CN102703160B - Preparation method of graphite-bi-selenylation niobium nanocomposite - Google Patents
Preparation method of graphite-bi-selenylation niobium nanocomposite Download PDFInfo
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- CN102703160B CN102703160B CN201210149531.8A CN201210149531A CN102703160B CN 102703160 B CN102703160 B CN 102703160B CN 201210149531 A CN201210149531 A CN 201210149531A CN 102703160 B CN102703160 B CN 102703160B
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Abstract
The invention relates to a preparation method of a graphite-bi-selenylation niobium nanocomposite. The preparation method enables niobium powder, selenium powder and graphite powder to serve as raw materials, conducts solid-phase reaction at certain temperature conditions and synthetizes sheet-shaped particles formed by a graphite-selenylation niobium nanocomposite. The preparation method is simple in process, high in productivity, environmental friendly, free of pollution and capable of achieving large-scale industrial preparation. Simultaneously, nano materials are small in size and have good physical chemistry effects so that the nano materials can serve as an excellent annexing agent of an electric contact material.
Description
Technical field
The present invention relates to a kind of synthetic method of nano-complex, particularly a kind of preparation method of graphite-bis-selenizing niobium, belongs to inorganic composite materials technical field.
Background technology
Graphite is as a kind of traditional solid lubricant, also have the advantage such as heat conduction, conduction and light weight, inexpensive that unreactiveness is good, high temperature resistant, corrosion-resistant and good concurrently, in antifriction metal (AFM), pottery, the macromolecular materials such as aluminium, silver, copper, nickel, SiC, polytetrafluoroethylene (PTFE), polyimide (PI), polyamide (PA), epoxy resin (EP), be widely used.
Graphite Powder 99 be a kind of Dark grey have metalluster and opaque finely squamose solid.Graphite is very soft, has soapy feeling, has good conductivity, is a kind of cell negative electrode material.The technical process of Graphite Powder 99 is, sending the raw ore ore after explosion to stone breaking machine by mine car pulverizes, the grinding machine of scoring again carries out flotation, send again the graphite wet feed floatingly selecting to ball mill grinding selected, sending the wet feed pack of choosing to pouring dry machine drenches dry, become pouring siccative, drenching siccative has been graphite finished product.Pouring siccative being sent between drying vehicle, dried rear pack, is common graphite powder, the carbon content average out to 90% of final product.
Two selenizing niobiums are the pewter powder with metalluster.Crystal is six side's laminate structures, density 6.30g/cm
3, resistivity 5.35 × 10
-4Ω cm, has very high thermostability, and in nitrogen, use temperature can reach 600 DEG C, reaches 900 DEG C in inert atmosphere; Except concentrated nitric acid, general acid, alkali and organic solvent are had to satisfactory stability; In vacuum, 900 ~ 1000 DEG C are decomposed generation selenizing niobium and elemental selenium or resolve into niobium and selenium completely; In air, 300 DEG C start oxidation.By metal niobium powder and selenium in sealed vessel at 600 ~ 800 DEG C reaction or Niobium Pentxoxide and Selenium hydride all can make two selenizing niobiums 800 ~ 1000 DEG C of reactions.Two selenizing niobiums are good solid lubricant, resistance to abrasion is good, relative friction coefficient is 0.12, it is a kind of layer structure material that has favorable lubricating property and superconductivity concurrently, be with a wide range of applications at the aspect such as high-temperature solid lubrication, superconduction, its preparation and property research has been caused to people's extensive attention.Tang etc. prepare NbSe by Nb and Se by solid state reaction
3nanofiber and NbSe
2micron film, Hor etc. are by Se and NbSe
3nanofiber is prepared NbSe
2nano wire, Nath etc. pass through NbSe
3pyrolysis obtain NbSe
2nanotube, Tsuneta etc. reach the NbSe of 100-200nm by gas phase transmission (CVT) method acquisition diameter
2nanotube and nanofiber, Sekar etc. pass through at N
2nbCl at atmosphere and 280 DEG C
5pyrolysis and with the chemical combination of Se, then cooling in different media, obtained respectively the NbSe of 10 ~ 70nm
2nanometer sheet and diameter 2-25nm, length reach the nano wire of tens microns.But niobium source is expensive, and Nb, Se, NbSe
2easily and O
2reaction, and Nb can also with N
2reaction.Therefore, synthetic atmosphere protection requires strict, and cost is high, and these have all limited its application greatly, realizes its green, low cost, mass-producing preparation, has important theoretical investigation and practical application meaning.
