CN104409706A - Molybdenum disulfide/sulfur-and-nitrogen-doped graphene nanosheet composite material as well as preparation method and application thereof - Google Patents
Molybdenum disulfide/sulfur-and-nitrogen-doped graphene nanosheet composite material as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a molybdenum disulfide/sulfur-and-nitrogen-doped graphene nanosheet composite material as well as a preparation method and an application thereof. According to the composite material, molybdenum disulfide is supported on a sulfur-and-nitrogen-doped graphene nanosheet. The preparation method of the composite material comprises steps as follows: ammonium tetrathiomolybdate, graphene oxide and thiourea are dissolved in N,N-dimethyl formamide and evenly mixed, a mixed solution is obtained, and then the mixed solution is dried and finally sintered in a protective gas; the mass ratio of the ammonium tetrathiomolybdate to the graphene oxide to the thiourea is in a range of (1-500):15:(10-1,000). The molybdenum disulfide/sulfur-and-nitrogen-doped graphene nanosheet composite material is wide in application range and can be applied to fields of lithium ion batteries, supercapacitors, hydrogen separation, photocatalysis, nanometer devices and the like.
Description
Technical field
The present invention relates to inorganic nano material, particularly relate to a kind of nano composite material and its preparation method and application.
Background technology
Current lithium ion battery is as the free of contamination chemical power source of a kind of novel high-energy, be subject to the favor of global energy chemical research person, with traditional primary cell compared with secondary cell, lithium ion battery has the advantages such as discharge voltage is high, self discharge is little, memory-less effect, be widely used in the fields such as information, electronics, traffic, national defense and military. in many transition metal materials, MoS
2as the stratified material of a kind Graphene, except having except extensive use in territories such as lubrication and catalysis necks, scientific research personnel finds that it also has huge application prospect in lithium cell cathode material field in recent years.MoS
2theoretical capacity as lithium ion battery negative material reaches every moles of active species in 670mAh/g(assumed response process has four mole electron to participate in reaction).Research shows in charge and discharge process, easily polarize consequently by the electrode material of bulky grain size, and capacity attenuation is fast, nano material has large specific area can increase the contact area with electrolyte, relatively can reduce the diffusion length of electronics and ion, thus reduce the decay of capacity, but, large specific surface easily causes nano material to be reunited, and reduces the contact area with electrode solution; It is one of method effectively reducing nano material reunion that nano material is grown in certain substrate.
Recently, the grapheme material developed rapidly, due to its have surface area large, conduct electricity very well, the advantage such as pliability is good, chemical property is steady, be widely used in the fields such as chemistry, biology, electronics.In lithium ion battery negative material, Graphene has more superior removal lithium embedded performance compared with other material with carbon elements.In addition, Graphene can also prevent nano particle to reunite in cyclic process as resilient coating.The compound of usual molybdenum bisuphide and Graphene is all adopt the sulphur such as thioacetamide, thiocarbamide source, adopts ammonium molybdate or sodium molybdate to be that molybdenum source adds a certain amount of graphene oxide again and mixes and carry out the compound that hydro-thermal reaction obtains molybdenum bisuphide and Graphene.Molybdenum bisuphide is poor as a kind of semiconducting electrical conductivity, the conductivity that really can increase material with Graphene compound is conducive to electric transmission, but the graphene conductive that hydro-thermal reaction obtains not is very desirable, and the molybdenum bisuphide that hydro-thermal reaction obtains not is that growth in situ just mixes with it on Graphene, the molybdenum bisuphide of lamella and the contact defective tightness of Graphene, electric transmission path can be increased like this, the sample throughput that another aspect hydro-thermal reaction obtains is less, is unfavorable for large-scale production.
Summary of the invention
Technical problem to be solved by this invention is, overcome the deficiency and defect mentioned in above background technology, the composite material of a kind of specific area is large, chemical property is good molybdenum bisuphide/sulphur, nitrogen-doped graphene nanometer sheet is provided, also correspondingly provide a kind of preparation method simple, the molybdenum bisuphide/sulphur of large-scale production, the preparation method of the composite material of nitrogen-doped graphene nanometer sheet and the application in lithium ion battery preparation can be carried out.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes is a kind of molybdenum bisuphide/sulphur, nitrogen-doped graphene nanosheet composite material, and in described composite material, molybdenum bisuphide load is on the graphene nanometer sheet of sulphur, N doping.By MoS
2the transmission of electronics in electrochemical reaction process can not only be promoted after being compounded to form compound with Graphene, the change in volume problem of electrode in embedding lithium and de-lithium process can be slowed down simultaneously, prevent MoS
2the efflorescence of heap sum.
