CN106803589A - A kind of single dispersing class flower ball-shaped MoS2Raw powder's production technology - Google Patents
A kind of single dispersing class flower ball-shaped MoS2Raw powder's production technology Download PDFInfo
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- CN106803589A CN106803589A CN201710105252.4A CN201710105252A CN106803589A CN 106803589 A CN106803589 A CN 106803589A CN 201710105252 A CN201710105252 A CN 201710105252A CN 106803589 A CN106803589 A CN 106803589A
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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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- 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
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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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- 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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- 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 discloses a kind of single dispersing class flower ball-shaped MoS2Raw powder's production technology.Molybdate compound and sulfur-containing compound are separately added into different solvents by specified mol ratio, different additives are added dropwise in each solvent, stirring latter two solvent is well mixed, then mixed liquor is poured into reactor and is transferred in microwave reaction instrument, specified microwave power, heating rate, reaction temperature and reaction time are set, reactor removal heater cools down reactant by reaction after terminating, and cooling thing is obtained single dispersing class flower ball-shaped MoS through centrifuge washing drying2Powder.The inventive method step is controllable, required low raw-material cost, and preparation-obtained powder realizes single dispersing, even particle size, and the structure of powder is the class flower ball-shaped powder of nano-sheet composition, and the size of powder granule can be controlled by controlling technological parameter.
Description
Technical field
The invention belongs to field of energy source materials, more particularly to a kind of single dispersing class flower ball-shaped MoS2Raw powder's production technology,
Obtained MoS2Powder can be used for lithium ion battery negative material.
Background technology
The features such as lithium ion battery is due to small volume, lightweight, energy density high, memory-less effect has turned into current research
Focus.Compared with other energy and materials, the lithium ion battery extensive use on the mobile devices such as mobile phone, automobile.For total
It, the production and daily life that develop to us of lithium ion battery bring huge facility.Select suitable battery
Electrode material is the key factor for designing lithium ion battery, not only covers cost of material, operating voltage, energy density, power
Density and cycle life, in addition, the security of battery is premise key element.
Used as the business negative material of lithium rechargeable battery, graphite has lot of advantages, and such as operating potential is low, structure
The features such as stabilization, but its capacity is relatively low, about 370 mAhg-1, this shortcoming causes graphite as negative material
The requirement of following electric automobile cannot be met, it is therefore desirable to find energy density, power density higher and with security and stability
Negative material.
MoS2Possess the class Graphene layer structure of uniqueness, its unique crystal structure and theoretical capacity higher cause it
Wide application prospect has been shown in clean energy resource field.But, numerous results of study show, MoS2Negative material is filling
Due to lithiated product Li in discharge process2The gelatinous polymer layer that S forms thickness with electrolysis qualitative response inhibit continuous embedding lithium/
De- lithium reaction, so that it is used as the stability of secondary battery cathode material and forthright unsatisfactory again.To improve MoS2Electricity
Chemical property, scholars have carried out many work.Such as Liu et al. prepares high-sequential by the vacuum assisted process improved
MoS2, good cyclical stability is shown in negative material；Ding et al. is auxiliary by gentle polystyrene microsphere
The method of hydro-thermal is helped to prepare the MoS of stratiform2Microballoon, significantly improves cycle performance and high rate performance.
However, above-mentioned MoS2Preparation method technics comparing it is cumbersome, be difficult to control the flow of preparation technology, and currently report
MoS2Preparation method cannot be readily available monodispersed MoS again2Particle, and then constrain MoS2In lithium ion battery negative material
Application in material.
The content of the invention
In view of above-mentioned MoS2The technology of preparing defect of powder, it is inexpensive, high-quality it is an object of the invention to provide one kind
Single dispersing class flower ball-shaped MoS2Raw powder's production technology, the preparation method can not only allow MoS2Powder is uniformly dispersed, and such is spent
Spherical MoS2Powder is made up of substantial amounts of nano-sheet powder, and the specific surface area of powder has been significantly greatly increased, and promotes MoS2Negative pole material
Expect the cyclical stability in lithium ion battery.
