CN101857273A - Preparation method of nanoscale flaky molybdenum disulfide - Google Patents

Preparation method of nanoscale flaky molybdenum disulfide Download PDF

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Publication number
CN101857273A
CN101857273A CN 201010185621 CN201010185621A CN101857273A CN 101857273 A CN101857273 A CN 101857273A CN 201010185621 CN201010185621 CN 201010185621 CN 201010185621 A CN201010185621 A CN 201010185621A CN 101857273 A CN101857273 A CN 101857273A
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China
Prior art keywords
molybdenum disulfide
preparation
flaky molybdenum
nanoscale
nanoscale flaky
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CN 201010185621
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Chinese (zh)
Inventor
施利毅
杨廷廷
冯欣
汤庆利
方建慧
王钢领
时雯
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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Priority to CN 201010185621 priority Critical patent/CN101857273A/en
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Abstract

The invention discloses a preparation method of nanoscale flaky molybdenum disulfide, which is characterized by comprising the following steps: ammonium tetrathiomolybdate (ATTM) is used as a molybdenum source and a sulfur source, and oxalic acid is used as a reducing agent; the ATTM and the oxalic acid are added in aqueous solution under the condition of heating and stirring, and then amorphous molybdenum disulfide is obtained by a chemical precipitation process; and then the amorphous molybdenum disulfide is placed into a tube furnace on a quartz boat for heating at a high temperature in a nitrogen atmosphere to obtain the nanoscale flaky molybdenum disulfide. The invention adopts the chemical precipitation process and a high-temperature heating method to prepare the nanoscale flaky molybdenum disulfide which is expected to be produced in a large scale; and the preparation method has available raw materials, low cost and simple process.

Description

The preparation method of nanoscale flaky molybdenum disulfide
Technical field
The present invention relates to inorganic lubricant material molybdenumdisulphide (MoS 2) preparation field, especially nano-grade MoS 2The preparation method.
Background technology
Molybdenumdisulphide (MoS 2) be one of typical case's representative of sheet transient metal sulfide.MoS 2As a kind of solid lubricant commonly used, on the one hand because of having laminate structure, layer with layer between sulphur atom bonding force (Van der Waals force) a little less than, be easy to slip and show good antifriction function; Be exposed to MoS on the other hand 2The sulphur atom of plane of crystal produces very strong adhesive attraction to the metallic surface, forms very firm film, and lubricity is better than graphite.
MoS 2Have unique physics and chemical property with its special laminate structure, enjoy the good reputation of " lubricated king " in lubricated field always, be used widely in fields such as oil Hydrobon catalyst, photoelectrochemistry, non-water lithium cell, elastomerics novel material and coatings, to MoS 2Preparation and the research of using have caused area research persons' such as physical chemistry and Materials science extensive concern.
Suitable reductive agent can be reduced into Mo (IV) with Mo (VI) or Mo (V), as if control condition in reaction, the MoS of generation 2Granularity can reach nano level.By the strong reducing property of oxalic acid and oxammonium hydrochloride, Mo (VI) can be reduced into Mo (IV).
Summary of the invention
The object of the present invention is to provide that a kind of raw material is easy to get, cheap, technology simply prepares nano-grade MoS 2Method.
Purpose of the present invention is achieved through the following technical solutions.
A kind of nano-grade MoS 2The preparation method, step is as follows: be molybdenum source and sulphur source with the four thio ammonium molybdate, oxalic acid is reductive agent, deionized water is a solvent, three's mol ratio is followed successively by 1: 1～2: 400～500, at 70～90 ℃ of following stirring reaction 1～1.5h of temperature, makes amorphous molybdenumdisulphide through chemical precipitation method, high-temperature heating treatment under nitrogen atmosphere obtains nanoscale flaky molybdenum disulfide then.
Described reductive agent oxalic acid can replace with oxammonium hydrochloride, and other reaction conditions is identical.Preferred oxalic acid is reductive agent.
Described high-temperature heating treatment is specially, and under nitrogen atmosphere protection, the amorphous molybdenumdisulphide that chemical precipitation method is made places on the quartz boat and is heated to 800 ℃ in tube furnace, heating 1h, furnace cooling then.
Described flaky molybdenum disulfide, particle diameter is between 50-100nm.
Raw material four thio ammonium molybdate described in the present invention is homemade, mixes obtaining after leaving standstill according to stoichiometric ratio with the aqueous solution of ammonium molybdate and ammonium sulfide.
The present invention adopts chemical precipitation method and the synthetic preparation of heat method nano-grade MoS 2, technology is simple; Used raw material four thio ammonium molybdate by self-control obtain, oxalic acid buys and can get, raw material is easy to get and is cheap; The nanoscale flaky molybdenum disulfide purity that finally obtains is higher, and is expected to produce in enormous quantities.
Description of drawings
Fig. 1 is the sheet MoS that makes with the inventive method 2Field emission scanning electron microscope (SEM) photo;
Fig. 2 is the sheet MoS that makes with the inventive method 2X-ray diffraction (XRD) spectrogram.
Embodiment
After now specific embodiments of the invention being described in.
Embodiment 1: with 2.6g (NH 4) 2MoS 4(0.01mol) and 1.26gC 2H 2O 42H 2O (0.01mol) joins in the there-necked flask, again to wherein injecting the 70mL deionized water, and under 80 ℃ of heating in water bath, magnetic agitation 1h.To precipitate through suction filtration, washing and absolute ethanol washing after being cooled to room temperature, dry in 80 ℃ of baking ovens, get amorphous MoS 2Again with amorphous MoS 2Put in the quartz boat of silica tube, in tube furnace, be heated to 800 ℃, insulation 1h, furnace cooling then.A straight-through nitrogen finally obtains black MoS in the silica tube 2Powder.Directly under field emission scanning electron microscope, observe, can find a large amount of sheet structure MoS as Fig. 1 (a, b) 2Generation, and particle diameter is at 50-100nm.The XRD diffraction of Fig. 2 has confirmed that further product is sheet structure MoS 2
Embodiment 2: with 2.6g (NH 4) 2MoS 4(0.01mol) and 1.39gNH 2OHHCl (0.02mol) joins in the there-necked flask, again to wherein injecting the 100mL deionized water, and under 80 ℃ of heating in water bath, magnetic agitation 1h.To precipitate through suction filtration, washing and absolute ethanol washing after being cooled to room temperature, dry in 80 ℃ of baking ovens, get amorphous MoS 2Again with amorphous MoS 2Put in the quartz boat of silica tube, in tube furnace, be heated to 800 ℃, insulation 1h, furnace cooling then.A straight-through nitrogen in the silica tube.The MoS of gained 2Particle diameter increases to some extent, but still is sheet structure.

