CN110299512A - A kind of preparation method of the lithium metal battery cathode of carbon/tin multiple base support - Google Patents
A kind of preparation method of the lithium metal battery cathode of carbon/tin multiple base support Download PDFInfo
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- CN110299512A CN110299512A CN201910553278.4A CN201910553278A CN110299512A CN 110299512 A CN110299512 A CN 110299512A CN 201910553278 A CN201910553278 A CN 201910553278A CN 110299512 A CN110299512 A CN 110299512A
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H01M4/04—Processes of manufacture in general
- H01M4/0483—Processes of manufacture in general by methods including the handling of a melt
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- 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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Abstract
A kind of preparation method of the lithium metal battery cathode of carbon/tin multiple base support; hydro-thermal reaction is used first; tin oxide is carried on commercial carbon cloth; then heat under conditions of inert gas shielding; in carbon cloth surfaces in-situ preparation metallic tin; finally using metallic tin as close lithium site, the lithium metal of heating melting is carried on complex matrix, improved cathode of lithium is obtained；It is characteristic of the invention that metallic tin is utilized to the dual compatibility of carbon cloth and lithium metal, when improving lithium metal battery cathode circulation the defects of dendritic growth, it is prepared for the lithium metal battery cathode compared with high circulation stability and battery capacity and lower non-energy consumption of reaction.
Description
Technical field
The present invention relates to the preparation of cell negative electrode material, in particular to the lithium metal electricity of a kind of carbon/tin multiple base support
The preparation method of pond cathode.
Background technique:
Efficiently, the development of clean new energy is also that country becomes socialist modernization power, Optimization of Energy Structure
An important ring.Electrochemical energy storage is a part indispensable in new energy field, as most representative electrochemical energy storage
The development of one of device, lithium battery is concerned.Commercial li-ion battery is already close to its attainable theoretical limit of institute at present,
And requirement of the people to battery performance is being continuously improved, therefore, developing has the battery material of high-energy density extremely urgent.
Theoretical capacity (3860mAhg of the lithium metal due to its superelevation-1), low electrode potential (- 3.04V vs SHE) and by extensive
Concern and research.But the dendrite that lithium anode is formed during battery repeated charge makes the safety of battery
At extreme influence, the practical application process of lithium metal battery is seriously hindered.
Researcher uses all multi-methods to improve these defects, inhibits branch for example, by using the solid electrolyte of high-modulus
Brilliant undue growth prevents it from piercing through diaphragm and causes short circuit；Additive is added into electrolyte to promote high stability
The generation of SEI film and to SEI film carry out it is manually modified.However these methods can not solve this problem of the volume change of lithium.
Studies have shown that using having the base material of " close lithium " to modify lithium an- ode, it can be from increase cathode specific surface
Multiple angles such as product, control current density inhibit the growth of Li dendrite, avoid battery that short circuit occurs in cyclic process, reduce
The volume change of lithium metal.Developing low-cost, the host material with regulation lithium deposition and dissolution are for promoting lithium metal battery
Practical application process it is particularly important.
Summary of the invention:
The problems such as dendritic growth in order to solve lithium metal battery cathode, improves the cyclical stability of lithium metal battery cathode
And working efficiency, the purpose of the present invention is to provide a kind of preparation sides of carbon/tin multiple base support lithium metal battery cathode
Method improves the close lithium of carbon cloth using metallic tin to the dual compatibility of carbon and lithium by loading one layer of metallic tin in carbon cloth surfaces
Property, then at carbon/tin surfaces carried metal lithium, obtain carbon/tin multiple base support lithium metal battery cathode.
In order to achieve the above object, the technical solution of the present invention is as follows:
A kind of preparation method of the lithium metal battery cathode of carbon/tin multiple base support, comprising the following steps:
Step 1: weighing potassium stannate and urea is dissolved in the mixed solution of water and ethyl alcohol, after mixing evenly, solution is added
In hydrothermal reaction kettle, the commercial carbon cloth cut is added, product after reaction, is washed with deionized and is dried by heating
It is dry；
Step 2: first step products therefrom is calcined in inert atmosphere furnace, reaction terminates, obtained carbon/tin composite support
After the cooling room temperature of timbering material, product is transferred to vacuum environment；
Step 3: commercial lithium piece is melted at a temperature of 300~350 DEG C under vacuum conditions, then by composite support material
It is infiltrated on molten metal lithium, completes load, obtained product is exactly that carbon/tin composite material support lithium metal battery is negative
Pole.
