CN102703162A - Preparation method of NbSe2/C nanometer composite materials - Google Patents
Preparation method of NbSe2/C nanometer composite materials Download PDFInfo
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- CN102703162A CN102703162A CN2012101495197A CN201210149519A CN102703162A CN 102703162 A CN102703162 A CN 102703162A CN 2012101495197 A CN2012101495197 A CN 2012101495197A CN 201210149519 A CN201210149519 A CN 201210149519A CN 102703162 A CN102703162 A CN 102703162A
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Abstract
The invention relates to a preparation method of NbSe2/C nanometer composite materials. The method comprises the steps of taking Nb powder and Se powder as raw materials, performing hydrothermal synthesis with carbon source at low temperature, and preparing NbSe2/C nanometer composite materials with different shapes by changing proportion of the carbon source, hydrothermal synthesis time and temperature and so on. The experiment process of the preparation method is simple and easy to operate; the synthetic process is green and pollution-free; the prepared carbon-coated nanometer composite material is a novel solid lubricating and conducting material with high lubrication performance and conductivity.
Description
Technical field
The present invention relates to technical field of nano material, be specifically related to a kind of NbSe that has than high lubricating property and conductivity
2The preparation method of/C nano composite material.
Background technology
Because simple nano metal crystal grain is little, specific surface area is big, be easy to generate fast oxidizing reaction even spontaneous combustion take place, this big havoc its purity and stability in use, give this type material preparation, store with application and brought a very big difficult problem.Therefore, find that from Ruoff in 1993 and Tomita etc. the multi-layer graphene with good antioxidant property coats lanthanum carbide (LaC in arc evaporation graphite cigarette ash first
2/ C) since, aspects such as the clad nano metallic particles is synthetic at it, structure, character and potential application have obtained great achievement, have effectively promoted the development of new carbon, have enriched the research direction of nanosecond science and technology.But current carbon arc method technology still exists following problem: output is extremely low; Purity is low, and the graphite cigarette ash that the arc evaporation that contains in the product forms is difficult to isolation and purification; Graphite can form metallic carbide with many metals, like Cr
7C
3, SiC, TiC, Fe
7C
3, VC, WC etc., this selection and operation to inner nuclear material is had higher requirement.The existence of these situation has proposed great challenge to the scale preparation and the application of carbon arc law technology.
Current nano material preparation technical development is rapid; Formed multiple relatively sophisticated preparation method; Mainly comprise: solid phase method (mechanical milling method, solid reaction process), physical vaporous deposition (PVD method; Comprise: the auxiliary PVD method of thermal evaporation PVD method, plasma body, laser ablation method), 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 UW assist synthesis method) etc.
CN101944590A discloses the preparation method that a kind of carbon coats lithium titanate, and it may further comprise the steps: 1) take by weighing lithium source and titanium source, be scattered in zero(ppm) water or the deionized water; 2) add the long chain type aliphatic carboxylic acid, also dispersed with stirring is even to be heated to 30-100 ℃, obtains suspension liquid; 3) suspension liquid is changed in the reaction vessel of sealing heat, it is reacted under constant temperature; 4) after question response finishes,,, collect precursor with the mixed solution repetitive scrubbing of alcohol and water, centrifugal, dry with the reaction product cool to room temperature; And 5) precursor of collecting is put into the atmosphere furnace that is full of non-oxidizing gas and cure, the cooling back obtains carbon and coats lithium titanate.
CN101714634A provides a kind of microwave preparation of iron lithium phosphate of carbon coating; May further comprise the steps: the stoichiometric ratio in the iron lithium phosphate of preparation is obtained Li source compound, ferrous iron source compound and P source compound respectively as required, and adds microwave absorption, organic carbon source and liquid dispersant; The raw material that ball milling is obtained, and carry out drying treatment; Dried product is placed the microwave heating reaction chamber, in reaction chamber, feed shielding gas; To 550-850 ℃, feed carbon-source gas through microwave heating, pyrolysis carbon-source gas under 550-850 ℃ of temperature makes the iron lithium phosphate that carbon coats.The LiFePO 4 material that the present invention also provides a kind of carbon that makes according to the method described above to coat.
