CN105489860A - Anode material for lithium-ion battery and preparation method of anode material - Google Patents
Anode material for lithium-ion battery and preparation method of anode material Download PDFInfo
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Abstract
Description
技术领域technical field
本发明涉及化学合成工艺技术领域，具体地说是一种锂离子电池负极材料及其制备方法。The invention relates to the technical field of chemical synthesis technology, in particular to a lithium ion battery negative electrode material and a preparation method thereof.
背景技术Background technique
锂离子电池负极材料要求其具有良好的比容量与体积比容量，首次充放电效率高、循环性能好及降低成本。Sn最为负极材料具有的高比容量但其循环稳定性能差，充放电过程中体积变化大，限制了Sn作为离离子负极材料的发展。为解决Sn在充放电过程中的体积骤变，一般方法是把Sn制备成纳米颗粒，但因充放电过程中，Sn纳米粒子容易会发生团聚，本质问题仍无法解决。另一种方法是合成Sn/碳化合物来降低Sn的体积骤变。但是该方法退火温度很高，成本无法降低。Lithium-ion battery anode materials are required to have good specific capacity and volume specific capacity, high initial charge and discharge efficiency, good cycle performance and low cost. Sn is the most negative electrode material with high specific capacity, but its poor cycle stability and large volume change during charge and discharge limit the development of Sn as an ionizing negative electrode material. In order to solve the sudden volume change of Sn during the charge and discharge process, the general method is to prepare Sn into nanoparticles. However, during the charge and discharge process, Sn nanoparticles are prone to agglomeration, and the essential problem still cannot be solved. Another approach is to synthesize Sn/carbon compounds to reduce the sudden volume change of Sn. However, the annealing temperature of this method is very high, and the cost cannot be reduced.
发明内容Contents of the invention
为了弥补以上不足，本发明提供了一种Sn循环稳定好、有效提高了过渡金属碳酸盐的导电性的锂离子电池负极材料，以解决上述背景技术中的问题。In order to make up for the above deficiencies, the present invention provides a lithium-ion battery negative electrode material with good Sn cycle stability and effectively improved conductivity of transition metal carbonates, so as to solve the above-mentioned problems in the background technology.
本发明的技术方案是：Technical scheme of the present invention is:
一种锂离子电池负极材料，包括基体和分散在基体的金属纳米材料；A negative electrode material for a lithium ion battery, comprising a matrix and metal nanomaterials dispersed in the matrix;
所述基体为过渡金属碳酸盐MCO3；The matrix is transition metal carbonate MCO 3 ;
分散在基体中的金属纳米粒子为Sn。The metal nanoparticles dispersed in the matrix are Sn.
作为优选的技术方案，所述金属碳酸盐MCO3中M为Mn，Co，Ni,Fe中的一种、两种或三种。As a preferred technical solution, M in the metal carbonate MCO 3 is one, two or three of Mn, Co, Ni and Fe.
作为优选的技术方案，所述分散在基体中的金属纳米粒子Sn尺寸为60～80nm。As a preferred technical solution, the size of the metal nanoparticles Sn dispersed in the matrix is 60-80 nm.
本发明还提供了一种制备上述Sn循环稳定好、有效提高了过渡金属碳酸盐的导电性的锂离子电池负极材料的方法，以解决上述背景技术中的问题。The present invention also provides a method for preparing the lithium-ion battery negative electrode material with good Sn cycle stability and effectively improved conductivity of transition metal carbonates, so as to solve the above-mentioned problems in the background technology.
本发明的技术方案是：Technical scheme of the present invention is:
一种制备锂离子电池负极材料方法，包括步骤：A method for preparing negative electrode materials for lithium ion batteries, comprising the steps of:
1)将Mn、Co、Ni、Fe中的一种、两种或三种的醋酸盐加入乙二醇中，在温度为30～50℃时与尿素共沉积；1) Add one, two or three acetates of Mn, Co, Ni, Fe to ethylene glycol, and co-deposit with urea at a temperature of 30-50°C;
2)将Sn纳米粒子加入混合溶液中，搅拌40～80分钟；2) adding Sn nanoparticles into the mixed solution and stirring for 40-80 minutes;
3)将溶液置于高压灭菌器中，150～300℃下热处理15～24小时；3) placing the solution in an autoclave, and heat-treating at 150-300° C. for 15-24 hours;
4)将沉淀物分离，蒸馏水清洗，冷却干燥，制得Sn粒子嵌入式的过渡金属碳酸盐粉末，即所述锂离子电池负极材料。4) The precipitate is separated, washed with distilled water, cooled and dried to obtain a transition metal carbonate powder embedded with Sn particles, which is the negative electrode material of the lithium ion battery.
