CN100548891C - A kind of method for preparing flower-shaped molybdenum disulfide micro-balloon - Google Patents
A kind of method for preparing flower-shaped molybdenum disulfide micro-balloon Download PDFInfo
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- CN100548891C CN100548891C CNB2007100698738A CN200710069873A CN100548891C CN 100548891 C CN100548891 C CN 100548891C CN B2007100698738 A CNB2007100698738 A CN B2007100698738A CN 200710069873 A CN200710069873 A CN 200710069873A CN 100548891 C CN100548891 C CN 100548891C
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- Prior art keywords
- balloon
- molybdenum disulfide
- reactor
- flower
- shaped molybdenum
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- 238000000034 method Methods 0.000 title claims abstract description 22
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000654 additive Substances 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract description 3
- 239000011734 sodium Substances 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 3
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 3
- 230000010355 oscillation Effects 0.000 claims description 2
- GROMGGTZECPEKN-UHFFFAOYSA-N sodium metatitanate Chemical compound [Na+].[Na+].[O-][Ti](=O)O[Ti](=O)O[Ti]([O-])=O GROMGGTZECPEKN-UHFFFAOYSA-N 0.000 claims description 2
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 238000000643 oven drying Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000004005 microsphere Substances 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 230000018199 S phase Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000002638 heterogeneous catalyst Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
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Abstract
The method for preparing flower-shaped molybdenum disulfide micro-balloon disclosed by the invention, employing be hydrothermal synthesis method, step is as follows: with Na
2MoO
4, CS (NH
2)
2Place reactor with inorganic additives, and add the deionized water of 60% reactor capacity, reactor is sealed, put into 150～250 ℃ of thermostat containers, be incubated after at least 12 hours, be cooled to room temperature, with deionized water eccentric cleaning product to pH value is neutral, and drying gets flower-shaped molybdenum disulfide micro-balloon.The inventive method technology is simple to operation, and cost is low, and the product purity height that makes is expected to produce in enormous quantities.
Description
Technical field
The present invention relates to inorganic materials molybdenumdisulphide (MoS
2) the preparation method of preparation field, especially flower-shaped molybdenum disulfide micro-balloon.
Background technology
Nano molybdenum disulfide (MoS
2) because of having performances such as very high specific surface area and good light, electricity, lubricated, catalysis, be with a wide range of applications at aspects such as electronic probe, solid lubrication, heterogeneous catalyst, gas storage material and photocell materials.Nanometer MoS
2Comprise nanoparticle, nano thin-layer, soccerballene shape nanoparticle and nanotube.Under certain preparation condition, MoS
2Nano thin-layer can spontaneous composition cube or the special micrometer structure of spheric, and the latter promptly is called MoS
2Nano microsphere.MoS
2Nano microsphere has more high-specific surface area, more passage, has better properties in its Application Areas.Be used to prepare nanometer MoS so far
2Method mainly contain high temperature (800～1300 ℃) thermal reaction method (Gu as gas/reaction, chemical transformation, electron radiation, original position heating) and low temperature (～400 ℃) solvent process for thermosynthesizing (, solution chemistry synthetic as template synthesized).Adopt the elevated temperature heat reaction method to prepare flower-shaped MoS
2The bibliographical information of microballoon seldom, and cost height, complex process; Though and the low temperature method cost is lower, prepared MoS
2Mostly be one-dimentional structure or soccerballene shape nanoparticle, also do not adopt low temperature to prepare flower-shaped MoS at present
2The report of microballoon.
Summary of the invention
The purpose of this invention is to provide the flower-shaped MoS of preparation that a kind of technology is simple, cost is low
2The method of microballoon.
The flower-shaped MoS of preparation of the present invention
2The method of microballoon, employing be hydrothermal synthesis method, step is as follows:
With Na
2MoO
4, CS (NH
2)
2Place reactor with inorganic additives, Na
2MoO
4And CS (NH
2)
2Mass ratio be 0.5～1, inorganic additives and Na
2MoO
4Mass ratio be 0.2～1, and add the deionized water of 60% reactor capacity, reactor is sealed, put into 150～250 ℃ of thermostat containers, be incubated after at least 12 hours, be cooled to room temperature, with deionized water eccentric cleaning product to pH value is neutral, drying gets flower-shaped molybdenum disulfide micro-balloon, and the inorganic additives of saying is Tungstenic compound or titanium-containing compound.
