CN107611366B - A kind of preparation method of lithium ion battery negative material - Google Patents
A kind of preparation method of lithium ion battery negative material Download PDFInfo
- Publication number
- CN107611366B CN107611366B CN201710643919.6A CN201710643919A CN107611366B CN 107611366 B CN107611366 B CN 107611366B CN 201710643919 A CN201710643919 A CN 201710643919A CN 107611366 B CN107611366 B CN 107611366B
- Authority
- CN
- China
- Prior art keywords
- powder
- lithium ion
- preparation
- ion battery
- silicate glass
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- 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
Landscapes
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention relates to a kind of preparation methods of lithium ion battery negative material, belong to technical field of lithium ion.The present invention takes silicate glass to be placed in ball grinder, sodium chloride solution ball milling is added, be sieved to obtain silicate glass powder；Arabic gum and bassora gum are taken, ball milling in ball grinder is placed in, is sieved, obtains bassora gum and Arabic gum mix powder；Silicate glass ball-milled powder and Arabic gum are mixed with tragacanth gum powder, zinc powder stirring is added, obtains hydrocolloid powder mixture；Hydrocolloid powder is filled into mold, compression process, pressure maintaining are placed in baking oven, and after heat cure processing, standing is cooled to room temperature, and obtains solidifying substance；Solidifying substance is placed in tube-type atmosphere furnace, nitrogen is passed through and excludes air, control temperature charing, standing is cooled to room temperature to get a kind of carbon silicon composite cathode material.The resulting negative electrode material of the present invention has good rate capability and capacity height, good conductivity, electrical contact increase the application for expanding silicium cathode material.
Description
The present invention relates to a kind of preparation methods of lithium ion battery negative material, belong to technical field of lithium ion.
Background technique
For in the 21st century, with the development of economy and society, people are continuously increased the demand of the energy.But by the energy
What increase in demand generated, which pollutes oneself, becomes the main source of environmental pollution.Meanwhile more and more countries recognize and want in the world
It establishes one and had not only been able to satisfy the society that current social needs but also do not jeopardize future generations' survival and development, it is necessary to greatly develop new energy
It reduces environmental pollution with the green energy resources such as renewable energy.Green power supply is one of important directions of green energy resource.Therefore, green
The lithium ion battery of color safety attracts wide attention.
Currently, performance of lithium ion battery is superior, and it is widely used, it has a extensive future.Relative to traditional lead-acid battery, ni-Cd electricity
The secondary cells such as pond and nickel-metal hydride battery, lithium ion battery have energy density height, open-circuit voltage height, have extended cycle life, self discharge
Rate is small, memory-less effect and the outstanding advantages such as environmentally protective.Lithium ion battery is own through people's with the continuous progress of technology
It is widely used in life, such as portable electronic product, new energy vehicles field.However, lithium ion battery
Specific discharge capacity and energy density need it is further improve, come meet portable electronic product miniaturization and its space flight,
The requirement applied in terms of military, peak load regulation network and electric car.Therefore, the lithium ion battery of height ratio capacity and high-energy-density is researched and developed
Material oneself become the very important research topic of current research work.
Summary of the invention
The technical problems to be solved by the invention: for carbon material high rate performance difference and capacity it is low constrain carbon material into
One step application, while its poorly conductive, cyclic process volume expansion crush, electrical contact is reduced, and seriously constrain silicon-based anode material
The commercial applications problem of material, provides a kind of preparation method of lithium ion battery negative material.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) sodium chloride solution and discarded silicate glass are placed in ball grinder, ball milling, sieving by 1:10 in mass ratio
Obtain ball milling silicate powder；
(2) 1:1 in mass ratio, Arabic gum and bassora gum are placed in ball grinder, and ball milling is sieved to obtain ball milling hydrocolloid powder；
(3) according to parts by weight, 20 ~ 30 parts of silicate glasses, 40 ~ 60 parts of hydrocolloid powders and 1 ~ 2 part of zinc powder is taken to stir respectively
Mixing is mixed, uniformly mixed hydrocolloid powder mixture is obtained；
(4) the hydrocolloid powder mixture of preparation is filled into sheet mold, compression moulding, demoulding, heat cure handle, are quiet
It sets and is cooled to room temperature, obtain solidifying substance；
(5) solidifying substance being placed in tube-type atmosphere furnace, is passed through nitrogen and excludes air, charing process, standing is cooled to room temperature,
A kind of carbon silicon composite cathode material can be prepared into.
