CN103613137B - Hydrothermal synthesis method of molybdenum disulfide nanoflower - Google Patents
Hydrothermal synthesis method of molybdenum disulfide nanoflower Download PDFInfo
- Publication number
- CN103613137B CN103613137B CN201310547151.4A CN201310547151A CN103613137B CN 103613137 B CN103613137 B CN 103613137B CN 201310547151 A CN201310547151 A CN 201310547151A CN 103613137 B CN103613137 B CN 103613137B
- Authority
- CN
- China
- Prior art keywords
- molybdenum disulfide
- hydrothermal synthesis
- reaction
- nano flower
- synthesis method
- 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.)
- Expired - Fee Related
Links
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 27
- 239000002057 nanoflower Substances 0.000 title claims abstract description 27
- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 230000002829 reductive effect Effects 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 7
- 239000005864 Sulphur Substances 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 5
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 5
- 239000012535 impurity Substances 0.000 abstract description 7
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 4
- 239000011733 molybdenum Substances 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 239000011593 sulfur Substances 0.000 abstract description 2
- 229910052717 sulfur Inorganic materials 0.000 abstract description 2
- 239000003638 chemical reducing agent Substances 0.000 abstract 2
- 125000001741 organic sulfur group Chemical group 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 16
- 239000002086 nanomaterial Substances 0.000 description 6
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910001867 inorganic solvent Inorganic materials 0.000 description 2
- 239000003049 inorganic solvent Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N hydrogen thiocyanate Natural products SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- 150000002751 molybdenum Chemical class 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a hydrothermal synthesis method of molybdenum disulfide nanoflowers, which is mainly characterized by adding an inorganic molybdenum source, an organic sulfur source and a proper reducing agent into deionized water, uniformly mixing, transferring into a reaction autoclave, and heating at a high temperature for 24 hours. And washing the obtained solution for many times, performing centrifugal separation, and finally drying to obtain black solid powder, namely the molybdenum disulfide nanoflower. The invention has the beneficial effects that: the whole reaction and drying process is carried out in a sealed environment, so that direct exposure to air is avoided, and the purity of the product is ensured; the reducing agent can be used as a sulfur source and a catalyst, so that impurities are not generated, and the purity of the product is further improved.
Description
Technical field
The present invention relates to a kind of synthetic method of nano flower, particularly relate to the hydrothermal synthesis method of a kind of molybdenum disulfide nano flower.
Background technology
Nano material refers to the material having at least one dimension to be in nanoscale scope or to be made up of as elementary cell them in three dimensions.Nano material, due to its small size, can produce significant change in physics and chemistry properties usually.These changes, make applications to nanostructures research be developed rapidly, and are widely used in industries such as traditional material, medical device, electronics, coating.
Molybdenumdisulphide has hexagonal layered structure, is fixed between layers by Van der Waals force.The characteristic of this structure, is widely used in solid lubricant, Hydrobon catalyst, semiconductor material, intercalation material and lithium cell, also has very large purposes at aerospace field.The molybdenumdisulphide specific surface area of nanostructure is large, and surfactivity is high, is also having very wide application prospect as in catalyzer.
The performance of nano material and its preparation method have and contact closely.Nano molybdenum disulfide preparation generally can be divided into chemical method and Physical.Physical method prepares molybdenumdisulphide as mechanical attrition method, sublimation recrystallization method etc., although less to the destruction of lattice, the pattern of product is comparatively single, and fineness is limited.And the product purity that chemical process is urged to help method etc. to obtain as sluggish precipitation, hydrothermal method, solvent-thermal method, tensio-active agent is higher, morphology controllable, fineness is close to nano level.Nanometer flower-shaped structure has the character that high surface area, high reaction activity etc. are better than the nano material of other shapes, and as having very high catalytic activity, nano flower film has super-hydrophobicity, is applied to the electrochemical activity that electrode can improve electrode.
Existing employing hydrothermal method produces the technique of molybdenum disulfide nano flower, and when reactions steps, reaction environment can not get paying attention to always, causes whole reactions steps, all exposes in atmosphere, thus makes the product purity that obtains low.The present invention adopts high―temperature nuclei in sealed environment, and uses the method for reductive agent accelerated reaction process, and the molybdenum disulfide nano flower specific surface area of preparation is large, and purity is high.
Summary of the invention
The object of the invention is to the shortcoming and defect overcoming above-mentioned prior art, the hydrothermal synthesis method of a kind of molybdenum disulfide nano flower is provided, solve existing Hydrothermal Synthesis and obtain the general not high defect of molybdenum disulfide nano flower purity.
