WO2017032155A1 - Preparation method for lithium battery lithium titanate negative electrode slurry - Google Patents
Preparation method for lithium battery lithium titanate negative electrode slurry Download PDFInfo
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- WO2017032155A1 WO2017032155A1 PCT/CN2016/086292 CN2016086292W WO2017032155A1 WO 2017032155 A1 WO2017032155 A1 WO 2017032155A1 CN 2016086292 W CN2016086292 W CN 2016086292W WO 2017032155 A1 WO2017032155 A1 WO 2017032155A1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Definitions
- the patent relates to the field of lithium ion batteries, in particular to a preparation process and a method for a lithium titanate anode material slurry.
- Lithium-ion batteries have the advantages of high energy density, small self-discharge, no memory effect, wide operating voltage range, long service life and no environmental pollution. They are the main power source for new energy vehicles.
- Carbon materials have been widely used in lithium ion batteries because of their low cost, non-toxicity and superior electrochemical properties. Its interface state and fine structure have a great influence on electrode performance.
- commercial lithium-ion battery carbon anode materials can be divided into lithium titanate, hard carbon and soft carbon.
- graphite materials are still the mainstream of lithium-ion battery anode materials.
- Graphite-based carbon materials which have the advantages of low lithium insertion/deintercalation potential, suitable reversible capacity, abundant resources, and low price, are ideal anode materials for lithium ion batteries. However, its theoretical specific capacity is only 372 mAh/g, which limits the further improvement of the specific energy of lithium-ion batteries and cannot meet the needs of the increasingly high-energy portable mobile power sources.
- Li 4 Ti 5 O 12 is a new type of negative electrode material for lithium ion secondary batteries. Compared with other commercial materials, Li 4 Ti 5 O 12 has the advantages of good cycle performance, no reaction with electrolyte, high safety performance, and stable charge and discharge platform. It is one of the most excellent anode materials for lithium-ion batteries that has received much attention in recent years. Compared with carbon negative electrode materials, lithium titanate has many advantages.
- the deintercalation of lithium ions in lithium titanate is reversible, and the crystal form of lithium ion in the process of inserting or extracting lithium titanate is not Changed, volume change is less than 1%, so it is called "zero strain material", which can avoid the structure damage caused by the back and forth expansion of the electrode material in the charge and discharge cycle, thereby improving the cycle performance and service life of the electrode, reducing the The number of cycles increases and the specific capacity is greatly attenuated, which has better cycle performance than the carbon negative electrode; however, since lithium titanate is an insulating material, its electrical conductivity is low, resulting in the rate performance in the application of lithium battery. Poor problem, while the theoretical specific capacity of lithium titanate material is 175mAh/g, the actual specific capacity is greater than 160mAh/g, and has the disadvantages of low gram capacity.
- a lithium ion battery generally includes a positive electrode sheet, a negative electrode sheet, and a separator interposed between the positive electrode sheet and the negative electrode sheet.
- the positive electrode tab includes a positive electrode current collector and a positive electrode film coated on the positive electrode current collector
- the negative electrode plate includes a negative electrode current collector and is coated on the negative electrode set Negative film on the fluid.
- an active material such as lithium cobaltate, graphite, etc.
- a conductive agent such as acetylene black, carbon nanotubes, carbon fiber, etc.
- a binder such as polyvinylidene fluoride, polyvinylpyrrolidone, Carboxymethylcellulose sodium, styrene-butadiene rubber emulsion, etc.
- a solvent such as N-methylpyrrolidone, water, etc.
- the performance of the electrode paste has an important influence on the performance of the lithium ion battery.
- the effect of the active substance can be exerted during charging and discharging, and the average gram capacity is exerted. Will be improved to improve the performance of the full battery.
- the conventional negative electrode slurry preparation method is to carry out the high-speed double-planetary dispersion of the conductive agent with the thickener solution, and then add the negative electrode active material, stir for a certain period of time, and then add the binder to pass through the line. The time was stirred to obtain the final negative electrode slurry.
- This method firstly requires a long time treatment for the dispersion of the conductive agent, which takes a long time and is not ideal in the dispersion state, especially for the preparation of a slurry using a carbon nanotube (CNT), graphene or the like as a conductive agent; the second conventional process needs to be During the preparation of the slurry, the stirring system is kept under vacuum, which causes the internal temperature of the slurry system to rise easily, and at the same time, externally added circulating water for cooling, so the requirements and wear of the equipment are high.
- the above results in low slurry preparation efficiency, poor stability, and unsatisfactory effect, which will affect the preparation of the subsequent pole piece and the performance of the lithium battery.
- the object of the present invention is to provide a method for preparing a lithium battery lithium titanate negative electrode slurry, which can uniformly disperse the components of the slurry in a short time, and the prepared slurry has good uniformity and excellent stability. At the same time, the prepared battery sheet adhesion is improved, and thus the consistency of the battery and the electrochemical performance of the battery are improved.
- the lithium titanate and the conductive agent are added to the mixing tank in proportion and stirred for 30 to 40 minutes, and at the end of the time 1/2 and at the end, the powder on the paddle and the barrel is scraped;
- High-viscosity stirring adding 55% to 60% of the total amount of the thickener solution to the stirred powder, stirring and dispersing for 60 to 70 minutes, and at the time of 1/3, 2/3 and end When the slurry is scraped on the paddle and the barrel, the temperature of the slurry is controlled between 25 and 35 ° C;
- Low-viscosity stirring add 35 to 30% of the total amount of the thickener solution to the above-mentioned high-viscosity stirred slurry, stir and disperse for 60 to 70 minutes, and at time 1/3, 2/3 and At the end, scrape the slurry on the paddle and the barrel, and control the temperature of the slurry. Between 25 and 35 ° C;
- Viscosity test the viscosity of the slurry with low viscosity stirring in the above steps is tested for viscosity, such as in the normal range of 2000-5000 Mpa ⁇ S, directly into the next step; if it exceeds the above range, 5% of the total amount of thickener solution is added. ⁇ 10%, stir and disperse for a period of 30 to 40 minutes, and at time 1/2 and at the end, scrape the slurry on the paddle and the barrel, and then test the viscosity of the slurry to reach the viscosity range.
