CN108448066A - A kind of preparation method of adhesive-free, nearly room temperature gallium base fluid state metal-silicon composite negative pole without conductive additive - Google Patents
A kind of preparation method of adhesive-free, nearly room temperature gallium base fluid state metal-silicon composite negative pole without conductive additive Download PDFInfo
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- CN108448066A CN108448066A CN201810238524.2A CN201810238524A CN108448066A CN 108448066 A CN108448066 A CN 108448066A CN 201810238524 A CN201810238524 A CN 201810238524A CN 108448066 A CN108448066 A CN 108448066A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
A kind of preparation method of nearly room temperature gallium base fluid state metal silicon composite cathode the invention discloses adhesive-free, without conductive additive, it is related to field of new energy technologies, this method repairs the gap generated when silicon ruptures using the mobility and good electric conductivity of liquid metal, to ensure silicon particle and the good electrical contact of collector, high performance composite negative pole is finally obtained.Simultaneously, using liquid metal gallium, meeting partial oxidation forms the oxide of gallium in whipping process, lead to sticky increase, the principle to improve with the wellability of electrode holder, develop a kind of preparation method for the working electrode not needing adhesive and conductive additive, the preparation process for enormously simplifying working electrode has saved energy use, reduces pollution.
Description
Technical field
The present invention relates to field of new energy technologies more particularly to a kind of adhesive-free, without conductive additive
The preparation method of nearly room temperature gallium base fluid state metal-silicon composite negative pole.
Background technology
Development of EV be countries in the world automobile industry common recognition and competitively strive by hot spot.China is directed to electronic vapour
The problems such as course continuation mileage that vehicle is faced is short and safety is insufficient, clearly proposes Gonna breakthrough high security, long-life, high-energy
Density lithium ion power battery technology bottleneck, one of key among these are exactly to develop the electrode material of height ratio capacity, high security
Material, especially specific capacity are more than the negative material of 1200mAh/g.But existing commercial Li-ion battery negative material master
If graphite, theoretical capacity only has 372mAh/g.In addition, the electrode potential of graphite and lithium metal is very close in high magnification charge and discharge
Surface is easy to that the inhomogeneous deposition of lithium occurs when electric, to cause safety problem.Therefore, it is necessary to find security performance it is more preferable,
The novel anode material of specific capacity higher (>=1200mAh/g).
Silicon is acknowledged as the most potential negative material for substituting graphite and being used for power lithium-ion battery.The theoretical specific volume of silicon
Amount is 4200mAh/g, about the 11 of graphite times, is the highest negative material of theoretical specific capacity so far；Meanwhile the voltage of silicon
Platform is higher than graphite, and security performance is more preferable.But silicium cathode in charge and discharge along with huge volume change, complete lithiumation
Volume expansion is up to 420% afterwards, and silicon electrode is caused to be ruptured, powder due to volume expansion and contraction repeatedly in cyclic process
Change, fall off from collection liquid surface or the conductive network of electrode interior is destroyed, and then electrical contact is lost with collector, eventually leads to
The coulombic efficiency of silicium cathode reduces, high rate performance and cycle performance are deteriorated, and limits the commercial applications of silicium cathode.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of adhesive-free, without conductive additive
The preparation method of nearly room temperature gallium base fluid state metal-silicon composite negative pole, to solve silicon as cell negative electrode material, in charge and discharge process
In gradual dusting, cause to lose electrical contact between internal silicon particle and between silicon and collector, lead to the decline of cycle performance
It needs additionally to add adhesive in technical problem and composite negative pole preparation process and the technical issues of without conductive additive.
The present invention is achieved by the following technical solutions：
The preparation method of a kind of adhesive-free, nearly room temperature gallium base fluid state metal-silicon composite negative pole without conductive additive, packet
Include following steps：
(1) gallium is heated to 40 DEG C and maintained, until gallium melts, obtain liquid metal gallium；
(2) it maintains temperature at 40 DEG C or more, liquid metal gallium is stirred using magnetic agitation method, at this point, liquid metal gallium
Can partial oxidation form the oxide of gallium, cause quality to increase, while viscosity increases, with the electrodes such as silicon chip, stainless steel substrates, copper foil
The wellability of carrier improves；
(3) it Nano/micron silica flour is added, is mixed using churned mechanically mode, obtains uniform slurry, wherein silica flour
Mass ratio is no more than 40%；
(4) slurry is coated on electrode holder, heated under vacuum drying, obtains adhesive-free, is added without conduction
The working electrode of agent, the as described composite negative pole.
