CN102936003B - Preparation method of Nb1-xWxSe2 - Google Patents
Preparation method of Nb1-xWxSe2 Download PDFInfo
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- CN102936003B CN102936003B CN201210443139.4A CN201210443139A CN102936003B CN 102936003 B CN102936003 B CN 102936003B CN 201210443139 A CN201210443139 A CN 201210443139A CN 102936003 B CN102936003 B CN 102936003B
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- nanoribbon
- xwxse2
- nanosheet
- preparation
- irregular
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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
2preparation method.
Background technology
Find first the semi-conductor WS of stratiform from Tenne in 1992 etc.
2can form after the inorganic fullerene structure of similar carbon nanotube magnesium-yttrium-transition metal chalcogenide MX
2(M=Nb, Mo, W, Ta; X=Se, S) as good solid lubricant, it has obtained broad research.MX
2belong to close-packed hexagonal structure, have and laminate structure like graphite-like, interlayer non-metallic atom is by weak Van der Waals force combination, atoms metal and non-metallic atom in layer pass through covalent bonds, interlayer has lower shearing resistance, cause like this interlayer to be easy to slippage, can serve as good solid lubricant.Because can improve bearing lubrication oil loading capability, reduction friction, MX2 obtains investigators' concern as lubricating oil additive simultaneously.Doping can 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 doping can reduce costs, as by some low-cost metal-doped objects reducing costs that reached; Thereby doping can change Growth Habit obtain from adulterate before the different novel pattern of the pattern of material make it have new performance or its some performance strengthened.The domestic and international also bibliographical information about material in invention useless at present.
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 NbSe of interpolation
2fe-Ni-Cr high temperature self-lubricating composite material, make it at 550 ~ 750 DEG C, there is good self-lubricating property and excellent wear resistance.Another object of the present invention is to provide 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
2preparation method, it is characterized in that, comprise the following steps:
(1) press Nb
1-xw
xse
2stoichiometry take W powder, by (Nb+W)/Se mol ratio be that 1:2.2 takes Nb powder and Se powder, put into ball grinder;
(2) taking diameter is that the Stainless Steel Ball of 8 mm mixes and puts into ball grinder by ratio of grinding media to material 10:1, vacuumizes and pass into Ar gas in 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, puts into the quartz glass tube of an end opening, then elongate opening end with acetylene torch heating and become thin mouthful and deflate and being filled with the protection of Ar gas so, after again fusing seal up the mouth of pipe;
(4) quartz glass tube is put into tubular react furnace and be heated to 700 DEG C, 20 DEG C of temperature rise rate per minutes, after insulation 1h, naturally cool to room temperature with stove, obtain Nb
1-xw
xse
2;
Wherein, x is 1%～5%, preferably 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 in building-up process with W doping NbSe
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 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 adulterates
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, 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 by the mixing shape of nano belt and nanometer sheet, has good friction and wear behavior as lubricating oil additive.There is good practicality and economy.
Brief description of the drawings
Fig. 1 is the Nb before and after the doping prepared of embodiment 1
1-xw
xse
2xRD diffractogram;
Fig. 2 is the Nb before the pure doping prepared of embodiment 1
1-xw
xse
2scanning electron microscope (SEM) figure;
Fig. 3 is the Nb after the doping prepared of embodiment 1
1-xw
xse
2sEM figure;
Fig. 4 is the frictional coefficient result figure under different rotating speeds of the oil sample of A, the B sample of gained before and after embodiment 2 doping;
Fig. 5 is the frictional coefficient result figure under different loads of the oil sample of A, the B sample of gained before and after embodiment 2 doping.
Embodiment
Further illustrate the present invention below in conjunction with specific embodiment, the present embodiment is implemented under taking technical solution of the present invention as prerequisite, should understand these modes and only be not used in and limit the scope of the invention for the present invention is described.
