CN105140517A - Preparation method of non-water-soluble transition metal disulphide nanosheets - Google Patents
Preparation method of non-water-soluble transition metal disulphide nanosheets Download PDFInfo
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- CN105140517A CN105140517A CN201510583044.6A CN201510583044A CN105140517A CN 105140517 A CN105140517 A CN 105140517A CN 201510583044 A CN201510583044 A CN 201510583044A CN 105140517 A CN105140517 A CN 105140517A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection 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
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a preparation method of non-water-soluble transition metal disulphide nanosheets. The preparation method comprises the following steps that water-soluble salts containing transition metal elements are used as transition metal sources; thiourea is used as a sulphur source; the transition metal sources, the sulphur source and NaCl are added into deionized water to be dissolved according to the mol ratio of transition metal elements in the transition metal sources to the sulphur element in the sulphur source being 1: (1.8 to 2.5) and according to the mol ratio of the transition elements in the transition metal source to the NaCl being 1:(150 to 600); then, freezing and vacuum drying are performed to obtain a mixture; the prepared mixture is ground into powder; the powder is put into a tubular furnace constant-temperature region for calcination and chemical vapor deposition to obtain products; water washing and vacuum drying are carried out; the disulphide nanosheets are obtained. The disulphide nanosheets with the characteristics of high quality, uniform dimension, relatively controllable layer number, higher yield, lower relative preparing cost and the like can be obtained.
Description
Technical field
The present invention relates to a kind of pervasive preparation method of water-insoluble transition metal dichalcogenide nanometer sheet, can be applicable to and be not limited only to electrode material of secondary lithium ion battery field.
Background technology
The nano-scale two-dimensional structure of Graphene has the more special and magical physicochemical properties being different from macroscopical two-dimensional structure, and character unique like this causes scientists gradually to the concern of other nano-scale two-dimensional structures and research.
The water-insoluble transition metal dichalcogenide of monolayer and polymolecular layer, as MoS
2, WS
2, VS
2, FeS
2, CoS
2deng, because it has the close-packed hexagonal structure similar with Graphene and lamella way of stacking, caused scientists in recent years especially and studied interest greatly.Compared to their macroscopical block, the transition metal dichalcogenide nanometer sheet with two-dimensional structure and ultrathin presents unusual physics, chemistry and electrical properties, and has much application potential in fields such as photoelectron, electro-catalysis, transducer and stored energies.Up to the present, the method preparing the water-insoluble transition metal dichalcogenide nanometer sheet of single or multiple lift has a lot, and such as mechanical dissociation method, chemical vapour deposition technique, chemical Li embed stripping method, electrochemistry Li embedding stripping method, liquid phase stripping method and wet chemical methods etc.Although the method preparing water-insoluble transition metal dichalcogenide nanometer sheet has a lot, there are some problems all more or less due to the restriction of itself preparation condition in these methods.Stripping method is all generally using business-like water-insoluble transition metal dichalcogenide block powder as raw material, water-insoluble transition metal dichalcogenide nanometer sheet (Acc.Chem.Res.2014 is obtained by ultrasonic degradation or the chemical substance way of approximate physical such as to dissociate, 47,1067-1075) (Adv.Mater.2012,24,772-775) (J.Am.Chem.Soc.2013,135,10274-10277); Although the method is simply direct, the problems such as nanometer sheet also exists serious uneven, dispersed bad, the easy reunion of thickness distribution, easily damaged, quality is not good of preparation, simultaneously also along with the problem such as serious noise pollution, chemical contamination that stripping process produces.Chemical synthesis is generally for raw material with transition metal salt and sulfur-bearing inorganic matter or macromolecule, water-insoluble transition metal dichalcogenide nanometer sheet (Adv.EnergyMater.2014 is obtained by the way of the chemical reaction such as Hydrothermal Synthesis or chemical vapour deposition (CVD), 4,1301380) (Angew.Chem.2014,126,1290 – 1293) (J.Am.Chem.Soc.2013,135,5304-5307); Chemical synthesis can prepare that favorable dispersibility, area are larger, quality is higher, few the layer even water-insoluble transition metal dichalcogenide nanometer sheet of individual layer comparatively speaking, but also exists that product is very responsive to reaction condition, output is lower, technological requirement is strict and the weak point such as high energy consumption, high cost.