- Next step the viscosity of the slurry with low viscosity stirring in the above steps is tested for viscosity, such as in the normal range of 2000-5000 Mpa ⁇ S, directly into the next step; if it exceeds the above range, 5% of the total amount of thickener solution is added. ⁇ 10%, stir and disperse for a period of 30 to 40 minutes, and at time 1/2 and at the end, scrape the
- Adding binder adding binder SBR, stirring and dispersing, the time is 10 to 30 minutes;
- Vacuum defoaming Under low-speed stirring state, the barrel is vacuumed, the degree of vacuum is -0.09 ⁇ -0.1MPa, and the time is 15-30 minutes, that is, the lithium titanate negative electrode slurry prepared by the method of the invention is obtained. .
- lithium titanate is a mixture of one or both of lithium titanate prepared from anatase type titanium dioxide or rutile type titanium dioxide.
- the conductive agent in the above step 2 is one or a mixture of conductive carbon black, conductive graphite, carbon nanotubes, carbon fibers, and graphene.
- the mass ratio of each component of lithium titanate, conductive agent, thickener and binder is (90-97): (1-4): (1-5) : (1-3), the solvent is 80% to 120% of the total amount of each of the above components.
- the agitation device is a dual planetary vacuum agitator, and the slurry temperature is controlled by a method of introducing a constant temperature circulating water to the planetary agitating barrel at a corresponding temperature.
- the present invention has the following advantages:
- the preparation time is short: the preparation time of the lithium titanate negative electrode slurry of the invention is about 265 to 380 minutes, and in the subsequent preparation process, the accumulation of the actual experience can omit the viscosity test step and directly enter the final vacuum elimination.
- the bubble process can save 30 to 40 minutes. If there are multiple devices to prepare the thickener solution, it can save 60 to 100 minutes, compared with the conventional anode slurry preparation process for about 7 to 9 hours. Increased production efficiency;
- equipment wear is small: the invention only needs to vacuum the barrel in the final vacuum defoaming process, compared with the traditional process in the slurry preparation process, the stirring system has been kept vacuuming, resulting in the stirring process The heat is difficult to dissipate, the temperature of the slurry is easy to rise, and the effect is substantially improved.
- the short-time vacuum treatment reduces the burden on the equipment and reduces equipment wear;
- the lithium titanate negative electrode slurry prepared by the invention has a solid content of about 45 to 55%, and has a high solid content and a low viscosity compared with the conventional preparation process, so the proportion of water used is Correspondingly, the energy consumption required for evaporation of water during subsequent coating is reduced;
- the invention firstly stirs and disperses the negative electrode active material and the conductive agent to avoid agglomeration of the conductive agent in the slurry, and adopts high-viscosity stirring and dispersion in the early stage, and the mechanical force of the stirring paddle on the slurry (extrusion) , collision, friction) large, can play a good dispersion effect, and then use low viscosity mixing, so that the components are completely dispersed.
- the lithium battery prepared by using the lithium battery lithium titanate negative electrode provided by the invention has low internal resistance, is not easy to generate heat, has high energy density, good cycle performance and long service life.
- the preparation steps are as follows:
- the negative electrode active material and the conductive agent are added to the stirring tank to be stirred and dispersed for 30 minutes, and the powder on the paddle and the barrel is scraped at the time of 15 minutes and 30 minutes;
- the test result is 5332 Mpa ⁇ S, the value of the normal range is 5%, the total amount of the solvent is added, and the dispersion is stirred for 30 minutes, and the time is 15 minutes. And 30 minutes, scrape the slurry on the paddle and the barrel, and then test the viscosity of the slurry.
- the test result is 4215Mpa ⁇ S, which meets the viscosity range requirement;
- the barrel is vacuumed, the degree of vacuum is -0.09 ⁇ -0.1MPa, and the time is 15 minutes, that is, the lithium titanate negative electrode slurry prepared by the method of the invention is obtained, and the total consumption time is about 265. minute.
- the lithium titanate negative electrode slurry is coated, dried, rolled, and cut into negative electrode sheets, and then assembled with lithium iron phosphate positive electrode sheets, separators, electrolytes, and battery casings. After the charge and discharge activation, a 18650 type cylindrical lithium iron phosphate battery with an initial design capacity of 1350 mA was obtained.
- the preparation takes about 7 hours, and according to the conventional production process of the lithium battery, a cylindrical lithium iron phosphate battery of 18650 type with an initial design capacity of 1350 mA is obtained.
- Example 1 The electrical properties of the 18650-type cylindrical lithium iron phosphate battery prepared in Example 1 and Comparative Example 1 were tested and charged and discharged at 1 C, and the cycle capacity retention rate was 1000 times.
- Example 1 was 98.14%
- Comparative Example 1 was 96.85%
- the energy density and internal resistance test comparison results are shown in Table 1.
- the preparation steps are as follows:
- the negative electrode active material and the conductive agent are added to the stirring tank to be stirred and dispersed for 40 minutes, and the powder on the paddle and the barrel is scraped at the time of 20 minutes and 40 minutes;
- the barrel is vacuumed, the degree of vacuum is -0.09 ⁇ -0.1MPa, and the time is 30 minutes, that is, the lithium titanate negative electrode slurry prepared by the method of the invention is obtained, and the total consumption time is about 360. minute.
- the lithium titanate negative electrode slurry is coated, dried, rolled, and cut into negative electrode sheets, and then assembled with lithium cobaltate positive electrode sheets, separators, electrolytes, and battery casings. After the charge and discharge were activated, a 18650 type cylindrical battery with an initial design capacity of 1600 mA was obtained.
- the preparation takes about 7.5 hours, and according to the conventional production process of the lithium battery, a cylindrical type battery of 18650 type and an initial design capacity of 1600 mA is obtained.
- Example 2 The electrical properties of the 18650-type cylindrical battery prepared in Example 2 and Comparative Example 2 were tested and charged and discharged at 1 C, and the cycle capacity retention rate was 1000 times, and Example 2 was 97.23%, and Comparative Example 2 was 93.23%.
- the energy density and internal resistance test comparison results are shown in Table 1.
- the lithium battery prepared by using the lithium titanate negative electrode slurry prepared by the method of the present invention has higher energy density than the lithium battery produced by the conventional negative electrode slurry production process, and has an internal resistance. Both are lower than the lithium battery produced by the conventional negative electrode slurry production process.
