磷酸铁锂的合成与性能研究
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摘要
橄榄石晶型的LiFePO4正极材料已逐渐成为国内外新的研究热点。研究表明,该新型正极材料理论容量大(170mAh/g),平台特性好,电压极平稳,高温性能和热稳定性明显优于已知的其它正极材料,无毒,为真正的绿色材料。
固、液结合法合成LiFePO4/C材料,用Li2CO3、H3PO4、Fe2O3、葡萄糖、柠檬酸、蒸馏水为原料。将原料充分研磨均匀、烘干、球磨、焙烧,制得LiFePO4/C材料。用XRD对合成的LiFePO4/C材料进行结构测定,用激光粒度分析仪测定材料粒径。用恒流充放电、循环伏安扫描技术测试材料电化学性能。
实验研究发现,高温固液结合法合成LiFePO4时,加入碳能有效阻止材料颗粒长大,得到粒径细小均匀的材料。加入碳的作用有:①作为还原剂将Fe3+还原为Fe2+;②包覆在LiFePO4颗粒表面提高材料导电性;③控制高温固相合成LiFePO4材料的颗粒粒径。分别加入了葡萄糖、蔗糖、乳糖、乙炔黑作为碳添加剂合成LiFePO4/C材料,结果显示加入葡萄糖、乳糖效果较好,室温0.2C恒流放电比容量都在139.8mAh/g以上,乙炔黑效果较差,只有93.44mAh/g。
高温固相法合成LiFePO4/C材料,实验考察了焙烧温度、焙烧时间对材料性能的影响。分别在500℃、550℃、600℃、650℃、700℃、750℃、800℃下焙烧8小时制得材料,测试结果显示:室温、0.2C恒流放电,500℃、550℃制备的材料没有容量,600℃制备的材料比容量为20mAh/g,650℃、700℃制备的材料比容量为140mAh/g左右,750℃、800℃制备的材料比容量分别为120mAh/g、80mAh/g。实验表明,700℃合成的LiFePO4/C材料电化学性能最好。700℃分别焙烧2、4、6、8、12、16小时合成LiFePO4/C材料。实验表明,焙烧8h合成的LiFePO4/C材料电化学性能最好。
高温固相法合成LiFePO4/C材料,实验考察了掺杂1%MgCO3、CrO3、(NH4)6Mo7O24·4H2O对合成的LiFePO4/C材料电化学性能的影响。实验表明,掺杂1%CrO3合成的LiFePO4/C材料电化学性能最好,0.2C恒流放电比容量是145 mAh/g,同时提高了材料高倍率充放电性能和循环稳定性。
The crystal structure of LiFePO4 is Olivine. This type of cathode material has gradually become a new research focus in the world. Studies show that theoretical capacity of the new cathode material is 170mAh/g. The material's platform is very stable which can be compared with stable electrical source. The material has good cycle performance and the material's thermal stability is better than any other known cathode material. The material has medium voltage (3.4V) and is non-toxic and real green.
In this study, we synthesized carbon-coated lithium iron phosphate using a combination of solid phase synthesis with liquid phase ones. The raw materials are lithium carbonate, phosphoric acid, ferric oxide, glucose, citric acid and proper amount of distilled water. The procedures of synthesizing carbon coated lithium iron phosphate have raw material mixing, drying, ball milling and sintering. We determined carbon-coated lithium iron phosphate crystal structure using XRD technology and measured lithium iron phosphate particle size using laser particle size analyzer. We tested its electrochemical properties using charge-discharge instrument and cyclic voltammeter.