Among the present invention, said Tungstenic compound can be Tungsten oxide 99.999, wolframic acid or sodium wolframate, and titanium-containing compound can adopt titanium oxide, metatitanic acid or sodium titanate; Preferred Tungstenic compound.
In the preparation process of the present invention, all reagent are commerical prod, need not loaded down with trivial details preparation.
In the preparation process of the present invention, preferred calorstat temperature is 170～210 ℃.
In the preparation process of the present invention, mix, can before the reactor sealing, carry out sonic oscillation in order to make reactant.
The present invention adopts hydrothermal synthesis method to prepare flower-shaped molybdenum disulfide micro-balloon, and technology is simple to operation, and cost is low, and the product purity height that makes is expected to produce in enormous quantities.
Description of drawings
Fig. 1 is field emission scanning electron microscope (SEM) photo of the flower-shaped molybdenum disulfide micro-balloon that makes with the inventive method;
Fig. 2 is that the Electronic Speculum of the flower-shaped molybdenum disulfide micro-balloon that makes with the inventive method can spectrogram (EDX);
Fig. 3 is X-ray diffraction (XRD) spectrogram of the flower-shaped molybdenum disulfide micro-balloon that makes with the inventive method.
Embodiment
Further specify the present invention below in conjunction with example.
Embodiment 1
With 0.2g Na
2MoO
4, 0.2g CS (NH
2)
2Place the 50ml reactor with the 0.1g wolframic acid, behind the ultrasonic 30min, with reactor sealing and to put into temperature be 180 ℃ baking oven, behind the insulation 16h, being cooled to room temperature, is neutral with deionized water centrifuge washing product to pH value, gets black powder shape product behind 60 ℃ of oven dryings.Directly observe as Fig. 1 (a, b) under field emission scanning electron microscope, can find the generation of a large amount of flower-shaped microballoons, purity reaches 95%.These microballoons are formed by the thin layer of flaky thick about 8～30 nanometer of layer, and microsphere diameter is 500～700nm.Only have Mo and S in this globe of EDX analysis revealed of Fig. 2, and the atomic ratio of Mo and S is 1: 1.96, with MoS
2Atomic ratio approaching.The XRD diffraction of Fig. 3 has confirmed that further product is MoS
2Microballoon, phase composite are the MoS of six side's phases (2H)
2(with reference to card No:37-1492) and a small amount of rhombohedron be the MoS of (3R) mutually
2(with reference to card No:17-0744).Wolframic acid has brought out MoS as inorganic additives
2After the growth of microballoon, be not retained in the product, but in centrifugal process, be cleaned.
Embodiment 2
With 0.2g Na
2MoO
4, 0.2g CS (NH
2)
2Place the 50ml reactor with the 0.1g titanium oxide, behind the ultrasonic 30min, with reactor sealing and to put into temperature be 150 ℃ baking oven, behind the insulation 24h, being cooled to room temperature, is neutral with deionized water centrifuge washing product to pH value, gets black powder shape product behind 60 ℃ of oven dryings.The pattern of oven dry after product, structure etc. are all identical with embodiment 1.
Embodiment 3
With 0.2g Na
2MoO
4, 0.4g CS (NH
2)
2Place the 50ml reactor with the 0.04g metatitanic acid, behind the ultrasonic 30min, with reactor sealing and to put into temperature be 200 ℃ baking oven, behind the insulation 24h; Being cooled to room temperature, is neutral with deionized water centrifuge washing product to pH value, gets black powder shape product behind 60 ℃ of oven dryings.The pattern of oven dry after product, structure etc. are all identical with embodiment 1.
Embodiment 4
With 0.2g Na
2MoO
4, 0.3g CS (NH
2)
2Place the 50ml reactor with the 0.2g Tungsten oxide 99.999, behind the ultrasonic 30min, with reactor sealing and to put into temperature be 250 ℃ baking oven, insulation 12h; To be cooled to room temperature, be neutral with deionized water centrifuge washing product to pH value, get black powder shape product behind 60 ℃ of oven dryings.The pattern of oven dry after product, structure etc. are all identical with embodiment 1.
