CN102923677A - Method for preparing NbSe2 nano material - Google Patents
Method for preparing NbSe2 nano material Download PDFInfo
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- CN102923677A CN102923677A CN2012104432077A CN201210443207A CN102923677A CN 102923677 A CN102923677 A CN 102923677A CN 2012104432077 A CN2012104432077 A CN 2012104432077A CN 201210443207 A CN201210443207 A CN 201210443207A CN 102923677 A CN102923677 A CN 102923677A
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Abstract
The invention discloses a method for preparing a NbSe2 nano material. The method comprises steps of placing simple substance Nb powder, simple substance Se powder and NaCl in a ball milling tank, conducting alcohol wet grinding, and mixing and fining the simple substance Nb powder, the simple substance Se powder and the NaCl completely; after ball milling, placing sediment to an oven for drying; and placing the dried sediment to a reaction kettle, subjecting the dried sediment to high-temperature vacuum sintering and obtaining the NbSe2 nano material which has good performance and a good shape. A proper NaCl medium is added during reaction, the shape and the structure of product diselenide niobium are controlled through good transmission performance of the medium at the high temperature and control of content, reaction temperature and reaction time of the medium, the method is simple, the operation is easy, and the prepared NbSe2 nano material has good lubricating property, good electric conductivity and a good shape. The method is practical and economical.
Description
Technical field
The present invention relates to have two selenizing niobium particle preparing technical fields of better pattern, be specifically related to a kind of NbSe with high lubricity and conductivity nano material
2The preparations of nanomaterials method.
Background technology
The development of nano material technology of preparing rapidly, formed multiple relatively ripe preparation method, mainly comprise: solid phase method (mechanical milling method, solid reaction process), physical vaporous deposition (PVD method, comprise: thermal evaporation PVD method, plasmaassisted PVD method, laser ablation), chemical Vapor deposition process (CVD), liquid-phase synthesis process (comprise the precipitator method, solvent-thermal method, freeze-drying, also make cryochemistry synthesis method, sol-gel method, microemulsion method, microwave-assisted synthesis method and ultrasonic wave assist synthesis method) etc.Fused salt synthesis method (Molten Salt Synthesis) is a kind of short-cut method that is used for preparing oxide compound and stupalith.It can be implemented under the lower temperature of reaction or the short interior short-cut method for preparing the anisotropy powder of specific components of reaction times.In fused salt was synthetic, the melt of salt had played the effect of solvent and reaction medium.Compare with traditional methods such as solid phase, utilize molten-salt growth method synthesizing inorganic nano material to mainly contain following advantage:
(1) can obviously reduce synthesis temperature and Reaction time shorten, this can be summed up as because the formation of the melt of salt strengthens the flowability of reacted constituent in liquid phase, and rate of diffusion significantly improves; Because fused salt is applied between the powder granule of generation, stop the mutual reunion between the particle, so the powder structure that molten-salt growth method makes is even simultaneously, without reunion, or only has weakly agglomerated body to exist.
(2) can more easily control the shape and size of powder by molten-salt growth method, this can be relevant with the surface and interface between reactant and the salt-melting, because surface and interface can have the trend that reduces, finally causes the synthetic powder of molten-salt growth method to have specific pattern.The factor that affects the powder shape that molten-salt growth method synthesizes mainly comprises kind and the consumption of used salt, temperature of reaction and time etc.By changing these conditions, can make the anisotropy powder of specified shape.
(3) the molten-salt growth method suitability is very strong, almost to all materials, comprises the compound higher with synthesis temperature of many infusibilities, and various oxide ceramics with complicated ingredient, can both find some suitable fused salts, therefrom it is grown out.In addition, molten-salt growth method also can be conducive to the removing of impurity in reaction process and cleaning process subsequently, form highly purified reaction product therefore, and molten-salt growth method is a kind of comparatively simple method of synthetic anisotropy inorganic powder.But current the method also is not applied in the middle of the preparation of two selenizing niobiums.
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
2Preparations of nanomaterials method, method are simply and very effective, and the product of preparation has high lubricity and conductivity nano material.
Technical scheme: for achieving the above object, the technical solution used in the present invention is as follows:
A kind of NbSe
2The preparations of nanomaterials method may further comprise the steps:
(1) get simple substance Nb powder, simple substance Se powder and NaCl put into ball grinder, carry out the alcohol wet-milling, make it fully mix refinement;
(2) after ball milling is finished throw out being put into baking oven dries;
(3) will dry later throw out and put into reactor and carry out the high-temperature vacuum sintering, can obtain the NbSe of high-performance and good pattern
2Nano material.
The Nb powder that adds in the step (1) and the total mass of Se powder are 2 g, and wherein, the mol ratio of Nb and Se is 1:2.3～3.0.
In the step (1), the mass ratio of the total mass of the NaCl that adds and Nb powder and Se powder is 1:2～4.