Claims (4)

1. the preparation method of a nanoscale flaky molybdenum disulfide, it is characterized in that: be molybdenum source and sulphur source with the four thio ammonium molybdate, oxalic acid is reductive agent, deionized water is a solvent, three's mol ratio is followed successively by 1: 1～2: 400～500, at 70～90 ℃ of following stirring reaction 1～1.5h of temperature, makes amorphous molybdenumdisulphide through chemical precipitation method, high-temperature heating treatment under nitrogen atmosphere obtains nanoscale flaky molybdenum disulfide then.
2. the preparation method of nanoscale flaky molybdenum disulfide according to claim 1 is characterized in that used reductive agent oxalic acid replaces with oxammonium hydrochloride.
3. the preparation method of nanoscale flaky molybdenum disulfide according to claim 1; it is characterized in that described high-temperature heating treatment is: under nitrogen atmosphere protection; the amorphous molybdenumdisulphide that chemical precipitation method is made places on the quartz boat and is heated to 800 ℃ in tube furnace; heating 1h, furnace cooling then.
4. the preparation method of nanoscale flaky molybdenum disulfide according to claim 1 is characterized in that described flaky molybdenum disulfide, and particle diameter is between 50～100nm.
CN 201010185621 2010-05-26 2010-05-26 Preparation method of nanoscale flaky molybdenum disulfide Pending CN101857273A (en)

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Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102398920A (en) * 2011-11-07 2012-04-04 北京航空航天大学 Method for preparing two-dimensional nano molybdenum disulfide by jet cavitation technology
CN102583546A (en) * 2012-02-18 2012-07-18 长安大学 Method for synthesizing mesoporous molybdenum disulphide by taking mesoporous silica molecular sieve as hard template
CN102616854A (en) * 2011-01-31 2012-08-01 中国科学院过程工程研究所 Preparation method of monodisperse spherical MoS2 ultrafine powder
CN103237922A (en) * 2010-12-06 2013-08-07 剑桥显示技术有限公司 Adhesion layer for solution-processed transition metal oxides on inert metal contacts
CN104628036A (en) * 2013-11-13 2015-05-20 嵇天浩 MS2 (M=Mo, W or V) nano-sheet preparation method
CN104692463A (en) * 2015-02-15 2015-06-10 清华大学 Method for preparing oil-soluble nano-molybdenum disulfide
CN105032596A (en) * 2015-08-05 2015-11-11 哈尔滨工业大学 Method for grading particle sizes of nanoscaled molybdenum disulfide by adjusting pH value
CN106298259A (en) * 2016-08-22 2017-01-04 河南师范大学 A kind of preparation method of 2H phase monolayer molybdenum disulfide nano sheet
CN106544054A (en) * 2016-11-25 2017-03-29 青岛大学 A kind of Heavy oil hydrogenation method
CN106654259A (en) * 2016-07-27 2017-05-10 北京航空航天大学 Preparation method for molybdenum disulfide nanosheet lithium ion battery negative electrode material by physical method
CN106622298A (en) * 2016-11-15 2017-05-10 天津大学 Layered multi-metal molybdenum sulfide catalyst and preparation method
CN106732800A (en) * 2016-11-25 2017-05-31 青岛大学 A kind of in-situ preparation method of lipophilic nano molybdenum disulfide catalyst and application
CN106995694A (en) * 2017-05-04 2017-08-01 安徽师范大学 The detection method of molybdenum sulfide quantum dot of sulfydryl modification and preparation method thereof and 2,4,6 trinitrotoluenes
WO2018044241A1 (en) * 2016-09-05 2018-03-08 Agency For Science, Technology And Research Method of producing a methanation catalyst
US10161922B2 (en) 2015-12-31 2018-12-25 National Tsing Hua University Molybdenum disulfide sensor and method for fabricating the same
CN112028121A (en) * 2020-09-28 2020-12-04 四川大学 Preparation method of amorphous molybdenum disulfide nano material based on photocatalytic synthesis
CN115108587A (en) * 2022-06-24 2022-09-27 上海交通大学医学院附属仁济医院 Molybdenum disulfide-doped two-dimensional carbon nitrogen compound matrix and preparation method and application thereof

