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CN101540394A - Method for preparing lithium ferrosilicon silicate of lithium-ion battery cathode material - Google Patents

Method for preparing lithium ferrosilicon silicate of lithium-ion battery cathode material Download PDF

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CN101540394A
CN101540394A CN200910021964A CN200910021964A CN101540394A CN 101540394 A CN101540394 A CN 101540394A CN 200910021964 A CN200910021964 A CN 200910021964A CN 200910021964 A CN200910021964 A CN 200910021964A CN 101540394 A CN101540394 A CN 101540394A
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lithium
ferrous
preparation
silicate
ion battery
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CN101540394B (en
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刘文刚
许云华
任冰
杨蓉
周志斌
岑启宏
彭建洪
王永平
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Xian University of Architecture and Technology
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Abstract

本发明公开了一种锂离子电池正极材料硅酸亚铁锂的制备方法，该方法将一定比例的锂盐、亚铁盐和二氧化硅混合物粉末充分研磨后，在惰性气氛下煅烧，得到硅酸亚铁锂锂离子电池正极材料。本发明的硅酸亚铁锂材料制备工艺简单、安全，成本低廉。该工艺得到的硅酸亚铁锂材料具有成本低、电化学性能好、环境友好等优点。采用该方法制备的硅酸亚铁锂正极材料在锂离子电池领域具有广泛的应用前景。The invention discloses a preparation method of lithium ferrous silicate, a cathode material of a lithium ion battery. In the method, a certain proportion of lithium salt, ferrous salt and silicon dioxide mixture powder is fully ground, and then calcined in an inert atmosphere to obtain silicon Lithium ferrous acid lithium ion battery cathode material. The preparation process of the lithium ferrous silicate material of the invention is simple, safe and low in cost. The lithium ferrous silicate material obtained by the process has the advantages of low cost, good electrochemical performance, and environmental friendliness. The lithium ferrous silicate cathode material prepared by the method has broad application prospects in the field of lithium ion batteries.

Description

The preparation method of lithium ferrosilicon silicate of lithium-ion battery cathode material
Technical field
The present invention relates to technical field of lithium ion, especially design a kind of new type lithium ion battery positive electrode---the preparation method of ferrosilicon silicate of lithium.
Background technology
Lithium ion battery is since last century, the nineties was come out, owing to its high-energy-density, high power, excellent cycle performance are widely used in all kinds of portable type electronic products field.Along with development of global economy, energy problem is quite outstanding, so the research and development of hybrid vehicle and electric automobile have become global focus, and key technology wherein is exactly the lithium-ion electric pool technology.
Positive electrode is one of critical material of decision lithium ion battery performance, and commercial at present positive electrode is with LiCoO 2Be main, but because LiCoO 2The shortage of resources of middle cobalt costs an arm and a leg, and has toxicity, and environment is had certain pollution, therefore can not adapt to the requirement of large-sized power battery.LiMn 2O 4Though with low cost, cycle performance is poor, fail safe is also relatively poor.Beginning in 1997, many research groups have reported LiMPO 4(M=Fe, Mn, Co, Ni) anode material for lithium-ion batteries finds that this is the up-and-coming positive electrode of a class.Yet, LiFePO 4The electronic conductivity of material and tap density are difficult to improve simultaneously, are difficult to satisfy the needs of the big capacity lithium secondary battery of a new generation.2005, Nyte ' doctor n of Uppsala Univ Sweden synthesized Li first 2FeSiO 4Anode material for lithium-ion batteries obtains comparatively desirable chemical property.Li 2FeSiO 4Belong to rhombic system, space group Pmn2 1, lattice constant is a=6.2661 (5), b=5.3295 (5), c=5.0148 (4) With Li 3PO 4Low temperature structure similar.At Li 2FeSiO 4In the crystal, Li, Si, Fe form tetrahedral structure with O.Because silicate has that raw material is easy to get and is with low cost etc. tempting, Li 2FeSiO 4Be considered to have the new type lithium ion battery positive electrode of development potentiality.
Summary of the invention
The objective of the invention is to, a kind of preparation method of new type lithium ion battery positive electrode active materials ferrosilicon silicate of lithium is provided, the ferrosilicon silicate of lithium Stability Analysis of Structures of this method preparation, good with the electrolyte compatibility, good electrochemical is arranged.And easy and simple to handle, be easy to control, with low cost.
