CN104183834A - Preparation method of sulphur/silicon dioxide core-shell nanostructure for lithium sulphur battery anode - Google Patents
Preparation method of sulphur/silicon dioxide core-shell nanostructure for lithium sulphur battery anode Download PDFInfo
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- CN104183834A CN104183834A CN201410399926.2A CN201410399926A CN104183834A CN 104183834 A CN104183834 A CN 104183834A CN 201410399926 A CN201410399926 A CN 201410399926A CN 104183834 A CN104183834 A CN 104183834A
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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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- 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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- 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
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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 relates to a preparation method of a sulphur/silicon dioxide core-shell nanostructure for a lithium sulphur battery anode. The preparation method comprises the following steps: dispersing a surface active agent in sulfuric acid solution, dropwise adding sodium thiosulfate aqueous solution, stirring for 0.5-24h, washing products, and drying to obtain sulphur particles; and dispersing the sulphur particles and the surface active agent in ethanol solution, sequentially adding water, ammonia water and tetraethoxysilane solution, reacting for 0.5-12h at room temperature, washing products and drying to obtain the sulphur/silicon dioxide core-shell nanostructure. According to the preparation method, the sulphur particle is used as a template, nano-porous silicon dioxide is clad by a hydrolytic polycondensation process of tetraethoxysilane, the loss of the active substance in an electrode process can be effectively inhibited, and the cycling stability and the rate capability of the electrode are improved under the immobilization and catalytic action of the nano-porous silicon dioxide on the sulphur active substance, therefore, the high-performance composite anode material is obtained.
Description
Technical field
The present invention relates to the preparation method of sulphur positive electrode for a kind of lithium-sulfur cell, particularly relate to a kind of preparation method of sulphur/silica core-shell nanostructure for lithium-sulphur cell positive electrode.
Background technology
Day by day commercial lithium rechargeable battery is limited to theoretical capacity, cannot further significantly improve its energy density, and fuel cell is yet more difficult practical at short notice, and the technology of grasping at present far can not meet the demand of development.Therefore, need in a hurry research and development to there is high-energy-density more, the mechanism of new electrochemical power sources of the feature such as long circulation life, low cost and environmental friendliness more.
Take lithium metal as negative pole, elemental sulfur be the lithium-sulfur rechargeable battery (abbreviation lithium-sulfur cell) of positive active material because its theoretical capacity is high, raw material source is wide, cheap and environmentally friendly etc., and advantage has been subject to paying close attention to widely, is considered to the candidate of the tool potentiality of energy storage system of future generation.But, the dissolving of this polysulfide producing in discharge process of sulfur electrode and the effect of shuttling back and forth causing thus, active material utilization reduction, electrode cyclical stability and the poor problem of high-rate charge-discharge capability have directly been caused, can't meet at present the requirement of traffic and stored energy power battery, restrict the practical application of lithium-sulfur cell.
In the last few years, people mainly improved the performance of sulfur electrode by building sulfenyl composite material, and the complex carrier of employing is as amorphous carbon, carbon nano-tube and conducting polymer etc.Compare with these carbon-based supports, nanoporous oxide, if silicon dioxide, titanium dioxide and alundum (Al2O3) are as the fixing sulphur active material of carrier, can also play catalytic action to electrode process, thereby can more effectively suppress the loss of active material in electrode process, cyclical stability and the high rate performance of raising electrode, obtain high-performance composite sulfur positive electrode.In these oxide carriers, silicon dioxide because of its prepare easy, cost is low and advantages of environment protection receives much concern.Yet, existing silicon dioxide addition manner is difficult to realize it and mixes with the even of active material sulphur, nano-stephanoporate silicon dioxide load or coated sulphur, particularly the preparation of sulphur/silica core-shell nanostructure still faces very large challenge, and this has limited by nano-stephanoporate silicon dioxide modification and has obtained high-performance composite sulfur positive electrode.
The present invention is intended to seek a kind of method of preparing sulphur/silica core-shell nanostructure.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of sulphur/silica core-shell nanostructure for lithium-sulphur cell positive electrode.
