CN108807878A - A method of preparing molybdenum disulfide/vulcanization tin composite material of hollow structure - Google Patents
A method of preparing molybdenum disulfide/vulcanization tin composite material of hollow structure Download PDFInfo
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- CN108807878A CN108807878A CN201810426340.9A CN201810426340A CN108807878A CN 108807878 A CN108807878 A CN 108807878A CN 201810426340 A CN201810426340 A CN 201810426340A CN 108807878 A CN108807878 A CN 108807878A
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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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- 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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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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Abstract
The present invention relates to a kind of methods of the molybdenum disulfide preparing hollow structure/vulcanization tin composite material, water and ethyl alcohol is added to disperse sodium molybdate, sodium stannate, thioacetamide and silica template, ultrasonic mixing is uniform, it is put into and obtains the molybdenum disulfide vulcanization tin composite material containing template after carrying out hydro-thermal reaction in ptfe autoclave, finally pass through hf etching and remove template, obtains molybdenum disulfide/vulcanization tin composite material of hollow structure.The molybdenum disulfide of hollow structure prepared by the present invention/vulcanization tin composite material has preferable reactivity, there is synergistic effect in electrode reaction, it pretends and is applied to greatly improve its high rate performance and cyclical stability in lithium ion battery and sodium-ion battery for electrode material, there are the potentiality as a kind of excellent energy storage material and be widely used in lithium ion and sodium-ion battery.
Description
Technical field
The present invention relates to a kind of preparation methods of energy storage device material, more particularly, to a kind of two sulphur preparing hollow structure
Change the method for molybdenum/vulcanization tin composite material.
Background technology
With the development of the times, the continuous growth of world population, demand of the mankind to the energy is growing day by day, however the energy is withered
It exhausts, environmental problem etc. increasingly threatens the safety and social progress of the mankind.Explore environmentally friendly, sustainable, efficient new energy
It is most one of the reliable approach for fundamentally solving these problems.However, new energy further use and popularization have to by
Electricity generation system and energy-storage system are effectively combined, therefore further development energy storage technology becomes very urgent and important.Change
It learns power supply and mutually converting between electric energy and chemical energy may be implemented, can be obtained to enable source more reasonable and easily use.
Lithium ion battery [3] has many advantages, such as such as：Operating voltage is high, energy density is high, self-discharge rate is low and has extended cycle life, pacifies
Full performance is good and memory-less effect etc., this makes it as the hot spot studied extensively.However, the continuous increasing consumed with lithium battery
Add and lithium resource scarcity and be unevenly distributed so that many researchers transfer further develop such as sodium ion, magnesium ion, potassium from
A series of ion batteries similar to lithium ion battery such as son, it is intended to lithium is replaced with more cheap and rich reserves metal, with
Further alleviate resource and the scarcity of the energy.Molybdenum disulfide has class as a kind of typical transition metal binary compound
The layer structure of graphene, interlamellar spacing, which is 0.65nm, can facilitate lithium ion and other similar ion insertions, can answer
For electrochemical energy storage.Although molybdenum disulfide has many advantages, various problems are also faced in practical applications.For its
Application in terms of energy storage, molybdenum disulfide is during discharge and recharge reaction, due to the insertion of lithium ion and other metalloid ions
And abjection, its volume expansion, and then dusting, original nanostructure can be caused to cave in, cause to stack, cause its active site and
The reduction of specific surface area prevents it from fully increasing with electrolyte contacts, electron-transport path, is unfavorable for the reversible of electrode reaction
Property.
Invention content
The purpose of the present invention be exactly in order to overcome above-mentioned molybdenum disulfide material short slab present in electrode process and
A kind of method of the molybdenum disulfide preparing hollow structure/vulcanization tin composite material is provided, makes it in lithium ion battery and sodium ion
Multiplying power and cycle performance in the application of battery are highly improved.
The purpose of the present invention can be achieved through the following technical solutions：
A method of the molybdenum disulfide/vulcanization tin composite material preparing hollow structure, using following steps：
(1) water and ethyl alcohol is added to be uniformly dispersed sodium molybdate, sodium stannate, thioacetamide and silica template；
(2) ultrasound and stirring are carried out to the mixed solution that step (1) obtains；
(3) mixed liquor after stirring is transferred in reaction kettle and is heated；
(4) the product centrifuge washing obtained by step (3) is dried；
(5) sample that step (4) obtains is placed in tube furnace and is annealed；
(6) molybdenum disulfide/artificial gold of hollow structure is prepared in the powder hf etching for obtaining step (5)
Composite material.