Object of the present invention is achieved through the following technical solutions: a kind of hydrothermal synthesis method of molybdenum disulfide nano flower, comprises the following steps:
(1) prepare inorganic molybdenum source, organosulfur source and reductive agent, wherein inorganic molybdenum source accounts for the 40-50% of charging capacity, and organosulfur source accounts for the 40-50% of charging capacity, and reductive agent accounts for the 1-5% of charging capacity.
(2) material prepared in step (1) is all mixed in deionized water, and carries out stirring and make Homogeneous phase mixing;
(3) mixed solution that step (2) obtains is put into reaction autoclave and carry out reacting by heating, temperature is 180 DEG C ~ 240 DEG C, and heat-up time is 20 ~ 28h;
(4) the solution cooling obtained in waiting step (3), the washing then circulated to this solution and centrifugation, after circulation 3-5 time, then carry out drying by the throw out obtained, obtain molybdenum disulfide nano colored.
In the present invention, mixed solution is put into reaction autoclave sealing and carry out pyroreaction, provide a good reaction environment, can not contact with air, can not react with air, decrease impurity, and the present invention is the washing and centrifugation carrying out circulating, further reduces impurity.
Inorganic molybdenum source described in step (1) is molybdenum salt or molybdate, is preferably Sodium orthomolybdate.
Organosulfur source described in step (1) is the organic compound of sulfur-bearing, is preferably thiocarbamide.
Reductive agent described in step (1) is hydrazine or thiocyanide or thiocarbamide or thioacetamide, these compounds can not introduce new impurity as reductive agent, in the present invention, reductive agent adopts thiocarbamide, thiocarbamide has dual-use function in the reaction, not only can as sulphur source but also as reductive agent, do not have impurity to produce, ensure that the purity of product.
Mixed solution described in step (3) first should put into a lining container, close good after put into reaction autoclave again and carry out pyroreaction, in the present invention, lining container adopts tetrafluoroethylene, and when avoiding reacting, in autoclave body, metal ion participation reaction generation is polluted.
Washing described in step (4) refers to and adopts the alternately washing of inorganic solvent and organic solvent, removes organic and inorganic raw material remaining in product.
Described inorganic solvent adopts ionized water or clear water, and organic solvent adopts alcohol.
Drying described in step (4) carries out drying under referring to vacuum throw out being placed on 55 DEG C-65 DEG C, dry in vacuum, further ensures the purity of product.
The invention has the beneficial effects as follows:
(1), in whole reaction of the present invention, dry process, be all carry out in sealed environment, avoid direct exposed to air, ensure that the purity of product;
(2) the present invention adopts reductive agent namely as sulphur source, also can be used as catalyzer, does not have impurity and produces, improve the purity of product further.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of Hydrothermal Synthesis molybdenum disulfide nano flower in embodiment 1;
Fig. 2 is the X ray diffracting spectrum of Hydrothermal Synthesis molybdenum disulfide nano flower in embodiment 1;
Fig. 3 is the super-resolution transmission electron microscope picture of Hydrothermal Synthesis molybdenum disulfide nano flower in embodiment 2.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail:
[embodiment 1]
A hydrothermal synthesis method for molybdenum disulfide nano flower, comprises the following steps:
(1) prepare 0.72g Sodium orthomolybdate and 1g thioacetamide, wherein thioacetamide namely as sulphur source also as reductive agent;
(2) material of above-mentioned preparation is all mixed in 30mL deionized water, and carries out stirring and make Homogeneous phase mixing;
(3) mixed solution that step (2) obtains is put into reaction autoclave to heat, material in mixed solution is reacted, in reaction, temperature is 180 DEG C, and heat-up time is 28h;
(4) the solution naturally cooling obtained in waiting step (3), the washing then circulated to this solution and centrifugation, circulate after 3 times, then the throw out obtained carried out drying under the vacuum of 65 DEG C, obtain molybdenum disulfide nano flower.
Be the scanning electron microscope (SEM) photograph of the Hydrothermal Synthesis molybdenum disulfide nano flower of the present embodiment as Fig. 1, as can be seen from the figure, adopt we to prepare molybdenum disulfide nano flower and present homogeneous laminate structure, specific surface area is large, is conducive to the application as catalyzer; Fig. 2 is the X ray diffracting spectrum of the Hydrothermal Synthesis molybdenum disulfide nano flower of the present embodiment, as can be seen from the figure, adopts the diffraction peak without other impurity in the product of present method synthesis.
