CN102923777A - Preparation method of six-square-piece shaped selenium doping disulfide niobium - Google Patents
Preparation method of six-square-piece shaped selenium doping disulfide niobium Download PDFInfo
- Publication number
- CN102923777A CN102923777A CN2012104434528A CN201210443452A CN102923777A CN 102923777 A CN102923777 A CN 102923777A CN 2012104434528 A CN2012104434528 A CN 2012104434528A CN 201210443452 A CN201210443452 A CN 201210443452A CN 102923777 A CN102923777 A CN 102923777A
- Authority
- CN
- China
- Prior art keywords
- powder
- niobium
- disulfide
- preparation
- selenium doping
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Lubricants (AREA)
Abstract
The invention discloses a preparation method of six-square-piece shaped selenium doping disulfide niobium. The preparation method of the six-square-piece shaped selenium doping the disulfide niobium includes that (1) Se powder, S powder and Nb powder are taken, according to ball-powder weight ratio of 10:1, the Se powder, the S powder and the Nb powder are mixed, put in a ball-milling jar, protected by Ar air, rotates at a speed of 200 revolutions per minute (RMP), and milled for 9 to 10 hours in the ball-milling bar; and (2) after ball-milling mixing uniformity, a ready reactant is dried, put in a steel reaction kettle, sealed, and put in a tubular reaction furnace to be heated to 750 DEG C, and after two-hour heat preservation, the reactant naturally cools with the reaction furnace to room temperature, and therefore, Se doping NbS2 is obtained. The selenium doping the disulfide niobium is combined through a solid phase method, a craft process is green and pollution-free, safety of drugs is guaranteed, and an experimental method is simple and easy to operate. The selenium doping the disulfide niobium which is prepared by the preparation method forms a uniform hexagonal nanosheet shaped structure due to the fact that the selenium doping the disulfide niobium has a similar layered structure of pure disulfide niobium, but the feature of the disulfide niobium is different from a nanoribbon shaped structure of the pure disulfide niobium. The uniform hexagonal nanosheet shaped structure is good in dispersity and excellent in tribology performance, and the radial dimension of the uniform hexagonal nanosheet shaped structure is about one micrometer, the thickness of the uniform hexagonal nanosheet shaped structure is about 50 nanometers, and radius-thickness ratio of the uniform hexagonal nanosheet shaped structure is greater than 20.
Description
Technical field
The present invention relates to the solid lubrication technical field of nano material, be specifically related to a kind of preparation method of hexagonal flake selenium doping curing niobium.
Background technology
Development along with the industrial technology of modernization, lubricating oil can not be suitable under some specific environment, particularly under the environment of this harshness in outer space owing to easily evaporating, easily decomposing or crosslinked shortcoming, because the vapour pressure of mineral lubricating oils is very high, is unsuitable for 10
-1Use for a long time in the ultrahigh vacuum(HHV) more than the Pa, and in the high-altitude of 1000km, its vacuum tightness just can reach 10
-2~ 10
-3Pa.These special environment have surmounted the operating limit of lubricating oil, and this just forces people to remove to seek new lubricant.
Solid lubricant can satisfy under the special operation conditions such as high loading, high vacuum, high/low temperature, severe radiation and deep-etching lubricated requirement, can adapt to complicated Working environment, for mechanical means realize maximizing, microminiaturized, at a high speed, heavy duty and automatically control etc. created favourable condition.Along with nanoscale science and technology in mondial rise, the demand of the development of recent test technology and hi-tech development, the preparation of nano level friction materials and the research of tribological property thereof not only become in recent years one of most active forward position, tribology research field, also enjoy the concern of the research circle such as Materials science, physics and chemistry.
Transition-metal dichalcogenide is widely used in the industries such as petrochemical complex production desulfurization catalyst, elastic coating material, hydrogen storage material, storage lithium electrode material because having unique character, particularly nano material is as antifriction additive, in friction process, not only can form the film that one deck is easily sheared at friction surface, reduce frictional coefficient, and can also carry out filling up and repairing to a certain degree to friction surface, become one of focus of current Materials science research, on tribology, will have broad application prospects.Nano-solid lubricant preparation method is also varied, because solid phase reaction process is simple, preparation cost is low, and the product purity of preparation is high, favorable reproducibility, and reactant is pollution-free, so solid state reaction is extensively adopted by experimental study.