The preparation technology updating transition metal dichalcogenide nanometer sheet is basis and the guarantee of further investigation transition metal dichalcogenide nanometer sheet special nature.The synthesis of NaCl template two-dimensional confinement is exactly the water-insoluble transition metal dichalcogenide nanometer sheet preparation method of a kind of novelty that latest developments are got up.The consumption of NaCl directly can determine transition metal salt and the Content and distribution situation of sulfur-bearing macromolecule in a NaCl assembly, this is by the microscopic appearance of water-insoluble transition metal dichalcogenide that has influence on synthesized by calcining and structure, and the transition metal salt of proper proportion, sulphur source and NaCl successfully can prepare water-insoluble transition metal dichalcogenide nanometer sheet.
Summary of the invention
The pervasive preparation method of this water-insoluble transition metal dichalcogenide nanometer sheet provided by the invention, utilize the two-dimensional surface template of NaCl crystal and the space confinement effect of self-assembly thereof, in conjunction with a step chemical vapour deposition (CVD), the water-insoluble transition metal dichalcogenide nanometer sheet with features such as nanometer sheet quality are high, size uniformity, the number of plies are relatively controlled, output is higher, preparation cost is relatively low can be obtained.
The present invention is realized by the following technical programs:
A preparation method for water-insoluble transition metal dichalcogenide nanometer sheet, comprises the following steps:
(1). with the water soluble salt containing transition metal for transition metal source, take thiocarbamide as sulphur source, by the transition metal in transition metal source, the mol ratio of the element sulphur in sulphur source is 1:(1.8 ~ 2.5), and be 1:(150 ~ 600 by the mol ratio of the transition metal in transition metal source and NaCl), by transition metal source, sulphur source and NaCl add in deionized water and dissolve, stir wiring solution-forming, again ultrasonic mix after freezing at 0 DEG C, colder temperature in-50 DEG C ~-30 DEG C after solution freeze over carries out vacuumize, obtain mixture,
(2). the mixture grind into powder obtained by step (1), is laid in Noah's ark after crossing 100-300 mesh sieve, is placed in tube furnace flat-temperature zone and calcines: with N
2, a kind of gas of He and Ar or mist as inert gas source, be first that 200-400ml/min passes into inert gas 10-30 minute with deaeration with flow; Again using Ar as protection gas, shielding gas flow amount is fixed as 50-300ml/min, is warming up to 550-750 DEG C with the programming rate of 1-10 DEG C/min, insulation 1-3h carries out chemical vapour deposition (CVD), cools to room temperature with the furnace, obtain product M after reaction terminates;
(3). collect the powder product M that step (2) is obtained, be washed to till there is no NaCl in calcined product, the product after washing is carried out vacuumize, obtains water-insoluble transition metal dichalcogenide nanometer sheet.
The preparation method of above-mentioned water-insoluble transition metal dichalcogenide nanometer sheet, described water-insoluble transition metal dichalcogenide can be cobalt disulfide.
The present invention has the following advantages: the present invention utilizes typical case's water-insoluble transition metal dichalcogenide nanometer sheet material that raw material preparation cheap and easy to get is representative with molybdenum bisuphide, tungsten disulfide, cobalt disulfide nanometer sheet etc., with low cost, course of reaction is simple, controllability is strong.Such water-insoluble transition metal dichalcogenide nanometer sheet material degree of crystallinity is high simultaneously, and quality is good, and structure is homogeneous, and pattern is excellent, excellent performance; Wherein, molybdenum disulfide nano sheet is used for lithium ion battery negative and has certain specific capacity and cycle performance, and circulating under the current density of 100mA/g still to keep the specific capacity of more than 250mAh/g after 50 times.
Accompanying drawing explanation
Fig. 1 is the SEM photo that the embodiment of the present invention 1 prepares the aqueous precursor gel in molybdenum disulfide nano sheet process after freeze-drying.From this view it is apparent that the self assembly mode of NaCl and molybdenum source, the distribution situation of sulphur source a NaCl assembly.