In above-mentioned molybdenum bisuphide/sulphur, nitrogen-doped graphene nanosheet composite material, preferably, the disk of described composite material to be diameter be 40 ~ 100nm.
As a total technical conceive, the present invention also provides the preparation method of a kind of above-mentioned molybdenum bisuphide/sulphur, nitrogen-doped graphene nanosheet composite material, comprise the following steps: four thio ammonium molybdate, graphene oxide, thiocarbamide are dissolved in N, in dinethylformamide (DMF), ultrasonic, mix, obtain mixed solution, then above-mentioned mixed solution is dry, finally sinter in protective gas;
The mass ratio of described four thio ammonium molybdate, graphene oxide, thiocarbamide is 1 ~ 500:15:10 ~ 1000.
In above-mentioned preparation method, preferably, the volume of described DMF (DMF) and the corresponding relation of described graphene oxide quality are 1mL/mg ~ 1000 mL/mg.
In above-mentioned preparation method, preferably, the concrete steps of described drying are: at 90 ~ 110 DEG C, rotary evaporation carries out preliminarily dried, then further vacuumize at 80 ~ 120 DEG C.
In above-mentioned preparation method, preferably, it is characterized in that, described sintering is divided into three phases, the first stage: by the ramp to 450 DEG C of 1 ~ 10 DEG C/min, insulation 1 ~ 3h; Second stage: by the ramp to 800 DEG C of 1 ~ 10 DEG C/min, insulation 1 ~ 3h; Phase III is temperature-fall period: be cooled to 300 DEG C by the speed of 5 DEG C/min, then Temperature fall is to room temperature.
In above-mentioned preparation method, preferably, in the described first stage, protective gas is Ar/H
2, wherein the volume fraction of hydrogen is 10%; In second and third stage described, protective gas is argon gas.
As a total technical conceive, the present invention also provides a kind of above-mentioned molybdenum bisuphide/sulphur, nitrogen-doped graphene nanosheet composite material is preparing the application in lithium ion battery.
Design of the present invention is: four thio ammonium molybdate, graphene oxide, thiocarbamide are dissolved in DMF according to certain ratio and make it mix, drying is placed in tube furnace first through Ar/H
2(10%) 450 DEG C of process a period of time, make MoS
2the thermal decomposition of presoma four thio ammonium molybdate formed MoS
2and be laid on graphene oxide, high temperature sintering process under 800 DEG C of conditions in argon shield again, allow thiocarbamide decompose and produce hydrogen sulfide and ammonia, serve as sulphur source and nitrogenous source to graphene oxide defective place doping, make graphene oxide reduce under the high temperature conditions simultaneously, and make the larger-size graphene oxide of script while doping due to the fracture of some chemical bond and formation, cause the fragmentation of Graphene thus reduce Graphene size, final obtains molybdenum bisuphide/sulphur, nitrogen-doped graphene nanosheet composite material, this material has atom doped modification, the features such as specific area is large.
Compared with prior art, the invention has the advantages that:
(1) in the present invention, molybdenum bisuphide load, on the Graphene of sulphur, nitrogen-doping, not only reduces the particle diameter of Graphene, and makes composite material have atom doped modification, characteristic that specific area is large;
(2) molybdenum bisuphide/sulphur of the present invention, nitrogen-doped graphene nanosheet composite material preparation method simply, can carry out large-scale production;
(3) molybdenum bisuphide/sulphur of the present invention, nitrogen-doped graphene nanosheet composite material applied range, can be applicable in fields such as lithium ion battery, ultracapacitor, hydrogen precipitation, photocatalysis, nano-devices.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the molybdenum bisuphide/sulphur of the embodiment of the present invention 1 preparation, the transmission electron microscope photo (TEM) of nitrogen-doped graphene nanosheet composite material.
Fig. 2 is the molybdenum bisuphide/sulphur of the embodiment of the present invention 1 preparation, the x-ray XPS Analysis figure (XPS) of nitrogen-doped graphene nanosheet composite material.
Embodiment
For the ease of understanding the present invention, hereafter will do to describe more comprehensively, meticulously to the present invention in conjunction with Figure of description and preferred embodiment, but protection scope of the present invention is not limited to following specific embodiment.
