CN115207309A - Preparation method of lithium ion battery electrode material - Google Patents

Preparation method of lithium ion battery electrode material Download PDF

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CN115207309A
CN115207309A CN202210771061.2A CN202210771061A CN115207309A CN 115207309 A CN115207309 A CN 115207309A CN 202210771061 A CN202210771061 A CN 202210771061A CN 115207309 A CN115207309 A CN 115207309A
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sni
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王鹏飞
夏三霞
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Zhangjiagang Jianyou New Material Technology Co ltd
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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
    • H01M4/362—Composites
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    • C—CHEMISTRY; METALLURGY
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    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G19/00—Compounds of tin
    • C01G19/006—Compounds containing, besides tin, two or more other elements, with the exception of oxygen or hydrogen
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M4/04—Processes of manufacture in general
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    • H01M4/02—Electrodes composed of, or comprising, active material
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    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M4/00—Electrodes
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    • H—ELECTRICITY
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    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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    • Y02E60/10—Energy storage using batteries

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Abstract

The invention relates to a preparation method of an electrode material of a lithium ion battery, which is characterized in that 1L of titanium isopropoxide Ti (Oi-Pr) 4 With an appropriate amount of SnCl 2 ·2H 2 Solution mixing of O, adjusting the percentage of Sn doping by the Sn/Ti ratio in the precursor solution, for Sn-TiO 2 Electrospraying the ethanol solution to Cs 2 SnI 6‑x Br x Obtaining the final product Sn-TiO on the surface of the electrode slice 2 /Cs 2 SnI 6‑x Br x And an electrode layer. The prepared battery electrode material has good electrochemical performance and excellent stability.

Description

Preparation method of lithium ion battery electrode material
Technical Field
The invention belongs to the technical field of lithium ion battery preparation, and particularly relates to a preparation method of an electrode material with high specific capacity for a lithium ion battery.
Background
Lithium Ion Batteries (LIBs) have been an effective energy storage system as one of the most promising energy storage devices, until now and in the next few years, although other options such as magnesium, sodium batteries, etc. have been the research power. In order to make the LIB more competitive,conventional LiCoO with high voltage and high capacity electrode material must be sought 2 Cathode and graphite anode alternatives to improve the energy density of existing LIBs systems. The anode portion of a lithium ion battery plays a critical role, while the cathode portion plays a critical role. The conventional graphite-based negative electrode material of the commercially used lithium ion battery not only has low theoretical capacity (372 mAhg) -1 ) And the low power density greatly limits their application to accommodate the development of specific high specific capacity cathode materials.
Today, alloys (Si-Li, sn-Li, etc.), metal oxides (MnO, coO, etc.) and three-dimensional phosphate-based polyanionic structures (VPO 4, liVOPO4, etc.) are receiving much attention as replacement cathodes for conventional graphite-based cathode materials in lithium ion battery applications. Unfortunately, anodes using alloys and metal oxides typically experience severe volume changes during repeated cycling (e.g., about 300% Si, snO) 2 About 250%, etc.) that cause them to electrochemically react with lithium, which can cause the initial particle morphology powder to shatter and crack, thereby causing structural collapse of the active material. Glass anodes, as an alternative to rechargeable LIBs, have also received attention for their unique structure, such as the absence of grain boundaries, randomly distributed structural units and open network structures, as compared to crystalline anode materials. During lithiation, li + Ions may intercalate into structural defects of the amorphous metal oxide or the open network structure of the glass anode. In addition, the presence of percolation pathways in the glass material promotes Li + Diffusion of ions, resulting in higher rate capability. However, a major challenge with the use of glass anodes is also due to Li in the active material + Ions and electrons have a high degree of polarization and slow diffusion, and thus capacity rapidly decays during discharge/charge.