Sodium molybdate described in step (1), sodium stannate, thioacetamide and silica template mass ratio be 0.04-
0.15:0.02-0.1:0.2:The addition of 0.05-0.2, the water and ethyl alcohol is 10-50ml/0.04-0.15g sodium molybdates.
Ultrasonic frequency is 80 hertz, ultrasonic time 5-30min, mixing time 10-30min in step (2).
Step is heated in (3) by hydro-thermal reaction, reaction solution is transferred in autoclave, heating and temperature control
At 150-250 DEG C, time control is in 8-24h.
Step (4) adopts water as solvent when centrifuging, control rotating speed is 5000-10000rpm, and the time is 3-10 minutes, dry
Temperature be 40-80 DEG C, time 1-2d.
Step (5) is annealed under an inert atmosphere, and control heating rate is 5-10 DEG C/min, and annealing temperature is 400-800 DEG C,
Time is 200-600min.
The volumetric concentration of hydrofluoric acid in step (6) is controlled in 5-30%, and the time control of etching is in 1-10h.
Sodium molybdate in above-mentioned technological parameter, sodium stannate, thioacetamide and silica template mass ratio to finally producing
Physical performance has decisive influence.If the amount that silica template is added can cause to coat uneven, silica bulb too much
It is point exposed, chondritic cannot be formed, eventually leads in electrode process that the mechanical property of material is poor, material caves in,
Cycle performance and high rate performance are poor.If the amount that silica template is added can lead to oneself of molybdenum disulfide and artificial gold very little
Body aggregation stacks, and is reduced so as to cause exposed active site, reactivity reduces, and reduces the specific capacity of material.
The molybdenum disulfide for the hollow structure being prepared/vulcanization tin composite material is molybdenum disulfide and artificial gold In-situ reaction
The hollow spheres structure that assembles of ultrathin nanometer piece.
Compared with prior art, molybdenum disulfide/artificial gold composite wood of the hollow structure for the method synthesis that the present invention uses
Expect it is larger improve its multiplying power and cycle performance in lithium ion battery and sodium-ion battery, and preparation method is simple, material
The stability of material is preferable.During prepared product assembles for the ultrathin nanometer piece of molybdenum disulfide and artificial gold In-situ reaction
Empty chondritic.On the one hand, hollow structure can alleviate volume expansion, reduce destruction of the stress to electrode material, while can be with
It realizes structure nano, reduces the stacking phenomenon of molybdenum disulfide during the reaction, increase specific surface area, realize the efficient of ion
Transmission is conducive to the multiplying power and specific capacity that improve battery.On the other hand, composite construction by two kinds of materials by being uniformly compounded in one
It rises, can prevent in electrode process, little particle is gradually fused into bulky grain, causes to reunite.In prepared by this method
The molybdenum disulfide of hollow structure/vulcanization tin composite material can be used in lithium ion battery and sodium-ion battery, and improve the material
Multiplying power and cycle performance, have the potentiality as a kind of excellent electrode material and be widely used in energy storage device.
Description of the drawings
Fig. 1 is the scanning electron microscope of molybdenum disulfide/vulcanization tin composite material of hollow structure prepared by embodiment 1-4
Photo.
Fig. 2 is that the transmission electron microscope of molybdenum disulfide/vulcanization tin composite material of hollow structure prepared by embodiment 1 shines
Piece.
Fig. 3 is the lithium ion battery of molybdenum disulfide/vulcanization tin composite material assembling of hollow structure prepared by embodiment 1
High rate performance figure.
Fig. 4 is the lithium ion battery of molybdenum disulfide/vulcanization tin composite material assembling of hollow structure prepared by embodiment 1
Cycle performance figure.
Fig. 5 is the sodium-ion battery of molybdenum disulfide/vulcanization tin composite material assembling of hollow structure prepared by embodiment 1
Cycle performance figure.
