CN105742575A - Method for preparing porous silicon negative electrode of lithium ion battery by in-situ gelatin-polyvinyl alcohol cross-linking carbonization - Google Patents
Method for preparing porous silicon negative electrode of lithium ion battery by in-situ gelatin-polyvinyl alcohol cross-linking carbonization Download PDFInfo
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- CN105742575A CN105742575A CN201610157766.XA CN201610157766A CN105742575A CN 105742575 A CN105742575 A CN 105742575A CN 201610157766 A CN201610157766 A CN 201610157766A CN 105742575 A CN105742575 A CN 105742575A
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- polyvinyl alcohol
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- 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
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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- H01—ELECTRIC ELEMENTS
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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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
- H01M4/621—Binders
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H01M4/625—Carbon or graphite
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Abstract
The invention proposes a method for preparing a porous silicon negative electrode of a lithium ion battery by in-situ gelatin-polyvinyl alcohol cross-linking carbonization. The method comprises the following steps of mixing and stirring polyvinyl alcohol and gelatin to obtain a cross-linking bonding agent; grinding and mixing a silicon material and a conductive agent, and then adding the cross-linking bonding agent; applying the product onto a copper foil by a scrapper after uniform grinding; drying the product in a drying oven; placing the product in a tubular furnace for calcination in an inert atmosphere; and cooling the product to obtain the porous silicon negative electrode. According to the method, the gelatin and the polyvinyl alcohol cross-linking are taken as the bonding agent for use to prepare the porous silicon negative electrode, and a large amount of organic matters are further removed through carbonization; and meanwhile, the conductive performance of the electrode is improved, and the electrochemical performance of the silicon material is effectively improved. The porous silicon negative electrode is safe and non-toxic, the preparation process is simple and practical, and the porous silicon negative electrode material obtained through the preparation method is endowed with relatively high specific capacity and favorable cycle stability when taken as the negative electrode material of the lithium ion battery.
Description
Technical field
The present invention relates to the preparation side of a kind of eco-friendly lithium ion battery porous silicon negative electricity pole piece
Method, belongs to technical field of chemical industry electrode material manufacture process.Embodiment of the present invention preparation method is simple,
Easily operation, reproducible, with low cost, environmentally safe.
Background technology
In the face of constantly consuming and a large amount of releases of harmful substance in consumption process of non-renewable energy resources,
Research and development also efficiently utilize clean energy resource extremely urgent.At new energy field, lithium ion battery is because having height
Energy density, high working voltage, the advantage such as long circulation life and memory-less effect and be widely used in
Multiple fields, such as portable mobile apparatus, electric automobile, energy-accumulating power station etc..But, along with market
Job requirement to electric equipment improves constantly, and the energy density of lithium ion battery, power density, follows
Ring life-span and safety cannot meet the demand in market the most substantially.
Electrode material is as the important component part of lithium ion battery, and its performance is also required to further carry
High.At present, commercialization negative pole is mainly based on graphite, and its theoretical capacity only has 372mAh g-1,
The demand for development of lithium ion battery high-energy-density cannot be met.Silicon materials are as current numerous alternative
One of lithium ion battery negative material, it has high (～the 4200mAh g of theoretical specific capacity-1), suitably
Operating potential (< 0.5Vvs.Li/Li+), rich reserves and advantages of environment protection, cause
The extensive concern of persons.But, silicon materials are faced with a problem demanding prompt solution in actual applications,
I.e. silicon materials can occur violent change in volume (～400%) during removal lithium embedded repeatedly, causes electricity
The electrical contact of pole deteriorates, and material efflorescence and the excess growth of SEI film cause battery capacity to decline rapidly
And coulombic efficiency reduces.At present, mainly by reducing the particle diameter of silicon grain, on silicon grain surface
Carbon coated, and prepare silicon/carbon complex these three method and be modified.Prepare silicon composite to delay
The volumetric expansion solving silicon materials is a kind of relatively effective method, but the preparation process of this type of method of modifying
More complicated.