Fig. 2 is the SEM photo of the molybdenum disulfide nano sheet that the embodiment of the present invention 1 obtains.From the pattern and the size that this view it is apparent that molybdenum disulfide nano sheet.
Fig. 3 is the TEM photo of the molybdenum disulfide nano sheet that the embodiment of the present invention 1 obtains.From the overall structure that this view it is apparent that molybdenum disulfide nano sheet.
Fig. 4 is the TEM photo of the molybdenum disulfide nano sheet that the embodiment of the present invention 1 obtains.From the sheet number of layers and the lattice dot matrix that this view it is apparent that molybdenum disulfide nano sheet.
Fig. 5 is the XRD collection of illustrative plates of the molybdenum disulfide nano sheet that the embodiment of the present invention 1 obtains.
Fig. 6 is the charge-discharge performance figure of the lithium ion battery negative that the obtained molybdenum disulfide nano sheet of the embodiment of the present invention 1 obtains.
Fig. 7 is the SEM photo of the tungsten disulfide nano slices that the embodiment of the present invention 3 obtains.From the triangle and the hexagonal configuration that this view it is apparent that tungsten disulfide nano slices.
Fig. 8 is the FE-SEM photo of the tungsten disulfide nano slices that the embodiment of the present invention 3 obtains.From the size and the thickness that this view it is apparent that tungsten disulfide nano slices.
Fig. 9 is the TEM photo of the tungsten disulfide nano slices that the embodiment of the present invention 3 obtains.From the overall structure that this view it is apparent that tungsten disulfide nano slices.
Figure 10 is the TEM photo of the tungsten disulfide nano slices that the embodiment of the present invention 3 obtains.From the sheet number of layers and the lattice dot matrix that this view it is apparent that tungsten disulfide nano slices.
Figure 11 is the SEAD image of the tungsten disulfide nano slices that the embodiment of the present invention 3 obtains.From the monocrystalline feature diffraction pattern that this view it is apparent that tungsten disulfide nano slices.
Figure 12 is the XRD collection of illustrative plates of the tungsten disulfide nano slices that the embodiment of the present invention 3 obtains.
Figure 13 is the SEM photo of the cobalt disulfide nanometer sheet that the embodiment of the present invention 5 obtains.From the pattern and the size that this view it is apparent that cobalt disulfide nanometer sheet.
Figure 14 is the XRD collection of illustrative plates of the cobalt disulfide nanometer sheet that the embodiment of the present invention 5 obtains.
Embodiment
Below in conjunction with specific embodiment, particular content of the present invention is described as follows:
Embodiment 1:
Take 0.3531g ammonium molybdate, 0.3654g thiocarbamide and 17.55g sodium chloride, mixture is dissolved in the deionized water of 100ml, with the magnetic stirring apparatus of mixing speed 300r/min, stirring and dissolving wiring solution-forming, and then take power as the ultrasonic 15min of ultrasonic device of 400W, mix.Mixed liquor is put into refrigerator 12h to freeze, be placed on-50 DEG C of vacuumizes in freeze drier, until dry obtain mixture.Milled mixtures also crosses 150 mesh sieves, get 10g powder and be placed in Noah's ark, Noah's ark is put into tube furnace, pass into the Ar inert gas deaeration of 200ml/min, again with the Ar inert gas of 200ml/min, and be warming up to temperature 750 DEG C with the programming rate of 10 DEG C/min, insulation 2h carries out chemical vapour deposition (CVD), under Ar atmosphere protection, room temperature is cooled to after reaction terminates, obtain calcined product A, collect, porphyrize, be washed to till there is no NaCl in product, at-50 DEG C, vacuumize 8h is carried out in freeze drier, obtain molybdenum disulfide nano sheet, the how triangular in shape and hexagon of this molybdenum disulfide nano sheet, the length of single nanometer sheet is 0.1-40um, thickness is 0.6-100.0nm, the molybdenum disulfide nano sheet number of plies is 1-40 layer.
By 0.1458g molybdenum disulfide nano sheet, 0.1519gPVDF, 0.0183g conductive carbon black mixes after slurry is made in stirring and is applied to copper sheet as negative pole, with the LiPF of 1M
6as electrolyte, using lithium sheet as positive pole, obtained half-cell, the specific capacity of more than 250mAh/g still protected by its 50 circles that circulate under the current density of 100mA/g, as shown in Figure 6.
