CN105789595A - Preparation method of graphene/molybdenum disulfide composite material - Google Patents

Preparation method of graphene/molybdenum disulfide composite material Download PDF

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CN105789595A
CN105789595A CN201610265037.6A CN201610265037A CN105789595A CN 105789595 A CN105789595 A CN 105789595A CN 201610265037 A CN201610265037 A CN 201610265037A CN 105789595 A CN105789595 A CN 105789595A
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preparation
graphene
molybdenum bisuphide
glucose
composite
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CN105789595B (en
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李天军
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University of Shaoxing
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/362Composites
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/13Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/136Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/13Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139Processes of manufacture
    • H01M4/1397Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/581Chalcogenides or intercalation compounds thereof
    • H01M4/5815Sulfides
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624Electric conductive fillers
    • H01M4/625Carbon or graphite
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M2004/026Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027Negative electrodes
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention relates to a preparation method of a graphene/molybdenum disulfide composite material. The preparation method comprises the following process steps: (1) mixing glucose with ammonium tetrathiomolybdate, and performing grinding in an agate mortar; (2) mixing sodium chloride with potassium chloride, and performing ball milling in a ball milling machine; (3) uniformly mixing the material obtained in the step (1) with the material obtained in the step (2), and performing preheating treatment; (4) placing the mixed material after preheating treatment in a square porcelain boat, placing the porcelain boat in the middle position of a tubular furnace, leading inert gas for protection, and performing calcination under a certain heating rate; (5) performing heat preservation treatment after calcination; (6) under inert-gas protection, cooling naturally to room temperature, and taking out samples; (7) cleaning the obtained mixture with deionized water, and performing vacuum filtration so as to obtain products. According to the preparation method disclosed by the invention, cheap glucose is used as a carbon source, so that a new method for synthetizing graphene/ molybdenum disulfide nanocomposite materials is obtained, the synthesis steps are simple, the cost is low, and the preparation method has an industrial application value.

