Method of nanocrystalline composite cathode materials lixfeymzsio4/c

FIELD: metallurgy.

SUBSTANCE: initial components represent SiO2 or titaniferous magnetite and SiO2 to be mixed with carbonate Li(Li2CO3) at the ratio of 55-70 mol. % initial components, Li2CO3 and FeCO3 making the rest in equal amounts of cathode materials LixFeyMzSiO4/C. Then, powder is fused at 1180±5°C. After cooling, obtained alloy is ground to introduce therein, as high-molecular compound, polymethyl methacrylate or soot in amount of 2-5% of alloy. Then, thermal treatment is performed in cycling mode. For this it is heated to ≥600°C and held for 55-65 minutes. Now, it is cooled to room temperature in 5-10 cycles along with powder surface modification by carbon at heating.

EFFECT: storage battery higher discharge capacity.

5 dwg, 8 ex

 

The invention relates to a technology for obtaining nanocrystalline cathode materials used in lithium-ion batteries used in automotive, machinery, energy, aerospace and marine applications.

A method of obtaining highly dispersed cathode materials in LixFeyMzPO4/C [RF Patent №2444815]. Spend a mixture of lithium compounds with iron oxide and one or more compounds of metals with oxidation 2+, 3+, 4+, 5+, which suppliers ion-deputies from among the oxides, hydroxides or salts of phosphorus compounds containing PO43+group, and a carbon-containing compounds.

Original mix components and activate in mechanochemical activator, after which the resulting mixture was subjected to heat treatment at 650-800°C, cooled to room temperature and dispersed in mechanochemical activator, all processes are carried out in an inert atmosphere, and surface modification is carried out using carbon-containing compounds that are simultaneously active as a reducing agent and covering agent.

The disadvantage of this method is to obtain low values of capacitance. The method is quite expensive, complicated and unfair.

A method of obtaining the cathode material is a Sol-gel method [.Deng, S.Zhang Sinthesis and characterization of Li2Fe0.97Zn0.03SiO4(M=Zn2+, Cu2+, Ni2+) cathode materials for lithium ion batteries // Power sources, 196 (2011), p.386-392]. In this method was synthesized Li2Fe0.97Zn0.03SiO4. The hydrate of lithium acetate, citrate of iron, zinc acetate, tetraethylorthosilicate and citric acid were used as starting materials. The hydrate of lithium acetate, iron, and zinc are first dissolved in distilled water. A saturated aqueous solution of citric acid is added slowly to the above solution under stirring with a magnetic stirrer. To the resulting homogeneous solution was added a solution of ethanol tetraethylorthosilicate. Under a magnetic stirrer, the stirring was conducted at 80°C for 12 hours to obtain a transparent greenish solution. Then the solution was again stirred with a magnetic stirrer at 75°C for evaporation of ethanol and water. In the wet gel was dried in a vacuum oven at 100°C. the Dry gel is then calcined at 700°C for 12 h in an argon flow. Instead of zinc acetate can also be used as starting materials, the copper acetate and Nickel acetate.

The drawback of this method is costly, and the Sol-gel method is not industrial in comparison with solid-phase reactions and reactions in the liquid phase.

