WO2017032144A1 - 一种磷酸铁锂正极浆料的制备方法 - Google Patents

一种磷酸铁锂正极浆料的制备方法 Download PDF

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WO2017032144A1
WO2017032144A1 PCT/CN2016/085914 CN2016085914W WO2017032144A1 WO 2017032144 A1 WO2017032144 A1 WO 2017032144A1 CN 2016085914 W CN2016085914 W CN 2016085914W WO 2017032144 A1 WO2017032144 A1 WO 2017032144A1
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slurry
viscosity
iron phosphate
lithium iron
positive electrode
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田东
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田东
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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
    • H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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

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  • the patent relates to the field of lithium ion batteries, in particular to a preparation process and a method for a lithium iron phosphate cathode 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.
  • 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 a negative electrode film coated on the negative electrode current collector.
  • 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 positive electrode slurry preparation method is to carry out high-speed double planetary dispersion of a conductive agent with a binder solution, and then add a positive electrode active material, and stir for a certain period of time to obtain a final positive 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 iron phosphate positive electrode slurry for a lithium battery, so as to achieve uniform dispersion of 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.
  • Disperse powder Add lithium iron phosphate, conductive agent and binder to the mixing tank in proportion and stir for 30 to 40 minutes. At time 1/2 and at the end, scrape the paddle and the barrel. Powder
  • High-viscosity stirring adding 55% to 60% of the total amount of the solvent to the stirred powder, stirring and dispersing for 60 to 70 minutes, and scraping at time 1/3, 2/3 and at the end Stir the slurry on the paddle and the barrel, and the slurry temperature is controlled between 25 and 35 ° C;
  • Low-viscosity stirring adding 35 to 30% of the total amount of the solvent to the above-mentioned high-viscosity stirred slurry, stirring and dispersing for 60 to 70 minutes, and at the time of 1/3, 2/3 and at the end, Scrape the paddle and the slurry on the barrel, and the slurry temperature is controlled 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 5000-9000 Mpa ⁇ S, directly into the next vacuum defoaming; if it exceeds the above range, 5% of the total amount of solvent 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 5000-9000 Mpa ⁇ S, directly into the next vacuum defoaming; if it exceeds the above range, 5% of the total amount of solvent is added. ⁇ 10%, stir and disperse for a period of 30 to 40 minutes, and at time 1/2 and at the
  • Vacuum defoaming Under low-speed stirring, the barrel is evacuated, the degree of vacuum is -0.09 to -0.1 MPa, and the time is 15 to 30 minutes, that is, the positive electrode slurry prepared by the method of the invention is obtained.
  • the conductive agent in the above step 1 is one or a mixture of conductive carbon black, conductive graphite, carbon nanotubes, carbon fibers, and graphene.
  • the binder in the above step 1 is polyvinylidene fluoride (PVDF).
  • the solvent in the above step 2 is N-methylpyrrolidone (NMP).
  • the mass ratio of each component of the lithium iron phosphate, the conductive agent, and the binder is (90-97): (1-4): (1-5), and the solvent is the above components. 70% to 120% of the total weight.
  • the stirring device is a dual planetary vacuum mixer, and the slurry temperature is utilized to the planet.