Description

A kind of preparation method of Graphene/molybdenum bisuphide composite
[technical field]
The preparation method that the present invention relates to a kind of composite, the preparation method being specifically related to a kind of Graphene/molybdenum bisuphide composite, belong to novel energy resource material technology field.
[background technology]
Lithium ion battery, compared with conventional batteries, has the advantages such as running voltage is higher, specific energy is higher, more safe and memoryless.Since 21 century, environmental pollution is day by day serious, and energy shortage has had become as the major issue of restriction progress of human society development, and this just forces people urgently to develop the life mode of transportation producing energy-conserving and environment-protective more, to reduce a large amount of uses of the petrochemical industry class energy.Wherein the large-scale use of all kinds of electric vehicles is exactly a kind of important possible alternative that can reduce environmental pollution.In addition, for ensureing good flying power, each electric appliances in daily life is now also most adopts lithium ion battery, such as mobile phone, notebook computer, digital camera and videocorder etc..The new type lithium ion battery developing high energy storage density and long circulation life has been a kind of urgent social need, is the needs of current social development.The commonly used graphite of current lithium ion battery and its composite are as negative pole, and specific capacity is relatively low, it is difficult to meet the large power, electrically electrical automobile demand to energy density, and therefore research and development Novel high-specific capacity flexible lithium ion battery negative material has important practical significance.
Transition metal binary compound has excellent electricity, heat, light and catalysis characteristics, excites people and studies interest greatly.Molybdenum bisuphide (MoS2) it is a kind of typical transition metal binary lamellar compound, more and more important application is had in recent years at the key areas such as chemical catalysis, hydrogen storage, molybdenum bisuphide has the sandwich structure of uniqueness, layer structure is conducive to insertion and the deintercalation of lithium ion, and own vol change is little in electrochemical reaction, it is be very suitable for the material as lithium ion battery negative.But owing to molybdenum bisuphide material self-conductive is poor, fail to obtain scale application.Grapheme material has excellent electric conductivity, heat conductivility and high specific surface area, adopts Graphene/molybdenum bisuphide composite as the negative pole of lithium ion battery, is conducive to the fast transfer of electronics, improves battery performance.
And at present the synthetic method of Graphene/molybdenum bisuphide composite is first synthesized graphene oxide (GO) with Hummers method mostly, again with Material synthesis such as sodium molybdate, graphite oxide being reduced to Graphene (RGO), sulfur source, molybdenum source are converted into molybdenum bisuphide, complex steps, productivity is relatively low.It addition, adopt the graphene oxide of hydrothermal method synthesis to have the defect of hydrophilic difficult oleophylic, easily reunite in organic solvent, it is difficult to dispersion, also limit it as the practical application of lithium ion battery negative material to a certain extent.
Therefore, for solving above-mentioned technical problem, the preparation method of the Graphene of a kind of innovation of necessary offer/molybdenum bisuphide composite, to overcome described defect of the prior art.
[summary of the invention]
For solving the problems referred to above, it is an object of the invention to provide and a kind of can realize low cost, the method preparing Graphene/molybdenum bisuphide composite cathode material of lithium ion battery on a large scale.
For achieving the above object, the technical scheme that the present invention takes is: the preparation method of a kind of Graphene/molybdenum bisuphide composite, and it adopts one-step synthesis, comprises the technical steps that:
1), glucose and four thio ammonium molybdate are mixed, grinds in agate mortar;
2), sodium chloride and potassium chloride are mixed, through ball mill ball milling;
3), by step 1) and 2) in the material mixing that obtains uniform, and the pre-heat treatment;
4), the composite material after the pre-heat treatment is placed in square porcelain boat, porcelain boat is positioned over the centre position of tube furnace, pass into inert gas shielding, calcine under certain heating rate;
5), isothermal holding is carried out after calcining;
6), under inert gas shielding, it is naturally cooling to room temperature, takes out sample;
7), gained mixture deionized water is cleaned, and obtains product by vacuum filtration.
The preparation method of the Graphene of the present invention/molybdenum bisuphide composite is further: in step 1), and the mass ratio of described glucose and four thio ammonium molybdate is (1-8): (1-10).
The preparation method of the Graphene of the present invention/molybdenum bisuphide composite is further: step 2) in, the mass ratio of described sodium chloride and potassium chloride is (1-3): 1.
The preparation method of the Graphene of the present invention/molybdenum bisuphide composite is further: in step 3), and the temperature of the pre-heat treatment is 80 DEG C-200 DEG C.
The preparation method of the Graphene of the present invention/molybdenum bisuphide composite is further: in step 4), and heating rate is 5 DEG C-30 DEG C/min;Calcining heat is 950 DEG C-1300 DEG C;Described noble gas is nitrogen.
The preparation method of the Graphene of the present invention/molybdenum bisuphide composite is further: in step 5), and described temperature retention time is 30min-60min.
The preparation method of the Graphene of the present invention/molybdenum bisuphide composite is further: in step 6), be placed in beaker by mixture, adds deionized water, excusing from death stirring 30min, adopts the filter membrane of 0.5M to carry out vacuum filtration, repeated washing step 3-5 time;Products therefrom is placed in air dry oven and dries 24h.
The preparation method of the Graphene of the present invention/molybdenum bisuphide composite is further: in step 1), needs to add ammonium chloride in the mixture of glucose and four thio ammonium molybdate, and the mass ratio of described glucose and ammonium chloride is 4:5.
The preparation method of the Graphene of the present invention/molybdenum bisuphide composite is also: in step 1), glucose 0.1g, four thio ammonium molybdate 0.1g, grinds 50min;Step 2) in, sodium chloride 11.4g and potassium chloride 2.8g, grinds 50min;In step 3), at 150 DEG C of the pre-heat treatment 20h;In step 4), being warming up to 1000 DEG C, heating rate is 20 DEG C/min, is incubated 40min.
Compared with prior art, there is advantages that the present invention adopts cheap glucose as carbon source, it is achieved that the new method of synthesizing graphite alkene/molybdenum disulfide nano-composite material, synthesis step is simple, with low cost, has commercial application and is worth.
[accompanying drawing explanation]
Fig. 1 is the X ray diffracting spectrum (XRD) of gained sample of the present invention.
Fig. 2 is field emission scanning electron microscope (SEM) figure of gained sample of the present invention.
[detailed description of the invention]
Embodiment 1:
One, raw material is prefabricated
Weigh 0.8g glucose, 0.5g four thio ammonium molybdate, after being sufficiently mixed in glove box, be placed in agate mortar and grind 30min, obtain mixture A;Weigh 11.5g sodium chloride and 11.5g potassium chloride, to be placed in grinding in ball grinder 30min after being sufficiently mixed, obtain mixture B;Being mixed by mixture A and B, be placed in square porcelain boat, total mixture amount is less than 2/3rds of porcelain boat total amount.
Two, pretreatment
The mixture of gained in step one is placed in vacuum drying oven, at 80 DEG C of heat treatments 10;
Three, fuse salt environment reaction
Being placed in the middle of tube furnace boiler tube by gained mixture in step 2, pass into nitrogen protection, be warming up to 950 DEG C, heating rate is 5 DEG C/min, after reaching target temperature, is incubated 30min, naturally cools to room temperature, takes out.
Four, product washing
Porcelain boat product in step 3 is taken out, is placed in 500ml beaker, add deionized water, excusing from death stirring 30min, adopt the filter membrane of 0.5M to carry out vacuum filtration, again add deionized water, repeated washing step, altogether washing 3-5 time.Products therefrom is placed in air dry oven and dries 24h.
Embodiment 2:
One, raw material is prefabricated
Weigh 0.1g glucose, 0.1g four thio ammonium molybdate, after being sufficiently mixed in glove box, be placed in agate mortar and grind 50min, obtain mixture A;Weigh 11.4g sodium chloride and 2.8g potassium chloride, to be placed in grinding in ball grinder 50min after being sufficiently mixed, obtain mixture B;Being mixed by mixture A and B, be placed in square porcelain boat, total mixture amount is less than 2/3rds of porcelain boat total amount.
Two, pretreatment
The mixture of gained in step one is placed in vacuum drying oven, after 150 DEG C of heat treatment 20h;
Three, fuse salt environment reaction
Being placed in the middle of tube furnace boiler tube by gained mixture in step 2, pass into nitrogen protection, be warming up to 1000 DEG C, heating rate is 20 DEG C/min, after reaching target temperature, is incubated 40min, naturally cools to room temperature, takes out.
Four, product washing
Porcelain boat product in step 3 is taken out, is placed in 500ml beaker, add deionized water, excusing from death stirring 30min, adopt the filter membrane of 0.5M to carry out vacuum filtration, again add deionized water, repeated washing step, altogether washing 3-5 time.Products therefrom is placed in air dry oven and dries 24h.
Embodiment 3:
One, raw material is prefabricated
Weigh 0.5g glucose, the ammonium chloride of 1g, 0.05g four thio ammonium molybdate, after being sufficiently mixed in glove box, it is placed in agate mortar and grinds 60min, obtain mixture A;Weigh 13.5g sodium chloride and 11.5g potassium chloride, to be placed in grinding in ball grinder 60min after being sufficiently mixed, obtain mixture B;Being mixed by mixture A and B, be placed in square porcelain boat, total mixture amount is less than 2/3rds of porcelain boat total amount.
Two, pretreatment
The mixture of gained in step one is placed in vacuum drying oven, after 200 DEG C of heat treatment 30h, takes out after being naturally down to room temperature;
Three, fuse salt environment reaction
Being placed in the middle of tube furnace boiler tube by gained mixture in step 2, pass into nitrogen protection, be warming up to 1300 DEG C, heating rate is 30 DEG C/min, after reaching target temperature, is incubated 60min, naturally cools to room temperature, takes out.
Four, product washing
Porcelain boat product in step 3 is taken out, is placed in 500ml beaker, add deionized water, excusing from death stirring 30min, adopt the filter membrane of 0.5M to carry out vacuum filtration, again add deionized water, repeated washing step, altogether washing 3-5 time.Products therefrom is placed in air dry oven and dries 24h.
The technique concrete material characterization of gained sample adopting the present invention refers to shown in Figure of description 1 and accompanying drawing 2.
Above detailed description of the invention is only the preferred embodiment of this creation, not in order to limit this creation, and any amendment of making within all spirit in this creation and principle, equivalent replacement, improvement etc., should be included within the protection domain of this creation.