Abstract
A preparation method for a lithium battery lithium titanate negative electrode slurry. The various components of the slurry are uniformly dispersed within a relatively short time via steps such as thickener solution preparation, powder dispersion, high viscosity stirring, low viscosity stirring, viscosity testing, binder addition and vacuum defoaming. The prepared slurry has good uniformity and excellent stability, and the adhesion of a prepared battery pole piece is improved, thereby improving the consistency of a battery and the electrochemical performance of the battery. The preparation method has advantages such as a short preparation time, little equipment wear and tear, low production energy consumption and a good dispersion effect. A lithium battery made from the prepared lithium battery lithium titanate negative electrode slurry has a low internal resistance, does not easily generate heat, and has a high energy density, good cycling performance and a long service life.
Description
本专利涉及锂离子电池领域，具体为一种钛酸锂负极材料浆料的制备工艺及方法。The patent relates to the field of lithium ion batteries, in particular to a preparation process and a method for a lithium titanate anode material slurry.
目前随着全球性石油资源紧缺与气候环境的不断恶化，人类社会发展面临着严峻的挑战。发展清洁节能的新能源汽车受到世界各国的高度重视。新能源汽车的发展，关键在其动力电源。锂离子电池具有能量密度大、自放电小、无记忆效应、工作电压范围宽、使用寿命长、无环境污染等优点，是目前新能源汽车主要的动力电源。At present, with the shortage of global petroleum resources and the deteriorating climate environment, the development of human society faces severe challenges. The development of clean and energy-efficient new energy vehicles has been highly valued by countries around the world. The development of new energy vehicles is the key to their power supply. Lithium-ion batteries have the advantages of high energy density, small self-discharge, no memory effect, wide operating voltage range, long service life and no environmental pollution. They are the main power source for new energy vehicles.
碳材料以其价廉、无毒及其优越的电化学性能在锂离子电池中得到了广泛的应用，它本身的界面状况和微细结构对电极性能有很大的影响。目前，商品化的锂离子电池碳负极材料可分为钛酸锂、硬碳和软碳三类，其中石墨类材料依然是锂离子电池负极材料的主流。石墨类碳材料，具有较低的锂嵌入/脱嵌电位、合适的可逆容量且资源丰富、价格低廉等优点，是比较理想的锂离子电池负极材料。但其理论比容量只有372mAh/g，因而限制了锂离子电池比能量的进一步提高，不能满足日益发展的高能量便携式移动电源的需求。同时，石墨作为负极材料时，在首次充放电过程中在其表面形成一层固体电解质膜(SEI)，不可逆地消耗锂离子，形成不可逆容量损失。碳材料作为锂离子电池负极材料依然存在充放电容量低、初次循环不可逆损失大、溶剂分子共插层和制备成本高等缺点，这些也是在目前锂离子电池研究方面所需解决的关键问题。Carbon materials have been widely used in lithium ion batteries because of their low cost, non-toxicity and superior electrochemical properties. Its interface state and fine structure have a great influence on electrode performance. At present, commercial lithium-ion battery carbon anode materials can be divided into lithium titanate, hard carbon and soft carbon. Among them, graphite materials are still the mainstream of lithium-ion battery anode materials. Graphite-based carbon materials, which have the advantages of low lithium insertion/deintercalation potential, suitable reversible capacity, abundant resources, and low price, are ideal anode materials for lithium ion batteries. However, its theoretical specific capacity is only 372 mAh/g, which limits the further improvement of the specific energy of lithium-ion batteries and cannot meet the needs of the increasingly high-energy portable mobile power sources. At the same time, when graphite is used as a negative electrode material, a solid electrolyte membrane (SEI) is formed on the surface during the first charge and discharge process, and lithium ions are irreversibly consumed, resulting in irreversible capacity loss. As a negative electrode material for lithium ion batteries, carbon materials still have shortcomings such as low charge and discharge capacity, large irreversible loss of primary circulation, co-insertion of solvent molecules and high production cost. These are the key problems to be solved in the research of lithium ion batteries.
Li4Ti5O12作为一种新型的锂离子二次电池负极材料，与其它商业化的材料相比，具有循环性能好、不与电解液反应、安全性能高、充放电平台平稳等优点，是近几年来备受关注的最优异的锂离子电池负极材料之一。与碳负电极材料相比，钛酸锂有很多的优势，其中，锂离子在钛酸锂中的脱嵌是可逆的，而且锂离子在嵌入或脱出钛酸锂的过程中，其晶型不发生变化，体积变化小于1％，因此被称为“零应变材料”，能够避免充放电循环中由于电极材料的来回伸缩而导致结构的破坏，从而提高电极的循环性能和使用寿命，减少了随循环次数增加而带来比容量大幅度的衰减，具有比碳负极更优良的循环性能；但是，由于钛酸锂是一种绝缘材料，其电导率低，从而导致在锂电中的应用存在倍率性能较差的问题，同时钛酸锂材料理论比容量为175mAh/g，实际比容量大于160mAh/g，具有克容量较低等缺点。Li 4 Ti 5 O 12 is a new type of negative electrode material for lithium ion secondary batteries. Compared with other commercial materials, Li 4 Ti 5 O 12 has the advantages of good cycle performance, no reaction with electrolyte, high safety performance, and stable charge and discharge platform. It is one of the most excellent anode materials for lithium-ion batteries that has received much attention in recent years. Compared with carbon negative electrode materials, lithium titanate has many advantages. Among them, the deintercalation of lithium ions in lithium titanate is reversible, and the crystal form of lithium ion in the process of inserting or extracting lithium titanate is not Changed, volume change is less than 1%, so it is called "zero strain material", which can avoid the structure damage caused by the back and forth expansion of the electrode material in the charge and discharge cycle, thereby improving the cycle performance and service life of the electrode, reducing the The number of cycles increases and the specific capacity is greatly attenuated, which has better cycle performance than the carbon negative electrode; however, since lithium titanate is an insulating material, its electrical conductivity is low, resulting in the rate performance in the application of lithium battery. Poor problem, while the theoretical specific capacity of lithium titanate material is 175mAh/g, the actual specific capacity is greater than 160mAh/g, and has the disadvantages of low gram capacity.
