CN103904313A - Preparation method and application of tin oxide-aza graphene aerosol composite material - Google Patents
Preparation method and application of tin oxide-aza graphene aerosol composite material Download PDFInfo
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- H—ELECTRICITY
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- 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
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- H—ELECTRICITY
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- 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
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- 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
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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
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- H01M4/624—Electric conductive fillers
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- 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 discloses a preparation method of tin oxide-aza graphene aerosol composite material, and application of the tin oxide-aza graphene aerosol composite material in preparation of a negative pole of a lithium ion battery. The preparation method comprises the steps of feeding stronger ammonia water, tin source and PVP into graphene oxide water dispersion solution, evenly mixing, and carrying out hydrothermal reaction for 1-24h at the temperature of 100-300 DEG C; carrying out dialysis on the product obtained by the reaction in ultrapure water for at least one day; then, freezing a sample at the temperature of -20 DEG C for 4h, and carrying out freeze drying on the sample in the environment with the temperature of -53 DEG C and the pressure of -30Pa for at least 12h; carrying out vacuum drying on the obtained sample at the temperature of 70 DEG C for 10h; carrying out heat treatment at 550 DEG C in the argon atmosphere for 3h to obtain the tin oxide-aza graphene aerosol composite material. The aerosol composite material prepared by the method is self-support material with certain toughness and can be directly used as electrode material for assembling the battery after being simply cut and pressed, so that the complicated steps of feeding a conductive agent and an adhesive as well as preparing an electrode by the traditional pasting method can be omitted, and therefore, the cost of the lithium ion battery is lowered while a battery assembly technology is improved.
Description
Technical field
The present invention relates to a kind of preparation method and application thereof of tin oxide-azepine Graphene aerosol composite material, belong to material science and technical field of electrochemistry.
Background technology
Lithium ion battery is as a kind of energy storing device, has the features such as environmental protection, light, high power capacity, long-life.Since it realizes commercialization, through constantly perfect, its production technology is day by day ripe, is widely used in miniature portable equipment.And the especially development of hybrid electric vehicle of progress of science and technology proposes higher requirement constantly to the performance of lithium ion battery.At present, commercial lithium ion battery negative material is main mainly with carbon class material, and the theoretical capacity of material with carbon element only has 372mAhg
-1, and high rate performance is poor, also exists solvent to embed altogether the potential safety hazard of bringing, and can not meet the demand of people to battery performance and fail safe.Therefore, Novel anode material and preparation technology thereof and performance study not only have important theory significance but also have important application prospect.
Tin-based material has higher theoretical capacity and good security performance as lithium ion battery negative material, and higher natural reserves, thereby gets more and more people's extensive concerning.But tin-based material is done in the time of cycle charge discharge, to have larger bulk effect, and the destruction that can cause material structure, finally causes the quick decay of capacity.Therefore the change in volume that, alleviation tin-based material produces in the time of circulation embedding lithium, the key point that raising electrode stability becomes tin-based material research.The embedding lithium of stannic oxide materials reacts in two steps, is first reduced into simple substance tin, and then simple substance tin carries out lithiation again.First step reaction is irreversible under normal circumstances, but in the time that the size of material is reduced to nanoscale, first step reaction can be converted into reversible reaction, and therefore stannic oxide nano material capacity is expected to up to 1494mAhg
-1, the bulk effect of nano material can reduce greatly simultaneously.But fin oxide condutire is poor, and easy reunion of nano material cause a large amount of tin oxide inactivations, therefore need to be combined with the material of good conductivity to improve the structural stability of material monolithic, could effectively improve the chemical property of material.
Grapheme material has good conductivity, large specific area, high flexibility and significant chemical stability, is a kind of ideal carrier material that is applicable to electrochemical system.In lithium-ion battery system, the theoretical capacity of Graphene itself is also up to 744mAhg
-1, be also therefore the very promising lithium ion battery negative material of one.But because Graphene is a kind of two-dimensional material, the large π key of sheet interlayer easily interacts, and causes sheet of material stacking mutually, and this structure is unfavorable for the transmission of ion, can cause the active capacity of part of material to can not get performance, doubly the problem such as forthright difference.Document shows, the capacity of Graphene little its theoretical capacity conventionally far away, and decay is very fast, and therefore the structure of Graphene also needs reasonably to design.
Summary of the invention
The object of the present invention is to provide and a kind ofly prepare the method for tin oxide-azepine Graphene aerosol composite material and application in lithium ion battery negative preparation by a step hydro-thermal.The aerogel material of preparation is the self-supporting material with certain toughness, through simple cutting and compacting can be directly used in the electrode material of battery assembling, remove the loaded down with trivial details step of preparing electrode with traditional coating method that adds of conductive agent and adhesive from, thereby when having improved battery pack packing technique, also reduced the cost of lithium ion battery.