For example, the present invention patent in China with the patent authorization number of CN103078082B is a high-capacity V for lithium ion batteries 2 O 5 A thin film positive electrode material prepared by the method of: (1) Preparation of V 2 O 5 Sol: with powder V 2 O 5 As raw materialsAnd H 2 O 2 Stirring and mixing to prepare V 2 O 5 Sol; (2) preparing sols with different concentrations: the above V is mixed 2 O 5 The sol is prepared in the concentration ranges of: 0.002mol/L to 0.016mol/L sol; (3) pretreating a Pt substrate: immersing the Pt sheet in hydrogen peroxide for 10 minutes, then washing the Pt sheet with deionized water, and naturally drying the Pt sheet; (4) Preparation of V 2 O 5 Film electrode: pipette 10. Mu.L of V at the desired concentration 2 O 5 Spreading the sol on a Pt sheet, naturally air drying, calcining in a muffle furnace at 500 deg.C for 2h, naturally cooling to room temperature to obtain V 2 O 5 And a thin film electrode. V obtained by the invention 2 O 5 The film material has special microscopic appearance, and can improve the specific capacity of the lithium ion battery.
But at V 2 O 5 The glass-based electrode, which is mainly used, has a collapse structure after being cycled for a certain number of times, thereby seriously affecting the service life of the glass-based electrode material.
Disclosure of Invention
Aiming at the problems of low electrochemical performance and short cycle life of the existing glass-based lithium ion battery material in the charging and discharging processes, the invention provides Sn-TiO with high specific capacity and long cycle life 2 /Cs 2 SnI 6-x Br x An electrode material.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the lithium ion battery electrode material comprises the following steps:
1) 1-2kgCsI or CsBr powder mixture was dissolved in 10L of a mixed solvent of deionized water and isopropyl alcohol (deionized water: isopropanol =0.1, 1v/V), sonicated for 1 hour;
2) The solution of step 1) was filled into a stainless steel 27 gauge plastic syringe, the CsI solution was directly electrosprayed onto a copper foil using a syringe pump, and applied between a metal orifice and the ground at a distance of 10cm by a power supply
Figure RE-RE-GDA0003842999790000031
Then is turned onControlling the duration of the electrospray to further regulate the thickness of the CsI or CsBr layer, and heating the electrode plate in a box furnace for 20min;
3) Tin iodide (SnI) was added by a drop coating method 4 ) Or tin bromide (SnBr) 4 ) In ethanol (0.1 g ml) -1 ) The mixed solution in (a) is introduced into the CsI or CsBr layer and the process is repeated several times until the color of the covered CsI and CsBr layer changes from black to light yellow. Heating the electrode slice for 20-30min;
4) 1L of titanium isopropoxide Ti (Oi-Pr) 4 With an appropriate amount of SnCl 2 ·2H 2 Mixing O solution, adjusting Sn doping percentage by Sn/Ti ratio in precursor solution, replacing water with ethanol, performing electro-spray coating on Sn-TiO2 ethanol solution, and spraying to the Cs in the step 3) 2 SnI 6-x Br x Obtaining the final product Sn-TiO on the surface of the electrode slice 2 /Cs 2 SnI 6-x Br x And an electrode layer.
The reaction mechanism is as follows:
(1-x)CsI+xCsBr+SnX 4 (X＝I,Br)→ Cs 2 SnI 6-x Br x
preferably, the spinning speed of the injection pump is controlled at
Figure RE-RE-GDA0003842999790000041
Preferably, the heating is carried out in a Barnstead/Thermolyne mini-bench muffle furnace at a temperature of 1000 ℃ to 5000 ℃ for 20 minutes at ambient temperature.
Compared with the prior art, the invention has the following advantages:
1)Sn-TiO 2 /Cs 2 SnI 6-x Br x the oxidation state of Sn is 4+, which is more stable in the oxidation process and more resistant to hydrolysis in the processing and equipment operation process, and can realize stable electrochemical performance.
2)Sn-TiO 2 /Cs 2 SnI 6-x Br x In a composite structure, sn-TiO is used during the charge and discharge processes 2 Can play a certain protection role and can effectively prevent Cs 2 SnI 6-x Br x The structure is destroyed.
3)Sn-TiO 2 /Cs 2 SnI 6-x Br x The ordered nano phase and the disordered glass phase cooperatively enhance the ion dynamics and the electron dynamics in the charge and discharge process of the composite structure, and the stable structure is maintained in the discharge/charge cycle.
