CN101898750B - Solid lubricating oil additive MoSe2 nanosheet and preparation method thereof - Google Patents
Solid lubricating oil additive MoSe2 nanosheet and preparation method thereof Download PDFInfo
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- CN101898750B CN101898750B CN2009101806902A CN200910180690A CN101898750B CN 101898750 B CN101898750 B CN 101898750B CN 2009101806902 A CN2009101806902 A CN 2009101806902A CN 200910180690 A CN200910180690 A CN 200910180690A CN 101898750 B CN101898750 B CN 101898750B
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Abstract
The invention discloses a solid lubricating oil additive MoSe2 nanosheet and a preparation method thereof. Molybdenum powder and selenium powder are used as main raw materials to directly prepare the solid lubricating oil additive MoSe2 nanosheet through one-step solid phase reaction. The method of the invention has the advantages of easy acquisition of raw materials, low cost of raw materials, simple preparation technology, easy control of parameters and safe and environment-friendly production processes, and is especially suitable for large-scale industrial production. The solid lubricating oil additive MoSe2 nanosheet prepared by the method of the invention has the advantages of good crystallization, high purity and excellent lubricating property.
Description
Technical field
The present invention relates to the lubricant field, specifically, is a kind of solid lubrication oil additive MoSe
2Nanometer sheet and preparation method thereof.
Background technology
Magnesium-yttrium-transition metal sulphur, selenide have various physical properties, like metallicity, supraconductivity, magnetic, semiconductor property etc., all are widely used at photoelectric field, catalytic field, friction field etc.MoSe
2It is exactly a kind of magnesium-yttrium-transition metal selenide; It has and is similar to the laminar structured of graphite; With covalent bonds, interlayer then connects with Van der Waals force between interior Mo atom of layer and the Se atom, is easy to peel off between layer and the layer; Have good anisotropy and lower frictional coefficient, can be used as the body material of various fields such as main frame embedding, battery electrode, hydrogen storage material, catalyzer, lubricant.At present about MoSe
2Report actually rare, wherein synthetic MoSe
2Method comprise that mainly hydrothermal method, electrosynthesis, thermal decomposition method, laser melt method etc., still, above-mentioned synthetic MoSe
2Method all comprise complicated process control, and the synthetic product is unbodied MoSe often
2, also need further heat treatment process, for environment pollution is arranged simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of solid lubrication oil additive MoSe
2Nanometer sheet and preparation method thereof, the method through simple environmental protection is low-cost, prepare solid lubrication oil additive MoSe expeditiously
2Nanometer sheet.
Above-mentioned purpose realizes through following technical scheme: with molybdenum powder and selenium powder is raw material, directly prepares solid lubrication oil additive MoSe through the solid state reaction that settles at one go
2Nanometer sheet.Concrete steps are following:
(1) takes by weighing molybdenum powder (purity 99%) and selenium powder (purity 99.9%) according to 1: 3 mol ratio, mix the two and grind evenly, put into stainless steel cauldron with agate mortar;
(2) reaction kettle is placed in the high temperature box furnace, temperature in the stove is increased to 750 ℃, keep 1h according to the temperature rise rate of 10 ℃/min;
(3) make temperature natural cool to room temperature (needing 5h approximately) in the high temperature box furnace, open the chocolate powder that reaction kettle sees and be solid lubrication oil additive MoSe of the present invention
2Nanometer sheet.
The raw material of the inventive method is easy to get, cheap, preparation technology is simple, parameter is prone to control, utilizes solid reaction process to settle preparation MoSe at one go
2Nanometer sheet, the production process safety and environmental protection is particularly suitable for large-scale industrial production; The solid lubrication oil additive MoSe for preparing with the inventive method
2The nanometer sheet advantages of good crystallization, purity is high, and has excellent lubricating property.
Description of drawings
Fig. 1 is the solid lubrication oil additive MoSe of embodiment 1
2The X-ray energy spectrum of nanometer sheet (EDS) spectrogram;
Fig. 2 is the solid lubrication oil additive MoSe of embodiment 1
2Microscopic appearance picture under the nanometer sheet Electronic Speculum (SEM);
Fig. 3 is the solid lubrication oil additive MoSe of embodiment 1
2The microscopic appearance picture of nanometer sheet under high resolution electron microscopy (SEM);
Fig. 4 is the frictional coefficient change curve of embodiment 2.
Embodiment
Below further describe the present invention through embodiment; Can know by technological general knowledge; The present invention also can describe through other the scheme that does not break away from technical characterictic of the present invention, thus all within the scope of the present invention or the change that is equal in the scope of the invention all comprised by the present invention.
