CN109950464A - A kind of porous silicon-carbon cathode pole piece and preparation method thereof - Google Patents
A kind of porous silicon-carbon cathode pole piece and preparation method thereof Download PDFInfo
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- CN109950464A CN109950464A CN201910104110.5A CN201910104110A CN109950464A CN 109950464 A CN109950464 A CN 109950464A CN 201910104110 A CN201910104110 A CN 201910104110A CN 109950464 A CN109950464 A CN 109950464A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to a kind of porous silicon-carbon cathode pole piece and preparation method thereof, then porous silicon-carbon cathode pole piece cleans the preparation method is as follows: to copper foil progress surface etch, dry, preheating；Silicon-carbon cathode slurry is coated on drying copper foil surface using two-sided while extrusion coating machine；Coating pole piece is dried firmly；Two-sided bead is carried out to pole piece with pore creating material；Prelithiation processing is carried out in pole piece；Soft baking is carried out to pole piece, it is dry；Roll-in is carried out to pole piece；It is final to obtain silicon-carbon cathode pole piece finally in its double spread adhesion layer.The present invention obtains porous silicon-carbon cathode by the online pore-creating shot-peening of shot-peening agent, simple process, at low cost, and porous structure effectively inhibits silicon-carbon cathode swelling stress；Prelithiation processing is carried out to pole piece simultaneously and coated with nano adhesion layer is handled, significantly reduces silicon-carbon cathode irreversible capacity loss, enhances pole piece peel strength and flexibility, to improve silicon-carbon cathode coulombic efficiency and cycle life for the first time.
Description
Technical field
The invention belongs to lithium ion battery preparation technical fields, and in particular to a kind of porous carbon cathode pole piece and its preparation side
Method.
Background technique
In recent years, with telecommunications, portable terminal and new-energy automobile etc. to high capacity, long cruising ability it is urgent
Demand develops the research hotspot that high capacity, high magnification, the high performance lithium ion battery of long-life have become new energy field.When
For preceding commercialized lithium ion battery mainly using graphite as cathode, theoretical specific capacity only has 372mAh/g, and battery energy density is promoted
Space is limited.Silicon based anode material is rich because of its theoretical specific capacity high (about 4200mAh/g), de- lithium current potential low (< 0.5V), reserves
Rich, the environmental-friendly, advantages such as cost is relatively low and be considered as great potential next-generation lithium ion battery with high energy density cathode
Material.But silicon based anode material in charge and discharge process along with huge volume change (~300%), based particles are broken
It broken, dusting and falls off；The solid electrolyte layer (SEI) on silicon particle surface constantly grows, is crushed and re-forms, constantly consumption electricity
Solve the lithium source in liquid and anode；To cause huge irreversible capacity loss and quick energy attenuation, battery is recyclable to be made
It is lower with the service life.
In order to reduce the irreversible capacity loss of silicon based anode material, the coulombic efficiency and cycle performance of electrode are improved, is led to
Crossing silicon nanosizing, buffering element is added, constructs porous structure is considered as effective solution method.Piper etc.
(Adv.Mater.2014,26,3520-3525) synthesizes polyacrylonitrile coated Si nanofiber composite wood using method of electrostatic spinning
Material, significantly improves the specific capacity and cycle performance of silicon-based anode.Patent CN106941169A synthesizes silicon-using spray drying process
The porous negative electrode material of graphene is obviously improved and improves the chemical property of silicon based anode material.Although these methods can have
Effect reduces and inhibits the volume expansion of silicon based anode material, improves the specific capacity and cycle performance of electrode, but its preparation process with
Current slurry coating tablet making technology compatibility is poor, while the processes item such as template pore-creating, high temperature cabonization, vapor deposition being related to
It is harsh that part requires high, environmental condition to require, and production efficiency is low, it is difficult to mass production.
Summary of the invention
To solve the above-mentioned problems, the coulombic efficiency for the first time and cycle performance of silicon-carbon cathode are improved, the present invention provides one
Kind porous carbon cathode pole piece and preparation method thereof.Its step are as follows:
(1) copper foil unreels traction to wet etching unit, carries out surface quarter to copper foil using the two-sided spray mode of etching liquid
Erosion；Then two-sided spray clean is carried out to surface etch copper foil；Then it dries, temperature is 80-120 DEG C, while carrying out to copper foil
Preheating；
(2) silicon-carbon cathode slurry is coated on drying copper foil surface using configured back and forth two-sided while extrusion coating machine；
(3) coating pole piece is dried firmly, baking temperature is 80-150 DEG C, baking time 30-90s；
(4) two-sided bead is carried out to pole piece using pore creating material, pore creating material size is 5-20um；
(5) shot-blast unit, which will stablize lithium metal powder (SLMP) and be sprayed at the pole piece dried firmly, carries out prelithiation, lithium metal
Powder particles surface is Li2CO3Clad, lithium powder diameter are 1-10um；
(6) soft baking is carried out to pole piece, temperature is 50-100 DEG C；
(7) micro- roll-in is carried out after pole piece is dry；
(8) final to obtain silicon-carbon cathode pole piece in its double spread adhesion layer after pole piece roll-in.