Specific implementation mode
With reference to specific embodiment, the present invention is described in detail.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
Embodiment 1
100mL is added in 0.06g sodium molybdates, 0.07g sodium stannates, 0.2g thioacetamides and 0.07g silica templates
In beaker, water and ethyl alcohol 40mL (20 is added:20/v:V), it is uniformly dispersed.Mixed solution is subjected to ultrasound 10min, stirring
30min.Mixed liquor after stirring is transferred in ptfe autoclave, is heated to 250 DEG C, reacts 18h.Products therefrom is used
Deionized water is washed, rotating speed 6000rpm/min, and the time is 5 minutes, is then dried, and temperature is 50 DEG C, and the time is
1d.Obtained sample is placed in tube furnace and is annealed, condition is 650 DEG C, continues 5h, 5 DEG C/min of heating rate；The powder that will be obtained
Molybdenum disulfide/vulcanization tin composite material of hollow structure is prepared in end hf etching.Prepared sample such as Figure 1A institutes
Show, under a scanning electron microscope, it is observed that the flexible nano piece of ultra-thin curling uniformly assembles glomeration.Transmitted electron is aobvious
Micro mirror photo is as shown in Fig. 2, in transmission electron microscope, it is observed that the hollow ball of molybdenum disulfide artificial gold composite construction
Pattern.
Embodiment 2
100mL is added in 0.15g sodium molybdates, 0.02g sodium stannates, 0.2g thioacetamides and 0.06g silica templates
In beaker, water and ethyl alcohol 40mL (20 is added:20/v:V), it is uniformly dispersed.Mixed solution is subjected to ultrasound 10min, stirring
30min.Mixed liquor after stirring is transferred in ptfe autoclave, is heated to 250 DEG C, reacts 18h.Products therefrom is used
Deionized water is washed, rotating speed 6000rpm/min, and the time is 5 minutes, is then dried, and temperature is 50 DEG C, and the time is
1d.Obtained sample is placed in tube furnace and is annealed, condition is 650 DEG C, continues 5h, 5 DEG C/min of heating rate；The powder that will be obtained
Molybdenum disulfide/vulcanization tin composite material of hollow structure is prepared in end hf etching.Prepared sample such as Figure 1B institutes
Show.
Embodiment 3
100mL is added in 0.05g sodium molybdates, 0.05g sodium stannates, 0.2g thioacetamides and 0.2g silica templates to burn
In cup, water and ethyl alcohol 40mL (20 is added:20/v:V), it is uniformly dispersed.Mixed solution is subjected to ultrasound 10min, stirs 30min.
Mixed liquor after stirring is transferred in ptfe autoclave, is heated to 250 DEG C, reacts 18h.To products therefrom deionization
Water is washed, rotating speed 6000rpm/min, and the time is 5 minutes, is then dried, and temperature is 50 DEG C, time 1d.Will
To sample be placed in tube furnace and anneal, condition is 650 DEG C, continues 5h, 5 DEG C/min of heating rate；The powder hydrogen that will be obtained
Fluoric acid etches, and molybdenum disulfide/vulcanization tin composite material of hollow structure is prepared.Prepared sample is as shown in Figure 1 C.
Embodiment 4
100mL is added in 0.06g sodium molybdates, 0.04g sodium stannates, 0.2g thioacetamides and 0.09g silica templates
In beaker, water and ethyl alcohol 40mL (20 is added:20/v:V), it is uniformly dispersed.Mixed solution is subjected to ultrasound 10min, stirring
30min.Mixed liquor after stirring is transferred in ptfe autoclave, is heated to 250 DEG C, reacts 18h.Products therefrom is used
Deionized water is washed, rotating speed 6000rpm/min, and the time is 5 minutes, is then dried, and temperature is 50 DEG C, and the time is
1d.Obtained sample is placed in tube furnace and is annealed, condition is 650 DEG C, continues 5h, 5 DEG C/min of heating rate；The powder that will be obtained
Molybdenum disulfide/vulcanization tin composite material of hollow structure is prepared in end hf etching.Prepared sample such as Fig. 1 D institutes
Show.
Molybdenum disulfide/vulcanization tin composite material of the hollow structure of method that the present invention uses synthesis is larger improve its
Multiplying power in lithium ion battery and sodium-ion battery and cycle performance, and preparation method is simple, and the stability of material is preferable.Such as
Shown in Fig. 3, being applied to can larger its high rate performance of promotion in lithium ion battery；As shown in figure 4, applied in lithium ion battery
Can larger its cycle performance of promotion, have preferable cycle conservation rate；As shown in figure 5, applied to sodium-ion battery also have compared with
High specific capacity.The material can be used as a kind of excellent energy storage material and be widely used in lithium ion battery and sodium-ion battery.