We found that lithium iron phosphate using a combination of solid phase synthesis with liquid phase ones followed by heat treatment, the addition of carbon can be effective against lithium iron phosphate particles growing up, to get a small uniform particle size material in the experiment. The role of carbon added are:①As a reducing agent to reduce trivalent iron to ferrous iron;②coated lithium iron phosphate particles in the surface to improve electrical conductivity of materials;③controlling of high temperature solid state synthesizing lithium iron phosphate material particle size. In synthesizing lithium iron phosphate material process, we added glucose, sucrose, lactose, acetylene black separately. Lithium iron phosphate materials synthesizing with adding glucose, lactose show better electrochemical properties that specific capacity are all 139.8mAh/g or more at room temperature, while lithium iron phosphate materials synthesizing with adding acetylene black has only 93.44mAh/g . Constant charge and discharge rate was 0.2C.
We synthesized lithium iron phosphate with the solid state method. In the process of preparing composite materials, the sintering temperature and sintering time have great effects on the material's properties. We synthesized lithium iron phosphate at 500℃, 550℃, 600℃, 650℃, 700℃, 750℃, 800℃sintering temperature with 8 hours. Laboratory test results show: at room temperature, the constant charge and discharge rate was 0.2C, the material synthesized at 500℃, 550℃sintering temperature have no capacity. The material's specific capacity synthesized at 600℃sintering temperature is 20mAh/g. The material's specific capacity synthesized at 650℃, 700℃sintering temperature are all 140mAh/g around. The material's specific capacity synthesized at750℃, 800℃sintering temperature are 120mAh/g, 80mAh/g separately. The results show that the carbon-coated lithium iron phosphate synthesized at 700℃sintering temperature has the best chemical properties. We synthesized carbon-coated lithium iron phosphate at 700℃sintered 2, 4, 6, 8, 12, 16 hours separately. The results showed that carbon-coated lithium iron phosphate sintered 8 hours has the best electrochemical properties.
We synthesized lithium iron phosphate with the solid state method. In the experiment, we studied the effects that doping 1%MgCO3, CrO3, (NH4)6Mo7O24·4H2O in synthesizing carbon-coated lithium iron phosphate on its' electrochemical properties. The experimental result showed that carbon-coated lithium iron phosphate doped 1%CrO3 has the best electrochemical properties. Constant charge and discharge rate was 0.2C.Specific capacity of carbon-coated lithium iron phosphate doped 1%CrO3 is 145mAh/g, while enhancing the material's high rate discharge specific capacity and cycle stability.
固、液结合法合成LiFePO4/C材料,用Li2CO3、H3PO4、Fe2O3、葡萄糖、柠檬酸、蒸馏水为原料。将原料充分研磨均匀、烘干、球磨、焙烧,制得LiFePO4/C材料。用XRD对合成的LiFePO4/C材料进行结构测定,用激光粒度分析仪测定材料粒径。用恒流充放电、循环伏安扫描技术测试材料电化学性能。
实验研究发现,高温固液结合法合成LiFePO4时,加入碳能有效阻止材料颗粒长大,得到粒径细小均匀的材料。加入碳的作用有:①作为还原剂将Fe3+还原为Fe2+;②包覆在LiFePO4颗粒表面提高材料导电性;③控制高温固相合成LiFePO4材料的颗粒粒径。分别加入了葡萄糖、蔗糖、乳糖、乙炔黑作为碳添加剂合成LiFePO4/C材料,结果显示加入葡萄糖、乳糖效果较好,室温0.2C恒流放电比容量都在139.8mAh/g以上,乙炔黑效果较差,只有93.44mAh/g。
高温固相法合成LiFePO4/C材料,实验考察了焙烧温度、焙烧时间对材料性能的影响。分别在500℃、550℃、600℃、650℃、700℃、750℃、800℃下焙烧8小时制得材料,测试结果显示:室温、0.2C恒流放电,500℃、550℃制备的材料没有容量,600℃制备的材料比容量为20mAh/g,650℃、700℃制备的材料比容量为140mAh/g左右,750℃、800℃制备的材料比容量分别为120mAh/g、80mAh/g。实验表明,700℃合成的LiFePO4/C材料电化学性能最好。700℃分别焙烧2、4、6、8、12、16小时合成LiFePO4/C材料。实验表明,焙烧8h合成的LiFePO4/C材料电化学性能最好。
高温固相法合成LiFePO4/C材料,实验考察了掺杂1%MgCO3、CrO3、(NH4)6Mo7O24·4H2O对合成的LiFePO4/C材料电化学性能的影响。实验表明,掺杂1%CrO3合成的LiFePO4/C材料电化学性能最好,0.2C恒流放电比容量是145 mAh/g,同时提高了材料高倍率充放电性能和循环稳定性。
The crystal structure of LiFePO4 is Olivine. This type of cathode material has gradually become a new research focus in the world. Studies show that theoretical capacity of the new cathode material is 170mAh/g. The material's platform is very stable which can be compared with stable electrical source. The material has good cycle performance and the material's thermal stability is better than any other known cathode material. The material has medium voltage (3.4V) and is non-toxic and real green.
