CN103613137B - A kind of hydrothermal synthesis method of molybdenum disulfide nano flower - Google Patents
A kind of hydrothermal synthesis method of molybdenum disulfide nano flower Download PDFInfo
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- 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
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Abstract
The invention discloses the hydrothermal synthesis method of a kind of molybdenum disulfide nano flower, mainly inorganic molybdenum source, organosulfur source and suitable reductive agent are added and move on in reaction autoclave after mixing in deionized water, heat 24 hours.Gained solution is through repeatedly washing, and centrifugation, namely final drying obtains black solid powder is molybdenum disulfide nano flower.The invention has the beneficial effects as follows: 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; 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.
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.
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