Concentration of sodium chloride solution described in step (1) is 0.8mol/L.
Zinc powder described in step (3) is 250 ~ 300 mesh zinc particles.
Compression moulding pressure described in step (4) is 5 ~ 10MPa.
Heat curing temperature described in step (4) is 80 ~ 100 DEG C.
It is 45 ~ 50mL/min that nitrogen described in step (5), which is passed through flow,.
Charing process described in step (5) is 2 ~ 3h of heat preservation charing at 600 ~ 700 DEG C.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention greatly improves silicon by the way that Arabic gum and bassora gum are added when preparing silicon based anode material
The structural stability of material improves the capacity of overall electrode；
(2) present invention can improve the electricity of electrode material by joined zinc powder during prepared by carbon-silicon composite material
Subconductivity；
(3) addition of Arabic gum and bassora gum, for improving charge/discharge capacity under lithium ion battery high current density, changing
Kind capacity stability has obvious effect.
Specific embodiment
Discarded silicate glass is taken, is cleaned with clear water, natural drying is placed in ball grinder, and silicate glass matter is added
The sodium chloride solution for measuring 10% 0.8mol/L, 2 ~ 3h of ball milling, sieves with 100 mesh sieve under the revolving speed of 450 ~ 500r/min, obtains ball milling silicon
Silicate glass powder；The Arabic gum and bassora gum for taking equal quality, are placed in ball grinder, under the revolving speed of 500 ~ 550r/min
3 ~ 4h of ball milling takes out ball-milled powder and sieves with 100 mesh sieve, obtain bassora gum and Arabic gum mix powder after ball milling；It presses
Mass ratio 1:2 mixes discarded silicate glass ball-milled powder and Arabic gum with tragacanth gum powder, and 5% silicate glass is added
The zinc powder of quality persistently stirs 30 min with blender under the revolving speed of 150 ~ 180r/min, obtains uniformly mixed hydrocolloid powder
Mixture；The hydrocolloid powder mixture of preparation is filled into sheet mold, at room temperature, with 5 ~ 10MPa compression process, pressure maintaining
After 2 ~ 3min, demoulding is placed in 80 ~ 100 DEG C of baking ovens, after heat cure handles 1 ~ 2h, is stood cooling Zhishi temperature, is obtained solidifying substance；It will
Solidifying substance is placed in tube-type atmosphere furnace, is passed through nitrogen and is excluded air, and the flow for controlling nitrogen is 45 ~ 50mL/min, in nitrogen gas
At 600 ~ 700 DEG C, heat preservation 2 ~ 3h of charing, standing is cooled to room temperature for temperature control under atmosphere, can be prepared into a kind of carbon silicon Compound Negative
Pole material.The zinc powder is 250 ~ 300 mesh zinc particles.
Example 1
Discarded silicate glass is taken, is cleaned with clear water, natural drying is placed in ball grinder, and silicate glass matter is added
The sodium chloride solution for measuring 10% 0.8mol/L, ball milling 2h, sieves with 100 mesh sieve under the revolving speed of 450r/min, obtains ball milling glassy silicate
Glass powder；The Arabic gum and bassora gum for taking equal quality, are placed in ball grinder, the ball milling 3h under the revolving speed of 500r/min, to
After ball milling, takes out ball-milled powder and sieve with 100 mesh sieve, obtain bassora gum and Arabic gum mix powder；1:2 in mass ratio,
Discarded silicate glass ball-milled powder and Arabic gum are mixed with tragacanth gum powder, the 250 of 5% silicate glass quality are added
Zinc powder persistently stirs 30 min with blender under the revolving speed of 150r/min, obtains uniformly mixed hydrocolloid powder mixture；It will system
Standby hydrocolloid powder mixture is filled into sheet mold, and at room temperature, with 5MPa compression process, after pressure maintaining 2min, demoulding is simultaneously
It is placed in 80 DEG C of baking ovens, after heat cure handles 1h, stands cooling Zhishi temperature, obtain solidifying substance；Solidifying substance is placed in tube-type atmosphere furnace
In, it is passed through nitrogen and excludes air, the flow for controlling nitrogen is 45mL/min, and temperature control is at 600 DEG C in a nitrogen atmosphere, heat preservation
2 h are carbonized, standing is cooled to room temperature, and can be prepared into a kind of carbon silicon composite cathode material.
