CN103626231B - The preparation method of the carbosphere that a kind of molybdenumdisulphide is coated - Google Patents
The preparation method of the carbosphere that a kind of molybdenumdisulphide is coated Download PDFInfo
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- CN103626231B CN103626231B CN201310590498.7A CN201310590498A CN103626231B CN 103626231 B CN103626231 B CN 103626231B CN 201310590498 A CN201310590498 A CN 201310590498A CN 103626231 B CN103626231 B CN 103626231B
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Abstract
The invention discloses the preparation method of the coated carbosphere of a kind of molybdenumdisulphide, it is characterized in that step is as follows: (1) is by (NH
4)
2moO
4, KSCN, reductive agent and carbon source be dissolved in deionized water, dissolve and obtain solution, the pH value of regulator solution is 6 ~ 8; (2) after solution stirring step (1) obtained, stainless steel cauldron is moved into, sealing, after 140 DEG C ~ 260 DEG C reaction 24h, be cooled to room temperature, by reaction product separation, washing, drying, obtain the carbosphere that the molybdenumdisulphide of grey black is coated, particle diameter is 1-2 micron.Technique is simple, and with low cost, the product purity prepared is high, productive rate is high.
Description
Technical field
The present invention relates to field of nanometer material technology, particularly, is the preparation method of the coated carbosphere of a kind of molybdenumdisulphide.
Background technology
Molybdenumdisulphide, as important transient metal sulfide, has the laminate structure of similar graphite flake layer, is very strong covalent linkage in layer, and interlayer is then very weak Van der Waals Er Sili, and layer and layer are easy to peel off, and have good tribological property.Along with the rise of nanotechnology, various nano molybdenum disulfide particle, because of its special size and interfacial effect, causes the extensive concern of people.The preparation method of various novelty is also developed in succession, comprises thermal decomposition method, hot reducing method, hydrothermal method, spray-drying process, chemical vapour deposition, or even rays method.
In recent years, the synthesis of various doping molybdenumdisulphide material also have received to be paid close attention to widely, as Graphene composite molybdenum disulfide, copper base composite molybdenum disulfide, Ni-based composite molybdenum disulfide etc.By doping, molybdenum disulfide nano-composite material performance obtains certain lifting, particularly electrochemistry, lithium electrically and tribological property etc.
Summary of the invention
The preparation method of the carbosphere that the object of the present invention is to provide a kind of molybdenumdisulphide coated, is synthesized by simple hydrothermal method, and thus obtained microsphere pattern is homogeneous, productive rate is high, has better specific surface area and tribological property.
Above-mentioned purpose is achieved by the following technical solution:
A preparation method for the carbosphere of coated molybdenumdisulphide, comprises the following steps:
(1) obtain solution: by (NH
4)
2moO
4, KSCN, reductive agent and carbon source be dissolved in deionized water, dissolve and obtain solution, regulator solution pH value is 6 ~ 8;
((NH
4)
2moO
4, KSCN, reductive agent and carbon source the ratio of amount of substance be 0.5 ~ 1.5:2.5 ~ 3.5:1.5 ~ 2.5:0.5 ~ 1.5
Preferred proportion is 1:3:2:1, this ratio product property and pattern best;
Reductive agent is inorganic salt, example hydrochloric acid azanol or sodium borohydride;
Carbon source is carbohydrate, as glucose, fructose or sucrose;
(2), after solution stirring step (1) obtained, immigration stainless steel cauldron, sealing, after 120 DEG C ~ 260 DEG C reaction 24h, is cooled to room temperature, by the separation of gained reaction product, washing, drying, obtains molybdenumdisulphide carbon coated microballoon.
The present invention, production technique is simple and easy to control, and cost is inexpensive, and productive rate is high, is applicable to large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is the XRD spectra of the molybdenumdisulphide carbon coated microballoon that this bright embodiment 1 obtains.Illustrate that XRD peak position is consistent with standard diffraction figure (PDFNo.37-1492), product is MoS mainly
2nanostructure.Do not occur in XRD figure spectrum because C peak is more weak.
The EDS of the molybdenumdisulphide carbon coated microballoon that Fig. 2 obtains for this bright embodiment 1, only has the existence of C, Mo and S element, further demonstrates the formation of carbon ball in figure.
Fig. 3 is molybdenumdisulphide carbon coated microballoon field emission scanning electron microscope (SEM) photo that the embodiment of the present invention 1 obtains.Fig. 3 a clearly can see that the particle diameter of microballoon is 1 ~ 2mm's; See in Fig. 3 b that molybdenum disulfide particles is progressively coated to carbon ball on the surface clearly, finally define molybdenumdisulphide carbon coated microballoon.
Embodiment
The present invention is further described below by way of embodiment, as known by the technical knowledge, the present invention also describes by other the scheme not departing from the technology of the present invention feature, and the change therefore within the scope of the present invention all or equivalent scope of the invention is all included in the invention.