Further, copper thickness 5-16um, tensile strength > 300MPa, Fe, Si, Mn impurity content are lower than 10ppm；
Further, copper foil surface etching liquid calculates (30-60) %HCl, (20-30) %H by volume fraction2SO4, (10-
50) %H2O2；
Further, the pore creating material is one of ammonium carbonate, ammonium hydrogen carbonate, polyvinylpyrrolidone or a variety of；
Further, the mass ratio of silicon-carbon cathode slurry is carbon-coated nano silicon: graphene: sodium carboxymethylcellulose: fourth
Benzene rubber: deionized water=(70-85): (3-8): (2-5): (2-5): (80-110)；
Further, pole piece adhesion layer is sodium alginate, polyacrylic acid, polyethylene nitrile, chitosan, carboxymethyl cellulose
One of plain sodium, butadiene-styrene rubber, polyimides are a variety of, and surface adhesion layer is with a thickness of 10-100nm.
The invention has the benefit that pore creating material shot-peening is on semisolid cathode pole piece surface, pore creating material heat when pole piece soft baking
It decomposes and generates gas to which porous electrode be made, porous structure can provide the cushion space of silicon-carbon cathode expansion, keep electrode knot
Structure integrality；Porous electrode is prepared using pore creating materials such as ammonium hydrogen carbonate, technical process is simple, controllable, and pore creating material is low in cost,
Pore size distribution$ is uniform, porosity is high, is easy to large-scale production；Lithium powder prelithiation is carried out to porous electrode, lithium powder is uniformly distributed
On silicon-carbon cathode surface, silicon-carbon cathode irreversible capacity loss is can be effectively suppressed in prelithiation, hence it is evident that improve electrode coulombic efficiency and
Performance is recycled；Electrode expansion and deformation can be effectively suppressed in silicon-carbon cathode surface coating adhesion layer, improves and improvement pole piece adds
Work flexibility and cycle performance.
The present invention realizes copper foil roughening, double spread, pole piece pore-creating and prelithiation continuous production, production efficiency
It is high, process flow is short, high degree of automation.
Detailed description of the invention
Fig. 1 is porous silicon-carbon cathode pole piece structure schematic diagram；
Fig. 2 is porous silicon-carbon cathode pole piece preparation process layout；
Fig. 3 is wet process surface etch spray unit structural schematic diagram；
Fig. 4 is the two-sided shot-peening of pole piece and prelithiation schematic device.
Respectively mark is respectively as follows: 001-pore structure in figure；002-lithium metal powder；003-surface adhesion layer；004-copper foil；
005-silicon-carbon active material；11-unwinding units；12-wet etching units；13-copper foil water washing units；14-electric hot-airs
Machine；15-the face A extrusion coated units；16-the face B extrusion coated units；17-dry drying unit firmly；18-shot-peening units；19—
Soft baking drying unit；20-roll-in units；21-rolling units；121-etching liquid spray heads；122-etching liquid pipelines；
123-spray apertures；181-pressure charging valves；182-outlet valves；183-silicon-carbon cathode pole pieces；184-three-way air valves.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples, these embodiments be for illustrating the present invention,
Rather than limiting the invention.
Embodiment 1:
(1) copper foil current collector unreels traction to wet etching unit, is carried out using the two-sided spray mode of etching liquid to copper foil
Surface etch；Copper thickness is 10um, and tensile strength 310MPa, Fe, Si, Mn impurity content is lower than 10ppm；Etching liquid used by
Following substances are matched to obtain as 30%HCl by volume fraction；20%H2SO4；50%H2O2, copper foil surface etch period is 6s；So
After carry out two-sided spray clean；It is dry that online resistance air-heater is carried out after copper foil cleaning, temperature is 100 DEG C, while to copper foil into
Row preheating；
(2) silicon-carbon cathode slurry is coated on drying copper foil surface using two-sided while extrusion coating machine, wherein negative electrode slurry
Mass ratio is carbon-coated nano silicon: graphene: sodium carboxymethylcellulose: butadiene-styrene rubber: deionized water=75:5:5:5:100；
(3) coating pole piece is dried firmly, baking temperature is 120 DEG C, baking time 40s, obtains half dry state pole piece, pole
Piece water content is 20-35%；
(4) two-sided bead is carried out to pole piece using ammonium hydrogencarbonate pore creating material, pore creating material size is 8um；
(5) lithium metal powder (SLMP) will be stablized using shot-blast unit and is sprayed at the pole piece progress prelithiation dried firmly, lithium
Powder particles surface is Li2CO3Clad, lithium powder size are 1um；
(6) soft baking being carried out to pole piece, temperature is 70 DEG C,
(7) micro- roll-in is carried out after pole piece is dry, Roller compression rate is 12%,
(8) use dimple version in pole piece double spread polyacrylic acid adhesion layer after pole piece roll-in, adhesion layer is with a thickness of 10nm.