Drawings
FIG. 1 shows Sn-TiO of a lithium ion battery 2 /Cs 2 SnI 6-x Br x Electrode material permeation cycle chart
FIG. 2 shows Sn-TiO of a lithium ion battery 2 /Cs 2 SnI 6-x Br x Charge and discharge curve diagram of electrode material
FIG. 3 shows Sn-TiO of a lithium ion battery 2 /Cs 2 SnI 6-x Br x Cyclic voltammogram of electrode material
FIG. 4 shows Sn-TiO of a lithium ion battery 2 /Cs 2 SnI 6-x Br x Multiplying power diagram of electrode material
Detailed Description
The technical solutions of the present invention will be described clearly and completely below, and it should be apparent that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. Furthermore, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
In the present invention, the raw materials are all commercially available products.
Example 1: preparation method of lithium ion battery electrode material
1) 1kg of the CsI or CsBr powder mixture was dissolved in 10L of a mixed solvent of deionized water and isopropyl alcohol (deionized water: isopropanol =0.1, 1V/V), sonicated for 1 hour;
2) Putting the solution obtained in the step 1) into a plastic injector with a stainless steel needle head of No. 27, and directly electrospraying the CsI solution onto a copper foil by using an injection pumpApplied by power supply at a distance of 10cm between the metal orifice and the ground
Figure RE-RE-GDA0003842999790000051
The thickness of the CsI or CsBr layer is further regulated and controlled by controlling the duration time of the electrospray, and the electrode plate is heated in a box furnace for 20min;
3) Tin iodide (SnI) was applied by drop coating 4 ) Or tin bromide (SnBr) 4 ) In ethanol (0.1 g ml) -1 ) The mixed solution in (a) is introduced into the CsI or CsBr layer and the process is repeated several times until the color of the covered CsI and CsBr layer changes from black to light yellow. Heating the electrode slice for 20-30min;
4) 1L of titanium isopropoxide Ti (Oi-Pr) 4 With 2% SnCl 2 ·2H 2 Mixing O solution, adjusting Sn doping percentage by Sn/Ti ratio in precursor solution, replacing water with ethanol, performing electro-spray coating on Sn-TiO2 ethanol solution, and spraying to the Cs in the step 3) 2 SnI 6-x Br x Obtaining Sn-TiO on the surface of the electrode slice 2 /Cs 2 SnI 6-x Br x Electrode layer
And (3) adding 30 parts by weight of acetylene black and 10 parts by weight of binder into 60 parts of the product obtained in the step (4), grinding and coating the mixture on the surface of the copper foil current collector, and drying, clamping and tabletting to obtain the negative electrode material electrode plate. And sequentially placing the electrode plate, the diaphragm, the LB-008 electrolyte and the lithium sheet into a button battery shell to prepare the lithium ion battery. The above cell assembly process was all performed under an argon atmosphere. And (3) carrying out electrochemical performance test on the prepared battery, wherein the voltage window is 0.01-3V, and the current density is 1A/g.
Example 2: preparation method of lithium ion battery electrode material
1) 1-2kgCsI or CsBr powder mixture was dissolved in 10L of a mixed solvent of deionized water and isopropyl alcohol (deionized water: isopropanol =0.1, 1V/V), sonicated for 1 hour;
2) Putting the solution obtained in the step 1) into a plastic injector with a stainless steel needle head of No. 27, directly electrospraying the CsI solution onto a copper foil by using an injection pump, and passing through a power supplyApplied at a distance of 10cm between the metal orifice and the ground
Figure RE-RE-GDA0003842999790000061
The thickness of the CsI or CsBr layer is further regulated and controlled by controlling the duration time of the electrospray, and the electrode plate is heated in a box furnace for 20min;
3) Tin iodide (SnI) was applied by drop coating 4 ) Or tin bromide (SnBr) 4 ) In ethanol (0.1 g ml) -1 ) The mixed solution in (a) is introduced into the CsI or CsBr layer and the process is repeated several times until the color of the covered CsI and CsBr layer changes from black to light yellow. Heating the electrode slice for 20-30min;
4) 1L of titanium isopropoxide Ti (Oi-Pr) 4 With 2% SnCl 2 ·2H 2 Mixing O solution, adjusting Sn doping percentage by Sn/Ti ratio in precursor solution, replacing water with ethanol, performing electro-spray coating on Sn-TiO2 ethanol solution, and spraying to the Cs in the step 3) 2 SnI 6-x Br x Obtaining Sn-TiO on the surface of the electrode slice 2 /Cs 2 SnI 6-x Br x And an electrode layer.
