CN108808001B - Multi-element composite conductive layer and preparation method thereof - Google Patents
Multi-element composite conductive layer and preparation method thereofDownload PDFInfo
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Abstract
Description
Translated fromChinese技术领域technical field
本发明属于锂离子电池材料技术领域，具体涉及一种多元复合导电层及其制备方法。The invention belongs to the technical field of lithium ion battery materials, and particularly relates to a multi-component composite conductive layer and a preparation method thereof.
背景技术Background technique
从锂离子电池工作原理可知，电池的充放电过程，需要锂离子和电子的共同参与，因此，锂离子电池的电极必须是离子和电子的混合体，电极反应也只能发生在电解液、导电剂、活性材料的界面处。在锂离子电池中，阴极活性物质多为过渡金属氧化物或者过渡金属磷酸盐，大多属于半导体或绝缘体，导电性很差，必须加入导电剂来改善导电性；阳极石墨材料的导电性稍好，但是在多次充放电过程中，石墨材料的膨胀和收缩，使得石墨颗粒之间的接触减少，间隙增大，有些甚至脱离集流体，成为死的活性材料，不再参与电极反应，所以也需要加入导电剂来保持在电池循环过程中的电极材料导电性的稳定。现有常用的导电剂有炭黑、导电石墨、碳纳米管和纳米碳纤维等。It can be seen from the working principle of lithium ion batteries that the charging and discharging process of the battery requires the participation of lithium ions and electrons. Therefore, the electrodes of lithium ion batteries must be a mixture of ions and electrons, and the electrode reaction can only occur in the electrolyte, conductive agent and active material interface. In lithium-ion batteries, the cathode active materials are mostly transition metal oxides or transition metal phosphates, which are mostly semiconductors or insulators, and have poor conductivity. Conductive agents must be added to improve the conductivity; the conductivity of anode graphite materials is slightly better. However, in the process of multiple charge and discharge, the expansion and contraction of the graphite material reduces the contact between the graphite particles, increases the gap, and some even separate from the current collector, becoming a dead active material and no longer participating in the electrode reaction, so it is also necessary to Conductive agents are added to keep the conductivity of the electrode material stable during battery cycling. Commonly used conductive agents include carbon black, conductive graphite, carbon nanotubes, and carbon nanofibers.
现有技术中，常见的导电剂的制备方法主要是通过纳米碳系列的导电剂固相混合而成，其导电颗粒之间是通过吸附作用粘附在一起，存在粘附力差，形成的导电网络差，影响导电剂的导电性能。同时导电剂添加到正极材料里面仅仅起到导电的作用。如申请号为“CN201110030938.4”的中国专利公开了一种通过液相法制备的碳纳米管、炭黑以及石墨烯组成的复合导电剂，由于碳纳米管、炭黑及石墨烯之间的粘附力和结合力差，未充分发挥三者之间的各自优势，仅仅是起到导电的作用而已。In the prior art, the common preparation method of conductive agent is mainly formed by solid-phase mixing of nano-carbon series conductive agents, and the conductive particles are adhered together by adsorption, and there is poor adhesion. The network is poor, which affects the conductivity of the conductive agent. At the same time, the conductive agent added to the positive electrode material only plays a conductive role. For example, the Chinese patent with the application number of "CN201110030938.4" discloses a composite conductive agent composed of carbon nanotubes, carbon black and graphene prepared by a liquid phase method. Adhesion and bonding force are poor, and the respective advantages of the three are not fully utilized, and they only play a role in conducting electricity.
发明内容SUMMARY OF THE INVENTION
针对现有技术中的问题，本发明的目的在于提供一种多元复合导电层，该多元复合导电层中的各组分协同配合达到更好的导电性能，同时，该多元复合导电层与正极活性材料形成的膜层具有优异的抗剥离性能。In view of the problems in the prior art, the purpose of the present invention is to provide a multi-component composite conductive layer, the components in the multi-component composite conductive layer cooperate to achieve better electrical conductivity, and at the same time, the multi-component composite conductive layer and the positive electrode are active. The film layer formed by the material has excellent anti-peeling properties.
为了实现上述目的，本发明采用以下技术方案予以实现：In order to achieve the above object, the present invention adopts the following technical solutions to realize:
一种多元复合导电层的制备方法，包括将石墨烯粉体、石墨粉和镍粉构成的复合导电材料与PVDF、极性溶剂NMP混合均匀后涂覆到正极集流体上，接着以甲烷作为辅助气体，采用超音速火焰喷涂的方式将铝粉喷涂到正极集流体表面的涂层上，得到所述的多元复合导电层。A preparation method of a multi-component composite conductive layer, comprising the steps of uniformly mixing a composite conductive material composed of graphene powder, graphite powder and nickel powder with PVDF and polar solvent NMP, and then coating it on a positive electrode current collector, and then using methane as an auxiliary gas, and the aluminum powder is sprayed onto the coating on the surface of the positive electrode current collector by means of supersonic flame spraying to obtain the multi-component composite conductive layer.