作为优选的技术方案，所述步骤1)中将Mn、Co、Ni、Fe中的一种、两种或三种的醋酸盐加入乙二醇中，在温度为30～50℃时与尿素共沉积；其中金属的总含量与醋酸根的摩尔比为0.8：0.2，金属醋酸盐与乙二醇的摩尔比为0.01～0.02：1，尿素与乙二醇溶液的摩尔比为0.04～0.06：1。As a preferred technical scheme, in the step 1), one, two or three acetates of Mn, Co, Ni, Fe are added to ethylene glycol, and when the temperature is 30-50°C, it is mixed with urea Co-deposition; the molar ratio of total metal content to acetate is 0.8:0.2, the molar ratio of metal acetate to ethylene glycol is 0.01-0.02:1, and the molar ratio of urea to ethylene glycol solution is 0.04-0.06 :1.
作为优选的技术方案，所述步骤2)中Sn纳米粒子颗粒尺寸为60～80nm。As a preferred technical solution, the particle size of the Sn nanoparticles in the step 2) is 60-80 nm.
作为优选的技术方案，所述步骤3)中高压灭菌器中为饱和蒸汽压，热处理为常压。As a preferred technical solution, in the step 3), the autoclave is at saturated vapor pressure, and the heat treatment is at normal pressure.
作为优选的技术方案，所述步骤4)制得的Sn粒子嵌入式的过渡金属碳酸盐粉末中Sn粒子重量为所述过渡金属碳酸盐粉末重量的5～25％。As a preferred technical solution, the weight of Sn particles in the Sn particle-embedded transition metal carbonate powder prepared in step 4) is 5-25% of the weight of the transition metal carbonate powder.
本发明用一种低温一步式热溶剂法来合成Sn与过渡金属碳酸盐的化合物，有效解决了Sn循环稳定差的问题也提高了过渡金属碳酸盐的导电性。The invention uses a low-temperature one-step hot solvent method to synthesize the compound of Sn and transition metal carbonate, which effectively solves the problem of poor cycle stability of Sn and improves the conductivity of the transition metal carbonate.
由于采用了上述技术方案，一种锂离子电池负极材料及其制备方法，包括步骤：1)将Mn、Co、Ni、Fe中的一种、两种或三种的醋酸盐加入乙二醇中，在温度为30～50℃时与尿素共沉积；2)将Sn纳米粒子加入混合溶液中，搅拌40～80分钟；3)将溶液置于高压灭菌器中，150～300℃下热处理15～24小时；4)将沉淀物分离，蒸馏水清洗，冷却干燥，制得Sn粒子嵌入式的过渡金属碳酸盐粉末，即所述锂离子电池负极材料；本发明的锂离子负极材料具有良好的电化学性能，电能储存容量大，循环稳定性良好，在工作电流为100mA/g时，蓄电量大于900mAh/g在循环100次之后蓄电量仍大于550mAh/g。Owing to having adopted above-mentioned technical scheme, a kind of negative electrode material of lithium ion battery and preparation method thereof comprise the steps: 1) adding one, two or three kinds of acetates in Mn, Co, Ni, Fe to ethylene glycol 2) Add Sn nanoparticles into the mixed solution and stir for 40-80 minutes; 3) Put the solution in an autoclave and heat-treat it at 150-300°C 15～24 hours; 4) sediment is separated, washed with distilled water, cooled and dried to make the transition metal carbonate powder embedded in Sn particles, that is, the lithium ion battery negative electrode material; the lithium ion negative electrode material of the present invention has good Excellent electrochemical performance, large electric energy storage capacity, and good cycle stability. When the working current is 100mA/g, the storage capacity is greater than 900mAh/g, and the storage capacity is still greater than 550mAh/g after 100 cycles.
具体实施方式detailed description
一种锂离子电池负极材料，包括基体和分散在基体的金属纳米材料；A negative electrode material for a lithium ion battery, comprising a matrix and metal nanomaterials dispersed in the matrix;
所述基体为过渡金属碳酸盐MCO3；The matrix is transition metal carbonate MCO 3 ;
分散在基体中的金属纳米粒子为Sn。The metal nanoparticles dispersed in the matrix are Sn.