The NbSe of gained
2Nano material thickness is 100～500 nm.
In the step (1), Ball-milling Time is 2.0～24 h, and the preferred spheres time consuming is 12 h.
In the step (3), sintering time is 0.5～8 h, and preferred sintering time is 2～4 h.
In the step (3), firing temperature is 600～800 ℃, and preferred firing temperature is 700-800 ℃.
As everyone knows, the lubricity of solid lubricant mainly depends on crystal morphology and the internal structure with lubricant, in the reaction of solid simple substance selenium powder and the synthetic two selenizing niobiums of niobium powder, the two selenizing niobium patterns that ordinary method generates by control reaction times and controlling reaction temperature.And present method has added an amount of sodium chloride medium in reaction, by this medium good transmission performance at high temperature by control agent content and the temperature and time of reaction control pattern and the structure that generates product two selenizing niobiums, therefore can prepare and have high lubricity and excellent conductive performance and have the NbSe2 nano material of better pattern.
Beneficial effect: compared with prior art, the major advantage that the present invention has comprises: present method has added an amount of sodium chloride medium in reaction, control pattern and the structure that generates product two selenizing niobiums by this medium good transmission performance at high temperature by the content of control agent and the temperature and time of reaction, method is simple, easily operation, prepared NbSe2 nano material has high lubricity and excellent conductive performance and has better pattern.Have good practicality and economy.
Description of drawings
Fig. 1 is NbSe in the example 1
2The XRD spectra of nano material;
Fig. 2 is NbSe in the example 1
2The SEM figure of nano material;
Fig. 3 is NbSe in the example 1
2The TEM figure of nano material.
Embodiment
Further illustrate the present invention below in conjunction with specific embodiment, 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
Take by weighing the 0.5639gNb powder, 1.4362gSe powder and 4.000gNaCl mix and put into ball grinder, add simultaneously the alcohol of 100 mL in ball grinder, and its mixture is carried out the mixing and ball milling of 12h in planetary ball mill, make its abundant refinement and mixing.After mixing is finished mixture is put into baking oven and carry out the 12h oven dry, then will dry later mixture and put into reactor at 750 ℃ of lower sintering 2h of high temperature sintering furnace, from reactor, take out sinter, obtain the NbSe of high-performance and good pattern
2Nano material.As can be seen from Figure 1 with NbSe
2Standard diagram contrast degree of agreement is very high.Having generated thickness among Fig. 2 is the sheet of 500nm, and the relatively smooth sheet layer material NbSe in the relative homogeneous of thickness surface
2What can find out its generation among Fig. 3 is six side's chip architectures, coincide with the SEM picture.
Embodiment 2
Take by weighing the 0.5639gNb powder, 1.4362gSe powder and 4.000gNaCl mix and put into ball grinder, add simultaneously an amount of alcohol in ball grinder, and its mixture is carried out the mixing and ball milling of 12h in planetary ball mill, make its abundant refinement and mixing.After mixing is finished mixture is put into baking oven and carry out the 12h oven dry, then will dry later mixture and put into reactor at 800 ℃ of lower sintering 2h of high temperature sintering furnace, from reactor, take out sinter, obtain the NbSe of high-performance and good pattern
2Nano material.
Embodiment 3
Take by weighing the 0.5639gNb powder, 1.4362gSe powder and 4.000gNaCl mix and put into ball grinder, add simultaneously an amount of alcohol in ball grinder, and its mixture is carried out the mixing and ball milling of 6h in planetary ball mill, make its abundant refinement and mixing.After mixing is finished mixture is put into baking oven and carry out the 12h oven dry, then will dry later mixture and put into reactor at 750 ℃ of lower sintering 2h of high temperature sintering furnace, from reactor, take out sinter, obtain the NbSe of high-performance and good pattern
2Nano material.
Embodiment 4
Take by weighing 0.6789 gNb powder, 1.3229 gSe powder and 4.000gNaCl mix and put into ball grinder, add simultaneously an amount of alcohol in ball grinder, and its mixture is carried out the mixing and ball milling of 12h in planetary ball mill, make its abundant refinement and mixing.After mixing is finished mixture is put into baking oven and carry out the 12h oven dry, then will dry later mixture and put into reactor at 600 ℃ of lower sintering 2h of high temperature sintering furnace, from reactor, take out sinter, obtain the NbSe of high-performance and good pattern
2Nano material.
Embodiment 5
Take by weighing 0.6789 gNb powder, 1.3229 gSe powder and 8.000gNaCl mix and put into ball grinder, add simultaneously an amount of alcohol in ball grinder, and its mixture is carried out the mixing and ball milling of 12h in planetary ball mill, make its abundant refinement and mixing.After mixing is finished mixture is put into baking oven and carry out the 12h oven dry, then will dry later mixture and put into reactor at 750 ℃ of lower sintering 4h of high temperature sintering furnace, from reactor, take out sinter, obtain the NbSe of high-performance and good pattern
2Nano material.