优选的，所述的多元复合导电层包括以下重量份数的原料：PVDF 5～10份、NMP 40～55份、石墨烯粉体0.5～3份、石墨粉0.5～2份、镍粉0.1～0.5份。Preferably, the multi-component composite conductive layer includes the following raw materials in parts by weight: 5-10 parts of PVDF, 40-55 parts of NMP, 0.5-3 parts of graphene powder, 0.5-2 parts of graphite powder, and 0.1-2 parts of nickel powder. 0.5 servings.
优选的，所述的石墨粉为天然鳞片石墨、膨胀石墨、高取向石墨中的至少一种。Preferably, the graphite powder is at least one of natural flake graphite, expanded graphite, and highly oriented graphite.
优选的，所述的正极集流体为铝箔，所述铝箔的厚度为10～20μm。Preferably, the positive electrode current collector is an aluminum foil, and the thickness of the aluminum foil is 10-20 μm.
优选的，所述超音速火焰喷涂的喷涂参数为，采用氧气作为助燃气，氢气作为燃气，氮气作为送粉气体；Preferably, the spraying parameters of the supersonic flame spraying are that oxygen is used as auxiliary gas, hydrogen is used as fuel gas, and nitrogen is used as powder feeding gas;
所述氧气的压力为15～25bar，流量为400～900slpm，氢气的压力为6～8bar，流量为30～50slpm，辅助气体甲烷的压力为1～3bar，流量为5～10slpm，氮气的压力为4～8bar，流量为12～24slpm，送粉速度为10～50g/min，喷涂距离为200～300mm。The pressure of the oxygen is 15-25 bar, the flow is 400-900 slpm, the pressure of the hydrogen is 6-8 bar, the flow is 30-50 slpm, the pressure of the auxiliary gas methane is 1-3 bar, the flow is 5-10 slpm, and the pressure of the nitrogen is 4~8bar, flow rate is 12~24slpm, powder feeding speed is 10~50g/min, spraying distance is 200~300mm.
本发明还提供了一种采用上述制备方法制备得到的多元复合导电层。The present invention also provides a multi-component composite conductive layer prepared by the above-mentioned preparation method.
与现有技术相比，本发明具有以下技术效果：Compared with the prior art, the present invention has the following technical effects:
本发明提供的多元复合导电层，通过具有优异导电性能的石墨烯粉体和石墨粉掺和在一起并涂覆形成所述的导电层，并以甲烷作为辅助气体，采用超音速火焰喷涂的方式将铝粉喷涂到正极集流体表面的涂层上，该铝粉喷涂在正极集流体表面的涂层后形成蚀刻在涂层上的氧化物，具有一定的导电能力；The multi-component composite conductive layer provided by the present invention is formed by mixing graphene powder and graphite powder with excellent conductive properties and coating to form the conductive layer, and using methane as an auxiliary gas, the method of supersonic flame spraying is adopted The aluminum powder is sprayed on the coating on the surface of the positive electrode current collector, and the aluminum powder is sprayed on the coating on the surface of the positive electrode current collector to form an oxide etched on the coating, which has a certain conductivity;
其次，超音速火焰中夹杂着的甲烷气体在涂层中镍粉的催化作用下生成碳纳米管，该碳纳米管本身具有较高的强度，并且，由于碳纳米管的结构与石墨的片层结构相同，所以具有很好的电学性能，进一步的，该超音速火焰喷涂后在正极集流体涂层的表面形成碳纳米管，与深层的石墨烯粉体和石墨粉所形成的导电结构形成多层次，多元复合的导电形式，从而极大的提高了该多元复合导电层的导电性。Secondly, the methane gas mixed in the supersonic flame generates carbon nanotubes under the catalysis of nickel powder in the coating. The carbon nanotubes themselves have high strength, and due to the structure of carbon nanotubes and graphite sheets The structure is the same, so it has good electrical properties. Further, after the supersonic flame spraying, carbon nanotubes are formed on the surface of the positive electrode current collector coating, which forms more conductive structures with the deep graphene powder and graphite powder. It is a multi-layered and multi-composite conductive form, thereby greatly improving the conductivity of the multi-component composite conductive layer.
本发明的其他特征和优点将在随后的具体实施方式中予以详细说明。Other features and advantages of the present invention will be described in detail in the detailed description which follows.
