CN102936003A - Preparation method of Nb1-xWxSe2 - Google Patents
Preparation method of Nb1-xWxSe2 Download PDFInfo
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- CN102936003A CN102936003A CN2012104431394A CN201210443139A CN102936003A CN 102936003 A CN102936003 A CN 102936003A CN 2012104431394 A CN2012104431394 A CN 2012104431394A CN 201210443139 A CN201210443139 A CN 201210443139A CN 102936003 A CN102936003 A CN 102936003A
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- nanoribbon
- xwxse2
- preparation
- nanosheet
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Abstract
The invention discloses a preparation method of Nb1-xWxSe2. The method includes the steps of dosing, ball milling, drying and sintering. The obtained Nb1-xWxSe2 is in shapes of nanoribbon and irregular nanosheet, mainly the nanoribbon. The length of nanoribbon is approximately dozens of micrometers, the thickness of the nanoribbon is about 100 nanometers, the radial dimension of irregular nanosheet is 1 mum to 2 mums, and the thickness of the irregular nanosheet is about 100 nanometers. By mixing W with NbSe2 and by means of high-energy long-time ball milling and a solid-phase reaction, an Nb1-xWxSe2 nanometer lubricating material in special shapes and different sizes is prepared. A technical process is free of pollution, cost is low, medicine is safe and easy to obtain, and an experiment method is simple and easy to operate. The obtained Nb1-xWxSe2 nanometer lubrication material is in mixed shapes of nanoribbon and nanosheet, has good friction abrasion performance as lubrication oil additives, and has good practicality and economical performance.
Description
Technical field
The present invention relates to solid nano lubricant technical field, be specifically related to a kind of Nb
1-xW
xSe
2The preparation method.
Background technology
Find first the semi-conductor WS of stratiform from Tenne in 1992 etc.
2After can forming the inorganic fullerene structure of similar carbon nanotube, magnesium-yttrium-transition metal chalcogenide MX
2(M=Nb, Mo, W, Ta; X=Se, S) it has obtained broad research as good solid lubricant.MX
2Belong to close-packed hexagonal structure, have and laminate structure like the graphite-like, the interlayer non-metallic atom is by weak Van der Waals force combination, atoms metal and non-metallic atom in the layer pass through covalent bonds, interlayer has lower shearing resistance, cause like this interlayer to be easy to slippage, can be as good solid lubricant.Because can improve bearing lubrication oil loading capability, reduction friction, MX2 obtains investigators' concern as lubricating oil additive simultaneously.Mixing to change electric conductivity, photochemical catalysis and the mechanical property of original material, is not changing the performance that can be better than former material under its crystalline structure; Secondly mix and to reduce cost, as with some low-cost metal-doped purposes that has reached the reduction cost; Thereby doping can change Growth Habit and obtain the novel pattern different from the pattern of the front material that mixes and make it have new performance or its some performance is strengthened.The present domestic and international also bibliographical information about material in the invention useless.
Summary of the invention
Goal of the invention: for the deficiencies in the prior art, the object of the present invention is to provide a kind of interpolation NbSe
2The Fe-Ni-Cr high temperature self-lubricating composite material, make it under 550 ~ 750 ℃, have good self-lubricating property and excellent wear resistance.Another object of the present invention provides a kind of above-mentioned interpolation NbSe
2The preparation method of Fe-Ni-Cr high temperature self-lubricating composite material, method is simply and very effective, the product of preparation has good self-lubricating property and excellent wear resistance.
Technical scheme: for achieving the above object, the technical solution used in the present invention is as follows:
A kind of Nb
1-xW
xSe
2The preparation method, it is characterized in that, may further comprise the steps:
(1) presses Nb
1-xW
xSe
2Stoichiometry take by weighing the W powder, by (Nb+W)/Se mol ratio be that 1:2.2 takes by weighing Nb powder and Se powder, put into ball grinder;
(2) taking by weighing diameter is that the Stainless Steel Ball of 8 mm mixes by ratio of grinding media to material 10:1 and puts into ball grinder, vacuumizes and pass into Ar gas in the tank, carries out ball milling 9 h with QMISP2 type ball mill with rotating speed 200rpm;
(3) the question response thing of drying step (2) gained is put into the quartz glass tube of an end opening, then elongate opening end with the acetylene torch heating and become thin mouthful and deflate that to be filled with the protection of Ar gas right, after again fusing seal up the mouth of pipe;
(4) quartz glass tube is put into tubular react furnace and be heated to 700 ℃, 20 ℃ of temperature rise rate per minutes behind the insulation 1h, naturally cool to room temperature with stove, obtain Nb
1-xW
xSe
2
Wherein, x is 1%～5%, preferred 3%.
