CN1373528A - Postive electrode material of li-ion accumulator and its preparing process - Google Patents

Postive electrode material of li-ion accumulator and its preparing process Download PDF

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CN1373528A
CN1373528A CN 01107236 CN01107236A CN1373528A CN 1373528 A CN1373528 A CN 1373528A CN 01107236 CN01107236 CN 01107236 CN 01107236 A CN01107236 A CN 01107236A CN 1373528 A CN1373528 A CN 1373528A
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lithium
nitrate
compound
according
thallium
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CN 01107236
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刘兴泉
于作龙
李淑华
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中国科学院成都有机化学研究所
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/13Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/13Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy

Abstract

A positive electrode material for Li-ion battery is a composite spinel material, which is prepared from the Li-containing compound, Mn-containing compound, Tl-containing compound, Al-containing compound, and Cr or Ni or Co containing compound through mixing in a special mode, dispersing and chemical reaction. Its advantages are higher reversible discharge capacity, long cyclic life and high high-temp stability.

Description

一种锂离子蓄电池正极材料及其制备方法 A lithium ion secondary battery positive electrode material and its preparation method

本发明涉及一种二次锂离子电池正极材料及其制备方法,尤其涉及一种复合尖晶石锂离子蓄电池正极材料LixMn2-yz-δTlyAlzMδO4及其制备方法。 The present invention relates to a lithium ion secondary battery positive electrode material and a preparation method, in particular a positive electrode material LixMn2-yz-δTlyAlzMδO4 relates to a composite preparation method and spinel lithium ion battery. 其特点是:该材料是由Tl、Al和Cr或Ni或Co三种金属同时取代母体尖晶石LiMn2O4中部分Mn而生成的一种复合尖晶石型正极材料。 Its characteristics are: the material is Tl, Al and Cr or Ni or Co while three metals substituted for part of Mn in LiMn2O4 spinel precursor generated by a composite positive electrode material of spinel type. 其制备方法是:将一种含锂的化合物与一种含锰的化合物、一种含铊的化合物,一种含铝的化合物和一种含铬或镍或钴的化合物以适当的方式混合和分散,然后经过干燥、研磨和空气中焙烧,即得到组成为LixMn2-yz-δTlyAlzMδO4的黑色粉末正极材料,其中0<x≤2,0≤y≤1,0≤z≤1,0≤δ≤1,0<y+z+δ≤1,M代表Cr或Ni或Co。 The preparation method is: a compound containing a lithium compound with a manganese, thallium containing compound, a compound containing aluminum and chromium or nickel or cobalt compounds in an appropriate manner and mixed dispersion, then dried, ground and calcined in air, to obtain a composition of LixMn2-yz-δTlyAlzMδO4 black powder cathode material, where 0 <x≤2,0≤y≤1,0≤z≤1,0≤δ≤ 1,0 <y + z + δ≤1, M represents Cr or Ni or Co.

锂离子蓄电池是近年来迅速发展起来的高能二次电源,由于它对环境的友好性,被誉为21世纪的“绿色能源”。 Lithium-ion batteries are developed rapidly in recent years, high-energy secondary power supply due to its environmental friendliness, known as the 21st century "green energy."

锂离子蓄电池具有比能量高,自放电率低,循环寿命长,工作电压高、安全性能好和无记忆效应等优点,被广泛用于现代通讯,信息技术和现代军事及国防等领域,而且其应用范围还在不断向纵深发展。 Lithium ion batteries with high specific energy, low self-discharge, long cycle life, high operating voltage, the performance advantages of a good safety and no memory effect, are widely used in modern telecommunications, information technology and the art of modern military and defense, and its applications are still evolving in depth. 因此,锂离子蓄电池是一种前景十分诱人的新型“清洁能源”。 Therefore, the lithium-ion battery is a very promising new "clean energy."

