CN105789595B - A kind of preparation method of graphene/molybdenum disulfide composite material - Google Patents
A kind of preparation method of graphene/molybdenum disulfide composite material Download PDFInfo
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- CN105789595B CN105789595B CN201610265037.6A CN201610265037A CN105789595B CN 105789595 B CN105789595 B CN 105789595B CN 201610265037 A CN201610265037 A CN 201610265037A CN 105789595 B CN105789595 B CN 105789595B
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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Abstract
The present invention relates to a kind of preparation methods of graphene/molybdenum disulfide composite material, comprise the technical steps that：1）, glucose and four thio ammonium molybdate are mixed, ground in agate mortar；2）, sodium chloride and potassium chloride are mixed, through ball mill ball milling；3）, by step 1）With 2）In obtained material be uniformly mixed, and the pre-heat treatment；4）, the mixing material after the pre-heat treatment is placed in square porcelain boat, porcelain boat is positioned over to the centre position of tube furnace, inert gas shielding is passed through, is calcined under certain heating rate；5）, isothermal holding is carried out after calcining；6）, under inert gas shielding, room temperature is naturally cooling to, takes out sample；7）, gained mixture with deionized water is cleaned, and passes through vacuum filtration and obtains product.The present invention, as carbon source, realizes the new method of synthesizing graphite alkene/molybdenum disulfide nano-composite material, synthesis step is simple, of low cost, has commercial application value using cheap glucose.
Description
【Technical field】
The present invention relates to a kind of preparation methods of composite material, and in particular to a kind of graphene/molybdenum disulfide composite material
Preparation method, belong to novel energy resource material technology field.
【Background technology】
Lithium ion battery has operating voltage higher, than energy higher, safer and memoryless compared with conventional batteries
Etc. advantages.Since 21 century, environmental pollution getting worse, energy shortage has become the weight for restricting progress of human society development
Problem is wanted, this just forces people urgently to develop and produces more energy-saving and environment-friendly life mode of transportation, to reduce the petrochemical industry class energy
A large amount of uses.The large-scale use of wherein all kinds of electric vehicles be exactly it is a kind of it is important can reduce environmental pollution replace
Charg`e d'affaires's method.In addition, to ensure good cruising ability, each electric appliances in daily life are existing also most using lithium
Ion battery, such as mobile phone, laptop, digital camera and video recorder.Develop high energy storage density and long circulating
The new type lithium ion battery in service life has been a kind of urgent social demand, is the needs of current social development.Lithium-ion electric at present
Generally using graphite and its composite material as cathode, specific capacity is relatively low, it is difficult to meet high-power electric automobile to energy in pond
The demand of density, therefore research and develop Novel high-specific capacity flexible lithium ion battery negative material and have important practical significance.
Transition metal binary compound have excellent electricity, heat, light and catalysis characteristics, excite people greatly study it is emerging
Interest.Molybdenum disulfide（MoS2）It is a kind of typical transition metal binary lamellar compound, in recent years in the weight such as chemical catalysis, hydrogen storage
Field is wanted to have more and more important application, molybdenum disulfide has unique sandwich structure, and layer structure is conducive to lithium ion
Insertion and deintercalation, and in electrochemical reaction own vol variation it is small, be the material being very suitable for as negative electrode of lithium ion battery.
But since molybdenum disulfide material self-conductive is poor, fail to obtain scale application.Grapheme material has excellent electric conductivity
Can, heat conductivility and high specific surface area, using graphene/cathode of the molybdenum disulfide composite material as lithium ion battery,
Be conducive to the fast transfer of electronics, improve battery performance.
And the synthetic method of graphene/molybdenum disulfide composite material first in Hummers methods is synthesized mostly aoxidize at present
Graphene（GO）, then with Material synthesis such as sodium molybdates, graphite oxide is reduced to graphene（RGO）, sulphur source, molybdenum source are converted into two
Molybdenum sulfide, complex steps, yield are relatively low.In addition, there is lacking for hydrophilic difficult oleophylic using the graphene oxide of hydrothermal method synthesis
It falls into, easily reunites in organic solvent, it is difficult to it is scattered, lithium ion battery negative material is also limited it as to a certain extent
Practical application.
