CN105742593A - Cathode material for lithium-sulfur battery and preparation method of cathode material - Google Patents
Cathode material for lithium-sulfur battery and preparation method of cathode material Download PDFInfo
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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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Abstract
The invention discloses a cathode material for a lithium-sulfur battery and a preparation method of the cathode material. The cathode material is the cathode material, with a sulfur element layer inside and a surface coating layer outside, for a double-shell lithium-sulfur battery. The method comprises the following specific preparation steps: (1) dispersing a metal sulfide containing the surface coating layer into a dispersion solution, containing an oxidant, ferrous ions and iodide ions, of water and ethanol, and carrying out stirring reaction at 10-50 DEG C for 12-36 hours; and (2) carrying out suction filtration after reaction is ended, carrying out vacuum drying at 40-60 DEG C for 10-14 hours to obtain the cathode material, with the sulfur element layer inside and the surface coating layer outside, for the double-shell lithium-sulfur battery. According to the method, with the metal sulfide as a sulfur source, the sulfur ions in the metal sulfide are oxidized into a sulfur element through the oxidant, so that, on one hand, sulfur is tightly coated with the coating layer and suppression on sulfur dissolution is achieved; and on the other hand, more selection and subsequent treatment can be permitted for the surface coating layer due to the stable characteristics of the metal sulfide.
Description
Technical field
The invention belongs to lithium-sulfur rechargeable battery field of material preparation, relate to a kind of by oxidized metal sulfide system thio one-tenth lithium sulfur battery anode material and method thereof.
Background technology
Along with the demand of growing portable type electronic product, the secondary rechargeable battery of high-energy-density is increasingly becoming research emphasis.Lithium ion battery is the secondary cell that current combination property is best, has been widely used for portable type electronic product and the electric tools such as mobile phone, digital camera, notebook computer.Along with the energy-accumulating power station of various scales, electric automobile, the fast development of intelligent grid, the requirement to lithium ion battery energy density and power density is more and more higher.But, limited by battery system and electrode material theory lithium storage content, even if in view of using the positive and negative electrode material and more advanced design and manufacturing technology with more height ratio capacity from now on, the specific energy of lithium ion battery also will stay on 200Wh kg-1Left and right.Therefore, use the pure electric automobile of lithium ion battery be difficult to reach can be comparable with existing fuel vehicle continual mileage (generally at about 500km, it is desirable to battery specific energy reaches 350Wh Kg-1Above).In the various secondary cell systems currently studied, only lithium-sulfur cell and lithium-air battery can be competent at the requirement of high-energy-density.
Elemental sulfur is as anode material for lithium-ion batteries, and its theoretical capacity may be up to 1675mAh/g, and theoretical energy density reaches 2600Wh/kg.The rich reserves of sulfur, elemental sulfur is cheap, avirulence.So, lithium-sulfur cell is one of developing direction of following lithium secondary battery.
But, owing to low conductivity feature and the elemental sulfur of elemental sulfur react, with lithium, the numerous intermediate products (polysulfide) generated and be prone to dissolve in electrolyte, cause the problems such as active substance loss, self-discharge of battery and electrode passivation, it is typically at present to be filled in elemental sulfur and all kinds of has in the carbon element class material of high-specific surface area, high porosity and excellent conductive performance feature, conducting polymer composite, form composite, dissolve in electrolyte and the various negative effects thus caused limiting polysulfide in cyclic process.
But, common material surface method for coating is to be coated with Organic substance at particle surface, and calcining forms cladding product the most under reducing atmosphere.But sulfur is at high temperature calcined and can be gasified, therefore conventional method for coating is not suitable for the carbon cladding of sulfur, and the carbon cladding of sulfur generally requires extremely harsh capsulation condition, and preparation process is complicated.
Summary of the invention
For the problems referred to above, the invention provides a kind of sulfur positive electrode for battery material and preparation method thereof, the method is with metal sulfide for sulfur source, by oxidant, the sulphion in metal sulfide is oxidized to sulfur simple substance, on the one hand achieve sulfur and be closely coated on inside clad, achieve the suppression that sulfur is dissolved, on the one hand due to the stability characteristic (quality) of metal sulfide, can allow surface coating layer is more selected and subsequent treatment.