具体实施方式Detailed ways
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，下面结合具体实施例，进一步阐明本发明。In order to make the technical means, creation features, achievement goals and effects of the present invention easy to understand and understand, the present invention will be further explained below with reference to specific embodiments.
本发明提供了一种多元复合导电层的制备方法，包括将石墨烯粉体、石墨粉和镍粉构成的复合导电材料与PVDF、极性溶剂NMP混合均匀后涂覆到正极集流体上，接着以甲烷作为辅助气体，采用超音速火焰喷涂的方式将铝粉喷涂到正极集流体表面的涂层上，得到所述的多元复合导电层。The invention provides a preparation method of a multi-component composite conductive layer, which comprises the steps of uniformly mixing a composite conductive material composed of graphene powder, graphite powder and nickel powder with PVDF and polar solvent NMP, and then coating it on a positive electrode current collector, and then Using methane as an auxiliary gas, the aluminum powder is sprayed on the coating on the surface of the positive electrode current collector by means of supersonic flame spraying to obtain the multi-component composite conductive layer.
本发明中，所述的石墨烯粉体是一种碳原子构成的单层二维平面结构材料，具有良好的透光性能、导电性能、导热性能和力学性能；石墨烯的电阻率仅有10-6Ω·cm，比铜或银更低，是目前电阻率最小的材料；此外，石墨烯也是目前最薄却最坚硬的材料，因此，将石墨烯粉体作为构成锂离子电池导电剂的构成成分是绝佳的选择，本发明中所述的石墨烯粉体购自贵州鼎玺烯材高科技有限公司生产的石墨烯粉料；In the present invention, the graphene powder is a single-layer two-dimensional planar structure material composed of carbon atoms, which has good light transmittance, electrical conductivity, thermal conductivity and mechanical properties; the resistivity of graphene is only 10-6 Ω·cm, which is lower than copper or silver, and is currently the material with the smallest resistivity; in addition, graphene is also the thinnest but hardest material at present, so graphene powder is used as a conductive agent for lithium-ion batteries. The composition is an excellent choice, and the graphene powder described in the present invention is purchased from the graphene powder produced by Guizhou Dingxiene Materials High-Tech Co., Ltd.;
所述的石墨粉是很好的非金属导电物质之一，并且，石墨粉还具有耐高温、高强度的优点，即便是经历超高温电弧灼烧，石墨粉的重量损失也可以忽略不计，且其热膨胀系数也很小；石墨粉还具有润滑的特性，本发明中所述的石墨粉购自成安县祥瑞碳素有限公司；The graphite powder is one of the good non-metallic conductive substances, and the graphite powder also has the advantages of high temperature resistance and high strength. Even if it undergoes ultra-high temperature arc burning, the weight loss of the graphite powder can be ignored, and Its thermal expansion coefficient is also very small; the graphite powder also has lubricating properties, and the graphite powder described in the present invention is purchased from Chengan County Xiangrui Carbon Co., Ltd.;
本发明通过将具有优异导电性能的石墨烯粉体和石墨粉掺和在一起并涂覆在正极集流体的正反面，形成涂层，接着以甲烷作为辅助气体，采用超音速火焰喷涂的方式将铝粉喷涂到正极集流体表面的涂层上，该铝粉喷涂在正极集流体表面的涂层后形成蚀刻在涂层上的氧化物，具有一定的导电能力；其次，超音速火焰中夹杂着的甲烷气体在涂层中镍粉的催化作用下生成碳纳米管，该碳纳米管本身具有较高的强度，并且，由于碳纳米管的结构与石墨的片层结构相同，所以具有很好的电学性能，进一步的，该超音速火焰喷涂后在正极集流体涂层的表面形成碳纳米管，与深层的石墨烯粉体和石墨粉所形成的导电结构形成多层次，多元复合的导电形式，从而极大的提高了该导电层的导电性。In the present invention, graphene powder and graphite powder with excellent electrical conductivity are mixed together and coated on the front and back sides of the positive electrode current collector to form a coating, and then methane is used as an auxiliary gas, and supersonic flame spraying is used to spray The aluminum powder is sprayed on the coating on the surface of the positive electrode current collector, and the aluminum powder is sprayed on the coating on the surface of the positive electrode current collector to form an oxide etched on the coating, which has a certain conductivity; secondly, the supersonic flame is mixed with The methane gas in the coating generates carbon nanotubes under the catalysis of nickel powder. The carbon nanotubes themselves have high strength, and because the structure of carbon nanotubes is the same as that of graphite, it has good Electrical properties, further, after the supersonic flame spraying, carbon nanotubes are formed on the surface of the positive electrode current collector coating, and the conductive structure formed by the deep graphene powder and graphite powder forms a multi-level, multi-composite conductive form, Thus, the conductivity of the conductive layer is greatly improved.