Embodiment 2:
(1) copper foil current collector unreels traction to wet etching unit, is carried out using the two-sided spray mode of etching liquid to copper foil
Surface etch；Copper thickness is 8um, and tensile strength 305MPa, Fe, Si, Mn impurity content is lower than 10ppm；Copper foil current collector is wet
It is 60%HCl that etching liquid used in method surface etch is calculated by volume fraction；20%H2SO4；20%H2O2, the foil surface etch time is
8s；Then two-sided spray clean is carried out to surface etch copper foil, the drying of online resistance air-heater is carried out after copper foil cleaning, temperature is
120 DEG C, while copper foil is preheated；
(2) silicon-carbon cathode slurry, the negative electrode slurry are coated on drying copper foil surface using two-sided while extrusion coating machine
Mass ratio is carbon-coated nano silicon: graphene: sodium carboxymethylcellulose: butadiene-styrene rubber: deionized water=80:5:4:4:110；
(3) coating pole piece is dried firmly, baking temperature is 80 DEG C, baking time 90s, obtains half dry state pole piece, pole
Piece moisture content is 20-35%；
(4) two-sided bead is carried out to pole piece using Ammonium bicarbonate food grade pore creating material, pore creating material size is 20um；
Particularly, the pore creating material is injected in pole piece in compressed air-driven to tapered, porous spray head；
(5) lithium metal powder (SLMP) will be stablized using shot-blast unit and is sprayed at the pole piece progress prelithiation dried firmly, lithium
Powder particles surface is Li2CO3Clad, lithium powder size are 5um；
(6) soft baking is carried out to pole piece, temperature is 100 DEG C；
(7) micro- roll-in is carried out after pole piece is dry, Roller compression rate is 18-24%；
(8) after pole piece roll-in using dimple version in pole piece double spread sodium alginate adhesion layer, adhesion layer with a thickness of
100nm。
Embodiment 3:
(1) copper foil current collector unreels traction to wet etching unit, is carried out using the two-sided spray mode of etching liquid to copper foil
Surface etch；Copper thickness is 6um, and tensile strength 300MPa, Fe, Si, Mn impurity content is lower than 10ppm；Copper foil current collector is wet
Etch liquids fraction used in method surface etch is 45%HCl, 35%H2SO4, 20%H2O2, copper foil surface etch period is
10s；Two-sided spray clean is carried out to surface etch copper foil, the drying of online resistance air-heater, temperature 80 are carried out after copper foil cleaning
DEG C, while copper foil is preheated；
(2) silicon-carbon cathode slurry, the negative electrode slurry are coated on drying copper foil surface using two-sided while extrusion coating machine
Mass ratio is carbon-coated nano silicon: graphene: sodium carboxymethylcellulose: butadiene-styrene rubber: deionized water=78:6:5:5:105；
(3) coating pole piece is dried firmly, baking temperature is 150 DEG C, baking time 30s, obtains half dry state pole piece, pole
Piece moisture content is 20-35%；
(4) two-sided bead is carried out to pole piece using amine carbonate pore creating material, pore creating material size is 5um；
Particularly, the pore creating material is injected in pole piece in compressed air-driven to tapered, porous spray head；
(5) lithium metal powder (SLMP) will be stablized using shot-blast unit and is sprayed at the pole piece progress prelithiation dried firmly, lithium
Powder particles surface is Li2CO3Clad, lithium powder size are 10um；
(6) soft baking being carried out to pole piece, soft baking temperature is 50 DEG C,
(7) micro- roll-in is carried out after pole piece is dry, Roller compression rate is 20-25%；
(8) it uses dimple version in pole piece double spread sodium carboxymethylcellulose+butadiene-styrene rubber adhesion layer after pole piece roll-in, sticks
Attached layer is with a thickness of 20nm.
Cathode pole piece obtained and NCM523 tertiary cathode piece are assembled into full battery, charge-discharge test is carried out at 1C,
Voltage range is 1.5-3.6V.The porous silicon-carbon cathode of embodiment corresponds to the coulombic efficiency for the first time and 1000 charge and discharge cycles of battery
Capacity retention ratio afterwards is as shown in table 1.
