CN107507964A - A kind of preparation method of soft carbon, hard carbon core shell structure negative material - Google Patents
A kind of preparation method of soft carbon, hard carbon core shell structure negative material Download PDFInfo
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- CN107507964A CN107507964A CN201610414923.0A CN201610414923A CN107507964A CN 107507964 A CN107507964 A CN 107507964A CN 201610414923 A CN201610414923 A CN 201610414923A CN 107507964 A CN107507964 A CN 107507964A
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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
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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
- H01M4/36—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
- 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
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- 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
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Abstract
The present invention relates to battery material technical field, specifically a kind of soft carbon, the preparation method of hard carbon core shell structure negative material, it is characterised in that use following preparation method：(1), ammonium chloride is added to the water, stir to obtain aqueous ammonium chloride solution, then adds starch, continues to be uniformly mixing to obtain mixture；(2), pre- carbonization；(3) starch base hard carbon, is prepared；(4) emulsion, is prepared；(5), it is spray-dried；(6), heating carbonization, is cooled to room temperature and gets product.Compared with the existing technology, preparation method is simple, and cost is low, environmentally safe by the present invention；After the soft carbon prepared, hard carbon core shell structure negative material are applied to lithium ion battery, make the permanent hair styling that there is the characteristics of cyclical stability is strong, electric conductivity is strong, rate charge-discharge is good.
Description
Technical field
The present invention relates to battery material technical field, specifically a kind of soft carbon, hard carbon core shell structure negative pole
The preparation method of material.
Background technology
With the development of science and technology, people propose higher requirement to the performance of electrochmical power source (battery).
Such as, the development of integrated circuit technique makes electronic instrument small, portability, correspondingly requires that battery has
There is the characteristics of small volume, in light weight, higher than energy；Space exploration technology and national defence, military equipment technology
Continuous development requires that battery has high-energy-density and long storage life；The reinforcement of environmental protection consciousness makes people couple
The development growing interest of electric automobile, and this battery should then have big ratio energy and specific power.Numerous
Battery system in, lithium battery so that its operating voltage is high, energy density is big and shows one's talent the advantages that light weight,
Paid attention to by countries in the world.
The development of portable electric appts was advanced by leaps and bounds in the last few years.In addition, lithium rechargeable battery also by
Gradually it is pushed to field of traffic.Thus requirement to lithium rechargeable battery is constantly improving, due to it is this more
High requirement, limitation of the graphite cathode material in terms of capacity and power characteristic are just obvious all the more.This
Under background, hard carbon has promising negative material as one kind and gradually closed by more research workers very much
Note.
The content of the invention
The purpose of the present invention is overcome the deficiencies in the prior art, there is provided a kind of cyclical stability is strong, electric conductivity is strong,
The good soft carbon for lithium ion battery of rate charge-discharge, hard carbon core shell structure negative material.
To achieve the above object, a kind of soft carbon, the preparation method of hard carbon core shell structure negative material are designed, its
It is characterised by using following preparation method：
(1), ammonium chloride is added to the water, stir to obtain aqueous ammonium chloride solution, then adds starch, after
It is continuous to be uniformly mixing to obtain mixture；The mass concentration of described aqueous ammonium chloride solution is 0.5~30g/L,
The weight of ammonium chloride and starch ratio is 1: 1~200；
(2), mixture is put into vacuum drying chamber, is dried in vacuo 1 hour, be carbonized 1h in advance, obtains pre- carbon
Compound, vacuum drying temperature are 60 DEG C~100 DEG C, and pre- carburizing temperature is 100 DEG C~320 DEG C；
(3), pre- carbide is put into atmosphere furnace, and under inert gas shielding, temperature is 700~1000 DEG C,
Heating rate is 5 DEG C of min, and constant temperature time is 0.1~10 hour, drops to room temperature, obtains starch base hard carbon；
(4) covering and emulsifying agent, deionized water, are made into emulsion, emulsifying agent: covering: go from
The weight ratio of sub- water is 1~5: 50: 100~449；
(5) it is, starch base hard carbon: emulsion=1~1: 100 starch base hard carbon and emulsion by weight ratio
Stir, be spray-dried, the temperature of import is 180 DEG C~250 DEG C during spray drying, outlet
Temperature is 100 DEG C~120 DEG C；
(6), the product after spray drying is placed in tube furnace, under inert gas shielding, heating carbonization,
Carburizing temperature is 1000~2000 DEG C, and heating rate is 5 DEG C of min, and carbonization time is 1h~24h, cold
But got product to room temperature；
Described covering uses any in asphalt, coal tar pitch, petroleum residual oil or coal measures residual oil
Kind.