To the defective of carbon arc law technology, investigators the gas, liquid, solid of the conventional technology of preparing of nano material and organic cpds mutually charring process combine, develop the technology of preparing of multiple carbon encapsulated material.The carbon-coated nano material is as a kind of novel carbon composite nano-material, and its preparation and property research have become the research focus of material science.Because the compound method of inner nuclear material and the selection of carbon source material are flexible; And conventional carbonization temperature is gentle relatively; Usually in 500 ~ 1000 ℃ of scopes, equipment is simple, can realize scale preparation again; Therefore persons develop the method that carbon encapsulated material competitively adopts to become the current research, even part has realized suitability for industrialized production.
Summary of the invention
According to present domestic and international research present situation with consider the conventional lubrication material at the performance deficiency aspect the conductivity, the present invention proposes the NbSe that a kind of simply and very effectively preparation has high lubricity and excellent conductive performance and has better pattern
2The method of/C nano composite material.
Imagination of the present invention is that the method preparation through hydro-thermal has high lubricity and excellent conductive performance and has the NbSe of better pattern
2The method of/C nano composite material.As everyone knows, the lubricity of solid lubricant mainly depends on crystal morphology and the internal structure with lubricant, and conductivity wherein also depends on material internal electron distributions situation, and the contribution of organometallic conduction.In the traditional preparation method, just selenium powder and the mixing of niobium sphere of powder mill are carried out high-temperature firing then, obtain two higher selenizing niobium solid lubricants of purity, but its oxidation-resistance, and conductivity, bio-compatibility can not get good satisfying in application.Therefore need further to handle and obtain NbSe
2Nano structural material.
In order to achieve the above object, the present invention realizes through following technical scheme:
A kind of NbSe
2The preparation method of/C nano composite material may further comprise the steps:
(1) organic carbon source is dissolved in forms solution B in the solvent orange 2 A;
(2) niobium powder, selenium powder are taken by weighing by a certain percentage, be dissolved in and form solution D in the solvent C;
(3) solution D is joined in the solution B, process uniform aaerosol solution;
(4) under agitation condition, extraction agent is added in the above-mentioned aaerosol solution, obtain gelatinous throw out; Remove residual solvent, oven dry obtains throw out;
(5) obtain NbSe behind the throw out sintering after will drying
2/ C nano composite material.
Organic carbon source according to the invention is selected from the mixture of a kind of in glucose, lactose, resin, POE-g-MA or the long chain type aliphatic carboxylic acid or at least two kinds; Glucose for example; PAN, PAN/POE-g-MA/ resin, resin etc. all can be used as organic carbon source with embodiment of the present invention; Preferred PAN and/or POE-g-MA, further preferred POE-g-MA.
Solvent orange 2 A according to the invention is the mixture of a kind of in water, benzene,toluene,xylene or the THF or at least two kinds; For example water, benzene and/or toluene; The solvent that THF/toluene/YLENE etc. can dissolve corresponding organic carbon source all can be used for embodiment of the present invention; Those skilled in the art can select according to common practise of this area and the experience of oneself, and the present invention does not have particular restriction.The present invention is water, THF more preferably, further preferred THF.The mixture of a kind of in the preferred absolute ethyl alcohol of said solvent C, acetone, ether or the water or at least two kinds, absolute ethyl alcohol for example, acetone, acetone, acetone/water etc., further preferred absolute ethyl alcohol.
The niobium powder is the powder of metal niobium, and the dense oxidation film that generates on its surface has the valve metal character of unilateral conduction.Its oxide compound niobium oxides Nb
2O
5Be white powder, purity can reach 99.999%, is used to produce high-purity lithium niobate crystals and special optical glass additive.The stable chemical performance of this anode oxide film, resistivity are high, leakage current is little, specific inductivity is big.The niobium powder for capacitor electrical property is 3300 ~ 3600 μ FV/g than electric capacity, and leakage current value is 1 * 10
-3μ A/ (μ FV) adopts reduction-hydride process, sodium reduction etc. to produce, and is used to make electrolytic condenser and walkie-talkie and general industry electrical equipment.Selenium powder is powdery or particulate state, and outward appearance is pure, solid colour, and impurity such as no earth, stable components, moisture is even, and outward appearance is a grey black look hexagonal system metal, is dissolved in the vitriol oil, trichloromethane, is slightly soluble in dithiocarbonic anhydride, water insoluble, ethanol.Can be used for RF, the photographic exposure agent, metallurgical addition agent, petrochemical complex is made catalyzer, duplicates toner cartridge, the selenium photographic plate, alloy, and the pigment in plastics, paint, enamel and the glass etc.The scope of application: electronics, glass, pottery, chemistry, metallurgy, medical treatment and health care, environmental sanitation, industries such as RF.The ratio of niobium powder according to the invention, selenium powder is 1.0: 2.3 ~ 1.0: 3.0, for example 1.0: 2.32, and 1.0: 2.5,1.0: 2.58,1.0: 2.7,1.0: 2.86,1.0: 2.98 etc., further preferred 1.0: 2.5 ~ 1.0: 2.8, most preferably 1.0: 2.1.