PVDF is as commercialization binding agent, and it has acceptable viscosity and wide electrochemical window, but
Being the solvent needing to use poisonous NMP as PVDF, additionally PVDF is not have functional group
Direct coupled structure, be only capable of being combined with silicon by more weak Van der Waals force, it is impossible to play suppression silicon materials body
The long-pending effect expanded, and its meeting gelation or dissolving in organic electrolyte, therefore, PVDF is uncomfortable
The binding agent that cooperation is silicon materials uses.Gelatin is raw as water solublity commercial, inexpensive, eco-friendly
Thing macromole, has preferable adhesiveness because having carboxyl and amino, frequently as surfactant and
Dispersant uses, and it is insoluble in conventional organic electrolyte, thus can be as the binding agent of silicon materials
Use.Polyvinyl alcohol is also a kind of eco-friendly water-soluble macromolecule, and its chain structure has a lot of hydroxyl
Base, it is possible to cross linking of gelatin, generate the network of crosslinking.Utilize macromole by silicon materials bag
Cover, generate the cross-linked network of loose structure, be effectively improved the contact of silicon materials and electrolyte
Area, is more beneficial for the transmission of lithium ion；Again Organic substance is carried out partially carbonized, it is possible to be effectively improved
The electric conductivity of silicon electrode.The present invention relates to a kind of utilization gelatin-polyvinyl alcohol crosslinked carbonization in situ prepare
The method of lithium ion battery porous silicon negative pole.
Summary of the invention
The invention aims to improve the chemical property of lithium ion battery silicium cathode material, carry
Environment friendly in high electrode sheet preparation process, reduces the requirement to humidity in preparation process, and carries
The method that lithium ion battery porous silicon negative pole is prepared in a kind of original position gelatin-polyvinyl alcohol crosslinked carbonization gone out.
It is an object of the invention to be achieved through the following technical solutions.
The method that lithium ion battery porous silicon negative pole is prepared in a kind of original position gelatin-polyvinyl alcohol crosslinked carbonization,
Specifically comprise the following steps that
1) being dissolved in deionized water by polyvinyl alcohol, heated and stirred is dissolved；
2) gelatin being added to step 1) in the solution that obtains, heated and stirred is dissolved, and obtains cross-linked binder,
Wherein gelatin is 1:1～0.1:1 with the mass ratio of polyvinyl alcohol；
3) by after silica flour and conductive agent ground and mixed, in mortar, step 2 is added) cross-linked binder that obtains
Agent, wherein the mass ratio of silica flour, polyvinyl alcohol+gelatin and conductive agent is 6:3:1 or 6:2:2, grinds
Uniformly rear scraper for coating is on Copper Foil, and vacuum drying in an oven obtains electrode slice；
4) by step 3) in the electrode slice that obtains be placed in tube furnace and calcine under an inert atmosphere,
Precalcining 1～2 hours at 200～300 DEG C, then calcine 1～2 hour at 300 DEG C～600 DEG C, reaction
After end, under inert atmosphere protection, it is cooled to room temperature, obtains porous silicon negative pole.
Step 3) described in conductive agent be the one in Super-P, acetylene black, graphite or CNT or
Several mixing；
Step 3) described in dry temperature in baking oven be 30 DEG C～60 DEG C；
Beneficial effect
1, the present invention selects gelatin and polyvinyl alcohol crosslinked uses as binding agent, prepares porous silicon negative pole,
By further carbonization, remove major part Organic substance, improve the electric conductivity of electrode simultaneously, effectively change
It is apt to the chemical property of silicon materials.Lithium-ion button battery prepared by this porous silicon negative electricity pole piece
Carrying out constant current charge-discharge test, it shows high charging and discharging capacity and good cycle performance: 0.1C
(400mA·g-1Circulating 50 weeks under the conditions of), capacity is maintained at 1100mAh g-1Left and right.
2, safety non-toxic of the present invention, preparation is simple, prepares the silicium cathode electrode slice tool of gained
Having loose structure, after calcining, gelatin/polyvinyl alcohol occurs partially carbonized, and wherein the introducing of carbon effectively increases
Having added the electric conductivity of silicium cathode, cross-linked network provides certain buffering to the change in volume of silicon materials simultaneously
Inhibitory action, loose structure adds the contact area of electrolyte and electrode material, be more beneficial for lithium from
The transmission of son.This porous silicon negative electrode material shows higher as lithium ion battery negative material
Specific capacity and good cyclical stability.