锂锰尖晶石作为锂离子蓄电池的正极材料,近年来受到了世界各国的广泛关注。 Lithium manganese spinel as a cathode material for lithium ion batteries, in recent years has been widespread concern around the world. 由于其资源丰富,成本低,无环境污染和安全性能好而倍受亲睐。 Because of its rich resources, low cost, no environmental pollution and safety performance much pro-Lai. 但是由于锂锰尖晶石正极材料存在着循环性能差,尤其是高温(55℃)条件下稳定性更差的缺点,导致了锂锰尖晶石正极材料的应用受到限制。 However, since there is difference in the cycle performance of the lithium manganese spinel cathode material, in particular a high temperature (55 ℃) stability under conditions worse drawbacks, led to the use of lithium manganese spinel cathode material is limited. 国际上众多的研究者都在极力寻求克服和解决上述缺点的途径。 Many international researchers are struggling to find ways to overcome and solve the above drawbacks. 如:1.A de Kock,E Ferg,R J Gummow.J Power Sources,1998,70:247~2522.A D Robertson,S H Lu,W F Howard Jr.JElectrochem Soc,1999,144(10):35053.G G Amatucci,C N Schmutz,A Blyr,et al.J Power Sources,1997,69:11~254.G Pistioa,C Bellitto,A Antonni.PCT/WO 97/37394(1997)但是单独掺杂Al、Cr、Ni和Co阳离子对稳定性虽然有所提高,但是须以牺牲比容量为代价。 Such as: 1.A de Kock, E Ferg, RJ Gummow.J Power Sources, 1998,70: 247 ~ 2522.AD Robertson, SH Lu, WF Howard Jr.JElectrochem Soc, 1999,144 (10): 35053.GG Amatucci , CN Schmutz, A Blyr, et al.J Power Sources, 1997,69: 11 ~ 254.G Pistioa, C Bellitto, A Antonni.PCT / WO 97/37394 (1997) is individually doped with Al, Cr, Ni, and Co cations although stability has improved, but should be at the expense of specific capacity for the price. 我们曾对金属Tl原子掺杂的锂锰尖晶石正极材料进行了研究,即将金属Tl原子掺入锂锰尖晶石中以部分取代Mn原子时,正极材料的比容量不但没有降低,反而有所升高,而且其循环稳定性能也有所提高,但是其高温稳定性能仍不够理想。 We had metal atoms Tl-doped lithium manganese spinel cathode material is studied, i.e. the incorporation of the metal lithium manganese spinel Tl atoms to the Mn atoms when substituted, the specific capacity of the positive electrode material has not decreased portion, but there are the increased circulation and its stable performance also improved, but its high temperature stability is still not ideal. 因此,本发明将金属Tl原子与金属Al原子和Cr原子或Ni原子或Co原子同时掺入母体尖晶石,生成了一种复合尖晶石正极材料,不仅使材料的循环稳定性能有所提高,而且使高温稳定性能有了大幅度增加。 Accordingly, the present invention is a metal atom Al metal and Tl atoms and Cr atoms or Co or Ni atom atom simultaneously incorporated parent spinel, spinel generates a composite positive electrode material, not only the stability of the material circulating improved and the high temperature stability has greatly increased. 同时还保持了较高的循环比容量。 While maintaining the high specific capacity of the cycle.

下面结合实施例和附图对本发明作进一步的描述。 The following examples and drawings in conjunction with embodiments of the present invention will be further described.