Step according to the invention (1) is dissolved in organic carbon source in the solvent orange 2 A through magnetic agitation or ultrasonic.Other modes that can make organic carbon source be dissolved in solvent orange 2 A that those skilled in the art can be known all can be used for embodiment of the present invention, are preferred and unrestricted here.For example, organic carbon source is selected POE-g-MA for use, when solvent orange 2 A is selected THF for use, POE-g-MA is added in the tetrahydrofuran solvent, puts into baking oven and treats its swelling, and magnetic agitation forms the solution system of homogeneous to dissolving after the swelling.
Organic carbon source quality according to the invention counts 2% ~ 100% with the quality of niobium powder, and for example 2.1%, 10%, 20%, 28%, 40%, 60%, 80%, 85%, but the equal embodiment of the present invention of 98% grade, further preferred 75%.
Step according to the invention (3) is added to solution D and stirs in the solution B at least that 2h obtains uniform aaerosol solution; Churning time can be 2.03h, 2.51h, 3.2h, 4.8h, 5.98h, 7h etc., preferred 2.5 ~ 6h, further preferred 4h.
Step of the present invention (4) is removed residual solvent through suction filtration, washing.Washing is with the mixture of a kind of in the optional water of reagent, absolute ethyl alcohol, acetone or the ether or at least two kinds, further preferred absolute ethyl alcohol.Drying condition is 30 ~ 200 ℃ of following vacuum-dryings.Bake out temperature is 30.3 ℃, 40 ℃, and 50 ℃, 64 ℃, 90 ℃, 130 ℃, 175 ℃, 199 ℃, preferred 40 ℃.Described extraction agent is the mixture of a kind of in absolute ethyl alcohol, acetone or the ether or at least two kinds, absolute ethyl alcohol for example, acetone, absolute ethyl alcohol/acetone etc., further preferred absolute ethyl alcohol.
The described sintering of step of the present invention (5) carries out under vacuum condition; Sintering time is 1 ~ 8h, 1.03h for example, 2.01h, 3h, 3.98h, 6h, 7.89h etc., preferred 2 ~ 4h, further preferred 3.5h; Sintering temperature is 600 ~ 800 ℃, for example 600.2 ℃, and 660 ℃, 697 ℃, 749.8 ℃, 799 ℃ etc., preferred 700 ~ 750 ℃, further preferred 750 ℃.
The present invention also provides a kind of NbSe that obtains through method for preparing
2/ C nano composite material.Two selenizing niobiums are good solid lubricant, and resistance to abrasion is good, and relative friction coefficient is 0.12.Be a kind of material that has oilness and electroconductibility concurrently, be widely used in precision motor with aspects such as brush, special bearing, WW POT contacts.
Nano composite material is to be external phase with matrixes such as resin, rubber, pottery and metals; Be modified as disperse phase with metal, semi-conductor, rigid particles and other inorganic particulates of nano-scale, fiber, CNT etc.; Through suitable preparation method properties-correcting agent homogeneity ground is scattered in the body material; Formation one contains the compound system of nano-sized materials mutually, and this system material is referred to as nano composite material.Matrix material is because its excellent comprehensive performances; Particularly the designability of its performance is widely used in fields such as aerospace, national defence, traffic, physical culture; Nano composite material then is wherein the most attractive part; Development in recent years is very fast, and the strategy of world developed country new material development all is put into important position to the development of nano composite material.This research direction mainly comprises nanometer polymer based composites, CNT functional composite material, fine/nano tungsten-copper matrix material.