Therefore, in order to solve the above technical problems, a kind of graphene/molybdenum disulfide composite material it is necessory to provide innovation
Preparation method, to overcome the defect of the prior art.
【The content of the invention】
To solve the above problems, it can realize low cost it is an object of the invention to provide one kind, prepare graphite on a large scale
The method of alkene/molybdenum disulfide composite cathode material of lithium ion battery.
To achieve the above object, the technical solution taken of the present invention is：A kind of system of graphene/molybdenum disulfide composite material
Preparation Method uses one-step synthesis, comprises the technical steps that：
1）, glucose and four thio ammonium molybdate are mixed, ground in agate mortar；
2）, sodium chloride and potassium chloride are mixed, through ball mill ball milling；
3）, by step 1）With 2）In obtained material be uniformly mixed, and the pre-heat treatment；
4）, the mixing material after the pre-heat treatment is placed in square porcelain boat, porcelain boat is positioned over to the centre position of tube furnace,
Inert gas shielding is passed through, is calcined under certain heating rate；
5）, isothermal holding is carried out after calcining；
6）, under inert gas shielding, room temperature is naturally cooling to, takes out sample；
7）, gained mixture with deionized water is cleaned, and passes through vacuum filtration and obtains product.
The preparation method of graphene/molybdenum disulfide composite material of the present invention is further：Step 1）In, the glucose
Mass ratio with four thio ammonium molybdate is（1-8）:(1-10).
The preparation method of graphene/molybdenum disulfide composite material of the present invention is further：Step 2）In, the sodium chloride
Mass ratio with potassium chloride is（1-3）:1.
The preparation method of graphene/molybdenum disulfide composite material of the present invention is further：Step 3）In, the pre-heat treatment
Temperature is 80 DEG C -200 DEG C.
The preparation method of graphene/molybdenum disulfide composite material of the present invention is further：Step 4）In, heating rate is
5 DEG C -30 DEG C/min；Calcining heat is 950 DEG C -1300 DEG C；The inert gas is nitrogen.
The preparation method of graphene/molybdenum disulfide composite material of the present invention is further：Step 5）In, during the heat preservation
Between be 30min-60min.
The preparation method of graphene/molybdenum disulfide composite material of the present invention is further：Step 7）In, mixture is put
In beaker, deionized water is added in, 30min is stirred by ultrasonic, is filtered by vacuum using the filter membrane of 0.5M, repeated washing step 3-
5 times；Products therefrom is placed in air dry oven and dries for 24 hours.
The preparation method of graphene/molybdenum disulfide composite material of the present invention is further：Step 1）In, glucose and four
It needs to add in ammonium chloride in the mixture of ammonium thiomolybdate, the mass ratio of the glucose and ammonium chloride is 4:5.
The preparation method of graphene/molybdenum disulfide composite material of the present invention is also：Step 1）In, glucose 0.1g, four
Ammonium thiomolybdate 0.1g grinds 50min；Step 2）In, sodium chloride 11.4g and potassium chloride 2.8g, ball milling 50min；Step 3）In,
In 150 DEG C of the pre-heat treatment 20h；Step 5）In, 1000 DEG C are warming up to, heating rate is 20 DEG C/min, keeps the temperature 40min.
Compared with prior art, the present invention has the advantages that：The present invention using cheap glucose as carbon source,
The new method of synthesizing graphite alkene/molybdenum disulfide nano-composite material is realized, synthesis step is simple, of low cost, has industry
Change application value.
【Description of the drawings】
Fig. 1 is the X ray diffracting spectrum of sample obtained by the present invention（XRD）.
Fig. 2 is the field emission scanning electron microscope of present invention gained sample（SEM）Figure.