And (3) adding 30 parts by weight of acetylene black and 10 parts by weight of binder into 60 parts of the product obtained in the step (4), grinding and coating the mixture on the surface of the copper foil current collector, and drying, clamping and tabletting to obtain the negative electrode material electrode plate. And sequentially placing the electrode plate, the diaphragm, the LB-008 electrolyte and the lithium sheet into a button battery shell to prepare the lithium ion battery. The above cell assembly process was all performed under an argon atmosphere. The prepared battery is taken to carry out electrochemical performance test, the voltage window is 0.01-3V, and the current density is 1A/g.
Example 3: preparation method of lithium ion battery electrode material
1) 1-2kgCsI or CsBr powder mixture was dissolved in 10L of a mixed solvent of deionized water and isopropyl alcohol (deionized water: isopropanol =0.1, 1V/V), sonicated for 1 hour;
2) Putting the solution obtained in the step 1) into a plastic injector with a stainless steel needle head of No. 27, directly electrospraying the CsI solution onto a copper foil by using an injection pump, and passing through a power supply at a metal orificeApplied at a distance of 10cm from the ground
Figure RE-RE-GDA0003842999790000081
The thickness of the CsI or CsBr layer is further regulated and controlled by controlling the duration time of the electrospray, and the electrode plate is heated in a box furnace for 20min;
3) Tin iodide (SnI) was applied by drop coating 4 ) Or tin bromide (SnBr) 4 ) In ethanol (0.1 g ml) -1 ) The mixed solution in (a) is introduced into the CsI or CsBr layer and the process is repeated several times until the color of the covered CsI and CsBr layer changes from black to light yellow. Heating the electrode slice for 30min;
4) 1L of titanium isopropoxide Ti (Oi-Pr) 4 With 5% SnCl 2 ·2H 2 Mixing alcohol solution of O, carrying out electro-spray spraying on the Sn-TiO2 alcohol solution, and spraying the solution to the Cs in the step 3) 2 SnI 6-x Br x Obtaining Sn-TiO on the surface of the electrode slice 2 /Cs 2 SnI 6-x Br x Electrode layer
And sequentially placing the electrode plate, the diaphragm, the LB-008 electrolyte and the lithium sheet into a button battery shell to prepare the lithium ion battery. The above cell assembly process was all performed under an argon atmosphere. The prepared battery is taken to carry out electrochemical performance test, the voltage window is 0.01-3V, and the current density is 1A/g.
Example 4: preparation method of lithium ion battery electrode material
1) 1-2kgCsI or CsBr powder mixture was dissolved in 10L of a mixed solvent of deionized water and isopropyl alcohol (deionized water: isopropanol =0.1, 1V/V), sonicated for 1 hour;
2) The solution of step 1) was filled into a stainless steel 27 gauge plastic syringe, the CsI solution was directly electrosprayed onto a copper foil using a syringe pump, and applied between a metal orifice and the ground at a distance of 10cm by a power supply
Figure RE-RE-GDA0003842999790000091
Then the thickness of the CsI or CsBr layer is further regulated and controlled by controlling the duration of the electrospray, and the electrode plate is arranged in a boxHeating in a furnace for 20min;
3) Tin iodide (SnI) was applied by drop coating 4 ) Or tin bromide (SnBr) 4 ) In ethanol (0.1 g ml) -1 ) The mixed solution in (b) is introduced into the CsI or CsBr layer and the process is repeated several times until the color of the covered CsI or CsBr layer changes from black to light yellow. Heating the electrode slice for 20-30min;
4) 1L of titanium isopropoxide Ti (Oi-Pr) 4 And contains 5% of SnCl 2 ·2H 2 Mixing alcohol solution of O, carrying out electro-spray spraying on the Sn-TiO2 alcohol solution, and spraying the solution to the Cs in the step 3) 2 SnI 6-x Br x Obtaining Sn-TiO on the surface of the electrode slice 2 /Cs 2 SnI 6-x Br x And an electrode layer.
And sequentially placing the electrode plate, the diaphragm, the LB-008 electrolyte and the lithium sheet into a button battery shell to prepare the lithium ion battery. The above cell assembly process was all performed under an argon atmosphere. And (3) carrying out electrochemical performance test on the prepared battery, wherein the voltage window is 0.01-3V, and the current density is 1A/g.