CN102011024A discloses a kind of copper-graphite-bis-selenizing niobium (NbSe
2) self-lubricating material and preparation method thereof, be mainly with copper powder, Graphite Powder 99, nanometer two selenizing niobium powder (NbSe
2) be raw material, adopt sinter molding after powder metallurgic method compressing tablet, then the method that adopts repressing and re-sintering again after compressing tablet sinter molding obtain the copper-graphite-bis-selenizing niobium (NbSe all with good properties of antifriction and wear resistance under normal temperature and pressure and vacuum condition
2) self-lubricating material.
CN101800089A discloses a kind of nanometer NbSe
2copper-base solid self-lubricating composite material and preparation method thereof, is mainly taking Nb powder cheap and easy to get and Se powder as raw material, packs in quartz glass tube heating under the protection of rare gas element, insulation, the cooling nanometer NbSe that first obtains after the two is mixed into
2material, then after the latter is mixed with copper powder according to certain mass percent through colding pressing, sintering, cold pressing and obtain again.
Above two patents have all prepared NbSe by serial of methods
2self-lubricating composite, but technique or the more complicated of two kinds of methods, operator need to can on dutyly operate through the training of long period, and the problem occurring in operating process is also more, has had a strong impact on production efficiency, is difficult to adapt to the demand in market.
Summary of the invention
The object of the present invention is to provide a kind of method of synthetic graphite-bis-selenizing niobium nano composite material.Making method of the present invention is easy, and technique is simple, can synthesize in a large number pattern novelty, particle size homogeneous, the graphite-bis-selenizing niobium nano composite material of excellent performance.
In order to achieve the above object, the present invention is achieved through the following technical solutions:
A preparation method for graphite-bis-selenizing niobium nano composite material, comprises the following steps,
(1) niobium powder, selenium powder, Graphite Powder 99 are taken by a certain percentage and put into solvent, mix rear leaving standstill, remove upper strata alcohol clear liquid, put into baking oven oven dry and obtain powder;
(2) above-mentioned powder is packed into and in closed reactor, put into tube furnace again and be warming up at least 600 DEG C, be incubated at least 45min, furnace cooling, obtains graphite-bis-selenizing niobium nano composite material.
Niobium powder is the powder of metal niobium, has the valve metal character of unilateral conduction at the dense oxidation film of its Surface Creation.Its oxide compound niobium oxides Nb
2o
5for white powder, purity 99.999%, for the production of high-purity lithium niobate crystals and special optical glass additive.Stable chemical performance, the resistivity of this anode oxide film are high, leakage current is little, specific inductivity is large.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).Adopt reduction-hydride process, sodium reduction etc. to produce.For the manufacture of 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 without impurity such as earth, stable components, moisture is even, and outward appearance is black gray expandable hexagonal system metal, is dissolved in the vitriol oil, trichloromethane, is slightly soluble in dithiocarbonic anhydride, water insoluble, ethanol.Can be used for rectifier, photographic exposure agent, metallurgical addition agent, petrochemical catalyst, duplicates toner cartridge, selenium photographic plate, alloy, and pigment in plastics, paint, enamel and glass etc.The scope of application: electronics, glass, pottery, chemistry, metallurgy, medical treatment and health care, environmental sanitation, the industries such as rectifier.Graphite Powder 99 be a kind of Dark grey have metalluster and opaque finely squamose solid.Graphite is very soft, has soapy feeling, has good conductivity.The mol ratio of the described niobium powder of step of the present invention (1) and selenium powder is 1.0: 2.3 ~ 1.0: 3.0, for example 1.0: 2.32, and 1.0: 2.5,1.0: 2.6,1.0: 2.72,1.0: 2.85,1.0: 2.99 etc., be preferably 1.0: 2.5 ~ 1.0: 2.8, most preferably 1.0: 2: 7.The quality of Graphite Powder 99 is 50% ~ 150% of niobium opaque amount, for example 52%, 60%, 65%, 72%, 80%, 112%, 130%, 142%, 148% etc., preferably 60% ~ 100%, further preferably 75%.
The described solvent of step (1) is selected from the mixture of a kind of in dehydrated alcohol, ether or acetone or at least two kinds, for example dehydrated alcohol, ether/acetone, dehydrated alcohol/acetone etc., further preferred dehydrated alcohol.
The described hybrid mode of step (1) is selected from magnetic agitation, ball milling or ultrasonic batch mixing, further preferred magnetic agitation.Magnetic stirring apparatus is applicable to heating or heated and stirred is carried out simultaneously, and being applicable to viscosity is not very large liquid or solidliquid mixture.Magnetic stirring apparatus has utilized the principle of magnetic field and whirlpool, and liquid is put into after container, and stirrer is put into liquid simultaneously, when base produces behind magnetic field, drives stirrer to become circumference cyclic motion, thereby reaches the object of stirred liq.The time of magnetic agitation of the present invention is at least 1h, for example 1.02h, 1.31h, 2.6h, 3h, 4.2h, 4.99h, 6h, 8h etc., preferably 1.3 ~ 5h, further preferred 2h.
