CN106784663A - A kind of preparation method of the compound carbon cloth anode material of lithium-ion battery of antimony oxide - Google Patents

A kind of preparation method of the compound carbon cloth anode material of lithium-ion battery of antimony oxide Download PDF

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Publication number
CN106784663A
CN106784663A CN201611110077.XA CN201611110077A CN106784663A CN 106784663 A CN106784663 A CN 106784663A CN 201611110077 A CN201611110077 A CN 201611110077A CN 106784663 A CN106784663 A CN 106784663A
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carbon cloth
solution
lithium
anode material
ion battery
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费杰
崔亚丽
陈俊生
雒玉欣
韩瑞雪
黄剑锋
李嘉胤
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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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
    • 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
    • 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
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • 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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • 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
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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 preparation method of the compound carbon cloth anode material of lithium-ion battery of a kind of antimony oxide, by analytically pure SbCl3It is completely dissolved in ethanol, is subsequently adding a small amount of NaOH solution, stirring obtains colloidal sol, is designated as solution A；Take carbon cloth and be soaked in solution A, then take out drying；Carbon cloth after drying is soaked into solution A again, and adjusts PH to 8~9；Precursor liquid and carbon cloth are transferred into reactor to be reacted, reaction takes out carbon cloth after terminating, are cleaned with water and ethanol and dried after ultrasound, obtain Sb2O3CC anode material of lithium-ion batteries；The present invention prepares sodium-ion battery anode material Sb using solvent-thermal method2O3CC, simple to operate easy to control, short preparation period, product good dispersion is environmentally friendly；Products therefrom chemical composition is homogeneous, and good crystallinity, pattern is homogeneous, has been effectively combined the advantage of carbon cloth and antimony oxide, i.e., simultaneously there is specific capacity higher to keep preferable cycle characteristics again.