Embodiment 5
A kind of molybdenum disulfide preparing hollow structure/vulcanization tin composite material, using following steps：
(1) it is 0.04 in mass ratio by sodium molybdate, sodium stannate, thioacetamide and silica template:0.02:0.2:
0.05 is uniformly mixed, and it is 40ml/0.04g sodium molybdates to add the amount of water and ethyl alcohol；
(2) ultrasound 5min and stirring 10min are carried out to the mixed solution that step (1) obtains, supersonic frequency is controlled at 80 hertz
Hereby；
(3) mixed liquor after stirring is transferred in the autoclave of polytetrafluoroethylene (PTFE), is heated to 250 DEG C, continue 18h,
Carry out hydro-thermal reaction；
(4) product obtained by step (3) is centrifuged, rotating speed 6000rpm, deionized water washing, 50 DEG C of dry 1d.
(5) sample that step (4) obtains is placed in tube furnace and is annealed, 650 DEG C of temperature, holding 5h, 5 DEG C of heating rate/
min；
(6) 20% hf etching 3h of the powder for obtaining step (5), be prepared the molybdenum disulfide of hollow structure/
Vulcanize tin composite material.
Embodiment 6
A kind of molybdenum disulfide preparing hollow structure/vulcanization tin composite material, using following steps：
(1) it is 0.04 in mass ratio by sodium molybdate, sodium stannate, thioacetamide and silica template:0.02:0.2:
0.05 is uniformly mixed, and it is 10ml/0.04g sodium molybdates to add the amount of water and ethyl alcohol；
(2) ultrasound 10min and stirring 30min are carried out to the mixed solution that step (1) obtains, supersonic frequency is controlled at 80 hertz
Hereby；
(3) mixed liquor after stirring is transferred in the autoclave of polytetrafluoroethylene (PTFE), is heated to 150 DEG C, continued for 24 hours,
Carry out hydro-thermal reaction；
(4) product obtained by step (3) is centrifuged, rotating speed, 5000rpm, deionized water washing, 40 DEG C of dry 1d.
(5) sample that step (4) obtains is placed in tube furnace and is annealed, control heating rate is 5 DEG C/min, temperature 400
DEG C, keep 5h；
(6) 5% hf etching 10h of the powder for obtaining step (5), be prepared the molybdenum disulfide of hollow structure/
Vulcanize tin composite material.
Embodiment 7
A kind of molybdenum disulfide preparing hollow structure/vulcanization tin composite material, using following steps：
(1) it is 0.15 in mass ratio by sodium molybdate, sodium stannate, thioacetamide and silica template:0.1:0.2:0.2
It is uniformly mixed, it is 50ml/0.15g sodium molybdates to add the amount of water and ethyl alcohol；
(2) ultrasound 30min and stirring 10min are carried out to the mixed solution that step (1) obtains, supersonic frequency is controlled at 80 hertz
Hereby；
(3) mixed liquor after stirring is transferred in the autoclave of polytetrafluoroethylene (PTFE), is heated to 250 DEG C, continue 8h, into
Row hydro-thermal reaction；
(4) product obtained by step (3) is centrifuged, rotating speed 10000rpm, deionized water washing, 80 DEG C of dry 2d.
(5) sample that step (4) obtains is placed in tube furnace and is annealed, 800 DEG C of temperature keeps 200min, heating rate
10℃/min；
(6) 30% hf etching 1h of the powder for obtaining step (5), be prepared the molybdenum disulfide of hollow structure/
Vulcanize tin composite material.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (8)
1. a kind of method of the molybdenum disulfide preparing hollow structure/vulcanization tin composite material, which is characterized in that this method use with
Lower step：
(1) water and ethyl alcohol is added to be uniformly dispersed sodium molybdate, sodium stannate, thioacetamide and silica template；
(2) ultrasound and stirring are carried out to the mixed solution that step (1) obtains；
(3) mixed liquor after stirring is transferred in reaction kettle and is heated；
(4) the product centrifuge washing obtained by step (3) is dried；
(5) sample that step (4) obtains is placed in tube furnace and is annealed；
(6) the powder hf etching for obtaining step (5), molybdenum disulfide/artificial gold that hollow structure is prepared are compound
Material.
2. a kind of method of the molybdenum disulfide preparing hollow structure/vulcanization tin composite material according to claim 1, special
Sign is, sodium molybdate described in step (1), sodium stannate, thioacetamide and silica template mass ratio be 0.04-
0.15:0.02-0.1:0.2:0.05-0.2。
3. a kind of method of the molybdenum disulfide preparing hollow structure/vulcanization tin composite material according to claim 1, special
Sign is that the addition of water and ethyl alcohol described in step (1) is 10-50ml/0.04-0.15g sodium molybdates.