The described bake out temperature of step of the present invention (1) is at least 60 DEG C, for example 60.3 DEG C, and 70.4 DEG C, 75.8 DEG C, 87 DEG C, 102 DEG C, 120 DEG C, 129.7 DEG C, 160 DEG C etc., preferably 70 ~ 130 DEG C, further preferably 75 DEG C.
Tube furnace is all the high energy-conservation Novel electric furnace of high-performance that adopts international advanced technology to develop, and has the multiple tubular type type of furnaces such as single tube, two-tube, horizontal, openable, vertical, single warm area, two warm area, three-temperature-zone.Be mainly used in the use of the experiments such as universities and colleges, scientific research institutions, industrial and mining enterprises and small serial production.Have safe and reliable, simple to operate, temperature-controlled precision is high, high insulating effect, temperature range large, fire box temperature homogeneity is high, warm area is many, optional distribution atmosphere, vacuumize the type of furnace etc.The described temperature rise rate of step of the present invention (2) is 2 ~ 15 DEG C/min, for example 2.01 DEG C/min, 5.4 DEG C/min, 9.98 DEG C/min, 11.3 DEG C/min, 13 DEG C/min, 14.95 DEG C/min etc. all can be used for implementing the present invention, preferably 2 DEG C/min, 5 DEG C/min, 10 DEG C/min, further preferred 10 DEG C/min.
Step of the present invention (2) is preferably warming up to 600 ~ 900 DEG C, and for example 602 DEG C, 638.5 DEG C, 650.3 DEG C, 720 DEG C, 750.8 DEG C, 800 DEG C, 849.7 DEG C, 898 DEG C etc., more preferably 650 ~ 850 DEG C, further preferably 750 DEG C.
Step of the present invention (2) preferably soaking time is 1 ~ 8h, for example 1.02h, 1.54h, 2.2h, 3h, 3.98h, 4.5h, 6h, 7.99h etc., more preferably 1.5 ~ 4h, further preferred 2h.
The present invention also provides a kind of graphite-bis-selenizing niobium nano composite material preparing by above-mentioned method.
Nano composite material is taking matrixes such as resin, rubber, pottery and metals as external phase, be modified as disperse phase with metal, semi-conductor, rigid particles and other inorganic particulates of nano-scale, fiber, CNT (carbon nano-tube) etc., by suitable preparation method by properties-correcting agent homogeneity be scattered in 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 due to its good over-all properties, particularly the designability of its performance is widely used in the fields such as aerospace, national defence, traffic, physical culture, nano composite material is wherein the most attractive part, development in recent years is very fast, and the strategy of World Developed Countries new material development is all put into important position the development of nano composite material.This research direction mainly comprises nanometer polymer based composites, CNT (carbon nano-tube) functional composite material, fine/nano tungsten-copper matrix material.
Compared with prior art scheme, the present invention has following beneficial effect:
Preparation method of the present invention has the advantages such as synthetic route green is easy, with low cost, technique is simple, the easy control of parameter, is applicable to large-scale industrial production; Prepared graphite-bis-selenizing niobium tribological property excellence, electroconductibility are good, size is little, there is good physical chemistry effect, therefore can be used as the additive of good contact material, thereby there is industrial use widely in electrochemistry, friction, lubrication field.
Brief description of the drawings
Accompanying drawing 1 is the XRD spectra of the graphite-bis-selenizing niobium nano composite material of embodiment 1;
Accompanying drawing 2 is the scanning electron microscope picture of the graphite-bis-selenizing niobium nano composite material of embodiment 1;
Accompanying drawing 3 is the transmission electron microscope picture of the graphite-bis-selenizing niobium nano composite material of embodiment 1.
The present invention is described in more detail below.But following example is only simple and easy example of the present invention, does not represent or limit the 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 but non-limiting embodiment of the present invention is as follows:
Embodiment 1
Get niobium powder 0.60736g, selenium powder 1.39264g, Graphite Powder 99 0.45552g joins in the beaker of 50ml dehydrated alcohol, magnetic agitation 2h, mixes, and leaves standstill, pour out supernatant liquor, at 75 DEG C, dry residue dehydrated alcohol, the powder mixing is packed in homemade reactor, put into tubular react furnace, be warmed up to 650 DEG C with the speed of 10 DEG C/min, insulation 2h, cools to room temperature with the furnace and takes out sample, and gained powder is graphite-bis-selenizing niobium nano composite material.