Claims (9)

1. the preparation method of Graphene/molybdenum bisuphide composite, it is characterised in that: it adopts one-step synthesis, comprises the technical steps that:
1), glucose and four thio ammonium molybdate are mixed, grinds in agate mortar;
2), sodium chloride and potassium chloride are mixed, through ball mill ball milling;
3), by step 1) and 2) in the material mixing that obtains uniform, and the pre-heat treatment;
4), the composite material after the pre-heat treatment is placed in square porcelain boat, porcelain boat is positioned over the centre position of tube furnace, pass into inert gas shielding, calcine under certain heating rate;
5), isothermal holding is carried out after calcining;
6), under inert gas shielding, it is naturally cooling to room temperature, takes out sample;
7), gained mixture deionized water is cleaned, and obtains product by vacuum filtration.
2. the preparation method of Graphene/molybdenum bisuphide composite as claimed in claim 1, it is characterised in that: in step 1), the mass ratio of described glucose and four thio ammonium molybdate is (1-8): (1-10).
3. the preparation method of Graphene/molybdenum bisuphide composite as claimed in claim 1, it is characterised in that: step 2) in, the mass ratio of described sodium chloride and potassium chloride is (1-3): 1.
4. the preparation method of Graphene/molybdenum bisuphide composite as claimed in claim 1, it is characterised in that: in step 3), the temperature of the pre-heat treatment is 80 DEG C-200 DEG C.
5. the preparation method of Graphene/molybdenum bisuphide composite as claimed in claim 1, it is characterised in that: in step 4), heating rate is 5 DEG C-30 DEG C/min;Calcining heat is 950 DEG C-1300 DEG C;Described noble gas is nitrogen.
6. the preparation method of Graphene/molybdenum bisuphide composite as claimed in claim 1, it is characterised in that: in step 5), described temperature retention time is 30min-60min.
7. the preparation method of Graphene/molybdenum bisuphide composite as claimed in claim 1, it is characterised in that: in step 6), mixture is placed in beaker, add deionized water, excusing from death stirring 30min, adopts the filter membrane of 0.5M to carry out vacuum filtration, repeated washing step 3-5 time;Products therefrom is placed in air dry oven and dries 24h.
8. the preparation method of Graphene/molybdenum bisuphide composite as claimed in claim 1, it is characterised in that: in step 1), needing to add ammonium chloride in the mixture of glucose and four thio ammonium molybdate, the mass ratio of described glucose and ammonium chloride is 4:5.
9. the preparation method of Graphene/molybdenum bisuphide composite as claimed in claim 1, it is characterised in that: in step 1), glucose 0.1g, four thio ammonium molybdate 0.1g, grinds 50min;Step 2) in, sodium chloride 11.4g and potassium chloride 2.8g, grinds 50min;In step 3), at 150 DEG C of the pre-heat treatment 20h;In step 4), being warming up to 1000 DEG C, heating rate is 20 DEG C/min, is incubated 40min.
CN201610265037.6A 2016-04-25 2016-04-25 A kind of preparation method of graphene/molybdenum disulfide composite material Expired - Fee Related CN105789595B (en)