[embodiment 2]
A hydrothermal synthesis method for molybdenum disulfide nano flower, comprises the following steps:
(1) prepare 0.72g Sodium orthomolybdate and 1.14g thiocarbamide, wherein thiocarbamide both as sulphur source also as reductive agent;
(2) material of above-mentioned preparation is all mixed in deionized water, and carries out stirring and make Homogeneous phase mixing;
(3) mixed solution that step (2) obtains is put into polytetrafluoroethyllining lining container, then this container is put into reaction autoclave and heat, material in mixed solution is reacted, in reaction, temperature is 240 DEG C, and heat-up time is 20h;
(4) the solution naturally cooling obtained in waiting step (3), the washing then circulated to this solution and centrifugation, circulate after 5 times, then the throw out obtained carried out drying under the vacuum of 55 DEG C, obtain molybdenum disulfide nano flower.
It is the super-resolution transmission electron microscope picture of the Hydrothermal Synthesis molybdenum disulfide nano flower of the present embodiment as Fig. 3.
[embodiment 3]
A hydrothermal synthesis method for molybdenum disulfide nano flower, comprises the following steps:
(1) prepare 0.84g Sodium orthomolybdate and 1.20g thiocarbamide, wherein thiocarbamide both as sulphur source also as reductive agent;
(2) material of above-mentioned preparation is all mixed in deionized water, and carries out stirring and make Homogeneous phase mixing;
(3) mixed solution that step (2) obtains is put into polytetrafluoroethyllining lining container, then this container is put into reaction autoclave and heat, material in mixed solution is reacted, in reaction, temperature is 200 DEG C, and heat-up time is 24h;
(4) the solution naturally cooling obtained in waiting step (3), the washing then circulated to this solution and centrifugation, circulate after 4 times, then the throw out obtained carried out drying under the vacuum of 60 DEG C, obtain molybdenum disulfide nano flower.
Claims (1)
1. a hydrothermal synthesis method for molybdenum disulfide nano flower, is characterized in that: comprise the following steps:
(1) prepare 0.72g Sodium orthomolybdate and 1g thioacetamide, wherein thioacetamide both as sulphur source also as reductive agent;
(2) material of above-mentioned preparation is all mixed in 30mL deionized water, and carries out stirring and make Homogeneous phase mixing;
(3) mixed solution that step (2) obtains is put into reaction autoclave to heat, material in mixed solution is reacted, in reaction, temperature is 180 DEG C, and heat-up time is 28h;
(4) the solution naturally cooling obtained in waiting step (3), the washing then circulated to this solution and centrifugation, circulate after 3 times, then the throw out obtained carried out drying under the vacuum of 65 DEG C, obtain molybdenum disulfide nano flower.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201310547151.4A CN103613137B (en) | 2013-11-08 | 2013-11-08 | Hydrothermal synthesis method of molybdenum disulfide nanoflower |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201310547151.4A CN103613137B (en) | 2013-11-08 | 2013-11-08 | Hydrothermal synthesis method of molybdenum disulfide nanoflower |
Publications (2)
Publication Number | Publication Date |
---|---|
CN103613137A CN103613137A (en) | 2014-03-05 |
CN103613137B true CN103613137B (en) | 2015-07-29 |
Family
ID=50163867
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201310547151.4A Expired - Fee Related CN103613137B (en) | 2013-11-08 | 2013-11-08 | Hydrothermal synthesis method of molybdenum disulfide nanoflower |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN103613137B (en) |
Families Citing this family (28)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105366725B (en) * | 2014-08-29 | 2017-02-15 | 中国科学院大连化学物理研究所 | Method for hydro-thermally synthesizing MoS2 nanoflower with sulfur-containing biological reagent as sulfur source |
CN105439203B (en) * | 2014-09-25 | 2017-09-22 | 中国科学院大连化学物理研究所 | A kind of surface amphiphilic nano molybdenum disulfide hydrogenation catalyst and preparation method and application |
CN104649323B (en) * | 2015-01-21 | 2016-06-22 | 济南大学 | A kind of preparation method of strip molybdenum trioxide |