Embodiment 2
Get niobium powder 0.60736g, selenium powder 1.39264g, Graphite Powder 99 0.45552g joins in the beaker of 50ml dehydrated alcohol, magnetic agitation 2h, mixes, and leaves standstill, pour out supernatant liquid, at 75 DEG C, dry residue dehydrated alcohol, the powder mixing is packed in homemade reactor, put into tubular react furnace, be warmed up to 750 DEG C with the speed of 10 DEG C/min, insulation 2h, cools to room temperature with the furnace and takes out sample, and gained powder is graphite-bis-selenizing niobium nano composite material.
Embodiment 3
Get niobium powder 0.60736g, selenium powder 1.39264g, Graphite Powder 99 0.45552g joins in the beaker of 50ml dehydrated alcohol, magnetic agitation 2h, mixes, and leaves standstill, pour out supernatant liquid, at 75 DEG C, dry residue dehydrated alcohol, the powder mixing is packed in homemade reactor, put into tubular react furnace, be warmed up to 850 DEG C with the speed of 10 DEG C/min, insulation 2h, cools to room temperature with the furnace and takes out sample, and gained powder is graphite-bis-selenizing niobium nano composite material.
Embodiment 4
Get niobium powder 0.60736g, selenium powder 1.18731g, Graphite Powder 99 0.30368g joins in the beaker of 50ml ether, ultrasonic batch mixing 1h, mixes, and leaves standstill, pour out supernatant liquor, at 130 DEG C, dry residue ether, the powder mixing is packed in homemade reactor, put into tubular react furnace, be warmed up to 600 DEG C with the speed of 2 DEG C/min, insulation 8h, cools to room temperature with the furnace and takes out sample, and gained powder is graphite-bis-selenizing niobium nano composite material.
Embodiment 5
Get niobium powder 0.60736g, selenium powder 1.39264g, Graphite Powder 99 0.45552g joins in the beaker of 50ml acetone, magnetic agitation 1.3h, mixes, and leaves standstill, pour out supernatant liquid, at 70 DEG C, dry residue acetone, the powder mixing is packed in homemade reactor, put into tubular react furnace, be warmed up to 900 DEG C with the speed of 5 DEG C/min, insulation 4h, cools to room temperature with the furnace and takes out sample, and gained powder is graphite-bis-selenizing niobium nano composite material.
Embodiment 6
Get niobium powder 0.60736g, selenium powder 1.54867g, Graphite Powder 99 0.91104g joins in the beaker of 50ml dehydrated alcohol, ball milling 5h, mixes, and leaves standstill, pour out supernatant liquid, at 60 DEG C, dry residue dehydrated alcohol, the powder mixing is packed in homemade reactor, put into tubular react furnace, be warmed up to 650 DEG C with the speed of 15 DEG C/min, insulation 1.5h, cools to room temperature with the furnace and takes out sample, and gained powder is graphite-bis-selenizing niobium nano composite material.
Embodiment 7
Get niobium powder 0.60736g, selenium powder 1.29056g, Graphite Powder 99 0.45552g joins in the beaker of 50ml acetone, magnetic agitation 3h, mixes, and leaves standstill, pour out supernatant liquid, at 120 DEG C, dry residue acetone, the powder mixing is packed in homemade reactor, put into tubular react furnace, be warmed up to 800 DEG C with the speed of 8 DEG C/min, insulation 1h, cools to room temperature with the furnace and takes out sample, and gained powder is graphite-bis-selenizing niobium nano composite material.
Embodiment 8
Get niobium powder 0.60736g, selenium powder 1.39264g, Graphite Powder 99 0.60736g joins in the beaker of 50ml ether, magnetic agitation 2.8h, mixes, and leaves standstill, pour out supernatant liquid, at 75 DEG C, dry residue ether, the powder mixing is packed in homemade reactor, put into tubular react furnace, be warmed up to 700 DEG C with the speed of 12 DEG C/min, insulation 2h, cools to room temperature with the furnace and takes out sample, and gained powder is graphite-bis-selenizing niobium nano composite material.