Description

A kind of preparation method of the compound carbon cloth anode material of lithium-ion battery of antimony oxide
Technical field
The present invention relates to a kind of antimony oxide and carbon cloth composite (Sb2O3- CC) preparation method, and in particular to a kind of oxygen Change the preparation method of the compound carbon cloth anode material of lithium-ion battery of antimony.
Background technology
Energy and environment problem is two hang-ups that mankind nowadays social sustainable development faces.In environmental pollution increasingly Serious today, fossil fuel just seriously threatens our health due to a large amount of harmful substances that burning is produced.Progressively break away from Dependence of the human development to fossil fuel, improves the ecological environment of the earth, accelerates cleaning, renewable energy utilization and is developed into The common recognition of today's society.In recent years in a series of great new energy technologies development, such as energy-accumulating power station, electric automobile are secondary Battery is subject to special attention as simple efficient energy-storage system, it might even be possible to be considered as the crucial skill of above-mentioned application development Art.Lithium ion battery has that energy density is high, has extended cycle life, operating voltage is high, memory-less effect, self discharge are small, work temperature The advantages of degree wide ranges, it is considered to be most promising electrochmical power source, the work of various electronic products is widely used as at present Electrokinetic cell (electric motor car, submarine, the MISSILE LAUNCHING of power supply (mobile phone, notebook computer, digital camera etc.) and portable outfit Deng).But, global lithium resource is not rich, and elemental lithium abundance in the earth's crust is only 0.006% and skewness, lithium source price It is high to turn into the key factor for limiting its development；Simultaneously as the safety issue of lithium ion battery itself, is also practicality Change brings certain difficulty.Therefore, the excellent energy-storage battery new system of development comprehensive effectiveness of future generation is needed badly.
Sodium and lithium are in same main group, and with similar electrochemical properties, and sodium has great economic advantages, its Abundance in the earth's crust reaches 2.6%, is paid close attention at beginning of the eighties late 1970s, with electric automobile, intelligent grid The arrival in epoch, the battery for realizing charging repeatedly, discharging using sodium ion, because sodium resource reserve is abundant and easily realizes low Cost is produced, and the battery of future generation for substituting lithium ion battery is considered as by part expert.
Carbon cloth is high intensity, the new fiber materials of high modulus fibre of a kind of phosphorus content more than 95%.It is by piece The organic fibers such as shape graphite microcrystal are piled up along fiber axial direction and are formed, through micro crystal graphite obtained from carbonization and graphitization processing Material.It not only has the intrinsic intrinsic property of carbon material, and the soft machinability of textile fabric is had both again, is enhancing of new generation Fiber.Carbon cloth has many premium properties, and the axial strength and modulus of carbon cloth are high, and density is low, higher than performance, without creep, non-oxygen Change superhigh temperature resistant under environment, fatigue durability is good, between nonmetallic and metal between, thermal coefficient of expansion is small and tool for specific heat and electric conductivity There is anisotropy, good corrosion resistance, X-ray transparent is good, good electrical and thermal conductivity performance etc..As flexible current-collecting body, carbon cloth Cloth not only have more than excellent chemical property, the advantages of be also equipped with high mechanical strength.
Sb2O3Nano semiconductor material band gap very little, under relatively low electric-field intensity, electronics can just reach saturation Drift velocity, with excellent photoelectric conversion characteristic, charge transfer speed higher, steady in a long-term, response rapidly, repeatedly Property good, cheap, theoretical specific capacity up to 1103mAh/g, the antimony oxide prepared by various effective ways and its multiple Condensation material is used as anode material of lithium-ion battery, the advantage of good cycling stability high with specific capacity, while low manufacture cost, It is suitable to sodium-ion battery large-scale development with application.
The content of the invention
It is an object of the invention to provide a kind of technical process it is simple, reaction time is short, materials chemistry constitute homogeneous, pattern The Sb of size uniform and good cycling stability2O3The preparation method of-CC anode material of lithium-ion batteries.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：
1) take during 0.30-1.00g NaOH are dissolved completely in 10ml distilled water and obtain NaOH solution, then take 0.14~0.32g SbCl3It is dissolved completely in 40~50ml ethanol to obtain SbCl3Solution, to SbCl under magnetic agitation3A small amount of NaOH is added dropwise in solution molten Liquid obtains colloidal sol, is designated as solution A；
2) carbon cloth is soaked in solution A, then takes out drying；
3) carbon cloth after drying is soaked into solution A again, and adjusts solution and carbon cloth are transferred to reaction after PH to 8~9 Kettle, 120 DEG C~180 DEG C of reaction temperature, 3~24h of time；
4) carbon cloth is taken out, is cleaned with water and ethanol and is dried after ultrasound, obtain Sb2O3- CC anode material of lithium-ion batteries.
The present invention prepares sodium-ion battery anode material Sb using solvent-thermal method2O3- CC, it is simple to operate easy to control, prepare week Phase is short, product good dispersion, environmentally friendly.Products therefrom chemical composition is homogeneous, and good crystallinity, pattern is homogeneous, effectively ties The advantage of carbon cloth and antimony oxide is closed, i.e., simultaneously there is specific capacity higher to keep preferable cycle characteristics again.