The starch is in farina, cornstarch, wheaten starch, sweet potato starch, kudzuvine root starch
It is one or more.
Atmosphere in described atmosphere furnace is nitrogen or argon gas.
Compared with the existing technology, preparation method is simple, and cost is low, environmentally safe by the present invention；Prepare
Soft carbon, hard carbon core shell structure negative material be applied to lithium ion battery after, make the permanent hair styling that there is stable circulation
The characteristics of property is strong, electric conductivity is strong, rate charge-discharge is good.
Brief description of the drawings
Fig. 1 is the electron microscopic picture of embodiment 6.
Embodiment
Below in conjunction with embodiment, technical scheme is further described through.
Embodiment 1
Step 1：Weigh 2g ammonium chlorides to be added in 1000ml water, stir, it is beautiful then to add 100g
Rice starch, continue to stir, obtain mixture；
Step 2：Mixture is put into vacuum drying chamber, 100 DEG C are dried in vacuo 1 hour, 150 DEG C of pre- carbon
Change 1h, obtain pre- carbide；
Step 3：Pre- carbide is put into atmosphere furnace, is warming up under nitrogen protection with 5 DEG C/min speed
700 DEG C, constant temperature is cooled to room temperature after 5 hours, obtains starch base hard carbon.
Step 4：Pitch and emulsifying agent, deionized water are made into emulsion, described emulsifying agent: pitch:
The weight ratio of deionized water is 1: 50: 449；
Step 5：By starch base hard carbon: the weight of emulsion stirs than 1: 1, is spray-dried, spray
The temperature of import is 180 DEG C when mist is dried, and outlet temperature is 100 DEG C.
Step 6：Product after spray drying is placed in tube furnace, with 5 DEG C/min speed under nitrogen protection
1150 DEG C of carbonization 3h are heated to, room temperature is cooled to and produces soft carbon/hard carbon core shell structure negative material.
Embodiment 2
Step 1：Weigh 2g ammonium chlorides to be added in 1000ml water, stir, it is beautiful then to add 100g
Rice starch, continue to stir, obtain mixture；
Step 2：Mixture is put into vacuum drying chamber, 90 DEG C are dried in vacuo 1 hour, 150 DEG C of pre- carbonizations
1h, obtain pre- carbide；
Step 3：Pre- carbide is put into atmosphere furnace, is warming up under nitrogen protection with 5 DEG C/min speed
700 DEG C, constant temperature is cooled to room temperature after 2 hours, obtains starch base hard carbon.
Step 4：Petroleum residual oil and emulsifying agent, deionized water are made into emulsion, described emulsifying agent: stone
Dregs of fat oil: the weight ratio of deionized water is 1: 50: 200；
Step 5：By starch base hard carbon: the weight of emulsion stirs than 2: 3, is spray-dried, spray
The temperature of import is 180 DEG C when mist is dried, and outlet temperature is 100 DEG C；
Step 6：Product after spray drying is placed in tube furnace, with 5 DEG C/min speed under nitrogen protection
1250 DEG C of carbonization 3h are heated to, room temperature is cooled to and produces the soft carbon to be invented/hard carbon core shell structure negative pole material
Material.
Embodiment 3
Step 1：Weigh 3g ammonium chlorides to be added in 1000ml water, stir, it is beautiful then to add 100g
Rice starch, continue to stir, obtain mixture；
Step 2：Mixture is put into vacuum drying chamber, 90 DEG C are dried in vacuo 1 hour, 200 DEG C of pre- carbonizations
1h, obtain pre- carbide；
Step 3：Pre- carbide is put into atmosphere furnace, is warming up under nitrogen protection with 5 DEG C/min speed
1000 DEG C, constant temperature is cooled to room temperature after 2 hours, obtains starch base hard carbon.
Step 4：Petroleum residual oil and emulsifying agent, deionized water are made into emulsion, described emulsifying agent: coal
It is residual oil: the weight ratio of deionized water is 1: 50: 300；
Step 5：By starch base hard carbon: the weight of emulsion stirs than 2: 3, is spray-dried, spray
The temperature of import is 180 DEG C when mist is dried, and outlet temperature is 100 DEG C.