Preferably,
The gallium base fluid state metal-silicon composite negative pole also contains In (indium) and/or Sn (tin), general structure Ga-X-Si,
X is In, Sn or In-Sn；To repair the sky generated when silicon ruptures using the mobility of liquid metal and good electric conductivity
Gap ensures silicon particle and the good electrical contact of collector.
The preparation method of the gallium base fluid state metal-silicon composite negative pole further includes stirring liquid metal in magnetic agitation method
Gallium for a period of time after, indium metal block and/or metal block tin are added into liquid metal gallium, obtains liquid Ga-X alloys.Specially：
Indium metal block is added directly in liquid metal gallium, is stirred under atmosphere of inert gases, obtains liquid GaIn eutectic alloys；Or,
Metal block tin is added after liquid metal gallium is heated to 100 DEG C, is stirred under atmosphere of inert gases, obtains liquid GaSn eutectics and closes
Gold；Or, indium metal block and block tin are added after liquid metal gallium is heated to 100 DEG C, stirred under atmosphere of inert gases, obtains liquid
State Ga-In-Sn alloys.
In the step (5), electrode holder is silicon chip, stainless steel substrates or copper foil.
In the step (5), the coating thickness of slurry is 5-100 microns.
In the step (5), the temperature of heating, drying is 50 DEG C.
The present invention has the following advantages compared with prior art：The present invention provides a kind of adhesive-free, without conductive additive
Nearly room temperature gallium base fluid state metal-silicon composite negative pole preparation method, this method utilizes the mobility of liquid metal and good
Electric conductivity is final to obtain height to ensure silicon particle and the good electrical contact of collector the gap that generates when repairing silicon rupture
The composite negative pole of performance.Meanwhile using liquid metal gallium, meeting partial oxidation forms the oxide of gallium in whipping process, causes to glue
Property increase, the principle to improve with the wellability of electrode holder develops a kind of work not needing adhesive and conductive additive
The preparation method of electrode enormously simplifies the preparation process of working electrode, has saved energy use, reduces pollution.
Description of the drawings
Fig. 1 be liquid metal gallium different rotating speeds, different time magnetic agitation after, tested with the wellability of electrode holder
As a result；Wherein, Fig. 1 a are Liquid metal Ga and liquid Ga+Ga-O in different materials surface pictorial diagram, and Fig. 1 b are Liquid metal Ga
At 40 DEG C weight with magnetic agitation rotating speed and mixing time change curve；
Fig. 2 Different electrodes material object photo figure or displaing micro photo figure；Wherein, Fig. 2 a are conventional Si electrode material object photos；Figure
2b is Ga-Si combination electrode material object photos；Fig. 2 c are Ga-Si combination electrode optical microscope photographs；
Fig. 3 is the cyclical stability test result of Ga-Si combination electrodes；
Fig. 4 is the cyclical stability test result of GaIn10-Si combination electrodes.
Specific implementation mode
In following embodiments, method therefor is known to those skilled in the art the routine side of dawn unless otherwise instructed
Method, the materials such as reagent used are commercially available products unless otherwise instructed.
Embodiment 1
A kind of preparation method of Ga-Si composite negative poles is present embodiments provided, is included the following steps：
(1) gallium is heated to 40 DEG C and maintained, until gallium melts, liquid metal gallium is obtained, by liquid metal gallium
After dripping to stainless steel, polysilicon chip, copper foil surface, obtain as shown in Figure 1a results, it can be seen that gallium drips to above-mentioned load
All it is spherical dropping liquid when body surface face, after surface tilts, dropping liquid can be rolled freely, illustrate liquid metal gallium and stainless steel, more
Crystal silicon chip, the wellability of copper foil are very poor；
(2) maintain temperature at 40 DEG C, using magnetic agitation method stir liquid metal gallium, measure different rotating speeds (200rpm,
700rpm) after the magnetic agitation of different time, the weight growth pattern of liquid metal gallium as a result as shown in Figure 1 b, in figure can be with
Find out, with the increase of mixing time, the weight of liquid metal gallium is continuously increased, liquid metal gallium in whipping process with air
In oxygen combine, generate the oxide (Ga-0) of gallium, be cause liquid metal gallium weight increase the reason of；
The liquid metal gallium (mixture of liquid Ga+Ga-0) for taking stirring 300min, is dripped to stainless steel, polysilicon
Piece, copper foil surface, result figure is as shown in 1a, it can be seen from the figure that, and mixture has preferable viscosity, painting that can be highly uniform
The surface of above-mentioned three kinds of materials is overlayed on, a liquid lamella is formed；
(3) the liquid metal gallium for taking 700rpm stirrings 200min, is added micron silica flour, mixed using churned mechanically mode
It closes, obtains uniform slurry, the wherein mass ratio of silica flour is no more than 40%；
(4) slurry is coated on the electrode holders such as polysilicon chip, copper foil surface, coating thickness is 50 microns, vacuum item
The lower 50 DEG C of heating, dryings of part obtain adhesive-free, the Ga-Si combination electrodes (such as Fig. 2 b, c) without conductive additive.With conventional Si
Electrode (such as Fig. 2 a) is compared, and Ga-Si combination electrodes are white, homogeneous.