Compare with the prior art scheme, the present invention has following beneficial effect:
Experimentation of the present invention is simple to operation, the building-up process green non-pollution, and the carbon-coated nano matrix material of preparation is of a size of 10 ~ 1000nm, is a kind of novel solid lubrication and conducting material, has higher lubricity and conductivity.
Description of drawings
Accompanying drawing 1 is NbSe in the instance 1
2The XRD spectra of/C nano composite material;
Accompanying drawing 2 is NbSe in the instance 1
2The SEM picture of/C nano composite material;
Accompanying drawing 3 is the NbSe in the proportioning different in the instance 2
2The SEM picture of/C nano composite material.
Down in the face of further explain of the present invention.But following instance only is a simple and easy example of the present invention, does not represent or limits rights protection scope of the present invention, and interest field of the present invention is as the criterion with claims.
Embodiment
For the present invention is described better, be convenient to understand technical scheme of the present invention, typical case of the present invention but non-restrictive example is following:
Embodiment 1
Take by weighing 0.4803g POE-g-MA and be dissolved in the THF, be put in 33 ℃ the baking oven and treat its swelling.Be put in extremely dissolving of magnetic agitation in 38 ℃ of water-baths after the swelling.Take by weighing niobium powder 0.6406g, selenium powder 1.3596g (mass ratio is 1.0: 2.1) puts into absolute ethyl alcohol.Under the magnetic agitation condition, above-mentioned Nb-Se premixture is joined in the POE-g-MA solution, continue to stir 4h, obtain uniform aaerosol solution; Be extraction agent (coprecipitator) with about 30mL absolute ethyl alcohol then, under its condition of stirring of maintenance, pour at leisure in the aaerosol solution, obtain Nb, Se powder by the gelatinous precipitate of POE-g-MA parcel; Through suction filtration, absolute ethanol washing, remove residual THF reagent, after 40 ℃ of following vacuum-drying then; The later throw out of oven dry is put into reaction kettle carry out the high-temperature vacuum sintering; Sintering temperature is 750 ℃, and sintering time is 1h, obtains the NbSe of high-performance and good pattern
2/ C nano composite material.
Fig. 1 is NbSe
2The XRD figure spectrum of/C nano structural material is with standard N bSe
2The XRD figure spectrum matches, and the visible product that generates is pure NbSe
2, Fig. 2 is NbSe
2The SEM picture of/C nano structural material, by visible among the figure, the product sheet pattern of generation is obvious, can find out at NbSe
2Outer wall has one deck C to coat, and size ratio is more even.
Take by weighing 0.6406g POE-g-MA and be dissolved in the THF, be put in 33 ℃ the baking oven and treat its swelling.Be put in extremely dissolving of magnetic agitation in 38 ℃ of water-baths after the swelling.Take by weighing niobium powder 0.6406g, selenium powder 1.4734g (mass ratio is 1.0: 2.3) puts into acetone soln.Under the magnetic agitation condition, above-mentioned Nb-Se premixture is joined in the POE-g-MA solution, continue to stir 4h, obtain uniform aaerosol solution; Be extraction agent (coprecipitator) with about 30mL acetone then, under its condition of stirring of maintenance, pour at leisure in the aaerosol solution, obtain Nb, Se powder by the gelatinous precipitate of POE-g-MA parcel; Through suction filtration, absolute ethanol washing, remove residual THF reagent then, 40 ℃ of following vacuum-dryings; The later throw out of oven dry is put into reaction kettle carry out the high-temperature vacuum sintering; Sintering temperature is 750 ℃, and sintering time is 1h, obtains the NbSe of high-performance and good pattern
2/ C nano structural material.We can find out the NbSe that the different proportioning of adjustment obtains from Fig. 3
2/ C nano composite material pattern has some changes, and wherein under this proportioning, its sheet pattern is more obvious, and covered effect is desirable more.