锂离子电池一般包括正极片、负极片、间隔于正极片和负极片之间的隔膜。正极极片包括正极集流体和涂布在正极集流体上的正极膜片，负极片包括负极集流体和涂布在负极集
流体上的负极膜片。电极极片制备时，首先将活性物质(如钴酸锂、石墨等)、导电剂(如乙炔黑，碳纳米管、碳纤维等)、粘接剂(如聚偏氟乙烯、聚乙烯基吡咯烷酮、羧甲基纤维素钠、丁苯橡胶乳液等)和溶剂(如N-甲基吡咯烷酮、水等)一起制成电极浆料，再将其按要求涂覆在集流体表面，然后进行干燥，得到电池极片。A lithium ion battery generally includes a positive electrode sheet, a negative electrode sheet, and a separator interposed between the positive electrode sheet and the negative electrode sheet. The positive electrode tab includes a positive electrode current collector and a positive electrode film coated on the positive electrode current collector, and the negative electrode plate includes a negative electrode current collector and is coated on the negative electrode set
Negative film on the fluid. When preparing the electrode pole piece, firstly, an active material (such as lithium cobaltate, graphite, etc.), a conductive agent (such as acetylene black, carbon nanotubes, carbon fiber, etc.), a binder (such as polyvinylidene fluoride, polyvinylpyrrolidone, Carboxymethylcellulose sodium, styrene-butadiene rubber emulsion, etc.) and a solvent (such as N-methylpyrrolidone, water, etc.) are used together to form an electrode slurry, which is then coated on the surface of the current collector as required, and then dried to obtain Battery pole piece.
其中电极浆料的性能对锂离子电池的性能有着重要的影响。电极浆料中各组分分散得越均匀，极片便具有越好的加工性能，且电极各处的阻抗分布均匀，在充放电时活性物质的作用可以发挥得越大，其平均克容量发挥将会有所提升，从而提升全电池的性能。The performance of the electrode paste has an important influence on the performance of the lithium ion battery. The more uniform the components in the electrode slurry are dispersed, the better the processing performance of the pole piece, and the uniform distribution of the impedance of the electrode. The effect of the active substance can be exerted during charging and discharging, and the average gram capacity is exerted. Will be improved to improve the performance of the full battery.
实际应用上，传统的负极浆料制备方法是将导电剂用增稠剂溶液进行高转速的双行星式分散，然后加入负极活性物质，进行一定时间的搅拌后，再加入粘结剂经行短时间搅拌得到最终负极浆料。此种方法首先对导电剂的分散需要长时间处理，耗时长且分散状态并不理想，尤其是对于采用碳纳米管(CNT)、石墨烯等为导电剂的浆料制备；其次传统工艺需要在浆料制备过程中，对搅拌体系一直保持抽真空状态，造成浆料体系内部温度易升高，同时又在外部加循环水进行冷却，因此对设备的要求和磨损都很高。以上导致浆料制备效率低、稳定性差、效果不理想，对后续极片的制备、锂电池的性能都会造成影响。In practical application, the conventional negative electrode slurry preparation method is to carry out the high-speed double-planetary dispersion of the conductive agent with the thickener solution, and then add the negative electrode active material, stir for a certain period of time, and then add the binder to pass through the line. The time was stirred to obtain the final negative electrode slurry. This method firstly requires a long time treatment for the dispersion of the conductive agent, which takes a long time and is not ideal in the dispersion state, especially for the preparation of a slurry using a carbon nanotube (CNT), graphene or the like as a conductive agent; the second conventional process needs to be During the preparation of the slurry, the stirring system is kept under vacuum, which causes the internal temperature of the slurry system to rise easily, and at the same time, externally added circulating water for cooling, so the requirements and wear of the equipment are high. The above results in low slurry preparation efficiency, poor stability, and unsatisfactory effect, which will affect the preparation of the subsequent pole piece and the performance of the lithium battery.
发明内容Summary of the invention
为了克服现有技术中存在的问题，尤其对于粒径较小的钛酸锂负极材料，采用原始的合浆工艺，容易造成浆料产生颗粒，导电剂分散不均匀，浆料稳定性差，并最终影响到电池的一致性。本发明的目的是提供一种锂电池钛酸锂负极浆料的制备方法，以实现在较短时间内对浆料各组分均匀分散，其制备出的浆料均匀性好，稳定性优异，同时其制备的电池极片粘附力得到提高，并因此提高电池的一致性及其电池的电化学性能。In order to overcome the problems existing in the prior art, especially for the lithium titanate negative electrode material having a small particle size, the original mixing process is adopted, which is easy to cause particles to be generated in the slurry, the conductive agent is unevenly dispersed, the slurry stability is poor, and finally Affects the consistency of the battery. The object of the present invention is to provide a method for preparing a lithium battery lithium titanate negative electrode slurry, which can uniformly disperse the components of the slurry in a short time, and the prepared slurry has good uniformity and excellent stability. At the same time, the prepared battery sheet adhesion is improved, and thus the consistency of the battery and the electrochemical performance of the battery are improved.
为了实现上述发明目的，本发明采用如下所述的技术方案：In order to achieve the above object, the present invention adopts the technical solution as described below:
1、增稠剂溶液制备：将增稠剂羧甲基纤维素钠(CMC)按一定比例加入去离子水溶剂中，用搅拌机溶解均匀，取出备用，时间为60～100分钟；1. Preparation of thickener solution: Add the thickener sodium carboxymethylcellulose (CMC) to the deionized water solvent in a certain proportion, dissolve it evenly with a mixer, and take it out for 60-100 minutes;
2、分散粉体：将钛酸锂、导电剂按比例加入搅拌桶搅拌分散，时间为30～40分钟，并在时间1/2和结束时，刮搅拌桨和桶体上的粉体；2. Dispersing the powder: the lithium titanate and the conductive agent are added to the mixing tank in proportion and stirred for 30 to 40 minutes, and at the end of the time 1/2 and at the end, the powder on the paddle and the barrel is scraped;
3、高粘度搅拌：加入增稠剂溶液总量的55％～60％到上述搅拌后的粉体中，搅拌分散，时间为60～70分钟，并在时间1/3、2/3和结束时，刮搅拌桨和桶体上的浆料，浆料温度控制在25～35℃之间；3. High-viscosity stirring: adding 55% to 60% of the total amount of the thickener solution to the stirred powder, stirring and dispersing for 60 to 70 minutes, and at the time of 1/3, 2/3 and end When the slurry is scraped on the paddle and the barrel, the temperature of the slurry is controlled between 25 and 35 ° C;
4、低粘度搅拌：加入增稠剂溶液总量的35～30％到上述高粘度搅拌后的浆料中，搅拌分散，时间为60～70分钟，并在时间1/3、2/3和结束时，刮搅拌桨和桶体上的浆料，浆料温度控制
在25～35℃之间；4. Low-viscosity stirring: add 35 to 30% of the total amount of the thickener solution to the above-mentioned high-viscosity stirred slurry, stir and disperse for 60 to 70 minutes, and at time 1/3, 2/3 and At the end, scrape the slurry on the paddle and the barrel, and control the temperature of the slurry.