Accompanying drawing explanation
Fig. 1 is the SEM shape appearance figure of the porous silicon negative electricity pole piece of embodiment 1 preparation, and a is not for forge
The material burnt, b is the material at 500 DEG C after calcining；
Fig. 2 is that the porous silicon negative material of the different calcining heats of embodiment 1 preparation is at 400mA g-1
Under charging and discharging capacity change curve.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is elaborated.
Embodiment 1
The method that lithium ion battery porous silicon negative pole is prepared in a kind of original position gelatin-polyvinyl alcohol crosslinked carbonization,
Concretely comprise the following steps:
1) being dissolved in 4ml deionized water by 60mg polyvinyl alcohol, at 80 DEG C, heated and stirred is dissolved；
2) 60mg gelatin being added to step 1) in the solution that obtains, at 60 DEG C, heated and stirred is dissolved,
To cross-linked binder；
3) by after 240mg silica flour and 40mg Super-P ground and mixed, in mortar, step 2 is added)
The cross-linked binder arrived, grinding uniformly rear scraper for coating is on Copper Foil, and 60 DEG C of vacuum are dried in an oven
Dry, obtain electrode slice, its SEM pattern is as shown in Figure 1a；
4) by step 3) in the electrode slice that obtains be placed in tube furnace and calcine under an argon atmosphere,
Precalcining 2 hours at 300 DEG C, then calcine 1.5 hours at 500 DEG C, after reaction terminates, at argon
It is cooled to room temperature under atmosphere protection, obtains the porous silicon negative pole of crosslinking, calcine the silicon obtained at 500 DEG C and bear
The SEM pattern of pole is as shown in Figure 1 b.
Embodiment 2
The method that lithium ion battery porous silicon negative pole is prepared in a kind of original position gelatin-polyvinyl alcohol crosslinked carbonization,
Concretely comprise the following steps:
1) being dissolved in 2ml deionized water by 40mg polyvinyl alcohol, at 80 DEG C, heated and stirred is dissolved；
2) 40mg gelatin being added to step 1) in the solution that obtains, at 60 DEG C, heated and stirred is dissolved,
To cross-linked binder；
3) by after 240mg silica flour and 80mg Super-P ground and mixed, in mortar, step 2 is added)
The cross-linked binder arrived, grinding uniformly rear scraper for coating is on Copper Foil, and 60 DEG C of vacuum are dried in an oven
Dry, obtain electrode slice；
4) by step 3) in the electrode slice that obtains be placed in tube furnace and calcine under an argon atmosphere,
Precalcining 2 hours at 300 DEG C, then calcine 2 hours at 400 DEG C, after reaction terminates, at argon gas
It is cooled to room temperature under atmosphere protection, obtains the porous silicon negative pole of crosslinking.
Embodiment 3
The method that lithium ion battery porous silicon negative pole is prepared in a kind of original position gelatin-polyvinyl alcohol crosslinked carbonization,
Concretely comprise the following steps:
1) being dissolved in 4ml deionized water by 80mg polyvinyl alcohol, at 80 DEG C, heated and stirred is dissolved；
2) 40mg gelatin being added to step 1) in the solution that obtains, at 60 DEG C, heated and stirred is dissolved,
To cross-linked binder；
3) by after 240mg silica flour and 40mg CNT ground and mixed, in mortar, step 2 is added)
The cross-linked binder obtained, grind uniformly rear scraper for coating on Copper Foil, 60 DEG C of vacuum in an oven
Dry, obtain electrode slice；
4) by step 3) in the electrode slice that obtains be placed in tube furnace and calcine under an argon atmosphere,
Precalcining 2 hours at 300 DEG C, then calcine 1 hour at 600 DEG C, after reaction terminates, at argon gas
It is cooled to room temperature under atmosphere protection, obtains the porous silicon negative pole of crosslinking.