Embodiment 3
Take by weighing 0.0128g POE-g-MA and be dissolved in the THF, be put in 33 ℃ the baking oven and treat its swelling.Be put in extremely dissolving of magnetic agitation in 38 ℃ of water-baths after the swelling.Take by weighing niobium powder 0.6406g, selenium powder 1.9218g (mass ratio is 1.0: 3.0) puts into ether.Under the magnetic agitation condition, above-mentioned Nb-Se premixture is joined in the POE-g-MA solution, continue to stir 4h, obtain uniform aaerosol solution; Be extraction agent (coprecipitator) with about 30mL ether then, under its condition of stirring of maintenance, pour at leisure in the aaerosol solution, obtain Nb, Se powder by the gelatinous precipitate of POE-g-MA parcel; Remove residual THF reagent through suction filtration, washing with acetone then; 30 ℃ of following vacuum-dryings, the later throw out of oven dry to be put into reaction kettle carry out the high-temperature vacuum sintering, sintering temperature is 600 ℃; Sintering time is 8h, obtains the NbSe of high-performance and good pattern
2/ C nano composite material.
Embodiment 4
Take by weighing 0.2800g PAN and be dissolved in the YLENE, ultrasonic to dissolving.Take by weighing niobium powder 0.6406g, selenium powder 1.6015g (mass ratio is 1.0: 2.5) puts into absolute ethyl alcohol.Under the magnetic agitation condition, above-mentioned Nb-Se premixture is joined in the PAN solution, continue to stir 2.5h, obtain uniform aaerosol solution; Be extraction agent (coprecipitator) with about 30mL absolute ethyl alcohol then, under its condition of stirring of maintenance, pour at leisure in the aaerosol solution, obtain Nb, Se powder by the gelatinous precipitate of PAN parcel; Remove residual YLENE reagent through suction filtration, absolute ethanol washing then; 200 ℃ of following vacuum-dryings, the later throw out of oven dry to be put into reaction kettle carry out the high-temperature vacuum sintering, sintering temperature is 700 ℃; Sintering time is 3.5h, obtains the NbSe of high-performance and good pattern
2/ C nano composite material.
Embodiment 5
It is soluble in water to take by weighing 0.6406g glucose.Take by weighing niobium powder 0.6406g, selenium powder 1.7937g (mass ratio is 1.0: 2.8) puts into ether.Under the magnetic agitation condition, above-mentioned Nb-Se premixture is joined in the glucose solution, continue to stir 2h, obtain uniform aaerosol solution; Be extraction agent (coprecipitator) with about 30mL ether then, under its condition of stirring of maintenance, pour at leisure in the aaerosol solution, obtain Nb, Se powder by the gelatinous precipitate of glucose parcel; 65 ℃ of following vacuum-dryings, the later throw out of oven dry to be put into reaction kettle carry out the high-temperature vacuum sintering, sintering temperature is 800 ℃, sintering time is 2h, obtains the NbSe of high-performance and good pattern
2/ C nano composite material.
Embodiment 6
Taking by weighing the 0.5342g polar resin is dissolved in the toluene.Take by weighing niobium powder 0.6406g, selenium powder 1.3596g (mass ratio is 1.0: 2.1) puts into absolute ethyl alcohol.Under the magnetic agitation condition, above-mentioned Nb-Se premixture is joined in the polar resin solution, continue to stir 6h, obtain uniform aaerosol solution; Be extraction agent (coprecipitator) with about 30mL absolute ethyl alcohol then, under its condition of stirring of maintenance, pour at leisure in the aaerosol solution, obtain Nb, Se powder by the gelatinous precipitate of polar resin parcel; Remove residual toluene reagent through suction filtration, absolute ethanol washing then; 120 ℃ of following vacuum-dryings, the later throw out of oven dry to be put into reaction kettle carry out the high-temperature vacuum sintering, sintering temperature is 650 ℃; Sintering time is 4h, obtains the NbSe of high-performance and good pattern
2/ C nano composite material.
The NbSe that obtains through above-mentioned preparation method
2/ C nano composite material is of a size of 10 ~ 1000nm, is a kind of novel solid lubrication and conducting material, has higher lubricity and conductivity.
Applicant's statement, the present invention explains preparation method of the present invention through the foregoing description, but the present invention is not limited to above-mentioned preparation process, does not mean that promptly the present invention must rely on above-mentioned preparation process and could implement.The person of ordinary skill in the field should understand, and to any improvement of the present invention, to the interpolation of the equivalence replacement of raw material that the present invention selects for use and ancillary component, the selection of concrete mode etc., all drops within protection scope of the present invention and the open scope.