The method of the present invention is, using microwave radiation technology hydro-thermal/solvent-thermal method, well mixed reactant precursor aqueous solution to be added
Enter microwave reaction kettle, controlling reaction temperature and reaction time are the MoS that can obtain class flower ball-shaped structure2Powder granule.
Concretely comprise the following steps：
(1) by Mo:S elemental mole ratios are 1:1 ~ 1.2 weighs molybdenum source and sulphur source, and molybdenum source is dissolved in into deionized water obtained solution A, will
Sulphur source is dissolved in alcohol obtained solution B, and the volume ratio of deionized water and alcohol is 1:0.43~2.33.
(2) it is 9 ~ 12, obtained solution C, Xiang Bu to alkaline solution is added dropwise in solution A obtained in step (1) to adjust its pH value
Suddenly the amine solution that 1 ~ 5mL concentration is 95% is added dropwise in solution B obtained in (1), obtained solution D seals obtained solution respectively
C and solution D, stir 30 ~ 120 minutes, then mix solution C and solution D, stir 30 ~ 120 minutes prepared mixed solutions.
(3) mixed solution obtained in step (2) is poured into reactor and is sealed, in transfer reaction kettle to microwave reaction instrument,
Setting microwave power is 200 ~ 500 W, heating rate is 5 ~ 20 DEG C/min, is warming up to 180 ~ 200 DEG C and reacts 1 ~ 6 hour, reaction
Room temperature is cooled to after end and obtains suspension.
(4) by suspension obtained in step (3) respectively with deionized water and absolute ethyl alcohol centrifuge washing 5 ~ 6 times, centrifuge
Rotating speed be 4000 ~ 10000 revs/min, centrifugation time be 5 ~ 10 minutes, gained be centrifuged product in vacuum drying chamber in 80
Dried 8 ~ 48 hours at DEG C, be cooled to room temperature and single dispersing class flower ball-shaped MoS is obtained2Powder.
The molybdenum source is the one kind in ammonium heptamolybdate, ammonium tetramolybdate, ammonium dimolybdate, ammonium molybdate and sodium molybdate.
The sulphur source is the one kind in thiocarbamide, vulcanized sodium and thioacetamide.
The alcohol is the one kind in ethylene glycol, diethylene glycol (DEG) and glycerine.
The alkaline solution is the one kind in ammoniacal liquor, sodium hydroxide solution and potassium hydroxide solution.
Amine in the amine solution is the one kind in ethylenediamine, n-butylamine and triethylamine.
The inventive method step is controllable, and required low raw-material cost, preparation-obtained powder realizes single dispersing, and particle is big
Small uniform, the structure of powder is the class flower ball-shaped powder of nano-sheet composition, can control powder by controlling technological parameter
The size of grain.
Brief description of the drawings
Fig. 1 is single dispersing class flower ball-shaped MoS obtained in the embodiment of the present invention 12The X ray diffracting spectrum of powder.
Fig. 2 is single dispersing class flower ball-shaped MoS obtained in the embodiment of the present invention 12The field emission scanning electron microscope of powder
Figure.
Specific embodiment
Embodiment 1：
(1) by Mo:S elemental mole ratios are 1:1 weighs 0.196g ammonium molybdates and 0.076g thiocarbamides, by ammonium molybdate be dissolved in 50mL go from
Sub- water obtained solution A, 21.5mL ethylene glycol obtained solutions B is dissolved in by thiocarbamide.
(2) it is 9, obtained solution C, to step to ammonia spirit is added dropwise in solution A obtained in step (1) to adjust its pH value
(1) ethylenediamine solution that 1mL concentration is 95% is added dropwise in solution B obtained in, obtained solution D seals obtained solution C respectively
And solution D, stir 30 minutes, then solution C and solution D are mixed, stir 30 minutes prepared mixed solutions.