【Specific embodiment】
Embodiment 1：
First, raw material are prefabricated
0.8g glucose is weighed, 0.5g four thio ammonium molybdates after being sufficiently mixed in glove box, are placed in agate mortar and grind
30min is ground, obtains mixture A；11.5g sodium chloride and 11.5g potassium chloride are weighed, is ground after being sufficiently mixed with being placed in ball mill
30min obtains mixture B；Mixture A and B are mixed, are placed in square porcelain boat, total mixture amount is no more than porcelain boat total amount
2/3rds.
2nd, pretreatment
The mixture of gained in step 1 is placed in vacuum drying chamber, 10 are heat-treated at 80 DEG C；
3rd, fuse salt environment reaction
Gained mixture in step 2 is placed among tube furnace boiler tube, is passed through nitrogen protection, is warming up to 950 DEG C, heating
Rate is 5 DEG C/min, after reaching target temperature, keeps the temperature 30min, cooled to room temperature is taken out.
4th, product washs
Porcelain boat product in step 3 is taken out, is placed in 500ml beakers, adds in deionized water, 30min is stirred by ultrasonic, adopts
It is filtered by vacuum with the filter membrane of 0.5M, adds in deionized water again, wash repeatedly step, washed 3-5 times altogether.Products therefrom is put
It is dried for 24 hours in air dry oven.
Embodiment 2：
First, raw material are prefabricated
0.1g glucose is weighed, 0.1g four thio ammonium molybdates after being sufficiently mixed in glove box, are placed in agate mortar and grind
50min is ground, obtains mixture A；11.4g sodium chloride and 2.8g potassium chloride are weighed, to be placed in ball milling in ball mill after being sufficiently mixed
50min obtains mixture B；Mixture A and B are mixed, are placed in square porcelain boat, total mixture amount is no more than porcelain boat total amount
2/3rds.
2nd, pretreatment
The mixture of gained in step 1 is placed in vacuum drying chamber, after 150 DEG C are heat-treated 20h；
3rd, fuse salt environment reaction
Gained mixture in step 2 is placed among tube furnace boiler tube, is passed through nitrogen protection, is warming up to 1000 DEG C, heating
Rate is 20 DEG C/min, after reaching target temperature, keeps the temperature 40min, cooled to room temperature is taken out.
4th, product washs
Porcelain boat product in step 3 is taken out, is placed in 500ml beakers, adds in deionized water, 30min is stirred by ultrasonic, adopts
It is filtered by vacuum with the filter membrane of 0.5M, adds in deionized water again, wash repeatedly step, washed 3-5 times altogether.Products therefrom is put
It is dried for 24 hours in air dry oven.
Embodiment 3：
First, raw material are prefabricated
0.5g glucose, the ammonium chloride of 1g are weighed, 0.05g four thio ammonium molybdates after being sufficiently mixed in glove box, are placed in
60min is ground in agate mortar, obtains mixture A；13.5g sodium chloride and 11.5g potassium chloride are weighed, to be placed in after being sufficiently mixed
60min is ground in ball mill, obtains mixture B；Mixture A and B are mixed, are placed in square porcelain boat, total mixture amount does not surpass
Cross 2/3rds of porcelain boat total amount.
2nd, pretreatment
The mixture of gained in step 1 is placed in vacuum drying chamber, after 200 DEG C are heat-treated 30h, is down to room naturally
It is taken out after temperature；
3rd, fuse salt environment reaction
Gained mixture in step 2 is placed among tube furnace boiler tube, is passed through nitrogen protection, is warming up to 1300 DEG C, heating
Rate is 30 DEG C/min, after reaching target temperature, keeps the temperature 60min, cooled to room temperature is taken out.
4th, product washs
Porcelain boat product in step 3 is taken out, is placed in 500ml beakers, adds in deionized water, 30min is stirred by ultrasonic, adopts
It is filtered by vacuum with the filter membrane of 0.5M, adds in deionized water again, wash repeatedly step, washed 3-5 times altogether.Products therefrom is put
It is dried for 24 hours in air dry oven.