Example 2
Discarded silicate glass is taken, is cleaned with clear water, natural drying is placed in ball grinder, and silicate glass matter is added
The sodium chloride solution for measuring 10% 0.8mol/L, ball milling 2.5h, sieves with 100 mesh sieve under the revolving speed of 470r/min, obtains ball milling silicate
Glass powder；The Arabic gum and bassora gum for taking equal quality, are placed in ball grinder, the ball milling 3h under the revolving speed of 525r/min,
After ball milling, takes out ball-milled powder and sieve with 100 mesh sieve, obtain bassora gum and Arabic gum mix powder；In mass ratio 1:
2, discarded silicate glass ball-milled powder and Arabic gum are mixed with tragacanth gum powder, 5% silicate glass quality is added
270 mesh zinc powders persistently stir 30 min with blender under the revolving speed of 165r/min, obtain uniformly mixed hydrocolloid powder mixing
Object；The z hydrocolloid powder mixture prepared is filled into sheet mold, at room temperature, with 7MPa compression process, pressure maintaining 2.5min
Afterwards, demoulding is placed in 90 DEG C of baking ovens, after heat cure handles 1.5h, is stood cooling Zhishi temperature, is obtained solidifying substance；Solidifying substance is placed in
It in tube-type atmosphere furnace, is passed through nitrogen and excludes air, the flow for controlling nitrogen is 47mL/min, and temperature control in a nitrogen atmosphere exists
650 DEG C, heat preservation charing 2.5h, standing is cooled to room temperature, and can be prepared into a kind of carbon silicon composite cathode material.
Example 3
Discarded silicate glass is taken, is cleaned with clear water, natural drying is placed in ball grinder, and silicate glass matter is added
The sodium chloride solution for measuring 10% 0.8mol/L, ball milling 3h, sieves with 100 mesh sieve under the revolving speed of 500r/min, obtains ball milling glassy silicate
Glass powder；The Arabic gum and bassora gum for taking equal quality, are placed in ball grinder, the ball milling 4h under the revolving speed of 550r/min, to
After ball milling, takes out ball-milled powder and sieve with 100 mesh sieve, obtain bassora gum and Arabic gum mix powder；1:2 in mass ratio,
Discarded silicate glass ball-milled powder and Arabic gum are mixed with tragacanth gum powder, the 300 of 5% silicate glass quality are added
Mesh zinc powder persistently stirs 30 min with blender under the revolving speed of 180r/min, obtains uniformly mixed hydrocolloid powder mixture；It will
The hydrocolloid powder mixture of preparation is filled into sheet mold, at room temperature, with 10MPa compression process, after pressure maintaining 3min, demoulding
It is placed in 100 DEG C of baking ovens, after heat cure handles 2h, stands cooling Zhishi temperature, obtain solidifying substance；Solidifying substance is placed in tubular type atmosphere
It in furnace, is passed through nitrogen and excludes air, the flow for controlling nitrogen is 50mL/min, and temperature control is protected at 700 DEG C in a nitrogen atmosphere
Temperature charing 3h, standing are cooled to room temperature, and can be prepared into a kind of carbon silicon composite cathode material.
The lithium-ion electric that example and reference examples (lithium ion battery negative material of Zibo company production) are prepared
Pond negative electrode material is detected, and specific detection is as follows:
(1) charging and discharging curve, cycle performance and high rate performance test
By the button cell constant current charge-discharge test of assembling.Test equipment: NEWARE-BTS-5V/10mA battery
Test macro, new Weir Electronics Equipment Co., Ltd, Shenzhen.Test condition: room temperature, voltage range 0.005-
2.0FV, with 50mAg-1Current density research charging and discharging curve and cycle performance, with 50,100,500,1000mA-1Current density
Test high rate performance.
(2) cyclic voltammetric (CV) is tested
The button cell of assembling is subjected to cyclic voltammetry.Test equipment: CHI660D electrochemical workstation.It surveys
Strip part: 0.005 ~ 2.0V of voltage range, scanning speed 0.lmVS-1。
(3) AC impedance (EIS) is tested
The button cell of assembling is subjected to ac impedance measurement.Test equipment: CHI660D electrochemical workstation.It surveys
Strip part: frequency range 100kHz ~ 10mHz, disturbance voltage 5mV.Observe high rate performance and electric conductivity
Specific test result such as table 1.