The first step specifically: weigh 0.05~0.5g potassium stannate and 0.5~3g urea be dissolved in 10~40mL water and
In the mixed solution of 10~40mL ethyl alcohol, after mixing evenly, solution is added in hydrothermal reaction kettle, 1~4 piece of diameter 5- is added
The commercial carbon cloth that 15mm is cut heats 18~24 hours, after reaction by product deionization at 160~240 DEG C
Water washing 3~5 times is simultaneously dried.
The second step specifically: 400~600 DEG C of calcinings 2 are small in inert atmosphere furnace by first step products therefrom
When, heating rate is 5 DEG C of min-1, reaction terminates, and after the cooling room temperature of obtained carbon/tin composite support material, product is transferred to
Vacuum environment.
It is had the following characteristics that using carbon/tin multiple base support lithium metal battery cathode that the present invention prepares
One, carbon/tin composite substrate parent's lithium is preferable, the load of lithium metal can be completed in 20 seconds, and in circulating battery
In the process, metallic tin can effectively improve the deposition efficiency of lithium ion in carbon cloth surfaces as close lithium site.
Two, specific surface area is higher, and lithium ion is made to have more space sites in attachment it can be selected that so as to avoid negative
The protrusion of pole surface, it is suppressed that the generation of dendrite, and improve the transport efficiency of lithium.
Three, the cathode of lithium of multiple base support possesses higher battery capacity and cyclical stability.This method is lithium metal
The design of the supporter of cathode provides new thinking, using the carbon of metallic tin, the dual compatibility of lithium, improves carbon material parent lithium
While improve the stability of lithium metal battery cathode, provide thinking for the extensive use of lithium an- ode.
Detailed description of the invention
Fig. 1 is that carbon/tin multiple base support lithium anode Symmetrical cells and general commercial lithium metal Symmetrical cells exist
1mA·cm-2Under circulation correlation curve.
Fig. 2 is the full battery and general commercial of carbon/tin multiple base support lithium anode and LiFePO4 composition
Circulation of the full battery of lithium anode and LiFePO4 composition under conditions of 0.1C, 0.2C, 0.5C, 1C, 2C, which compares, to be illustrated
Figure.
Fig. 3 is the full battery of carbon/tin multiple base support lithium anode and LiFePO4 composition under the conditions of 0.2C
Circulation charge and discharge specific discharge capacity and coulombic efficiency schematic diagram.
Specific embodiment:
Below with reference to embodiment, the present invention is described in further detail.
Embodiment one
The present embodiment the following steps are included:
Step 1: weighing 0.108g potassium stannate, 0.675g urea is dissolved in the mixed solution of 15mL water and 15mL ethyl alcohol,
After mixing evenly, solution is added in hydrothermal reaction kettle, the commercial carbon cloth that 3 pieces of diameter 10mm are cut is added, at 180 DEG C
18 hours of lower heating, product is washed with deionized 3 times after reaction and is dried；
Step 2: first step products therefrom is calcined 2 hours for 600 DEG C in inert atmosphere furnace, heating rate is 5 DEG C of min-1, reaction terminates, and after the cooling room temperature of obtained carbon/tin composite support material, product is transferred to vacuum environment；
Step 3: under vacuum conditions melting commercial lithium piece at a temperature of 300 DEG C, then composite support material is infiltrated
In molten metal lithium, load is completed, obtained product is exactly carbon/tin composite material support lithium metal battery cathode.
Composite negative pole material can be improved the stability and displacement volume of cathode of lithium, as shown in Figure 1, the symmetrical electricity assembled
It pond can be and 1mAcm-2Constant current density, 1 mAhcm-2Charge/discharge capacity under conditions of to stablize circulation super
900 hours are spent, and keep overpotential in 4mV, in 5mAcm-2Under conditions of can stablize and circulate beyond 500 circles.With business
The full battery of LiFePO4 assembling is carrying out circulation formula, as shown in Fig. 2, discharge capacity can be kept under conditions of 2C
For 130mAhg-1, realize 85.52% or more displacement volume.In addition, the circulation specific discharge capacity of full battery can exceed that
155mAh·g-1, it still is able to after 200 circulations more than 142mAhg-1, as shown in figure 3, chemical property has clear improvement.
Embodiment two
The present embodiment the following steps are included:
Step 1: weighing 0.216g potassium stannate, 1.675g urea is dissolved in the mixed solution of 20mL water and 20mL ethyl alcohol,
After mixing evenly, solution is added in hydrothermal reaction kettle, the commercial carbon cloth that 3 pieces of diameter 5mm are cut is added, at 180 DEG C
24 hours are heated, product is washed with deionized 3 times after reaction and are dried；
Step 2: first step products therefrom is calcined 2 hours for 600 DEG C in inert atmosphere furnace, heating rate is 5 DEG C of min-1, reaction terminates, and after the cooling room temperature of obtained carbon/tin composite support material, product is transferred to vacuum environment；
Step 3: under vacuum conditions melting commercial lithium piece at a temperature of 300 DEG C, then composite support material is infiltrated
In molten metal lithium, load is completed, obtained product is exactly carbon/tin composite material support lithium metal battery cathode.