In order to realize above-mentioned task, the present invention takes following technical solution:
A kind of preparation method of lithium ferrosilicon silicate of lithium-ion battery cathode material is characterized in that, comprises the following steps:
1) in proportion raw material lithium salts, ferrous salt, silicon dioxide and additive are mixed, wherein the mol ratio of Li: Fe: Si is (1.9-2.1): (0.95-1.05): 1, and the addition of additive is 1～30% of a mixture gross mass;
2) mixed uniformly material is put into Equipment for Heating Processing; at flow velocity is heat treated in the inert gas protection of 100～5000ml/min; heating rate is 1 ℃/min～20 ℃/min, when temperature to be heated rises to 300 ℃～450 ℃, keeps; under this temperature, heated 1～30 hour; continue then to heat up, in 700 ℃～900 ℃ scope, heat treatment 10 hours～48 hours; slowly reduce to room temperature then, obtain the ferrous metasilicate lithium material.
Owing in the building-up process of ferrosilicon silicate of lithium, adopted additive among the present invention, these additives are distributed between the material granule by mixing, additive mainly plays two effects: the one, suppress the growth of ferrosilicon silicate of lithium individual particle, and reduce the particle diameter of individual particle.The 2nd, the pyrolytic carbon that the additive pyrolysis forms later on can be coated on particle surface or be present between the particle, thereby improves the electric conductivity between the particle effectively.So in building-up process, add additive can obtain particle diameter little, conduct electricity very well, ferrous metasilicate lithium material that chemical property is good.
The preparation method of lithium ferrosilicon silicate of lithium-ion battery cathode material of the present invention has the following advantages:
1, the raw material wide material sources are pollution-free, and cost is low;
2, the preparation technology of material is simple, safe;
3, prepared ferrosilicon silicate of lithium has good microstructure;
4, prepared ferrosilicon silicate of lithium Stability Analysis of Structures, good with the electrolyte compatibility, good electrochemical is arranged.
5, positive electrode involved in the present invention can be widely used in comprising all kinds of mobile electronic products and electric vehicle in all kinds of lithium ion batteries.
Description of drawings
Fig. 1 is the X-ray diffraction style of the prepared ferrosilicon silicate of lithium sample of the embodiment that provides of inventor 1, adopt the Japanese Rigaku D/MAX-2400 of company type X-ray diffractometer, Cu K α target is a radiation source, voltage is 46kV, electric current is 100mA, step-length is 0.02, sweep speed be 10 (°)/min, sweep limits (2 θ) is 3 °～90 °.
Fig. 2 is the ESEM picture of the prepared ferrosilicon silicate of lithium sample of the embodiment that provides of inventor 1, utilizes the JSM-6700F of NEC company type field emission scanning electron microscope (FESEM) to take.
Fig. 3 is the first charge-discharge curve chart by the prepared ferrous silicate lithium anode material of embodiment 1.
Fig. 4 is the cycle life curve chart by the prepared ferrous silicate lithium anode material of embodiment 1.
Fig. 5 is the first charge-discharge curve chart by the prepared ferrous silicate lithium anode material of embodiment 2.
Fig. 6 is the first charge-discharge curve chart by the prepared ferrous silicate lithium anode material of embodiment 3.
The embodiment that provides below in conjunction with accompanying drawing and inventor is described in further detail the present invention.
Embodiment
The present invention relates to the preparation method of lithium ferrosilicon silicate of lithium-ion battery cathode material, its step is as follows:
1, lithium salts, ferrous salt, silicon dioxide and additive are mixed in proportion that (mixed process can be carried out, as mixing in inclined mill, cone-type mixer, the three-dimensional mixer 1～24 hour in the mixing apparatus of routine; Also available wet chemical method mixes as sol-gel process, spray drying process), wherein, the mol ratio of Li: Fe: Si is (1.9-2.1): (0.95-1.05): the addition of 1 additive is 1～30% of a mixture gross mass;
Above-mentioned additive can be the organic compound that can be decomposed into conductive carbon class material after carbon black, graphite or the pyrolysis;
2; mixed uniformly raw material are put into Equipment for Heating Processing, and (any Equipment for Heating Processing that can evenly add thermal reaction mixture under atmosphere protection all can be used; as the tubular type atmosphere furnace; rotation atmosphere furnace or atmosphere protection continuous tunnel furnace; box type furnace etc.); at flow velocity is heat treated in the inert gas shielding of 100～5000ml/min; heating rate is 1～20 ℃/min; when temperature to be heated rises to 300～450 ℃; keep temperature-resistant; under this temperature, heated 1～30 hour; continue then to heat up; in 700～900 ℃ scope; room temperature is slowly reduced in heat treatment 10～48 hours then, just can obtain the ferrous metasilicate lithium material.