1 cell negative electrode material performance comparison table of table
| Performance characterization | Example 1 | Example 2 | Example 3 | Reference examples |
| High rate performance (mA-1) | 100 | 500 | 1000 | 50 |
| Cyclic voltammetric (V) | 0.5 | 1 | 2 | 0.1 |
| AC impedance (kHz) | 100 | 500 | 1000 | 98 |
| High rate performance and electric conductivity | Good rate capability conducts electricity very well | Good rate capability conducts electricity very well | Good rate capability conducts electricity very well | Difference of magnification can good poorly conductive |
As shown in Table 1, lithium ion battery negative material prepared by the present invention high rate performance with higher and biggish appearance
Amount；And good conductivity, electrical contact increase, and expand the commercial applications range of silicon based anode material.
Claims (6)
1. a kind of preparation method of lithium ion battery negative material, it is characterised in that preparation step are as follows:
(1) discarded silicate glass is taken, is cleaned with clear water, natural drying is placed in ball grinder, and silicate glass matter is added
The sodium chloride solution for measuring 10% 0.8mol/L, 2 ~ 3h of ball milling, sieves with 100 mesh sieve under the revolving speed of 450 ~ 500r/min, obtains ball milling silicon
Silicate glass powder；
(2) 1:1 in mass ratio, Arabic gum and bassora gum are placed in ball grinder, and ball milling is sieved to obtain ball milling hydrocolloid powder；
(3) 1:2 in mass ratio mixes ball milling silicate glass powder and Arabic gum with tragacanth gum powder, and 5% silicic acid is added
The zinc powder of salt glass quality persistently stirs 30 min with blender under the revolving speed of 150 ~ 180r/min, obtains uniformly mixed glue
Body mixture of powders；
(4) the hydrocolloid powder mixture of preparation is filled into sheet mold, compression moulding, demoulding, heat cure processing, stand it is cold
But to room temperature, solidifying substance is obtained；
(5) solidifying substance is placed in tube-type atmosphere furnace, is passed through nitrogen and excludes air, charing process, standing is cooled to room temperature
It is prepared into a kind of carbon silicon composite cathode material.
2. according to a kind of preparation method of lithium ion battery negative material described in claim 1, it is characterised in that: step (3) institute
The zinc powder stated is 250 ~ 300 mesh zinc particles.
3. according to a kind of preparation method of lithium ion battery negative material described in claim 1, it is characterised in that: step (4) institute
The compression moulding pressure stated is 5 ~ 10MPa.
4. according to a kind of preparation method of lithium ion battery negative material described in claim 1, it is characterised in that: step (4) institute
The heat curing temperature stated is 80 ~ 100 DEG C.
5. according to a kind of preparation method of lithium ion battery negative material described in claim 1, it is characterised in that: step (5) institute
It is 45 ~ 50mL/min that the nitrogen stated, which is passed through flow,.
6. according to a kind of preparation method of lithium ion battery negative material described in claim 1, it is characterised in that: step (5) institute
The charing process stated is 2 ~ 3h of heat preservation charing at 600 ~ 700 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710643919.6A CN107611366B (en) | 2017-07-31 | 2017-07-31 | A kind of preparation method of lithium ion battery negative material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710643919.6A CN107611366B (en) | 2017-07-31 | 2017-07-31 | A kind of preparation method of lithium ion battery negative material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107611366A CN107611366A (en) | 2018-01-19 |
| CN107611366B true CN107611366B (en) | 2019-11-19 |
Family
ID=61064216
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710643919.6A Expired - Fee Related CN107611366B (en) | 2017-07-31 | 2017-07-31 | A kind of preparation method of lithium ion battery negative material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107611366B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108963208B (en) * | 2018-06-22 | 2020-09-15 | 清华大学深圳研究生院 | Preparation method of silicon-carbon negative electrode material and lithium ion battery |
| PL3826770T3 (en) | 2018-07-24 | 2024-10-28 | Camx Power, L.L.C. | Dry milling additive and process |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103236530A (en) * | 2013-04-26 | 2013-08-07 | 奇瑞汽车股份有限公司 | Silicon-carbon composite material, preparation method thereof, and lithium ion battery containing material |
| CN104900843A (en) * | 2015-06-13 | 2015-09-09 | 田东 | Preparation method of silicon carbon composite anode material |
