CN101857273A - Preparation method of nanoscale flaky molybdenum disulfide - Google Patents
Preparation method of nanoscale flaky molybdenum disulfide Download PDFInfo
- 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
- Authority
- CN
- China
- Prior art keywords
- molybdenum disulfide
- preparation
- flaky molybdenum
- nanoscale
- nanoscale flaky
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Lubricants (AREA)
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
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010185621 CN101857273A (en) | 2010-05-26 | 2010-05-26 | Preparation method of nanoscale flaky molybdenum disulfide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010185621 CN101857273A (en) | 2010-05-26 | 2010-05-26 | Preparation method of nanoscale flaky molybdenum disulfide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101857273A true CN101857273A (en) | 2010-10-13 |
Family
ID=42943472
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010185621 Pending CN101857273A (en) | 2010-05-26 | 2010-05-26 | Preparation method of nanoscale flaky molybdenum disulfide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101857273A (en) |
Cited By (17)
| 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 |
| CN106622298A (en) * | 2016-11-15 | 2017-05-10 | 天津大学 | Layered multi-metal molybdenum sulfide catalyst and preparation 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 |
| 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6156693A (en) * | 1998-10-09 | 2000-12-05 | Penn State Research Foundation | Method for preparing a highly active, unsupported high-surface-area ub. MoS.s2 catalyst |
-
2010
- 2010-05-26 CN CN 201010185621 patent/CN101857273A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6156693A (en) * | 1998-10-09 | 2000-12-05 | Penn State Research Foundation | Method for preparing a highly active, unsupported high-surface-area ub. MoS.s2 catalyst |
Non-Patent Citations (3)
| Title |
|---|
| 《广东化工》 20071231 王泉山等 液相化学法合成纳米二硫化钼研究进展 第33页，1.1.2 直接还原法 1-4 第34卷, 第9期 2 * |
| 《无机化学学报》 20090131 吴壮志等 纳米MoS2空心球的制备与表征 第65-69页 1-4 第25卷, 第1期 2 * |
| 《材料导报》 20030930 杨刚等 纳米二硫化钼的形态调控制备研究 第63页1.1 MoS2纳米颗粒的制备；2.1 二硫化钼微晶的扫描电镜形貌分析 1-4 第17卷, 2 * |
Cited By (25)
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| CN106544054B (en) * | 2016-11-25 | 2018-12-11 | 青岛大学 | A kind of Heavy oil hydrogenation method |
| CN106544054A (en) * | 2016-11-25 | 2017-03-29 | 青岛大学 | A kind of Heavy oil hydrogenation 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 |
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101857273A (en) | Preparation method of nanoscale flaky molybdenum disulfide | |
| Deshmukh et al. | Chemical synthesis of ZnO nanorods: Investigations of electrochemical performance and photo-electrochemical water splitting applications | |
| Pusawale et al. | Chemical synthesis of nanocrystalline SnO2 thin films for supercapacitor application | |
| Chen et al. | Microwave–hydrothermal crystallization of polymorphic MnO2 for electrochemical energy storage | |
| Chen et al. | Preparation and characterization of nanocrystalline zinc oxide by a novel solvothermal oxidation route | |
| CN108565434B (en) | Preparation method of tungsten disulfide/nitrogen and sulfur co-doped graphene compound | |
| CN103613136A (en) | Preparation method of square MoO3 nanosheet | |
| CN105381807A (en) | Preparation method of molybdenum diselenide/cobalt diselenide nanocomposite | |
| Aghazadeh et al. | Preparation of Mn5O8 and Mn3O4 nano-rods through cathodic electrochemical deposition-heat treatment (CED-HT) | |
| CN103539210A (en) | Preparation method of cobalt molybdate microcrystals | |
| CN104401980A (en) | Hydrothermal preparation method of Fe2O3-SnO2/graphene ternary composite nano-material | |
| CN105329946A (en) | Molybdenum disulfide nanosheet with rich active sites as well as preparation method and application of molybdenum disulfide nanosheet | |
| CN105060347A (en) | Method for synthesizing ultrathin molybdenum disulfide nanocrystals | |
| Mao et al. | A new route for synthesizing VO2 (B) nanoribbons and 1D vanadium-based nanostructures | |
| CN110482608A (en) | A kind of flower-shaped tungsten disulfide microballoon and preparation method thereof | |
| Ma et al. | Supercritical preparation of hexagonal γ-alumina nanosheets and its electrocatalytic properties | |
| Ghosh et al. | Effect of ageing on Sn 6 O 4 (OH) 4 in aqueous medium—simultaneous production of SnO and SnO 2 nanoparticles at room temperature | |
| Xie et al. | Shape-controlled synthesis of zinc phosphate nanostructures by an aqueous solution route at room temperature | |
| Lei et al. | Liquid phase deposition (LPD) of TiO2 thin films as photoanodes for cathodic protection of stainless steel | |
| Schmidt et al. | Molybdenum-based two-dimensional materials: Synthesis, dispersion, exfoliation and thin film deposition | |
| Tripathi et al. | Ecofriendly approach to making graphene–tin/tin oxide nanocomposite electrodes for energy storage | |
| CN109231276B (en) | Preparation of alpha-MnO by reducing potassium permanganate with sulfamic acid2Method and application of nanowires | |
| CN105206816B (en) | A kind of preparation method of nickel sulfide graphene nanocomposite material | |
| Bronusiene et al. | Effect of ascorbic acid on the properties of tin sulfide films for supercapacitor application | |
| Zhang et al. | Facile fabrication of VO2 (M) by thermolysis of ammonium metavanadate (NH4VO3) under sealed condition |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20101013 |