4. a kind of method of the molybdenum disulfide preparing hollow structure/vulcanization tin composite material according to claim 1, special
Sign is that ultrasonic frequency is 80 hertz, ultrasonic time 5-30min, mixing time 10-30min in step (2).
5. a kind of method of the molybdenum disulfide preparing hollow structure/vulcanization tin composite material according to claim 1, special
Sign is that step is heated in (3) by hydro-thermal reaction, reaction solution is transferred in autoclave, heating and temperature control
At 150-250 DEG C, time control is in 8-24h.
6. a kind of method of the molybdenum disulfide preparing hollow structure/vulcanization tin composite material according to claim 1, special
Sign is that step (4) adopts water as solvent when centrifuging, and control rotating speed is 5000-10000rpm, and the time is 3-10 minutes, dry
Temperature be 40-80 DEG C, time 1-2d.
7. a kind of method of the molybdenum disulfide preparing hollow structure/vulcanization tin composite material according to claim 1, special
Sign is that step (5) is annealed under an inert atmosphere, and control heating rate is 5-10 DEG C/min, and annealing temperature is 400-800 DEG C,
Time is 200-600min.
8. a kind of method of the molybdenum disulfide preparing hollow structure/vulcanization tin composite material according to claim 1, special
Sign is that the volumetric concentration of the hydrofluoric acid in step (6) is controlled in 5-30%, and the time control of etching is in 1-10h.
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Cited By (8)
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| CN110233254A (en) * | 2019-07-01 | 2019-09-13 | 郑州大学 | A kind of lithium ion battery negative material shape Fe that rings a bell3O4/C/MoS2Hydridization particle |
| CN110697777A (en) * | 2019-10-09 | 2020-01-17 | 西北工业大学 | Preparation method of tin molybdenum disulfide with hollow structure |
| CN111106346A (en) * | 2019-12-17 | 2020-05-05 | 合肥国轩高科动力能源有限公司 | SnS2rGO modified sulfur cathode material and preparation method and application thereof |
| CN111628155A (en) * | 2020-06-23 | 2020-09-04 | 广西师范大学 | Molybdenum-tin bimetallic sulfide as negative electrode material of lithium ion/sodium ion battery and preparation method thereof |
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| CN114560502A (en) * | 2020-11-27 | 2022-05-31 | 国电南瑞科技股份有限公司 | Three-dimensional nano molybdenum-based lithium ion battery cathode material and preparation method thereof |
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| CN110233254A (en) * | 2019-07-01 | 2019-09-13 | 郑州大学 | A kind of lithium ion battery negative material shape Fe that rings a bell3O4/C/MoS2Hydridization particle |
| CN110233254B (en) * | 2019-07-01 | 2022-05-24 | 郑州大学 | Bell-shaped Fe for lithium ion battery cathode material3O4/C/MoS2Hybrid microparticles |
| CN110697777A (en) * | 2019-10-09 | 2020-01-17 | 西北工业大学 | Preparation method of tin molybdenum disulfide with hollow structure |
| CN111106346A (en) * | 2019-12-17 | 2020-05-05 | 合肥国轩高科动力能源有限公司 | SnS2rGO modified sulfur cathode material and preparation method and application thereof |
| CN111106346B (en) * | 2019-12-17 | 2022-03-11 | 合肥国轩高科动力能源有限公司 | SnS2rGO modified sulfur cathode material and preparation method and application thereof |
| CN111628155A (en) * | 2020-06-23 | 2020-09-04 | 广西师范大学 | Molybdenum-tin bimetallic sulfide as negative electrode material of lithium ion/sodium ion battery and preparation method thereof |
| CN111628155B (en) * | 2020-06-23 | 2022-04-22 | 广西师范大学 | Molybdenum-tin bimetallic sulfide as negative electrode material of lithium ion/sodium ion battery and preparation method thereof |
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| CN112490018A (en) * | 2020-12-09 | 2021-03-12 | 桂林电子科技大学 | Composite material based on silicon dioxide metal sulfide and preparation method and application thereof |
| CN114094076A (en) * | 2021-11-15 | 2022-02-25 | 珠海冠宇电池股份有限公司 | Negative plate and lithium ion battery comprising same |
| CN114094076B (en) * | 2021-11-15 | 2023-10-13 | 珠海冠宇电池股份有限公司 | Negative plate and lithium ion battery comprising same |
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Application publication date: 20181113 |