CN105006553A - Preparation method of sulfur/carbon/oxide combined electrode material - Google Patents
Preparation method of sulfur/carbon/oxide combined electrode material Download PDFInfo
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- CN105006553A CN105006553A CN201510414029.9A CN201510414029A CN105006553A CN 105006553 A CN105006553 A CN 105006553A CN 201510414029 A CN201510414029 A CN 201510414029A CN 105006553 A CN105006553 A CN 105006553A
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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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- H—ELECTRICITY
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Abstract
The invention relates to a preparation method of a sulfur/carbon/oxide combined electrode material. The preparation method comprises depositing sulfur and oxide on a carbon material as a carrier with excellent performances to obtain the sulfur/carbon/oxide combined electrode material. The carbon material is one of graphene, CMK-3, carbon nanotubes and carbon black. The oxide is one of silica, copper oxide, silver oxide, nickel oxide, ferrous oxide, tin oxide and titanium oxide. The sulfur/carbon/oxide combined electrode material comprises 50-90wt% of sulfur, 5-20wt% of carbon and 5-30wt% of the oxide. Through control of acid types and pH, and organic solvent types and properties, the sulfur/carbon/oxide combined electrode material with fine particles and high coating uniformity is obtained. The sulfur/carbon/oxide combined electrode material as a lithium-sulfur battery positive pole material has high specific capacity and excellent cycling properties and has a good application prospect in the field of batteries.
Description
Technical field
The present invention relates to a kind of preparation method of electrode material, be specifically related to a kind of preparation method of sulphur/carbon/oxide combination electrode material.
Background technology
Lithium-sulfur cell has that specific capacity is high, low cost and other advantages, is the energy-storage battery having very much development potentiality.Sulphur positive electrode is one of key factor of restriction lithium-sulfur cell popularization., in charge and discharge process, there is volumetric expansion and contraction and electrode material come off from metal collector surface, causing lithium-sulfur cell capacity rapid decay, utilization efficiency low in commercial battery sulphur poorly conductive.At present, the material with carbon element of conventional bigger serface, high conductivity supports sulphur simple substance, and the carbon/sulphur composite material exhibits of preparation goes out the high rate performance of high specific capacity, good cycle performance and excellence.Patent (a kind of preparation method of nano-sulfur/graphene oxide composite material of height ratio capacity; 201210248009) by synthesis of nano sulfur granules under the protection of surfactant; by the interaction between surfactant and graphene oxide, graphene oxide and material with carbon element are adsorbed in equably the surface of nano-sulfur particles again, are formed and there is hud typed nano-sulfur/graphene oxide composite electrode material.This material has Stability Analysis of Structures, conductivity high, and cycle performance obviously improves.Patent (a kind of preparation method of lithium sulphur positive electrode, 201210371963.3) adopts sulphur organic solution evaporation and diffusion to carbon material surface, obtains sulphur/carbon composite; This carbon/sulphur composite material first capacity reaches 900mAh/g, and after 10 circulations, capability retention is greater than 48%.
Novel structure, the material with carbon element that hole dimension is little effectively limits the granular size of sulphur simple substance, carbon conductive good material improves the conductance of elemental sulfur simultaneously. but the volumetric expansion of sulphur/carbon composite sulphur in charge and discharge process and contraction, if sulfur granules top layer is without other coating, will inevitably occur that sulfur granules comes off and causes Capacity fading phenomenon.
Summary of the invention
The object of the invention is the preparation method providing a kind of sulphur/carbon/oxide combination electrode material, overcomes the defect of existing technology of preparing, improves the cycle life of sulfur electrode material.For achieving the above object, technical scheme of the present invention is:
A kind of preparation method of sulphur/carbon/oxide combination electrode material; Comprise:
1) weigh the organic solution that the sodium thiosulfate of certain mass and material with carbon element are mixed in deionized water, stir:
2) slowly instill acid solution, agitation and filtration, oven dry etc., obtain sulphur/material with carbon element;
3) weigh the sulphur/material with carbon element of certain mass, alcoholic solution that oxide precursor, surfactant are mixed in deionized water, stir:
4) slowly drip aqueous slkali, at the uniform velocity stir 1 ~ 5 hour, leave standstill, centrifugation, washing, oven dry, 100 ~ 200 DEG C of atmosphere sinterings, obtain sulphur/carbon/oxide combination electrode material.
