CN105217687A - A kind of molybdenum disulfide nano sheet preparation method based on sodium-chlor template - Google Patents
A kind of molybdenum disulfide nano sheet preparation method based on sodium-chlor template Download PDFInfo
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- CN105217687A CN105217687A CN201510583045.0A CN201510583045A CN105217687A CN 105217687 A CN105217687 A CN 105217687A CN 201510583045 A CN201510583045 A CN 201510583045A CN 105217687 A CN105217687 A CN 105217687A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—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
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention relates to a kind of molybdenum disulfide nano sheet preparation method based on sodium-chlor template, comprise: with one or both mixtures in ammonium molybdate, Sodium orthomolybdate for molybdenum source, take thiocarbamide as sulphur source, be 1:(1.8 ~ 2.5 by the sulphur mol ratio in the molybdenum in molybdenum source, sulphur source), and be 1:(150 ~ 600 by the mol ratio of the molybdenum in molybdenum source and NaCl), molybdenum source, sulphur source and NaCl are added in deionized water and dissolves, more freezing and carry out vacuum-drying, obtain mixture; By obtained mixture grind into powder, be laid on after sieving in Noah's ark, be placed in tube furnace flat-temperature zone and carry out calcining and chemical vapour deposition, obtain product A; Wash and carry out vacuum-drying, obtaining molybdenum disulfide nano sheet.The present invention can obtain the molybdenum disulfide nano sheet with features such as quality are high, size uniformity, the number of plies are relatively controlled, output is higher, preparation cost is relatively low.
Description
Technical field
The present invention relates to a kind of molybdenum disulfide nano sheet material and preparation method thereof, can be applicable to and be not limited only to electrode material of secondary lithium ion battery field.
Background technology
Molybdenumdisulphide is as the typical transition metal dichalcogenide of one, and the physics and chemistry character of its uniqueness causes scientists interest receive large quantifier elimination widely in recent years.Molybdenumdisulphide has the close-packed hexagonal structure being similar to Graphene, similar lamella way of stacking; Single molybdenumdisulphide molecular layer is combined into the sandwich-like covalently bonded of S-Mo-S by two-layer S atomic shell, one deck Mo atomic shell, then combines with more weak van der waals forces between molybdenumdisulphide molecular layer.Compared to Graphene, molybdenumdisulphide has larger (002) spacing that width is 0.62nm, and can store more lithium ion at sheet interlayer, it can reach 669mAh/g as lithium ion battery anode active material theoretical specific capacity; Meanwhile, more active site position of coming out, molybdenumdisulphide lamella edge is also conducive to as H
+etc. absorption and the reaction of active positive ion, molybdenumdisulphide is made to have good catalytic reaction activity; In addition, molybdenumdisulphide also has the photovoltaic effect etc. of good rub resistance, erosion resistance and uniqueness, is also widely used in the industries such as automobile, boats and ships, semi-conductor.
Along with progressively going deep into of research, scientists finds that the two-dimentional microtexture of molybdenumdisulphide uniqueness may be the root place of its peculiar property; Utilize the two-dimensional layered structure of molybdenumdisulphide and other materials to carry out compound and on properties, constantly obtain new peak especially.And nanometer sheet a kind of avatar that to be two dimensional character best, therefore, preparing high-quality molybdenum disulfide nano sheet has become the problem that in scientific research and industrial application, must solve.Stripping method prepared main, the most ripe method of molybdenum disulfide nano sheet in the last few years, generally using business-like molybdenumdisulphide block powder as starting material, molybdenum disulfide nano sheet (Adv.Mater.2012 is prepared by the mode of ultrasonic degradation or chemical stripping, 24,772 – 775) (J.Am.Chem.Soc.2013,135,10274-10277); Although stripping method is simply direct, also there is certain problem, as easily damaged in nanometer sheet, of low quality, dimensional thickness skewness, preparation time are grown, are easily caused noise pollution and chemical pollution etc.Synthesis method can obtain that degree of crystallinity is high, the measured molybdenum disulfide nano structure of matter, but because nanometer sheet itself has larger specific surface area, it spontaneously can tend to heap superimposition and reunite to reduce system Gibbs free energy, therefore up to the present, the way utilizing synthesis is all often obtain a kind of similar flower-shaped structure (Electrochim.Acta.2014,115,165-169) (RSCAdv.2015,5,7938 – 7943), very difficult acquisition is dispersed better, quality is higher, the molybdenum disulfide nano sheet of size uniformity.