Using the working electrode of the present embodiment as the cathode of lithium battery, button cell is made, and fill to the battery
Discharge cycles stability test (the results are shown in Figure 3), the results showed that, after 140 cycles, cyclical stability is still up to
1500mAh/g, cyclical stability are preferable.
Embodiment 2
A kind of preparation method of Ga-In-Si composite negative poles is present embodiments provided, is included the following steps：
(1) gallium is heated to 40 DEG C and maintained, until gallium melts, obtain liquid metal gallium；
(2) it maintains temperature at 40 DEG C, liquid metal gallium is stirred using magnetic agitation method, obtain liquid Ga+Ga-O mixing
Object, with the extension of mixing time, it can be seen that the viscosity enhancing of liquid Ga+Ga-O mixtures；
(3) indium metal block (90wt%Ga-10wt%In) is added in liquid Ga+Ga-O mixtures, in inert gas (argon
Gas) hour is stirred under atmosphere, obtain liquid GaIn10 eutectic alloys；
(4) Nano/micron silica flour is added in liquid GaIn10 eutectic alloys, is mixed, is obtained using churned mechanically mode
Uniform slurry is obtained, the wherein mass ratio of silica flour is no more than 40%；
(5) slurry is coated on the electrode holders such as stainless steel, polysilicon chip, copper foil surface, coating thickness is 100 micro-
Rice, the lower 50 DEG C of heating, dryings of vacuum condition obtain adhesive-free, the Ga-In-Si combination electrodes without conductive additive.
Using the combination electrode of the present embodiment as the cathode of lithium battery, button cell is made, and fill to the battery
Discharge cycles stability test (the results are shown in Figure 4), the results showed that, under the test of C/10 multiplying powers, the specific volume after recycling 150 times
Amount is still up to 1530mAh/g, and cyclical stability is fabulous.
Embodiment 3
A kind of preparation method of Ga-Sn-Si composite negative poles is present embodiments provided, is included the following steps：
(1) gallium is heated to 40 DEG C and maintained, until gallium melts, obtain liquid metal gallium；
(2) it maintains temperature at 40 DEG C, liquid metal gallium is stirred using magnetic agitation method, obtain liquid Ga+Ga-O mixing
Object；
(3) metal block tin is added after liquid Ga+Ga-O mixtures being heated to 100 DEG C
(88wt%Ga-12wt%Sn) after stirring a hour under inertia (argon gas) atmosphere, obtains liquid GaSn12
Eutectic alloy；
(4) Nano/micron silica flour is added in liquid GaSn12 eutectic alloys, is mixed, is obtained using churned mechanically mode
Uniform slurry is obtained, the wherein mass ratio of silica flour is no more than 40%；
(5) slurry being coated on the electrode holders such as stainless steel, polysilicon chip, copper foil surface, coating thickness is 5 microns,
The lower 50 DEG C of heating, dryings of vacuum condition obtain adhesive-free, the Ga-Sn-Si composite negative poles without conductive additive.
Embodiment 4
A kind of preparation method of GaInSn-Si composite negative poles is present embodiments provided, is included the following steps：
(1) gallium is heated to 40 DEG C and maintained, until gallium melts, obtain liquid metal gallium；
(2) it maintains temperature at 40 DEG C, liquid metal gallium is stirred using magnetic agitation method, obtain liquid Ga+Ga-O mixing
Object；
(3) after liquid Ga+Ga-O mixtures being heated to 100 DEG C, indium metal block and block tin (68wt%Ga- is added
22wt%In-10wt%Sn), liquid Ga-In-Sn alloys, i.e. GaInSn are obtained after stirring in an inert atmosphere；
(4) Nano/micron silica flour is added in GaInSn, is mixed using churned mechanically mode, obtains uniform slurry,
Wherein the mass ratio of silica flour is no more than 40%；
(5) slurry being coated on the electrode holders such as stainless steel, polysilicon chip, copper foil surface, coating thickness is 20 microns,
The lower 50 DEG C of heating, dryings of vacuum condition obtain adhesive-free, the GaInSn-Si composite negative poles without conductive additive.
It is a kind of detailed embodiment and specific operating process of the present invention above, is before being with technical solution of the present invention
It puts and is implemented, but protection scope of the present invention is not limited to the above embodiments.