  • the mixing drum is controlled by a method of introducing a constant temperature circulating water of a corresponding temperature.
  • the present invention has the following advantages:
  • the preparation time of the positive electrode slurry of the invention is about 195 to 250 minutes, and in the subsequent preparation process, the accumulation of several practical experiences can omit the viscosity test step and directly enter the final vacuum defoaming process. Thereby, it can save 30-40 minutes, and the production time is greatly improved compared with the preparation time of about 5-8 hours of the conventional preparation process;
  • 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 solid content of the positive electrode slurry prepared by the invention is about 45-60%, which has the characteristics of high solid content and low viscosity compared with the conventional preparation process, so the amount of solvent used is correspondingly reduced. Reduces the energy required to evaporate and recover the solvent during subsequent coating processes;
  • the invention firstly stirs and disperses lithium iron phosphate, conductive agent and binder to avoid agglomeration of conductive agent in the slurry.
  • high viscosity stirring and dispersion are used, and the mechanical effect of the stirring paddle on the slurry is adopted.
  • the force (extrusion, collision, friction) is large, and it can achieve a good dispersion effect, and then the low-viscosity agitation is used to completely disperse the components.
  • the lithium battery prepared by using the lithium iron phosphate positive electrode slurry of the lithium battery 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 barrel is evacuated, the degree of vacuum is -0.09 to -0.1 MPa, and the time is 30 minutes, that is, the positive electrode slurry prepared by the method of the invention is obtained, and the total consumption time is about 250 minutes.
  • the positive electrode slurry is coated, dried, rolled, and cut into positive electrode sheets, and then assembled with negative electrode sheets, separators, electrolytes, and battery casings, and then activated by charge and discharge.
  • Model 18650 cylindrical lithium iron phosphate battery with an initial design capacity of 1350 mA.
  • the preparation takes about 7 hours, and according to the conventional production process of the lithium battery, a 18650 type cylindrical lithium iron phosphate battery 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 97.92%, and Comparative Example 1 was The results of 95.23%, energy density and internal resistance test are shown in Table 1.
  • the barrel is evacuated, the degree of vacuum is -0.09 to -0.1 MPa, and the time is 15 minutes, that is, the positive electrode slurry prepared by the method of the invention is obtained, and the total consumption time is about 165 minutes.
  • the positive electrode slurry is coated, dried, rolled, and cut into positive electrode sheets, and then assembled with negative electrode sheets, separators, electrolytes, and battery casings, and then activated by charge and discharge.
  • Model 18650 cylindrical lithium iron phosphate battery with an initial design capacity of 1300 mA.
  • 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 1300 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 iron phosphate positive electrode slurry prepared by the method of the invention has higher energy density than the lithium battery produced by the conventional positive electrode slurry production process, and has an internal resistance. Both are lower than the lithium battery produced by the conventional positive electrode slurry production process.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