Porous silicon negative electricity pole piece embodiment 1 obtained is as working electrode, and lithium metal is to electrode,
The LiF of 1mol/L6/ EC-DMC (volume ratio 1: 1) is electrolyte, assembles in argon gas atmosphere glove box
Become after lithium ion half-cell, carry out electrochemical property test, voltage range be 0.01～
1.5V(vs.Li+/ Li), electric current density is 400mA g-1。
Test result: the porous silicon negative pole that 600 DEG C of calcinings obtain is at 400mA g-1Fill during lower discharge and recharge
Specific discharge capacity change curve is (embedding lithium) specific capacity and charging (de-lithium) as in figure 2 it is shown, it discharges first
Specific capacity is respectively 1508.7mAh g-1、1164.1mAh g-1, its electric discharge (embedding lithium) after circulating 50 weeks
Specific capacity and charging (de-lithium) specific capacity are respectively 1157.2mAh g-1、1126.5mAh g-1。
Claims (3)
1. the side of lithium ion battery porous silicon negative pole is prepared in original position gelatin-polyvinyl alcohol crosslinked carbonization
Method, it is characterised in that specifically comprise the following steps that
1) being dissolved in deionized water by polyvinyl alcohol, heated and stirred is dissolved；
2) gelatin being added to step 1) in the solution that obtains, heated and stirred is dissolved, and obtains cross-linked binder,
Wherein gelatin is 1:1～0.1:1 with the mass ratio of polyvinyl alcohol；
3) by after silica flour and conductive agent ground and mixed, in mortar, step 2 is added) cross-linked binder that obtains
Agent, wherein the mass ratio of silica flour, polyvinyl alcohol+gelatin and conductive agent is 6:3:1 or 6:2:2, grinds
Uniformly rear scraper for coating is on Copper Foil, and vacuum drying in an oven obtains electrode slice；
4) by step 3) in the electrode slice that obtains be placed in tube furnace and calcine under an inert atmosphere,
Precalcining 1～2 hours at 200～300 DEG C, then calcine 1～2 hour at 300 DEG C～600 DEG C, reaction
After end, under inert atmosphere protection, it is cooled to room temperature, obtains porous silicon negative pole.
2. the method for claim 1, it is characterised in that: step 3) described in conductive agent be
The mixing of one or more in Super-P, acetylene black, graphite or CNT.
3. the method for claim 1, it is characterised in that: step 3) described in baking oven dries
Dry temperature is 30 DEG C～60 DEG C.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106229487A (en) * | 2016-08-25 | 2016-12-14 | 北京化工大学 | The method of lithium-sulfur cell charcoal/lithium sulfide composite positive pole prepared by a kind of carbon thermal reduction lithium sulfate |
| CN108335800A (en) * | 2017-12-29 | 2018-07-27 | 天津工业大学 | Copper silicon integrated electrode and preparation method thereof |
| CN108511740A (en) * | 2017-03-13 | 2018-09-07 | 万向二三股份公司 | A kind of high-specific-capacity silicon carbon electrode coating preparation method |
| CN110299511A (en) * | 2019-05-27 | 2019-10-01 | 南方科技大学 | Nano composite negative plate, preparation method thereof and lithium ion battery |
| CN110828189A (en) * | 2018-08-08 | 2020-02-21 | 丰田自动车株式会社 | Positive electrode for lithium ion capacitor, lithium ion capacitor using same, and method for producing same |
| CN111244454A (en) * | 2019-10-10 | 2020-06-05 | 江苏正力新能电池技术有限公司 | High-proportion silicon cathode water system composite binder and application thereof |
| CN111446426A (en) * | 2019-01-16 | 2020-07-24 | 通用汽车环球科技运作有限责任公司 | Method for manufacturing high performance electrode |
| CN112038631A (en) * | 2020-09-03 | 2020-12-04 | 青海凯金新能源材料有限公司 | Lithium battery electrode plate with surface coated with natural graphite and processing technology thereof |