Between 25 and 35 ° C;
5、粘度测试：将上述步骤低粘度搅拌的浆料粘度进行粘度测试，如在正常范围2000～5000Mpa·S，直接进入下一步；如超过上述范围，则添加增稠剂溶液总量的5％～10％，再搅拌分散，时间为30～40分钟，并在时间1/2和结束时，刮搅拌桨和桶体上的浆料，再检测一次浆料粘度，达到粘度范围要求即可进入下一步；5. Viscosity test: the viscosity of the slurry with low viscosity stirring in the above steps is tested for viscosity, such as in the normal range of 2000-5000 Mpa·S, directly into the next step; if it exceeds the above range, 5% of the total amount of thickener solution is added. ~10%, stir and disperse for a period of 30 to 40 minutes, and at time 1/2 and at the end, scrape the slurry on the paddle and the barrel, and then test the viscosity of the slurry to reach the viscosity range. Next step;
6、粘结剂添加：加入粘结剂SBR，搅拌分散，时间为10～30分钟；6. Adding binder: adding binder SBR, stirring and dispersing, the time is 10 to 30 minutes;
7、真空消泡：在低速搅拌状态下，对桶体进行抽真空，真空度为-0.09～-0.1MPa，时间为15～30分钟，即得到本发明方法所制备的钛酸锂负极浆料。7. Vacuum defoaming: Under low-speed stirring state, the barrel is vacuumed, the degree of vacuum is -0.09~-0.1MPa, and the time is 15-30 minutes, that is, the lithium titanate negative electrode slurry prepared by the method of the invention is obtained. .
上述步骤2中钛酸锂为锐钛型二氧化钛或金红石型二氧化钛所制备的钛酸锂中的一种或两种的混合。In the above step 2, lithium titanate is a mixture of one or both of lithium titanate prepared from anatase type titanium dioxide or rutile type titanium dioxide.
上述步骤2中导电剂为导电炭黑、导电石墨、碳纳米管、碳纤维、石墨烯中的一种或多种混合物。The conductive agent in the above step 2 is one or a mixture of conductive carbon black, conductive graphite, carbon nanotubes, carbon fibers, and graphene.
上述步骤1、步骤2和步骤6中，钛酸锂、导电剂、增稠剂、粘结剂各组分的质量比依次为(90-97)：(1-4)：(1-5)：(1-3)，溶剂为上述各组分总量的80％～120％。In the above steps 1, 2 and 6, the mass ratio of each component of lithium titanate, conductive agent, thickener and binder is (90-97): (1-4): (1-5) : (1-3), the solvent is 80% to 120% of the total amount of each of the above components.
上述各步骤中，搅拌设备是双行星真空搅拌机，浆料温度是利用向行星搅拌桶通入相应温度的恒温循环水的方法来控制的。In the above steps, the agitation device is a dual planetary vacuum agitator, and the slurry temperature is controlled by a method of introducing a constant temperature circulating water to the planetary agitating barrel at a corresponding temperature.
由于采用上述技术方案，本发明具有以下优越性：Due to the adoption of the above technical solutions, the present invention has the following advantages:
1、制备时间短：本发明钛酸锂负极浆料制备时间全程约为265～380分钟，且在后续制备过程中，通过几次实际经验的积累，可省略粘度测试步骤，直接进入最后真空消泡过程，由此可节省30～40分钟，如有多台设备先制备好增稠剂溶液，又可节省60～100分钟，相比常规负极浆料制备工艺约7～9小时的时间，大大提高了生产效率；1. The preparation time is short: the preparation time of the lithium titanate negative electrode slurry of the invention is about 265 to 380 minutes, and in the subsequent preparation process, the accumulation of the actual experience can omit the viscosity test step and directly enter the final vacuum elimination. The bubble process can save 30 to 40 minutes. If there are multiple devices to prepare the thickener solution, it can save 60 to 100 minutes, compared with the conventional anode slurry preparation process for about 7 to 9 hours. Increased production efficiency;
2、设备磨损小：本发明只在最后真空消泡过程中才需要对桶体进行抽真空，相比传统工艺需要在浆料制备过程中，对搅拌体系一直保持抽真空状态，造成搅拌过程中热量难散发，浆料温度易升高的弊端，具有实质性改善效果，短时间抽真空处理降低设备负担，减小设备磨损；2, equipment wear is small: the invention only needs to vacuum the barrel in the final vacuum defoaming process, compared with the traditional process in the slurry preparation process, the stirring system has been kept vacuuming, resulting in the stirring process The heat is difficult to dissipate, the temperature of the slurry is easy to rise, and the effect is substantially improved. The short-time vacuum treatment reduces the burden on the equipment and reduces equipment wear;
3、生产能耗低：本发明所制得的钛酸锂负极浆料固含量约为45～55％，相比常规制备工艺，具有高固含量、低粘度的特点，因此使用的水的比例也相应减少，降低了后续涂布过程中对水分蒸发所需的能耗；3. Low production energy consumption: The lithium titanate negative electrode slurry prepared by the invention has a solid content of about 45 to 55%, and has a high solid content and a low viscosity compared with the conventional preparation process, so the proportion of water used is Correspondingly, the energy consumption required for evaporation of water during subsequent coating is reduced;
4、分散效果好：本发明先将负极活性物质、导电剂进行搅拌分散，避免了导电剂在浆料中产生团聚，前期采用高粘度搅拌分散，搅拌桨对浆料的机械作用力(挤压、碰撞、摩擦)大，能起到很好的分散效果，再采用低粘度搅拌，使各组分彻底被分散开。
4. Good dispersion effect: The invention firstly stirs and disperses the negative electrode active material and the conductive agent to avoid agglomeration of the conductive agent in the slurry, and adopts high-viscosity stirring and dispersion in the early stage, and the mechanical force of the stirring paddle on the slurry (extrusion) , collision, friction) large, can play a good dispersion effect, and then use low viscosity mixing, so that the components are completely dispersed.
