CN103771354A - Preparation method and application of TixNb1-xSe2 nanomaterials - Google Patents
Preparation method and application of TixNb1-xSe2 nanomaterials Download PDFInfo
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- CN103771354A CN103771354A CN201310669217.7A CN201310669217A CN103771354A CN 103771354 A CN103771354 A CN 103771354A CN 201310669217 A CN201310669217 A CN 201310669217A CN 103771354 A CN103771354 A CN 103771354A
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Abstract
The invention discloses a preparation method of TixNb1-xSe2 nanomaterials. Nanomaterials with different shapes can be prepared from raw materials, i.e., Nb powder, Se powder and Ti powder by using a solid-phase reaction method. The preparation method comprises the steps: proportioning; ball milling; drying; sintering. Raw materials are uniformly mixed and filled into a quartz glass tube after being ball-milled and dried and are heated under the protection of inert gases, subjected to heat preservation and cooled to obtain the TixNb1-xSe2 nanomaterials. The prepared TixNb1-xSe2 nanomaterials are mainly nanoribbons and nanosheets, wherein each nanoribbon is about 30nm thick, about 200nm wide and about over 10mum long, and each nanosheet is about 2mum long in radial direction and about 300nm thick. The prepared powder is added into base oil, so that the TixNb1-xSe2 nanomaterials have better frictional wear performance; the preparation method is simple in process, safe, environment-friendly and low in cost.
Description
Technical field
The present invention relates to lubricant technical field, relate in particular to a kind of Ti
xnb
1-xse
2the preparation method of nano material and application thereof.
Background technology
Magnesium-yttrium-transition metal sulphur selenium compound MX
2(M=Nb, Mo, W, Ta; X=Se, S) there is various physical propertiess such as metallicity, supraconductivity, magnetic, semiconductor property, it has obtained broad research as good solid lubricant.MX
2crystal is the hexahedron structure that X-M-X atom forms.Every one deck X-M atom is with very strong covalent bonds, and is with very weak van der waals bond combination between layers, and layer is directly easy to peel off with layer, has good anisotropy and lower frictional coefficient, can be used as good solid lubricant.
NbSe
2there is with it selection that becomes development of new material compared with good tribological property under low resistivity and vacuum-drying environment.With respect to graphite, MoS
2, NbSe
2without natural mineral, and Nb, Se source cost are high, thereby synthetic expensive limited its application, and it is adulterated and is reduced costs, and will greatly expand its Application Areas.The niobite of niobium tantalum symbiosis and the superalloy that contains the elements such as Nb, Ti, Ta, in the time of this type of insoluble metal element of hydrometallurgical process, separation difficulty, if do not separate and can conduct develop doping NbSe
2the raw material of novel material, can reduce energy consumption and reduce raw materials cost.Doping does not change former material crystalline structure can make its performance be better than the performance of former material, thus doping can also change the habit of crystal obtain from adulterate before the different novel pattern of the pattern of material make it have new performance.Used as lubricating oil additive slip between easy genetic horizon in the time being subject to shearing force.At present, using less in the research of tribological field as base oil additive the material of doping, also yet there are no and have both at home and abroad about Ti doping NbSe simultaneously
2report.
Summary of the invention
The object of the present invention is to provide a kind of Ti
xnb
1-xse
2the preparation method of nano material and as base oil additive and NbSe
2compare it and have better oilness and good wear resistance.There is the features such as technique is simple, production process safety and environmental protection.
Technical scheme: the present invention realizes by following technique means: take selenium powder, niobium powder and titanium valve as raw material, directly prepare base oil additive Ti by solid state reaction
xnb
1-xse
2nano belt and nanometer sheet.It has good dispersiveness, mechanical property and wear resisting property, and preparation technology is simple, cost is low and production process safety and environmental protection.
The present invention adopts following technical scheme:
Ti of the present invention
xnb
1-xse
2preparation method's concrete steps of nano material are as follows:
(1) configuration raw mixture: press Ti
xnb
1-xse
2stoichiometry claim Ti powder, by Se:(Nb+Ti) mol ratio of=2～3:1 takes Nb powder and Se powder, mix;
(2) take the Stainless Steel Ball of 10mm in the ratio of the weight ratio 8～10:1 of ball material and raw mixture, the raw material and the Stainless Steel Ball that in step (1), mix are put into planetary ball mill, after vacuumizing, under argon shield, carry out ball milling, ball milling 24h;
(3) the question response thing of drying step (2) gained installs in silica tube, deflate and pass into argon gas, by putting into tubular react furnace after silica tube sealing, being heated to 650 ℃～800 ℃ with the speed of 5 ℃/min, after insulation 0.5h～2h, cool to room temperature with the furnace, obtain Ti
xnb
1-xse
2nano material, wherein x is 1%～5%.
In step (1), preferably by Se:(Nb+Ti) mol ratio of=2.2:1 takes Nb powder and Se powder.