| CN114788052A (en) * | 2019-12-18 | 2022-07-22 | 瓦尔塔创新有限责任公司 | Battery with metallic lithium anode and method of manufacture |
| CN114975944A (en) * | 2022-06-08 | 2022-08-30 | 陕西科技大学 | Silicon-carbon negative electrode material with high-strength carbon matrix and preparation method thereof |
| CN114975943A (en) * | 2022-06-08 | 2022-08-30 | 陕西科技大学 | Preparation method for constructing gelatin/silicon nanoparticle microspheres based on emulsification self-assembly method |
| CN114975942A (en) * | 2022-06-08 | 2022-08-30 | 陕西科技大学 | Silicon-carbon cathode material with micro/nano structure and preparation method thereof |
| CN116190660A (en) * | 2023-03-10 | 2023-05-30 | 南京航空航天大学 | Adhesive, preparation method and application thereof, silicon-based negative electrode and preparation method thereof |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106229487A (en) * | 2016-08-25 | 2016-12-14 | 北京化工大学 | The method of lithium-sulfur cell charcoal/lithium sulfide composite positive pole prepared by a kind of carbon thermal reduction lithium sulfate |
| CN108511740A (en) * | 2017-03-13 | 2018-09-07 | 万向二三股份公司 | A kind of high-specific-capacity silicon carbon electrode coating preparation method |
| CN108335800A (en) * | 2017-12-29 | 2018-07-27 | 天津工业大学 | Copper silicon integrated electrode and preparation method thereof |
| CN110828189A (en) * | 2018-08-08 | 2020-02-21 | 丰田自动车株式会社 | Positive electrode for lithium ion capacitor, lithium ion capacitor using same, and method for producing same |
| CN110828189B (en) * | 2018-08-08 | 2021-06-15 | 丰田自动车株式会社 | Positive electrode for lithium ion capacitor, and methods for producing same |
| CN111446426A (en) * | 2019-01-16 | 2020-07-24 | 通用汽车环球科技运作有限责任公司 | Method for manufacturing high performance electrode |
| CN110299511A (en) * | 2019-05-27 | 2019-10-01 | 南方科技大学 | Nano composite negative plate, preparation method thereof and lithium ion battery |
| CN110299511B (en) * | 2019-05-27 | 2020-10-09 | 南方科技大学 | Nano composite negative plate, preparation method thereof and lithium ion battery |
| CN111244454A (en) * | 2019-10-10 | 2020-06-05 | 江苏正力新能电池技术有限公司 | High-proportion silicon cathode water system composite binder and application thereof |
| CN114788052A (en) * | 2019-12-18 | 2022-07-22 | 瓦尔塔创新有限责任公司 | Battery with metallic lithium anode and method of manufacture |
| CN112038631A (en) * | 2020-09-03 | 2020-12-04 | 青海凯金新能源材料有限公司 | Lithium battery electrode plate with surface coated with natural graphite and processing technology thereof |
| CN114975944A (en) * | 2022-06-08 | 2022-08-30 | 陕西科技大学 | Silicon-carbon negative electrode material with high-strength carbon matrix and preparation method thereof |
| CN114975943A (en) * | 2022-06-08 | 2022-08-30 | 陕西科技大学 | Preparation method for constructing gelatin/silicon nanoparticle microspheres based on emulsification self-assembly method |
| CN114975942A (en) * | 2022-06-08 | 2022-08-30 | 陕西科技大学 | Silicon-carbon cathode material with micro/nano structure and preparation method thereof |
| CN114975942B (en) * | 2022-06-08 | 2023-06-13 | 陕西科技大学 | Micro/nano structure silicon-carbon negative electrode material and preparation method thereof |
| CN114975944B (en) * | 2022-06-08 | 2023-08-29 | 陕西科技大学 | Silicon-carbon negative electrode material with high-strength carbon matrix and preparation method thereof |
| CN116190660A (en) * | 2023-03-10 | 2023-05-30 | 南京航空航天大学 | Adhesive, preparation method and application thereof, silicon-based negative electrode and preparation method thereof |
| CN116190660B (en) * | 2023-03-10 | 2024-01-30 | 南京航空航天大学 | Adhesive, preparation method and application thereof, silicon-based negative electrode and preparation method thereof |
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