Summary of the invention
The object of this invention is to provide a kind of molybdenum disulfide nano sheet and preparation method.Molybdenum disulfide nano sheet preparation method provided by the invention, NaCl is utilized to make template, the ratio fully controlled well between molybdate, thiocarbamide, NaCl, make molybdate and thiocarbamide discontinuously arranged in single NaCl self-assembly, template is by the growth in a thickness direction of restriction nanometer sheet simultaneously, after a step chemical vapour deposition, the molybdenum disulfide nano sheet with features such as 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,
Based on a molybdenum disulfide nano sheet preparation method for sodium-chlor template, comprise the following steps:
(1). with one or both mixtures in ammonium molybdate, Sodium orthomolybdate for molybdenum source, take thiocarbamide as sulphur source, be 1:(1.8 ~ 2.5 by the sulphur mol ratio in the molybdenum in molybdenum source, sulphur source), and be 1:(150 ~ 600 by the mol ratio of the molybdenum in molybdenum source and NaCl), molybdenum source, sulphur source and NaCl are added in deionized water and dissolve, stir wiring solution-forming, more ultrasonic mix after freezing at 0 DEG C, after solution freeze over, carry out vacuum-drying, obtain mixture;
(2). the mixture grind into powder obtained by step (1), be laid on after crossing 100-300 mesh sieve in Noah's ark, being placed in tube furnace flat-temperature zone to calcine: using a kind of gas of N2, He and Ar or mixed gas as inert gas source, is first that 200-400ml/min passes into rare gas element 10-30 minute with excluding air with flow; Again using Ar as protection gas, shielding gas flow amount is fixed as 50-300ml/min, is warming up to 600-750 DEG C with the heat-up rate of 1-10 DEG C/min, insulation 1-3h carries out chemical vapour deposition, cools to room temperature with the furnace, obtain product A after reaction terminates;
(3). collect the powder product A that step (2) is obtained, be washed to till there is no NaCl in calcinate, the product after washing is placed in and carries out vacuum-drying, obtain molybdenum disulfide nano sheet.
Wherein, in step (3), the product after washing is placed in freeze drier at the temperature of-50 DEG C ~-30 DEG C and carries out vacuum-drying 8h, obtain molybdenum disulfide nano sheet.
This molybdenum disulfide nano sheet can be applied to lithium ion battery negative.
The present invention has the following advantages: the present invention utilizes raw material cheap and easy to get to prepare molybdenum disulfide nano sheet, with low cost, and reaction process is simple, controllability is strong.This kind of material crystalline degree is high simultaneously, quality is good, and structure is homogeneous, and pattern is excellent, excellent performance, molybdenum disulfide nano sheet is used for lithium ion battery negative and has certain specific storage and cycle performance, and circulating under the current density of 100mA/g still to keep the specific storage of more than 250mAh/g after 50 times.
Accompanying drawing explanation
Fig. 1 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. 2 is the FE-SEM photo of the molybdenum disulfide nano sheet that the embodiment of the present invention 1 obtains.From the thickness 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 one-piece construction 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 that this view it is apparent that molybdenum disulfide nano sheet.
Fig. 5 is the TEM photo of the molybdenum disulfide nano sheet that the embodiment of the present invention 1 obtains.From the typical cellular shape lattice dot matrix that this view it is apparent that molybdenum disulfide nano sheet.
Fig. 6 is the SEAD image of the molybdenum disulfide nano sheet that the embodiment of the present invention 1 obtains.From the feature diffraction pattern that this view it is apparent that molybdenum disulfide nano sheet.
Fig. 7 is the XRD figure spectrum of the molybdenum disulfide nano sheet that the embodiment of the present invention 1 obtains.
Fig. 8 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.
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 35.1g sodium-chlor, mixture is dissolved in the deionized water of 200ml, with the magnetic stirring apparatus of stirring velocity 300r/min, stirring and dissolving wiring solution-forming, and then take power as the ultrasonic 15min of ultrasonic device of 400W, mix.Mixed solution is put into refrigerator 12h to freeze, be placed on-50 DEG C of vacuum-dryings in freeze drier, until dry obtain mixture.Grinding mixture 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 rare gas element excluding air of 200ml/min, again with the Ar rare gas element of 200ml/min, and be warming up to temperature 750 DEG C with the heat-up rate of 10 DEG C/min, insulation 2h carries out chemical vapour deposition, under Ar atmosphere protection, room temperature is cooled to after reaction terminates, obtain calcinate A, collect, porphyrize, be washed to till there is no NaCl in product, at-50 DEG C, vacuum-drying 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 0.1285g molybdenum disulfide nano sheet, 0.1338gPVDF, 0.0161g 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 electrolytic solution, using lithium sheet as positive pole, obtained half-cell, the specific storage 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 0.1765g ammonium molybdate, 0.1827g thiocarbamide and 17.55g sodium-chlor, mixture is dissolved in the deionized water of 150ml, with the magnetic stirring apparatus of stirring velocity 300r/min, stirring and dissolving wiring solution-forming, and then take power as the ultrasonic 15min of ultrasonic device of 400W, mix.Mixed solution is put into refrigerator 12h to freeze, be placed on-50 DEG C of vacuum-dryings in freeze drier, until dry obtain mixture.Grinding mixture 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 rare gas element excluding air of 200ml/min; temperature 600 DEG C is warming up to the heat-up rate of 10 DEG C/min again with the Ar rare gas element of 200ml/min; insulation 3h carries out chemical vapour deposition; under Ar atmosphere protection, room temperature is cooled to after reaction terminates; obtain calcinate A; collect, porphyrize, is washed to till not having NaCl in product; in freeze drier, at-50 DEG C, carry out vacuum-drying 8h, obtain molybdenum disulfide nano sheet.