A preparation method for sulphur for lithium-sulphur cell positive electrode/silica core-shell nanostructure, comprises the following steps:
(1) preparation of sulfur granules: surfactant-dispersed, in sulfuric acid solution, is dripped to the aqueous solution of sodium thiosulfate, stir 0.5 ~ 24 hour, product is washed and is dried, obtain sulfur granules product;
(2) preparation of sulphur/silica core-shell nanostructure: the sulfur granules that step (1) is obtained is distributed in ethanolic solution together with surfactant, add successively subsequently water, ammoniacal liquor and teos solution, room temperature reaction 0.5 ~ 12 hour, product is washed and is dried, obtain described sulphur/silica core-shell nanostructure.
In step (1), described surfactant is one or more in polyvinylpyrrolidone, softex kw, diallyl dimethyl ammoniumchloride, kayexalate; The mass concentration of described surfactant is 1 ~ 100 grams per liter; The concentration of described sulfuric acid solution is 0.1 ~ 100 mM/l; Described sodium thiosulfate and H
2sO
4mol ratio be 1 ~ 100:1.
In step (2), the concentration of described sulfur granules in ethanolic solution is 0.01 ~ 10 grams per liter; Described surfactant is one or more in polyvinylpyrrolidone, softex kw, diallyl dimethyl ammoniumchloride, kayexalate; The mass concentration of described surfactant is 0.1 ~ 10 grams per liter;
In the present invention, NH in described ammoniacal liquor
3quality percentage composition be 25 ~ 28%, SiO in described teos solution
2quality percentage composition higher than 28.0%.The volume proportion of described ethanolic solution, water, ammoniacal liquor and teos solution is 1:0.1 ~ 0.5:0.1 ~ 0.5:0.00005 ~ 0.001.
In the present invention, room temperature institute how is 0 ~ 40
oc.
The present invention has following useful technique effect:
(1) to adopt nano-stephanoporate silicon dioxide be that carrier is coated sulfur granules in the present invention, nano-stephanoporate silicon dioxide carrier is sulphur active material fixedly, can also play catalytic action to electrode process, thereby can effectively suppress the loss of active material in electrode process, cyclical stability and the high rate performance of raising electrode, obtain high-performance composite sulfur positive electrode.
(2) the present invention be take sulfur granules as template, adopts the hydrolytie polycondensation process clad nano porous silica of tetraethoxysilane, has overcome a preparation difficult problem for sulphur/silica core-shell nanostructure; Preparation method is easy, environmentally friendly, can accomplish scale production.
(3) the present invention, by controlling concentration and the ratio of reaction time, reaction raw materials, can regulate the ratio of the size of sulfur granules, the thickness of nano-stephanoporate silicon dioxide layer and silicon dioxide and sulphur, the storage lithium performance of the step control composite system of going forward side by side.
Accompanying drawing explanation
The X ray diffracting spectrum of the sulfur granules that Fig. 1: embodiment 1 makes and sulphur/silica core-shell nanostructure.
The transmission electron microscope photo of the sulfur granules that Fig. 2: embodiment 1 makes.
The energy spectrogram of sulphur/silica core-shell nanostructure that Fig. 3: embodiment 1 makes.
The transmission electron microscope photo of sulphur/silica core-shell nanostructure that Fig. 4: embodiment 1 makes.
The high-resolution-ration transmission electric-lens photo of sulphur/silica core-shell nanostructure that Fig. 5: embodiment 1 makes.
Embodiment
Below in conjunction with specific embodiment, describe the present invention.Protection scope of the present invention is not limited with embodiment, but is limited by claim.
embodiment 1:
A preparation method for sulphur for lithium-sulphur cell positive electrode/silica core-shell nanostructure, step is as follows:
(1) preparation of sulfur granules: 5 grams of polyvinylpyrrolidones are distributed in the sulfuric acid solution of 500 milliliters 3 mM/ls, drip the aqueous solution of the sodium thiosulfate of 50 milliliter of 0.3 mol/L, stir 2 hours, product is washed and is dried, obtain sulfur granules product;
(2) sulphur/silica core-shell nanostructure: 0.1 gram of sulfur granules that step (1) is obtained is distributed in 60 milliliters of ethanolic solutions together with 80 milligrams of softex kws, add successively subsequently 15 ml waters, 0.75 milliliter of ammoniacal liquor and 0.15 milliliter of teos solution, room temperature reaction 1 hour, product is washed and is dried, obtain described sulphur/silica core-shell nanostructure.