Claims (10)
1. NbSe
2The preparation method of/C nano composite material may further comprise the steps:
(1) organic carbon source is dissolved in forms solution B in the solvent orange 2 A;
(2) niobium powder, selenium powder are taken by weighing by 1.0: 2.3 ~ 1.0: 3.0 mass ratio, form solution D in the adding solvent C;
(3) solution D is joined in the solution B, process uniform aaerosol solution;
(4) under agitation condition, extraction agent is added in the above-mentioned aaerosol solution, obtain gelatinous throw out; Remove residual solvent, oven dry obtains throw out;
(5) obtain NbSe behind the throw out sintering after will drying
2/ C nano composite material.
2. the method for claim 1; It is characterized in that; Said organic carbon source is selected from the mixture of a kind of in glucose, lactose, resin, POE-g-MA or the long chain type aliphatic carboxylic acid or at least two kinds, preferred PAN and/or POE-g-MA, further preferred POE-g-MA.
3. according to claim 1 or claim 2 method is characterized in that, said solvent orange 2 A is the mixture of a kind of in water, benzene,toluene,xylene or the THF or at least two kinds, preferably water, THF, further preferred THF;
Preferably, the mixture of a kind of in the preferred absolute ethyl alcohol of said solvent C, acetone, ether or the water or at least two kinds, further preferred absolute ethyl alcohol.
4. like the described method of one of claim 1-3, it is characterized in that, the mass ratio of said niobium powder, selenium powder is preferably 1.0: 2.5 ~ and 1.0: 2.8, most preferably 1.0: 2.1.
5. like the described method of one of claim 1-4, it is characterized in that said step (1) is dissolved in organic carbon source in the solvent orange 2 A through magnetic agitation or ultrasonic.
6. like the described method of one of claim 1-5, it is characterized in that said organic carbon source quality counts 2% ~ 100% with the quality of niobium powder, further preferred 75%.
7. like the described method of one of claim 1-6, it is characterized in that step (3) is added to solution D and stirs in the solution B at least that 2h obtains uniform aaerosol solution;
Preferably, the preferred 2.5 ~ 6h of churning time, further preferred 4h.
8. like the described method of one of claim 1-7; It is characterized in that; Step (4) is removed residual solvent through suction filtration, washing, and washing is with the mixture of a kind of in the optional water of reagent, absolute ethyl alcohol, acetone or the ether or at least two kinds, further preferred absolute ethyl alcohol;
Preferably, described extraction agent is the mixture of a kind of in absolute ethyl alcohol, acetone or the ether or at least two kinds, further preferred absolute ethyl alcohol;
Preferably, drying condition is 30 ~ 200 ℃ of following vacuum-dryings.
9. like the described method of one of claim 1-8, it is characterized in that the described sintering of step (5) carries out under vacuum condition; Sintering time is 1 ~ 8h, preferred 2 ~ 4h, further preferred 3.5h;
Preferably, sintering temperature is 600 ~ 800 ℃, preferred 700 ~ 750 ℃, and further preferred 750 ℃.
10. NbSe through preparing like the described method of one of claim 1-9
2/ C nano composite material is characterized in that, said scantling is 10 ~ 1000nm.
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| CN102923677A (en) * | 2012-11-08 | 2013-02-13 | 镇江中孚复合材料有限公司 | Method for preparing NbSe2 nano material |
| 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 |
| CN107946559A (en) * | 2017-11-07 | 2018-04-20 | 陕西科技大学 | A kind of solvent hot preparation sodium-ion battery anode Sb2Se3The method of/C composite |
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| CN102923677A (en) * | 2012-11-08 | 2013-02-13 | 镇江中孚复合材料有限公司 | Method for preparing NbSe2 nano material |
| 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 |
| CN107946559A (en) * | 2017-11-07 | 2018-04-20 | 陕西科技大学 | A kind of solvent hot preparation sodium-ion battery anode Sb2Se3The method of/C composite |
| CN107946559B (en) * | 2017-11-07 | 2020-04-10 | 陕西科技大学 | Sb for solvothermal preparation of sodium ion battery cathode2Se3Method for preparing/C composite material |
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| CN102703162B (en) | 2014-10-22 |
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