实施例1称取1.36g硝酸亚铊和3.81g碳酸锂及17.87g电解二氧化锰混合均匀,然后称取0.76g硝酸铝和0.89g硝酸镍溶于1∶4的乙醇/水介质中,然后再将上述混合物加入混合溶液中研磨均匀,蒸去溶剂,105℃-125℃烘干过夜,再研磨成细粉,在马弗炉中800℃~850℃空气气氛中焙烧12h,随炉冷却即得正极材料样品,材料呈尖晶石结构(见附图1)。 Example 1 3.81g said lithium carbonate and thallium nitrate and electrolytic manganese dioxide 17.87g 1.36g homogeneous mixing takes, weighed 0.76g and 0.89g of aluminum nitrate and nickel nitrate dissolved in ethanol / water medium 1:4, and then the mixture was then added to the mixed solution of the polishing uniformity, the solvent was distilled off, 105 ℃ -125 ℃ dried overnight and ground to a fine powder in a muffle furnace 800 ℃ ~ 850 ℃ calcined in an air atmosphere for 12h, i.e. furnace cooling samples obtained positive electrode material, the material was a spinel structure (see Figure 1). 然后以此作为正极活性物质,以乙炔黑为导电剂,聚四氟乙烯为粘接剂,三者重量比为正极材料∶导电剂∶粘接剂=85∶10∶5。 Then as the positive electrode active material, acetylene black as a conductive agent, polytetrafluoroethylene as a binder, the weight ratio of the three positive electrode material: conductive agent: binder = 85:10:5. 以铝箔为集流体,1.0mol/L LiClO4/EC(碳酸乙烯酯)+DEC(碳酸二乙酯)(1∶1 Vol.)为电解液,Cellgard 2400为隔膜,金属锂片为对电极,在充满氩气的不锈钢手套箱中装配成模拟扣式电池,然后在上海正方电子电器有限公司生产的DC-5型电池性能测试仪上进行恒流充放电。 Aluminum foil as current collector, 1.0mol / L LiClO4 / EC (ethylene carbonate) + DEC (diethyl carbonate) (1:1 Vol.) As the electrolyte, Cellgard 2400 as the separator, metal lithium sheets as the counter electrode, in a glove box filled with argon gas in a stainless steel cell fitted into an analog button, and then constant current discharge at the Shanghai Electronics Co., Ltd. square DC-5 manufactured battery performance tester. 充放电电流0.1mA~0.5mA,充放电截止电压4.35V~3.3V,充放电速率为0.4C~0.5C。 Discharge current 0.1mA ~ 0.5mA, discharge cut-off voltage of 4.35V ~ 3.3V, charge and discharge rate of 0.4C ~ 0.5C. 测试结果表明,该材料的首次充电比容量为119.20mAh/g,放电比容量为114.8mAh/g,效率为96.3%。 Test results show that the material is first charge capacity was 119.20mAh / g, the discharge capacity was 114.8mAh / g, efficiency of 96.3%.

实施例2将实施例1中的0.89g硝酸镍用1.225g硝酸铬代替,其它步骤和条件同实施例1。 Example 2 0.89g of nickel nitrate in the embodiment of Example 1 with chromium nitrate instead 1.225g, other steps and conditions were the same as in Example 1. 测试结果表明,该材料的首次充电比容量为121.30mAh/g,放电比容量为115.70mAh/g,效率为95.4%。 Test results show that the material is first charge capacity was 121.30mAh / g, the discharge capacity was 115.70mAh / g, efficiency of 95.4%.

实施例3将实施例1中的0.89g硝酸镍用0.88g硝酸钴代替,其它步骤和条件同实施例1。 Example 3 0.89g of nickel nitrate in Example 1 was replaced with 0.88g of cobalt nitrate to embodiments, other steps and conditions were the same as in Example 1. 测试结果表明,该材料的首次充电比容量为118.30mAh/g,放电比容量为113.70mAh/g,效率为96.1%。 Test results show that the material is first charge capacity was 118.30mAh / g, the discharge capacity was 113.70mAh / g, efficiency of 96.1%.

对比例1称取3.81g碳酸锂和18.43g电解二氧化锰混合均匀,以后步骤和条件同实施例1。 Comparative Example 1 weighed 18.43g and 3.81g of lithium carbonate mixed electrolytic manganese dioxide after the same steps and conditions as in Example 1. 材料的组成为LixMn2-y-zAlyNizO4。 Constituent material for LixMn2-y-zAlyNizO4. 测试结果表明,该材料的首次充电比容量为110.80mAh/g,放电比容量为107.10mAh/g,效率为96.7%。 Test results show that the material is first charge capacity was 110.80mAh / g, the discharge capacity was 107.10mAh / g, efficiency of 96.7%.