It is an object of the invention to be achieved through the following technical solutions:
A kind of positive material for lithium-sulfur battery, its be internal be sulfur simple substance layer, outside is the bivalve layer positive material for lithium-sulfur battery of surface coating layer.
The preparation method of a kind of above-mentioned positive material for lithium-sulfur battery, by carrying out oxidation sulfur processed, to prepare lithium sulfur battery anode material to the metal sulfide being coated with face coat in advance.Concrete preparation process is as follows:
One, the metal sulfide containing surface coating layer is dispersed in the dispersion soln containing oxidant, ferrous ion, the water of iodide ion and ethanol, stirring reaction 12-36h under conditions of 10-50 DEG C, wherein: metal sulfide is 1:2-12:0-0.5:0-1:0.5-5 with the thing mass ratio of oxidant, ferrous ion, iodide ion and water, ethanol is 1-10:1 with the volume ratio of water；
Two, reaction terminates rear sucking filtration, is vacuum dried 10-14h under the conditions of 40-60 DEG C, and obtaining internal is sulfur simple substance layer, and outside is the bivalve layer positive material for lithium-sulfur battery of surface coating layer.
In the present invention, the metal of described metal sulfide is the mixture of one or more in Zn, Fe, Cd, Pb, Mn etc..
In the present invention, described oxidant is elemental iodine.
In the present invention, the surface of described metal sulfide can carry out charcoal, inorganic conductive material, semi-conducting material, the cladding of lithium ion quick conductor material in advance.
The present invention use metal sulfide as sulfur source, metal sulfide as: zinc sulfide, cadmium sulfide, copper sulfide etc., there is splendid chemical stability and high-temperature stability, it is allowed to carry out Surface coating on its surface and do not react；Follow-up under the high temperature conditions face coat can be carried out post processing, form charcoal clad or the Surface coating coating of high-crystallinity, realized the generation of sulfur simple substance the most on this basis by redox reaction.Thus fundamentally solve due to sulfur simple substance poor high temperature stability, it is difficult to the problem that conventional method carries out being coated with is used on surface.On the other hand, sulfur simple substance is changed into owing to the method uses by the metal sulfide within clad, it is ensured that sulfur simple substance is present in inside clad.
Accompanying drawing explanation
Fig. 1 is zinc sulphide morphology；
Fig. 2 is the thermogravimetric curve of carbon-sulfur compound 1-4；
Fig. 3 is carbon-sulfur compound pattern: carbon-sulfur compound 1(a, b)；Carbon-sulfur compound 2(c, d)；Carbon-sulfur compound 1(e, f)；Carbon-sulfur compound 1(g, h)；
Fig. 4 is battery performance；
Fig. 5 is the thermogravimetric curve of carbon-sulfur compound 5-8；
Fig. 6 is cadmium sulfide pattern；
Fig. 7 is the thermogravimetric curve of carbon-sulfur compound 9；
Fig. 8 is the thermogravimetric curve of carbon-sulfur compound 10；
Fig. 9 is the pattern of the sulfur pure metals of coated by titanium dioxide；
Figure 10 is the thermogravimetric curve of coated by titanium dioxide sulfur.
Detailed description of the invention
Below in conjunction with embodiment, technical scheme is further described; but it is not limited thereto; every technical solution of the present invention is modified or equivalent, without deviating from the spirit and scope of technical solution of the present invention, all should contain in protection scope of the present invention.
Embodiment
1
One, prepared by zinc sulfide:
1.12g zinc nitrate hexahydrate mixing 0.12g Sublimed Sulfur is dispersed in 200ml ethylene glycol, puts in the reactor that 250ml polytetrafluoro is pure, 150 DEG C, react 24h under conditions of rotating speed 600rmb/min.Standing to room temperature, dehydrated alcohol, deionized water are centrifuged each three times, dry 24h for 80 DEG C, and gained zinc sulphide morphology, as it is shown in figure 1, as can be seen from Figure 1 obtained zinc sulfide particle diameter is at about 120nm, is uniformly dispersed.