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Cited By (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103237922A (en) * 2010-12-06 2013-08-07 剑桥显示技术有限公司 Adhesion layer for solution-processed transition metal oxides on inert metal contacts
CN103237922B (en) * 2010-12-06 2015-04-01 剑桥显示技术有限公司 Adhesion layer for solution-processed transition metal oxides on inert metal contacts
CN102616854A (en) * 2011-01-31 2012-08-01 中国科学院过程工程研究所 Preparation method of monodisperse spherical MoS2 ultrafine powder
CN102616854B (en) * 2011-01-31 2014-11-05 中国科学院过程工程研究所 Preparation method of monodisperse spherical MoS2 ultrafine powder
CN102398920A (en) * 2011-11-07 2012-04-04 北京航空航天大学 Method for preparing two-dimensional nano molybdenum disulfide by jet cavitation technology
CN102398920B (en) * 2011-11-07 2013-07-03 北京航空航天大学 Method for preparing two-dimensional nano molybdenum disulfide by jet cavitation technology
CN102583546A (en) * 2012-02-18 2012-07-18 长安大学 Method for synthesizing mesoporous molybdenum disulphide by taking mesoporous silica molecular sieve as hard template
CN104628036A (en) * 2013-11-13 2015-05-20 嵇天浩 MS2 (M=Mo, W or V) nano-sheet preparation method
CN104692463A (en) * 2015-02-15 2015-06-10 清华大学 Method for preparing oil-soluble nano-molybdenum disulfide
CN105032596A (en) * 2015-08-05 2015-11-11 哈尔滨工业大学 Method for grading particle sizes of nanoscaled molybdenum disulfide by adjusting pH value
US10161922B2 (en) 2015-12-31 2018-12-25 National Tsing Hua University Molybdenum disulfide sensor and method for fabricating the same
CN106654259A (en) * 2016-07-27 2017-05-10 北京航空航天大学 Preparation method for molybdenum disulfide nanosheet lithium ion battery negative electrode material by physical method
CN106298259B (en) * 2016-08-22 2018-03-06 河南师范大学 A kind of preparation method of 2H phases individual layer molybdenum disulfide nano sheet
CN106298259A (en) * 2016-08-22 2017-01-04 河南师范大学 A kind of preparation method of 2H phase monolayer molybdenum disulfide nano sheet
WO2018044241A1 (en) * 2016-09-05 2018-03-08 Agency For Science, Technology And Research Method of producing a methanation catalyst
CN106622298A (en) * 2016-11-15 2017-05-10 天津大学 Layered multi-metal molybdenum sulfide catalyst and preparation method
CN106732800B (en) * 2016-11-25 2019-06-11 青岛大学 A kind of in-situ preparation method and application of lipophilic nano molybdenum disulfide catalyst
CN106732800A (en) * 2016-11-25 2017-05-31 青岛大学 A kind of in-situ preparation method of lipophilic nano molybdenum disulfide catalyst and application
CN106544054A (en) * 2016-11-25 2017-03-29 青岛大学 A kind of Heavy oil hydrogenation method
CN106544054B (en) * 2016-11-25 2018-12-11 青岛大学 A kind of Heavy oil hydrogenation method
CN106995694A (en) * 2017-05-04 2017-08-01 安徽师范大学 The detection method of molybdenum sulfide quantum dot of sulfydryl modification and preparation method thereof and 2,4,6 trinitrotoluenes
CN106995694B (en) * 2017-05-04 2019-08-13 安徽师范大学 The detection method of mercapto-modified molybdenum sulfide quantum dot and preparation method thereof and 2,4,6- trinitrotoluene
CN112028121A (en) * 2020-09-28 2020-12-04 四川大学 Preparation method of amorphous molybdenum disulfide nano material based on photocatalytic synthesis
CN112028121B (en) * 2020-09-28 2021-08-03 四川大学 Preparation method of amorphous molybdenum disulfide nano material based on photocatalytic synthesis
CN115108587A (en) * 2022-06-24 2022-09-27 上海交通大学医学院附属仁济医院 Molybdenum disulfide-doped two-dimensional carbon nitrogen compound matrix and preparation method and application thereof

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