For realizing above-mentioned technical purpose, the present invention by the following technical solutions:
A preparation method for tin oxide-azepine Graphene aerosol composite material, comprises the following steps:
(1) utilize Hummers method to prepare the graphene oxide aqueous dispersions that concentration is 0.5-5mg/ml;
(2) in the graphene oxide aqueous dispersions preparing to step (1), adding mass concentration is the concentrated ammonia liquor of 25-28%, stirs, and the addition of concentrated ammonia liquor is: every 300mg graphene oxide adds 1-3ml concentrated ammonia liquor;
(3) in the solution obtaining to step (2), add Xi Yuan, stirring and dissolving, every 300mg graphene oxide adds the amount of Xi Yuan to be: 0 < tin source addition≤1g;
(4) in the solution obtaining to step (3), add polyvinylpyrrolidone (PVP), stirring and dissolving, the consumption of PVP is: every 400mg Xi Yuan adds 20-100mg PVP(Mw=55000), ultrasonic dispersion 2h;
(5) mixed liquor of step (4) is transferred in hydrothermal reaction kettle, carried out hydro-thermal reaction, hydrothermal temperature is 100-300 DEG C, reaction time 1-24h;
(6) step (5) gained sample is dialysed in ultra-pure water at least one day;
(7) by step (6) gained sample first at-20 DEG C of freezing 4h, and then in-53 DEG C, the environment of-30Pa at least 12h of freeze drying;
(8) by step (7) gained sample vacuumize 10h at 70 DEG C, then in argon gas atmosphere 550 DEG C of heat treatment 3h, to obtain final product;
Wherein, in step (3), the Xi Yuan adding is one or more in butter of tin, stannous chloride or stannous sulfate, mixes with arbitrary proportion.
Tin oxide-azepine Graphene aerosol composite material that the present invention prepares, the particle diameter of its stannic oxide materials is 5nm ± 2nm, the Capacitance reserve that circulates after 100 times is at 1100mAhg
-1, coulomb efficiency is more than 97% (except first lap).
Tin oxide-azepine Graphene aerosol composite material that the present invention prepares application in lithium ion battery negative preparation, cuts out and is pressed into required electrode film by the material direct physical of drying and moulding, can be used as electrode for lithium-ion battery system.
Graphene aerosol not only can keep the original chemical property of Graphene, and its three-dimensional porous structure also can effectively prevent that graphene nanometer sheet from adsorbing mutually, the electronics special delivery path of multidimensional is provided and shortens mass transfer distance.Therefore, tin oxide nano particle is combined with Graphene aerosol, not only be conducive to prevent that graphene nanometer sheet is mutually stacking, can also improve the poor problem of fin oxide condutire, prevent the reunion of nano particle simultaneously, the bulk effect of buffer oxide tin in cyclic process, is conducive to improve the chemical property of material.Because Graphene embedding lithium does not have obvious electromotive force platform, and Graphene is two-dimensional sheet material, unfavorable to ion diffusion in electrochemical system, and in Graphene, the element such as doping and modification boron, nitrogen can effectively improve the chemical property of material.Wherein nitrogen doping can produce a large amount of pyridine nitrogen and make material production defect, and electronics redistributes, and chemical property is improved.Electron deficient structure is conducive to lithium ion passes therein, can effectively solve the diffusion problem of ion in graphene sheet layer.
Tin oxide-azepine Graphene aerosol composite material and preparation method thereof of the present invention, the one step hydro thermal method of employing, simple to operate, mild condition, the composition of material and pattern are all easy to control, environmentally safe.Can synchronously realize the doping of the hydrolysis of Xi Yuan, the reduction of graphene oxide, aerocolloidal formation and nitrogen, and composition is controlled; The composite structure preparing is stable, and capacitance is high, can directly be used for lithium-ion battery system as electrode through simple cutting, has removed the loaded down with trivial details step that traditional coating method is prepared electrode from, has reduced production cost, can be expected to realize suitability for industrialized production.
Brief description of the drawings
Fig. 1 is the photo of tin oxide-azepine Graphene aerogel material of preparing of the embodiment of the present invention 1;
Fig. 2 is the charge-discharge performance figure of tin oxide-azepine Graphene aerogel material of preparing of the embodiment of the present invention 1.
Embodiment
Below in conjunction with embodiment, content of the present invention is described.