Studies show that to have the transient metal sulfide MS of unique enclosed construction
2(M=Nb, W, Mo etc.) nano material not only has good chemical stability, also has excellent lubricity.NbS
2The same MoS of crystalline structure structure
2Similar, have typical laminate structure, because NbS
2Natural mineral extremely rare, make its price be higher than MoS far away
2, its application is restricted, and therefore therefore the corresponding research work of carrying out has also just been lacked, and strengthens the research of nanometer sulfide is had very large realistic meaning.The NbS of common report
2Basic is some nano wire nano-tube nano rods etc.
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 preparation method of hexagonal flake selenium doping curing niobium, process for solid phase synthesis is simple, green non-pollution, the selenium doping NbS of gained
2Nano-hexagonal sheet radial dimension is 1um approximately, the about 50nm of thickness, and radius-thickness ratio has the tribological property that is better than pure curing niobium greater than 20.
Technical scheme: for achieving the above object, the technical solution used in the present invention is as follows:
A kind of preparation method of hexagonal flake selenium doping curing niobium may further comprise the steps:
(1) get Se powder, S powder and Nb powder, mix by ratio of grinding media to material 10:1 and put into ball grinder, the protection of Ar gas is lower, rotating speed 200rpm, ball milling 9 ~ 10h; The mol ratio of S powder and Nb powder is 2:1, and the S powder is excessive 40%, and the mol ratio of Se and S powder is 5:95;
(2) the question response thing after ball milling is mixed is dry, puts into steel bomb, and sealing is put into tubular react furnace and is heated to 750 ℃, naturally cools to room temperature with stove behind the insulation 2h, obtains the NbS that Se mixes
2
In the step (2), heat-up rate is 20 ℃/min.
Wherein, said S excessive 40% refers to 40% of the excessive S of S and the total amount of substance of Nb.The mol ratio of said Se and S is the ratio that 5:95 refers to Se and total amount of substance of all S that add, comprises excessive 40%.Be: when the Nb amount of substance is 2mol, then the S amount of substance is 4mol+(4mol+2mol) * 40%=6.4mol.The amount of substance of Se is 6.4mol*5/95.
The present invention adopt doping 5%(Se account for Se and the total amount of substance of S 5%) the Se solid phase prepare NbS
2, make NbS
2By tabular pattern novelty and the very uniform nano-sheet of being transformed into of nano belt, the frictional behaviour test shows that the nanometer sheet performance after the doping is far superior to the nanometer band plate.
Beneficial effect: compared with prior art, the major advantage that the present invention has comprises: the present invention synthesizes selenium doping curing niobium with solid phase method, the technological process green non-pollution, and drug safety is easy to get, and experimental technique is simple to operation.The prepared selenium doping curing niobium of the present invention is to have and the similar laminate structure of pure curing niobium, but because its pattern is different from the nano strip structure of pure curing niobium, and the hexagonal nano sheet structure of formation homogeneous, it is better dispersed, radial dimension is 1um approximately, the about 50nm of thickness, and radius-thickness ratio is greater than 20, have more excellent tribological property, have good practicality and economy.
Description of drawings
Fig. 1 is scanning electron microscope (SEM) figure of the pure curing niobium of embodiment 1 preparation;
Fig. 2 is the SEM figure of the selenium doping curing niobium of embodiment 2 preparations;
Fig. 3 is the XRD diffractogram of selenium doping curing niobium of pure curing niobium, embodiment 2 preparations of embodiment 1 preparation;
Fig. 4 is the frictional coefficient figure of selenium doping curing niobium of pure curing niobium, embodiment 2 preparations of embodiment 1 preparation.
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.
Embodiment 1
S powder and Nb powder are taken by weighing (S excessive 40%) by their stoichiometric ratio, and the Stainless Steel Ball of diameter 8mm mixes by ratio of grinding media to material 10:1 and put into ball grinder, vacuumize and pass into Ar gas in the tank, 5 times repeatedly, carry out ball milling 9h with rotating speed 200rpm.Put into steel bomb after the question response thing drying after again ball milling being mixed, then sealing puts it into and is heated to 750 ℃ in the tubular react furnace, and 20 ℃ of temperature rise rate per minutes naturally cool to room temperature with stove behind the insulation 2h, obtain NbS
2Sample.
