CN106803589B - A kind of monodisperse class flower ball-shaped MoS2Raw powder's production technology - Google Patents
A kind of monodisperse class flower ball-shaped MoS2Raw powder's production technology Download PDFInfo
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- CN106803589B CN106803589B CN201710105252.4A CN201710105252A CN106803589B CN 106803589 B CN106803589 B CN 106803589B CN 201710105252 A CN201710105252 A CN 201710105252A CN 106803589 B CN106803589 B CN 106803589B
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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 monodisperse class flower ball-shaped MoS2Raw powder's production technology.Molybdate compound and sulfur-containing compound are separately added into different solvents by specified molar ratio, different additives is added dropwise in each solvent, latter two solvent is stirred to be uniformly mixed, then mixed liquor is poured into reaction kettle and is transferred in microwave reaction instrument, specified microwave power, heating rate, reaction temperature and reaction time are set, keep reactant cooling reaction kettle removal heating device after reaction, cooled material obtains monodisperse class flower ball-shaped MoS through centrifuge washing drying2Powder.The method of the present invention step is controllable, required low raw-material cost, and preparation-obtained powder realizes monodisperse, 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, in particular to a kind of monodisperse class flower ball-shaped MoS2Raw powder's production technology,
Obtained MoS2Powder can be used for lithium ion battery negative material.
Background technique
Lithium ion battery has become current research due to the features such as small in size, light-weight, energy density is high, memory-less effect
Hot spot.Compared with other energy and materials, lithium ion battery is widely applied in the mobile devices such as mobile phone, automobile.For total
It, the development of lithium ion battery brings huge convenience to our production and daily life.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 safety of battery is premise element.
As the business negative electrode material of lithium ion secondary battery, graphite has lot of advantages, such as operating potential is low, structure
The features such as stablizing, however its capacity is relatively low, about 370 mAhg-1, this disadvantage makes graphite as negative electrode material
Be unable to satisfy the requirement of the following electric car, it is therefore desirable to find energy density, power density it is higher and have security and stability
Negative electrode material.
MoS2Possess unique class graphene layer structure, unique crystal structure and higher theoretical capacity make it
Wide application prospect has been shown in clean energy resource field.But numerous results of study shows MoS2Negative electrode material is being filled
Due to lithiated product Li in discharge process2S and electrolysis qualitative response formed thick gelatinous polymer layer inhibit continuous embedding lithium/
De- lithium reaction, to make it 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. people prepares high-sequential by the vacuum assisted process improved
MoS2, good cyclical stability is shown in negative electrode material；Ding et al. is auxiliary by mild polystyrene microsphere
The method for helping hydro-thermal prepares 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 process of preparation process, and currently report
MoS2Preparation method can not be easy to get monodispersed MoS again2Particle, and then constrain MoS2In negative electrode of lithium ion battery material
Application in material.
Summary of the invention
In view of above-mentioned MoS2The technology of preparing defect of powder, the object of the present invention is to provide a kind of inexpensive, high quality
Monodisperse 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 of a large amount of nano-sheet powder, and the specific surface area of powder has been significantly greatly increased, and promotes MoS2Cathode material
Expect the cyclical stability in lithium ion battery.
Method of the invention is to be added uniformly mixed reactant precursor solution using microwave-assisted hydro-thermal/solvent-thermal method
Enter microwave reaction kettle, controls reaction temperature and the MoS of class flower ball-shaped structure can be obtained in the reaction time2Powder granule.
Specific steps are as follows:
(1) it is that 1:1 ~ 1.2 weigh molybdenum source and sulphur source by Mo:S elemental mole ratios, molybdenum source is dissolved in deionized water obtained solution
Sulphur source is dissolved in alcohol obtained solution B by A, and the volume ratio of deionized water and alcohol is 1:0.43 ~ 2.33.
(2) it is 9 ~ 12 that alkaline solution is added dropwise into solution A made from step (1) and adjusts its pH value, obtained solution C, Xiang Bu
Suddenly the amine solution that 1 ~ 5mL concentration is 95% is added dropwise in solution B made from (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 obtained mixed solutions.
(3) mixed solution made from step (2) is poured into reaction kettle and is sealed, transfer reaction kettle into 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
After be cooled to room temperature to obtain suspension.
(4) suspension made from step (3) is used into deionized water and dehydrated alcohol centrifuge washing 5 ~ 6 times, centrifuge respectively
Revolving speed be 4000 ~ 10000 revs/min, centrifugation time be 5 ~ 10 minutes, gained be centrifuged product in vacuum oven in 80
It is 8 ~ 48 hours dry at DEG C, it is cooled to room temperature and obtains monodisperse class flower ball-shaped MoS2Powder.