所述金属碳酸盐MCO3中M为Mn，Co，Ni,Fe中的一种、两种或三种。M in the metal carbonate MCO 3 is one, two or three of Mn, Co, Ni and Fe.
所述分散在基体中的金属纳米粒子Sn尺寸为60～80nm。The size of the metal nanoparticles Sn dispersed in the matrix is 60-80nm.
一种制备锂离子电池负极材料方法，包括步骤：A method for preparing negative electrode materials for lithium ion batteries, comprising the steps of:
1)将Mn、Co、Ni、Fe中的一种、两种或三种的醋酸盐加入乙二醇中，在温度为30～50℃时与尿素共沉积；1) Add one, two or three acetates of Mn, Co, Ni, Fe to ethylene glycol, and co-deposit with urea at a temperature of 30-50°C;
2)将Sn纳米粒子加入混合溶液中，搅拌40～80分钟；2) adding Sn nanoparticles into the mixed solution and stirring for 40-80 minutes;
3)将溶液置于高压灭菌器中，150～300℃下热处理15～24小时；3) placing the solution in an autoclave, and heat-treating at 150-300° C. for 15-24 hours;
4)将沉淀物分离，蒸馏水清洗，冷却干燥，制得Sn粒子嵌入式的过渡金属碳酸盐粉末，即所述锂离子电池负极材料。4) The precipitate is separated, washed with distilled water, cooled and dried to obtain a transition metal carbonate powder embedded with Sn particles, which is the negative electrode material of the lithium ion battery.
所述步骤1)中将Mn、Co、Ni、Fe中的一种、两种或三种的醋酸盐加入乙二醇中，在温度为30～50℃时与尿素共沉积；其中金属的总含量与醋酸根的摩尔比为0.8：0.2，金属醋酸盐与乙二醇的摩尔比为0.01～0.02：1，尿素与乙二醇溶液的摩尔比为0.04～0.06：1。In the step 1), one, two or three acetates of Mn, Co, Ni and Fe are added to ethylene glycol, and are co-deposited with urea at a temperature of 30-50° C.; The molar ratio of total content to acetate is 0.8:0.2, the molar ratio of metal acetate to ethylene glycol is 0.01-0.02:1, and the molar ratio of urea to ethylene glycol solution is 0.04-0.06:1.
所述步骤2)中Sn纳米粒子颗粒尺寸为60～80nm。The size of the Sn nanoparticles in the step 2) is 60-80nm.
所述步骤3)中高压灭菌器中为饱和蒸汽压，热处理为常压。The autoclave in the step 3) is saturated vapor pressure, and the heat treatment is normal pressure.
所述步骤4)制得的Sn粒子嵌入式的过渡金属碳酸盐粉末中Sn粒子重量为所述过渡金属碳酸盐粉末重量的5～25％。The weight of Sn particles in the Sn particle-embedded transition metal carbonate powder prepared in the step 4) is 5-25% of the weight of the transition metal carbonate powder.
本发明用一种低温一步式热溶剂法来合成Sn与过渡金属碳酸盐的化合物，有效解决了Sn循环稳定差的问题也提高了过渡金属碳酸盐的导电性。The invention uses a low-temperature one-step hot solvent method to synthesize the compound of Sn and transition metal carbonate, which effectively solves the problem of poor cycle stability of Sn and improves the conductivity of the transition metal carbonate.
下面结合具体实施例进一步阐述本发明。The present invention is further described below in conjunction with specific examples.
实施例一：Embodiment one:
一种制备锂离子电池负极材料方法，包括步骤：A method for preparing negative electrode materials for lithium ion batteries, comprising the steps of:
1)将Mn的醋酸盐加入乙二醇中，在温度为30℃时与尿素共沉积；1) Add Mn acetate to ethylene glycol, and co-deposit with urea at a temperature of 30°C;
2)将Sn纳米粒子加入混合溶液中，搅拌40分钟；2) adding Sn nanoparticles into the mixed solution and stirring for 40 minutes;
3)将溶液置于高压灭菌器中，150℃下热处理15～24小时；3) placing the solution in an autoclave, and heat-treating at 150° C. for 15 to 24 hours;
4)将沉淀物分离，蒸馏水清洗，冷却干燥，制得Sn粒子嵌入式的过渡金属碳酸盐粉末，即所述锂离子电池负极材料。4) The precipitate is separated, washed with distilled water, cooled and dried to obtain a transition metal carbonate powder embedded with Sn particles, which is the negative electrode material of the lithium ion battery.