Embodiment 1:
It is 2mg ml that the concentrated ammonia liquor of 1.5ml is joined to 150ml concentration
-1graphene oxide aqueous dispersions in, stir 30min to mixing; Then by the PVP(Mw=55000 of 0.8g butter of tin and 160mg) join in solution, stirring and dissolving, ultrasonic dispersion 1h mixes to solution; Then mixed liquor is all transferred in hydrothermal reaction kettle, kept 160 DEG C of reaction 12h; Reaction finishes afterproduct and in ultra-pure water, dialyses at least one day; Then by sample at-20 DEG C of freezing 4h, and then at least 12h of freeze drying in-53 DEG C, the environment of-30Pa; Gained sample is vacuumize 10h at 70 DEG C, then in argon gas atmosphere 550 DEG C of heat treatment 3h, obtain tin oxide-azepine Graphene aerogel material.After measured, wherein the average grain diameter of granules of stannic oxide is 5nm, and the Capacitance reserve that circulates after 100 times is at 1100mAhg
-1left and right, coulomb efficiency is more than 97%.
Embodiment 2:
It is 0.5mg ml that the concentrated ammonia liquor of 3ml is joined to 600ml concentration
-1graphene oxide aqueous dispersions in, stir 30min to mixing; Then by the PVP(Mw=55000 of 1.0g butter of tin and 250mg) join in solution, stirring and dissolving, ultrasonic dispersion 1h mixes to solution; Then mixed liquor is all transferred in hydrothermal reaction kettle, kept 100 DEG C of reaction 24h; Reaction finishes afterproduct and in ultra-pure water, dialyses at least one day; Then by sample at-20 DEG C of freezing 4h, and then at least 12h of freeze drying in-53 DEG C, the environment of-30Pa; Gained sample is vacuumize 10h at 70 DEG C, then in argon gas atmosphere 550 DEG C of heat treatment 3h, obtain tin oxide-azepine Graphene aerogel material.After measured, the average grain diameter of its stannic oxide materials is 4nm, and the Capacitance reserve that circulates after 100 times is at 920mAhg
-1left and right, coulomb efficiency is more than 97%.
Embodiment 3:
It is 3mg ml that the concentrated ammonia liquor of 1.5ml is joined to 100ml concentration
-1graphene oxide aqueous dispersions in, stir 30min to mixing; Then by the PVP(Mw=55000 of 0.6g stannous sulfate and 75mg) join in solution, stirring and dissolving, ultrasonic dispersion 1h mixes to solution; Then mixed liquor is all transferred in hydrothermal reaction kettle, kept 180 DEG C of reaction 8h; Reaction finishes afterproduct and in ultra-pure water, dialyses at least one day; Then by sample at-20 DEG C of freezing 4h, and then at least 12h of freeze drying in-53 DEG C, the environment of-30Pa; Gained sample is vacuumize 10h at 70 DEG C, then in argon gas atmosphere 550 DEG C of heat treatment 3h, obtain tin oxide-azepine Graphene aerogel material.After measured, the average grain diameter of its stannic oxide materials is 5nm, and the Capacitance reserve that circulates after 100 times is at 1040mAhg
-1left and right, coulomb efficiency is more than 97%.
Embodiment 4:
It is 5mg ml that the concentrated ammonia liquor of 1ml is joined to 60ml concentration
-1graphene oxide aqueous dispersions in, stir 30min to mixing; Then by the PVP(Mw=55000 of 0.5g stannous chloride and 25mg) join in solution, stirring and dissolving, ultrasonic dispersion 1h mixes to solution; Then mixed liquor is all transferred in hydrothermal reaction kettle, kept 300 DEG C of reaction 1h; Reaction finishes afterproduct and in ultra-pure water, dialyses at least one day; Then by sample at-20 DEG C of freezing 4h, and then at least 12h of freeze drying in-53 DEG C, the environment of-30Pa; Gained sample is vacuumize 10h at 70 DEG C, then in argon gas atmosphere 550 DEG C of heat treatment 3h, obtain tin oxide-azepine Graphene aerogel material.After measured, the average grain diameter of its stannic oxide materials is 7nm, and the Capacitance reserve that circulates after 100 times is at 1000mAhg
-1left and right, coulomb efficiency is more than 97%.
By reference to the accompanying drawings the specific embodiment of the present invention is described although above-mentioned; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendments that creative work can make or distortion still in protection scope of the present invention.