The molybdenum source is one of ammonium heptamolybdate, ammonium tetramolybdate, ammonium dimolybdate, ammonium molybdate and sodium molybdate.
The sulphur source is one of thiocarbamide, vulcanized sodium and thioacetamide.
The alcohol is one of ethylene glycol, diethylene glycol (DEG) and glycerine.
The alkaline solution is one of ammonium hydroxide, sodium hydroxide solution and potassium hydroxide solution.
Amine in the amine solution is one of ethylenediamine, n-butylamine and triethylamine.
The method of the present invention step is controllable, required low raw-material cost, and preparation-obtained powder realizes that monodisperse, particle are big
Small uniformly 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.
Detailed description of the invention
Fig. 1 is monodisperse class flower ball-shaped MoS made from the embodiment of the present invention 12The X ray diffracting spectrum of powder.
Fig. 2 is monodisperse class flower ball-shaped MoS made from the embodiment of the present invention 12The field emission scanning electron microscope of powder
Figure.
Specific embodiment
Embodiment 1:
(1) it is that 1:1 weighs 0.196g ammonium molybdate and 0.076g thiocarbamide by Mo:S elemental mole ratios, ammonium molybdate is dissolved in 50mL
Thiocarbamide is dissolved in 21.5mL ethylene glycol obtained solution B by deionized water obtained solution A.
(2) it is 9, obtained solution C that ammonia spirit is added dropwise into solution A made from step (1) and adjusts its pH value, to step
(1) ethylenediamine solution that 1mL concentration is 95% is added dropwise in solution B made from, obtained solution D seals obtained solution C respectively
And solution D, it stirs 30 minutes, then mixes solution C and solution D, stir 30 minutes obtained mixed solutions.
(3) mixed solution made from step (2) is poured into reaction kettle and is sealed, transfer reaction kettle into 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, is cooled to room after reaction
Temperature obtains suspension.
(4) suspension made from step (3) is used into deionized water and dehydrated alcohol centrifuge washing 5 times respectively, centrifuge
Revolving speed is 4000 revs/min, and centrifugation time is 10 minutes, and gained is centrifuged product, and drying 8 is small at 80 DEG C in vacuum oven
When, it is cooled to room temperature and obtains monodisperse class flower ball-shaped MoS2Powder.
Embodiment 2:
It (1) is that 1:1.2 weighs 1.235g ammonium heptamolybdate and 0.655g vulcanized sodium by Mo:S elemental mole ratios, by ammonium heptamolybdate
It is dissolved in 20mL deionized water obtained solution A, vulcanized sodium is dissolved in 46.6 mL diethylene glycol (DEG)s and obtains solution B.
(2) into solution A made from step (1) be added dropwise sodium hydroxide solution adjust its pH value be 12, obtained solution C, to
It is added dropwise the n-butylamine solution that 5mL concentration is 95% in solution B made from step (1), obtained solution D is sealed obtained molten respectively
Liquid C and solution D stir 120 minutes, then mix solution C and solution D, stir 120 minutes obtained mixed solutions.
(3) mixed solution made from step (2) is poured into reaction kettle and is sealed, transfer reaction kettle into 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, is cooled to after reaction
Room temperature obtains suspension.
(4) suspension made from step (3) is used into deionized water and dehydrated alcohol centrifuge washing 6 times respectively, centrifuge
Revolving speed is 10000 revs/min, and centrifugation time is 5 minutes, and gained is centrifuged product, and drying 48 is small at 80 DEG C in vacuum oven
When, it is cooled to room temperature and obtains monodisperse class flower ball-shaped MoS2Powder.
Embodiment 3:
It (1) is that 1:1.1 weighs 0.628g ammonium tetramolybdate and 0.331g thioacetamide by Mo:S elemental mole ratios, by four molybdenums
Sour ammonium is dissolved in 25mL deionized water obtained solution A, and thioacetamide is dissolved in 25mL glycerine obtained solution B.
(2) into solution A made from step (1) be added dropwise potassium hydroxide solution adjust its pH value be 10, obtained solution C, to
The triethylamine solution that dropwise addition 2.5mL concentration is 95% in solution B made from step (1), obtained solution D, respectively obtained by sealing
Solution C and solution D stir 60 minutes, then mix solution C and solution D, stir 60 minutes obtained mixed solutions.
(3) mixed solution made from step (2) is poured into reaction kettle and is sealed, transfer reaction kettle into 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, is cooled to after reaction
Room temperature obtains suspension.
(4) suspension made from step (3) is used into deionized water and dehydrated alcohol centrifuge washing 6 times respectively, centrifuge
Revolving speed is 5000 revs/min, and centrifugation time is 7 minutes, and gained is centrifuged product, and drying 12 is small at 80 DEG C in vacuum oven
When, it is cooled to room temperature and obtains monodisperse class flower ball-shaped MoS2Powder.