In step (1), Nb powder is 200 orders, Ti powder 300 orders, Se powder 300 orders.
In step (2), preferably take the Stainless Steel Ball of 10mm in the ratio of the weight ratio 10:1 of ball material and raw mixture.
In step (2), the speed 200r/min of star formula ball mill.
In step (3), be preferably heated to 750 ℃ with the speed of 5 ℃/min.
In step (3), be preferably incubated 1h.
In step (3), the diameter of quartz glass tube is 15mm.
The Ti that the present invention is prepared
xnb
1-xse
2nano material can be used as lubricating oil additive and uses.
Positively effect of the present invention is as follows:
The present invention utilizes solid state reaction, adopts Ti doping NbSe in building-up process
2prepare the Ti of special appearance
xnb
1-xse
2nano belt and nanometer sheet.The about 30nm of nano belt mean thickness, wide about 200nm, is about tens microns; The radially about 2um of nanometer sheet, average thick about 300nm.Simple, the synthetic environmental protection of technique that solid reaction process is prepared material, the nano belt of synthesized and nanometer sheet are a kind of novel solid lubricants, have more excellent performance as lubricating oil additive.
Accompanying drawing explanation
Fig. 1 is NbSe before embodiment 1 doping
2(A) with the rear Ti of doping
xnb
1-xse
2(B) XRD diffracting spectrum.
Fig. 2 is the Ti of embodiment 1
xnb
1-xse
2the SEM picture under scanning electron microscope (x gets 0%, 750 ℃) of nano material.
Fig. 3 is the Ti of embodiment 1
xnb
1-xse
2the SEM picture under scanning electron microscope of nano material (x gets 5%, temperature 650 ℃).
Fig. 4 is the Ti of embodiment 1
xnb
1-xse
2the SEM picture under scanning electron microscope of nano material (x gets 5%, temperature 750 ℃).
Fig. 5 is doping front and back gained A, B (x gets 5%) sample frictional coefficient result figure under different loads in embodiment 2.
Embodiment
Further describe the present invention by embodiment below, as known by the technical knowledge, the present invention also can describe by other the scheme that does not depart from the technology of the present invention feature, and therefore changes within the scope of the present invention all or that be equal in the scope of the invention are all included in the invention.
Embodiment 1:
Be prepared as follows Ti
xnb
1-xse
2nano material:
(1) raw material is taken to Nb powder, Se powder by certain mol proportion, Ti powder takes respectively the percent value of corresponding (Nb+Ti) total molar mass by x value.Wherein x value get respectively 0% Sample A and x get 5% sample B, (Nb+Ti)/Se mol ratio is 1:2.2;
(2) Stainless Steel Ball that is 10mm by diameter is put into ball grinder for 1:10 mixes in mass ratio, seal and extract air in tank, repeatedly pass into and extract argon gas 5 times, by ball grinder put into planetary ball mill with the rotating speed of 200r/min to ball grinder powder ball milling 24h to mix;
(3) the question response thing mixing is packed in the hyaline-quartz pipe of one end sealing, utilize acetylene heated quarty tube to molten state, by silica tube gradually drawing-down become an aperture, after silica tube is vacuumized, pass into argon shield, repeatedly with acetylene heating, hyaline-quartz pipe is thoroughly being sealed after 5 times;
(4) the hyaline-quartz pipe that reactant is housed is put in reactor (prevent silica tube from blowing), then puts it in tubular oven, be heated to 750 ℃ with the speed of 5 ℃/min from room temperature, insulation 1h, cools to room temperature with the furnace;
(5) in silica tube, generate Ti
xnb
1-xse
2nano material, opens hyaline-quartz pipe and can obtain Sample A and sample B.
The nano material that the present embodiment is obtained is carried out X-ray diffraction analysis, and the XRD figure that obtains Sample A, B is composed as shown in Figure 1; The scanning electron microscope (SEM) of A as shown in Figure 2; The SEM of B schemes as shown in Figure 3,4.The Ti that adopts the present invention to prepare
xnb
1-xse
2nano material, is hexagonal nano-flake sheet before doping, the about 2um～3um of radial dimension, the about 800nm～1um of thickness; After doping, be nano belt and nanometer sheet, tens microns of nanometer belt lengths, wide about 200nm, thick about 30nm.
By the Ti of embodiment 1
xnb
1-xse
2nano material Sample A (with 5% massfraction) and B (respectively according to 3%, 5%, 7% massfraction) add in HVI500 base oil, and ultrasonic wave is disperseed, and is configured to muddy oil sample.On UMT-2 type friction wear testing machine, investigate base oil and contain different mass mark Ti
xnb
1-xse
2the tribological property of additive oil sample.In experiment, use 45
#the bead that steel disk and 440C diameter are 4mm turns round friction, and load is 10-50N, experimental period 25min.