Water in described step 1 and organic volume ratio are 0.1 ~ 0.8;
Organic substance in described step 1 is the one of methyl alcohol, ethanol, ethylene glycol, glycerol, oxolane;
In described step 2, the pH of acid solution controls 2 ~ 6; Acid is phosphoric acid class, sulphonic acids, C1 ~ C5 straight chain organic acid one;
In described step 2, acid controls 1.01 ~ 1.3 with the mol ratio of sodium thiosulfate;
In described step 3, oxide precursor is the one of organosilicon, acetate, formates, sulfonate, grape hydrochlorate, salicylate;
Described material with carbon element is Graphene, CMK-3, the one of carbon nano-tube or carbon black;
Described oxide is the one of silicon dioxide, cupric oxide, silver oxide, nickel oxide, ferrous oxide, tin oxide and titanium oxide;
Described sulphur accounts for 50 ~ 90% of sulphur/carbon/oxide combination electrode material gross mass, and material with carbon element accounts for 5 ~ 20% of sulphur/carbon/oxide combination electrode material gross mass, and oxide accounts for 5 ~ 30% of sulphur/carbon/oxide combination electrode material gross mass.
The preparation method of sulphur/carbon/oxide combination electrode material provided by the invention, compared with other sulphur method for preparing anode material, tool has the following advantages:
1) present invention process is simple, easy to operate, is conducive to suitability for industrialized production.
2) pH value that regulation and control are sour and kind, control sulphur deposition rate; Obtain small-sized sulphur/carbon composite;
3) sulfur electrode material inner layer is material with carbon element, external sheath oxide; This structure is not only conducive to electrical conductivity, and stops sulphur simple substance particle to come off in charge and discharge cycles process.
4) in sulphur/carbon/oxide combination electrode material, sulphur accounts for 50 ~ 90% of sulphur/carbon/oxide combination electrode material gross mass, material with carbon element accounts for 5 ~ 20% of sulphur/carbon/oxide combination electrode material gross mass, and oxide accounts for 5 ~ 30% of sulphur/carbon/oxide combination electrode material gross mass.The sulfur electrode material of prepared nucleocapsid structure, has height ratio capacity and long circulation life; 0.1C circulates after 100 times, and capacity is greater than 730mAh/g.
Accompanying drawing illustrates:
Fig. 1 is the XRD of sulphur/carbon/oxide combination electrode material of the present invention.
Fig. 2 is the SEM of sulphur/carbon/oxide combination electrode material of the present invention.
Fig. 3 is the circulation volume of sulphur/carbon/oxide combination electrode material of the present invention.
Embodiment
For summary of the invention of the present invention, Characteristic can be understood further, hereby lift following examples, and coordinate accompanying drawing to be described in detail as follows:
Refer to accompanying drawing 1,2,3
Embodiment 1
A kind of Composition Design of sulphur/carbon/oxide combination electrode material is:
Silica, 23wt%; Sulphur simple substance, mass fraction 70%; Graphene, mass fraction 7wt%;
A kind of preparation method of sulphur/carbon/oxide combination electrode material: comprise the following steps:
1) the five water sodium thiosulfate and the 0.14 gram of Graphene that weigh 10.4 grams are mixed in 30 ml water ethanolic solutions, configuration hypo solution: wherein, the volume ratio of water and ethanol is 0.5;
2) slowly instill phosphoric acid solution, the pH of phosphoric acid solution controls 4; The mol ratio of phosphoric acid and sodium thiosulfate controls 1.2; Agitation and filtration, oven dry etc., obtain sulphur/grapheme material;
3) sulphur/grapheme material, 1.59 grams of tetraethoxysilanes, surfactant are mixed in the alcoholic solution of deionized water, stir:
4) slowly drip aqueous slkali, at the uniform velocity stir 3 hours, leave standstill, centrifugation, washing, oven dry, 150 DEG C, atmosphere sintering obtain sulphur/graphene/silicon dioxide combination electrode material.
The SEM of Fig. 1 to be the XRD of sulphur/graphene/silicon dioxide combination electrode material, Fig. 2 be sulphur/graphene/silicon dioxide combination electrode material.Sulphur is supported on graphenic surface, silicon dioxide is coated further sulphur/graphene composite material.Fig. 3 is the cycle performance of sulphur/graphene/silicon dioxide combination electrode material.The preparation and property test of sulfur electrode; Sulfur electrode material, acetylene black and PVDF among NMPs to be mixed in mass ratio at 80: 10: 5, be coated on aluminium foil is electrode film, metal lithium sheet is to electrode, CELGARD 2400 is barrier film, the LiPF6/EC+DMCWEI of 1mol/L is electrolyte, be assembled into button cell being full of in Ar glove box, adopt Land battery test system to carry out constant current charge-discharge test.Charging/discharging voltage scope is 3.0 ~ 1V, and current density is that after 100 circulations of 170mA/g. composite material, specific discharge capacity still keeps 738mAh/g.