Fig. 1 is the sulfur granules that synthesized by embodiment 1 and the X ray diffracting spectrum of sulphur/silica core-shell nanostructure.As seen from the figure, the crystalline phase of sulphur/silica core-shell nanostructure is consistent with the crystalline phase of sulfur granules, is the sulphur (JCPDS 08-0247) of quadrature phase, and silica shell is unbodied state.Fig. 2 is the transmission electron microscope photo of the synthetic sulfur granules of the present embodiment.As seen from the figure, the basic glomeration of the pattern of prepared sulphur, and spheroidal particle distribution of sizes is more even.Fig. 3 is the energy spectrogram of the synthetic sulphur/silica core-shell nanostructure of the present embodiment.As seen from the figure, the element peak of sulphur comes from the sulfur granules core of core-shell nano structure, and the element peak of silicon and oxygen comes from the silica shell of core-shell nano structure.Fig. 4 and Fig. 5 are respectively transmission electron microscope photo and the high-resolution-ration transmission electric-lens photos of the synthetic sulphur/silica core-shell nanostructure of the present embodiment.As seen from the figure, product has demonstrated typical nucleocapsid structure, and the surface of sulfur granules core has been coated the silica shell of the uniform nanoporous of one deck.Nano-stephanoporate silicon dioxide carrier is sulphur active material fixedly, can also play catalytic action to electrode process, thereby can effectively suppress the loss of active material in electrode process, cyclical stability and the high rate performance of raising electrode, be conducive to obtain high-performance composite sulfur positive electrode.
embodiment 2:
A preparation method for sulphur for lithium-sulphur cell positive electrode/silica core-shell nanostructure, step is as follows:
(1) preparation of sulfur granules: 1 gram of polyvinylpyrrolidone is distributed in the sulfuric acid solution of 1 liter 0.1 mM/l, drip the aqueous solution of the sodium thiosulfate of 25 milliliters 4 mM/ls, stir 0.5 hour, product is washed and is dried, obtain sulfur granules product;
(2) sulphur/silica core-shell nanostructure: 0.3 milligram of sulfur granules that step (1) is obtained is distributed in 30 milliliters of ethanolic solutions together with 3 milligrams of softex kws, add successively subsequently 3 ml waters, 3 milliliters of ammoniacal liquor and 1.5 microlitre teos solutions, room temperature reaction 0.5 hour, product is washed and is dried, obtain described sulphur/silica core-shell nanostructure.Its result is similar with embodiment 1.
embodiment 3:
A preparation method for sulphur for lithium-sulphur cell positive electrode/silica core-shell nanostructure, step is as follows:
(1) preparation of sulfur granules: 100 grams of polyvinylpyrrolidones are distributed in the sulfuric acid solution of 1 liter 100 mM/ls, drip the aqueous solution of the sodium thiosulfate of 250 milliliter of 40 mol/L, stir 24 hours, product is washed and is dried, obtain sulfur granules product;
(2) sulphur/silica core-shell nanostructure: 1.2 grams of sulfur granules that step (1) is obtained are distributed in 120 milliliters of ethanolic solutions together with 1.2 milligrams of polyvinylpyrrolidones, add successively subsequently 60 ml waters, 60 milliliters of ammoniacal liquor and 0.12 milliliter of teos solution, room temperature reaction 12 hours, product is washed and is dried, obtain described sulphur/silica core-shell nanostructure.Its result is similar with embodiment 1.