Brief description of the drawings
Fig. 1 is Sb prepared by the embodiment of the present invention 12O3The XRD spectrum of compound carbon cloth anode material of lithium-ion battery.
Fig. 2, Fig. 3 are Sb prepared by the embodiment of the present invention 42O3The SEM photograph of compound carbon cloth anode material of lithium-ion battery.
Fig. 4 is Sb prepared by the embodiment of the present invention 62O3Compound carbon cloth anode material of lithium-ion battery is in 0.01~3.00V electricity Between pressure, 132mAg-1Under current density, the charge-discharge performance figure that circulation is 50 times.
Specific embodiment
Below in conjunction with the accompanying drawings and embodiment is described in further detail to the present invention：
Embodiment 1：
1) take during 1.00g NaOH are dissolved completely in 10ml distilled water and obtain NaOH solution, then take 0.32g SbCl3It is completely molten Solution obtains SbCl in 40ml ethanol3Solution, to SbCl under magnetic agitation3A small amount of NaOH solution is added dropwise in solution and obtains colloidal sol, be designated as Solution A；
2) carbon cloth is soaked in solution A, then takes out drying；
3) carbon cloth after drying is soaked into solution A again, and adjusts solution and carbon cloth are transferred to reaction after PH to 8~9 Kettle, 120 DEG C of reaction temperature, time 6h；
4) carbon cloth is taken out, is cleaned with water and ethanol and is dried after ultrasound, obtain Sb2O3- CC anode material of lithium-ion batteries.
It can be seen from figure 1 that the Sb grown on carbon cloth2O3It is oblique side's phase, crystallinity is preferable.
Embodiment 2：
1) take during 0.60g NaOH are dissolved completely in 10ml distilled water and obtain NaOH solution, then take 0.28g SbCl3It is completely molten Solution obtains SbCl in 40ml ethanol3Solution, to SbCl under magnetic agitation3A small amount of NaOH solution is added dropwise in solution and obtains colloidal sol, be designated as Solution A；
2) carbon cloth is soaked in solution A, then takes out drying；
3) carbon cloth after drying is soaked into solution A again, and adjusts solution and carbon cloth are transferred to reaction after PH to 8~9 Kettle, 150 DEG C of reaction temperature, time 6h；
4) carbon cloth is taken out, is cleaned with water and ethanol and is dried after ultrasound, obtain Sb2O3- CC anode material of lithium-ion batteries.
Embodiment 3：
1) take during 0.80g NaOH are dissolved completely in 10ml distilled water and obtain NaOH solution, then take 0.28g SbCl3It is completely molten Solution obtains SbCl in 40ml ethanol3Solution, to SbCl under magnetic agitation3A small amount of NaOH solution is added dropwise in solution and obtains colloidal sol, be designated as Solution A；
2) carbon cloth is soaked in solution A, then takes out drying；
3) carbon cloth after drying is soaked into solution A again, and adjusts solution and carbon cloth are transferred to reaction after PH to 8~9 Kettle, 180 DEG C of reaction temperature, time 6h；
4) carbon cloth is taken out, is cleaned with water and ethanol and is dried after ultrasound, obtain Sb2O3- CC anode material of lithium-ion batteries.
Embodiment 4：
1) take during 0.30g NaOH are dissolved completely in 10ml distilled water and obtain NaOH solution, then take 0.14g SbCl3It is completely molten Solution obtains SbCl in 50ml ethanol3Solution, to SbCl under magnetic agitation3A small amount of NaOH solution is added dropwise in solution and obtains colloidal sol, be designated as Solution A；
2) carbon cloth is soaked in solution A, then takes out drying；
3) carbon cloth after drying is soaked into solution A again, and adjusts solution and carbon cloth are transferred to reaction after PH to 8~9 Kettle, 150 DEG C of reaction temperature, time 12h；
4) carbon cloth is taken out, is cleaned with water and ethanol and is dried after ultrasound, obtain Sb2O3- CC anode material of lithium-ion batteries.
The composite from Fig. 2,3 as can be seen that as obtained in this method, the Sb grown on carbon cloth2O3For nanometer is spherical, Growth fraction is more uniform, and associativity is good.
Embodiment 5：
1) take during 0.50g NaOH are dissolved completely in 10ml distilled water and obtain NaOH solution, then take 0.14g SbCl3It is completely molten Solution obtains SbCl in 50ml ethanol3Solution, to SbCl under magnetic agitation3A small amount of NaOH solution is added dropwise in solution and obtains colloidal sol, be designated as Solution A；
2) carbon cloth is soaked in solution A, then takes out drying；
3) carbon cloth after drying is soaked into solution A again, and adjusts solution and carbon cloth are transferred to reaction after PH to 8~9 Kettle, 150 DEG C of reaction temperature, time 24h；
4) carbon cloth is taken out, is cleaned with water and ethanol and is dried after ultrasound, obtain Sb2O3- CC anode material of lithium-ion batteries.
Embodiment 6：
1) take during 0.30g NaOH are dissolved completely in 10ml distilled water and obtain NaOH solution, then take 0.14g SbCl3It is completely molten Solution obtains SbCl in 50ml ethanol3Solution, to SbCl under magnetic agitation3A small amount of NaOH solution is added dropwise in solution and obtains colloidal sol, be designated as Solution A；
2) carbon cloth is soaked in solution A, then takes out drying；
3) carbon cloth after drying is soaked into solution A again, and adjusts solution and carbon cloth are transferred to reaction after PH to 8~9 Kettle, 150 DEG C of reaction temperature, time 3h；
4) carbon cloth is taken out, is cleaned with water and ethanol and is dried after ultrasound, obtain Sb2O3- CC anode material of lithium-ion batteries.
As can be seen from Figure 4 battery is in 50mAg-1First discharge specific capacity is 272.13mAhg under current density-1, it Some declines of specific discharge capacity several times, tend to be steady after about 10 times afterwards, and final specific discharge capacity is approximately kept at 200mAhg-1Left and right.