Embodiment 4:
(1) it is that 1:1 weighs 0.340g ammonium dimolybdate and 0.152g thiocarbamide by Mo:S elemental mole ratios, ammonium dimolybdate is dissolved in
Thiocarbamide is dissolved in 30mL ethylene glycol obtained solution B by 20mL deionized water obtained solution A.
(2) into solution A made from step (1) be added dropwise sodium hydroxide solution adjust its pH value be 10, obtained solution C, to
It is added dropwise the ethylenediamine solution that 1mL concentration is 95% in solution B made from step (1), obtained solution D is sealed obtained molten respectively
Liquid C and solution D stir 60 minutes, then mix solution C and solution D, stir 60 minutes obtained mixed solutions.
(3) mixed solution made from step (2) is poured into reaction kettle and is sealed, transfer reaction kettle into 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, is cooled to after reaction
Room temperature obtains suspension.
(4) suspension made from step (3) is used into deionized water and dehydrated alcohol centrifuge washing 6 times respectively, centrifuge
Revolving speed is 7000 revs/min, and centrifugation time is 8 minutes, and gained is centrifuged product, and drying 36 is small at 80 DEG C in vacuum oven
When, it is cooled to room temperature and obtains monodisperse class flower ball-shaped MoS2Powder.
Embodiment 5:
(1) it is that 1:1.2 weighs 0.968 g sodium molybdate and 0.365 g thiocarbamide by Mo:S elemental mole ratios, sodium molybdate is dissolved in
Thiocarbamide is dissolved in 60mL ethylene glycol obtained solution B by 40mL deionized water obtained solution A.
(2) it is 10, obtained solution C that ammonia spirit is added dropwise into solution A made from step (1) and adjusts its pH value, to step
(1) the n-butylamine solution that 1mL concentration is 95% is added dropwise in solution B made from, obtained solution D seals obtained solution C respectively
And solution D, it stirs 90 minutes, then mixes solution C and solution D, stir 90 minutes obtained mixed solutions.
(3) mixed solution made from step (2) is poured into reaction kettle and is sealed, transfer reaction kettle into 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, is cooled to after reaction
Room temperature obtains suspension.
(4) suspension made from step (3) is used into deionized water and dehydrated alcohol centrifuge washing 6 times respectively, centrifuge
Revolving speed is 4500 revs/min, and centrifugation time is 6 minutes, and gained is centrifuged product, and drying 24 is small at 80 DEG C in vacuum oven
When, it is cooled to room temperature and obtains monodisperse class flower ball-shaped MoS2Powder.
Claims (1)
1. a kind of monodisperse class flower ball-shaped MoS2Raw powder's production technology, it is characterised in that specific steps are as follows:
(1) it is that 1:1 ~ 1.2 weigh molybdenum source and sulphur source by Mo:S elemental mole ratios, molybdenum source is dissolved in deionized water obtained solution A, it 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 that alkaline solution is added dropwise into solution A made from step (1) and adjusts its pH value, to step (1)
It is added dropwise the amine solution that 1 ~ 5mL concentration is 95% in solution B obtained, 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 obtained mixed solutions；
(3) mixed solution made from step (2) is poured into reaction kettle and is sealed, transfer reaction kettle is into 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 terminates
After be cooled to room temperature to obtain suspension；
(4) suspension made from step (3) is used into deionized water and dehydrated alcohol centrifuge washing 5 ~ 6 times respectively, centrifuge turns
Speed is 4000 ~ 10000 revs/min, and centrifugation time is 5 ~ 10 minutes, and gained centrifugation product is in vacuum oven at 80 DEG C
It is 8 ~ 48 hours dry, it is cooled to room temperature and obtains monodisperse class flower ball-shaped MoS2Powder；
The molybdenum source is one of ammonium heptamolybdate, ammonium tetramolybdate, ammonium dimolybdate, ammonium molybdate and sodium molybdate；
The sulphur source is one of thiocarbamide, vulcanized sodium and thioacetamide；
The alcohol is one of ethylene glycol, diethylene glycol (DEG) and glycerine；
The alkaline solution is one of ammonium hydroxide, sodium hydroxide solution and potassium hydroxide solution；
Amine in the amine solution is one of ethylenediamine, n-butylamine and triethylamine.
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| 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 |
| CN109081377B (en) * | 2018-10-19 | 2020-07-28 | 岭南师范学院 | Three-dimensional molybdenum disulfide flower ball array and preparation method and application thereof |
| CN111320207B (en) * | 2018-12-14 | 2021-09-24 | 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 |
| 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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