Embodiment 2
A kind of Composition Design of sulphur/carbon/oxide combination electrode material is:
Cupric oxide, 15wt%; Sulphur simple substance, mass fraction 75%; Graphene, mass fraction 10wt%;
Silver oxide, 19wt%; Sulphur simple substance, mass fraction 71%; Carbon nano-tube, mass fraction 10wt%;
Nickel oxide, 10wt%; Sulphur simple substance, mass fraction 81%; CMK-3, mass fraction 9wt%;
A kind of preparation method of sulphur/carbon/oxide combination electrode material: comprise the following steps:
1) weigh the organic solution that the sodium thiosulfate of certain mass and material with carbon element are mixed in deionized water, stir:
2) slowly instill acetum, the pH of acetum controls 5; The mol ratio of acetic acid and sodium thiosulfate controls 1.25; Agitation and filtration, oven dry etc., obtain sulphur/material with carbon element;
3) sulphur/material with carbon element, tetraethoxysilane, surfactant are mixed in the alcoholic solution of deionized water, stir:
4) slowly drip aqueous slkali, at the uniform velocity stir 4 hours, leave standstill, centrifugation, washing, oven dry obtain sulphur/carbon/oxide combination electrode material.
The preparation and property test of sulfur electrode; Sulfur electrode material, acetylene black and PVDF among NMPs to be mixed in mass ratio at 80: 10: 5, be coated on aluminium foil is electrode film, metal lithium sheet is to electrode, CELGARD 2400 is barrier film, the LiPF6/EC+DMCWEI of 1mol/L is electrolyte, be assembled into button cell being full of in Ar glove box, adopt Land battery test system to carry out constant current charge-discharge test.Charging/discharging voltage scope is 3.0 ~ 1V, and current density is that after 100 circulations of 170mA/g. composite material, specific discharge capacity is greater than 730mAh/g.
Embodiment 3
A kind of Composition Design of sulphur/carbon/oxide combination electrode material with embodiment 1,
Comprise the following steps:
1) tetrahydrofuran solution that the five water sodium thiosulfate of 10.4 grams and 0.14 gram of Graphene are mixed in 30 ml waters is weighed, configuration hypo solution: wherein, the volume ratio of water and oxolane is 0.6;
2) slowly instill benzene sulfonic acid solution, the pH of phosphoric acid solution controls 4.75; The mol ratio of benzene sulfonic acid and sodium thiosulfate controls 1.1; Agitation and filtration, oven dry etc., obtain sulphur/grapheme material;
3) sulphur/grapheme material of certain mass ratio, methyl trichlorosilicane, surfactant are mixed in the alcoholic solution of deionized water, stir:
4) slowly drip aqueous slkali, at the uniform velocity stir 5 hours, leave standstill, centrifugation, washing, oven dry obtain sulphur/graphene/silicon dioxide combination electrode material.
The preparation and property test of sulfur electrode; Sulfur electrode material, acetylene black and PVDF among NMPs to be mixed in mass ratio at 80: 10: 5, be coated on aluminium foil is electrode film, metal lithium sheet is to electrode, CELGARD 2400 is barrier film, the LiPF6/EC+DMCWEI of 1mol/L is electrolyte, be assembled into button cell being full of in Ar glove box, adopt Land battery test system to carry out constant current charge-discharge test.Charging/discharging voltage scope is 3.0 ~ 1V, and current density is that after 100 circulations of 170mA/g. composite material, specific discharge capacity is greater than 730mAh/g.
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.
Claims (1)
1. a preparation method for sulphur/carbon/oxide combination electrode material, is characterized in that: with the material with carbon element of high-specific surface area for carrier, and deposition sulphur, oxide, obtain sulphur/carbon/oxide combination electrode material; Material with carbon element is Graphene, CMK-3, the one of carbon nano-tube or carbon black; Oxide is the one of silicon dioxide, cupric oxide, silver oxide, nickel oxide, ferrous oxide, tin oxide and titanium oxide; Sulphur accounts for 50 ~ 90% of sulphur/carbon/oxide combination electrode material gross mass, and carbon accounts for 5 ~ 20% of sulphur/carbon/oxide combination electrode material gross mass, and oxide accounts for 5 ~ 30% of sulphur/carbon/oxide combination electrode material gross mass; The preparation method of sulphur/carbon/oxide combination electrode material comprises the steps:
1) weigh the organic solution that the sodium thiosulfate of certain mass and material with carbon element are mixed in deionized water, stir:
Wherein: water and organic volume ratio are 0.1 ~ 0.8; Organic substance is the one of methyl alcohol, ethanol, ethylene glycol, glycerol, oxolane;
2) slowly instill acid solution, agitation and filtration, oven dry etc., obtain sulphur/material with carbon element;
Wherein, the pH of acid solution controls 2 ~ 6; Acid is phosphoric acid class, sulphonic acids, C1 ~ C5 straight chain organic acid one; Acid controls 1.01 ~ 1.3 with the mol ratio of sodium thiosulfate;
3) weigh the sulphur/material with carbon element of certain mass, alcoholic solution that oxide precursor, surfactant are mixed in deionized water, stir:
Wherein, oxide precursor is the one of organosilicon, acetate, formates, sulfonate, grape hydrochlorate, salicylate;
4) slowly drip aqueous slkali, at the uniform velocity stir 1 ~ 5 hour, leave standstill, centrifugation, washing, oven dry, 100 ~ 200 DEG C of atmosphere sinterings, obtain sulphur/carbon/oxide combination electrode material.