Referring to FIG. 2, which shows the cycle performance of example 1 (d), example 2 (c), example 3 (b) and example 4 (a), it can be seen that
Test example 1 showed more excellent electrochemical performance.
Sn-TiO prepared in example 2 2 /Cs 2 SnI 6-x Br x After the cycle test is completed, the battery is disassembled, the electrode material is taken out to be tested by a scanning electron microscope as shown in figure 1, (a) before the cycle with the size of 100 microns, (b) after the cycle with the size of 100 microns, the ordered phase can be found to be uniformly dispersed in the disordered phase, and the good distribution state indicates that the Sn-TiO in the charging and discharging process is shown in the Sn-TiO 2 /Cs 2 SnI 6-x Br x Has a stable structural state and is one of the reasons for good cycle performance. Test example 2:
Sn-TiO prepared in example 2 2 /Cs 2 SnI 6-x Br x The electrode material is tested by using a blue electrode 220E, and specific capacities at current densities of 0.1C, 0.2C, 0.5C, 1C, 2C, 1C, 0.5C, 0.2C and 0.1C can be found in a specific capacity shown in figure 3Are 289mAhg respectively -1 ,215mAhg -1 , 102mAhg -1 ,53mAhg -1 ,24mAhg -1 ,67mAhg -1 ,136mAhg -1 ,223mAhg -1 The material has good cycling stability, which shows that the material can bear large-rate charge and discharge and has good stability.
Test example 3:
Sn-TiO prepared in example 2 2 /Cs 2 SnI 6-x Br x The electrode material adopts CHI660E electrochemical workstation to carry out cyclic voltammetry test, and Sn-TiO can be found from figure 3 2 /Cs 2 SnI 6-x Br x The cyclic voltammograms of (1) are nearly coincident and the first turn of reduction peak occurs at 0.51 eV, 0.72eV, the oxidation peak occurs at 0.25eV,0.48eV is formed by Cs, sn gain and loss electrons, and the first time is due to the formation of the initial discharge SEI film, and Sn-TiO 2 /Cs 2 SnI 6-x Br x The first effect of the method is 92%, has very excellent electrochemical performance, can be further explored, and is used in industrial production.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (3)

1. The preparation method of the electrode material of the lithium ion battery is characterized by comprising the following steps of:
1) 1-2kg of the CsI or CsBr powder mixture was dissolved in 10L of a mixed solvent of deionized water and isopropyl alcohol (deionized water: isopropanol =0.1, 1v/V), sonicated for 1 hour;
2) The solution obtained in the step 1) is filled into a plastic injector with a stainless steel needle head of No. 27, the CsI solution is directly electrosprayed onto a copper foil by using a syringe pump, and the CsI solution is applied between a metal hole opening and the ground at a distance of 10cm through a power supply
Figure FDA0003724221990000011
The thickness of the CsI or CsBr layer is further regulated and controlled by controlling the duration time of the electrospray, and the electrode plate is heated in a box furnace for 20min;
3) Tin iodide (SnI) was added by a drop coating method 4 ) Or tin bromide (SnBr) 4 ) In ethanol (0.1 g ml) -1 ) The mixed solution in (a) is introduced into the CsI or CsBr layer and the process is repeated several times until the color of the covered CsI and CsBr layer changes from black to light yellow. Heating the electrode slice for 20-30min;
4) 1L of titanium isopropoxide Ti (Oi-Pr) 4 With an appropriate amount of SnCl 2 ·2H 2 Mixing O solution, adjusting Sn doping percentage by Sn/Ti ratio in precursor solution, replacing water with ethanol, and adding Sn-TiO 2 Carrying out electrospray spraying on the ethanol solution, and spraying to the Cs in the step 3) 2 SnI 6-x Br x Obtaining the final product Sn-TiO on the surface of the electrode slice 2 /Cs 2 SnI 6-x Br x And an electrode layer.
2. The preparation method of the lithium ion battery electrode material is characterized in that the spinning speed of the injection pump is controlled at
Figure FDA0003724221990000012
3. The preparation method of the electrode material of the lithium ion battery is characterized in that the Barnstead/Thermolyne mini-desk type muffle furnace is heated for 10-20 minutes at the ambient temperature of 1000-5000 ℃.
CN202210771061.2A 2022-06-30 2022-06-30 Preparation method of lithium ion battery electrode material Pending CN115207309A (en)

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