CN104966817A - Molybdenum disulfide-carbon three-dimensional porous network composite and preparation method thereof - Google Patents
Molybdenum disulfide-carbon three-dimensional porous network composite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a molybdenum disulfide-carbon three-dimensional porous network composite and a preparation method thereof. The composite is prepared by compounding molybdenum disulfide nanosheets and carbon. The preparation method comprises the following steps: with NaCl as a dispersant and template, fully dissolving and mixing NaCl, a molybdenum source and a sulfur source and carrying out freeze drying and porphyrization so as to obtain a mixture; putting the mixture in a tubular furnace and carrying out calcining under the protection of argon so as to obtain a calcined product A; and washing the calcined product A and drying the washed calcined product A so as to obtain the molybdenum disulfide-carbon three-dimensional porous network composite. The invention has the following advantages: preparation process is safe and harmless, operation is simple, and yield is high; and the prepared molybdenum disulfide-carbon three-dimensional porous network composite has good reversible capacity and cycle stability as a cathode material of a lithium ion battery.
Description
Technical field
The present invention relates to three-dimensional porous network composite material and the preparation method of a kind of molybdenum bisuphide and carbon, belong to electrode material of secondary lithium ion battery field.
Background technology
Due to electric property and the physical property of its uniqueness, two-dimension nano materials has caused the increasing research interest of people, as Graphene and other similar inorganic matters; They are widely used in the fields such as catalyst, transducer, lithium ion battery.Two-dimensional nano sheet layer material self has larger surface energy, is combined between each molecular layer by van der waals force.In actual application, so two-dimentional lamellar structure is more prone to spontaneous compression and reunites to reduce system surface energy, lamella is combined tightr, this is extremely unfavorable for the application of sheet layer material in lithium ion battery negative material etc.
Molybdenum bisuphide is as the typical layer to layer transition metal sulfide of one, and its broad interlamellar spacing is extremely conducive to embedding lithium; Therefore, molybdenum bisuphide is a kind of very outstanding, electrode material intercalation main body that can be applied to high energy density cells, and its theoretical specific capacity can reach 669mAh/g.But, molybdenum disulfide nano sheet as exemplary two dimensional nanostructure can tend to spontaneous reunion in practical application or even in production dry run, cause the active site bit-loss at sheet surfaces and edge, cause two-dimensional structure to destroy, all peculiar properties had of other two-dimensional ultrathin nanostructures also can fade away thereupon simultaneously.Therefore, stoping molybdenum disulfide nano sheet to be reunited is this material urgent problem in actual applications.At present, in order to strengthen molybdenum bisuphide chemical property and the method maintaining its unique two-dimensional nanostructure mainly contains two kinds: one, with the compound such as Graphene, carbon nano-fiber; Nano-sized carbon is as skeleton, greatly enhance the conductivity of material, simultaneously pliable and tough carbon phase skeleton not only can stop that the motion of molybdenum bisuphide lamella is reunited to prevent it, and can also alleviate active material because of embedding/take off lithium and cause change in volume to produce mechanical stress (
adv. Funct. Mater. 2014,
24, 125-130) (
angew. Chem. Int. Ed. 2014,
53, 2152-2156).Its two, build molybdenum bisuphide three-dimensional porous structure; First, porousness can ensure the abundant infiltration of electrolyte, and micrometer structure is worked in coordination with mutually with nanostructure, accelerates the diffusion of lithium ion, makes it fully to contact with active material, three-dimensionalityly whole material can be formed a conductive network, accelerates the transmission of electronics; Secondly, molybdenum bisuphide comparatively graphite has more active site position, makes embedding/de-lithium more rapid, be conducive to material fast charging and discharging (
adv. Mater. 2014,
26, 964-969).But these synthetic methods above all exist certain problem, the interface cohesion of such as molybdenum bisuphide and Graphene is bad, three-dimensional structure stability deficiency, preparation technology's more complicated, energy resource consumption are more high.
One of the effective means that template growth in situ is all considered to build unique texture all the time, improves interface cohesion, improves stability of material.
Summary of the invention
The object of this invention is to provide three-dimensional porous network composite material and the preparation method of a kind of molybdenum bisuphide and carbon.This composite material has good charge-discharge performance as lithium ion battery negative material, has a extensive future, and its preparation method process is simple, can be mass.