Two, prepared by charcoal cladding zinc sulfide:
Charcoal bag zinc sulfide-1:145mg zinc sulfide mixing 25mg resorcinol, pours in 80ml ethanol, ultrasonic disperse 30min.Adding 50ul formaldehyde and the ammonia of 2ml 28%, 30 degree are stirred vigorously reaction 24h.Proceed in the reactor of 100ml polytetrafluoro liner, 100 DEG C, react 24h under conditions of rotating speed 400rmb/min.Standing to room temperature, dehydrated alcohol, deionized water are centrifuged each three times, put in tube furnace after 80 DEG C of drying 24h, and argon shield 700 DEG C processes 240min, 5 DEG C/min of heating rate.After being down to room temperature, take out and grind, stand-by.
Charcoal bag zinc sulfide-2:145mg zinc sulfide mixing 20mg resorcinol, pours in 80ml ethanol, ultrasonic disperse 30min.Adding 40ul formaldehyde and the ammonia of 2ml 28%, 30 DEG C are stirred vigorously reaction 24h.Proceed in the reactor of 100ml polytetrafluoro liner, 100 DEG C, react 24h under conditions of rotating speed 400rmb/min.Standing to room temperature, dehydrated alcohol, deionized water are centrifuged each three times, put in tube furnace after 80 DEG C of drying 24h, argon shield 700 DEG C sintering 240min, 5 DEG C/min of heating rate.After being down to room temperature, take out and grind, stand-by.
Charcoal bag zinc sulfide-3:145mg zinc sulfide mixing 15mg resorcinol, pours in 80ml ethanol, ultrasonic disperse 30min.Adding 30ul formaldehyde and the ammonia of 2ml 28%, 30 DEG C are stirred vigorously reaction 24h.Proceed in the reactor of 100ml polytetrafluoro liner, 100 DEG C, react 24h under conditions of rotating speed 400rmb/min.Standing to room temperature, dehydrated alcohol, deionized water are centrifuged each three times, put in tube furnace after 80 DEG C of drying 24h, argon shield 700 DEG C sintering 240min, 5 DEG C/min of heating rate.After being down to room temperature, take out and grind, stand-by.
Charcoal bag zinc sulfide-4:145mg zinc sulfide mixing 10mg resorcinol, pours in 80ml ethanol, ultrasonic disperse 30min.Adding 20ul formaldehyde and the ammonia of 2ml 28%, 30 degree are stirred vigorously reaction 24h.Proceed in the reactor of 100ml polytetrafluoro liner, 100 DEG C, react 24h under conditions of rotating speed 400rmb/min.Standing to room temperature, dehydrated alcohol, deionized water are centrifuged each three times, put in tube furnace after 80 DEG C of drying 24h, argon shield 700 DEG C sintering 240min, 5 DEG C/min of heating rate.After being down to room temperature, take out and grind, stand-by.
Three, the preparation of carbon-sulfur compound:
Weigh in the 250ml flask that 200mg charcoal bag zinc sulfide puts into 20ml ethanol and 20ml deionized water mixed solution, containing anhydrous sodium iodide 0.3g, ferrous sulfate heptahydrate 0.834g, elemental iodine 3.6g in solution.Subsequently 20 DEG C be stirred vigorously reaction 24h after, sucking filtration, 60 DEG C dry 12h prepare carbon-sulfur compound 1-4.The thermogravimetric curve of carbon-sulfur compound 1-4 is shown in that Fig. 2, pattern are shown in Fig. 3, is prepared into electrode, assembles button cell and tests, and battery performance is shown in Fig. 4.
From figure 2 it can be seen that the sulfur content of carbon-sulfur compound 1-4 is followed successively by 56%, 65%, 76%, 85%.