发明提供一种锂电池磷酸铁锂正极浆料的制备方法，通过分散粉体、高粘度搅拌、低粘度搅拌、粘度测试、真空消泡等步骤，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。本发明具有制备时间短、设备磨损小、生产能耗低、分散效果好等有点。采用本发明提供的锂电池磷酸铁锂正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。

Description

一种磷酸铁锂正极浆料的制备方法 技术领域
本专利涉及锂离子电池领域，具体为一种磷酸铁锂正极材料浆料的制备工艺及方法。
背景技术
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。
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。
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。
实际应用上，传统的正极浆料制备方法是将导电剂用粘结剂溶液进行高转速的双行星式分散，然后加入正极活性物质，进行一定时间的搅拌后得到最终正极浆料。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。
发明内容
为了克服现有技术中存在的问题，尤其对于纳米磷酸铁锂材料，采用原始的合浆工艺，容易造成浆料产生颗粒、果冻，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磷酸铁锂正极浆料的制备方法，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。
为了实现上述发明目的，本发明采用如下所述的技术方案：
1、分散粉体：将磷酸铁锂、导电剂、粘结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、高粘度搅拌：加入溶剂总量的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、低粘度搅拌：加入溶剂总量的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、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5000～9000Mpa·S，直接进入下一步真空消泡；如超过上述范围，则添加溶剂总量的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、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正极浆料。
上述步骤1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。
上述步骤1中粘结剂为聚偏氟乙烯(PVDF)。
上述步骤2中溶剂为N-甲基吡咯烷酮(NMP)。
上述步骤1和步骤2中，磷酸铁锂、导电剂、粘结剂各组分的质量比依次为(90-97)：(1-4)：(1-5)，溶剂为上述各组分总重量的70％～120％。
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。
由于采用上述技术方案，本发明具有以下优越性：
1、制备时间短：本发明正极浆料制备时间全程约为195～250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，由此又可节省30～40分钟，相比常规制备工艺约5～8小时的制备时间，大大提高了生产效率；
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；
3、生产能耗低：本发明所制得的正极浆料固含量约为45～60％，相比常规制备工艺，具有高固含量、低粘度的特点，因此使用的溶剂量也相应减少，降低了后续涂布过程中对溶剂蒸发和回收所需的能耗；
4、分散效果好：本发明先将磷酸铁锂、导电剂、粘结剂进行搅拌分散，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。
采用本发明提供的锂电池磷酸铁锂正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。
具体实施方式
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。
实施例1
以SP为导电剂，PVDF为粘结剂，按照LiFePO4：SP：PVDF＝95.7：2.3：2.0的质量比，溶剂NMP为上述各组分总量的100％。制备步骤如下：
1、将各组分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、加入NMP总量的55％到上述搅拌后的粉体中，搅拌分散，时间为70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、加入溶剂总量的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、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9514Mpa·S，超正常范围值，添加溶剂总量的5％，再搅拌分散，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浆料，再检测一次浆料粘度，测试结果为8627Mpa·S，达到粘度范围要求；
5、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正极浆料，共耗时约250分钟。
按照锂电池常规生产工艺，将正极浆料经涂布、干燥、轧膜、分切制成正极片，然后与负极片、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。
对比例1
按照常规的磷酸铁锂正极浆料生产工艺，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的圆柱型磷酸铁锂电池。
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97.92％，对比例1为95.23％，能量密度及内阻测试对比结果如表1所示。
实施例2
以SP和KS-6为导电剂，PVDF为粘结剂，按照LiFePO4：SP：KS-6：PVDF＝93：2.2：1.3：3.5的质量比，溶剂NMP为上述各组分总量的120％。制备步骤如下：
1、将各组分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、加入NMP总量的60％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、加入溶剂总量的30％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、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7149Mpa·S，属于正常范围值，达到要求；
5、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正极浆料，共耗时约165分钟。
按照锂电池常规生产工艺，将正极浆料经涂布、干燥、轧膜、分切制成正极片，然后与负极片、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1300mA的圆柱磷酸铁锂电池。
对比例2
按照常规的磷酸铁锂正极浆料生产工艺，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1300mA的圆柱型磷酸铁锂电池。
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。
表1.各实施例与对比例的能量密度及内阻测试对比结果
项目 能量密度(Wh/kg) 内阻(mΩ)
实施例1 127.6 46.8
对比例1 118.4 50.2
实施例2 119.5 44.3
对比例2 109.4 48.5
从上表可以看出，采用本发明方法制备的磷酸铁锂正极浆料所制得的锂电池，在能量密度上均高于常规正极浆料生产工艺所制得的锂电池，在内阻上均低于常规正极浆料生产工艺所制得的锂电池。
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。

Claims (6)

  1. 一种磷酸铁锂正极浆料的制备方法，其制备步骤如下：
    (1)分散粉体：将磷酸铁锂、导电剂、粘结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)高粘度搅拌：加入溶剂总量的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)低粘度搅拌：加入溶剂总量的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)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5000～9000Mpa·S，直接进入下一步真空消泡；如超过上述范围，则添加溶剂总量的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)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正极浆料。
  2. 根据权利要求1所述的一种磷酸铁锂正极浆料的制备方法，其特征是，上述步骤(1)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。
  3. 根据权利要求1所述的一种磷酸铁锂正极浆料的制备方法，其特征是，上述步骤(1)中粘结剂为聚偏氟乙烯。
  4. 根据权利要求1所述的一种磷酸铁锂正极浆料的制备方法，其特征是，上述步骤(2)中溶剂为N-甲基吡咯烷酮。
  5. 根据权利要求1所述的一种磷酸铁锂正极浆料的制备方法，其特征是，上述步骤(1)和步骤(2)中，磷酸铁锂、导电剂、粘结剂各组分的质量比依次为(90-97)：(1-4)：(1-5)，溶剂为上述各组分总重量的70％～120％。
  6. 根据权利要求1所述的一种磷酸铁锂正极浆料的制备方法，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。
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