Step 6：Product after spray drying is placed in tube furnace, with 5 DEG C/min speed under nitrogen protection
1250 DEG C of carbonization 3h are heated to, room temperature is cooled to and produces soft carbon/hard carbon core shell structure negative material.
Embodiment 4
Step 1：Weigh 3g ammonium chlorides to be added in 1000ml water, stir, it is beautiful then to add 100g
Rice starch, continue to stir, obtain mixture；
Step 2：Mixture is put into vacuum drying chamber, 90 DEG C are dried in vacuo 1 hour, 200 DEG C of pre- carbonizations
1h, obtain pre- carbide；
Step 3：Pre- carbide is put into atmosphere furnace, is warming up under nitrogen protection with 5 DEG C/min speed
1000 DEG C, constant temperature is cooled to room temperature after 2 hours, obtains starch base hard carbon.
Step 4：Petroleum residual oil and emulsifying agent, deionized water are made into emulsion, described emulsifying agent: coal
It is residual oil: the weight ratio of deionized water is 1: 50: 300；
Step 5：By starch base hard carbon: emulsion stirs by weight 2: 3, is spray-dried, spray
The temperature of import is 180 DEG C when mist is dried, and outlet temperature is 100 DEG C；
Step 6：Product after spray drying is placed in tube furnace, with 5 DEG C/min speed under nitrogen protection
1750 DEG C of carbonization 3h are heated to, room temperature is cooled to and produces soft carbon, hard carbon core shell structure negative material.
Embodiment 5
Step 1：Weigh 3g ammonium chlorides to be added in 1000ml water, stir, then add 100g horses
Bell sweet potato starch, continue to stir, obtain mixture；
Step 2：Mixture is put into vacuum drying chamber, 90 DEG C are dried in vacuo 1 hour, 200 DEG C of pre- carbonizations
1h, obtain pre- carbide；
Step 3：Pre- carbide is put into atmosphere furnace, is warming up under nitrogen protection with 5 DEG C/min speed
1000 DEG C, constant temperature is cooled to room temperature after 2 hours, obtains starch base hard carbon；
Step 4：Petroleum residual oil and emulsifying agent, deionized water are made into emulsion, described emulsifying agent: coal
It is residual oil: the weight ratio of deionized water is 1: 50: 300；
Step 5：By starch base hard carbon: the weight of emulsion stirs than 2: 3, is spray-dried, spray
The temperature of import is 180 DEG C when mist is dried, and outlet temperature is 100 DEG C；
Step 6：Product after spray drying is placed in tube furnace, with 5 DEG C/min speed under nitrogen protection
1250 DEG C of carbonization 3h are heated to, room temperature is cooled to and produces soft carbon/hard carbon core shell structure negative material.
Embodiment 6
Step 1：Weigh 3g ammonium chlorides to be added in 1000ml water, stir, it is small then to add 100g
Wheat starch, continue to stir, obtain mixture；
Step 2：Mixture is put into vacuum drying chamber, 90 DEG C are dried in vacuo 1 hour, 200 DEG C of pre- carbonizations
1h, obtain pre- carbide；
Step 3：Pre- carbide is put into atmosphere furnace, is warming up under nitrogen protection with 5 DEG C/min speed
1000 DEG C, constant temperature is cooled to room temperature after 2 hours, obtains starch base hard carbon.
Step 4：Petroleum residual oil and emulsifying agent, deionized water are made into emulsion, described emulsifying agent: coal
It is residual oil: the weight ratio of deionized water is 1: 50: 300；
Step 5：By starch base hard carbon: the weight of emulsion stirs than 2: 3, is spray-dried, spray
The temperature of import is 180 DEG C when mist is dried, and outlet temperature is 100 DEG C；
Step 6：Product after spray drying is placed in tube furnace, with 5 DEG C/min speed under nitrogen protection
1750 DEG C of carbonization 3h are heated to, room temperature is cooled to and produces soft carbon/hard carbon core shell structure negative material.