Wherein, the lithium salts, the ferrous salt that prepare above-mentioned positive electrode active materials all do not have particular restriction, can adopt commercially available prod or product well known in the art, as lithium salts can select lithium metasilicate, lithium carbonate, lithium hydroxide, lithium oxalate, lithium acetate, lithium chloride, lithium nitrate, lithium phosphate etc. wherein any, perhaps said mixture etc. can.Ferrous salt can select ferrous oxalate, ferrous acetate, frerrous chloride, ferrous phosphate etc. wherein any, perhaps said mixture etc. can.
Additive can be selected from carbon black, graphite, sucrose, citric acid, glucose, polyvinyl alcohol, soluble starch, phenolic resins, furfural resin, poly-one or more mixtures to benzene, benzene naphthalene dicarboxylic copolymer, benzene anthracene bipolymer, the luxuriant and rich with fragrance bipolymer of benzene, benzene naphthalene terpolymer, benzene naphthalene anthracene terpolymer etc.
Described inert gas such as nitrogen, argon gas or its mist.
In order to be illustrated more clearly in the present invention, the inventor provides following embodiment, need to prove, these embodiment are some more excellent examples, the invention is not restricted to these embodiment.
Embodiment 1:
With 2.7g lithium metasilicate, 5.4g ferrous oxalate, 2g sucrose mixing and ball milling 24 hours under ethanol medium, use equipment to be planetary ball mill, the autobiography rotating speed is 200r/min.With the mixed-powder of abundant mixed grinding 60 ℃ of vacuumizes 24 hours; then with the pressure compressing tablet of 10MPa; under the argon gas atmosphere protection of 1L/min; speed with 10 ℃/min rises to 400 ℃; insulation is 2 hours under this temperature; speed with 10 ℃/min rises to 800 ℃ then, is incubated 10h under this temperature, is cooled to room temperature then and has both obtained the ferrosilicon silicate of lithium sample.
Fig. 1 is the XRD figure spectrum of gained ferrosilicon silicate of lithium, and most diffraction maximum can be corresponding with the characteristic peak of ferrosilicon silicate of lithium among the figure, also has a spot of impurity simultaneously.Fig. 2 is the stereoscan photograph of gained ferrosilicon silicate of lithium, the granularity of synthetic material between 0.5-3 μ m, subsphaeroidal pattern, distribution uniform.
Embodiment 1 gained sample carries out electrochemical property test as follows: ferrosilicon silicate of lithium sample powder, conductive black and PVDF (polyvinylidene fluoride) are pressed 80: 10: 10 mixed of mass ratio, add an amount of organic solvent NMP (N-methyl pyrrolidone), be applied on the aluminium foil 120 ℃ of dry 12h in vacuum drying chamber after fully stirring into even pastel.Cut-off directly is that the small pieces of 16mm are positive pole, and metal lithium sheet is a negative pole, and the Celgard2400 microporous polypropylene membrane is a barrier film, to be dissolved in the 1molL that volume ratio is EC (ethylene carbonate)/DMC (1, the 2-dimethyl carbonate) of 1: 1 -1LiPF 6Be electrolyte, in being full of the glove box of argon gas, be assembled into CR2032 type button cell.Button cell is placed its chemical property of test on the CT2001A type battery test system.Charge-discharge magnification is C/10, and voltage range is 1.5V-4.8V.Fig. 3 is this material first charge-discharge curve, and as seen from the figure, the charging capacity of the material that is synthesized reaches 242mAh/g, and reversible capacity is 137mAh/g, and Fig. 4 provides 10 cyclic curve figure of this material, and as seen the cycle performance of this material is good.
Embodiment 2:
With 2.85g lithium carbonate, 2.3g silicon dioxide, 5.4g ferrous oxalate and 2g sucrose mixing and ball milling 24 hours under ethanol medium, use equipment to be planetary ball mill, the autobiography rotating speed is 250r/min.With the mixed-powder of abundant mixed grinding 60 ℃ of vacuumizes 24 hours; then with the pressure compressing tablet of 10MPa; under the argon gas atmosphere protection of 2L/min; speed with 10 ℃/min rises to 400 ℃; insulation is 2 hours under this temperature; speed with 20 ℃/min rises to 850 ℃ then, is incubated 15h under this temperature, is cooled to room temperature then and has both obtained the ferrosilicon silicate of lithium sample.Test its chemical property according to the method for embodiment 1, as shown in Figure 5, its first circulating and reversible capacity is 142mAh/g.
