CN109004199B - Preparation method of biomass hard carbon material for negative electrode of sodium-ion battery - Google Patents
Preparation method of biomass hard carbon material for negative electrode of sodium-ion battery Download PDFInfo
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- CN109004199B CN109004199B CN201810859808.3A CN201810859808A CN109004199B CN 109004199 B CN109004199 B CN 109004199B CN 201810859808 A CN201810859808 A CN 201810859808A CN 109004199 B CN109004199 B CN 109004199B
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Abstract
The invention discloses a preparation method of a biomass hard carbon material for a sodium ion battery cathode, which adopts cheap and easily-obtained biomass as a carbon source and prepares the hard carbon material for the sodium ion battery cathode by a simple and convenient method, and can effectively reduce the cost of the sodium ion battery. Meanwhile, the hard carbon material has large carbon layer spacing, can accommodate the intercalation and deintercalation of sodium ions, and the prepared sodium ion battery has excellent electrochemical performance, has good industrialization prospect and is very suitable for being applied to large-scale energy storage systems.
Description
Technical Field
The invention relates to a preparation method of a sodium ion secondary battery cathode material, in particular to a preparation method of a biomass hard carbon material for a sodium ion battery cathode.
Background
Lithium ion secondary batteries have been widely used in mobile devices and electric vehicles in recent years due to their advantages of high energy density, long service life, high rated voltage, good rate capability, low self-discharge, and environmental friendliness. However, the reserves of lithium ore on earth are limited and not evenly distributed. Half of the global lithium ore resources are distributed in the America, and the lithium ore resources in China are not abundant. With the development of lithium ion batteries, the price of lithium ores is inevitably increased, and the lithium ores are exhausted, which is not beneficial to the requirement of sustainable development, so that the application of the lithium ion batteries to a large-scale electrochemical energy storage system may have some problems.
Sodium has been drawing attention because sodium has similar physicochemical properties to lithium as an element belonging to the same group as lithium. The sodium element is used as an element with more than sixth content in the earth crust, the reserve on the earth is far more abundant than that of lithium, the price is lower, and the cost can be effectively reduced if the sodium-ion battery is applied to an electrochemical energy storage system on a large scale. However, in order to meet the requirement of large-scale energy storage devices, the development of sodium ion battery materials with high energy density and sustainability is required.
Since the radius of sodium ions is larger than that of lithium ions, sodium storage capacity exhibited in sodium ion batteries is not high as a graphite material most successfully commercialized in lithium ion batteries. While hard carbon materials are considered to be the most promising anode materials for commercial sodium ion batteries because they have a larger carbon layer spacing than graphite, and are capable of accommodating a larger deintercalation of sodium ions. The biomass hard carbon material is wide in source, green and pollution-free, and is widely concerned by people. At present, reports of preparing biomass hard carbon by using peanut shells, straws and weeds as carbon sources are provided, but the prepared hard carbon material is generally low in capacity and difficult to meet the requirements of commercialization of sodium ion batteries.
Therefore, it is urgently needed to develop a biomass hard carbon material with simple preparation method, low cost and high sodium storage capacity.
Disclosure of Invention
The invention aims to provide a method for preparing a biomass hard carbon material for a cathode of a sodium-ion battery, which is simple to operate. The hard carbon material prepared by the method has the advantages of large specific surface area, rich micropores, simple preparation process and excellent electrochemical performance, and is an excellent sodium-ion battery cathode material.
In order to achieve the purpose, the invention adopts the following technical scheme:
(1) washing the biomass material with deionized water and drying in a vacuum drying oven;
(2) under the atmosphere of protective gas, carbonizing the material obtained in the step (1) at high temperature in a high-temperature furnace; the temperature is 800-1400 ℃, the carbonization time is 2-5 h, and the heating rate is 1-10 ℃/min;
(3) grinding the material obtained in the step (2) into powder, stirring in an acid or alkali solution with the concentration of 0.5-2M for 6-12 h, washing to be neutral by using deionized water, and performing vacuum drying in a vacuum drying oven to obtain the biomass hard carbon material for the cathode of the sodium-ion battery.
Further, the biomass material used in the step (1) is a lotus family plant, including lotus seedpod, lotus seed, lotus leaf, lotus root and other parts of lotus and canary goldthread.
Further, the temperature of vacuum drying in the step (1) is 60-120 ℃, and the time is 8-24 hours.
Further, the protective gas in the step (2) is argon or nitrogen, and the flow rate of the protective gas is 100-300 sccm.