S, Se powder and Nb powder are taken by weighing (S, Se total amount excessive 40% by their stoichiometric ratio, the Se powder make its account for S and the total amount of substance of Se 5%), put into ball grinder with the Stainless Steel Ball of diameter 8mm by ratio of grinding media to material 10:1 mixing, vacuumize and pass into Ar gas in the tank, 5 times repeatedly, carry out ball milling 9h with rotating speed 200rpm.Put into steel bomb after the question response thing drying after again ball milling being mixed, then sealing puts it into and is heated to 750 ℃ in the tubular react furnace, and 20 ℃ of temperature rise rate per minutes naturally cool to room temperature with stove behind the insulation 2h, obtain the NbS that Se mixes
2
Embodiment 3
The pure curing niobium of embodiment 1 preparation, the selenium doping curing niobium of embodiment 2 preparations are carried out electron-microscope scanning, and the result respectively as depicted in figs. 1 and 2.Adopt the selenium doping NbS of the present invention's preparation
2Hexagonal flake structure (Fig. 2) for the size homogeneous is different from pure NbS
2Nano belt structure (Fig. 1), selenium doping NbS
2Dispersed better radial dimension is 1um approximately, the about 50nm of thickness, radius-thickness ratio is greater than 20.Selenium doping curing niobium is to have and the similar laminate structure of pure curing niobium, but because its pattern is different from the nano strip structure of pure curing niobium, and forming the hexagonal nano sheet structure of homogeneous, it has more excellent tribological property.
The pure curing niobium of embodiment 1 preparation, the selenium doping curing niobium of embodiment 2 preparations are carried out the XRD diffraction experiment, the result as shown in Figure 3, as seen, Se doping NbS
2Has more excellent tribological property.
The NbS that embodiment 1 is prepared respectively
2, the prepared Se doping NbS of embodiment 2
2Be 2% to add in the Witco 70 by massfraction, with neat liquid paraffin oil sample as a comparison, with span80 as dispersion agent, carry out frictional experiment at UMT-2 ball-dish friction and wear tester behind the supersound process 30min, test experiments load is divided the frictional coefficient under 0.4k, 0.6kg, 1kg, 3kg, the 5kg, resulting experimental result as shown in Figure 4, as seen, Se doping NbS
2Has more excellent tribological property.
Claims (2)
1. the preparation method of a hexagonal flake selenium doping curing niobium is characterized in that, may further comprise the steps:
(1) get Se powder, S powder and Nb powder, mix by ratio of grinding media to material 10:1 and put into ball grinder, the protection of Ar gas is lower, rotating speed 200rpm, ball milling 9 ~ 10h; The mol ratio of S powder and Nb powder is 2:1, and the S powder is excessive 40%, and the mol ratio of Se and S powder is 5:95;
(2) the question response thing after ball milling is mixed is dry, puts into steel bomb, and sealing is put into tubular react furnace and is heated to 750 ℃, naturally cools to room temperature with stove behind the insulation 2h, obtains the NbS that Se mixes
2
2. the preparation method of hexagonal flake selenium doping curing niobium according to claim 1, it is characterized in that: in the step (2), heat-up rate is 20 ℃/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210443452.8A CN102923777B (en) | 2012-11-08 | 2012-11-08 | Preparation method of six-square-piece shaped selenium doping disulfide niobium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210443452.8A CN102923777B (en) | 2012-11-08 | 2012-11-08 | Preparation method of six-square-piece shaped selenium doping disulfide niobium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102923777A true CN102923777A (en) | 2013-02-13 |
| CN102923777B CN102923777B (en) | 2014-10-22 |
Family
ID=47638741