对比例2将对比例1中的0.89g硝酸镍用1.225g硝酸铬代替,其它步骤和条件同对比例1,材料的组成为LixMn2-y-zAlyCrzO4。 0.89g of nickel nitrate in Example 2 of Comparative Example 1 was replaced with 1.225 g of chromium nitrate, other steps and conditions with Comparative Example 1, the constituent material of LixMn2-y-zAlyCrzO4. 测试结果表明,该材料的首次充电比容量为109.20mAh/g,首次放电比容量为105.40mAh/g,效率为96.5%。 Test results show that the material is first charge capacity was 109.20mAh / g, the initial discharge capacity was 105.40mAh / g, efficiency of 96.5%.

实施例4材料的制备和条件同实施例2,考察材料在常温(25℃)下的循环性能。 Example 4 Preparation conditions and materials as in Example 2, the cycle performance materials investigated at room temperature (25 ℃) a. 测试结果为充放电循环75次后,材料的充电比容量为111.70mAh/g,材料的放电比容量仍保持在110.80mAh/g,仅下降了4.23%,如附图2所示。 After the charging and discharging cycle test result is 75, the charging material 111.70mAh / g, the discharge capacity of the material remains at 110.80mAh / g, decreased by only 4.23%, as shown in Figure 2 specific capacity.

实施例5材料的制备和条件同实施例2,考察材料在高温(55℃)下的循环稳定性。 Example 5 Preparation conditions and materials as in Example 2, the cycle stability of the material at a high temperature (55 ℃) a. 测试结果为充放电循环40次后,材料的充电比容量为107.10mAh/g,放电比容量仍保持在105.80mAh/g。 After the charging and discharging cycle test result is 40 times, the charging capacity ratio of the material 107.10mAh / g, the discharge capacity remains 105.80mAh / g. 下降了8.71%,如附图3所示。 Decreased by 8.71%, as shown in figures 3.

对比例3材料的制备和条件同对比例2,考察材料在常温(25℃)和高温(55℃)下的循环性能和稳定性能。 Comparative Example 3 Preparation conditions and with the material 2, the material investigated at room temperature (25 ℃) and cycle performance and stability at high temperature Comparative Example (55 ℃). 测试结果为:常温下循环75次后,材料的充电比容量为99.15mAh/g,材料的放电比容量为98.26mAh/g,下降了6.78%;高温下循环40次后,材料的充电比容量为93.96mAh/g,放电比容量为92.74mAh/g,下降了8.45%。 Test results: After 75 cycles at room temperature, the charging capacity ratio of the material 99.15mAh / g, the discharge capacity of the material 98.26mAh / g, decreased by 6.78%; after 40 cycles at a high temperature, the charging capacity ratio of the material is 93.96mAh / g, the discharge capacity was 92.74mAh / g, decreased by 8.45%.

实施例6材料的制备和条件同实施例3,考察材料在常温(25℃)下的循环性能。 Materials and conditions of Example 6 Preparation embodiment same as in Example 3, the cycle performance materials investigated at room temperature (25 ℃) a. 测试结果为充放电循环15次后,材料的充电比容量为114.70mAh/g,材料的放电比容量仍保持在113.30mAh/g,效率为98.8%,放电比容量仅下降了0.35%。 The test results after 15 cycles of charge and discharge, the charging material 114.70mAh / g, the discharge capacity of the material remains at 113.30mAh / g specific capacity, efficiency 98.8%, only 0.35% decrease of discharge capacity ratio.

Claims (9)