In this study, we synthesized carbon-coated lithium iron phosphate using a combination of solid phase synthesis with liquid phase ones. The raw materials are lithium carbonate, phosphoric acid, ferric oxide, glucose, citric acid and proper amount of distilled water. The procedures of synthesizing carbon coated lithium iron phosphate have raw material mixing, drying, ball milling and sintering. We determined carbon-coated lithium iron phosphate crystal structure using XRD technology and measured lithium iron phosphate particle size using laser particle size analyzer. We tested its electrochemical properties using charge-discharge instrument and cyclic voltammeter.
We found that lithium iron phosphate using a combination of solid phase synthesis with liquid phase ones followed by heat treatment, the addition of carbon can be effective against lithium iron phosphate particles growing up, to get a small uniform particle size material in the experiment. The role of carbon added are:①As a reducing agent to reduce trivalent iron to ferrous iron;②coated lithium iron phosphate particles in the surface to improve electrical conductivity of materials;③controlling of high temperature solid state synthesizing lithium iron phosphate material particle size. In synthesizing lithium iron phosphate material process, we added glucose, sucrose, lactose, acetylene black separately. Lithium iron phosphate materials synthesizing with adding glucose, lactose show better electrochemical properties that specific capacity are all 139.8mAh/g or more at room temperature, while lithium iron phosphate materials synthesizing with adding acetylene black has only 93.44mAh/g . Constant charge and discharge rate was 0.2C.
We synthesized lithium iron phosphate with the solid state method. In the process of preparing composite materials, the sintering temperature and sintering time have great effects on the material's properties. We synthesized lithium iron phosphate at 500℃, 550℃, 600℃, 650℃, 700℃, 750℃, 800℃sintering temperature with 8 hours. Laboratory test results show: at room temperature, the constant charge and discharge rate was 0.2C, the material synthesized at 500℃, 550℃sintering temperature have no capacity. The material's specific capacity synthesized at 600℃sintering temperature is 20mAh/g. The material's specific capacity synthesized at 650℃, 700℃sintering temperature are all 140mAh/g around. The material's specific capacity synthesized at750℃, 800℃sintering temperature are 120mAh/g, 80mAh/g separately. The results show that the carbon-coated lithium iron phosphate synthesized at 700℃sintering temperature has the best chemical properties. We synthesized carbon-coated lithium iron phosphate at 700℃sintered 2, 4, 6, 8, 12, 16 hours separately. The results showed that carbon-coated lithium iron phosphate sintered 8 hours has the best electrochemical properties.
We synthesized lithium iron phosphate with the solid state method. In the experiment, we studied the effects that doping 1%MgCO3, CrO3, (NH4)6Mo7O24·4H2O in synthesizing carbon-coated lithium iron phosphate on its' electrochemical properties. The experimental result showed that carbon-coated lithium iron phosphate doped 1%CrO3 has the best electrochemical properties. Constant charge and discharge rate was 0.2C.Specific capacity of carbon-coated lithium iron phosphate doped 1%CrO3 is 145mAh/g, while enhancing the material's high rate discharge specific capacity and cycle stability.
引文
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