From figure 3, it can be seen that carbon-sulfur compound 1-3 maintains intact carbon shell spherical structure, but the structure of carbon-sulfur compound 4 is relatively low due to carbon content, has suffered to destroy.
Figure 4, it is seen that carbon-sulfur compound 1-3 is under the conditions of 0.1C discharge and recharge, maintaining good cyclical stability, carbon-sulfur compound 4 is due to structural damage, and stability test is poor.
Embodiment
2
Based on charcoal bag zinc sulfide-2, change sulfur technique processed and obtain carbon-sulfur compound-5: weigh 200mg charcoal bag zinc sulfide in containing in the 20ml ethanol 250ml flask with 10ml deionized water mixed solution, containing elemental iodine 0.9 g in solution.Subsequently 10 DEG C be stirred vigorously reaction 12h after, the solid sample of sucking filtration, 40 DEG C dry 14h.
Embodiment
3
Based on charcoal bag zinc sulfide-2, change sulfur technique processed and obtain carbon-sulfur compound-6: weigh 200mg charcoal bag zinc sulfide in containing in the 40ml ethanol 250ml flask with 10ml deionized water mixed solution, containing anhydrous sodium iodide 0.9g, ferrous sulfate heptahydrate 3.256g, elemental iodine 1.8 g in solution.Subsequently 30 DEG C be stirred vigorously reaction 18h after, the solid sample of sucking filtration, 50 DEG C dry 12h.
Embodiment
4
Based on charcoal bag zinc sulfide-2, change sulfur technique processed and obtain carbon-sulfur compound-7: weigh 200mg charcoal bag zinc sulfide, in the 250ml flask containing 10ml ethanol and 10ml deionized water mixed solution.Containing anhydrous sodium iodide 1.8 g, ferrous sulfate heptahydrate 6.512g, elemental iodine 4.8 g in solution.Subsequently 40 DEG C be stirred vigorously reaction 30h after, the solid sample of sucking filtration, 60 DEG C dry 10h.
Embodiment
5
Based on charcoal bag zinc sulfide-2, change sulfur technique processed and obtain carbon-sulfur compound-8: weigh 200mg charcoal bag zinc sulfide in containing in the 100ml ethanol 250ml flask with 10ml deionized water mixed solution, containing anhydrous sodium iodide 3.6g, ferrous sulfate heptahydrate 6.512g, elemental iodine 0.9 g in solution.Subsequently 50 DEG C be stirred vigorously reaction 36h after, the solid sample of sucking filtration, 60 DEG C dry 12h.
The thermogravimetric curve of material prepared by embodiment 2-5 is shown in Fig. 5.As can be seen from Figure 5: although change condition can successfully prepare the carbon-sulfur compound of sulfur-bearing, but the productivity of sulfur also changes with the change of condition, there is the proportioning of optimum.
Embodiment
6
One, the preparation of cadmium sulfide:
2.48g six nitric hydrate cadmium mixing 0.12g Sublimed Sulfur is dispersed in 200ml ethylene glycol, puts in the reactor that 250ml polytetrafluoro is pure, 150 DEG C, react 24h under conditions of rotating speed 600rmb/min.Standing to room temperature, dehydrated alcohol, deionized water are centrifuged each three times, dry 24h for 80 DEG C, and as shown in Figure 6, as can be seen from Figure 6 obtained cadmium sulfide particle diameter, at about 100nm, is uniformly dispersed gained cadmium sulfide pattern.
Two, prepared by charcoal cladding cadmium sulfide:
Charcoal bag cadmium sulfide: 250mg zinc sulfide mixing 25mg resorcinol, pours in 80ml ethanol, ultrasonic disperse 30min.Adding 50ul formaldehyde and the ammonia of 2ml 28%, 30 degree are stirred vigorously reaction 24h.Proceed in the reactor of 100ml polytetrafluoro liner, 100 DEG C, react 24h under conditions of rotating speed 400rmb/min.Standing to room temperature, dehydrated alcohol, deionized water are centrifuged each three times, put in tube furnace after 80 DEG C of drying 24h, and argon shield 800 DEG C processes 240min, 5 DEG C/min of heating rate.After being down to room temperature, take out and grind, stand-by.