The known method proceduralizing cathode material 0.8Li 2FeSiO4/0.4Li2SiO3/C and Li2FeSiO4/C in the stoichiometric ratio of Li:Fe:Si1/43:1:1,5 (low Fe content compared to pure Li2FeSiO4with application of the synthesis, selected as a prototype [Jingyu Bai, Zhengliang Gong Nanostructured 0,8Li2FeSiO4/0,4Li2SiO3/C composite cathode material with enhanced electrochemical performance for lithium-ion batteries // J. Mat. Chem., No. 22, 2012, p.12128-12132]. As a precursor was used 0,8Li2FeSiO4/0,4Li2SiO3/C. For the synthesis was used Sol-gel method. 0,008 mol of iron powder and to 0.016 mol of citric acid were mixed in 30 ml of deionized water and stirred at 80°C. Then the stoichiometric LiAc·2H2O (0,024 mol) and Si(OC2H5)4(0.012 mol) are dissolved and then continue stirring for another 4 hours. 0.01 mol of ethylene glycol is added to the solution and heated to 120°C, incubated for 2 hours for polymerization and dried at 70°C in vacuum. After drying, is crushed into a powder and calcined in a stream of argon at 650°C for 10 h After which the cathode material is mixed with acetylene and a binder of polyvinylidene fluoride (PVDF) in a weight ratio of 80:10:10 in a ball mill at a speed of 500 pmin-1within 4 hours, using as solvent N-methyl-2-pyrolidone (NRM). Then the suspension is applied on aluminum foil and dried in HAC is the mind at 70°C for 2 hours. In the method used amorphous Li2SiO3(lithium-ion conductor) as a transmission channel for improved lithium ion diffusion in Li2Fe-SiO4and 0.8Li2FeSiO4/0.4Li2SiO3/C composite material, which contains an active cathode material in Li2FeSiO4in the crystalline phase, surrounded by amorphous Li2SiO3. The resulting material formed secondary micron size particles with primary nanocrystallites (20 nm)comprising an active cathode material in Li2FeSiO4in the crystalline phase, surrounded by amorphous Li2SiO3and amorphous carbon.

The disadvantage of this method is the high cost of the process, its complexity, and quite time consuming, and relatively low values of specific discharge capacity of the material.

The task is to develop a simple, rapid and cheap method of producing nanocrystalline composite cathode materials in LixFeyMzSiO4/C and the increase in specific discharge capacity of the material.

For solving the problem of method for obtaining nanocrystalline composite cathode materials in LixFeyMzSiO4A /C, which consists in the fact that, as initial components choose SiO2or titanomagnetite and SiO2in equal amounts, is the quiet mixed with Li carbonate (Li 2CO3) in the ratio of 55-70 mol.% from the source, the rest of Li2CO3and FeCO3in equal amounts. Melt the powder at a temperature of 1180±5°C. Then cooling the alloy to the formation of the amorphous structure. According to x-ray analysis and electron microscopy these materials are amorphous (figure 1). Thus, the homogeneity of the structure.

For uniform distribution of carbon and coating material particles carry out the grinding of amorphous alloy with high molecular compound (methyl methacrylate) (PMMA) or carbon black in an amount of from 2 to 5% of the alloy. The particle size after grinding is 100-2000 nm. Next, perform a heat treatment in the mode of Cycling, and it is heated to a temperature of ≥600°C, incubated for 55-65 minutes, cooled to room temperature, perform 5-10 cycles, combining with the heating surface modification of the carbon powder.

Grinding allows the graft polymerization of the radical group SN to the particles of the powder and thereby uniform coating. PMMA is used to obtain highly dispersed state of matter with a minimum of time grinding. Mode thermal Cycling allows to obtain nanocrystalline composite material Li2FeSiO4consisting of nanocrystalline and amorphous phases, with mo is oficerowie the surface of the carbon particles. According to electron microscopy in the lumen of the structure of the material consists of crystalline phase Li2FeSiO4and amorphous phase (figure 2). Cooling from the liquid state initial phases, followed by cyclic heat treatment allows to obtain a stable amount of the nanocrystalline phase Li2FeSiO4and amorphous phases, which ensures high characteristics of the specific discharge capacity of the material, accelerates the process of heat treatment up to 6 hours. Adding high-molecular compounds in a certain amount, you can simplify the modification of the surface of the powder, which leads to improvement of specific discharge capacity of the cathode material. Using as a starting material of silicon oxide and a mixture of titanomagnetite and silicon oxide significantly reduces the process.

The set of distinctive features is necessary and sufficient to solve the task.

At the melting temperature of 1180±5°With formation of amorphous phase, heat is no longer appropriate, ±5°C is the temperature measurement error.

The ratio of initial substances 55-70 mol.% SiO2selected based on the fact that these limits correspond to the low-melting eutectic in the system Li2O-SiO2.

At a temperature of cycles equal to 600°C., the necessary growth of the crystal is achieved phase Li 2FeSiO4whose size is larger than 200 nm. At a temperature of <600°C significantly increases the time of heat treatment, reaching more than 10 days.