| CN106450329A (en) * | 2016-10-15 | 2017-02-22 | 成都育芽科技有限公司 | High-capacity high-stability silicon-carbon composite nano material for lithium battery electrodes |
| CN106848269A (en) * | 2017-04-26 | 2017-06-13 | 国家纳米科学中心 | A kind of three-dimensional conductive networking Si-C composite material and its preparation method and application |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101375328B1 (en) * | 2007-07-27 | 2014-03-19 | 삼성에스디아이 주식회사 | Si/C composite, anode materials and lithium battery using the same |
-
2017
- 2017-07-31 CN CN201710643919.6A patent/CN107611366B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103236530A (en) * | 2013-04-26 | 2013-08-07 | 奇瑞汽车股份有限公司 | Silicon-carbon composite material, preparation method thereof, and lithium ion battery containing material |
| CN104900843A (en) * | 2015-06-13 | 2015-09-09 | 田东 | Preparation method of silicon carbon composite anode material |
| CN106450329A (en) * | 2016-10-15 | 2017-02-22 | 成都育芽科技有限公司 | High-capacity high-stability silicon-carbon composite nano material for lithium battery electrodes |
| CN106848269A (en) * | 2017-04-26 | 2017-06-13 | 国家纳米科学中心 | A kind of three-dimensional conductive networking Si-C composite material and its preparation method and application |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107611366A (en) | 2018-01-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103887502B (en) | A kind of Delanium lithium ion battery negative material and preparation method thereof | |
| CN104966822A (en) | Multilayer coated lithium titanate cathode material of lithium ion battery and preparation method of multilayer coated lithium titanate cathode material | |
| CN102569759A (en) | Process for preparing materials of silicon-porous carbon negative electrodes of lithium-ion batteries | |
| CN109244539A (en) | Organic-inorganic composite solid electrolyte material and its preparation method and application | |
| CN105762363B (en) | A kind of preparation method of the lithium ion battery negative material based on ZIF complexs | |
| CN104377353A (en) | Preparation method of lithium iron phosphate and nickel cobalt lithium manganate composite positive electrode material | |
| CN102496704A (en) | Lithium titanate/titanium black anode material and preparation method thereof | |
| CN106784843A (en) | It is a kind of more than 300wh/kg high-energy-densities, the preparation method of high security battery | |
| CN107910521A (en) | A kind of fluorinated carbon material, preparation and the application of ruthenium modification | |
| CN107611366B (en) | A kind of preparation method of lithium ion battery negative material | |
| CN105762346A (en) | Preparation method of spherical lithium titanate-graphene composite material for cathodes of lithium ion batteries | |
| CN109244531A (en) | A kind of high purity copper matrix graphite alkene composite lithium ion cell and preparation method thereof | |
| CN103943856A (en) | Preparation method of phthalocyanine-lithium iron phosphate composite anode material | |
| CN103872306A (en) | Preparation method of lithium titanate negative electrode slurry | |
| CN105655588B (en) | A kind of silica modified fluorinated carbon material and preparation method | |
| CN107425215A (en) | A kind of Preparation method and use of starch base composite hard carbon cathode material | |
| CN105047894A (en) | Preparation method of halogen-doped carbon and silicon nano-material and application thereof | |
| CN102903892A (en) | Method for manufacturing industrial energy storage type lithium battery pole piece | |
| CN112397711B (en) | Water-based zinc ion battery positive electrode material and preparation method and application thereof | |
| CN105720267A (en) | Preparation method of lithium ion phosphate power battery cathode plate | |
| CN111326721A (en) | Preparation method of composite negative electrode pre-embedded lithium material | |
| CN109962238A (en) | Method for in-situ preparation of carbon/nitrogen composite protective film on surface of metal compound particle material | |
| CN106033810A (en) | A kind of MoS2/graphene composite material and preparation method thereof | |
| CN104485440B (en) | Preparation method, product, and applications of aluminum oxide-coated lithium cobalt oxide material | |
| CN103633326B (en) | The production method of LiFePO4 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20191025 Address after: 753000 the Ningxia Hui Autonomous Region Shizuishan Dawukou District Industrial Park Xin Sheng northbound Applicant after: Ningxia Ximo New Material Technology Co.,Ltd. Address before: 213102, Mount Huangshan Road, Xinbei District, Jiangsu, Changzhou, 99-4-35 Applicant before: CHANGZHOU NUODING PRECISION MACHINERY MANUFACTURING CO.,LTD. |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20191119 Termination date: 20210731 |