根据本发明，本发明中所述多元复合导电层中各原料的组成可以在较宽的范围内选择，为了确保所述的复合导电层具有优异的导电性和良好的加工性，所述的多元复合导电层包括以下重量份数的原料：PVDF 5～10份、NMP 40～55份、石墨烯粉体0.5～3份、石墨粉0.5～2份、镍粉0.1～0.5份。According to the present invention, the composition of each raw material in the multi-component composite conductive layer in the present invention can be selected within a wide range. In order to ensure that the composite conductive layer has excellent conductivity and good processability, the multi-component composite conductive layer The composite conductive layer includes the following raw materials by weight: 5-10 parts of PVDF, 40-55 parts of NMP, 0.5-3 parts of graphene powder, 0.5-2 parts of graphite powder, and 0.1-0.5 part of nickel powder.
本发明中，所述的石墨粉为天然鳞片石墨、膨胀石墨、高取向石墨中的至少一种。In the present invention, the graphite powder is at least one of natural flake graphite, expanded graphite, and highly oriented graphite.
本发明中，所述的正极集流体为铝箔，所述铝箔的厚度为10～20μm。In the present invention, the positive electrode current collector is an aluminum foil, and the thickness of the aluminum foil is 10-20 μm.
本发明中，所述超音速火焰喷涂的喷涂参数为，采用氧气作为助燃气，氢气作为燃气，氮气作为送粉气体；In the present invention, the spraying parameters of the supersonic flame spraying are as follows: oxygen is used as auxiliary gas, hydrogen is used as fuel gas, and nitrogen is used as powder feeding gas;
所述氧气的压力为15～25bar，流量为400～900slpm，氢气的压力为6～8bar，流量为30～50slpm，辅助气体甲烷的压力为1～3bar，流量为5～10slpm，氮气的压力为4～8bar，流量为12～24slpm，送粉速度为10～50g/min，喷涂距离为200～300mm。The pressure of the oxygen is 15-25 bar, the flow is 400-900 slpm, the pressure of the hydrogen is 6-8 bar, the flow is 30-50 slpm, the pressure of the auxiliary gas methane is 1-3 bar, the flow is 5-10 slpm, and the pressure of the nitrogen is 4~8bar, flow rate is 12~24slpm, powder feeding speed is 10~50g/min, spraying distance is 200~300mm.
本发明还提供了一种包括上述多元复合导电层的锂离子电池正极极片，包括上述多元复合导电层的锂离子电池正极极片，极大的提高了正极极片的导电性能。The present invention also provides a lithium ion battery positive pole piece comprising the above-mentioned multi-component composite conductive layer, and a lithium ion battery positive pole piece including the above-mentioned multi-component composite conductive layer, which greatly improves the conductivity of the positive pole piece.
本发明提供的锂离子电池的正极极片，包括正极集流体以及位于该正极集流体正反两面的正极材料涂层；The positive electrode plate of the lithium ion battery provided by the present invention includes a positive electrode current collector and a positive electrode material coating on the positive and negative sides of the positive electrode current collector;
所述的正极材料涂层包括正极活性物质、多元复合导电剂、正极粘合剂以及溶剂。The positive electrode material coating includes a positive electrode active material, a multi-component composite conductive agent, a positive electrode binder and a solvent.
所述的正极活性物质选自NCM523/LMFP、NCM622/LMFP、NCM523、NCM622以及NCM111中的一种或两种以上的混合物。The positive active material is selected from one or more mixtures of NCM523/LMFP, NCM622/LMFP, NCM523, NCM622 and NCM111.
所述锂离子电池的正极极片的制备方法为：The preparation method of the positive pole piece of the lithium ion battery is:
(1)在合浆缸中依次加入PVDF和极性溶剂NMP，保持合浆缸为真空状态，打胶40～60min，然后加入石墨烯粉体、石墨粉和镍粉；继续打胶1～2h，得到混合液；(1) Add PVDF and polar solvent NMP in sequence to the mixing tank, keep the mixing tank in a vacuum state, and glue for 40-60 minutes, then add graphene powder, graphite powder and nickel powder; continue to glue for 1-2 hours , get the mixture;
(2)将正极活性物质加入到上述混合液中搅拌混合，然后加入极性溶剂NMP调节浆料粘度至6000～8000mPa·s，该过程中保持合浆缸为真空状态；(2) adding the positive active material to the above-mentioned mixed solution, stirring and mixing, then adding the polar solvent NMP to adjust the viscosity of the slurry to 6000-8000 mPa·s, and keeping the mixing cylinder in a vacuum state during this process;
(3)将上述浆料低速匀浆，然后均匀涂布在正极集流体的正反两面，在100～120℃的温度下烘烤10～15s后，以甲烷作为辅助气体，采用超音速火焰喷涂的方式将铝粉喷涂到正极集流体表面的涂层上，得到正极极片。(3) Homogenize the above-mentioned slurry at a low speed, then evenly coat it on both sides of the positive electrode current collector, bake it at a temperature of 100-120 ° C for 10-15 s, use methane as an auxiliary gas, and use supersonic flame spraying The aluminum powder is sprayed onto the coating on the surface of the positive electrode current collector by the method to obtain the positive electrode piece.