(3) mixed solution obtained in step (2) is poured into reactor and is sealed, in transfer reaction kettle to microwave reaction instrument,
Setting microwave power is 200W, heating rate is 5 DEG C/min, is warming up to 180 DEG C and reacts 6 hours, and reaction is cooled to room after terminating
Temperature obtains suspension.
(4) by suspension obtained in step (3) respectively with deionized water and absolute ethyl alcohol centrifuge washing 5 times, centrifuge
Rotating speed is 4000 revs/min, and centrifugation time is 10 minutes, and it is small in drying 8 at 80 DEG C in vacuum drying chamber that gained is centrifuged product
When, it is cooled to room temperature and single dispersing class flower ball-shaped MoS is obtained2Powder.
Embodiment 2：
(1) by Mo:S elemental mole ratios are 1:1.2 weigh 1.235g ammonium heptamolybdates and 0.655g vulcanized sodium, and ammonium heptamolybdate is dissolved in
20mL deionized water obtained solution A, are dissolved in vulcanized sodium 46.6 mL diethylene glycol (DEG)s and obtain solution B.
(2) its pH value is adjusted for 12, obtained solution C to dropwise addition sodium hydroxide solution in solution A obtained in step (1), to
It is added dropwise the n-butylamine solution that 5mL concentration is 95% in solution B obtained in step (1), obtained solution D seals obtained molten respectively
Liquid C and solution D, stir 120 minutes, then mix solution C and solution D, stir 120 minutes prepared mixed solutions.
(3) mixed solution obtained in step (2) is poured into reactor and is sealed, in transfer reaction kettle to microwave reaction instrument,
Setting microwave power is 500W, heating rate is 20 DEG C/min, is warming up to 200 DEG C and reacts 1 hour, and reaction is cooled to after terminating
Room temperature obtains suspension.
(4) by suspension obtained in step (3) respectively with deionized water and absolute ethyl alcohol centrifuge washing 6 times, centrifuge
Rotating speed is 10000 revs/min, and centrifugation time is 5 minutes, and it is small in drying 48 at 80 DEG C in vacuum drying chamber that gained is centrifuged product
When, it is cooled to room temperature and single dispersing class flower ball-shaped MoS is obtained2Powder.
Embodiment 3：
(1) by Mo:S elemental mole ratios are 1:1.1 weigh 0.628g ammonium tetramolybdates and 0.331g thioacetamides, by ammonium tetramolybdate
25mL deionized water obtained solution A are dissolved in, thioacetamide is dissolved in 25mL glycerine obtained solutions B.
(2) its pH value is adjusted for 10, obtained solution C to dropwise addition potassium hydroxide solution in solution A obtained in step (1), to
It is added dropwise the triethylamine solution that 2.5mL concentration is 95% in solution B obtained in step (1), obtained solution D seals obtained respectively
Solution C and solution D, stir 60 minutes, then mix solution C and solution D, stir 60 minutes prepared mixed solutions.
(3) mixed solution obtained in step (2) is poured into reactor and is sealed, in transfer reaction kettle to microwave reaction instrument,
Setting microwave power is 400W, heating rate is 10 DEG C/min, is warming up to 190 DEG C and reacts 4 hours, and reaction is cooled to after terminating
Room temperature obtains suspension.
(4) by suspension obtained in step (3) respectively with deionized water and absolute ethyl alcohol centrifuge washing 6 times, centrifuge
Rotating speed is 5000 revs/min, and centrifugation time is 7 minutes, and it is small in drying 12 at 80 DEG C in vacuum drying chamber that gained is centrifuged product
When, it is cooled to room temperature and single dispersing class flower ball-shaped MoS is obtained2Powder.
Embodiment 4：
(1) by Mo:S elemental mole ratios are 1:1 weighs 0.340g ammonium dimolybdates and 0.152g thiocarbamides, and ammonium dimolybdate is dissolved in into 20mL
Deionized water obtained solution A, 30mL ethylene glycol obtained solutions B is dissolved in by thiocarbamide.