Embodiment 7
Step 1：Weigh 3g ammonium chlorides to be added in 1000ml water, stir, then add 100g kinds
Sweet potato starch, continue to stir, obtain mixture；
Step 2：Mixture is put into vacuum drying chamber, 90 DEG C are dried in vacuo 1 hour, 170 DEG C of pre- carbonizations
1h, obtain pre- carbide；
Step 3：Pre- carbide is put into atmosphere furnace, is warming up under nitrogen protection with 5 DEG C/min speed
800 DEG C, constant temperature is cooled to room temperature after 7 hours, obtains starch base hard carbon.
Step 4：Petroleum residual oil and emulsifying agent, deionized water are made into emulsion, described emulsifying agent: coal
It is residual oil: the weight ratio of deionized water is 1: 50: 250；
Step 5：By starch base hard carbon: the weight of emulsion stirs than 2: 3, is spray-dried, spray
The temperature of import is 180 DEG C when mist is dried, and outlet temperature is 100 DEG C.
Step 6：Product after spray drying is placed in tube furnace, with 5 DEG C/min speed under nitrogen protection
1750 DEG C of carbonization 3h are heated to, room temperature is cooled to and produces soft carbon/hard carbon core shell structure negative material.
Embodiment 8
Step 1：Weigh 3g ammonium chlorides to be added in 1000ml water, stir, then add 100g Pueraria lobotas
Powder, continue to stir, obtain mixture, stir；
Step 2：Mixture is put into vacuum drying chamber, 90 DEG C are dried in vacuo 1 hour, 200 DEG C of pre- carbonizations
1h, obtain pre- carbide；
Step 3：Pre- carbide is put into atmosphere furnace, is warming up under nitrogen protection with 5 DEG C/min speed
1000 DEG C, constant temperature is cooled to room temperature after 2 hours, obtains starch base hard carbon.
Step 4：Petroleum residual oil and emulsifying agent, deionized water are made into emulsion, described emulsifying agent: coal
It is residual oil: the weight ratio of deionized water is 1: 50: 300；
Step 5：By starch base hard carbon: the weight of emulsion stirs than 2: 3, is spray-dried, spray
The temperature of import is 180 DEG C when mist is dried, and outlet temperature is 100 DEG C.
Step 6：Product after spray drying is placed in tube furnace, with 5 DEG C/min speed under nitrogen protection
1950 DEG C of carbonization 3h are heated to, room temperature is cooled to and produces soft carbon/hard carbon core shell structure negative material.
The soft carbon prepared in the embodiment of the present invention, hard carbon core shell structure negative material are subjected to following half-cell
Test：
Soft carbon prepared by the present invention, hard carbon core shell structure negative material, the N- containing 6~7% Kynoar
Methyl pyrrolidone and 2% conductive black are well mixed, and are applied on copper foil, and the pole piece coated is put into temperature
It is standby to be dried in vacuo 4 hours in 110 DEG C of vacuum drying chambers.
Simulated battery is assemblied in the German Braun glove box of applying argon gas and carried out, electrolyte 1M
LiPF6+EC: DEC: DMC=1: 1: 1 (volume ratio), metal lithium sheet are to electrode, chemical property
Test carried out on U.S. ArbinBT2000 type cell testers, charging/discharging voltage scope be 0.005 to
1.0V, charge-discharge velocity 0.1C, test result see the table below：
The soft carbon prepared in the embodiment of the present invention, hard carbon core shell structure negative material are carried out into following full battery to survey：
Referring to Fig. 1, soft carbon prepared by the embodiment of the present invention 6, hard carbon core shell structure negative material are as lithium battery
Negative pole, cobalt acid lithium is molten as positive pole, 1M-LiPF6EC: DMC: EMC=1: 1: 1 (volume ratio)
Liquid makees electrolyte assembling and helps battery, tests it in 670 weeks capability retentions of 1C charge and discharges 94.18%.
Claims (3)
1. the preparation method of a kind of soft carbon, hard carbon core shell structure negative material, it is characterised in that prepared using following
Method：
(1), ammonium chloride is added to the water, stir to obtain aqueous ammonium chloride solution, then adds starch, after
It is continuous to be uniformly mixing to obtain mixture；The mass concentration of described aqueous ammonium chloride solution is 0.5~30g/L,
The weight of ammonium chloride and starch ratio is 1: 1~200；
(2), mixture is put into vacuum drying chamber, is dried in vacuo 1 hour, be carbonized 1h in advance, obtains pre- carbon
Compound, vacuum drying temperature are 60 DEG C~100 DEG C, and pre- carburizing temperature is 100 DEG C~320 DEG C；
(3), pre- carbide is put into atmosphere furnace, and under inert gas shielding, temperature is 700~1000 DEG C,
Heating rate is 5 DEG C of min, and constant temperature drops to room temperature after 0.1~10 hour, obtains starch base hard carbon；
(4) covering and emulsifying agent, deionized water, are made into emulsion, described emulsifying agent: covering:
The weight ratio of deionized water is 1~5: 50: 100~449；
(5) it is, starch base hard carbon: emulsion=1~1: 100 starch base hard carbon and emulsion by weight ratio
Stir, be spray-dried, the temperature of import is 180 DEG C~250 DEG C during spray drying, outlet
Temperature is 100 DEG C~120 DEG C；
(6), the product after spray drying is placed in tube furnace, under inert gas shielding, heating carbonization,
Carburizing temperature is 1000~2000 DEG C, and heating rate is 5 DEG C/min, and carbonization time is 1h~24h,
Room temperature is cooled to get product；
Described covering uses any in asphalt, coal tar pitch, petroleum residual oil or coal measures residual oil
Kind.