embodiment 4:
A preparation method for sulphur for lithium-sulphur cell positive electrode/silica core-shell nanostructure, step is as follows:
(1) preparation of sulfur granules: 60 grams of diallyl dimethyl ammoniumchloride are distributed in the sulfuric acid solution of 1 liter 18 mM/ls, drip the aqueous solution of the sodium thiosulfate of 500 milliliter of 2 mol/L, stir 15 hours, product is washed and is dried, obtain sulfur granules product;
(2) sulphur/silica core-shell nanostructure: 0.3 gram of sulfur granules that step (1) is obtained is distributed in 60 milliliters of ethanolic solutions together with 0.3 gram of kayexalate, add successively subsequently 18 ml waters, 18 milliliters of ammoniacal liquor and 0.03 milliliter of teos solution, room temperature reaction 45 minutes, product is washed and is dried, obtain described sulphur/silica core-shell nanostructure.Its result is similar with embodiment 1.
embodiment 5:
A preparation method for sulphur for lithium-sulphur cell positive electrode/silica core-shell nanostructure, step is as follows:
(1) preparation of sulfur granules: 5 grams of kayexalates are distributed in the sulfuric acid solution of 1 liter 2 mM/ls, drip the aqueous solution of the sodium thiosulfate of 120 milliliter of 0.1 mol/L, stir 1 hour, product is washed and is dried, obtain sulfur granules product;
(2) sulphur/silica core-shell nanostructure: 2.4 milligrams of sulfur granules that step (1) is obtained are distributed in 30 milliliters of ethanolic solutions together with 15 milligrams of diallyl dimethyl ammoniumchloride, add successively subsequently 4.5 ml waters, 4.5 milliliters of ammoniacal liquor and 80 microlitre teos solutions, room temperature reaction 6 hours, product is washed and is dried, obtain described sulphur/silica core-shell nanostructure.Its result is similar with embodiment 1.
Claims (7)
1. a preparation method for sulphur/silica core-shell nanostructure for lithium-sulphur cell positive electrode, is characterized in that, comprises the following steps:
(1) preparation of sulfur granules: surfactant-dispersed, in sulfuric acid solution, is dripped to the aqueous solution of sodium thiosulfate, stir 0.5 ~ 24 hour, product is washed and is dried, obtain sulfur granules product;
(2) preparation of sulphur/silica core-shell nanostructure: the sulfur granules that step (1) is obtained is distributed in ethanolic solution together with surfactant, add successively subsequently water, ammoniacal liquor and teos solution, room temperature reaction 0.5 ~ 12 hour, product is washed and is dried, obtain described sulphur/silica core-shell nanostructure.
2. the preparation method of sulphur/silica core-shell nanostructure for lithium-sulphur cell positive electrode according to claim 1, it is characterized in that: in step (1), described surfactant is one or more in polyvinylpyrrolidone, softex kw, diallyl dimethyl ammoniumchloride, kayexalate; The mass concentration of described surfactant is 1 ~ 100 grams per liter.
3. the preparation method of sulphur/silica core-shell nanostructure for lithium-sulphur cell positive electrode according to claim 1, is characterized in that: in step (1), the concentration of described sulfuric acid solution is 0.1 ~ 100 mM/l; Described sodium thiosulfate and H
2sO
4mol ratio be 1 ~ 100:1.
4. the preparation method of sulphur/silica core-shell nanostructure for lithium-sulphur cell positive electrode according to claim 1, is characterized in that: in step (2), the concentration of described sulfur granules in ethanolic solution is 0.01 ~ 10 grams per liter.
5. the preparation method of sulphur/silica core-shell nanostructure for lithium-sulphur cell positive electrode according to claim 1, it is characterized in that: in step (2), described surfactant is one or more in polyvinylpyrrolidone, softex kw, diallyl dimethyl ammoniumchloride, kayexalate; The mass concentration of described surfactant is 0.1 ~ 10 grams per liter.
6. the preparation method of sulphur/silica core-shell nanostructure for lithium-sulphur cell positive electrode according to claim 1, it is characterized in that: in step (2), the volume proportion of described ethanolic solution, water, ammoniacal liquor and teos solution is 1:0.1 ~ 0.5:0.1 ~ 0.5:0.00005 ~ 0.001.