(2) its pH value is adjusted for 10, obtained solution C to dropwise addition sodium hydroxide solution in solution A obtained in step (1), to
It is added dropwise the ethylenediamine solution that 1mL concentration is 95% in solution B obtained in step (1), obtained solution D seals obtained molten respectively
Liquid C and solution D, stir 60 minutes, then mix solution C and solution D, stir 60 minutes prepared mixed solutions.
(3) mixed solution obtained in step (2) is poured into reactor and is sealed, in transfer reaction kettle to microwave reaction instrument,
Setting microwave power is 300 W, heating rate is 8 DEG C/min, is warming up to 200 DEG C and reacts 4 hours, and reaction is cooled to after terminating
Room temperature obtains suspension.
(4) by suspension obtained in step (3) respectively with deionized water and absolute ethyl alcohol centrifuge washing 6 times, centrifuge
Rotating speed is 7000 revs/min, and centrifugation time is 8 minutes, and it is small in drying 36 at 80 DEG C in vacuum drying chamber that gained is centrifuged product
When, it is cooled to room temperature and single dispersing class flower ball-shaped MoS is obtained2Powder.
Embodiment 5：
(1) by Mo:S elemental mole ratios are 1:1.2 weigh 0.968 g sodium molybdates and 0.365 g thiocarbamides, and sodium molybdate is dissolved in into 40mL
Deionized water obtained solution A, 60mL ethylene glycol obtained solutions B is dissolved in by thiocarbamide.
(2) it is 10, obtained solution C, to step to ammonia spirit is added dropwise in solution A obtained in step (1) to adjust its pH value
(1) the n-butylamine solution that 1mL concentration is 95% is added dropwise in solution B obtained in, obtained solution D seals obtained solution C respectively
And solution D, stir 90 minutes, then solution C and solution D are mixed, stir 90 minutes prepared mixed solutions.
(3) mixed solution obtained in step (2) is poured into reactor and is sealed, in transfer reaction kettle to microwave reaction instrument,
Setting microwave power is 400 W, heating rate is 7 DEG C/min, is warming up to 190 DEG C and reacts 5 hours, and reaction is cooled to after terminating
Room temperature obtains suspension.
(4) by suspension obtained in step (3) respectively with deionized water and absolute ethyl alcohol centrifuge washing 6 times, centrifuge
Rotating speed is 4500 revs/min, and centrifugation time is 6 minutes, and it is small in drying 24 at 80 DEG C in vacuum drying chamber that gained is centrifuged product
When, it is cooled to room temperature and single dispersing class flower ball-shaped MoS is obtained2Powder.