Embodiment 2:
Take 0.3531g ammonium molybdate, 0.3654g thiocarbamide and 35.1g sodium chloride, mixture is dissolved in the deionized water of 150ml, with the magnetic stirring apparatus of mixing speed 300r/min, stirring and dissolving wiring solution-forming, and then take power as the ultrasonic 15min of ultrasonic device of 400W, mix.Mixed liquor is put into refrigerator 12h to freeze, be placed on-50 DEG C of vacuumizes in freeze drier, until dry obtain mixture.Milled mixtures also crosses 100 mesh sieves; get 10g powder and be placed in Noah's ark; Noah's ark is put into tube furnace; pass into the Ar inert gas deaeration of 200ml/min; temperature 600 DEG C is warming up to the programming rate of 10 DEG C/min again with the Ar inert gas of 200ml/min; insulation 3h carries out chemical vapour deposition (CVD); under Ar atmosphere protection, room temperature is cooled to after reaction terminates; obtain calcined product A; collect, porphyrize, is washed to till not having NaCl in product; in freeze drier, at-50 DEG C, carry out vacuumize 8h, obtain molybdenum disulfide nano sheet.
Embodiment 3:
Take 0.2463g ammonium metatungstate, 0.1827g thiocarbamide and 23.4g sodium chloride, mixture is dissolved in the deionized water of 100ml, with the magnetic stirring apparatus of mixing speed 300r/min, stirring and dissolving wiring solution-forming, and then take power as the ultrasonic 15min of ultrasonic device of 400W, mix.Mixed liquor is put into refrigerator 12h to freeze, be placed on-40 DEG C of vacuumizes in freeze drier, until dry obtain mixture.Milled mixtures also crosses 150 mesh sieves, get 10g powder and be placed in Noah's ark, Noah's ark is put into tube furnace, pass into the Ar inert gas deaeration of 200ml/min, again with the Ar inert gas of 200ml/min, and be warming up to temperature 750 DEG C with the programming rate of 10 DEG C/min, insulation 2h carries out chemical vapour deposition (CVD), under Ar atmosphere protection, room temperature is cooled to after reaction terminates, obtain calcined product B, collect, porphyrize, be washed to till there is no NaCl in product, at-50 DEG C, vacuumize 8h is carried out in freeze drier, obtain tungsten disulfide nano slices, the how triangular in shape and hexagon of this tungsten disulfide nano slices, the length of single nanometer sheet is 0.1-20um, thickness is 0.8-100.0nm, the tungsten disulfide nano slices number of plies is 1-30 layer.
Embodiment 4:
Take 0.3299g sodium tungstate, 0.1827g thiocarbamide and 11.7g sodium chloride, mixture is dissolved in the deionized water of 50ml, with the magnetic stirring apparatus of mixing speed 300r/min, stirring and dissolving wiring solution-forming, and then take power as the ultrasonic 20min of ultrasonic device of 400W, mix.Mixed liquor is put into refrigerator 12h to freeze, be placed on-30 DEG C of vacuumizes in freeze drier, until dry obtain mixture.Milled mixtures also crosses 100 mesh sieves; get 10g powder and be placed in Noah's ark; Noah's ark is put into tube furnace; pass into the Ar inert gas deaeration of 200ml/min; temperature 600 DEG C is warming up to the programming rate of 10 DEG C/min again with the Ar inert gas of 200ml/min; insulation 3h carries out chemical vapour deposition (CVD); under Ar atmosphere protection, room temperature is cooled to after reaction terminates; obtain calcined product B; collect, porphyrize, is washed to till not having NaCl in product; in freeze drier, at-50 DEG C, carry out vacuumize 8h, obtain tungsten disulfide nano slices.