The present invention is realized by the following technical programs, the three-dimensional porous network composite material of a kind of molybdenum bisuphide and carbon, it is characterized in that, this composite material is a kind of three-dimensional porous network be made up of the molybdenum disulfide nano sheet of sheet and carbon compound, the aperture of three-dimensional porous network is 0.1-3um, the radius of network is 1-15 μm, the length of molybdenum disulfide nano sheet is wherein 1-30nm, and thickness is 0.6-15.0nm, and the molybdenum disulfide nano sheet number of plies is 1-20 layer; In this composite material, the mass percent of molybdenum bisuphide and carbon is: (0.65 ~ 0.95): (0.35 ~ 0.05).
The preparation method of the molybdenum bisuphide of said structure and the three-dimensional porous network composite material of carbon, is characterized in that comprising the following steps:
(1). with one or both mixtures in ammonium molybdate, sodium molybdate for molybdenum source, take thiocarbamide as sulphur source, be 1:(1.8 ~ 2.5 by the mol ratio of the sulphur in the molybdenum in molybdenum source, sulphur source), and be 1:(5 ~ 15 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, stir wiring solution-forming, again ultrasonic mix after freezing at 0 DEG C, treat that solution freeze over is placed on freeze drier and carries out vacuumize temperature-50 DEG C ~-30 DEG C, 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 in He and Ar or mist as inert gas source, be first that 200-400 ml/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 500-750 DEG C with the programming rate of 1-10 DEG C/min, insulation 2-3h carries out chemical vapour deposition (CVD), cools to room temperature with the furnace, obtain powder 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 this product, at temperature is 60 ~ 120 DEG C, dries 8h, obtain the three-dimensional porous network composite material of molybdenum bisuphide and carbon.
The present invention has the following advantages: the present invention utilizes raw material cheap and easy to get to prepare the three-dimensional porous network composite material of molybdenum bisuphide and carbon, and with low cost, course of reaction is simple, controllability is strong.This material interface combines good simultaneously, and structure is homogeneous, and pattern is excellent, excellent performance, has good specific capacity and cycle performance for lithium ion battery negative, circulates and still can keep the specific capacity of more than 580mAh/g after 30 times under the current density of 100mA/g.
Accompanying drawing explanation
fig. 1the SEM photo of the molybdenum bisuphide obtained for the embodiment of the present invention 1 and the three-dimensional porous network composite material of carbon.From this
figureobviously find out the pattern of the three-dimensional porous network of molybdenum bisuphide and carbon.
fig. 2the TEM photo of the molybdenum bisuphide obtained for the embodiment of the present invention 1 and the three-dimensional porous network composite material of carbon.From this
figureobviously find out the structure of the three-dimensional porous network of molybdenum bisuphide and carbon.
fig. 3the XRD of the molybdenum bisuphide obtained for the embodiment of the present invention 1 and the three-dimensional porous network composite material of carbon
figurespectrum.
fig. 4the TG of the molybdenum bisuphide obtained for the embodiment of the present invention 1 and the three-dimensional porous network composite material of carbon
figurespectrum.
fig. 5the nitrogen thermostatic absorption of the molybdenum bisuphide obtained for the embodiment of the present invention 1 and the three-dimensional porous network composite material of carbon takes off
accompanying drawingspectrum.
fig. 6the pore analysis of the molybdenum bisuphide obtained for the embodiment of the present invention 1 and the three-dimensional porous network composite material of carbon
figurespectrum.
fig. 7the charge-discharge performance of the lithium ion battery negative obtained for adopting the three-dimensional porous network composite material of the obtained molybdenum bisuphide of the embodiment of the present invention 1 and carbon
figure.
Embodiment
Below in conjunction with specific embodiment, particular content of the present invention is described as follows:
Embodiment 1:
Take 3.531g ammonium molybdate, 3.045g thiocarbamide and 8.775g 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 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, dry at 80 DEG C, obtain the three-dimensional porous network composite material of molybdenum bisuphide and carbon, the length of its molybdenum disulfide nano sheet is at 1-30nm, thickness is at 0.6-15.0nm, the molybdenum disulfide nano sheet number of plies is at 1-20 layer, the aperture of the three-dimensional porous network of molybdenum bisuphide and carbon is 0.1-3um, radius is 1-15 μm.
