CN106064833A - One is prepared 2H MoS by molybdenum concntrate2the method of nanometer sheet - Google Patents

One is prepared 2H MoS by molybdenum concntrate2the method of nanometer sheet Download PDF

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Publication number
CN106064833A
CN106064833A CN201610361918.8A CN201610361918A CN106064833A CN 106064833 A CN106064833 A CN 106064833A CN 201610361918 A CN201610361918 A CN 201610361918A CN 106064833 A CN106064833 A CN 106064833A
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CN
China
Prior art keywords
mos
nanometer sheet
prepared
molybdenum concntrate
micropowder
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CN201610361918.8A
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Chinese (zh)
Inventor
唐军利
崔玉青
席莎
周新文
何凯
朱琦
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Jinduicheng Molybdenum Co Ltd
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Jinduicheng Molybdenum Co Ltd
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Priority to CN201610361918.8A priority Critical patent/CN106064833A/en
Publication of CN106064833A publication Critical patent/CN106064833A/en
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/06—Sulfides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like

Abstract

The invention discloses one and prepared 2H MoS by molybdenum concntrate2The method of nanometer sheet, is first placed on molybdenum concntrate in jet mill, is ground into micropowder；Then micropowder is joined H2O2In, add ethanol stirring and evenly mixing, after stratification, take upper liquid and filter, the solids filtered out is vacuum dried, obtain 2H MoS2Nanometer sheet.The present invention uses molybdenum concntrate to operate preparation 2H MoS at ambient pressure2Nanometer sheet, the method technique is simple, preparation efficiency is high, and whole process energy consumption is low, pollution-free, environmentally friendly, it is possible to be widely used in commercial production, the 2H MoS prepared2Nanometer sheet can be widely applied to energy storage and conversion, is catalyzed, lubricates and the field such as various composites.