Embodiment 3:
With 1.85g lithium hydroxide, 2.3g silicon dioxide, 5.4g ferrous oxalate and 1.5g citric acid mixing and ball milling 24 hours under ethanol medium, use equipment to be planetary ball mill, the autobiography rotating speed is 250r/min.With the mixed-powder of abundant mixed grinding 60 ℃ of vacuumizes 24 hours; then with the pressure compressing tablet of 10MPa; under the argon gas atmosphere protection of 1.5L/min; speed with 5 ℃/min rises to 400 ℃; insulation is 1 hour under this temperature; speed with 10 ℃/min rises to 750 ℃ then, is incubated 15h under this temperature, is cooled to room temperature then and has both obtained the ferrosilicon silicate of lithium sample.Test its chemical property according to the method for embodiment 1, as shown in Figure 6, its first circulating and reversible capacity is 118mAh/g.
Embodiment 4:
Different is for present embodiment and embodiment 1, only additive is changed into the 0.5g conductive black, and all the other are with embodiment 1, and the first circulating and reversible capacity of gained positive electrode is 138mAh/g.
Embodiment 5:
Different is for present embodiment and embodiment 2, only additive is changed into the 1g citric acid, and all the other are with embodiment 2, and the first circulating and reversible capacity of gained positive electrode is 125mAh/g.
Embodiment 6:
Different is for present embodiment and embodiment 3, only additive is changed into the 1.8g soluble starch, and all the other are with embodiment 3, and the first circulating and reversible capacity of gained positive electrode is 128mAh/g.

Claims (5)

1、一种锂离子电池正极材料硅酸亚铁锂的制备方法，其特征在于，包括下列步骤：1, a kind of preparation method of lithium ferrous silicate of cathode material of lithium ion battery, is characterized in that, comprises the following steps: 1)按比例将原料锂盐、亚铁盐、二氧化硅和添加剂混合，其中Li∶Fe∶Si的摩尔比为(1.9-2.1)∶(0.95-1.05)∶1，添加剂的加入量为混合物总质量的1～30％；1) Mix the raw materials lithium salt, ferrous salt, silicon dioxide and additives in proportion, wherein the molar ratio of Li:Fe:Si is (1.9-2.1):(0.95-1.05):1, and the amount of additives added is the mixture 1-30% of the total mass; 2)将均匀混合的物料放入热处理设备中，在流速为100～5000ml/min的惰性气流保护中加热处理，升温速率为1℃/min～20℃/min，待热处理温度升至300℃～450℃时，保持，在该温度下加热1～30小时，然后继续升温，在700℃～900℃的范围内，热处理10小时～48小时，然后缓慢降至室温，得到硅酸亚铁锂材料。2) Put the uniformly mixed materials into the heat treatment equipment, heat treatment in the protection of inert gas flow with a flow rate of 100-5000ml/min, the heating rate is 1°C/min-20°C/min, and the temperature to be heat-treated is raised to 300°C- Keep at 450°C, heat at this temperature for 1 to 30 hours, then continue to heat up, heat treatment in the range of 700°C to 900°C for 10 hours to 48 hours, and then slowly lower to room temperature to obtain lithium ferrous silicate material . 2、如权利要求1所述的制备方法，其特征在于，所述锂盐选自硅酸锂、碳酸锂、氢氧化锂、草酸锂、醋酸锂、氯化锂、硝酸锂、磷酸锂其中的一种或几种混合物。2. The preparation method according to claim 1, wherein the lithium salt is selected from lithium silicate, lithium carbonate, lithium hydroxide, lithium oxalate, lithium acetate, lithium chloride, lithium nitrate, and lithium phosphate. One or several mixtures. 3、如权利要求1所述的制备方法，其特征在于，所述铁盐选自草酸亚铁、醋酸亚铁、氯化亚铁、磷酸亚铁中的其中一种或几种混合物。3. The preparation method according to claim 1, wherein the iron salt is selected from one or a mixture of ferrous oxalate, ferrous acetate, ferrous chloride and ferrous phosphate. 4、如权利要求1所述的制备方法，其特征在于，所述添加剂选自炭黑、石墨、蔗糖、柠檬酸、葡萄糖、聚乙烯醇、可溶性淀粉、酚醛树脂、糠醛树脂、聚对苯、苯萘二元共聚物、苯蒽二元共聚物、苯菲二元共聚物、苯萘三元共聚物、苯萘蒽三元共聚物等的一种或几种混合物。4. The preparation method according to claim 1, wherein the additive is selected from carbon black, graphite, sucrose, citric acid, glucose, polyvinyl alcohol, soluble starch, phenolic resin, furfural resin, polyparaphenylene, One or several mixtures of benzene-naphthalene binary copolymer, benzoanthracene binary copolymer, benzophenanthrene binary copolymer, benzene-naphthalene terpolymer, benzonaphthalene-anthracene terpolymer, etc. 5、如权利要求1所述的制备方法，其特征在于，所述惰性气流选自氮气或氩气，或者是氮气和氩气的混合气体。5. The preparation method according to claim 1, characterized in that the inert gas flow is selected from nitrogen or argon, or a mixed gas of nitrogen and argon.
