02 | 2014-03-05 | 镇江市高等专科学校 | Method for synthesizing ultrathin niobium diselenide nanosheet by pressureless sintering |
| CN105776154A (en) * | 2016-05-10 | 2016-07-20 | 电子科技大学 | Preparation method of tungsten diselenide nanosheet |
| CN105967155A (en) * | 2016-05-10 | 2016-09-28 | 电子科技大学 | Method for preparing tungsten diselenide nanoflower |
| CN105967155B (en) * | 2016-05-10 | 2018-04-13 | 电子科技大学 | The preparation method of two tungsten selenide nano flowers |
| CN107601443A (en) * | 2017-11-09 | 2018-01-19 | 安徽大学 | A kind of preparation method of ultra-thin tungsten selenide nanometer sheet |
| CN107601443B (en) * | 2017-11-09 | 2020-01-14 | 安徽大学 | Preparation method of ultrathin tungsten selenide nanosheets |
| CN107662906A (en) * | 2017-11-10 | 2018-02-06 | 福州大学 | A kind of preparation method of two selenizings W film and the application of photocatalytic reduction of carbon oxide |
| CN110282975A (en) * | 2019-07-08 | 2019-09-27 | 先导薄膜材料（广东）有限公司 | A kind of Germanium selenide target and preparation method thereof |
| CN113501505A (en) * | 2021-08-19 | 2021-10-15 | 河北大学 | Two-dimensional tungsten selenide nano material and preparation method thereof |
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Application publication date: 20110615 |