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CN106564952A (en) * 2016-11-04 2017-04-19 西安建筑科技大学 Method for preparing graphene-like molybdenum disulfide-graphene composite material by reducing carbohydrate organic carbon
CN106582720A (en) * 2016-11-04 2017-04-26 西安建筑科技大学 Method for preparing graphene-like molybdenum disulfide-bismuth molybdate composite material through saccharide organic carbon reduction
CN106622297A (en) * 2016-11-04 2017-05-10 西安建筑科技大学 A method of preparing a graphene-like molybdenum disulfide-graphene composite material through protein substance reduction
CN106732667A (en) * 2016-11-04 2017-05-31 西安建筑科技大学 A kind of protein matter reduction prepares the preparation method of class Graphene molybdenum bisuphide bismuth molybdate composite
CN107376971A (en) * 2017-07-25 2017-11-24 洛阳理工学院 The synthetic method of one species graphitic nitralloy carbon/molybdenum disulfide nano-composite material
CN109148842A (en) * 2018-07-29 2019-01-04 大连理工大学 A kind of no gradient-heated quickly prepares the method and its application of carbon load disulphide
CN109904398A (en) * 2017-12-08 2019-06-18 中国石油化工股份有限公司 A kind of molybdenum disulfide/graphene composite material
CN109904397A (en) * 2017-12-08 2019-06-18 中国石油化工股份有限公司 A kind of molybdenum disulfide/C/ graphene composite material
CN109904399A (en) * 2017-12-08 2019-06-18 中国石油化工股份有限公司 A kind of molybdenum disulfide/C/ three-dimensional graphene composite material
CN111447821A (en) * 2020-05-18 2020-07-24 哈尔滨工业大学 Preparation method of carbide/carbon nano composite material
CN114806675A (en) * 2022-04-14 2022-07-29 中国科学院兰州化学物理研究所 Composite nano molybdenum disulfide water-soluble lubricating additive and preparation method thereof
CN115466459A (en) * 2022-09-06 2022-12-13 成都航空职业技术学院 Modified polypropylene fused deposition molding granule and preparation method thereof

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CN106564952A (en) * 2016-11-04 2017-04-19 西安建筑科技大学 Method for preparing graphene-like molybdenum disulfide-graphene composite material by reducing carbohydrate organic carbon
CN106582720A (en) * 2016-11-04 2017-04-26 西安建筑科技大学 Method for preparing graphene-like molybdenum disulfide-bismuth molybdate composite material through saccharide organic carbon reduction
CN106622297A (en) * 2016-11-04 2017-05-10 西安建筑科技大学 A method of preparing a graphene-like molybdenum disulfide-graphene composite material through protein substance reduction
CN106732667A (en) * 2016-11-04 2017-05-31 西安建筑科技大学 A kind of protein matter reduction prepares the preparation method of class Graphene molybdenum bisuphide bismuth molybdate composite
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CN106582720B (en) * 2016-11-04 2018-12-07 西安建筑科技大学 A kind of carbohydrate organic carbon reduction preparation class graphene molybdenum disulfide-bismuth molybdate composite material method
CN106732667B (en) * 2016-11-04 2018-12-14 西安建筑科技大学 A kind of protein matter reduction preparation class graphene molybdenum disulfide-bismuth molybdate composite material preparation method
CN106622297B (en) * 2016-11-04 2018-12-14 西安建筑科技大学 A kind of protein matter reduction preparation class graphene molybdenum disulfide-graphene composite material method
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