Claims (1)

1. a kind of antimony oxide is combined the preparation method of carbon cloth anode material of lithium-ion battery, it is characterised in that：
1) take during 0.30-1.00g NaOH are dissolved completely in 10ml distilled water and obtain NaOH solution, then take 0.14~0.32g SbCl3 It is dissolved completely in 40~50ml ethanol to obtain SbCl3Solution, to SbCl under magnetic agitation3NaOH solution is added dropwise in solution and obtains molten Glue, is designated as solution A；
2) carbon cloth is soaked in solution A, then takes out drying；
3) carbon cloth after drying is soaked into solution A again, and adjusts solution and carbon cloth are transferred to reactor after PH to 8~9, instead Answer 120 DEG C~180 DEG C of temperature, 3~24h of time；
4) carbon cloth is taken out, is cleaned with water and ethanol and is dried after ultrasound, obtain Sb2O3- CC anode material of lithium-ion batteries.
CN201611110077.XA 2016-12-06 2016-12-06 A kind of preparation method of the compound carbon cloth anode material of lithium-ion battery of antimony oxide Pending CN106784663A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108470882A (en) * 2018-03-30 2018-08-31 江汉大学 Tin oxide is modified carbon cloth base lithium and sodium metal negative electrode and preparation method thereof
CN110190246A (en) * 2019-06-24 2019-08-30 陕西科技大学 A kind of Sb2O3The preparation method of/carbon felt flexibility anode material of lithium-ion battery
CN110265643A (en) * 2019-06-24 2019-09-20 陕西科技大学 A kind of Sb2O5The preparation method of/carbon cloth flexibility anode material of lithium-ion battery
CN110265644A (en) * 2019-06-24 2019-09-20 陕西科技大学 A kind of preparation method of antimony pentoxide/polyacrylic acid of reticulated porous structures/carbon cloth flexibility anode material of lithium-ion battery
CN110277550A (en) * 2019-06-24 2019-09-24 陕西科技大学 A kind of different valence state and crystal form sb oxide/carbon cloth make the preparation method of flexible anode material of lithium-ion battery
CN110565362A (en) * 2019-09-24 2019-12-13 陕西科技大学 Preparation method of carbon cloth material loaded with antimony pentoxide with different morphologies and application of carbon cloth material to negative electrode of sodium-ion battery

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
王青尧: "锑基纳米材料的水热法制备及表征", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108470882A (en) * 2018-03-30 2018-08-31 江汉大学 Tin oxide is modified carbon cloth base lithium and sodium metal negative electrode and preparation method thereof
CN110190246A (en) * 2019-06-24 2019-08-30 陕西科技大学 A kind of Sb2O3The preparation method of/carbon felt flexibility anode material of lithium-ion battery
CN110265643A (en) * 2019-06-24 2019-09-20 陕西科技大学 A kind of Sb2O5The preparation method of/carbon cloth flexibility anode material of lithium-ion battery
CN110265644A (en) * 2019-06-24 2019-09-20 陕西科技大学 A kind of preparation method of antimony pentoxide/polyacrylic acid of reticulated porous structures/carbon cloth flexibility anode material of lithium-ion battery
CN110277550A (en) * 2019-06-24 2019-09-24 陕西科技大学 A kind of different valence state and crystal form sb oxide/carbon cloth make the preparation method of flexible anode material of lithium-ion battery
CN110565362A (en) * 2019-09-24 2019-12-13 陕西科技大学 Preparation method of carbon cloth material loaded with antimony pentoxide with different morphologies and application of carbon cloth material to negative electrode of sodium-ion battery

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Application publication date: 20170531