Embodiment 1
Raw material is taken by certain mol proportion, and the percent value that W powder takes corresponding (Nb+W) total molar mass by x value is respectively according to chemical formula Nb
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 respectively diameter and be 8mm mixes and puts into ball grinder by ratio of grinding media to material 10:1, vacuumizes and pass into Ar gas in tank, 5 times repeatedly, carries out ball milling 9 hours with QMISP2 type ball mill with rotating speed 200rpm.After question response thing is dried, put into the quartz glass tube of an end opening of φ 8 mm × 10 mm, 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 in tubular react furnace and be heated to 700 DEG C, 20 DEG C of temperature rise rate per minutes, naturally cool to room temperature with stove after 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.The Nb that adopts the present invention to prepare
1-xw
xse
2, before doping, be hexagonal nano-flake, the radial dimension of sheet approximately 2 μ m, general 500 nm of thickness; After doping, be the mixing shape of nano belt and nanometer sheet, thick approximately 100 nm of size, as depicted in figs. 1 and 2.
Embodiment 2
By the Nb of preparation
1-xw
xse
2add in base oil HVI750 with different mass mark respectively, utilize ultrasonic generator that pressed powder is evenly spread in base oil, be mixed with dirty solution oil sample.The tribological property of the mixing oil sample of investigating base oil and contain different mass mark additive on UMT-2 type friction wear testing machine, the changing conditions of frictional coefficient under mensuration different loads and 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, when experiment, upper sample maintains static, lower sample rotates, rotating speed is 100-500 rpm, and load is 10-50 N, and experimental period is 30 min.Testing Stainless Steel Ball model used 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 doping, 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 doping, as shown in Figure 5, the prepared Nb1-xWxSe2 nano-lubricating material of visible the present invention is by the mixing shape of nano belt and nanometer sheet, has good friction and wear behavior as lubricating oil additive.
Claims (2)
1. a Nb
1-xw
xse
2preparation method, it is characterized in that, comprise the following steps:
(1) press Nb
1-xw
xse
2stoichiometry take W powder, by (Nb+W)/Se mol ratio be that 1:2.2 takes Nb powder and Se powder, put into ball grinder;
(2) taking diameter is that the Stainless Steel Ball of 8 mm mixes and puts into ball grinder by ratio of grinding media to material 10:1, vacuumizes and pass into Ar gas in 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, puts into the quartz glass tube of an end opening, then elongate opening end with acetylene torch heating and become thin mouthful and deflate and being filled with the protection of Ar gas, and then the mouth of pipe is sealed up in fusing;
(4) quartz glass tube is put into tubular react furnace and be heated to 700 DEG C, 20 DEG C of temperature rise rate per minutes, after insulation 1h, naturally cool to room temperature with stove, obtain Nb
1-xw
xse
2;
Wherein, x is 1%～5%.
2. Nb according to claim 1
1-xw
xse
2preparation 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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|---|---|---|---|
| CN201210443139.4A CN102936003B (en) | 2012-11-08 | 2012-11-08 | Preparation method of Nb1-xWxSe2 |
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|---|---|---|---|
| CN201210443139.4A CN102936003B (en) | 2012-11-08 | 2012-11-08 | Preparation method of Nb1-xWxSe2 |
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| CN102936003B true CN102936003B (en) | 2014-08-13 |
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|---|---|---|---|---|
| CN103642556B (en) * | 2013-11-12 | 2015-07-08 | 江苏大学 | Preparation method of NbSe2/CeNbO4 nanocomposite |
| 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 |
Citations (2)
| 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 |
| 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 |
Family Cites Families (1)
| 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 |
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2012
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Patent Citations (2)
| 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 |
| 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 (4)
| Title |
|---|
| JP特开平11-106775A 1999.04.20 |
| JP特许第3054291号B2 2000.06.19 |
| 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》.1985,第108-109页. |
| 第四节 硒化物和碲化物的性能和作用;N.M.费多尔钦科 等;《粉末冶金复合减摩材料》;19850831;第108-109页 * |
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