Description

One is prepared 2H-MoS by molybdenum concntrate2The method of nanometer sheet
Technical field
The invention belongs to technical field of nanometer material preparation, be specifically related to one and prepared 2H-MoS by molybdenum concntrate2Nanometer sheet Method.
Background technology
MoS2It is a kind of typical transition metal stratiform compound, there are tri-kinds of crystal structure: 1T-MoS of 1T, 2H, 3R2For Metastability, crystalline structure has metallicity, and Mo atom is octahedral coordination, and structure cell is made up of 1 S-Mo-S monolayer.2H- MoS2For stable phase, crystalline structure has semiconductive and lubricity, and Mo atom is triangular prism coordination, and structure cell is by 2 S-Mo- S monolayer forms, and the molybdenum ore of natural output is to there is typical layer structure under 2H type, room temperature.3R-MoS2Also it is metastable Property, Mo atom is triangular prism coordination, and structure cell is made up of 3 S-Mo-S monolayers.Only 2H-MoS2There is the lubrication of excellence Property, characteristic of semiconductor, when it becomes ultra-thin two-dimension structural material, MoS2Energy gap increase along with the less of its number of plies Adding, during to monolayer, not only its energy gap is increased to 1.90eV by 1.29eV during body phase material, and electronic band structure is also Direct band gap is become from non-immediate band gap.
The MoS of monolayer2Compare the Graphene of zero band gap, in terms of opto-electronic device, show the most excellent characteristic, make Obtain people to be expected to obtain a kind of novel MoS thinner than silicon2Chip.Additionally, MoS2Because of the two-dimensional layered structure that it is intrinsic The embedding de-of lithium ion can be facilitated to make it have higher electrochemical lithium storage performance in lithium ion battery, and obtained people Extensive concern, in terms of catalyst, the MoS of two-dimensional structure2Also there is broader practice prospect.
MoS at present2The preparation method of nanometer sheet is broadly divided into micromechanics stripping method, lithium ion graft process, liquid chromatography ultrasound stripping From method, hydro-thermal method and CVD etc..Micromechanics stripping method technique is simple, and charge stripping efficiency is high, but yields poorly and poor repeatability.Lithium The charge stripping efficiency of ion insertion stripping method is high, but preparation method is complicated, and intercalator is environmentally sensitive, and production cost is high, during preparation Between longer.Liquid chromatography ultrasound stripping method simple and fast, it is possible to be suitable for large-scale production, but general extent of exfoliation is the highest, obtains nanometer Sheet solution concentration is less, high to ultrasound condition dependency.Hydro-thermal method has the advantages such as simple to operate, mild condition, pollution be little, but In course of reaction, nanoparticle is easily reunited, and is difficult to control the nanometer sheet of synthesis monolayer, and the crystal structure that CVD typically results in is relatively Difference, needs annealed process mostly, and technique is the most immature.
Above MoS2The technology of preparing of nanometer sheet, mostly is artificial synthesis, generally 3R or the 2H+3R type of synthesis, and half Conductor performance and greasy property inferior 2H type, preparation process cycle length, technique is loaded down with trivial details, energy consumption is big, and efficiency remains to be further improved.
Summary of the invention
It is an object of the invention to provide one and prepared 2H-MoS by molybdenum concntrate2The method of nanometer sheet, it is achieved low cost, mental retardation Consumption, high efficiency, eco-friendly 2H-MoS2The preparation of nanometer sheet, solves existing preparation method preparation process cycle length, technique Problem loaded down with trivial details, inefficient, that energy consumption is big.
The technical solution adopted in the present invention is, one is prepared 2H-MoS by molybdenum concntrate2The method of nanometer sheet, first by molybdenum essence Ore deposit is placed in jet mill, is ground into micropowder；Then micropowder is joined H2O2(30%), in, ethanol is added also Stirring and evenly mixing, after stratification, takes upper liquid and filters, be vacuum dried the solids filtered out, obtain 2H-MoS2 Nanometer sheet.
Preferably, content >=59% of Mo in molybdenum concntrate.
Preferably, micropowder laser particle size D50=0.5～0.8 μm.
Preferably, H2O2(30%) quality is 50～200 times of micropowder, the quality of ethanol be micropowder 800～ 1500 times.
Preferably, mixing time is 1～8h.
Preferably, it is dried under vacuum to moisture≤0.2%.
Preferably, 2H-MoS2The lateral dimension of nanometer sheet is 0.2～5 μm, and thickness is 1～2nm.
The invention has the beneficial effects as follows, the present invention uses molybdenum concntrate to operate preparation 2H-MoS at ambient pressure2Nanometer sheet, the party Method technique is simple, preparation efficiency is high, and whole process energy consumption is low, pollution-free, environmentally friendly, it is possible to be widely used in industry raw Produce, the 2H-MoS prepared2Nanometer sheet can be widely applied to energy storage and conversion, is catalyzed, lubricates and various composite In field.
Accompanying drawing explanation
Fig. 1 is the XRD diffracting spectrum of molybdenum concntrate；
Fig. 2 is 2H-MoS prepared by the present invention2The shape appearance figure of the atomic force microscope of nanometer sheet；
Fig. 3 is 2H-MoS prepared by the present invention2The datagram of the atomic force microscope of nanometer sheet.
Detailed description of the invention
The present invention is described in further detail with detailed description of the invention below in conjunction with the accompanying drawings, but the present invention is not limited to These embodiments.
The present invention is prepared 2H-MoS by molybdenum concntrate2The method of nanometer sheet particularly as follows:
First the molybdenum concntrate of Mo content >=59% is placed in jet mill, is ground into laser particle size D50=0.5～0.8 The micropowder of μm；Then micropowder is joined H2O2In (mass fraction 30%), add ethanol, wherein H2O2(30%) Quality is 50～200 times of micropowder, and the quality of ethanol is 800～1500 times of micropowder.Mixed liquor is sufficiently stirred for 1～ 8h, after static layering, takes upper liquid and filters, the solids filtered out is dried under vacuum to moisture≤0.2%, Obtain 2H-MoS2Nanometer sheet.
The MoS of 2H type can be prepared according to above method2Nanometer sheet.Being different from synthetic method, the present invention uses 2H The molybdenum concntrate of type is raw material, as it is shown in figure 1, prepare MoS with it2Nanometer sheet, the product obtained is 2H type, preparation method is simple, Efficiency is high, and energy consumption is low.From Fig. 2, the atomic force microscope figure (AFM) of 3,2H-MoS prepared by the present invention2Nanometer sheet is horizontal To a size of 0.2～5 μm, thickness is about 1～2nm.The productivity of this sized nanostructures sheet is 30-50%.
The method further illustrating this powder with embodiment below.
Molybdenum concntrate (Mo >=59%) after purification is positioned in jet mill, is ground into laser particle size D500.5～ Micropowder between 0.8 μm.
Embodiment 1
Take above-mentioned micropowder (D50=0.5 μm) 1g, join 50mL H2O2(30%), in, add 800mL ethanol, hold Stratification after continuous stirring 1h, takes upper liquid, filters, is dried under vacuum to moisture≤0.2%, obtain 2H-MoS2Nanometer sheet, Place freezen protective.
Embodiment 2
Take above-mentioned micropowder (D50=0.7 μm) 1g, join 100mL H2O2(30%), in, 1200mL ethanol is added, Stratification after continuously stirred 4h, takes upper liquid, filters, is dried under vacuum to moisture≤0.2%, obtains 2H-MoS2Nanometer Sheet, places freezen protective.
Embodiment 3
Take above-mentioned micropowder (D50=0.8 μm) 1g, join 200mL H2O2(30%), in, 1500mL ethanol is added, Stratification after continuously stirred 8h, takes upper liquid, filters, is dried under vacuum to moisture≤0.2%, obtains 2H-MoS2Nanometer Sheet, places freezen protective.
The present invention uses molybdenum concntrate to operate preparation 2H-MoS at ambient pressure2Nanometer sheet, the method technique is simple, preparation efficiency Height, and whole process energy consumption is low, pollution-free, environmentally friendly, it is possible to be widely used in commercial production, the 2H-MoS for preparing2 Nanometer sheet can be widely applied to energy storage and conversion, is catalyzed, lubricates and the field such as various composites.
Above description of the present invention is section Example, but the invention is not limited in above-mentioned detailed description of the invention. Above-mentioned detailed description of the invention is schematic, is not restrictive.The material of every employing present invention and method, do not taking off In the case of present inventive concept and scope of the claimed protection, all concrete expansions all belong to protection scope of the present invention it In.