Embodiment 5:
Take 0.2910g cobalt nitrate, 0.1827g thiocarbamide and 23.4g sodium chloride, mixture is dissolved in the deionized water of 100ml, with the magnetic stirring apparatus of mixing speed 300r/min, stirring and dissolving wiring solution-forming, and then take power as the ultrasonic 20min of ultrasonic device of 400W, mix.Mixed liquor is put into refrigerator 12h to freeze, be placed on-30 DEG C of vacuumizes in freeze drier, until dry obtain mixture.Milled mixtures also crosses 100 mesh sieves, get 10g powder and be placed in Noah's ark, Noah's ark is put into tube furnace, pass into the Ar inert gas deaeration of 200ml/min, again with the Ar inert gas of 200ml/min, and be warming up to temperature 550 DEG C with the programming rate of 10 DEG C/min, insulation 2h carries out chemical vapour deposition (CVD), under Ar atmosphere protection, room temperature is cooled to after reaction terminates, obtain calcined product C, collect, porphyrize, be washed to till there is no NaCl in product, at-50 DEG C, vacuumize 8h is carried out in freeze drier, obtain cobalt disulfide nanometer sheet, this cobalt disulfide nanometer sheet is many in roundlet plate-like, the length of single nanometer sheet is 50-150nm.
Embodiment 6:
Take 0.2910g cobalt nitrate, 0.1827g thiocarbamide and 35.1g sodium chloride, mixture is dissolved in the deionized water of 150ml, with the magnetic stirring apparatus of mixing speed 300r/min, stirring and dissolving wiring solution-forming, and then take power as the ultrasonic 20min of ultrasonic device of 400W, mix.Mixed liquor is put into refrigerator 12h to freeze, be placed on-30 DEG C of vacuumizes in freeze drier, until dry obtain mixture.Milled mixtures also crosses 100 mesh sieves; get 10g powder and be placed in Noah's ark; Noah's ark is put into tube furnace; pass into the Ar inert gas deaeration of 200ml/min; temperature 550 DEG C is warming up to the programming rate of 10 DEG C/min again with the Ar inert gas of 200ml/min; insulation 2h carries out chemical vapour deposition (CVD); under Ar atmosphere protection, room temperature is cooled to after reaction terminates; obtain calcined product C; collect, porphyrize, is washed to till not having NaCl in product; in freeze drier, at-50 DEG C, carry out vacuumize 8h, obtain cobalt disulfide nanometer sheet.
Claims (2)
1. a preparation method for water-insoluble transition metal dichalcogenide nanometer sheet, comprises the following steps:
(1). with the water soluble salt containing transition metal for transition metal source, take thiocarbamide as sulphur source, by the transition metal in transition metal source, the mol ratio of the element sulphur in sulphur source is 1:(1.8 ~ 2.5), and be 1:(150 ~ 600 by the mol ratio of the transition metal in transition metal source and NaCl), by transition metal source, sulphur source and NaCl add in deionized water and dissolve, stir wiring solution-forming, again ultrasonic mix after freezing at 0 DEG C, colder temperature in-50 DEG C ~-30 DEG C after solution freeze over carries out vacuumize, obtain mixture,
(2). the mixture grind into powder obtained by step (1), is laid in Noah's ark after crossing 100-300 mesh sieve, is placed in tube furnace flat-temperature zone and calcines: with N
2, a kind of gas of He and Ar or mist as inert gas source, be first that 200-400ml/min passes into inert gas 10-30 minute with deaeration with flow; Again using Ar as protection gas, shielding gas flow amount is fixed as 50-300ml/min, is warming up to 550-750 DEG C with the programming rate of 1-10 DEG C/min, insulation 1-3h carries out chemical vapour deposition (CVD), cools to room temperature with the furnace, obtain product M after reaction terminates;
(3). collect the powder product M that step (2) is obtained, be washed to till there is no NaCl in calcined product, the product after washing is carried out vacuumize, obtains water-insoluble transition metal dichalcogenide nanometer sheet.
2. the preparation method of water-insoluble transition metal dichalcogenide nanometer sheet according to claim 1, is characterized in that, described water-insoluble transition metal dichalcogenide is cobalt disulfide.
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| CN107090586A (en) * | 2017-04-13 | 2017-08-25 | 上海应用技术大学 | A kind of FeS2RGO composites, preparation method and applications |
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| CN105417582A (en) * | 2015-12-22 | 2016-03-23 | 镇江市高等专科学校 | Method for preparing graphite-like tungsten disulfide nano-sheet |
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