Claims (3)
1. method for preparing flower-shaped molybdenum disulfide micro-balloon is characterized in that step is as follows:
With Na
2MoO
4, CS (NH
2)
2Place reactor with inorganic additives, Na
2MoO
4And CS (NH
2)
2Mass ratio be 0.5～1, inorganic additives and Na
2MoO
4Mass ratio be 0.2～1, and add the deionized water of 60% reactor capacity, with the reactor sealing, put into 150～250 ℃ of thermostat containers, be incubated after at least 12 hours, being cooled to room temperature, is neutral with deionized water eccentric cleaning product to pH value, drying, get flower-shaped molybdenum disulfide micro-balloon, said inorganic additives is Tungstenic compound or titanium-containing compound, and Tungstenic compound is Tungsten oxide 99.999, wolframic acid or sodium wolframate, and titanium-containing compound is titanium oxide, metatitanic acid or sodium titanate.
2. by the described method for preparing flower-shaped molybdenum disulfide micro-balloon of claim 1, it is characterized in that calorstat temperature is 170～210 ℃.
3. by the described method for preparing flower-shaped molybdenum disulfide micro-balloon of claim 1, it is characterized in that carrying out sonic oscillation before the reactor sealing.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100698738A CN100548891C (en) | 2007-07-03 | 2007-07-03 | A kind of method for preparing flower-shaped molybdenum disulfide micro-balloon |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100698738A CN100548891C (en) | 2007-07-03 | 2007-07-03 | A kind of method for preparing flower-shaped molybdenum disulfide micro-balloon |
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| Publication Number | Publication Date |
|---|---|
| CN101113021A CN101113021A (en) | 2008-01-30 |
| CN100548891C true CN100548891C (en) | 2009-10-14 |
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Families Citing this family (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103086436A (en) * | 2011-11-03 | 2013-05-08 | 中国科学院兰州化学物理研究所 | Preparation method of nano-molybdenum disulfide |
| 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 |
| CN102701281B (en) * | 2012-05-14 | 2015-09-16 | 无锡润鹏复合新材料有限公司 | A kind of preparation method of flower-shaped molybdenumdisulphide tiny balloon |
| CN102849798B (en) * | 2012-08-29 | 2014-02-26 | 北京化工大学 | Molybdenum disulfide nano-sheet film material and its preparation methods |
| CN102992281B (en) * | 2012-12-10 | 2015-04-22 | 江苏大学 | Nanometer flower-shaped MoSe2 and preparation method thereof |
| CN103466710B (en) * | 2013-09-04 | 2014-10-08 | 东南大学 | Method for preparing three-dimensional spumescence MoS2 |
| CN103613138B (en) * | 2013-11-21 | 2015-09-16 | 镇江市高等专科学校 | A kind of preparation method of nanometer lubricating additive of cadmium doping molybdenumdisulphide |
| 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 |
| CN105731542B (en) * | 2014-12-10 | 2018-09-04 | 中国石油天然气股份有限公司 | Method for preparing molybdenum disulfide microspheres in reverse microemulsion system |
| CN105329946A (en) * | 2015-11-16 | 2016-02-17 | 暨南大学 | Molybdenum disulfide nanosheet with rich active sites as well as preparation method and application of molybdenum disulfide nanosheet |
| CN105923655B (en) * | 2016-04-22 | 2017-06-06 | 合肥工业大学 | It is a kind of by calcining the method that nanometer fibrous poly- molybdic acid ammonium sodium and vulcanization prepare molybdenum disulfide nano tube |
| CN106381481B (en) * | 2016-09-18 | 2018-09-14 | 河南师范大学 | A kind of preparation method of metal-doped molybdenum disulfide film |
| CN106732668A (en) * | 2016-11-18 | 2017-05-31 | 中国计量大学 | A kind of hydrothermal preparing process of flower-shaped molybdenum bisuphide/cupric oxide composite nano materials |
| CN106702425B (en) * | 2016-12-09 | 2018-10-02 | 济南大学 | A method of preparing molybdenum disulfide/copper/cobalt catalytic hydrogen evolution layer in foam iron surface |
| 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 |
| CN108155028B (en) * | 2017-12-29 | 2020-03-17 | 安徽大学 | Preparation method of flower-like molybdenum disulfide high-performance supercapacitor electrode |
| CN109081377B (en) * | 2018-10-19 | 2020-07-28 | 岭南师范学院 | Three-dimensional molybdenum disulfide flower ball array and preparation method and application 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 |
-
2007
- 2007-07-03 CN CNB2007100698738A patent/CN100548891C/en not_active Expired - Fee Related
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| CN101113021A (en) | 2008-01-30 |
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