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CN101920971A (en) * 2010-06-28 2010-12-22 宁波大学 A kind of preparation method of silicate cathode material for lithium ion battery
CN101944594A (en) * 2010-09-14 2011-01-12 耿世达 Lithium ferrous silicate anode material for high-performance lithium ion battery and preparation method thereof
CN101982410A (en) * 2010-10-15 2011-03-02 福建师范大学 Preparation method of rare earth compound doped lithium ferrous silicate cathode material
CN102315438A (en) * 2011-05-23 2012-01-11 江苏正彤电子科技有限公司 A porous C/Li2MSiO4/C (M=Fe, mn, co) composite anode material and its preparation method
CN102509776A (en) * 2011-10-19 2012-06-20 兰州理工大学 Method for preparing doped ferrous-lithium metasilicate anode material from micro silicon powder
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CN101920971B (en) * 2010-06-28 2011-11-16 宁波大学 Preparation method of silicate positive electrode material for lithium ion battery
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CN101944594B (en) * 2010-09-14 2013-01-09 耿世达 Lithium ferrous silicate anode material for high-performance lithium ion battery and preparation method thereof
CN101944594A (en) * 2010-09-14 2011-01-12 耿世达 Lithium ferrous silicate anode material for high-performance lithium ion battery and preparation method thereof
CN101982410A (en) * 2010-10-15 2011-03-02 福建师范大学 Preparation method of rare earth compound doped lithium ferrous silicate cathode material
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WO2012110931A1 (en) * 2011-02-14 2012-08-23 Basf Se Electrode materials and process for producing them
CN102315438A (en) * 2011-05-23 2012-01-11 江苏正彤电子科技有限公司 A porous C/Li2MSiO4/C (M=Fe, mn, co) composite anode material and its preparation method
US9397332B2 (en) * 2011-06-14 2016-07-19 Hoganas Ab (Publ) Lithium insertion material for cathodes and a method for producing the same
US20140145121A1 (en) * 2011-06-14 2014-05-29 Höganäs Ab (Publ) Novel method and product
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CN108807988A (en) * 2018-07-25 2018-11-13 四川理工学院 A kind of preparation method of the spherical ferrous silicate lithium anode material of lithium ion battery
CN108807988B (en) * 2018-07-25 2021-04-20 四川理工学院 Preparation method of spherical lithium ferrous silicate cathode material for lithium ion battery
CN109638274A (en) * 2018-12-14 2019-04-16 中科廊坊过程工程研究院 A kind of molybdenum ytterbium is co-doped with silicic acid ferrisodium combination electrode material and preparation method thereof
CN109638274B (en) * 2018-12-14 2022-03-11 廊坊绿色工业技术服务中心 Molybdenum-ytterbium co-doped sodium iron silicate composite electrode material and preparation method thereof
CN111048766A (en) * 2019-12-27 2020-04-21 惠州亿纬锂能股份有限公司 Lithium iron silicate/carbon cathode material and preparation method and application thereof
CN111647863A (en) * 2020-07-02 2020-09-11 河北大学 Li2FexSiO4Preparation method and application of positive electrode film
CN111647863B (en) * 2020-07-02 2022-03-25 河北大学 Li2FexSiO4Preparation method and application of positive electrode film

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