CN105624756B (en) * | 2015-12-29 | 2018-01-19 | 中国石油大学(华东) | A kind of high activity molybdenum sulfide film elctro-catalyst and preparation method thereof |
CN106994357B (en) * | 2016-01-22 | 2019-07-19 | 天津大学 | A kind of the molybdenum disulfide material and its synthetic method of witch culture |
CN105712404B (en) * | 2016-04-21 | 2018-05-18 | 华南师范大学 | A kind of MoS2The preparation method of quantum dot |
CN106311282B (en) * | 2016-08-09 | 2019-01-15 | 河南工程学院 | A kind of porous monolayer 1T MoS2The preparation method and applications of nanometer sheet |
CN106381190B (en) * | 2016-08-16 | 2019-07-23 | 镇江市高等专科学校 | Graphite-like carbon nitrence-molybdenum disulfide composite nano materials, Its Preparation Method And Use |
CN108083336B (en) * | 2016-11-23 | 2022-05-17 | 中国科学院大连化学物理研究所 | Method for preparing molybdenum disulfide with various shapes by organic amine-guided hydrothermal method |
CN108498858B (en) * | 2017-02-24 | 2020-02-14 | 中国科学院上海硅酸盐研究所 | Molybdenum disulfide nanosheet in-situ modified biological ceramic support and preparation method and application thereof |
CN106994360A (en) * | 2017-04-05 | 2017-08-01 | 江苏大学 | A kind of preparation method of Z configurations visible light catalytic decomposition water composite |
CN107102039B (en) * | 2017-04-24 | 2018-04-27 | 太原理工大学 | A kind of preparation method of Ag doping molybdenum disulfide composite material mixture |
CN108786855A (en) * | 2017-05-04 | 2018-11-13 | 中国计量大学 | A kind of preparation method of mesoporous molybdenum disulfide visible light catalyst material and its application in degradation antibiotic waste water field |
CN107804873B (en) * | 2017-11-20 | 2019-08-27 | 吉林大学 | The method and application of the flower-shaped molybdenum disulfide electrode material of one step hydrothermal synthesis |
CN108314084B (en) * | 2018-02-09 | 2019-12-20 | 西北工业大学 | Preparation method of metal phase molybdenum disulfide nanospheres |
CN108493409B (en) * | 2018-03-12 | 2021-02-26 | 安徽大学 | Preparation method of nitrogen-doped carbon-coated flower-shaped nano molybdenum disulfide |
CN108325548B (en) * | 2018-03-15 | 2023-03-31 | 内蒙古大学 | Molybdenum sulfide-based catalyst for preparing low-carbon alcohol from synthesis gas and preparation method thereof |
CN109174131A (en) * | 2018-08-29 | 2019-01-11 | 厦门大学 | The molybdenum disulfide nano floral material and its synthetic method of nickel cobalt modification and application |
CN109019616A (en) * | 2018-09-30 | 2018-12-18 | 江南大学 | A kind of preparation and application of silica/molybdenum disulfide three-dimensional hybrid material |
CN109721105A (en) * | 2018-12-29 | 2019-05-07 | 银隆新能源股份有限公司 | Molybdenum disulfide nano floral material and preparation method thereof, molybdenum disulfide nano flower negative electrode material and preparation method thereof and battery |
CN109762369B (en) * | 2019-02-28 | 2021-02-26 | 中山大学惠州研究院 | Preparation method of water-based high-dispersity nano molybdenum disulfide |
CN109913292B (en) * | 2019-04-04 | 2022-04-15 | 上海绿晟环保科技有限公司 | Multifunctional additive for cutting fluid and preparation method and application thereof |
CN111661876A (en) * | 2020-05-29 | 2020-09-15 | 江苏大学 | Preparation method and application of petal-shaped two-dimensional molybdenum sulfide nano material |
CN112490345A (en) * | 2020-11-25 | 2021-03-12 | 中国电子科技集团公司第十八研究所 | Thermal battery anode material and preparation method thereof |
CN113044883B (en) * | 2021-03-15 | 2022-10-14 | 陕西科技大学 | Preparation method of three-dimensional embroidered spherical tungsten disulfide electrode material |
CN113502489B (en) * | 2021-06-24 | 2022-09-23 | 杭州师范大学 | Preparation method and application of electrocatalyst for reduction of alkyne into olefin |
CN115254084B (en) * | 2022-02-17 | 2023-12-19 | 昆明理工大学 | Preparation method and application of composite catalyst with black material loaded with metal nano particles |
CN114854387B (en) * | 2022-05-24 | 2023-02-03 | 中国石油大学(北京) | Nano flower-nano sheet dual-inorganic nano profile control and flooding system and application thereof |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101851006A (en) * | 2010-06-08 | 2010-10-06 | 南开大学 | Method for preparing MoS2 microspheres by solvent hot method |
CN102701281A (en) * | 2012-05-14 | 2012-10-03 | 无锡润鹏复合新材料有限公司 | Preparation method of flower-shaped hollow molybdenum disulfide microspheres |