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210443452.8A Expired - Fee Related CN102923777B (en) | 2012-11-08 | 2012-11-08 | Preparation method of six-square-piece shaped selenium doping disulfide niobium |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102923777B (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103627922A (en) * | 2013-12-03 | 2014-03-12 | 江苏大学 | Ternary alloy self-lubricating composite material and preparation method thereof |
| CN103641078A (en) * | 2013-12-03 | 2014-03-19 | 江苏大学 | Preparation method of solid lubricating sulfur niobium selenide nano sheet |
| CN103771354A (en) * | 2013-12-12 | 2014-05-07 | 江苏大学 | Preparation method and application of TixNb1-xSe2 nanomaterials |
| CN103922293A (en) * | 2014-04-15 | 2014-07-16 | 江苏大学 | Preparation method of Nb<1-x>Ta<x>Se<2> nanomaterial |
| CN105154195A (en) * | 2015-08-27 | 2015-12-16 | 中国科学院兰州化学物理研究所 | Extreme pressure complex grease composition |
| CN105836801A (en) * | 2016-03-07 | 2016-08-10 | 重庆工业职业技术学院 | Three-dimensional porous NbS2 nano-material, and preparation method and application thereof |
| CN106590818A (en) * | 2016-10-20 | 2017-04-26 | 江苏大学 | Nano composite material serving as lubricating oil additive and preparation method |
| CN107539964A (en) * | 2017-09-30 | 2018-01-05 | 江苏理工学院 | A kind of selenizing molybdenum powder body material of hexagonal flake two and preparation method thereof |
| CN109306498A (en) * | 2018-10-26 | 2019-02-05 | 浙江大学 | The preparation method and product of a kind of two-dimensional ultrathin curing niobium nanometer sheet and application |
| CN111188024A (en) * | 2020-02-14 | 2020-05-22 | 安徽大学 | Method for preparing niobium diselenide nanosheet array with photoelectric response based on chemical vapor deposition |
| CN111892982A (en) * | 2020-08-21 | 2020-11-06 | 北京化工大学 | Preparation method of nitrogen-doped nano lubricating material |
| CN113149076A (en) * | 2021-05-27 | 2021-07-23 | 吉林大学 | Preparation method of phosphorus-selenium co-doped niobium disulfide nano material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1413910A (en) * | 2002-11-27 | 2003-04-30 | 南开大学 | Transition metal sulfied nano-pipe and preparation process and its application |
-
2012
- 2012-11-08 CN CN201210443452.8A patent/CN102923777B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1413910A (en) * | 2002-11-27 | 2003-04-30 | 南开大学 | Transition metal sulfied nano-pipe and preparation process and its application |
Non-Patent Citations (2)
| Title |
|---|
| YI DING等: "First principles study of structural,vibrational and electronic properties of graphene-like MX2 (M=Mo,Nb,W,Ta;X=S,Se,Te) monolayers", 《PHYSICA B》, 23 March 2011 (2011-03-23), pages 2254 - 2260, XP028407992, DOI: doi:10.1016/j.physb.2011.03.044 * |
| 丁建等: "NbSex微纳米材料的制备及其摩擦学性能", 《材料科学与工程学报》, vol. 28, no. 2, 30 April 2010 (2010-04-30), pages 212 - 216 * |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103641078A (en) * | 2013-12-03 | 2014-03-19 | 江苏大学 | Preparation method of solid lubricating sulfur niobium selenide nano sheet |
| CN103641078B (en) * | 2013-12-03 | 2015-11-18 | 江苏大学 | A kind of preparation method of solid lubrication sulphur selenizing niobium nanometer sheet |
| CN103627922B (en) * | 2013-12-03 | 2015-12-30 | 江苏大学 | A kind of ternary alloy self-lubricating composite and preparation method thereof |
| CN103627922A (en) * | 2013-12-03 | 2014-03-12 | 江苏大学 | Ternary alloy self-lubricating composite material and preparation method thereof |
| CN103771354A (en) * | 2013-12-12 | 2014-05-07 | 江苏大学 | Preparation method and application of TixNb1-xSe2 nanomaterials |
| CN103922293A (en) * | 2014-04-15 | 2014-07-16 | 江苏大学 | Preparation method of Nb<1-x>Ta<x>Se<2> nanomaterial |
| CN105154195B (en) * | 2015-08-27 | 2018-07-10 | 中国科学院兰州化学物理研究所 | A kind of extreme pressure compound lithium base grease composition |
| CN105154195A (en) * | 2015-08-27 | 2015-12-16 | 中国科学院兰州化学物理研究所 | Extreme pressure complex grease composition |
| CN105836801A (en) * | 2016-03-07 | 2016-08-10 | 重庆工业职业技术学院 | Three-dimensional porous NbS2 nano-material, and preparation method and application thereof |
| CN106590818A (en) * | 2016-10-20 | 2017-04-26 | 江苏大学 | Nano composite material serving as lubricating oil additive and preparation method |