所述步骤1)中将5mmol的Mn的醋酸盐加入8ml乙二醇中，在温度为30℃时与20mmol尿素共沉积；In the step 1), add 5 mmol of Mn acetate into 8 ml of ethylene glycol, and co-deposit with 20 mmol of urea at a temperature of 30° C.;
所述步骤2)中Sn纳米粒子颗粒尺寸为60nm，重量含量为MnCO3的5％；In the step 2), the particle size of Sn nanoparticles is 60nm, and the weight content is 5% of MnCO 3 ;
所述步骤3)中高压灭菌器中为饱和蒸汽压，热处理为常压。The autoclave in the step 3) is saturated vapor pressure, and the heat treatment is normal pressure.
实施例二：Embodiment two:
一种制备锂离子电池负极材料方法，包括步骤：A method for preparing negative electrode materials for lithium ion batteries, comprising the steps of:
1)将Co的醋酸盐加入乙二醇中，在温度为40℃时与尿素共沉积；1) Add Co acetate to ethylene glycol and co-deposit with urea at a temperature of 40°C;
2)将Sn纳米粒子加入混合溶液中，搅拌50分钟；2) adding Sn nanoparticles into the mixed solution and stirring for 50 minutes;
3)将溶液置于高压灭菌器中，200℃下热处理18小时；3) Place the solution in an autoclave and heat-treat it at 200°C for 18 hours;
4)将沉淀物分离，蒸馏水清洗，冷却干燥，制得Sn粒子嵌入式的过渡金属碳酸盐粉末，即所述锂离子电池负极材料。4) The precipitate is separated, washed with distilled water, cooled and dried to obtain a transition metal carbonate powder embedded with Sn particles, which is the negative electrode material of the lithium ion battery.
所述步骤1)中将7mmol的Co的醋酸盐加入10ml的乙二醇中，在温度为40℃时与22mmol的尿素共沉积；In the step 1), 7 mmol of Co acetate was added to 10 ml of ethylene glycol, and co-deposited with 22 mmol of urea at a temperature of 40° C.;
所述步骤2)中Sn纳米粒子颗粒尺寸为70nm，重量含量为CoCO3的15％。The particle size of the Sn nanoparticles in the step 2) is 70nm, and the weight content is 15% of CoCO 3 .
所述步骤3)中高压灭菌器中为饱和蒸汽压，热处理为常压。The autoclave in the step 3) is saturated vapor pressure, and the heat treatment is normal pressure.
实施例三：Embodiment three:
一种制备锂离子电池负极材料方法，包括步骤：A method for preparing negative electrode materials for lithium ion batteries, comprising the steps of:
1)将Ni的醋酸盐加入乙二醇中，在温度为50℃时与尿素共沉积；1) Add Ni acetate to ethylene glycol, and co-deposit with urea at a temperature of 50°C;
2)将Sn纳米粒子加入混合溶液中，搅拌80分钟；2) adding Sn nanoparticles into the mixed solution and stirring for 80 minutes;
3)将溶液置于高压灭菌器中，250℃下热处理20小时；3) The solution is placed in an autoclave, and heat-treated at 250° C. for 20 hours;
4)将沉淀物分离，蒸馏水清洗，冷却干燥，制得Sn粒子嵌入式的过渡金属碳酸盐粉末，即所述锂离子电池负极材料。4) The precipitate is separated, washed with distilled water, cooled and dried to obtain a transition metal carbonate powder embedded with Sn particles, which is the negative electrode material of the lithium ion battery.
所述步骤1)中将6mmol的Ni的醋酸盐加入10ml乙二醇中，在温度为50℃时与23mmol尿素共沉积；In the step 1), 6 mmol of Ni acetate was added to 10 ml of ethylene glycol, and co-deposited with 23 mmol of urea at a temperature of 50° C.;
所述步骤2)中Sn纳米粒子颗粒尺寸为80nm，重量含量为NiCO3的25％。The particle size of the Sn nanoparticles in the step 2) is 80nm, and the weight content is 25% of NiCO 3 .
所述步骤3)中高压灭菌器中为饱和蒸汽压，热处理为常压。The autoclave in the step 3) is saturated vapor pressure, and the heat treatment is normal pressure.