Three, the preparation of carbon-sulfur compound:
Weigh in the 250ml flask that 200mg charcoal bag cadmium sulfide puts into 20ml ethanol and 20ml deionized water mixed solution, containing anhydrous sodium iodide 0.3g, ferrous sulfate heptahydrate 0.834g, elemental iodine 3.6g in solution.Subsequently 20 DEG C be stirred vigorously reaction 24h after, sucking filtration, 60 DEG C dry 12h, the thermogravimetric curve of gained carbon-sulfur compound 9 is shown in Fig. 7.As can be seen from Figure 7 cadmium sulfide is used to achieve the sulfur content of 65% equally as carbon-sulfur compound prepared by sulfur source.
Embodiment
7
Weigh 100mg charcoal bag zinc sulfide-2 mixing 100mg and the charcoal bag cadmium sulfide composition mixture in embodiment 6, put in the 250ml flask of 20ml ethanol and 20ml deionized water mixed solution, containing elemental iodine 3.6g in solution.Subsequently 20 DEG C be stirred vigorously reaction 24h after, sucking filtration, 60 DEG C dry 12h, the thermogravimetric curve of gained carbon-sulfur compound 10 is shown in Fig. 8.As shown in Figure 8, zinc sulfide and cadmium sulfide are simultaneously as sulfur source, for the content not impact of sulfur.
Embodiment
8
TiO2Prepared by the material of the sulfur simple substance of cladding
Weigh 145mg zinc sulfide mixing 25mg titanium chloride, pour in 80ml ethanol, ultrasonic disperse 30min.Uniformly being slowly dropped into the ammonia of 2ml 28% in 30min, 30 degree are stirred vigorously reaction 24h, stand to room temperature, and dehydrated alcohol, deionized water are centrifuged each three times, put in tube furnace after 80 DEG C of drying 24h, and argon shield 800 DEG C processes 240min, 5 DEG C/min of heating rate.After being down to room temperature, take out and grind, stand-by.
Weigh 200mg TiO2Bag zinc sulfide is put in the 250ml flask of 20ml ethanol and 20ml deionized water mixed solution, containing elemental iodine 3.6g in solution.Subsequently 20 DEG C be stirred vigorously reaction 24h after, sucking filtration, 60 DEG C dry 12h, gained TiO2The pattern of the sulfur pure metals of cladding is shown in that Fig. 9, thermogravimetric curve are shown in Figure 10.As shown in Figure 9, irregular granules the most free in product, show in the basic conditions, titanium particle and hydroxyl define uniform titanium dioxide in zinc sulfide surface recombination, are coated on its surface.As shown in Figure 10, the sulfur content of this material is 40%.
Claims (6)
1. a positive material for lithium-sulfur battery, it is characterised in that described positive electrode is internal for sulfur simple substance layer, and outside is the bivalve layer positive material for lithium-sulfur battery of surface coating layer.
Positive material for lithium-sulfur battery the most according to claim 1, it is characterised in that described surface coating layer is charcoal, inorganic conductive material, semi-conducting material or lithium ion quick conductor material.
3. the preparation method of a positive material for lithium-sulfur battery, it is characterised in that the concrete preparation process of described method is as follows:
One, the metal sulfide containing surface coating layer is dispersed in the dispersion soln containing oxidant, ferrous ion, the water of iodide ion and ethanol, stirring reaction 12-36h under conditions of 10-50 DEG C, wherein: metal sulfide is 1:2-12:0-0.5:0-1:0.5-5 with the thing mass ratio of oxidant, ferrous ion, iodide ion and water, ethanol is 1-10:1 with the volume ratio of water；
Two, reaction terminates rear sucking filtration, is vacuum dried 10-14h under the conditions of 40-60 DEG C, and obtaining internal is sulfur simple substance layer, and outside is the bivalve layer positive material for lithium-sulfur battery of surface coating layer.