  1. 1.一种锂离子蓄电池正极材料及其制备方法,其特征是:将一种含锂的化合物与一种含锰的化合物、一种含铊的化合物、一种含铝的化合物和一种含铬或镍或钴的化合物以湿化学法混合和分散,然后经过105℃~125℃恒温干燥2~12h,再研磨成细粉,并在空气中650℃~850℃焙烧6~24h,随炉自然冷却,即得到流动性极好的黑色粉体材料。 1. A lithium ion secondary battery positive electrode material and a preparation method, wherein: a compound containing a lithium compound with a manganese, thallium containing compound, a compound containing aluminum and containing chromium or nickel or cobalt compound to a wet chemical mixed and dispersed, and then through a thermostat 105 ℃ ~ 125 ℃ dried 2 ~ 12h, then ground to a fine powder, and calcined in air for 6 ~ 24h 650 ℃ ~ 850 ℃, the furnace naturally cooled, i.e., to obtain excellent fluidity black powder material. 该材料呈尖晶石结构,用作二次锂离子电池的正极材料,具有比容量高、循环寿命长和高温稳定性好等特点。 The material is in spinel structure as a positive electrode material for a secondary lithium ion battery having a high specific capacity, long cycle life and good high temperature stability.
  2. 2.根据权利要求1,其特征是所得黑色粉体材料的组成为LixMn2-yz-δTlyAlzMδO4,其中0<x≤2,0≤y≤1,0≤z≤1,0≤δ≤1,0<y+z+δ≤1,M为Cr或Ni或Co。 According to claim 1, characterized in that the composition of the resulting black powder material is LixMn2-yz-δTlyAlzMδO4, where 0 <x≤2,0≤y≤1,0≤z≤1,0≤δ≤1,0 <y + z + δ≤1, M is Cr or Ni or Co.
  3. 3.根据权利要求1,其特征是含锂的化合物在氢氧化锂、硝酸锂、碳酸锂、醋酸锂和草酸锂中选择。 According to claim 1, wherein the lithium-containing compound selected lithium hydroxide, lithium nitrate, lithium carbonate, lithium acetate and lithium oxalate in.
  4. 4.根据权利要求1,其特征是含锰的化合物在碳酸锰、醋酸锰、硝酸锰、草酸锰和二氧化锰(包括化学二氧化锰和电解二氧化锰)中选择。 According to claim 1, wherein the compound is selected manganese carbonate, manganese acetate, manganese nitrate, manganese oxalate, and manganese dioxide (including chemical manganese dioxide and electrolytic manganese dioxide) in the.
  5. 5.根据权利要求1,其特征是含铊的化合物在碳酸铊、硝酸铊、硝酸亚铊、氧化铊和卤化铊中选择。 According to claim 1, wherein the thallium-containing compound selected thallium carbonate, thallium nitrate, thallium nitrate, thallium oxide, and thallium halide.
  6. 6.根据权利要求1,其特征是含铝的化合物在硝酸铝、醋酸铝、卤化铝和碱式碳酸铝中选择。 According to claim 1, characterized in that the aluminum compound is selected aluminum nitrate, aluminum acetate, aluminum halides and basic aluminum carbonate.
  7. 7.根据权利要求1,其特征是含铬的化合物在硝酸铬、氢氧化铬、氧化铬和碱式碳酸铬中选择。 According to claim 1, characterized in that the chromium-containing compound selected chromium nitrate, chromium hydroxide, chromium oxide and basic chromium carbonate.
  8. 8.根据权利要求1,其特征是含钴的化合物在钴的硝酸盐、醋酸盐和草酸盐选择。 According to claim 1, wherein the compound containing cobalt is a cobalt nitrate, acetate, and oxalate selection.
  9. 9.根据权利要求1,其特征是含镍的化合物在镍的硝酸盐、醋酸盐和草酸盐选择。 According to claim 1, characterized in that a nickel-containing compounds of nickel nitrate, acetate, and oxalate selection.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100423328C (en) 2005-01-14 2008-10-01 哈尔滨光宇电源股份有限公司 Preparation method of positive electrode material of lithium ion secondary cell
CN100526222C (en) 2003-11-26 2009-08-12 3M创新有限公司 Solid state synthesis of lithium-nickel-cobalt-manganese mixed metal oxides for use in lithium ion battery cathode material

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100526222C (en) 2003-11-26 2009-08-12 3M创新有限公司 Solid state synthesis of lithium-nickel-cobalt-manganese mixed metal oxides for use in lithium ion battery cathode material
CN100423328C (en) 2005-01-14 2008-10-01 哈尔滨光宇电源股份有限公司 Preparation method of positive electrode material of lithium ion secondary cell

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