The Sample A of gained and containing the oil sample of different mass mark B the frictional coefficient result under different loads as shown in Figure 5, Ti prepared by visible the present invention
xnb
1-xse
2nano material and NbSe
2compare, there is better friction and wear behavior as base oil additive.
Although illustrated and described embodiments of the invention, for the ordinary skill in the art, be appreciated that without departing from the principles and spirit of the present invention and can carry out multiple variation, modification, replacement and modification to these embodiment, scope of the present invention is limited by claims and equivalent thereof.
Claims (9)
1. a Ti
xnb
1-xse
2the preparation method of nano material, is characterized in that: the concrete steps of the method are as follows:
(1) configuration raw mixture: press Ti
xnb
1-xse
2stoichiometry claim Ti powder, by Se:(Nb+Ti) mol ratio of=2～3:1 takes Nb powder and Se powder, mix;
(2) take the Stainless Steel Ball of 10mm in the ratio of the weight ratio 8～10:1 of ball material and raw mixture, the raw material and the Stainless Steel Ball that in step (1), mix are put into planetary ball mill, after vacuumizing, pass into argon gas, under argon shield, carry out ball milling, ball milling 24h;
(3) the question response thing of drying step (2) gained installs in silica tube, deflate and pass into argon gas, by putting into tubular react furnace after silica tube sealing, being heated to 650 ℃～800 ℃ with the speed of 5 ℃/min, after insulation 0.5h～2h, cool to room temperature with the furnace, obtain Ti
xnb
1-xse
2nano material, wherein x is 1%～5%.
2. preparation method as claimed in claim 1, is characterized in that: in step (1), by Se:(Nb+Ti) mol ratio of=2.2:1 takes Nb powder and Se powder.
3. preparation method as claimed in claim 1, is characterized in that: in step (1), Nb powder is 200 orders, Ti powder 300 orders, Se powder 300 orders.
4. preparation method as claimed in claim 1, is characterized in that: in step (2), take the Stainless Steel Ball of 10mm in the ratio of the weight ratio 10:1 of ball material and raw mixture.
5. preparation method as claimed in claim 1, is characterized in that: in step (2), and the speed 200r/min of star formula ball mill.
6. preparation method as claimed in claim 1, is characterized in that: in step (3), be heated to 750 ℃ with the speed of 5 ℃/min.
7. preparation method as claimed in claim 1, is characterized in that: in step (3), and insulation 1h.
8. preparation method as claimed in claim 1, is characterized in that: in step (3), the diameter of quartz glass tube is 15mm.
9. the prepared Ti of preparation method as described in claim 1-8 any one
xnb
1-xse
2nano material is as the purposes of lubricating oil additive.
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104988375A (en) * | 2015-07-30 | 2015-10-21 | 清远先导材料有限公司 | Tellurium manganese iron alloy and preparing method thereof |
| CN112447940A (en) * | 2019-09-04 | 2021-03-05 | 通用汽车环球科技运作有限责任公司 | Titanium niobium oxide and titanium oxide composite anode material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4021968A1 (en) * | 1989-07-10 | 1991-01-17 | Central Glass Co Ltd | METHOD FOR CLEANING CARBON PARTS IMPROVED WITH INORGANIC DEPOSITS |
| JP2003024790A (en) * | 2001-04-30 | 2003-01-28 | Rohm & Haas Co | Improved catalyst |
| CN102923777A (en) * | 2012-11-08 | 2013-02-13 | 镇江中孚复合材料有限公司 | Preparation method of six-square-piece shaped selenium doping disulfide niobium |
-
2013
- 2013-12-12 CN CN201310669217.7A patent/CN103771354A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4021968A1 (en) * | 1989-07-10 | 1991-01-17 | Central Glass Co Ltd | METHOD FOR CLEANING CARBON PARTS IMPROVED WITH INORGANIC DEPOSITS |
| JP2003024790A (en) * | 2001-04-30 | 2003-01-28 | Rohm & Haas Co | Improved catalyst |
| CN102923777A (en) * | 2012-11-08 | 2013-02-13 | 镇江中孚复合材料有限公司 | Preparation method of six-square-piece shaped selenium doping disulfide niobium |
Non-Patent Citations (3)
| Title |
|---|
| JIAQING LIANG ET AL.: "Preparation and tribological properties of Nb1-xTixSe2 micro/nanoparticles", 《ADVANCED MATERIALS RESEARCH》 * |
| 胡志立等: "Nb1-xWxSe2的制备及其摩擦学性能研究", 《真空科学与技术学报》 * |
| 胡志立等: "W掺杂NbSe2及其Cu基复合材料摩擦学性能研究", 《无机化学学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104988375A (en) * | 2015-07-30 | 2015-10-21 | 清远先导材料有限公司 | Tellurium manganese iron alloy and preparing method thereof |
| CN112447940A (en) * | 2019-09-04 | 2021-03-05 | 通用汽车环球科技运作有限责任公司 | Titanium niobium oxide and titanium oxide composite anode material |
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Application publication date: 20140507 |