本发明提供的锂离子电池正极极片的制备方法中，规避了传统技术中采用辊压的方式对涂布完成的集流体进行压实作业，而是采用高速气流对集流体表面初步烘干的涂层进行气压，同样达到了压实的目的；避免了辊压时候出现的皱边、断带、粘辊的问题。In the preparation method of the positive electrode plate of lithium ion battery provided by the present invention, the compaction operation of the coated current collector by means of roller pressing in the traditional technology is avoided, but the surface of the current collector is preliminarily dried by high-speed airflow. The coating is subjected to air pressure, which also achieves the purpose of compaction; it avoids the problems of wrinkling, tape breakage and roller sticking during rolling.
以下通过具体的实施例对本发明提供的多元复合导电层做进一步的说明。The multi-component composite conductive layer provided by the present invention will be further described below through specific examples.
实施例1Example 1
一种锂离子电池正极极片，包括正极集流体以及位于该正极集流体正反两面的正极材料涂层；A positive electrode plate of a lithium ion battery, comprising a positive electrode current collector and a positive electrode material coating on the positive and negative sides of the positive electrode current collector;
所述的正极集流体是厚度为20μm的铝箔；The positive electrode current collector is an aluminum foil with a thickness of 20 μm;
所述的正极材料涂层包括正极活性物质、多元复合导电剂、正极粘合剂以及溶剂；The positive electrode material coating comprises a positive electrode active material, a multi-component composite conductive agent, a positive electrode binder and a solvent;
所述正极活性物质为NCM523/LMFP复合正极材料；The positive electrode active material is NCM523/LMFP composite positive electrode material;
所述锂离子电池正极极片的制备方法包括下述步骤：The preparation method of the lithium ion battery positive pole piece comprises the following steps:
(1)在合浆缸中依次加入12份PVDF和45份极性溶剂NMP，保持合浆缸为真空状态，打胶50min，然后加入3份石墨烯粉体、1份石墨粉和0.3份镍粉；继续打胶2h，得到混合液；(1) Add 12 parts of PVDF and 45 parts of polar solvent NMP into the mixing cylinder in turn, keep the mixing cylinder in a vacuum state, and glue for 50 minutes, then add 3 parts of graphene powder, 1 part of graphite powder and 0.3 part of nickel powder; continue to be glued for 2h to obtain a mixed solution;
(2)将上述混合液2.5倍重量的正极活性物质加入到上述混合液中搅拌混合，然后加入极性溶剂NMP调节浆料粘度至7000mPa·s，该过程中保持合浆缸为真空状态；(2) the positive active material of above-mentioned mixed solution 2.5 times of weight is added in above-mentioned mixed solution and stirred and mixed, then add polar solvent NMP to adjust slurry viscosity to 7000mPa s, keep mixing cylinder in vacuum state in this process;
(3)将上述浆料低速匀浆，然后均匀涂布在正极集流体的正反两面，在110℃的温度下烘烤15s后，以甲烷作为辅助气体，采用超音速火焰喷涂的方式将铝粉喷涂到正极集流体表面的涂层上，得到正极极片；(3) Homogenize the above slurry at a low speed, and then evenly coat it on both sides of the positive electrode current collector. After baking at a temperature of 110 ° C for 15 s, use methane as an auxiliary gas, and use supersonic flame spraying to spray aluminum. The powder is sprayed on the coating on the surface of the positive electrode current collector to obtain a positive electrode sheet;
所述超音速火焰喷涂的喷涂参数为，采用氧气作为助燃气，氢气作为燃气，氮气作为送粉气体；The spraying parameters of the supersonic flame spraying are that oxygen is used as auxiliary gas, hydrogen is used as fuel gas, and nitrogen is used as powder feeding gas;
所述氧气的压力为20bar，流量为600slpm，氢气的压力为7bar，流量为40slpm，辅助气体甲烷的压力为2bar，流量为8slpm，氮气的压力为6bar，流量为15slpm，送粉速度为30g/min，喷涂距离为250mm。The pressure of the oxygen is 20bar, the flow is 600slpm, the pressure of hydrogen is 7bar, the flow is 40slpm, the pressure of the auxiliary gas methane is 2bar, the flow is 8slpm, the pressure of nitrogen is 6bar, the flow is 15slpm, and the powder feeding speed is 30g/ min, the spraying distance is 250mm.