采用本发明提供的锂电池钛酸锂负极浆料所制得的锂电池，内阻低，不易发热，而且能量密度高、循环性能好、使用寿命长。The lithium battery prepared by using the lithium battery lithium titanate negative electrode provided by the invention has low internal resistance, is not easy to generate heat, has high energy density, good cycle performance and long service life.
下面通过具体实施例，对本发明的技术方案作进一步的具体说明。The technical solution of the present invention will be further specifically described below through specific embodiments.
实施例1Example 1
以锐钛型二氧化钛所制备的钛酸锂为负极，SP为导电剂，按Li4Ti5O12：SP：CMC：SBR＝94.0：1.5：2.0：2.5的质量比，溶剂去离子水为上述各组分总量的100％。制备步骤如下：Lithium titanate prepared by anatase titanium dioxide is used as a negative electrode, SP is a conductive agent, and the mass ratio of Li 4 Ti 5 O 12 :SP:CMC:SBR=94.0:1.5:2.0:2.5, solvent deionized water is the above 100% of the total amount of each component. The preparation steps are as follows:
1、将增稠剂CMC加入去离子水溶剂中，用搅拌机溶解均匀，取出备用，时间为60分钟；1. Add the thickener CMC to the deionized water solvent, dissolve it evenly with a stirrer, and take it out for a period of 60 minutes;
2、将负极活性物质、导电剂加入搅拌桶搅拌分散，时间为30分钟，并在时间15分钟和30分钟时，刮搅拌桨和桶体上的粉体；2. The negative electrode active material and the conductive agent are added to the stirring tank to be stirred and dispersed for 30 minutes, and the powder on the paddle and the barrel is scraped at the time of 15 minutes and 30 minutes;
3、加入增稠剂溶液总量的55％到上述搅拌后的粉体中，搅拌分散，时间为60分钟，并在时间20分钟、40分钟和60分钟时，刮搅拌桨和桶体上的浆料，浆料温度控制在25～35℃之间；3. Add 55% of the total amount of the thickener solution to the stirred powder, stir and disperse for 60 minutes, and scrape the paddle and barrel on the time of 20 minutes, 40 minutes and 60 minutes. Slurry, the temperature of the slurry is controlled between 25 and 35 ° C;
4、加入增稠剂溶液总量的35％到上述高粘度搅拌后的浆料中，搅拌分散，时间为60分钟，并在时间20分钟、40分钟和60分钟时，刮搅拌桨和桶体上的浆料，浆料温度控制在25～35℃之间；4. Add 35% of the total amount of the thickener solution to the above high-viscosity stirred slurry, stir and disperse for 60 minutes, and scrape the paddle and barrel at times of 20 minutes, 40 minutes, and 60 minutes. On the slurry, the temperature of the slurry is controlled between 25 and 35 ° C;
5、将上述步骤低粘度搅拌的浆料粘度进行粘度测试，测试结果为5332Mpa·S，超正常范围值，添加溶剂总量的5％，再搅拌分散，时间为30分钟，并在时间15分钟和30分钟时，刮搅拌桨和桶体上的浆料，再检测一次浆料粘度，测试结果为4215Mpa·S，达到粘度范围要求；5. Perform the viscosity test on the viscosity of the slurry with low viscosity stirring in the above steps. The test result is 5332 Mpa·S, the value of the normal range is 5%, the total amount of the solvent is added, and the dispersion is stirred for 30 minutes, and the time is 15 minutes. And 30 minutes, scrape the slurry on the paddle and the barrel, and then test the viscosity of the slurry. The test result is 4215Mpa·S, which meets the viscosity range requirement;
6、加入粘结剂SBR，搅拌分散，时间为10分钟；6. Add the binder SBR, stir and disperse for 10 minutes;
7、在低速搅拌状态下，对桶体进行抽真空，真空度为-0.09～-0.1MPa，时间为15分钟，即得到本发明方法所制备的钛酸锂负极浆料，共耗时约265分钟。7. Under low-speed stirring state, the barrel is vacuumed, the degree of vacuum is -0.09~-0.1MPa, and the time is 15 minutes, that is, the lithium titanate negative electrode slurry prepared by the method of the invention is obtained, and the total consumption time is about 265. minute.
按照锂电池常规生产工艺，将钛酸锂负极浆料经涂布、干燥、轧膜、分切制成负极片，然后与磷酸铁锂正极片、隔膜、电解液、电池外壳进行组装成，经充放电活化后制得18650型、初始设计容量为1350mA的圆柱磷酸铁锂电池。According to the conventional production process of lithium battery, the lithium titanate negative electrode slurry is coated, dried, rolled, and cut into negative electrode sheets, and then assembled with lithium iron phosphate positive electrode sheets, separators, electrolytes, and battery casings. After the charge and discharge activation, a 18650 type cylindrical lithium iron phosphate battery with an initial design capacity of 1350 mA was obtained.
对比例1Comparative example 1
按照常规的负极浆料生产工艺，制备耗时约7个小时，按照锂电池常规生产工艺，制得18650型、初始设计容量为1350mA的圆柱磷酸铁锂电池。According to the conventional negative electrode slurry production process, the preparation takes about 7 hours, and according to the conventional production process of the lithium battery, a cylindrical lithium iron phosphate battery of 18650 type with an initial design capacity of 1350 mA is obtained.
对实施例1和对比例1所制得的18650型圆柱磷酸铁锂电池进行电学性能测试，其在1C下充放,1000次的循环容量保持率，实施例1为98.14％，对比例1为96.85％，能量密度及内阻测试对比结果如表1所示。
The electrical properties of the 18650-type cylindrical lithium iron phosphate battery prepared in Example 1 and Comparative Example 1 were tested and charged and discharged at 1 C, and the cycle capacity retention rate was 1000 times. Example 1 was 98.14%, and Comparative Example 1 was 96.85%, the energy density and internal resistance test comparison results are shown in Table 1.