实施例四Embodiment four
一种制备锂离子电池负极材料方法，包括步骤：A method for preparing negative electrode materials for lithium ion batteries, comprising the steps of:
1)将Fe的醋酸盐加入乙二醇中，在温度为38℃时与尿素共沉积；1) Fe acetate is added to ethylene glycol and co-deposited with urea at a temperature of 38°C;
2)将Sn纳米粒子加入混合溶液中，搅拌60分钟；2) adding Sn nanoparticles into the mixed solution and stirring for 60 minutes;
3)将溶液置于高压灭菌器中，240℃下热处理22小时；3) Place the solution in an autoclave and heat-treat it at 240°C for 22 hours;
4)将沉淀物分离，蒸馏水清洗，冷却干燥，制得Sn粒子嵌入式的过渡金属碳酸盐粉末，即所述锂离子电池负极材料。4) The precipitate is separated, washed with distilled water, cooled and dried to obtain a transition metal carbonate powder embedded with Sn particles, which is the negative electrode material of the lithium ion battery.
所述步骤1)中将5mmol的Fe的醋酸盐加入10ml的乙二醇中，在温度为45℃时与22mmol的尿素共沉积。In the step 1), 5 mmol of Fe acetate was added into 10 ml of ethylene glycol, and co-deposited with 22 mmol of urea at a temperature of 45° C.
所述步骤2)中Sn纳米粒子颗粒尺寸为65nm，重量含量为FeCO3的10％。The particle size of the Sn nanoparticles in the step 2) is 65nm, and the weight content is 10% of FeCO 3 .
所述步骤3)中高压灭菌器中为饱和蒸汽压，热处理为常压。The autoclave in the step 3) is saturated vapor pressure, and the heat treatment is normal pressure.
实施例五Embodiment five
一种制备锂离子电池负极材料方法，包括步骤：A method for preparing negative electrode materials for lithium ion batteries, comprising the steps of:
1)将Mn、Co、Ni的醋酸盐加入乙二醇中，在温度为50℃时与尿素共沉积；1) Add acetates of Mn, Co and Ni to ethylene glycol, and co-deposit with urea at a temperature of 50°C;
2)将Sn纳米粒子加入混合溶液中，搅拌80分钟；2) adding Sn nanoparticles into the mixed solution and stirring for 80 minutes;
3)将溶液置于高压灭菌器中，300℃下热处理24小时；3) Place the solution in an autoclave and heat-treat it at 300°C for 24 hours;
4)将沉淀物分离，蒸馏水清洗，冷却干燥，制得Sn粒子嵌入式的过渡金属碳酸盐粉末，即所述锂离子电池负极材料。4) The precipitate is separated, washed with distilled water, cooled and dried to obtain a transition metal carbonate powder embedded with Sn particles, which is the negative electrode material of the lithium ion battery.
所述步骤1)中将6mmol的Mn、Co、Ni的醋酸盐加入10ml乙二醇中，Mn:Co:Ni的摩尔比例为0.5:0.15:0.15，金属总和与醋酸根的摩尔比例为0.8:0.2，在温度为50℃时与22.7mmol的尿素共沉积。In the step 1), the acetate of 6mmol of Mn, Co, Ni is added in 10ml of ethylene glycol, the molar ratio of Mn:Co:Ni is 0.5:0.15:0.15, and the molar ratio of metal sum to acetate is 0.8 :0.2, co-deposition with 22.7mmol of urea at a temperature of 50°C.
所述步骤2)中Sn纳米粒子颗粒尺寸为80nm，重量含量为过渡金属碳酸盐的25％。The particle size of the Sn nanoparticles in the step 2) is 80nm, and the weight content is 25% of the transition metal carbonate.
所述步骤3)中高压灭菌器中为饱和蒸汽压，热处理为常压。The autoclave in the step 3) is saturated vapor pressure, and the heat treatment is normal pressure.
以上显示和描述了本发明的基本原理、主要特征及本发明的优点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。The basic principles, main features and advantages of the present invention have been shown and described above. Those skilled in the industry should understand that the present invention is not limited by the above-mentioned embodiments. What are described in the above-mentioned embodiments and the description only illustrate the principle of the present invention. Without departing from the spirit and scope of the present invention, the present invention will also have Variations and improvements are possible, which fall within the scope of the claimed invention. The protection scope of the present invention is defined by the appended claims and their equivalents.
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