实施例2Example 2
一种锂离子电池正极极片，包括正极集流体以及位于该正极集流体正反两面的正极材料涂层；A positive electrode plate of a lithium ion battery, comprising a positive electrode current collector and a positive electrode material coating on the positive and negative sides of the positive electrode current collector;
所述的正极集流体是厚度为20μm的铝箔；The positive electrode current collector is an aluminum foil with a thickness of 20 μm;
所述的正极材料涂层包括正极活性物质、多元复合导电剂、正极粘合剂以及溶剂；The positive electrode material coating comprises a positive electrode active material, a multi-component composite conductive agent, a positive electrode binder and a solvent;
所述正极活性物质为NCM523/LMFP复合正极材料；The positive electrode active material is NCM523/LMFP composite positive electrode material;
所述锂离子电池正极极片的制备方法包括下述步骤：The preparation method of the lithium ion battery positive pole piece comprises the following steps:
(1)在合浆缸中依次加入10份PVDF和40份极性溶剂NMP，保持合浆缸为真空状态，打胶40min，然后加入1份石墨烯粉体、0.5份石墨粉和0.1份镍粉；继续打胶1h，得到混合液；(1) Add 10 parts of PVDF and 40 parts of polar solvent NMP in sequence to the mixing tank, keep the mixing tank in a vacuum state, and glue for 40 minutes, then add 1 part of graphene powder, 0.5 part of graphite powder and 0.1 part of nickel powder; continue to glue for 1h to obtain a mixed solution;
(2)将上述混合液2倍重量的正极活性物质加入到上述混合液中搅拌混合，然后加入极性溶剂NMP调节浆料粘度至6000mPa·s，该过程中保持合浆缸为真空状态；(2) the positive active material of above-mentioned mixed solution 2 times of weight is added in above-mentioned mixed solution and stirred and mixed, then add polar solvent NMP to adjust slurry viscosity to 6000mPa s, keep mixing cylinder in vacuum state in this process;
(3)将上述浆料低速匀浆，然后均匀涂布在正极集流体的正反两面，在100℃的温度下烘烤15s后，以甲烷作为辅助气体，采用超音速火焰喷涂的方式将铝粉喷涂到正极集流体表面的涂层上，得到正极极片；(3) Homogenize the above slurry at a low speed, and then evenly coat it on both sides of the positive electrode current collector. After baking at a temperature of 100 ° C for 15 s, use methane as an auxiliary gas, and use supersonic flame spraying to spray aluminum. The powder is sprayed on the coating on the surface of the positive electrode current collector to obtain a positive electrode sheet;
所述超音速火焰喷涂的喷涂参数为，采用氧气作为助燃气，氢气作为燃气，氮气作为送粉气体；The spraying parameters of the supersonic flame spraying are that oxygen is used as auxiliary gas, hydrogen is used as fuel gas, and nitrogen is used as powder feeding gas;
所述氧气的压力为20bar，流量为600slpm，氢气的压力为7bar，流量为40slpm，辅助气体甲烷的压力为2bar，流量为8slpm，氮气的压力为6bar，流量为15slpm，送粉速度为30g/min，喷涂距离为250mm。The pressure of the oxygen is 20bar, the flow is 600slpm, the pressure of hydrogen is 7bar, the flow is 40slpm, the pressure of the auxiliary gas methane is 2bar, the flow is 8slpm, the pressure of nitrogen is 6bar, the flow is 15slpm, and the powder feeding speed is 30g/ min, the spraying distance is 250mm.