Unless otherwise defined, hereinafter used all technical terms are identical with the implication that those skilled in the art understand usually.The object of technical term used herein just in order to describe specific embodiment is not be intended to limit the scope of the invention.
Unless otherwise specified, the various raw material, reagent, instrument and equipment etc. used in the present invention are all bought by market and are obtained or prepare by existing method.
embodiment 1
A kind of molybdenum bisuphide/sulphur of the present invention, nitrogen-doped graphene nanosheet composite material, in this composite material, molybdenum bisuphide load is on the graphene nanometer sheet of sulphur, N doping; The disk of this composite material to be diameter be 40 ~ 100nm.
Molybdenum bisuphide/the sulphur of the present embodiment, the preparation method of nitrogen-doped graphene nanosheet composite material, comprise the following steps: take 0.22g four thio ammonium molybdate respectively, 0.15g graphene oxide, 1.5g thiocarbamide, be dissolved in 150mL DMF ultrasonic mix after, after with Rotary Evaporators, in oil bath, 110 DEG C of rotary evaporations remove most of solvent, take out sample 120 DEG C of vacuumizes in surface plate, be placed in quartz boat with mortar porphyrize after taking out after bone dry, be placed in tube furnace, argon gas/hydrogen (10%) and argon gas is connected with threeway, hunt leak with suds again, check that each interface is with or without gas leak phenomenon, guarantee everywhere without after gas leak phenomenon, first logical 20min argon gas, change argon gas/hydrogen (10%) again into, and heating schedule is set to 5 DEG C/min is warming up to 450 DEG C, insulation 3h, recycling threeway changes argon gas into gas, continue to be warming up to 800 DEG C by 450 DEG C with 5 DEG C/min, insulation 1h, 300 DEG C are cooled to again with 5 DEG C/min, Temperature fall is to room temperature again, turn off gas, collect the sample in quartz boat, be molybdenum bisuphide/sulphur, nitrogen-doped graphene nanosheet composite material.
Molybdenum bisuphide/the sulphur of the present embodiment, nitrogen-doped graphene nanosheet composite material can be applicable to the fields such as lithium ion battery, ultracapacitor, hydrogen precipitation, photocatalysis, nano-device.
Fig. 1 be the present embodiment prepare molybdenum bisuphide/sulphur, nitrogen-doped graphene nanosheet composite material transmission electron microscope photo (TEM); As seen from Figure 1, molybdenum bisuphide load on the Graphene of sulphur, N doping with the nanometer sheet of its formation 40 ~ 100nm.Fig. 2 be the present embodiment prepare molybdenum bisuphide/sulphur, nitrogen-doped graphene nanosheet composite material x-ray XPS Analysis figure (XPS).As shown in Figure 2, Graphene is doped with sulphur, nitrogen-atoms.
embodiment 2
A kind of molybdenum bisuphide/sulphur of the present invention, nitrogen-doped graphene nanosheet composite material, in this composite material, molybdenum bisuphide load is on the graphene nanometer sheet of sulphur, N doping; The disk of this composite material to be diameter be 40 ~ 100nm.
Molybdenum bisuphide/the sulphur of the present embodiment, the preparation method of nitrogen-doped graphene nanosheet composite material, comprise the following steps: take 0.3g four thio ammonium molybdate respectively, 0.15g graphene oxide, 2g thiocarbamide, be dissolved in 500mL DMF ultrasonic mix after, after with Rotary Evaporators, in oil bath, 90 DEG C of rotary evaporations remove most of solvent, take out sample 100 DEG C of vacuumizes in surface plate, be placed in quartz boat with mortar porphyrize after taking out after bone dry, be placed in tube furnace, argon gas/hydrogen (10%) and argon gas is connected with threeway, hunt leak with suds again, check that each interface is with or without gas leak phenomenon, guarantee everywhere without after gas leak phenomenon, first logical 20min argon gas, change argon gas/hydrogen (10%) again into, and heating schedule is set to 10 DEG C/min is warming up to 450 DEG C, insulation 2h, recycling threeway changes argon gas into gas, continue to be warming up to 800 DEG C by 450 DEG C with 10 DEG C/min, insulation 2h, 300 DEG C are cooled to again with 5 DEG C/min, Temperature fall is to room temperature again, turn off gas, collect the sample in quartz boat, be molybdenum bisuphide/sulphur, nitrogen-doped graphene nanosheet composite material.