Preferably, the high-temperature carbonization in the step (2) is divided into two-stage heat treatment, wherein the heat treatment temperature of the first stage is 800-1000 ℃, the heating rate is 5-10 ℃/min, and the constant-temperature heat treatment time is 1-2 hours; the heat treatment temperature of the second stage is 1200-1400 ℃, the heating rate is 1-2 ℃/min, and the constant temperature heat treatment time is 1-2 hours. In the first stage of heat treatment process, biomass is pyrolyzed, a large amount of organic molecules are rapidly released, and a rich hole structure is formed; in the second stage of heat treatment, the biomass is slowly graphitized and crystallized, so that the structural strength and the electrical conductivity are improved.
Further, 1.0mol/L hydrochloric acid is preferably used for treating the obtained hard carbon powder material in the step (3), so that the cycle performance and rate capability of the material are improved.
Further, the temperature of vacuum drying in the step (3) is 60-120 ℃, and the time is 8-24 hours.
According to another aspect of the present invention, there is provided a sodium ion battery comprising an anode prepared from the hard carbon anode material prepared according to the above preparation method and an electrolyte, wherein the electrolyte comprises a material selected from NaClO4、NaPF6NaTFSI and NaBF4And a non-aqueous solvent selected from the group consisting of ethylene carbonate, diethyl carbonate, propylene carbonate, dimethyl carbonate, diglyme and glyme.
According to the sodium ion battery of the present invention, the electrolyte preferably contains 1M NaClO4Ethylene Carbonate (EC) and diethyl carbonate (DEC), wherein the volume ratio of Ethylene Carbonate (EC) to diethyl carbonate (DEC) is 1: 1.
According to the sodium ion battery, the negative electrode is prepared by uniformly grinding the hard carbon negative electrode material, acetylene black and a binder (such as polyvinylidene fluoride (PVDF)) according to the mass ratio of 8:1:1, mixing the ground materials with a solvent (such as N-methyl pyrrolidone (NMP)) to prepare negative electrode slurry, and coating the negative electrode slurry on a copper foil current collector.
Compared with the prior art, the invention has the following advantages and technical effects:
the biomass hard carbon material prepared by the invention uses lotus seedpod as a carbon source. The lotus seedpod is a common biomass in life, and is usually discarded in a large amount, so that the lotus seedpod can be used as a carbon source, resources can be effectively saved, and waste is avoided. The biomass hard carbon material used as the negative electrode material of the sodium-ion battery can effectively reduce the cost of the battery. The hard carbon material prepared by the invention has larger carbon layer spacing, larger specific surface area and more micropores, is beneficial to the desorption and adsorption of sodium ions, has higher capacity and has good industrialization prospect.
Drawings
FIG. 1 is an SEM photograph of a biomass hard carbon material prepared in example 1 of the present invention.
FIG. 2 is an XRD pattern of the biomass hard carbon material prepared in examples 1 to 3 of the present invention.
FIG. 3 is a graph showing the carbon dioxide adsorption and desorption curves for preparing the biomass hard carbon material in examples 1 to 3 of the present invention.
FIG. 4 is a graph showing the distribution of pore diameters in the preparation of a biomass hard carbon material in examples 1 to 3 of the present invention.
FIG. 5 is a graph showing the cycle performance at a current density of 50mA/g of batteries fabricated from the biomass hard carbon material according to examples 1 to 3 of the present invention.
Detailed Description
In order that the invention may be better understood, the invention is further illustrated by the following examples, which are intended to be illustrative only and are not to be construed as limiting the invention.
Example 1
A preparation method of a biomass hard carbon material for a sodium ion battery negative electrode comprises the following steps:
1) the lotus seedpod is washed by deionized water and dried in a vacuum drying oven at 80 ℃ for 24 hours;
2) under the argon atmosphere with the flow rate of 200sccm, heating the material obtained in the step 1) to 1000 ℃ at the speed of 5 ℃/min in a tubular furnace, and preserving heat for 1h, then heating to 1200 ℃ at the speed of 2 ℃/min, and preserving heat for 1 h;
3) grinding the material obtained in the step 2) into powder, stirring in a 1M hydrochloric acid solution for 12h, then washing with deionized water to neutrality, and vacuum-drying in a vacuum drying oven at 80 ℃ for 12h to obtain the biomass hard carbon material for the cathode of the sodium ion battery, wherein the label is LS 1200H.
Fig. 1 is an SEM image of the biomass hard carbon material prepared in this example, and it can be seen that many micron-sized pores exist in the material, which are beneficial to the infiltration of electrolyte and the shuttle of sodium ions.
FIG. 2 shows the XRD pattern of the biomass hard carbon material prepared in this example, and the carbon layer spacing can be calculated by Bragg equation
The carbon layer spacing is far larger than that of graphite, and the desorption of sodium ions can be effectively accommodated.