Prepared Nb
1-xW
xSe
2, pattern is nano belt and random nanometer sheet, is mainly nano belt; Nanometer belt length 20 μ m～50 μ m, thick 100 nm, irregular nanometer sheet radial dimension 1 μ m～2 μ m, mean thickness is 100 nm.
Nb of the present invention
1-xW
xSe
2The preparation method of nano-lubricating material adopts with W doping NbSe in the building-up process
2Prepare the Nb of special appearance
1-xW
xSe
2Nano belt.The present invention adopts solid phase method preparation method technique simple, synthetic green non-pollution, and the nano belt of being synthesized is a kind of novel solid lubrication nano material, is a kind of very outstanding lubricating oil additive.
Beneficial effect: compared with prior art, the major advantage that the present invention has comprises: the present invention is by the W NbSe that mixes
2, and utilize the long-time ball milling of high energy, prepare the Nb of special appearance and different size by solid state reaction
1-xW
xSe
2Nano-lubricating material, the technological process green non-pollution, with low cost, drug safety is easy to get, and experimental technique is simple to operation.Prepared Nb
1-xW
xSe
2Nano-lubricating material is the mixing shape by nano belt and nanometer sheet, has preferably friction and wear behavior as lubricating oil additive.Have good practicality and economy.
Description of drawings
Fig. 1 is the Nb of the doping front and back of embodiment 1 preparation
1-xW
xSe
2The XRD diffractogram;
Fig. 2 is the front Nb of pure doping of embodiment 1 preparation
1-xW
xSe
2Scanning electron microscope (SEM) figure;
Fig. 3 is the Nb after the doping of embodiment 1 preparation
1-xW
xSe
2SEM figure;
Fig. 4 is the figure as a result of the frictional coefficient under different rotating speeds of oil sample of A, the B sample of gained before and after embodiment 2 mixes;
Fig. 5 is the figure as a result of the frictional coefficient under different loads of oil sample of A, the B sample of gained before and after embodiment 2 mixes.
Embodiment
Further illustrate the present invention below in conjunction with specific embodiment, the present embodiment is implemented under take technical solution of the present invention as prerequisite, should understand these modes and only be used for explanation the present invention and be not used in and limit the scope of the invention.
Raw material is taken by weighing by certain mol proportion, and the W powder takes by weighing the percent value of corresponding (Nb+W) total molar mass according to chemical formula Nb by the x value respectively
1-xW
xSe
2Middle x value is 0%, 3%, is labeled as respectively A, B, and wherein (Nb+W)/Se mol ratio is 1:2.2.The Stainless Steel Ball that takes by weighing respectively diameter and be 8mm mixes by ratio of grinding media to material 10:1 puts into ball grinder, vacuumizes and pass into Ar gas in the tank, 5 times repeatedly, carries out ball milling 9 hours with QMISP2 type ball mill with rotating speed 200rpm.To put into the quartz glass tube of the end opening of φ 8 mm * 10 mm after the question response thing drying, then become thin mouth and deflate to be filled with the protection of Ar gas and then to melt with acetylene torch heating elongation opening end to seal up the mouth of pipe; Put it into and be heated to 700 ℃ in the tubular react furnace, 20 ℃ of temperature rise rate per minutes naturally cool to room temperature with stove behind the insulation 1h and open reactor and obtain Sample A, B.The XRD of A, B sample as shown in Figure 1; The scanning electron microscope of A as shown in Figure 2; The scanning of B as shown in Figure 3.Adopt the Nb of the present invention's preparation
1-xW
xSe
2, be hexagonal nano-flake before mixing, the radial dimension of sheet is 2 μ m approximately, general 500 nm of thickness; Be the mixing shape of nano belt and nanometer sheet after mixing, thick approximately 100 nm of size, as depicted in figs. 1 and 2.
Embodiment 2
Nb with preparation
1-xW
xSe
2Add among the base oil HVI750 with the different mass mark respectively, utilize ultrasonic generator that pressed powder is evenly spread in the base oil, be mixed with the dirty solution oil sample.Investigate base oil and the tribological property that contains the mixing oil sample of different mass mark additive at UMT-2 type friction wear testing machine, measure the changing conditions of frictional coefficient under different loads and the different rotating speeds.Friction pair adopts ball-dish contact form, upper sample is that material mark 440C diameter is the Stainless Steel Ball of 4 mm, lower sample is the 45# steel disk of φ 20 mm * 5 mm, upper sample maintains static during experiment, lower sample rotates, rotating speed is 100-500 rpm, and load is 10-50 N, and experimental period is 30 min.Testing used Stainless Steel Ball model is 440-C (9Cr18), and diameter is 3 mm, and hardness is HRC62.