Molybdenum bisuphide/the sulphur of the present embodiment, nitrogen-doped graphene nanosheet composite material can be applicable to the fields such as lithium ion battery, ultracapacitor, hydrogen precipitation, photocatalysis, nano-device.
embodiment 3
A kind of molybdenum bisuphide/sulphur of the present invention, nitrogen-doped graphene nanosheet composite material, in this composite material, molybdenum bisuphide load is on the graphene nanometer sheet of sulphur, N doping; The disk of this composite material to be diameter be 40 ~ 100nm.
Molybdenum bisuphide/the sulphur of the present embodiment, the preparation method of nitrogen-doped graphene nanosheet composite material, comprise the following steps: take 0.2g four thio ammonium molybdate respectively, 0.2g graphene oxide, 2.5g thiocarbamide, be dissolved in 1000mL DMF ultrasonic mix after, after with Rotary Evaporators, in oil bath, 100 DEG C of rotary evaporations remove most of solvent, take out sample 80 DEG C of vacuumizes in surface plate, be placed in quartz boat with mortar porphyrize after taking out after bone dry, be placed in tube furnace, argon gas/hydrogen (10%) and argon gas is connected with threeway, hunt leak with suds again, check that each interface is with or without gas leak phenomenon, guarantee everywhere without after gas leak phenomenon, first logical 20min argon gas, change argon gas/hydrogen (10%) again into, and heating schedule is set to 5 DEG C/min is warming up to 450 DEG C, insulation 3h, recycling threeway changes argon gas into gas, continue to be warming up to 800 DEG C by 450 DEG C with 5 DEG C/min, insulation 2h, 300 DEG C are cooled to again with 5 DEG C/min, Temperature fall is to room temperature again, turn off gas, collect the sample in quartz boat, be molybdenum bisuphide/sulphur, nitrogen-doped graphene nanosheet composite material.
Molybdenum bisuphide/the sulphur of the present embodiment, nitrogen-doped graphene nanosheet composite material can be applicable to the fields such as lithium ion battery, ultracapacitor, hydrogen precipitation, photocatalysis, nano-device.
embodiment 4
A kind of molybdenum bisuphide/sulphur of the present invention, nitrogen-doped graphene nanosheet composite material, in this composite material, molybdenum bisuphide load is on the graphene nanometer sheet of sulphur, N doping; The disk of this composite material to be diameter be 40 ~ 100nm.
Molybdenum bisuphide/the sulphur of the present embodiment, the preparation method of nitrogen-doped graphene nanosheet composite material, comprise the following steps: take 0.3g four thio ammonium molybdate respectively, 0.15g graphene oxide, 2.0g thiocarbamide, be dissolved in 1200mL DMF ultrasonic mix after, after with Rotary Evaporators, in oil bath, 110 DEG C of rotary evaporations remove most of solvent, take out sample 120 DEG C of vacuumizes in surface plate, be placed in quartz boat with mortar porphyrize after taking out after bone dry, be placed in tube furnace, argon gas/hydrogen (10%) and argon gas is connected with threeway, hunt leak with suds again, check that each interface is with or without gas leak phenomenon, guarantee everywhere without after gas leak phenomenon, first logical 20min argon gas, change argon gas/hydrogen (10%) again into, and heating schedule is set to 5 DEG C/min is warming up to 450 DEG C, insulation 2h, recycling threeway changes argon gas into gas, continue to be warming up to 800 DEG C by 450 DEG C with 5 DEG C/min, insulation 1h, 300 DEG C are cooled to again with 5 DEG C/min, Temperature fall is to room temperature again, turn off gas, collect the sample in quartz boat, be molybdenum bisuphide/sulphur, nitrogen-doped graphene nanosheet composite material.
Molybdenum bisuphide/the sulphur of the present embodiment, nitrogen-doped graphene nanosheet composite material can be applicable to the fields such as lithium ion battery, ultracapacitor, hydrogen precipitation, photocatalysis, nano-device.
The foregoing is only case study on implementation of the present invention; not thereby the scope of the claims of the present invention is limited; every specification of the present invention and accompanying drawing equivalent structure that content is done or equivalent flow process of utilizing converts; or be directly or indirectly used in other relevant technical fields, include in protection scope of the present invention.
Claims (8)
1. molybdenum bisuphide/sulphur, a nitrogen-doped graphene nanosheet composite material, is characterized in that, in described composite material, molybdenum bisuphide load is on the graphene nanometer sheet of sulphur, N doping.