Claims (7)

1. prepared 2H-MoS by molybdenum concntrate for one kind2The method of nanometer sheet, it is characterised in that first molybdenum concntrate is placed on comminution by gas stream In machine, it is ground into micropowder；Then micropowder is joined H2O2In, add ethanol stirring and evenly mixing, after stratification, take Upper liquid filters, and is vacuum dried the solids filtered out, obtains 2H-MoS2Nanometer sheet.
The most according to claim 1 prepared 2H-MoS by molybdenum concntrate2The method of nanometer sheet, it is characterised in that described molybdenum concntrate Content >=59% of middle Mo.
The most according to claim 1 prepared 2H-MoS by molybdenum concntrate2The method of nanometer sheet, it is characterised in that described micropowder Laser particle size D50=0.5～0.8 μm.
The most according to claim 1 prepared 2H-MoS by molybdenum concntrate2The method of nanometer sheet, it is characterised in that described H2O2Matter Amount mark is 30%, described H2O2Quality is described micropowder 50～200 times, the quality of described ethanol is described micropowder 800～1500 times.
The most according to claim 1 prepared 2H-MoS by molybdenum concntrate2The method of nanometer sheet, it is characterised in that during described stirring Between be 1～8h.
The most according to claim 1 prepared 2H-MoS by molybdenum concntrate2The method of nanometer sheet, it is characterised in that described vacuum is done Dry to moisture≤0.2%.
The most according to claim 1 prepared 2H-MoS by molybdenum concntrate2The method of nanometer sheet, it is characterised in that described 2H- MoS2The lateral dimension of nanometer sheet is 0.2～5 μm, and thickness is 1～2nm.
CN201610361918.8A 2016-05-26 2016-05-26 One is prepared 2H MoS by molybdenum concntrate2the method of nanometer sheet Pending CN106064833A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101641291A (en) * 2006-11-16 2010-02-03 雅宝荷兰有限责任公司 By molybdenum glance purified molybdenum technical oxide
CN103771517A (en) * 2014-01-17 2014-05-07 哈尔滨工业大学 Method for preparing liquid phase dispersion-based two-dimensional MoS2 nanosheets
CN104495935A (en) * 2014-12-03 2015-04-08 安徽百特新材料科技有限公司 Preparation method of molybdenum disulfide nanosheet in stripping manner
CN104609474A (en) * 2015-01-29 2015-05-13 南昌航空大学 Method for preparing few-layer MoS2 nanosheets

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101641291A (en) * 2006-11-16 2010-02-03 雅宝荷兰有限责任公司 By molybdenum glance purified molybdenum technical oxide
CN103771517A (en) * 2014-01-17 2014-05-07 哈尔滨工业大学 Method for preparing liquid phase dispersion-based two-dimensional MoS2 nanosheets
CN104495935A (en) * 2014-12-03 2015-04-08 安徽百特新材料科技有限公司 Preparation method of molybdenum disulfide nanosheet in stripping manner
CN104609474A (en) * 2015-01-29 2015-05-13 南昌航空大学 Method for preparing few-layer MoS2 nanosheets

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