The specific material characterization of sample obtained by technique using the present invention is referred to shown in Figure of description 1 and attached drawing 2.
Claims (8)
1. a kind of preparation method of graphene/molybdenum disulfide composite material, it is characterised in that：It uses one-step synthesis, including
Following processing step：
1）, glucose and four thio ammonium molybdate are mixed, ground in agate mortar；
2）, sodium chloride and potassium chloride are mixed, through ball mill ball milling；
3）, by step 1）With 2）In obtained material be uniformly mixed, and the pre-heat treatment；
4）, the mixing material after the pre-heat treatment is placed in square porcelain boat, porcelain boat is positioned over to the centre position of tube furnace, is passed through
Inert gas shielding is calcined under certain heating rate；
5）, isothermal holding is carried out after calcining；
6）, under inert gas shielding, room temperature is naturally cooling to, takes out sample；
7）, gained mixture with deionized water is cleaned, and passes through vacuum filtration and obtains product.
2. the preparation method of graphene as described in claim 1/molybdenum disulfide composite material, it is characterised in that：Step 1）In,
The mass ratio of the glucose and four thio ammonium molybdate is（1-8）:(1-10).
3. the preparation method of graphene as described in claim 1/molybdenum disulfide composite material, it is characterised in that：Step 2）In,
The mass ratio of the sodium chloride and potassium chloride is（1-3）:1.
4. the preparation method of graphene as described in claim 1/molybdenum disulfide composite material, it is characterised in that：Step 3）In,
The temperature of the pre-heat treatment is 80 DEG C -200 DEG C.
5. the preparation method of graphene as described in claim 1/molybdenum disulfide composite material, it is characterised in that：Step 4）In,
Heating rate is 5 DEG C -30 DEG C/min；Calcining heat is 950 DEG C -1300 DEG C；The inert gas is nitrogen.
6. the preparation method of graphene as described in claim 1/molybdenum disulfide composite material, it is characterised in that：Step 5）In,
The soaking time is 30min-60min.
7. the preparation method of graphene as described in claim 1/molybdenum disulfide composite material, it is characterised in that：Step 1）In,
It needs to add in ammonium chloride in the mixture of glucose and four thio ammonium molybdate, the mass ratio of the glucose and ammonium chloride is 4:5.
8. the preparation method of graphene as described in claim 1/molybdenum disulfide composite material, it is characterised in that：Step 1）In,
Glucose 0.1g, four thio ammonium molybdate 0.1g grind 50min；Step 2）In, sodium chloride 11.4g and potassium chloride 2.8g, ball milling
50min；Step 3）In, in 150 DEG C of the pre-heat treatment 20h；Step 5）In, 1000 DEG C are warming up to, heating rate is 20 DEG C/min,
Keep the temperature 40min.
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| 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 |
| 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 |
| 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 |
| CN106564952B (en) * | 2016-11-04 | 2018-06-29 | 西安建筑科技大学 | A kind of method that carbohydrate organic carbon reduction prepares class graphene molybdenum disulfide-graphene composite material |
| CN107376971B (en) * | 2017-07-25 | 2020-01-21 | 洛阳理工学院 | Synthetic method of graphite-like carbon nitride/molybdenum disulfide nano composite material |
| CN109904397B (en) * | 2017-12-08 | 2020-08-04 | 中国石油化工股份有限公司 | Molybdenum disulfide/C/graphene composite material |
| CN109904399B (en) * | 2017-12-08 | 2022-07-08 | 中国石油化工股份有限公司 | Molybdenum disulfide/C/three-dimensional graphene composite material |
| 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 |
| 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 |
| CN111447821B (en) * | 2020-05-18 | 2022-06-21 | 哈尔滨工业大学 | Preparation method of carbide/carbon nano composite material |
| CN114806675B (en) * | 2022-04-14 | 2023-03-03 | 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 |
| CN115466459B (en) * | 2022-09-06 | 2024-02-27 | 成都航空职业技术学院 | Modified polypropylene fused deposition molding granule and preparation method thereof |
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