2. molybdenum bisuphide/sulphur according to claim 1, nitrogen-doped graphene nanosheet composite material, is characterized in that, the disk of described composite material to be diameter be 40 ~ 100nm.
3. the preparation method of molybdenum bisuphide/sulphur as claimed in claim 1 or 2, nitrogen-doped graphene nanosheet composite material, it is characterized in that, comprise the following steps: four thio ammonium molybdate, graphene oxide, thiocarbamide are dissolved in N, in dinethylformamide, mix, obtain mixed solution, then that above-mentioned mixed solution is dry, finally sinter in protective gas;
The mass ratio of described four thio ammonium molybdate, graphene oxide, thiocarbamide is 1 ~ 500:15:10 ~ 1000.
4. preparation method according to claim 3, is characterized in that, the volume of described DMF and the corresponding relation of described graphene oxide quality are 1mL/mg ~ 1000 mL/mg.
5. preparation method according to claim 3, is characterized in that, the concrete steps of described drying are: at 90 ~ 110 DEG C, rotary evaporation carries out preliminarily dried, then further vacuumize at 80 ~ 120 DEG C.
6. the preparation method according to any one of claim 3 ~ 5, is characterized in that, described sintering is divided into three phases, the first stage: by the ramp to 450 DEG C of 1 ~ 10 DEG C/min, insulation 1 ~ 3h; Second stage: by the ramp to 800 DEG C of 1 ~ 10 DEG C/min, insulation 1 ~ 3h; Phase III is temperature-fall period: be cooled to 300 DEG C by the speed of 5 DEG C/min, then Temperature fall is to room temperature.
7. preparation method according to claim 6, is characterized in that, in the described first stage, protective gas is argon gas and hydrogen, and wherein the volume fraction of hydrogen is 10%; In second and third stage described, protective gas is argon gas.
8. a molybdenum bisuphide/sulphur as claimed in claim 1 or 2, nitrogen-doped graphene nanosheet composite material are preparing the application in lithium ion battery.
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| CN105280887A (en) * | 2015-09-14 | 2016-01-27 | 天津大学 | Preparation method for negative electrode of lithium-ion battery |
| CN105591077A (en) * | 2015-12-17 | 2016-05-18 | 中南大学 | Preparation method of molybdenum carbide/nitrogen-sulfur codoped spongy graphene cathode composite for sodium-ion battery |
| CN105720251A (en) * | 2015-12-20 | 2016-06-29 | 华南理工大学 | Antimony sulfide based composite material of sodium-ion battery and preparation method of antimony sulfide based composite material |
| CN106040264A (en) * | 2016-06-23 | 2016-10-26 | 中国石油大学(华东) | Micron molybdenum disulfide hydrogen evolution electro-catalytic material, preparation method and application of micron molybdenum disulfide hydrogen evolution electro-catalytic material |
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| CN108963215A (en) * | 2018-07-03 | 2018-12-07 | 陕西科技大学 | The fixed porous MoS of N doped graphene flexible substrates with three-dimensional structure2Nano material and its preparation method and application |
| CN109449410A (en) * | 2018-10-30 | 2019-03-08 | 陕西科技大学 | A kind of preparation method of nitrogen, sulphur codope tungsten disulfide anode material of lithium-ion battery |
| WO2019119351A1 (en) * | 2017-12-21 | 2019-06-27 | 惠州拓邦电气技术有限公司 | Lithium ion battery negative electrode material and preparation method therefor, and lithium ion battery |
| CN113241440A (en) * | 2021-05-20 | 2021-08-10 | 中国科学院过程工程研究所 | Molybdenum disulfide/sulfur-doped graphene composite material and preparation method and application thereof |
| CN113243060A (en) * | 2019-05-03 | 2021-08-10 | 株式会社Lg化学 | Separator for lithium secondary battery and lithium secondary battery comprising same |
| CN113413870A (en) * | 2021-05-17 | 2021-09-21 | 中国科学院青海盐湖研究所 | Magnesium oxide-metal sulfide-biomass charcoal composite material and preparation method and application thereof |
| CN114551906A (en) * | 2021-12-31 | 2022-05-27 | 广西科技大学 | Three-dimensional nitrogen-doped graphene/molybdenum disulfide zinc-air battery material with long cycle life and preparation method thereof |
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