Applicant's statement, the present invention illustrates preparation method of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned preparation process, does not mean that the present invention must rely on above-mentioned preparation process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, and the selections of the equivalence replacement to the selected raw material of the present invention and the interpolation of ancillary component, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
Claims (24)
1. a preparation method for graphite-bis-selenizing niobium nano composite material, comprises the following steps:
(1) niobium powder, selenium powder, Graphite Powder 99 are put into solvent, mix rear leaving standstill, remove supernatant liquor, put into baking oven and dry and obtain powder at least 60 DEG C; Wherein the mol ratio of niobium powder and selenium powder is 1.0:2.6～1.0:3.0, and the quality of graphite is 60%～150% of niobium opaque amount;
(2) above-mentioned powder is packed into and in closed reactor, put into tube furnace again and be warming up at least 600 DEG C, be incubated at least 45min, furnace cooling, obtains graphite-bis-selenizing niobium nano composite material.
2. the method for claim 1, is characterized in that, the mol ratio of the described niobium powder of step (1) and selenium powder is 1.0:2.6～1.0:2.8.
3. method as claimed in claim 2, is characterized in that, the mol ratio of described niobium powder and selenium powder is 1.0:2.7.
4. method as claimed in claim 1 or 2, is characterized in that, the quality of Graphite Powder 99 is 60%～100% of niobium opaque amount.
5. method as claimed in claim 4, is characterized in that, the quality of Graphite Powder 99 is 75% of niobium opaque amount.
6. the method as described in one of claim 1-3, is characterized in that, the described solvent of step (1) is selected from the mixture of a kind of in dehydrated alcohol, ether or acetone or at least two kinds.
7. method as claimed in claim 6, is characterized in that, described solvent is dehydrated alcohol.
8. method as claimed in claim 1, is characterized in that, the described hybrid mode of step (1) is selected from magnetic agitation, ball milling or ultrasonic batch mixing.
9. method as claimed in claim 8, is characterized in that, described hybrid mode is magnetic agitation.
10. the method for claim 1, is characterized in that, the mixing time of step (1) is at least 1h.
11. methods as claimed in claim 10, is characterized in that, mixing time is 1.3～5h.
12. methods as claimed in claim 11, is characterized in that, mixing time is 2h.
13. the method for claim 1, is characterized in that, the described bake out temperature of step (1) is 70～130 DEG C.
14. methods as claimed in claim 13, is characterized in that, described bake out temperature is 75 DEG C.
15. the method for claim 1, is characterized in that, the described temperature rise rate of step (2) is 2～15 DEG C/min.
16. methods as claimed in claim 15, is characterized in that, described temperature rise rate is 2 DEG C/min, 5 DEG C/min, 10 DEG C/min.
17. methods as claimed in claim 16, is characterized in that, described temperature rise rate is 10 DEG C/min.
18. the method for claim 1, is characterized in that, step (2) is warming up to 600～900 DEG C.
19. methods as claimed in claim 18, is characterized in that, step (2) is warming up to 650～850 DEG C.
20. methods as claimed in claim 19, is characterized in that, step (2) is warming up to 750 DEG C.
21. the method for claim 1, is characterized in that, step (2) soaking time is 1～8h.
22. methods as claimed in claim 21, is characterized in that, soaking time is 1.5～4h.
23. methods as claimed in claim 22, is characterized in that, soaking time is 2h.
24. 1 kinds of graphite-bis-selenizing niobium nano composite materials that prepare by the method one of claim 1-23 Suo Shu.
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| 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 process of niobium diselenide or niobium disulfide/carbon wear-resistant nano composite material |
| CN109137030A (en) * | 2018-06-29 | 2019-01-04 | 洛阳师范学院 | A kind of preparation method of two selenizings niobium pentoxide film |
| CN110010884A (en) * | 2019-04-15 | 2019-07-12 | 东北大学 | A kind of additive-free niobium base carbon-containing electrode piece and preparation method thereof |
| CN110116992A (en) * | 2019-05-08 | 2019-08-13 | 上海电力学院 | A kind of preparation method and application of two selenizing niobium of sodium ion battery electrode material |
| CN111224116B (en) * | 2020-02-24 | 2021-12-07 | 中新国际联合研究院 | Catalyst for fuel cell and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102011024A (en) * | 2010-11-19 | 2011-04-13 | 无锡润鹏复合新材料有限公司 | Copper-graphite-niobium diselenide (NbSe2) self-lubricating material and preparation method thereof |
| CN102127484A (en) * | 2010-12-03 | 2011-07-20 | 无锡润鹏复合新材料有限公司 | Preparation method of tungsten diselenide nano-clathrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102011024A (en) * | 2010-11-19 | 2011-04-13 | 无锡润鹏复合新材料有限公司 | Copper-graphite-niobium diselenide (NbSe2) self-lubricating material and preparation method thereof |
| CN102127484A (en) * | 2010-12-03 | 2011-07-20 | 无锡润鹏复合新材料有限公司 | Preparation method of tungsten diselenide nano-clathrate |
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