Embodiment 1:
0.88g (NH
4)
2moO
4, 1.20gKSCN, 0.56gNH
2oHHCl and 0.4g glucose is dissolved in the deionized water of 60mL, after dissolving completely, then uses 2molL
-1naOH regulate about pH value to 8.After stirring 30min, mixed solution is transferred in the stainless steel cauldron of 100ml, is placed in vacuum drying oven in 180 DEG C of insulation 24h, is cooled to room temperature.Reaction product, after centrifugation, uses deionized water and dehydrated alcohol repetitive scrubbing respectively, and finally 80 DEG C of dry 10h obtain the powder product of grey black under vacuum, and the carbosphere that namely molybdenumdisulphide is coated, yield is 90%.
The component that embodiment 2 to embodiment 4 adopts is as shown in the table:
Note: the experiment obtaining frictional coefficient in table 1 utilizes ultrasonic generator dispersion agent span80 and the coated carbosphere of molybdenumdisulphide to be distributed to uniformly in base oil (paraffin), the dirty solution oil sample frictional experiment that to be mixed with containing massfraction be 1%-5% (only listing the frictional coefficient that content is 5% in table 1) carries out frictional experiment on CETRUMT-2 multifunction friction wear testing machine.Adopt ball-disc type contact, rotating speed is 50 ~ 400rpm, and load is 10N ~ 50N, and experimental period is 30min.Testing Stainless Steel Ball model used is 440-C (9Cr18), and diameter is 3mm, and hardness is HRC62.
Claims (3)
1. a preparation method for the carbosphere that molybdenumdisulphide is coated, is characterized in that comprising the steps:
(1) by ((NH4)
2moO
4, KSCN, reductive agent and carbon source be dissolved in deionized water, dissolve and obtain solution, the pH value of regulator solution is 6 ~ 8; Reductive agent is oxammonium hydrochloride or sodium borohydride; Carbon source is glucose, fructose or sucrose;
(2) after solution stirring step (1) obtained, stainless steel cauldron is moved into, sealing, after 140 DEG C ~ 260 DEG C reaction 24h, be cooled to room temperature, by reaction product separation, washing, drying, obtain the carbosphere that the molybdenumdisulphide of grey black is coated, particle diameter is 1-2 micron.
2. the preparation method of the carbosphere that molybdenumdisulphide is coated according to claim 1, is characterized in that described ((NH
4)
2moO
4, KSCN, reductive agent and carbon source the ratio of amount of substance be 0.5 ~ 1.5:2.5 ~ 3.5:1.5 ~ 2.5:0.5 ~ 1
3. the preparation method of the carbosphere that molybdenumdisulphide is coated according to claim 1, is characterized in that described ((NH
4)
2moO
4, KSCN, reductive agent and carbon source the ratio of amount of substance be 1:3:2:1.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105742081A (en) * | 2016-05-12 | 2016-07-06 | 安徽大学 | Rambutan structured molybdenum sulfide coated carbon sphere composite material as well as preparation method and application thereof |
| CN106521540B (en) * | 2016-10-25 | 2018-10-26 | 东华理工大学 | A method of it is co-deposited and prepares the flower-shaped molybdenum disulfide material of class graphene |
| CN107983272A (en) * | 2016-10-26 | 2018-05-04 | 中国科学院化学研究所 | Sulfide encapsulated particles and preparation method and application |
| CN106848228A (en) * | 2017-01-24 | 2017-06-13 | 同济大学 | A kind of method for preparing molybdenum bisuphide/carbon combined multi-stage Porous materials |
| CN108417789A (en) * | 2018-01-30 | 2018-08-17 | 合肥国轩高科动力能源有限公司 | A kind of MoS for negative electrode of lithium ion battery2/ C microballoon composite material and preparation methods |
| CN110357161B (en) * | 2019-07-03 | 2021-09-28 | 山东省分析测试中心 | MCHS @ molybdenum disulfide nanocomposite based on core-shell structure and preparation method and application thereof |
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| CN1752020A (en) * | 2005-06-22 | 2006-03-29 | 浙江大学 | Preparation method of inorganic fullerene molybdenum disulfide and its application |
| CN1994896A (en) * | 2006-12-20 | 2007-07-11 | 浙江大学 | Preparation method of one-step hydrothermal synthesis of carbon/molybdenum disulfide composite microsphere |
| 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 |
| CN102992405A (en) * | 2012-12-10 | 2013-03-27 | 江苏大学 | Preparation method for molybdenum disulfide nanometer nuclear shell nano-structure |
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| CN1752020A (en) * | 2005-06-22 | 2006-03-29 | 浙江大学 | Preparation method of inorganic fullerene molybdenum disulfide and its application |
| CN1994896A (en) * | 2006-12-20 | 2007-07-11 | 浙江大学 | Preparation method of one-step hydrothermal synthesis of carbon/molybdenum disulfide composite microsphere |
| 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 |
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