Obtained carbon/tin complex matrix support lithium an- ode cyclical stability with higher and real work are held
Amount.
Embodiment three
The present embodiment the following steps are included:
Step 1: weighing 0.5g potassium stannate, 3g urea is dissolved in the mixed solution of 40mL water and 40mL ethyl alcohol, stirs evenly
Afterwards, solution is added in hydrothermal reaction kettle, adds the commercial carbon cloth that 4 pieces of diameter 10mm are cut, 24 are heated at 240 DEG C
Hour, product is washed with deionized 5 times after reaction and is dried；
Step 2: first step products therefrom is calcined 2 hours for 600 DEG C in inert atmosphere furnace, heating rate is 5 DEG C of min-1, reaction terminates, and after the cooling room temperature of obtained carbon/tin composite support material, product is transferred to vacuum environment；
Step 3: under vacuum conditions melting commercial lithium piece at a temperature of 350 DEG C, then composite support material is infiltrated
In molten metal lithium, load is completed, obtained product is exactly carbon/tin composite material support lithium metal battery cathode.
Obtained carbon/tin complex matrix support lithium an- ode cyclical stability with higher and real work are held
Amount.
Example IV
The present embodiment the following steps are included:
Step 1: weighing 0.05g potassium stannate, 0.5g urea is dissolved in the mixed solution of 10mL water and 10mL ethyl alcohol, stirring
After uniformly, solution is added in hydrothermal reaction kettle, the commercial carbon cloth that 1 piece of diameter 15mm is cut is added, added at 160 DEG C
Hot 18 hours, product is washed with deionized 3 times after reaction and is dried；
Step 2: first step products therefrom is calcined 2 hours for 600 DEG C in inert atmosphere furnace, heating rate is 5 DEG C of min-1, to the end of reacting, after the cooling room temperature of carbon to be obtained/tin composite support material, product is transferred to vacuum environment；
Step 3: under vacuum conditions melting commercial lithium piece at a temperature of 300 DEG C, then composite support material is infiltrated
In molten metal lithium, load is completed, obtained product is exactly carbon/tin composite material support lithium metal battery cathode.
Obtained carbon/tin complex matrix support lithium an- ode cyclical stability with higher and real work are held
Amount.
Claims (4)
1. a kind of preparation method of carbon/tin multiple base support lithium metal battery cathode, which is characterized in that including following step
It is rapid:
Step 1: weighing potassium stannate and urea is dissolved in the mixed solution of water and ethyl alcohol, after mixing evenly, hydro-thermal is added in solution
In reaction kettle, the commercial carbon cloth cut is added, product is washed with deionized and is dried after reaction by heating；
Step 2: first step products therefrom is calcined in inert atmosphere furnace, reaction terminates, obtained carbon/tin composite support timbering
After expecting cooling room temperature, product is transferred to vacuum environment；
Step 3: melting commercial lithium piece at a temperature of 300~350 DEG C under vacuum conditions, then composite support material is infiltrated
In molten metal lithium, load is completed, obtained product is exactly carbon/tin composite material support lithium metal battery cathode.
2. a kind of preparation method of the lithium metal battery cathode of carbon/tin multiple base support according to claim 1, special
Sign is, the first step specifically: weigh 0.05~0.5g potassium stannate and 0.5~3g urea is dissolved in 10~40mL water and 10
In the mixed solution of~40mL ethyl alcohol, after mixing evenly, solution is added in hydrothermal reaction kettle, 1~4 piece of diameter 5- is added
The commercial carbon cloth that 15mm is cut heats 18~24 hours, after reaction by product deionization at 160~240 DEG C
Water washing 3~5 times is simultaneously dried.
3. a kind of preparation method of the lithium metal battery cathode of carbon/tin multiple base support according to claim 1, special
Sign is, the second step specifically: first step products therefrom is calcined 2 hours for 400~600 DEG C in inert atmosphere furnace,
Heating rate is 5 DEG C of min-1, reaction terminates, and after the cooling room temperature of obtained carbon/tin composite support material, product is transferred to vacuum
Environment.