| CN107539964A (en) * | 2017-09-30 | 2018-01-05 | 江苏理工学院 | A kind of selenizing molybdenum powder body material of hexagonal flake two and preparation method thereof |
| 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 |
| CN109306498A (en) * | 2018-10-26 | 2019-02-05 | 浙江大学 | The preparation method and product of a kind of two-dimensional ultrathin curing niobium nanometer sheet and application |
| CN111188024A (en) * | 2020-02-14 | 2020-05-22 | 安徽大学 | Method for preparing niobium diselenide nanosheet array with photoelectric response based on chemical vapor deposition |
| CN111892982A (en) * | 2020-08-21 | 2020-11-06 | 北京化工大学 | Preparation method of nitrogen-doped nano lubricating material |
| CN113149076A (en) * | 2021-05-27 | 2021-07-23 | 吉林大学 | Preparation method of phosphorus-selenium co-doped niobium disulfide nano material |
| CN113149076B (en) * | 2021-05-27 | 2022-07-01 | 吉林大学 | Preparation method of phosphorus-selenium co-doped niobium disulfide nano material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102923777B (en) | 2014-10-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102923777B (en) | Preparation method of six-square-piece shaped selenium doping disulfide niobium | |
| CN101792931B (en) | Metal sulfide single crystal material and preparation method | |
| Bai et al. | Unusual formation of ZnCo2O4 3D hierarchical twin microspheres as a high‐rate and ultralong‐life lithium‐ion battery anode material | |
| EP3893308B1 (en) | Inorganic sulfide solid electrolyte having high air stability, and preparation method and use thereof | |
| Zhang et al. | Facile synthesis of Sb2S3/MoS2 heterostructure as anode material for sodium-ion batteries | |
| Xu et al. | Rose flower-like NiCo2O4 with hierarchically porous structures for highly reversible lithium storage | |
| Wu et al. | SnS2 nanoparticle-integrated graphene nanosheets as high-performance and cycle-stable anodes for lithium and sodium storage | |
| CN103073060B (en) | Method for preparing hexagonal molybdenum disulfide nanosheet as anti-friction additive | |
| Jia et al. | ZnSe nanoparticles decorated with hollow N-doped carbon nanocubes for high-performance anode material of sodium ion batteries | |
| Zhao et al. | Improved dehydrogenation performance of LiBH4 by 3D hierarchical flower-like MoS2 spheres additives | |
| Zhang et al. | MoS2 coated hollow carbon spheres for anodes of lithium ion batteries | |
| Kim et al. | Supersonically sprayed rGO− Zn2SnO4 composites as flexible, binder-free, scalable, and high-capacity lithium ion battery anodes | |
| CN102992281A (en) | Nanometer flower-shaped MoSe2 and preparation method thereof | |
| CN102863025A (en) | Preparation method of piece-shaped tungsten disulfide nanometer lubricating oil additive | |
| CN102701283A (en) | Preparation method of tungsten disulfide nanorods | |
| CN112920880A (en) | Preparation method of 2D MOFs nanosheet-based lubricant | |
| CN103602362A (en) | Preparation method of ferrous disulfide-graphene composite nano lubricant | |
| Dai et al. | Si@ SnS2–Reduced Graphene Oxide Composite Anodes for High‐Capacity Lithium‐Ion Batteries | |
| CN104962340B (en) | Inorganic fullerene molybdenum disulfide/Graphene compounded lubricant and preparation method thereof | |
| CN109135890A (en) | A kind of modification of lubricating oils and preparation method thereof | |
| Feng et al. | Study on conductivity and tribological properties of polyaniline/molybdenum disulfide composites in lithium complex grease | |
| CN101798070A (en) | NbSe2 nano lubricating wire and preparation method thereof | |
| Shukla et al. | Ternary composite of methionine-functionalized graphene oxide, lanthanum-doped yttria nanoparticles, and molybdenum disulfide nanosheets for thin-film lubrication | |
| Yu et al. | Hybrid ZnSe‐SnSe2 Nanoparticles Embedded in N‐doped Carbon Nanocube Heterostructures with Enhanced and Ultra‐stable Lithium‐Storage Performance | |
| Dong et al. | C/Sn/RGO Nanocomposites as Higher Initial Coulombic Efficiency Anode for Sodium‐Ion Batteries |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20141022 Termination date: 20161108 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |