CN104362319A - Preparation method of porous tin-carbon composite negative material - Google Patents
Preparation method of porous tin-carbon composite negative material Download PDFInfo
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- CN104362319A CN104362319A CN201410674911.2A CN201410674911A CN104362319A CN 104362319 A CN104362319 A CN 104362319A CN 201410674911 A CN201410674911 A CN 201410674911A CN 104362319 A CN104362319 A CN 104362319A
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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
- H01M4/364—Composites as mixtures
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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
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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
- 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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/134—Electrodes based on metals, Si or alloys
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/387—Tin or alloys based on tin
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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
- H01M4/58—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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- 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
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Abstract
The invention belongs to the technical field of batteries, and particularly relates to a preparation method of a porous tin-carbon composite negative material, a composite material prepared through the method and a corresponding battery. The preparation method comprises the following steps of: firstly loading tin oxide, a carbon source and carbonate into a ball-milling tank according to the stoichiometric ratio, and carrying out ball-milling mixing to obtain a precursor; then placing the precursor into a flowing inert atmosphere, and calcining in a tube furnace; finally washing and drying an obtained calcined product to obtain the porous tin-carbon composite negative material. The porous tin-carbon composite negative material obtained through the method disclosed by the invention has the advantages of high capacity, excellent electrochemical property, low cost, simple production process and easiness for operation.
Description
Technical field
The invention belongs to cell art, be specifically related to a kind of preparation method of porous tin carbon compound cathode materials and composite material obtained by this method thereof and corresponding battery thereof.
Background technology
Owing to having, operating voltage is high, energy density is large, fail safe is high for lithium ion battery, and self discharge is low, have extended cycle life and the advantage such as memory-less effect, is widely used in consumer and power type electronic product.But limited lithium resource reserves and high material cost thereof are its extensive use brings huge obstacle.The advanced battery system that development resource is enriched, with low cost and fail safe is high is the inevitable outlet solving Future New Energy Source development.Sodium element and lithium are in same main group, and chemical property is similar, and also relatively, and the aboundresources of sodium, refines cost also low than lithium to electrode potential.If substitute lithium with sodium, develop the sodium-ion battery of excellent working performance, it will have the competitive advantage larger than lithium ion battery.Anode material of lithium-ion battery conventional is at present hard carbon material, but its theoretical specific capacity is lower, cycle life is poor, is easy to the problems such as sodium dendrite precipitation occur, and the sodium electrode material seeking high power capacity and excellent cycling performance has become the study hotspot in current battery field.
In recent years, large quantifier elimination has turned to the Novel anode material system found and can substitute material with carbon element, and tin-based material becomes candidate material.Tin base cathode material, not only there is environmental friendliness, higher theoretical specific capacity (847mAh/g), several times and even the decades of times of hard carbon class negative material, and content comparatively abundant (in the earth's crust, abundance is 2.2ppm) in the earth's crust, be considered to the desirable negative material of high-energy-density sodium-ion battery.But the change in volume of tin base cathode material in embedding de-sodium process is very large, very easily causes electrode efflorescence, structural collapse, thus loses electro-chemical activity, causes it cannot directly be used as sodium-ion battery negative pole and use.For adapting to high-energy-density sodium-ion battery development need, anode material of lithium-ion battery of new generation must be developed.
Summary of the invention
In order to solve the problem, the object of the invention is to, provide a kind of low cost, technique simple, being applicable to the preparation method of the porous tin carbon composite of large-scale production;
Two of object of the present invention is the porous tin carbon composite providing described method obtained;
Three of object of the present invention is the negative pole providing described porous tin carbon composite obtained;
Four of object of the present invention is to provide the sodium-ion battery and lithium ion battery that comprise the negative pole that described porous tin carbon composite obtains.
The present invention is achieved through the following technical solutions:
A preparation method for porous tin carbon composite, is characterized in that, comprises following preparation process:
A. by tin oxide, carbon source and carbonate according to metering than loading ball grinder, with 200 ~ 400 revs/min of ball millings 0.5 ~ 12 hour, obtain mixing presoma;
B. presoma is placed in slumpability atmosphere in devices such as tube furnaces, is warming up to 500 ~ 1000 DEG C with 2 ~ 5 DEG C/min of heating rates, be incubated 1 ~ 6 hour, cool to room temperature with the furnace;
C. the calcined product washing obtained for several times, 50 ~ 100 DEG C of oven dry, obtains described porous tin carbon negative pole material.
Preferably, described carbonate is one or both compositions in sodium carbonate, lithium carbonate.
Preferably, described carbon source is one or more compositions in sucrose, glucose, acetylene black, conductive black, graphite.
Preferably, in described tin carbon composite, tin accounting example is 20 ~ 95%.
Preferably, by the washing of centrifugal or filter type for several times, solvent for use is one or more in water, ethanol, methyl alcohol to described calcined product.
A kind of battery cathode, comprises the porous tin carbon composite that described preparation method obtains.
A kind of sodium-ion battery, contains described high power capacity porous tin Carbon anode.
A kind of lithium ion battery, contains described high power capacity porous tin Carbon anode.
The present invention utilizes simple ball milling-calcining-oven dry preparation porous tinbase composite negative pole material, on the one hand, because the present invention adopts tin oxide, the wherein redox reaction of carbon and tin oxide, therefore the material mixing obtained as raw material relative to pure phase simple substance evenly, not easily have impurity to occur, and the material that finally can synthesize is the coated tin composite material of carbon of porous.On the other hand, the carbon source of employing is sucrose, glucose, acetylene black, conductive black, graphite, and these raw material are widely distributed at occurring in nature, cheap, environmental protection; Adopt several kinds of carbon source (sucrose, glucose, acetylene black, conductive black, graphite) to carry out reduction-oxidation tin simultaneously, the tin carbon composite of in-stiu coating can be obtained.Especially introduce carbonate (sodium carbonate, lithium carbonate), utilize it in presoma high-temperature reaction process, decompose carbon dioxide and wash removing catabolite oxide with water, making final tin carbon composite reach the structure of porous.Especially it can be used as the negative material of sodium-ion battery, because it has loose structure, make its change in volume in embedding de-sodium process little, electrode efflorescence can not be caused, structural collapse, thus lose electro-chemical activity.Can directly be used as sodium-ion battery negative pole to use, adapt to high-energy-density sodium-ion battery development need.Certainly, also can use as the negative pole of lithium ion battery.
Accompanying drawing explanation
Fig. 1 is porous tin carbon composite charge-discharge property figure of the present invention.
concrete execution mode
Below in conjunction with embodiment, the present invention is described in further detail, understands the present invention to help those skilled in the art.
Embodiment 1
The preparation method of porous tin carbon composite, comprises following preparation process:
A. tin oxide, sucrose and sodium carbonate are loaded ball grinder according to amount of substance=1:1:1, with 300 revs/min of ball millings 4 hours, obtain mixing presoma;
B. presoma is placed in flowing nitrogen atmosphere in devices such as tube furnaces, is warming up to 600 DEG C with 3 DEG C/min of heating rates, be incubated 6 hours, cool to room temperature with the furnace;
C. the calcined product deionized water obtained washes rear centrifugation, and washing for several times, 80 DEG C of oven dry, obtains porous tin carbon composite.
Embodiment 2
The preparation method of porous tin carbon composite, comprises following preparation process:
A. tin oxide, glucose and lithium carbonate are loaded ball grinder according to amount of substance=0.6:1.2:1.2, with 400 revs/min of ball millings 1 hour, obtain mixing presoma;
B. presoma is placed in flowing nitrogen atmosphere in devices such as tube furnaces, is warming up to 500 DEG C with 5 DEG C/min of heating rates, be incubated 1 hour, cool to room temperature with the furnace;
C. the calcined product deionized water obtained washes rear centrifugation, and washing for several times, 50 DEG C of oven dry, obtains porous tin carbon composite.
Embodiment 3
The preparation method of porous tin carbon composite, comprises following preparation process:
A. tin oxide, graphite and sodium carbonate are loaded ball grinder according to amount of substance=2.8:0.1:0.1, with 200 revs/min of ball millings 12 hours, obtain mixing presoma;
B. presoma is placed in flowing nitrogen atmosphere in devices such as tube furnaces, is warming up to 1000 DEG C with 2 DEG C/min of heating rates, be incubated 3 hours, cool to room temperature with the furnace;
C. the calcined product deionized water obtained washes rear centrifugation, and washing for several times, 100 DEG C of oven dry, obtains porous tin carbon composite.
Embodiment 4
The preparation method of porous tin carbon composite, comprises following preparation process:
A. tin oxide, glucose, acetylene black, sodium carbonate and lithium carbonate are loaded ball grinder according to amount of substance=1.5:0.5:0.25:0.5:0.25, with 250 revs/min of ball millings 18 hours, obtain mixing presoma;
B. presoma is placed in flowing nitrogen atmosphere in devices such as tube furnaces, is warming up to 800 DEG C with 3 DEG C/min of heating rates, be incubated 4 hours, cool to room temperature with the furnace;
C. the calcined product deionized water obtained washes rear centrifugation, and washing for several times, 700 DEG C of oven dry, obtains porous tin carbon composite.
Embodiment 5
The preparation method of porous tin carbon composite, comprises following preparation process:
A. tin oxide, sucrose, glucose, conductive black, graphite and sodium carbonate are loaded ball grinder according to amount of substance=2:1:0.1:0.1:0.1:0.1:0.6, with 350 revs/min of ball millings 5 hours, obtain mixing presoma;
B. presoma is placed in flowing nitrogen atmosphere in devices such as tube furnaces, is warming up to 800 DEG C with 4 DEG C/min of heating rates, be incubated 4 hours, cool to room temperature with the furnace;
C. the calcined product deionized water obtained washes rear centrifugation, and washing for several times, 60 DEG C of oven dry, obtains porous tin carbon composite.
Above-described embodiment, just preferred embodiment of the present invention, not exhaustive; Not be used for limiting the scope of the present invention, therefore all equivalences done with the feature described in the claims in the present invention and principle change or modify, and all should be included within the claims in the present invention scope.
Claims (9)
1. a preparation method for porous tin carbon composite, is characterized in that, comprises following preparation process:
A. by tin oxide, carbon source and carbonate according to metering than loading ball grinder, with 200 ~ 400 revs/min of ball millings 0.5 ~ 12 hour, obtain mixing presoma;
B. presoma is placed in slumpability atmosphere in tube furnace, is warming up to 500 ~ 1000 DEG C with 2 ~ 5 DEG C/min of heating rates, be incubated after 1 ~ 6 hour, cool to room temperature with the furnace;
C. the calcined product obtained in B is washed, 50 ~ 100 DEG C of oven dry, obtain described porous tin carbon composite.
2. the preparation method of porous tin carbon composite as claimed in claim 1, it is characterized in that, described carbonate is one or both compositions in sodium carbonate, lithium carbonate.
3. the preparation method of porous tin carbon composite as claimed in claim 1, it is characterized in that, described carbon source is one or more compositions in sucrose, glucose, acetylene black, conductive black, graphite.
4. the preparation method of porous tin carbon composite as claimed in claim 1, it is characterized in that, in described tin carbon composite, the weight ratio of tin is 20 ~ 95%.
5. the preparation method of porous tin carbon composite as claimed in claim 1, is characterized in that, described calcined product by centrifugal or filter type washing for several times.
6. the preparation method of porous tin carbon composite as claimed in claim 5, is characterized in that, cleaning solvent used is one or more in water, ethanol, methyl alcohol.
7. a battery cathode, is characterized in that, comprises the porous tin carbon composite that preparation method described in any one in claim 1-6 obtains.
8. a sodium-ion battery, is characterized in that, contains the porous of high power capacity described in claim 7 tin Carbon anode.
9. a lithium ion battery, is characterized in that, contains the porous of high power capacity described in claim 7 tin Carbon anode.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104766962A (en) * | 2015-04-17 | 2015-07-08 | 辽宁工程技术大学 | Preparation method of carbon-cladding graphite oxide/Sn composite cathode material of lithium ion battery |
| CN105406065A (en) * | 2015-11-30 | 2016-03-16 | 安泰科技股份有限公司 | SnS2-C negative electrode nanocomposite and preparation method and application therefor |
| CN105655557A (en) * | 2016-01-18 | 2016-06-08 | 浙江大学 | Preparation method of carbon-wrapping-tin nanometer material with carbon shells not completely filled with tin |
| CN106784736A (en) * | 2017-02-08 | 2017-05-31 | 大连理工大学 | A kind of sodium-ion battery negative pole coats the preparation method and application of tin particles nanometer sheet with coal tar pitch resin base amorphous carbon |
| CN108140818A (en) * | 2015-10-06 | 2018-06-08 | 法拉典有限公司 | A kind of method for being used to prepare hard carbon composite material |
| CN109411717A (en) * | 2018-09-28 | 2019-03-01 | 华南理工大学 | A kind of negative electrode material and preparation method thereof through prelithiation with high reversible capacity |
| CN111531181A (en) * | 2020-05-11 | 2020-08-14 | 中国科学院重庆绿色智能技术研究院 | Preparation method of high-performance porous honeycomb tin-carbon lithium battery cathode material |
| CN112599738A (en) * | 2020-12-14 | 2021-04-02 | 大连海事大学 | Tin-carbon composite material for lithium ion battery cathode and preparation method and application thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104766962A (en) * | 2015-04-17 | 2015-07-08 | 辽宁工程技术大学 | Preparation method of carbon-cladding graphite oxide/Sn composite cathode material of lithium ion battery |
| CN108140818A (en) * | 2015-10-06 | 2018-06-08 | 法拉典有限公司 | A kind of method for being used to prepare hard carbon composite material |
| CN108140818B (en) * | 2015-10-06 | 2021-07-20 | 法拉典有限公司 | Method for preparing hard carbon composite material |
| CN105406065A (en) * | 2015-11-30 | 2016-03-16 | 安泰科技股份有限公司 | SnS2-C negative electrode nanocomposite and preparation method and application therefor |
| CN105655557A (en) * | 2016-01-18 | 2016-06-08 | 浙江大学 | Preparation method of carbon-wrapping-tin nanometer material with carbon shells not completely filled with tin |
| CN105655557B (en) * | 2016-01-18 | 2018-07-27 | 浙江大学 | A kind of preparation method of the carbon tinning nano material of the not completely filled carbon shell of tin |
| CN106784736A (en) * | 2017-02-08 | 2017-05-31 | 大连理工大学 | A kind of sodium-ion battery negative pole coats the preparation method and application of tin particles nanometer sheet with coal tar pitch resin base amorphous carbon |
| CN109411717A (en) * | 2018-09-28 | 2019-03-01 | 华南理工大学 | A kind of negative electrode material and preparation method thereof through prelithiation with high reversible capacity |
| CN111531181A (en) * | 2020-05-11 | 2020-08-14 | 中国科学院重庆绿色智能技术研究院 | Preparation method of high-performance porous honeycomb tin-carbon lithium battery cathode material |
| CN111531181B (en) * | 2020-05-11 | 2022-12-16 | 中国科学院重庆绿色智能技术研究院 | Preparation method of high-performance porous honeycomb tin-carbon lithium battery cathode material |
| CN112599738A (en) * | 2020-12-14 | 2021-04-02 | 大连海事大学 | Tin-carbon composite material for lithium ion battery cathode and preparation method and application thereof |
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