Embodiment 1: preparation solid lubrication oil additive MoSe
2Nanometer sheet
Take by weighing molybdenum powder (purity 99%) and selenium powder (purity 99.9%) according to 1: 3 mol ratio, mix the two and grind evenly, put into stainless steel cauldron with agate mortar; Reaction kettle is placed in the high temperature box furnace, temperature in the stove is increased to 750 ℃, keep 1h according to the temperature rise rate of 10 ℃/min; Make temperature natural cool to room temperature (needing 5h approximately) in the high temperature box furnace, open the chocolate powder that reaction kettle sees and be solid lubrication oil additive MoSe
2Nanometer sheet.
Solid lubrication oil additive MoSe to present embodiment
2Nanometer sheet is carried out X-ray energy spectrum (EDS) test, and the result is as shown in Figure 1, the atomic ratio of visible Se/Mo be 1: 2 (Se:63.9%, Mo:36.10%).
Observe the shape characteristic of the solid lubrication oil additive MoSe2 nanometer sheet of present embodiment through ESEM (SEM), the result is as shown in Figure 2, visible product MoSe
2Form by large-sized coacervate.
Under the high power ESEM, further observe, the result is as shown in Figure 3, can find out that product is made up of at the lamella of 10～50nm at 100～500nm, thickness length.
Embodiment 2: test solid lubrication oil additive MoSe
2The frictional behaviour of nanometer sheet
MoSe with embodiment 1
2Nanometer sheet is added among the base oil 150bn according to 1%, 5%, 7% mass concentration respectively, and tests above-mentioned three kinds and added MoSe
2The base oil 150bn of nanometer sheet and the pure oil of the 150bn frictional coefficient under different loads (0.5kg, 1kg, 2kg, 3kg, 4kg, 5kg); Make load-frictional coefficient relation curve to measuring the result; The result is as shown in Figure 4, can find out, under different loads, has added MoSe
2The frictional coefficient of the base oil 150bn of the nanometer sheet all frictional coefficient than the pure oil of 150bn is low; Under the identical condition of load, MoSe in base oil 150bn
2The mass concentration of nanometer sheet is 5% o'clock, and frictional coefficient is minimum.Be solid lubrication oil additive MoSe of the present invention
2Nanometer sheet can significantly improve the lubricity of lubricating oil.
Claims (3)
1. the preparation method of a solid lubrication oil additive MoSe2 nanometer sheet is characterized in that may further comprise the steps:
(1) takes by weighing molybdenum powder and selenium powder according to 1: 3 mol ratio, mix the two and grind evenly, put into stainless steel cauldron with agate mortar;
(2) reaction kettle is placed in the high temperature box furnace, temperature in the stove is increased to 750 ℃, keep 1h according to the temperature rise rate of 10 ℃/min;
(3) make temperature natural cool to room temperature in the high temperature box furnace, open the chocolate powder that reaction kettle sees and be solid lubrication oil additive MoSe
2Nanometer sheet.
2. preparation method according to claim 1 is characterized in that, said molybdenum powder purity is 99%, and said selenium powder purity is 99.9%.
3. the solid lubrication oil additive MoSe that method according to claim 1 prepares
2Nanometer sheet.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101806902A CN101898750B (en) | 2009-10-28 | 2009-10-28 | Solid lubricating oil additive MoSe2 nanosheet and preparation method thereof |
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|---|---|---|---|
| CN2009101806902A CN101898750B (en) | 2009-10-28 | 2009-10-28 | Solid lubricating oil additive MoSe2 nanosheet and preparation method thereof |
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| CN101898750A CN101898750A (en) | 2010-12-01 |
| CN101898750B true CN101898750B (en) | 2012-05-23 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127484B (en) * | 2010-12-03 | 2013-11-20 | 无锡润鹏复合新材料有限公司 | Preparation method of tungsten diselenide nano-clathrate |
| 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 |
| CN103143373B (en) * | 2013-03-13 | 2014-10-29 | 南开大学 | Method for preparing hydrodesulfurization catalyst |
| CN103614777A (en) * | 2013-10-15 | 2014-03-05 | 中国科学院理化技术研究所 | Preparation method of large-area single-layer or multi-layer molybdenum diselenide single chip |
| CN106145065B (en) * | 2016-07-04 | 2018-04-24 | 江苏大学 | Transition metal chalcogenide MX2Ultrathin nanometer piece, preparation method and its usage |
| CN107539964B (en) * | 2017-09-30 | 2019-11-26 | 江苏理工学院 | A kind of two selenizing molybdenum powder body material of hexagonal flake and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1563299A (en) * | 2004-04-20 | 2005-01-12 | 杨海滨 | Hub structural nano solid lubricant and preparaton method |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1563299A (en) * | 2004-04-20 | 2005-01-12 | 杨海滨 | Hub structural nano solid lubricant and preparaton method |
Non-Patent Citations (1)
| Title |
|---|
| HuaQiang Shi,etc..Synthesis of MoSe2 nano-flakes modified with dithiophsphinic acid extractant at low temperature.《Materials Letters》.2008,第62卷3649-3651. * |
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