Claims (10)
1. NbSe
2The preparations of nanomaterials method is characterized in that, may further comprise the steps:
(1) get simple substance Nb powder, simple substance Se powder and NaCl put into ball grinder, carry out the alcohol wet-milling, make it fully mix refinement;
(2) after ball milling is finished throw out being put into baking oven dries;
(3) will dry later throw out and put into reactor and carry out the high-temperature vacuum sintering, can obtain the NbSe of high-performance and good pattern
2Nano material.
2. NbSe according to claim 1
2The preparations of nanomaterials method is characterized in that: in the step (1), the Nb powder that adds and the total mass of Se powder are 2 g, and wherein, the mol ratio of Nb and Se is 1:2.3～3.0.
3. NbSe according to claim 1
2The preparations of nanomaterials method is characterized in that: in the step (1), and the NaCl that adds, with, the total mass of Nb powder and Se powder, mass ratio is 1:2～4.
4. NbSe according to claim 1
2The preparations of nanomaterials method is characterized in that: the NbSe of gained
2Nano material thickness is at 100～500 nm.
5. NbSe according to claim 1
2The preparations of nanomaterials method is characterized in that: in the step (1), Ball-milling Time is 2.0～24 h.
6. according to claim 1 or 3 described NbSe
2The preparations of nanomaterials method is characterized in that: in the step (1), Ball-milling Time is 12 h.
7. NbSe according to claim 1
2The preparations of nanomaterials method is characterized in that: in the step (3), sintering time is 0.5～8 h.
8. NbSe according to claim 1 or 5
2The preparations of nanomaterials method is characterized in that: in the step (3), sintering time is 2～4 h.
9. NbSe according to claim 1
2The preparations of nanomaterials method is characterized in that: in the step (3), firing temperature is 600～800 ℃.
10. according to claim 1 or 7 described NbSe
2The preparations of nanomaterials method is characterized in that: in the step (3), firing temperature is 700～800 ℃.
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Cited By (5)
| 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 |
| CN104962235A (en) * | 2015-05-20 | 2015-10-07 | 常州机电职业技术学院 | Preparation method of niobium diselenide or niobium disulphide/carbon wear-resistant nano composite material |
| CN105399060A (en) * | 2015-09-28 | 2016-03-16 | 中国科学院重庆绿色智能技术研究院 | Method for rapid synthesis of two-dimensional layered nanometer material |
| CN108975288A (en) * | 2018-07-25 | 2018-12-11 | 西南大学 | A kind of NbSe2Preparation method of electrode material and products thereof and application |
| CN113560152A (en) * | 2021-07-26 | 2021-10-29 | 中国科学院兰州化学物理研究所 | Surface lubrication treatment method for vacuum current-carrying sliding electric contact component |
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| CN101800089A (en) * | 2009-10-28 | 2010-08-11 | 无锡润鹏复合新材料有限公司 | Nanometer NbSe2 copper-base solid self-lubricating composite material and preparation method thereof |
| CN101798070A (en) * | 2009-10-28 | 2010-08-11 | 无锡润鹏复合新材料有限公司 | NbSe2 nano lubricating wire and preparation method thereof |
| CN102703162A (en) * | 2012-05-14 | 2012-10-03 | 无锡润鹏复合新材料有限公司 | Preparation method of NbSe2/C nanometer composite materials |
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Patent Citations (3)
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| CN101800089A (en) * | 2009-10-28 | 2010-08-11 | 无锡润鹏复合新材料有限公司 | Nanometer NbSe2 copper-base solid self-lubricating composite material and preparation method thereof |
| CN101798070A (en) * | 2009-10-28 | 2010-08-11 | 无锡润鹏复合新材料有限公司 | NbSe2 nano lubricating wire and preparation method thereof |
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Cited By (7)
| 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 |
| CN104962235A (en) * | 2015-05-20 | 2015-10-07 | 常州机电职业技术学院 | Preparation method of niobium diselenide or niobium disulphide/carbon wear-resistant nano composite material |
| CN105399060A (en) * | 2015-09-28 | 2016-03-16 | 中国科学院重庆绿色智能技术研究院 | Method for rapid synthesis of two-dimensional layered nanometer material |
| CN108975288A (en) * | 2018-07-25 | 2018-12-11 | 西南大学 | A kind of NbSe2Preparation method of electrode material and products thereof and application |
| CN108975288B (en) * | 2018-07-25 | 2020-06-30 | 西南大学 | NbSe2Preparation method of electrode material, product and application thereof |
| CN113560152A (en) * | 2021-07-26 | 2021-10-29 | 中国科学院兰州化学物理研究所 | Surface lubrication treatment method for vacuum current-carrying sliding electric contact component |
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