The preparation method of positive material for lithium-sulfur battery the most according to claim 3, it is characterised in that the metal of described metal sulfide is the mixture of one or more in Zn, Fe, Cd, Pb, Mn.
The preparation method of positive material for lithium-sulfur battery the most according to claim 3, it is characterised in that described oxidant is elemental iodine.
The preparation method of positive material for lithium-sulfur battery the most according to claim 3, it is characterised in that described surface coating layer is charcoal, inorganic conductive material, semi-conducting material or lithium ion quick conductor material.
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Cited By (7)
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| CN106953092A (en) * | 2017-04-14 | 2017-07-14 | 哈尔滨工业大学 | A kind of preparation method of positive material for lithium-sulfur battery |
| CN108321389A (en) * | 2018-01-16 | 2018-07-24 | 浙江衡远新能源科技有限公司 | A kind of lithium ion battery carbon coating zinc sulfide nano-sphere negative material and preparation method thereof |
| CN108899493A (en) * | 2018-06-22 | 2018-11-27 | 中南大学 | A kind of nano-sulfur/metal sulfide composite material and preparation method and the application as electrode material |
| CN108963195A (en) * | 2017-05-18 | 2018-12-07 | 中国科学院宁波材料技术与工程研究所 | A kind of lithium selenium cell anode composite material and preparation method thereof |
| CN110364697A (en) * | 2018-03-26 | 2019-10-22 | 丰田自动车株式会社 | Positive electrode and the secondary cell for using the positive electrode |
| CN110635122A (en) * | 2019-09-27 | 2019-12-31 | 清华大学深圳国际研究生院 | Ultrathin folded carbon layer coated ZnS composite interlayer material and preparation method and application thereof |
| CN111584858A (en) * | 2020-05-06 | 2020-08-25 | 电子科技大学 | Lithium-sulfur battery with hollow hexagonal rod-shaped structure zinc sulfide loaded sulfur elementary substance as positive electrode material and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106953092A (en) * | 2017-04-14 | 2017-07-14 | 哈尔滨工业大学 | A kind of preparation method of positive material for lithium-sulfur battery |
| CN108963195A (en) * | 2017-05-18 | 2018-12-07 | 中国科学院宁波材料技术与工程研究所 | A kind of lithium selenium cell anode composite material and preparation method thereof |
| CN108321389A (en) * | 2018-01-16 | 2018-07-24 | 浙江衡远新能源科技有限公司 | A kind of lithium ion battery carbon coating zinc sulfide nano-sphere negative material and preparation method thereof |
| CN110364697A (en) * | 2018-03-26 | 2019-10-22 | 丰田自动车株式会社 | Positive electrode and the secondary cell for using the positive electrode |
| CN110364697B (en) * | 2018-03-26 | 2022-06-28 | 丰田自动车株式会社 | Positive electrode material and secondary battery using the same |
| CN108899493A (en) * | 2018-06-22 | 2018-11-27 | 中南大学 | A kind of nano-sulfur/metal sulfide composite material and preparation method and the application as electrode material |
| CN108899493B (en) * | 2018-06-22 | 2020-07-31 | 中南大学 | Nano sulfur/metal sulfide composite material, preparation method thereof and application of nano sulfur/metal sulfide composite material as electrode material |
| CN110635122A (en) * | 2019-09-27 | 2019-12-31 | 清华大学深圳国际研究生院 | Ultrathin folded carbon layer coated ZnS composite interlayer material and preparation method and application thereof |
| CN110635122B (en) * | 2019-09-27 | 2021-06-25 | 清华大学深圳国际研究生院 | Ultrathin folded carbon layer coated ZnS composite interlayer material and preparation method and application thereof |
| CN111584858A (en) * | 2020-05-06 | 2020-08-25 | 电子科技大学 | Lithium-sulfur battery with hollow hexagonal rod-shaped structure zinc sulfide loaded sulfur elementary substance as positive electrode material and preparation method thereof |
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Application publication date: 20160706 |