By the three-dimensional porous network composite material of 0.2032g molybdenum bisuphide and carbon, the PVDF of 0.2117g, 0.0254g 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 580mAh/g still protected by its 30 circles that circulate under the current density of 100mA/g,
as Fig. 1shown in.
Embodiment 2:
Take 3.531g ammonium molybdate, 2.736g thiocarbamide and 5.85g 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 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 750 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 A; collect, porphyrize, is washed to till not having NaCl in product; dry at 80 DEG C, obtain the three-dimensional porous network composite material of molybdenum bisuphide and carbon.
Embodiment 3:
Take 3.531g ammonium molybdate, 3.806g thiocarbamide and 13.162g sodium chloride, mixture is dissolved in the deionized water of 75ml, 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; temperature 500 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; dry at 80 DEG C, obtain the three-dimensional porous network composite material of molybdenum bisuphide and carbon.
Embodiment 4:
Take 3.531g ammonium molybdate, 3.350g 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 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 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; temperature 650 DEG C is warming up to the programming rate of 10 DEG C/min again with the Ar inert gas of 200ml/min; insulation 2.5h 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; dry at 80 DEG C, obtain the three-dimensional porous network composite material of molybdenum bisuphide and carbon.
Claims (2)
1. the three-dimensional porous network composite material of a molybdenum bisuphide and carbon, it is characterized in that, this composite material is a kind of three-dimensional porous network be made up of the molybdenum disulfide nano sheet of sheet and carbon compound, the aperture of three-dimensional porous network is 0.1-3um, the radius of network is 1-15 μm, the length of molybdenum disulfide nano sheet is wherein 1-30nm, thickness is 0.6-15.0nm, and the molybdenum disulfide nano sheet number of plies is 1-20 layer; In this composite material, the mass percent of molybdenum bisuphide and carbon is: (0.65 ~ 0.95): (0.35 ~ 0.05).
2. press a preparation method for the three-dimensional porous network composite material of molybdenum bisuphide according to claim 1 and carbon, it is characterized in that comprising the following steps:
With one or both mixtures in ammonium molybdate, sodium molybdate 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:(5 ~ 15 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, stir wiring solution-forming, again ultrasonic mix after freezing at 0 DEG C, treat that solution freeze over is placed on freeze drier and carries out vacuumize temperature-50 DEG C ~-30 DEG C, 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 in He and Ar or mist as inert gas source, be first that 200-400 ml/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 500-750 DEG C with the programming rate of 1-10 DEG C/min, insulation 2-3h carries out chemical vapour deposition (CVD), cools to room temperature with the furnace, obtain powder 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 this product, at temperature is 60 ~ 120 DEG C, dries 8h, obtains the net composites of three-dimensional porous molybdenum bisuphide and carbon.
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| CN106058200A (en) * | 2016-07-25 | 2016-10-26 | 天津大学 | Method for modifying titanium-dioxide lithium-ion battery negative pole material simultaneously by using carbon and monolayer molybdenum disulfide |
| CN106784284A (en) * | 2016-12-18 | 2017-05-31 | 苏州思创源博电子科技有限公司 | A kind of preparation method of molybdenum bisuphide composite thermoelectric material |
| CN106848228A (en) * | 2017-01-24 | 2017-06-13 | 同济大学 | A kind of method for preparing molybdenum bisuphide/carbon combined multi-stage Porous materials |
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| CN110683522B (en) * | 2019-10-08 | 2021-06-11 | 中南大学 | Transition metal chalcogen family carbon-based heterostructure composite material with regular morphology and preparation method and application thereof |
| CN113735173A (en) * | 2021-09-08 | 2021-12-03 | 北京航空航天大学 | Molybdenum sulfide-molybdenum nitride composite material and preparation method and application thereof |
| CN114618425A (en) * | 2021-12-23 | 2022-06-14 | 武汉大学(肇庆)资源与环境技术研究院 | Molybdenum disulfide/diatomite composite material and preparation method and application thereof |
| CN114618425B (en) * | 2021-12-23 | 2023-11-03 | 武汉大学(肇庆)资源与环境技术研究院 | Molybdenum disulfide/diatomite composite material and preparation method and application thereof |
| CN115000370A (en) * | 2022-06-02 | 2022-09-02 | 烟台大学 | Molybdenum dioxide confinement growth and modification three-dimensional porous carbon composite electrode material and preparation method thereof |
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