实施例2Example 2
以金红石型二氧化钛所制备的钛酸锂为负极，SP为导电剂，按Li4Ti5O12：SP：CMC：SBR＝94.5：2.0：1.6：1.9的质量比，溶剂去离子水为上述各组分总量的80％。制备步骤如下：Lithium titanate prepared by rutile titanium dioxide is used as a negative electrode, SP is a conductive agent, and the mass ratio of Li 4 Ti 5 O 12 :SP:CMC:SBR=94.5:2.0:1.6:1.9, solvent deionized water is used as the above 80% of the total amount of the components. The preparation steps are as follows:
1、将增稠剂CMC加入去离子水溶剂中，用搅拌机溶解均匀，取出备用，时间为120分钟；1. Add the thickener CMC to the deionized water solvent, dissolve it evenly with a stirrer, and take it out for a period of 120 minutes;
2、将负极活性物质、导电剂加入搅拌桶搅拌分散，时间为40分钟，并在时间20分钟和40分钟时，刮搅拌桨和桶体上的粉体；2. The negative electrode active material and the conductive agent are added to the stirring tank to be stirred and dispersed for 40 minutes, and the powder on the paddle and the barrel is scraped at the time of 20 minutes and 40 minutes;
3、加入增稠剂溶液总量的60％到上述搅拌后的粉体中，搅拌分散，时间为70分钟，并在时间23分钟、46分钟和70分钟时，刮搅拌桨和桶体上的浆料，浆料温度控制在25～35℃之间；3. Add 60% of the total amount of the thickener solution to the stirred powder, stir and disperse for 70 minutes, and scrape the paddle and barrel on the time of 23 minutes, 46 minutes and 70 minutes. Slurry, the temperature of the slurry is controlled between 25 and 35 ° C;
4、加入增稠剂溶液总量的35％到上述高粘度搅拌后的浆料中，搅拌分散，时间为70分钟，并在时间23分钟、46分钟和70分钟时，刮搅拌桨和桶体上的浆料，浆料温度控制在25～35℃之间；4. Add 35% of the total amount of the thickener solution to the above high-viscosity stirred slurry, stir and disperse for 70 minutes, and scrape the paddle and barrel at 23 minutes, 46 minutes and 70 minutes. On the slurry, the temperature of the slurry is controlled between 25 and 35 ° C;
5、将上述步骤低粘度搅拌的浆料粘度进行粘度测试，测试结果为4578Mpa·S，属于正常范围值，达到要求；5. Perform the viscosity test on the viscosity of the slurry with low viscosity stirring in the above steps. The test result is 4578Mpa·S, which is a normal range value and meets the requirements;
6、加入粘结剂SBR，搅拌分散，时间为30分钟；6, adding binder SBR, stirring and dispersion, the time is 30 minutes;
7、在低速搅拌状态下，对桶体进行抽真空，真空度为-0.09～-0.1MPa，时间为30分钟，即得到本发明方法所制备的钛酸锂负极浆料，共耗时约360分钟。7. Under low-speed stirring state, the barrel is vacuumed, the degree of vacuum is -0.09~-0.1MPa, and the time is 30 minutes, that is, the lithium titanate negative electrode slurry prepared by the method of the invention is obtained, and the total consumption time is about 360. minute.
按照锂电池常规生产工艺，将钛酸锂负极浆料经涂布、干燥、轧膜、分切制成负极片，然后与钴酸锂正极片、隔膜、电解液、电池外壳进行组装成，经充放电活化后制得18650型、初始设计容量为1600mA的圆柱型电池。According to the conventional production process of lithium battery, the lithium titanate negative electrode slurry is coated, dried, rolled, and cut into negative electrode sheets, and then assembled with lithium cobaltate positive electrode sheets, separators, electrolytes, and battery casings. After the charge and discharge were activated, a 18650 type cylindrical battery with an initial design capacity of 1600 mA was obtained.
对比例2Comparative example 2
按照常规的负极浆料生产工艺，制备耗时约7.5个小时，按照锂电池常规生产工艺，制得18650型、初始设计容量为1600mA的圆柱型电池。According to the conventional negative electrode slurry production process, the preparation takes about 7.5 hours, and according to the conventional production process of the lithium battery, a cylindrical type battery of 18650 type and an initial design capacity of 1600 mA is obtained.
对实施例2和对比例2所制得的18650型圆柱电池进行电学性能测试，其在1C下充放,1000次的循环容量保持率，实施例2为97.23％，对比例2为93.23％，能量密度及内阻测试对比结果如表1所示。The electrical properties of the 18650-type cylindrical battery prepared in Example 2 and Comparative Example 2 were tested and charged and discharged at 1 C, and the cycle capacity retention rate was 1000 times, and Example 2 was 97.23%, and Comparative Example 2 was 93.23%. The energy density and internal resistance test comparison results are shown in Table 1.
表1.各实施例与对比例的能量密度及内阻测试对比结果
Table 1. Comparison of energy density and internal resistance test of each example and comparative example
| 项目project | 能量密度(Wh/kg)Energy density (Wh/kg) | 内阻(mΩ)Internal resistance (mΩ) |
| 实施例1Example 1 | 127.6127.6 | 46.846.8 |
| 对比例1Comparative example 1 | 118.4118.4 | 50.250.2 |
| 实施例2Example 2 | 154.7154.7 | 38.138.1 |
| 对比例2Comparative example 2 | 142.9142.9 | 40.340.3 |
从上表可以看出，采用本发明方法制备的钛酸锂负极浆料所制得的锂电池，在能量密度上均高于常规负极浆料生产工艺所制得的锂电池，在内阻上均低于常规负极浆料生产工艺所制得的锂电池。As can be seen from the above table, the lithium battery prepared by using the lithium titanate negative electrode slurry prepared by the method of the present invention has higher energy density than the lithium battery produced by the conventional negative electrode slurry production process, and has an internal resistance. Both are lower than the lithium battery produced by the conventional negative electrode slurry production process.