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Cited By (8)
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| CN105390700A (en) * | 2015-11-16 | 2016-03-09 | 哈尔滨工业大学 | Method for modifying positive electrode of lithium ion battery by adding metal oxide/carbon composite material |
| CN106450195A (en) * | 2016-10-18 | 2017-02-22 | 中国科学院化学研究所 | Positive electrode material of lithium sulfur battery, preparation method of positive electrode material and lithium sulfur battery containing positive electrode material |
| CN106876673A (en) * | 2017-03-10 | 2017-06-20 | 哈尔滨工业大学 | The method that one-step method prepares titanium dioxide and the double-deck core shell structure lithium sulfur battery anode material of cladding altogether of Graphene |
| CN106981637A (en) * | 2017-04-26 | 2017-07-25 | 清华大学 | SiO2/TiO2/ C/S lithium sulfur battery anode materials and preparation method thereof |
| CN107492639A (en) * | 2017-07-28 | 2017-12-19 | 清华大学 | A kind of lithium-sulfur battery composite anode material and preparation method |
| CN107591523A (en) * | 2017-08-22 | 2018-01-16 | 桂林电子科技大学 | A kind of iron, nickel dopped activated carbon sulfur materials and its preparation method and application |
| CN113488629A (en) * | 2021-07-23 | 2021-10-08 | 江西省科学院应用化学研究所 | Spherical carbon-coated tungsten oxide/sulfur positive electrode material of core-shell structure loaded with multiple rare earth oxides and preparation method thereof |
| WO2023229200A1 (en) * | 2022-05-27 | 2023-11-30 | 주식회사 엘지에너지솔루션 | Silica-coated sulfur-carbon composite and lithium-sulfur battery comprising same |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105390700A (en) * | 2015-11-16 | 2016-03-09 | 哈尔滨工业大学 | Method for modifying positive electrode of lithium ion battery by adding metal oxide/carbon composite material |
| CN105390700B (en) * | 2015-11-16 | 2019-11-29 | 哈尔滨工业大学 | A method of by adding metal oxide/carbon composite modification lithium-ion battery anode |
| CN106450195A (en) * | 2016-10-18 | 2017-02-22 | 中国科学院化学研究所 | Positive electrode material of lithium sulfur battery, preparation method of positive electrode material and lithium sulfur battery containing positive electrode material |
| CN106876673A (en) * | 2017-03-10 | 2017-06-20 | 哈尔滨工业大学 | The method that one-step method prepares titanium dioxide and the double-deck core shell structure lithium sulfur battery anode material of cladding altogether of Graphene |
| CN106876673B (en) * | 2017-03-10 | 2019-06-11 | 哈尔滨工业大学 | The method that one-step method prepares the core-shell structure lithium sulfur battery anode material that titanium dioxide and graphene bilayer coat altogether |
| CN106981637A (en) * | 2017-04-26 | 2017-07-25 | 清华大学 | SiO2/TiO2/ C/S lithium sulfur battery anode materials and preparation method thereof |
| CN106981637B (en) * | 2017-04-26 | 2019-07-26 | 清华大学 | SiO2/TiO2/ C/S lithium sulfur battery anode material and preparation method thereof |
| CN107492639A (en) * | 2017-07-28 | 2017-12-19 | 清华大学 | A kind of lithium-sulfur battery composite anode material and preparation method |
| CN107591523A (en) * | 2017-08-22 | 2018-01-16 | 桂林电子科技大学 | A kind of iron, nickel dopped activated carbon sulfur materials and its preparation method and application |
| CN113488629A (en) * | 2021-07-23 | 2021-10-08 | 江西省科学院应用化学研究所 | Spherical carbon-coated tungsten oxide/sulfur positive electrode material of core-shell structure loaded with multiple rare earth oxides and preparation method thereof |
| CN113488629B (en) * | 2021-07-23 | 2022-05-27 | 江西省科学院应用化学研究所 | Spherical carbon-coated tungsten oxide/sulfur positive electrode material of core-shell structure loaded with multiple rare earth oxides and preparation method thereof |
| WO2023229200A1 (en) * | 2022-05-27 | 2023-11-30 | 주식회사 엘지에너지솔루션 | Silica-coated sulfur-carbon composite and lithium-sulfur battery comprising same |
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