Claims (1)
1. a kind of single dispersing class flower ball-shaped MoS2Raw powder's production technology, it is characterised in that concretely comprise the following steps：
(1) by Mo:S elemental mole ratios are 1:1 ~ 1.2 weighs molybdenum source and sulphur source, and molybdenum source is dissolved in into deionized water obtained solution A, will
Sulphur source is dissolved in alcohol obtained solution B, and the volume ratio of deionized water and alcohol is 1:0.43~2.33；
(2) it is 9 ~ 12, obtained solution C to alkaline solution is added dropwise in solution A obtained in step (1) to adjust its pH value, to step (1)
It is added dropwise the amine solution that 1 ~ 5mL concentration is 95% in obtained solution B, obtained solution D seals obtained solution C and molten respectively
Liquid D, stirs 30 ~ 120 minutes, then mixes solution C and solution D, stirs 30 ~ 120 minutes prepared mixed solutions；
(3) mixed solution obtained in step (2) is poured into reactor and is sealed, in transfer reaction kettle to microwave reaction instrument, set
Microwave power is 200 ~ 500 W, heating rate is 5 ~ 20 DEG C/min, is warming up to 180 ~ 200 DEG C and reacts 1 ~ 6 hour, and reaction terminates
After be cooled to room temperature and obtain suspension；
(4) by suspension obtained in step (3) respectively with deionized water and absolute ethyl alcohol centrifuge washing 5 ~ 6 times, centrifuge turns
Speed is 4000 ~ 10000 revs/min, and centrifugation time is 5 ~ 10 minutes, and gained is centrifuged product in vacuum drying chamber at 80 DEG C
Dry 8 ~ 48 hours, be cooled to room temperature and single dispersing class flower ball-shaped MoS is obtained2Powder；
The molybdenum source is the one kind in ammonium heptamolybdate, ammonium tetramolybdate, ammonium dimolybdate, ammonium molybdate and sodium molybdate；
The sulphur source is the one kind in thiocarbamide, vulcanized sodium and thioacetamide；
The alcohol is the one kind in ethylene glycol, diethylene glycol (DEG) and glycerine；
The alkaline solution is the one kind in ammoniacal liquor, sodium hydroxide solution and potassium hydroxide solution；
Amine in the amine solution is the one kind in ethylenediamine, n-butylamine and triethylamine.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107579248A (en) * | 2017-08-23 | 2018-01-12 | 江汉大学 | The preparation method and applications of negative electrode of lithium ion battery molybdenum disulfide |
| CN108358245A (en) * | 2018-05-16 | 2018-08-03 | 重庆文理学院 | A kind of rose shape MoS2The preparation method of nano flower |
| CN109081377A (en) * | 2018-10-19 | 2018-12-25 | 岭南师范学院 | A kind of three-dimensional molybdenum disulfide bouquet array and its preparation method and application |
| CN111320207A (en) * | 2018-12-14 | 2020-06-23 | 中国科学院大连化学物理研究所 | Preparation and application of molybdenum sulfide material |
| CN112002884A (en) * | 2020-08-27 | 2020-11-27 | 扬州大学 | Flower ball shaped MoSe1.48S0.52@ C positive electrode composite material and aluminum ion battery |
| CN114671472A (en) * | 2022-04-02 | 2022-06-28 | 成都大学 | Preparation method of nickel sulfide nanoparticles for preparing formic acid through electrocatalysis |
| CN115744990A (en) * | 2022-11-24 | 2023-03-07 | 南昌大学 | Method for thermally synthesizing multi-morphology nano molybdenum disulfide lubricant additive by water/solvent |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107579248A (en) * | 2017-08-23 | 2018-01-12 | 江汉大学 | The preparation method and applications of negative electrode of lithium ion battery molybdenum disulfide |
| CN108358245A (en) * | 2018-05-16 | 2018-08-03 | 重庆文理学院 | A kind of rose shape MoS2The preparation method of nano flower |
| CN109081377A (en) * | 2018-10-19 | 2018-12-25 | 岭南师范学院 | A kind of three-dimensional molybdenum disulfide bouquet array and its preparation method and application |
| CN111320207A (en) * | 2018-12-14 | 2020-06-23 | 中国科学院大连化学物理研究所 | Preparation and application of molybdenum sulfide material |
| CN112002884A (en) * | 2020-08-27 | 2020-11-27 | 扬州大学 | Flower ball shaped MoSe1.48S0.52@ C positive electrode composite material and aluminum ion battery |
| CN114671472A (en) * | 2022-04-02 | 2022-06-28 | 成都大学 | Preparation method of nickel sulfide nanoparticles for preparing formic acid through electrocatalysis |
| CN114671472B (en) * | 2022-04-02 | 2024-03-01 | 成都大学 | Preparation method of nickel sulfide nano particles for preparing formic acid by electrocatalytic reaction |
| CN115744990A (en) * | 2022-11-24 | 2023-03-07 | 南昌大学 | Method for thermally synthesizing multi-morphology nano molybdenum disulfide lubricant additive by water/solvent |
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