Example 2
A preparation method of a biomass hard carbon material for a sodium ion battery negative electrode comprises the following steps:
1) the lotus seedpod is washed by deionized water and dried in a vacuum drying oven at 80 ℃ for 24 hours;
2) heating the material obtained in the step 1) to 1000 ℃ at a speed of 5 ℃/min in a tubular furnace under the argon atmosphere with the flow rate of 200sccm, and preserving heat for 2 h;
3) grinding the material obtained in the step 2) into powder, stirring in a 1M hydrochloric acid solution for 12h, then washing with deionized water to neutrality, and vacuum-drying in a vacuum drying oven at 80 ℃ for 12h to obtain the biomass hard carbon material for the cathode of the sodium ion battery, wherein the label is LS 1000H.
Example 3
A preparation method of a biomass hard carbon material for a sodium ion battery negative electrode comprises the following steps:
1) the lotus seedpod is washed by deionized water and dried in a vacuum drying oven at 80 ℃ for 24 hours;
2) heating the material obtained in the step 1) to 1400 ℃ in a tubular furnace at a speed of 5 ℃/min under the argon atmosphere with the flow rate of 200sccm, and preserving heat for 2 h;
3) grinding the material obtained in the step 2) into powder, stirring in a 1M hydrochloric acid solution for 12h, then washing with deionized water to neutrality, and vacuum-drying in a vacuum drying oven at 80 ℃ for 12h to obtain the biomass hard carbon material for the cathode of the sodium ion battery, which is labeled as LS 1400H.
Example 4
A preparation method of a biomass hard carbon material for a sodium ion battery negative electrode comprises the following steps:
1) the lotus seedpod is washed by deionized water and dried in a vacuum drying oven at 80 ℃ for 24 hours;
2) heating the material obtained in the step 1) to 1200 ℃ at a speed of 5 ℃/min in a tubular furnace under a nitrogen atmosphere with a flow rate of 200sccm, and preserving heat for 2 h;
3) grinding the material obtained in the step 2) into powder, stirring in a 1M sulfuric acid solution for 12h, then washing with deionized water to neutrality, and vacuum-drying in a vacuum drying oven at 80 ℃ for 12h to obtain the biomass hard carbon material for the cathode of the sodium ion battery.
Example 5
A preparation method of a biomass hard carbon material for a sodium ion battery negative electrode comprises the following steps:
1) the lotus seedpod is washed by deionized water and dried in a vacuum drying oven at 80 ℃ for 24 hours;
2) heating the material obtained in the step 1) to 1200 ℃ at a speed of 2 ℃/min in a tubular furnace under a nitrogen atmosphere with a flow rate of 200sccm, and preserving heat for 2 h;
3) grinding the material obtained in the step 2) into powder, stirring in a 1M hydrochloric acid solution for 12h, then washing with deionized water to neutrality, and vacuum-drying in a vacuum drying oven at 80 ℃ for 12h to obtain the biomass hard carbon material for the cathode of the sodium ion battery.
Example 6
A preparation method of a biomass hard carbon material for a sodium ion battery negative electrode comprises the following steps:
1) the lotus seedpod is washed by deionized water and dried in a vacuum drying oven at 80 ℃ for 24 hours;
2) heating the material obtained in the step 1) to 1200 ℃ at a speed of 5 ℃/min in a tubular furnace under a nitrogen atmosphere with a flow rate of 200sccm, and preserving heat for 5 hours;
3) grinding the material obtained in the step 2) into powder, stirring in a 1M hydrochloric acid solution for 12h, then washing with deionized water to neutrality, and vacuum-drying in a vacuum drying oven at 80 ℃ for 12h to obtain the biomass hard carbon material for the cathode of the sodium ion battery.
Example 7
A preparation method of a biomass hard carbon material for a sodium ion battery negative electrode comprises the following steps:
1) the lotus seedpod is washed by deionized water and dried in a vacuum drying oven at 80 ℃ for 24 hours;
2) heating the material obtained in the step 1) to 1200 ℃ at a speed of 2 ℃/min in a tubular furnace under a nitrogen atmosphere with a flow rate of 200sccm, and preserving heat for 2 h;
3) grinding the material obtained in the step 2) into powder, stirring in a 1M potassium hydroxide solution for 12h, then washing with deionized water to neutrality, and vacuum-drying in a vacuum drying oven at 80 ℃ for 12h to obtain the biomass hard carbon material for the cathode of the sodium-ion battery.
Example 8
A preparation method of a biomass hard carbon material for a sodium ion battery negative electrode comprises the following steps:
1) washing semen Nelumbinis with deionized water, and drying in vacuum drying oven at 80 deg.C for 24 hr;
2) heating the material obtained in the step 1) to 1200 ℃ at a speed of 5 ℃/min in a tubular furnace under the argon atmosphere with the flow rate of 200sccm, and preserving the heat for 2 h;
3) grinding the material obtained in the step 2) into powder, stirring in a 1M hydrochloric acid solution for 12h, then washing with deionized water to neutrality, and vacuum-drying in a vacuum drying oven at 80 ℃ for 12h to obtain the biomass hard carbon material for the cathode of the sodium ion battery.