以上显示和描述了本发明的基本原理和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 and main features of the present invention and the advantages of the present invention are shown and described above, and those skilled in the art should understand that the present invention is not limited by the above embodiments, and that the above embodiments and descriptions are merely illustrative of the present invention. The present invention is subject to various modifications and improvements without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The requirements and their equivalents are defined.
Claims (5)
- 一种锂电池钛酸锂负极浆料的制备方法，其制备步骤如下：A preparation method of lithium battery lithium titanate negative electrode slurry, the preparation steps are as follows:(1)增稠剂溶液制备：将增稠剂羧甲基纤维素钠(CMC)按一定比例加入去离子水溶剂中，用搅拌机溶解均匀，取出备用，时间为60～100分钟；(1) preparation of thickener solution: the thickener sodium carboxymethyl cellulose (CMC) is added to the deionized water solvent in a certain proportion, dissolved uniformly by a stirrer, and taken out for use, the time is 60-100 minutes;(2)分散粉体：将钛酸锂、导电剂按比例加入搅拌桶搅拌分散，时间为30～40分钟，并在时间1/2和结束时，刮搅拌桨和桶体上的粉体；(2) dispersing powder: lithium titanate and conductive agent are added to the mixing tank in proportion and stirred for 30 to 40 minutes, and at time 1/2 and at the end, the powder on the paddle and the barrel is scraped;(3)高粘度搅拌：加入增稠剂溶液总量的55％～60％到上述搅拌后的粉体中，搅拌分散，时间为60～70分钟，并在时间1/3、2/3和结束时，刮搅拌桨和桶体上的浆料，浆料温度控制在25～35℃之间；(3) High-viscosity stirring: adding 55% to 60% of the total amount of the thickener solution to the stirred powder, stirring and dispersing for 60 to 70 minutes, and at times 1/3, 2/3 and At the end, the slurry on the paddle and the barrel is scraped, and the temperature of the slurry is controlled between 25 and 35 ° C;(4)低粘度搅拌：加入增稠剂溶液总量的35～30％到上述高粘度搅拌后的浆料中，搅拌分散，时间为60～70分钟，并在时间1/3、2/3和结束时，刮搅拌桨和桶体上的浆料，浆料温度控制在25～35℃之间；(4) Low-viscosity stirring: adding 35 to 30% of the total amount of the thickener solution to the above-mentioned high-viscosity stirred slurry, stirring and dispersing for 60 to 70 minutes, and at time 1/3, 2/3 And at the end, scraping the slurry on the paddle and the barrel, the temperature of the slurry is controlled between 25 and 35 ° C;(5)粘度测试：将上述步骤低粘度搅拌的浆料粘度进行粘度测试，如在正常范围2000～5000Mpa·S，直接进入下一步；如超过上述范围，则添加增稠剂溶液总量的5％～10％，再搅拌分散，时间为30～40分钟，并在时间1/2和结束时，刮搅拌桨和桶体上的浆料，再检测一次浆料粘度，达到粘度范围要求即可进入下一步；(5) Viscosity test: the viscosity of the slurry with low viscosity stirring in the above steps is tested for viscosity, such as in the normal range of 2000-5000 Mpa·S, directly into the next step; if the above range is exceeded, the total amount of the thickener solution is added 5 %～10%, stir and disperse for 30-40 minutes, and at time 1/2 and at the end, scrape the slurry on the paddle and barrel, and then test the viscosity of the slurry to reach the viscosity range. Go to the next step;(6)粘结剂添加：加入粘结剂SBR，搅拌分散，时间为10～30分钟；(6) binder addition: adding binder SBR, stirring and dispersing, the time is 10 to 30 minutes;(7)真空消泡：在低速搅拌状态下，对桶体进行抽真空，真空度为-0.09～-0.1MPa，时间为15～30分钟，即得到本发明方法所制备的钛酸锂负极浆料。(7) Vacuum defoaming: under low-speed stirring, the barrel is evacuated, the degree of vacuum is -0.09~-0.1MPa, and the time is 15-30 minutes, that is, the lithium titanate negative electrode slurry prepared by the method of the invention is obtained. material.
- 根据权利要求1所述的一种锂电池钛酸锂负极浆料的制备方法，其特征是，上述步骤(2)中钛酸锂为锐钛型二氧化钛或金红石型二氧化钛所制备的钛酸锂中的一种或两种的混合。The method for preparing a lithium battery lithium titanate negative electrode slurry according to claim 1, wherein in the step (2), the lithium titanate is lithium titanate prepared by anatase titanium dioxide or rutile titanium dioxide. One or a mixture of two.
- 根据权利要求1所述的一种锂电池钛酸锂负极浆料的制备方法，其特征是，上述步骤(2)中导电剂为导电炭黑、导电石墨、碳纳米管、碳纤维、石墨烯中的一种或多种混合物。The method for preparing a lithium battery lithium titanate negative electrode slurry according to claim 1, wherein the conductive agent in the step (2) is conductive carbon black, conductive graphite, carbon nanotubes, carbon fibers, and graphene. One or more mixtures.
- 根据权利要求1所述的一种锂电池钛酸锂负极浆料的制备方法，其特征是，上述步骤(1)、步骤(2)和步骤(6)中，钛酸锂、导电剂、增稠剂、粘结剂各组分的质量比依次为(90-97)：(1-4)：(1-5)：(1-3)，溶剂为上述各组分总量的80％～120％。The method for preparing a lithium battery lithium titanate negative electrode slurry according to claim 1, wherein in the above steps (1), (2) and (6), lithium titanate, a conductive agent, and an increase The mass ratio of the components of the thickener and the binder is (90-97): (1-4): (1-5): (1-3), and the solvent is 80% of the total amount of the above components. 120%.
- 根据权利要求1所述的一种锂电池钛酸锂负极浆料的制备方法，其特征是，上述各步骤中，搅拌设备是双行星真空搅拌机，浆料温度是利用向行星搅拌桶通入相应温度的恒温循环水的方法来控制的。 The method for preparing a lithium battery lithium titanate negative electrode slurry according to claim 1, wherein in the above steps, the stirring device is a double planetary vacuum agitator, and the slurry temperature is transferred to the planetary agitating barrel. The temperature is controlled by a constant temperature circulating water method.
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| CN108172756B (en) * | 2018-01-31 | 2020-07-14 | 北京国能电池科技股份有限公司 | Preparation method of negative electrode slurry |
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