2. a kind of soft carbon, the preparation method of hard carbon core shell structure negative material as claimed in claim 1, it is special
Sign is：The starch is farina, cornstarch, wheaten starch, sweet potato starch, kudzuvine root starch
In one or more.
3. a kind of soft carbon, the preparation method of hard carbon core shell structure negative material as claimed in claim 1, it is special
Sign is：Atmosphere in described atmosphere furnace is nitrogen or argon gas.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108682804A (en) * | 2018-04-25 | 2018-10-19 | 福建翔丰华新能源材料有限公司 | A kind of hard carbon cladding soft carbon is used as the preparation method of lithium ion battery negative material |
| CN108878774A (en) * | 2018-06-26 | 2018-11-23 | 上海汉行科技有限公司 | A kind of complex carbon material and its preparation method and application |
| CN109742399A (en) * | 2018-12-18 | 2019-05-10 | 宁波容百新能源科技股份有限公司 | A kind of anode material of lithium-ion battery and preparation method thereof |
| CN110877908A (en) * | 2018-09-06 | 2020-03-13 | 天津大学 | Preparation method of corn starch pyrolysis hard carbon electrode material |
| CN116731527A (en) * | 2023-06-15 | 2023-09-12 | 浙江华宇钠电新能源科技有限公司 | Asphalt mixture and application thereof in preparing sodium ion battery for vehicle |
| CN117384323A (en) * | 2023-12-12 | 2024-01-12 | 成都锂能科技有限公司 | Starch-based precursor material and preparation method and application thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108682804A (en) * | 2018-04-25 | 2018-10-19 | 福建翔丰华新能源材料有限公司 | A kind of hard carbon cladding soft carbon is used as the preparation method of lithium ion battery negative material |
| CN108682804B (en) * | 2018-04-25 | 2021-05-25 | 深圳市翔丰华科技股份有限公司 | Preparation method of lithium ion battery cathode material with hard carbon-coated soft carbon |
| CN108878774A (en) * | 2018-06-26 | 2018-11-23 | 上海汉行科技有限公司 | A kind of complex carbon material and its preparation method and application |
| CN108878774B (en) * | 2018-06-26 | 2020-11-24 | 上海汉行科技有限公司 | Composite carbon material and preparation method and application thereof |
| CN110877908A (en) * | 2018-09-06 | 2020-03-13 | 天津大学 | Preparation method of corn starch pyrolysis hard carbon electrode material |
| CN110877908B (en) * | 2018-09-06 | 2022-07-01 | 天津大学 | Preparation method of corn starch pyrolysis hard carbon electrode material |
| CN109742399A (en) * | 2018-12-18 | 2019-05-10 | 宁波容百新能源科技股份有限公司 | A kind of anode material of lithium-ion battery and preparation method thereof |
| CN116731527A (en) * | 2023-06-15 | 2023-09-12 | 浙江华宇钠电新能源科技有限公司 | Asphalt mixture and application thereof in preparing sodium ion battery for vehicle |
| CN116731527B (en) * | 2023-06-15 | 2023-10-31 | 浙江华宇钠电新能源科技有限公司 | Asphalt mixture and application thereof in preparing sodium ion battery for vehicle |
| CN117384323A (en) * | 2023-12-12 | 2024-01-12 | 成都锂能科技有限公司 | Starch-based precursor material and preparation method and application thereof |
| CN117384323B (en) * | 2023-12-12 | 2024-03-08 | 成都锂能科技有限公司 | Starch-based precursor material and preparation method and application thereof |
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Application publication date: 20171222 |