Claims (5)
1. a preparation method for tin oxide-azepine Graphene aerosol composite material, is characterized in that, comprises the following steps:
(1) utilize Hummers method to prepare the graphene oxide aqueous dispersions that concentration is 0.5-5mg/ml;
(2) in the graphene oxide aqueous dispersions preparing to step (1), add concentrated ammonia liquor, stir, the amount of concentrated ammonia liquor is: every 300mg graphene oxide adds 1-3ml concentrated ammonia liquor;
(3) in the solution obtaining to step (2), add Xi Yuan, stirring and dissolving, every 300mg graphene oxide adds the amount of Xi Yuan to be: 0 < tin source addition≤1g;
(4) in the solution obtaining to step (3), adding mean molecule quantity is 55000 PVP, stirring and dissolving, and the consumption of PVP is: every 400mg Xi Yuan adds 20-100mg PVP, ultrasonic dispersion 2h;
(5) mixed liquor of step (4) is transferred in hydrothermal reaction kettle, carried out hydro-thermal reaction, hydrothermal temperature is 100-300 DEG C, reaction time 1-24h;
(6) step (5) gained sample is dialysed in ultra-pure water at least one day;
(7) by step (6) gained sample first at-20 DEG C of freezing 4h, and then at least 12h of freeze drying in-53 DEG C, the environment of-30Pa;
(8) by step (7) gained sample vacuumize 10h at 70 DEG C, then in argon gas atmosphere 550 DEG C of heat treatment 3h, to obtain final product;
Wherein, in step (3), the Xi Yuan adding is one or more in butter of tin, stannous chloride or stannous sulfate, mixes with arbitrary proportion.
2. the preparation method of a kind of tin oxide-azepine Graphene aerosol composite material as claimed in claim 1, is characterized in that, the concentrated ammonia liquor of 1.5ml is joined in the graphene oxide aqueous dispersions that 150ml concentration is 2mg/ml, stirs 30min to mixing; Then the PVP that is 55000 by the mean molecule quantity of 0.8g butter of tin and 160mg joins in solution, stirring and dissolving, and ultrasonic dispersion 1h mixes to solution; Then mixed liquor is all transferred in hydrothermal reaction kettle, kept 160 DEG C of reaction 12h; Reaction finishes afterproduct and in ultra-pure water, dialyses at least one day; Then by sample at-20 DEG C of freezing 4h, and then in-53 DEG C, the environment of-30Pa at least 12h of freeze drying; Gained sample is vacuumize 10h at 70 DEG C, then in argon gas atmosphere 550 DEG C of heat treatment 3h, obtain tin oxide-azepine Graphene aerogel material.
3. tin oxide-azepine Graphene aerosol composite material that preparation method claimed in claim 1 prepares, is characterized in that, the particle diameter of its stannic oxide nano material is 5nm ± 2nm, and the Capacitance reserve that circulates after 100 times is at 1100mAhg
-1, coulomb efficiency is higher than 97%.
4. tin oxide-azepine Graphene aerosol composite material claimed in claim 3 is in the application of preparing in lithium ion battery negative material.
5. tin oxide-azepine Graphene aerosol composite material as claimed in claim 4 is in the application of preparing in lithium ion battery negative material, it is characterized in that, required electrode film is cut out and be pressed into tin oxide-azepine Graphene aerosol composite material direct physical of drying and moulding.
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CN104659345A (en) * | 2015-02-06 | 2015-05-27 | 中国石油大学(华东) | Composite martial for lithium battery and button battery prepared from composite martial |
CN105185956A (en) * | 2015-06-19 | 2015-12-23 | 合肥国轩高科动力能源有限公司 | Sponge-like silicon graphene and carbon nano-tube composite negative electrode material preparation method |
CN112151780A (en) * | 2020-09-21 | 2020-12-29 | 江苏塔菲尔新能源科技股份有限公司 | Nano lithium iron phosphate/graphene oxide composite material and preparation method and application thereof |
CN112903762A (en) * | 2021-02-09 | 2021-06-04 | 建木柔电(深圳)智能设备有限公司 | Carbon monoxide gas sensor based on graphene aerosol material |
CN114392730A (en) * | 2022-01-11 | 2022-04-26 | 河南康宁特环保科技股份有限公司 | Preparation method of high-dispersion hierarchical pore Ti-based SCR catalyst |
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CN104659345A (en) * | 2015-02-06 | 2015-05-27 | 中国石油大学(华东) | Composite martial for lithium battery and button battery prepared from composite martial |
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CN105185956B (en) * | 2015-06-19 | 2018-01-12 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of spongy 3 SiC 2/graphite alkene and CNT composite negative pole material |
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CN112903762A (en) * | 2021-02-09 | 2021-06-04 | 建木柔电(深圳)智能设备有限公司 | Carbon monoxide gas sensor based on graphene aerosol material |
CN114392730A (en) * | 2022-01-11 | 2022-04-26 | 河南康宁特环保科技股份有限公司 | Preparation method of high-dispersion hierarchical pore Ti-based SCR catalyst |
CN114392730B (en) * | 2022-01-11 | 2023-09-12 | 河南康宁特环保科技股份有限公司 | Preparation method of high-dispersion hierarchical pore Ti-based SCR catalyst |
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