实施例3Example 3
一种锂离子电池正极极片，包括正极集流体以及位于该正极集流体正反两面的正极材料涂层；A positive electrode plate of a lithium ion battery, comprising a positive electrode current collector and a positive electrode material coating on the positive and negative sides of the positive electrode current collector;
所述的正极集流体是厚度为20μm的铝箔；The positive electrode current collector is an aluminum foil with a thickness of 20 μm;
所述的正极材料涂层包括正极活性物质、多元复合导电剂、正极粘合剂以及溶剂；The positive electrode material coating comprises a positive electrode active material, a multi-component composite conductive agent, a positive electrode binder and a solvent;
所述正极活性物质为NCM523/LMFP复合正极材料；The positive electrode active material is NCM523/LMFP composite positive electrode material;
所述锂离子电池正极极片的制备方法包括下述步骤：The preparation method of the lithium ion battery positive pole piece comprises the following steps:
(1)在合浆缸中依次加入15份PVDF和55份极性溶剂NMP，保持合浆缸为真空状态，打胶50min，然后加入5份石墨烯粉体、2份石墨粉和0.5份镍粉；继续打胶2h，得到混合液；(1) Add 15 parts of PVDF and 55 parts of polar solvent NMP into the mixing cylinder in turn, keep the mixing cylinder in a vacuum state, and glue for 50 minutes, then add 5 parts of graphene powder, 2 parts of graphite powder and 0.5 parts of nickel powder; continue to be glued for 2h to obtain a mixed solution;
(2)将上述混合液3.5倍重量的正极活性物质加入到上述混合液中搅拌混合，然后加入极性溶剂NMP调节浆料粘度至8000mPa·s，该过程中保持合浆缸为真空状态；(2) the positive active material of above-mentioned mixed solution 3.5 times of weight is added in above-mentioned mixed solution and stirred and mixed, then add polar solvent NMP to adjust slurry viscosity to 8000mPa·s, keep mixing cylinder in vacuum state in this process;
(3)将上述浆料低速匀浆，然后均匀涂布在正极集流体的正反两面，在120℃的温度下烘烤10s后，以甲烷作为辅助气体，采用超音速火焰喷涂的方式将铝粉喷涂到正极集流体表面的涂层上，得到正极极片；(3) Homogenize the above slurry at a low speed, and then evenly coat it on both sides of the positive electrode current collector. After baking at a temperature of 120°C for 10 s, use methane as an auxiliary gas to spray aluminum with supersonic flame. The powder is sprayed on the coating on the surface of the positive electrode current collector to obtain a positive electrode sheet;
所述超音速火焰喷涂的喷涂参数为，采用氧气作为助燃气，氢气作为燃气，氮气作为送粉气体；The spraying parameters of the supersonic flame spraying are that oxygen is used as auxiliary gas, hydrogen is used as fuel gas, and nitrogen is used as powder feeding gas;
所述氧气的压力为20bar，流量为600slpm，氢气的压力为7bar，流量为40slpm，辅助气体甲烷的压力为2bar，流量为8slpm，氮气的压力为6bar，流量为15slpm，送粉速度为30g/min，喷涂距离为250mm。The pressure of the oxygen is 20bar, the flow is 600slpm, the pressure of hydrogen is 7bar, the flow is 40slpm, the pressure of the auxiliary gas methane is 2bar, the flow is 8slpm, the pressure of nitrogen is 6bar, the flow is 15slpm, and the powder feeding speed is 30g/ min, the spraying distance is 250mm.
实施例4Example 4
本实施例与实施例1的锂离子电池正极极片及其制备方法基本相同，不同的是，采用的正极活性物质为NCM622/LMFP复合材料。This embodiment is basically the same as the positive electrode plate of the lithium ion battery and the preparation method thereof in Example 1, the difference is that the positive electrode active material used is NCM622/LMFP composite material.
实施例5Example 5
本实施例与实施例1的锂离子电池正极极片及其制备方法基本相同，不同的是，采用的正极活性物质为NCM523。This embodiment is basically the same as the positive electrode plate of the lithium ion battery and the preparation method thereof in Embodiment 1, the difference is that the positive electrode active material used is NCM523.
实施例6Example 6
本实施例与实施例1的锂离子电池正极极片及其制备方法基本相同，不同的是，采用的正极活性物质为NCM622。This embodiment is basically the same as the positive electrode plate of the lithium ion battery and the preparation method thereof in Embodiment 1, the difference is that the positive electrode active material used is NCM622.
实施例7Example 7
本实施例与实施例1的锂离子电池正极极片及其制备方法基本相同，不同的是，采用的正极活性物质为NCM111。This embodiment is basically the same as the positive electrode plate of the lithium ion battery and the preparation method thereof in Embodiment 1, the difference is that the positive electrode active material used is NCM111.