Claims (7)
1. the preparation method of a kind of adhesive-free, nearly room temperature gallium base fluid state metal-silicon composite negative pole without conductive additive, special
Sign is, includes the following steps：
(1) gallium is heated to 40 DEG C and maintained, until gallium melts, obtain liquid metal gallium；
(2) it maintains temperature at 40 DEG C or more, liquid metal gallium is stirred using magnetic agitation method；
(3) nanometer or micron silica flour is added, is mixed using churned mechanically mode, obtains uniform slurry, the wherein matter of silica flour
Amount is than being no more than 40%；
(4) slurry is coated on electrode holder, heated under vacuum drying obtains adhesive-free, without conductive additive
The composite negative pole.
2. a kind of adhesive-free according to claim 1, the nearly room temperature gallium base fluid state metal-silicon without conductive additive are compound
The preparation method of cathode, which is characterized in that the gallium base fluid state metal-silicon composite negative pole also contains In and/or Sn, general structure
For Ga-X-Si, X In, Sn or In-Sn.
3. a kind of adhesive-free according to claim 2, the nearly room temperature gallium base fluid state metal-silicon without conductive additive are compound
The preparation method of cathode, which is characterized in that the preparation method of the gallium base fluid state metal-silicon composite negative pole further includes, in magnetic force
After paddling process stirs liquid metal gallium, indium metal block and/or metal block tin are added into liquid metal gallium, obtains liquid Ga-X and closes
Gold.
4. a kind of adhesive-free according to claim 3, the nearly room temperature gallium base fluid state metal-silicon without conductive additive are compound
The preparation method of cathode, which is characterized in that indium metal block is added directly in liquid metal gallium, is stirred under atmosphere of inert gases
It mixes, obtains liquid GaIn eutectic alloys；Or, metal block tin is added after liquid metal gallium is heated to 100 DEG C, in inert gas atmosphere
Lower stirring is enclosed, liquid GaSn eutectic alloys are obtained；Or, indium metal block and block tin are added after liquid metal gallium is heated to 100 DEG C,
It is stirred under atmosphere of inert gases, obtains liquid Ga-In-Sn alloys.
5. a kind of adhesive-free according to claim 1-4, the nearly room temperature gallium base fluid state metal-silicon without conductive additive are multiple
Close the preparation method of cathode, which is characterized in that in the step (4), electrode holder is silicon chip, stainless steel substrates or copper foil.
6. a kind of adhesive-free according to claim 1-4, the nearly room temperature gallium base fluid state metal-silicon without conductive additive are multiple
Close the preparation method of cathode, which is characterized in that in the step (4), the coating thickness of slurry is 5-100 microns.
7. a kind of adhesive-free according to claim 1-4, the nearly room temperature gallium base fluid state metal-silicon without conductive additive are multiple
Close the preparation method of cathode, which is characterized in that in the step (4), the temperature of heating, drying is 50 DEG C.
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| CN112751077A (en) * | 2019-10-30 | 2021-05-04 | 通用汽车环球科技运作有限责任公司 | Liquid metal interfacial layer for solid electrolyte and method therefor |
| CN113555527A (en) * | 2021-07-21 | 2021-10-26 | 珠海冠宇电池股份有限公司 | Negative plate and lithium ion battery |
| CN113991194A (en) * | 2021-10-29 | 2022-01-28 | 山东大学 | Liquid metal modified two-dimensional siloxene cathode and preparation method and application thereof |
| CN114005995A (en) * | 2021-11-01 | 2022-02-01 | 天津理工大学 | Preparation method of flexible metal electrode |
| CN115425248A (en) * | 2022-10-14 | 2022-12-02 | 吉林大学 | Noble metal loaded multilayer hollow microsphere liquid metal-based catalyst and preparation method thereof |
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| CN113991194A (en) * | 2021-10-29 | 2022-01-28 | 山东大学 | Liquid metal modified two-dimensional siloxene cathode and preparation method and application thereof |
| CN113991194B (en) * | 2021-10-29 | 2023-08-15 | 山东大学 | Liquid metal modified two-dimensional siloxanene negative electrode and preparation method and application thereof |
| CN114005995A (en) * | 2021-11-01 | 2022-02-01 | 天津理工大学 | Preparation method of flexible metal electrode |
| CN114005995B (en) * | 2021-11-01 | 2023-11-10 | 天津理工大学 | Preparation method of flexible metal electrode |
| CN115425248A (en) * | 2022-10-14 | 2022-12-02 | 吉林大学 | Noble metal loaded multilayer hollow microsphere liquid metal-based catalyst and preparation method thereof |
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