Comparative example 1
Using not carrying out, roughening of copper foil, the silicon-carbon cathode pole piece of bead and prelithiation processing and identical NCM523 are positive
Piece is assembled into full battery, and charge-discharge test, the coulombic efficiency for the first time of 1 silicon-carbon cathode of comparative example and 1000 charge and discharges are carried out at 1C
Capacity retention ratio after electricity circulation is as shown in table 1.
| Coulombic efficiency % for the first time | Capacity retention ratio % after circulation 1000 times | |
| Embodiment 1 | 92.2 | 70.2 |
| Embodiment 2 | 88.5 | 68.5 |
| Embodiment 3 | 90.6 | 69.2 |
| Comparative example 1 | 85.0 | 42.8 |
Table 1: silicon-carbon cathode pole piece electrochemical property test result
The experimental results showed that a kind of porous silicon-carbon cathode pole piece provided by the invention, coulombic efficiency and cycle performance for the first time
It has obtained significantly improving.
Claims (10)
1. a kind of preparation method of porous silicon-carbon cathode pole piece, its step are as follows:
(1) it is performed etching in copper foil surface with etching liquid, is then cleaned, dry, preheating；
(2) silicon-carbon cathode slurry is coated on drying copper foil surface using two-sided while extrusion coating machine；
(3) coating pole piece is dried firmly；
(4) pore creating material is sprayed on pole piece and carries out two-sided bead；
(5) lithium powder is sprayed at pole piece and carries out prelithiation processing；
(6) soft baking is carried out to pole piece, it is dry；
(7) roll-in is carried out to pole piece；
(8) final to obtain silicon-carbon cathode pole piece finally in its double spread adhesion layer.
2. a kind of preparation method of porous silicon-carbon cathode pole piece according to claim 1, it is characterized in that: the copper thickness
For 5-16um, tensile strength is greater than 300MPa, and Fe, Si, Mn impurity content are lower than 10ppm.
3. a kind of preparation method of porous silicon-carbon cathode pole piece according to claim 1, it is characterized in that: in the step 1,
Using two-sided spray mode.
4. a kind of preparation method of porous silicon-carbon cathode pole piece according to claim 1, it is characterized in that: in the step 1,
Etching liquid is calculated by volume fraction, HCl (30-60) %, H2SO4(20-30) %, H2O2(10-50) %, in the drying process, temperature
Degree is 80-120 DEG C.
5. a kind of preparation method of porous silicon-carbon cathode pole piece according to claim 1, it is characterized in that: in the step 2,
The mass ratio of silicon-carbon cathode slurry is carbon-coated nano silicon: graphene: sodium carboxymethylcellulose: butadiene-styrene rubber: deionized water=
(70-85): (3-8): (2-5): (2-5): (80-110).
6. a kind of preparation method of porous silicon-carbon cathode pole piece according to claim 1, it is characterized in that: in the step 3,
Hard temperature of drying is 80-150 DEG C, time 30-90s.
7. a kind of preparation method of porous silicon-carbon cathode pole piece according to claim 1, it is characterized in that: in the step 4,
Pore creating material partial size is 5-20um；Pore creating material is one of ammonium carbonate, ammonium hydrogen carbonate, polyvinylpyrrolidone or a variety of.
8. a kind of preparation method of porous silicon-carbon cathode pole piece according to claim 1, it is characterized in that: in the step 5,
Lithium powder particles surface is Li2CO3Clad, lithium powder diameter are 1-10um.
9. a kind of preparation method of porous silicon-carbon cathode pole piece according to claim 1, it is characterized in that: in the step 6,
Soft baking temperature is 50-100 DEG C.
10. a kind of preparation method of porous silicon-carbon cathode pole piece according to claim 1, it is characterized in that: the step 8
In, pole piece adhesion layer be sodium alginate, polyacrylic acid, polyethylene nitrile, chitosan, sodium carboxymethylcellulose, butadiene-styrene rubber,
One of polyimides (PI) is a variety of, and surface adhesion layer is with a thickness of 10-100nm.
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| CN110444750A (en) * | 2019-08-07 | 2019-11-12 | 宁德新能源科技有限公司 | Negative electrode material and electrochemical appliance and electronic device comprising it |
| CN111933922A (en) * | 2020-08-06 | 2020-11-13 | 中科(马鞍山)新材料科创园有限公司 | Negative pole piece with coating layer, preparation method and application thereof |
| CN112271296A (en) * | 2020-10-20 | 2021-01-26 | 西安工程大学 | Porous conductive soft suspension silicon cathode and preparation method thereof |
| CN113363413A (en) * | 2021-06-02 | 2021-09-07 | 昆山宝创新能源科技有限公司 | Pre-lithiated silicon-based negative electrode plate and preparation method and application thereof |
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