When the number of cycles from 5 to 10 percentage of the amorphous phase is from 10 to 30% of the total powder. With this ratio of amorphous and crystalline phases is possible to achieve a high intensity discharge capacity.

When the content of PMMA <2% of the alloy, the carbon content corresponds to less than 0.7%, which gives a low value of electrical conductivity of the material and, consequently, low values of specific bit of power. When the content of PMMA >5% of the alloy, the carbon content of more than 2.3%, which also gives low values of specific discharge capacity.

Figure 3 and 4 shows the results of x-ray analysis of the modified carbon cathode material, and his picture.

Example 1. To obtain nanocrystalline composite cathode materials in LixFeyMzSiO4/C selected mixture of SiO2, Li2CO3and FeCO3in the ratio of SiO255 mol.%, the rest of Li2CO3and FeCO3. Heated to a temperature of 1180°C. the Cooled air before formation of the amorphous structure. Carry out grinding with simultaneous introduction 2% PMMA from the alloy in energonaprjazhenie mill. The resulting powder is subjected to thermo is iliauni, namely heated to a temperature of 600°C, incubated for 60 min, perform 5 cycles (figure 5). The specific discharge capacity obtained cathode material is 169 mA·h/g at a speed of C/10

Example 2. In the conditions of example 1, the ratio of SiO2- 70 mol.%, the rest of Li2CO3and FeCO3. The specific discharge capacity obtained cathode material is 139 mA·h/g at a speed of C/10.

Example 3. In the conditions of example 1, the ratio of SiO2- 63 mol.%, the rest of Li2CO3and FeCO3. The specific discharge capacity obtained cathode material is 165 mA·h/g at a speed of C/10.

Example 4. In the conditions of example 1, the grinding is carried out with the addition of polymethyl methacrylate (PMMA) in the amount of 5% of the alloy. The specific discharge capacity obtained cathode material is 165 mA·h/g at a speed of C/10.

Example 5. In the conditions of example 1, the grinding is carried out with the addition of carbon black in the amount of 3% of the alloy. The specific discharge capacity obtained cathode material is 164 mA·h/g at a speed of C/10.

Example 6. In the conditions of example 1 are conducted thermal Cycling in the amount of 10 cycles. The specific discharge capacity obtained cathode material is 166 mA·h/g at a speed of C/10.

Example 7. In the conditions of example 1 are conducted thermal Cycling of 7 cycles. As overdosed rasego connection using polymethylmethacrylate (PMMA) in the amount of 3% of the alloy. The specific discharge capacity obtained cathode material is 171 mA·h/g at a speed of C/10.

Example 8. In the conditions of example 2 a mixture of titanomagnetite and SiO2in equal shares for a total of 70%, the rest of Li2CO3and FeCO3. The specific discharge capacity obtained cathode material is 163 mA·h/g at a speed of C/10.

The proposed method allows you to more quickly, easily and cheaply compared to the prototype to obtain nanocrystalline composite cathode material in LixFeyMzSiO4/C with a simultaneous increase in specific discharge capacity.

The method of obtaining nanocrystalline composite cathode materials in LixFeyMzSiO4A /C, which consists in mixing the starting components, their grinding, further heat treatment and cooling to the formation of the amorphous structure with the subsequent addition of high-molecular compounds, characterized in that as starting components choose SiO2or titanomagnetite and SiO2mixed with Li carbonate(Li2CO3) in the ratio of 55-70 mol.% from the source, the rest of Li2CO3and FeCO3in equal amounts, after which the powder is melted at a temperature of 1180±5°C, after cooling to carry out the grinding of the alloy with ignoreme the essential introduction as high-molecular compounds methyl methacrylate) or carbon black in an amount of from 2 to 5% of the alloy, next, carry out thermal treatment in the mode of Cycling, and it is heated to a temperature of ≥600°C, incubated for 55-65 minutes, cooled to room temperature, carrying 5-10 cycles and combining with the heating surface modification of the carbon powder.



 

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