Embodiment 3:
Take 0.1765g Sodium orthomolybdate, 0.1827g thiocarbamide and 26.325g sodium-chlor, mixture is dissolved in the deionized water of 200ml, with the magnetic stirring apparatus of stirring velocity 300r/min, stirring and dissolving wiring solution-forming, and then take power as the ultrasonic 15min of ultrasonic device of 400W, mix.Mixed solution is put into refrigerator 12h to freeze, be placed on-40 DEG C of vacuum-dryings in freeze drier, until dry obtain mixture.Grinding mixture 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 rare gas element excluding air of 200ml/min; temperature 750 DEG C is warming up to the heat-up rate of 10 DEG C/min again with the Ar rare gas element of 200ml/min; insulation 2h carries out chemical vapour deposition; under Ar atmosphere protection, room temperature is cooled to after reaction terminates; obtain calcinate A; collect, porphyrize, is washed to till not having NaCl in product; in freeze drier, at-50 DEG C, carry out vacuum-drying 8h, obtain molybdenum disulfide nano sheet.
Embodiment 4:
Take 0.1765g Sodium orthomolybdate, 0.1827g thiocarbamide and 35.1g sodium-chlor, mixture is dissolved in the deionized water of 200ml, with the magnetic stirring apparatus of stirring velocity 300r/min, stirring and dissolving wiring solution-forming, and then take power as the ultrasonic 20min of ultrasonic device of 400W, mix.Mixed solution is put into refrigerator 12h to freeze, be placed on-30 DEG C of vacuum-dryings in freeze drier, until dry obtain mixture.Grinding mixture 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 rare gas element excluding air of 200ml/min; temperature 600 DEG C is warming up to the heat-up rate of 10 DEG C/min again with the Ar rare gas element of 200ml/min; insulation 3h carries out chemical vapour deposition; under Ar atmosphere protection, room temperature is cooled to after reaction terminates; obtain calcinate A; collect, porphyrize, is washed to till not having NaCl in product; in freeze drier, at-50 DEG C, carry out vacuum-drying 8h, obtain molybdenum disulfide nano sheet.
Claims (2)
1., based on a molybdenum disulfide nano sheet preparation method for sodium-chlor template, comprise the following steps:
(1). with one or both mixtures in ammonium molybdate, Sodium orthomolybdate for molybdenum source, take thiocarbamide as sulphur source, be 1:(1.8 ~ 2.5 by the sulphur mol ratio in the molybdenum in molybdenum source, sulphur source), and be 1:(150 ~ 600 by the mol ratio of the molybdenum in molybdenum source and NaCl), molybdenum source, sulphur source and NaCl are added in deionized water and dissolve, stir wiring solution-forming, more ultrasonic mix after freezing at 0 DEG C, after solution freeze over, carry out vacuum-drying, 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 mixed gas as inert gas source, be first that 200-400ml/min passes into rare gas element 10-30 minute with excluding air with flow; Again using Ar as protection gas, shielding gas flow amount is fixed as 50-300ml/min, is warming up to 600-750 DEG C with the heat-up rate of 1-10 DEG C/min, insulation 1-3h carries out chemical vapour deposition, cools to room temperature with the furnace, obtain product A after reaction terminates;
(3). collect the powder product A that step (2) is obtained, be washed to till there is no NaCl in calcinate, the product after washing is placed in and carries out vacuum-drying, obtain molybdenum disulfide nano sheet.
2. preparation method according to claim 1, is characterized in that, the product after washing is placed in freeze drier at the temperature of-50 DEG C ~-30 DEG C and carries out vacuum-drying 8h, obtain molybdenum disulfide nano sheet.
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| CN107747106B (en) * | 2017-09-22 | 2020-02-07 | 天津大学 | Nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material and preparation |
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| CN109128149A (en) * | 2018-08-22 | 2019-01-04 | 天津大学 | The method for preparing three-dimensional carbon nanomaterial in aluminium powder surface in situ using sodium chloride template |
| CN109371381B (en) * | 2018-11-29 | 2021-01-15 | 河北工业大学 | Method for preparing single-layer molybdenum sulfide/tungsten sulfide in-plane heterojunction by low-temperature one-step method |
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| CN111558383A (en) * | 2020-05-22 | 2020-08-21 | 重庆工商大学 | Preparation method of transition metal doped 3R type molybdenum disulfide catalyst |
| CN111558383B (en) * | 2020-05-22 | 2022-05-06 | 重庆工商大学 | Preparation method of transition metal doped 3R type molybdenum disulfide catalyst |
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Application publication date: 20160106 |