FIG. 2 is an XRD pattern of the biomass hard carbon material prepared in examples 1 to 3 of the present invention, and the carbon layer spacing can be calculated by Bragg equation. Fig. 3-4 are a carbon dioxide adsorption and desorption curve and a pore size distribution diagram of the biomass hard carbon material respectively, and the specific surface area and the pore volume of the material are calculated by a BET equation. The calculation results are shown in table 1. It can be seen that the material has a large specific surface area and abundant micropores, which is beneficial to the adsorption of sodium ions and enhances the electrochemical performance of the material.
TABLE 1
Sodium ion battery assembly and electrochemical performance testing
(1) Respectively and uniformly mixing the hard carbon powder materials (LS1200H, LS1000H and LS1400H) prepared in the embodiments 1-3, acetylene black and polyvinylidene fluoride (PVDF) binder with a solvent N-methyl pyrrolidone (NMP) according to a mass ratio of 8:1:1 by adopting a smear method, uniformly grinding for 1 hour to prepare negative electrode slurry, coating the negative electrode slurry on a copper foil current collector, and drying for 12 hours in a vacuum drying box at the temperature of 80 ℃; and rolling and cutting to obtain the hard carbon negative pole piece.
(2) Selecting a part of the cut, uniform and complete pole pieces, weighing by using a precision balance, and calculating the mass ((m total-m copper) × 0.8) of the active material; and (3) assembling a CR2032 type button battery together with the positive electrode shell, the negative electrode shell, the glass fiber diaphragm, the sodium sheet (the diameter is 12mm and the thickness is 1mm) and the electrolyte according to correct operation steps in a glove box under the argon atmosphere by using the sodium sheet as a counter electrode and a reference electrode. The electrolyte used is dissolved with 1M NaClO4The assembled battery was sealed with a button cell sealer, taken out from the glove box, and allowed to stand at room temperature for 24 hours.
The electrochemical performance of the prepared sodium ion batteries is respectively tested, the test used instrument is a LAND CT2001A tester (blue electronic Co., Ltd., Wuhan city), the test cycle period is set to be 200 weeks, and specifically: cycling the battery for 200 weeks at a voltage range of 0.01-2.5V and a current density of 50 mA/g; the specific charge capacity (mAh/g) after activation and the specific charge capacity (mAh/g) after 200 cycles of charge and discharge were measured, and the capacity retention ratio after 200 cycles of charge and discharge was calculated (i.e., specific charge capacity after 200 cycles of charge and discharge divided by specific charge capacity after activation × 100%).
Fig. 5 is a graph of the cycle performance of the batteries prepared from the biomass hard carbon materials prepared in examples 1 to 3 at a current density of 50mA/g, and it can be seen that the LS1200H material has a reversible capacity of 328.8mAh/g, and maintains a capacity of 295mAh/g after 200 weeks of cycle, which shows good cycle performance.
Claims (1)
1. A sodium ion battery comprises a positive electrode, a negative electrode and electrolyte, wherein the positive electrode adopts a sodium sheet, and the electrolyte is dissolved with 1M NaClO4The mixed solution of Ethylene Carbonate (EC) and diethyl carbonate (DEC), wherein the volume ratio of EC to DEC is 1: 1; the negative electrode is prepared by uniformly grinding a biomass hard carbon material, acetylene black and a binder polyvinylidene fluoride (PVDF) according to the mass ratio of 8:1:1, mixing with a solvent N-methyl pyrrolidone (NMP) to prepare negative electrode slurry, and coating the negative electrode slurry on a copper foil current collector;
wherein the biomass hard carbon material is prepared by the following preparation method:
1) the lotus seedpod is washed by deionized water and dried in a vacuum drying oven at 80 ℃ for 24 hours;
2) under the argon atmosphere with the flow rate of 200sccm, heating the material obtained in the step 1) to 1000 ℃ at the speed of 5 ℃/min in a tubular furnace, and preserving heat for 1h, then heating to 1200 ℃ at the speed of 2 ℃/min, and preserving heat for 1 h;
3) grinding the material obtained in the step 2) into powder, stirring in 1M hydrochloric acid solution for 12h, then washing with deionized water to neutrality, and vacuum-drying in a vacuum drying oven at 80 ℃ for 12h to obtain the biomass hard carbon material for the cathode of the sodium ion battery;
the hard carbon material has a carbon layer spacing of
The specific surface area is 140.7m2Per g, pore volume 0.055cm3/g。
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