The frictional coefficient result under different rotating speeds of the oil sample of the A of gained, B sample before and after mixing, as shown in Figure 4, the frictional coefficient result under different loads of the oil sample of the A of gained, B sample before and after mixing, as shown in Figure 5, as seen the prepared Nb1-xWxSe2 nano-lubricating material of the present invention is the mixing shape by nano belt and nanometer sheet, has preferably friction and wear behavior as lubricating oil additive.
Claims (2)
1. Nb
1-xW
xSe
2The preparation method, it is characterized in that, may further comprise the steps:
(1) presses Nb
1-xW
xSe
2Stoichiometry take by weighing the W powder, by (Nb+W)/Se mol ratio be that 1:2.2 takes by weighing Nb powder and Se powder, put into ball grinder;
(2) taking by weighing diameter is that the Stainless Steel Ball of 8 mm mixes by ratio of grinding media to material 10:1 and puts into ball grinder, vacuumizes and pass into Ar gas in the tank, carries out ball milling 9 h with QMISP2 type ball mill with rotating speed 200 rpm;
(3) the question response thing of drying step (2) gained is put into the quartz glass tube of an end opening, then elongate opening end with the acetylene torch heating and become thin mouthful and deflate that to be filled with the protection of Ar gas right, after again fusing seal up the mouth of pipe;
(4) quartz glass tube is put into tubular react furnace and be heated to 700 ℃, 20 ℃ of temperature rise rate per minutes behind the insulation 1h, naturally cool to room temperature with stove, obtain Nb
1-xW
xSe
2
Wherein, x is 1%～5%.
2. described Nb according to claim 1
1-xW
xSe
2The preparation method, it is characterized in that prepared Nb
1-xW
xSe
2, pattern is nano belt and random nanometer sheet, is mainly nano belt; Nanometer belt length 20 μ m～50 μ m, thick 100 nm, irregular nanometer sheet radial dimension 1 μ m～2 μ m, mean thickness is 100 nm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210443139.4A CN102936003B (en) | 2012-11-08 | 2012-11-08 | Preparation method of Nb1-xWxSe2 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103642556A (en) * | 2013-11-12 | 2014-03-19 | 江苏大学 | Preparation method of NbSe2/CeNbO4 nanocomposite |
| CN104649236A (en) * | 2015-01-19 | 2015-05-27 | 东南大学 | Method for quickly preparing high-quality FeSe0.5Te0.5 superconductive polycrystal |
| CN108598456A (en) * | 2018-05-18 | 2018-09-28 | 江苏大学 | A kind of preparation method of lithium ion battery porous composite oxide negative material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11106775A (en) * | 1997-10-03 | 1999-04-20 | Taiho Kogyo Co Ltd | Solid lubricating film composition and plain bering material prepared therefrom |
| JP3054291B2 (en) * | 1993-04-28 | 2000-06-19 | トヨタ自動車株式会社 | Composition for sliding members |
| 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 |
-
2012
- 2012-11-08 CN CN201210443139.4A patent/CN102936003B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3054291B2 (en) * | 1993-04-28 | 2000-06-19 | トヨタ自動車株式会社 | Composition for sliding members |
| JPH11106775A (en) * | 1997-10-03 | 1999-04-20 | Taiho Kogyo Co Ltd | Solid lubricating film composition and plain bering material prepared therefrom |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| N.M.费多尔钦科 等: "第四节 硒化物和碲化物的性能和作用", 《粉末冶金复合减摩材料》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103642556A (en) * | 2013-11-12 | 2014-03-19 | 江苏大学 | Preparation method of NbSe2/CeNbO4 nanocomposite |
| CN103642556B (en) * | 2013-11-12 | 2015-07-08 | 江苏大学 | Preparation method of NbSe2/CeNbO4 nanocomposite |
| CN104649236A (en) * | 2015-01-19 | 2015-05-27 | 东南大学 | Method for quickly preparing high-quality FeSe0.5Te0.5 superconductive polycrystal |
| CN104649236B (en) * | 2015-01-19 | 2017-02-22 | 东南大学 | Method for quickly preparing high-quality FeSe0.5Te0.5 superconductive polycrystal |
| CN108598456A (en) * | 2018-05-18 | 2018-09-28 | 江苏大学 | A kind of preparation method of lithium ion battery porous composite oxide negative material |
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| Publication number | Publication date |
|---|---|
| CN102936003B (en) | 2014-08-13 |
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