4. a kind of preparation method of the lithium metal battery cathode of carbon/tin multiple base support according to claim 1, special
Sign is,
Step 1: weighing 0.108g potassium stannate, 0.675g urea is dissolved in the mixed solution of 15mL water and 15mL ethyl alcohol, and stirring is equal
After even, solution is added in hydrothermal reaction kettle, the commercial carbon cloth that 3 pieces of diameter 10mm are cut is added, heats 18 at 180 DEG C
Product is washed with deionized 3 times after reaction and dried by a hour；
Step 2: first step products therefrom is calcined 2 hours for 600 DEG C in inert atmosphere furnace, heating rate is 5 DEG C of min-1, instead
It should terminate, after the cooling room temperature of obtained carbon/tin composite support material, product is transferred to vacuum environment；
Step 3: under vacuum conditions melting commercial lithium piece at a temperature of 300 DEG C, then composite support material is infiltrated on molten
The lithium metal melted, completes load, and obtained product is exactly carbon/tin composite material support lithium metal battery cathode.
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Cited By (9)
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| CN111613773A (en) * | 2020-04-21 | 2020-09-01 | 浙江锋锂新能源科技有限公司 | Composite of glass fiber with hierarchical structure and metallic lithium and preparation method thereof |
| CN111952567A (en) * | 2020-08-18 | 2020-11-17 | 武汉工程大学 | Organic lithium-philic composite cathode taking three-dimensional conductive carbon material as substrate and preparation method thereof |
| CN112713260A (en) * | 2019-10-25 | 2021-04-27 | 广州汽车集团股份有限公司 | Flexible lithium metal battery cathode, preparation method thereof and lithium metal battery |
| CN113782730A (en) * | 2021-08-18 | 2021-12-10 | 武汉理工大学 | Carbon cloth-based potassium metal composite electrode and preparation method and application thereof |
| CN114512637A (en) * | 2022-01-20 | 2022-05-17 | 武汉工程大学 | Three-dimensional composite lithium metal cathode with multifunctional interface layer and preparation method thereof |
| CN114551895A (en) * | 2021-07-08 | 2022-05-27 | 万向一二三股份公司 | Manufacturing method of flexible lithium metal battery cathode |
| CN114678508A (en) * | 2022-04-13 | 2022-06-28 | 电子科技大学长三角研究院(湖州) | Carbon-based supported metal sulfide composite material and preparation method and application thereof |
| CN115513427A (en) * | 2022-09-15 | 2022-12-23 | 大连大学 | Composite lithium metal negative electrode and preparation method thereof |
| CN116014071A (en) * | 2023-02-16 | 2023-04-25 | 吉林省翰驰科技有限公司 | Preparation method of three-dimensional lithium metal anode |
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| CN111613773B (en) * | 2020-04-21 | 2022-06-14 | 浙江锋锂新能源科技有限公司 | Composite of glass fiber with hierarchical structure and metallic lithium and preparation method thereof |
| CN111613773A (en) * | 2020-04-21 | 2020-09-01 | 浙江锋锂新能源科技有限公司 | Composite of glass fiber with hierarchical structure and metallic lithium and preparation method thereof |
| CN111952567A (en) * | 2020-08-18 | 2020-11-17 | 武汉工程大学 | Organic lithium-philic composite cathode taking three-dimensional conductive carbon material as substrate and preparation method thereof |
| CN111952567B (en) * | 2020-08-18 | 2023-09-22 | 武汉工程大学 | Organic lithium-philic composite negative electrode with three-dimensional conductive carbon material as substrate and preparation method thereof |
| CN114551895A (en) * | 2021-07-08 | 2022-05-27 | 万向一二三股份公司 | Manufacturing method of flexible lithium metal battery cathode |
| CN114551895B (en) * | 2021-07-08 | 2023-10-03 | 万向一二三股份公司 | Manufacturing method of flexible lithium metal battery negative electrode |
| CN113782730A (en) * | 2021-08-18 | 2021-12-10 | 武汉理工大学 | Carbon cloth-based potassium metal composite electrode and preparation method and application thereof |
| CN114512637A (en) * | 2022-01-20 | 2022-05-17 | 武汉工程大学 | Three-dimensional composite lithium metal cathode with multifunctional interface layer and preparation method thereof |
| CN114678508A (en) * | 2022-04-13 | 2022-06-28 | 电子科技大学长三角研究院(湖州) | Carbon-based supported metal sulfide composite material and preparation method and application thereof |
| CN115513427A (en) * | 2022-09-15 | 2022-12-23 | 大连大学 | Composite lithium metal negative electrode and preparation method thereof |
| CN116014071A (en) * | 2023-02-16 | 2023-04-25 | 吉林省翰驰科技有限公司 | Preparation method of three-dimensional lithium metal anode |
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