CN103073060A (en) * | 2013-03-05 | 2013-05-01 | 苏州惠丰润滑油有限公司 | Method for preparing hexagonal molybdenum disulfide nanosheet as anti-friction additive |
-
2013
- 2013-11-08 CN CN201310547151.4A patent/CN103613137B/en not_active Expired - Fee Related
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101851006A (en) * | 2010-06-08 | 2010-10-06 | 南开大学 | Method for preparing MoS2 microspheres by solvent hot method |
CN102701281A (en) * | 2012-05-14 | 2012-10-03 | 无锡润鹏复合新材料有限公司 | Preparation method of flower-shaped hollow molybdenum disulfide microspheres |
CN103073060A (en) * | 2013-03-05 | 2013-05-01 | 苏州惠丰润滑油有限公司 | Method for preparing hexagonal molybdenum disulfide nanosheet as anti-friction additive |
Non-Patent Citations (3)
Title |
---|
"A facile method to prepare MoS2 with nanoflower-like morphology";Ronghui Wei et al.;《Materials Chemistry and Physics》;20081231;第108卷;第188-191页 * |
"金属硫化物微/纳米材料的水热合成";王博;《中国优秀硕士学位论文全文数据库》;20121016;正文第16、18-19页 * |
任萍等."水热法制备二硫化钼微球花及其结构表征".《有色金属(冶金部分)》.2011,(第10期),第47-49、53页. * |
Also Published As
Publication number | Publication date |
---|---|
CN103613137A (en) | 2014-03-05 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN103613137B (en) | Hydrothermal synthesis method of molybdenum disulfide nanoflower | |
CN102070140B (en) | Method for preparing high-specific surface area graphene material by utilizing strong base chemical treatment | |
CN107376971B (en) | Synthetic method of graphite-like carbon nitride/molybdenum disulfide nano composite material | |
CN102583336B (en) | Preparation method of magnetic-functionalized graphene composite material | |
Vadivel et al. | d-Pencillamine assisted microwave synthesis of Bi2S3 microflowers/RGO composites for photocatalytic degradation—A facile green approach | |
Luo et al. | Preparation and photocatalytic activity of TiO 2-loaded Ti 3 C 2 with small interlayer spacing | |
CN108439470B (en) | Preparation method and application of molybdenum disulfide nanosheet | |
Peng et al. | Synthesis of a sulfur-graphene composite as an enhanced metal-free photocatalyst | |
Salavati-Niasari et al. | Surfactant-free fabrication of copper sulfides (CuS, Cu 2 S) via hydrothermal method | |
Zhao et al. | Synthesis of graphene-based CdS@ CuS core-shell nanorods by cation-exchange for efficient degradation of ciprofloxacin | |
CN106732668A (en) | A kind of hydrothermal preparing process of flower-shaped molybdenum bisuphide/cupric oxide composite nano materials | |
CN109748322B (en) | Synthesis method and application of alpha-MnS nano particles and alpha-MnS/rGO composite material | |
CN105126820B (en) | Preparation method of three-dimensional graphene/tungsten-based nanosheet/magnesium-doped zinc oxide layer-by-layer assembly structure | |
CN106058206A (en) | Composite material of flower-like carbon-loaded MoS2 nanoparticles and preparation method and application thereof | |
CN108483502A (en) | A kind of preparation method and application of rhenium disulfide nanometer sheet | |
CN110690419B (en) | Transition metal chalcogenide composite material and preparation method and application thereof | |
CN103613136A (en) | Preparation method of square MoO3 nanosheet | |
CN105944721A (en) | Hydrothermal preparation method of flaky nano copper oxide/graphene composite materials | |
CN105923625B (en) | A kind of preparation method of graphene-supported uniform single oxide quantum dot | |
CN108217730A (en) | A kind of method of hydrothermal synthesis molybdenum disulfide nano sheet under cryogenic conditions | |
CN103641169A (en) | Synthetic method of Bi2S3-MoS2 nanometer heterostructure | |
CN109734132A (en) | A method of controlling synthesis of carbon/molybdenum disulfide particle in mixed solvent system | |
CN104857945A (en) | Preparation method of zinc oxide/carbon micro-sphere composite material | |
CN105834446A (en) | Synthetic method for ultrathin layered NiO-CoOx nanosheet loading NiCo nano particle composite | |
CN112939083A (en) | Molybdenum disulfide/ferroferric oxide/graphene nanosheet composite wave absorber and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150729 Termination date: 20161108 |
|
CF01 | Termination of patent right due to non-payment of annual fee |