7. the preparation method of sulphur/silica core-shell nanostructure for lithium-sulphur cell positive electrode according to claim 1, is characterized in that: in step (2), and NH in described ammoniacal liquor
3quality percentage composition be 25 ~ 28%, SiO in described teos solution
2quality percentage composition higher than 28.0%.
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Cited By (7)
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| CN105006553A (en) * | 2015-07-11 | 2015-10-28 | 中国计量学院 | Preparation method of sulfur/carbon/oxide combined electrode material |
| CN105742587A (en) * | 2016-02-25 | 2016-07-06 | 南京师范大学 | Preparation method of sulfur/silica gel three-dimensional composite material for positive electrode of lithium-sulfur battery |
| KR20170116095A (en) * | 2015-02-13 | 2017-10-18 | 더 리전트 오브 더 유니버시티 오브 캘리포니아 | Coated sulfur particles electrode and method |
| CN108793083A (en) * | 2018-04-25 | 2018-11-13 | 安徽师范大学 | A kind of three-dimensional porous sulfur granules nano material and preparation method thereof, a kind of lithium-sulphur cell positive electrode and lithium-sulfur cell |
| CN112897497A (en) * | 2021-01-18 | 2021-06-04 | 广东技术师范大学 | Sulfur reduction reaction catalytic material and preparation method and application thereof |
| CN114072937A (en) * | 2019-07-03 | 2022-02-18 | 尤米科尔公司 | Lithium nickel manganese cobalt composite oxides as positive electrode active materials for rechargeable lithium ion batteries |
| WO2023279149A1 (en) * | 2021-07-05 | 2023-01-12 | The University Of Sydney | Lithium sulfur battery additive |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11362335B2 (en) * | 2015-02-13 | 2022-06-14 | The Regents Of The University Of California | Coated sulfur particle electrode and method |
| KR20170116095A (en) * | 2015-02-13 | 2017-10-18 | 더 리전트 오브 더 유니버시티 오브 캘리포니아 | Coated sulfur particles electrode and method |
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| KR102591407B1 (en) * | 2015-02-13 | 2023-10-18 | 더 리전트 오브 더 유니버시티 오브 캘리포니아 | Coated sulfur particle electrode and method |
| CN107431174B (en) * | 2015-02-13 | 2021-11-16 | 加利福尼亚大学董事会 | Coated sulfur particle electrode and method |
| CN105006553B (en) * | 2015-07-11 | 2017-06-23 | 中国计量学院 | A kind of preparation method of sulphur/carbon/oxide combination electrode material |
| CN105006553A (en) * | 2015-07-11 | 2015-10-28 | 中国计量学院 | Preparation method of sulfur/carbon/oxide combined electrode material |
| CN105742587A (en) * | 2016-02-25 | 2016-07-06 | 南京师范大学 | Preparation method of sulfur/silica gel three-dimensional composite material for positive electrode of lithium-sulfur battery |
| CN105742587B (en) * | 2016-02-25 | 2018-10-23 | 南京师范大学 | A kind of preparation method of lithium-sulphur cell positive electrode sulphur/silica dioxide gel three-dimensional composite material |
| CN108793083A (en) * | 2018-04-25 | 2018-11-13 | 安徽师范大学 | A kind of three-dimensional porous sulfur granules nano material and preparation method thereof, a kind of lithium-sulphur cell positive electrode and lithium-sulfur cell |
| CN114072937A (en) * | 2019-07-03 | 2022-02-18 | 尤米科尔公司 | Lithium nickel manganese cobalt composite oxides as positive electrode active materials for rechargeable lithium ion batteries |
| CN112897497A (en) * | 2021-01-18 | 2021-06-04 | 广东技术师范大学 | Sulfur reduction reaction catalytic material and preparation method and application thereof |
| WO2023279149A1 (en) * | 2021-07-05 | 2023-01-12 | The University Of Sydney | Lithium sulfur battery additive |
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Application publication date: 20141203 |