对比例1Comparative Example 1
本实施例与实施例1的锂离子电池正极极片及其制备方法基本相同，不同的是，在所述的制备方法的步骤(1)中，不添加镍粉，其余不变。具体的：This embodiment is basically the same as the lithium ion battery positive electrode piece and the preparation method thereof in Embodiment 1. The difference is that in step (1) of the preparation method, no nickel powder is added, and the rest remain unchanged. specific:
所述锂离子电池正极极片的制备方法包括下述步骤：The preparation method of the lithium ion battery positive pole piece comprises the following steps:
(1)在合浆缸中依次加入12份PVDF和45份极性溶剂NMP，保持合浆缸为真空状态，打胶50min，然后加入3份石墨烯粉体和1份石墨粉；继续打胶2h，得到混合液；(1) Add 12 parts of PVDF and 45 parts of polar solvent NMP in sequence to the mixing tank, keep the mixing tank in a vacuum state, and glue for 50 minutes, then add 3 parts of graphene powder and 1 part of graphite powder; continue to glue 2h to obtain a mixed solution;
(2)将上述混合液2.5倍重量的正极活性物质加入到上述混合液中搅拌混合，然后加入极性溶剂NMP调节浆料粘度至7000mPa·s，该过程中保持合浆缸为真空状态；(2) the positive active material of above-mentioned mixed solution 2.5 times of weight is added in above-mentioned mixed solution and stirred and mixed, then add polar solvent NMP to adjust slurry viscosity to 7000mPa s, keep mixing cylinder in vacuum state in this process;
(3)将上述浆料低速匀浆，然后均匀涂布在正极集流体的正反两面，在110℃的温度下烘烤15s后，以甲烷作为辅助气体，采用超音速火焰喷涂的方式将铝粉喷涂到正极集流体表面的涂层上，得到正极极片；(3) Homogenize the above slurry at a low speed, and then evenly coat it on both sides of the positive electrode current collector. After baking at a temperature of 110 ° C for 15 s, use methane as an auxiliary gas, and use supersonic flame spraying to spray aluminum. The powder is sprayed on the coating on the surface of the positive electrode current collector to obtain a positive electrode sheet;
所述超音速火焰喷涂的喷涂参数为，采用氧气作为助燃气，氢气作为燃气，氮气作为送粉气体；The spraying parameters of the supersonic flame spraying are that oxygen is used as auxiliary gas, hydrogen is used as fuel gas, and nitrogen is used as powder feeding gas;
所述氧气的压力为20bar，流量为600slpm，氢气的压力为7bar，流量为40slpm，辅助气体甲烷的压力为2bar，流量为8slpm，氮气的压力为6bar，流量为15slpm，送粉速度为30g/min，喷涂距离为250mm。The pressure of the oxygen is 20bar, the flow is 600slpm, the pressure of hydrogen is 7bar, the flow is 40slpm, the pressure of the auxiliary gas methane is 2bar, the flow is 8slpm, the pressure of nitrogen is 6bar, the flow is 15slpm, and the powder feeding speed is 30g/ min, the spraying distance is 250mm.
对比例2Comparative Example 2
本实施例与实施例1的锂离子电池正极极片及其制备方法基本相同，不同的是，在所述的制备方法的步骤(1)中，不添加石墨烯粉体，其余不变。具体的：This embodiment is basically the same as the lithium ion battery positive electrode plate and the preparation method thereof in Embodiment 1. The difference is that in step (1) of the preparation method, no graphene powder is added, and the rest remain unchanged. specific:
所述锂离子电池正极极片的制备方法包括下述步骤：The preparation method of the lithium ion battery positive pole piece comprises the following steps:
(1)在合浆缸中依次加入12份PVDF和45份极性溶剂NMP，保持合浆缸为真空状态，打胶50min，然后加入1份石墨粉和0.3份镍粉；继续打胶2h，得到混合液；(1) Add 12 parts of PVDF and 45 parts of polar solvent NMP in sequence to the mixing tank, keep the mixing tank in a vacuum state, and glue for 50 minutes, then add 1 part of graphite powder and 0.3 parts of nickel powder; continue to glue for 2 hours, get the mixture;
(2)将上述混合液2.5倍重量的正极活性物质加入到上述混合液中搅拌混合，然后加入极性溶剂NMP调节浆料粘度至7000mPa·s，该过程中保持合浆缸为真空状态；(2) the positive active material of above-mentioned mixed solution 2.5 times of weight is added in above-mentioned mixed solution and stirred and mixed, then add polar solvent NMP to adjust slurry viscosity to 7000mPa s, keep mixing cylinder in vacuum state in this process;
(3)将上述浆料低速匀浆，然后均匀涂布在正极集流体的正反两面，在110℃的温度下烘烤15s后，以甲烷作为辅助气体，采用超音速火焰喷涂的方式将铝粉喷涂到正极集流体表面的涂层上，得到正极极片；(3) Homogenize the above slurry at a low speed, and then evenly coat it on both sides of the positive electrode current collector. After baking at a temperature of 110 ° C for 15 s, use methane as an auxiliary gas, and use supersonic flame spraying to spray aluminum. The powder is sprayed on the coating on the surface of the positive electrode current collector to obtain a positive electrode sheet;
所述超音速火焰喷涂的喷涂参数为，采用氧气作为助燃气，氢气作为燃气，氮气作为送粉气体；The spraying parameters of the supersonic flame spraying are that oxygen is used as auxiliary gas, hydrogen is used as fuel gas, and nitrogen is used as powder feeding gas;
所述氧气的压力为20bar，流量为600slpm，氢气的压力为7bar，流量为40slpm，辅助气体甲烷的压力为2bar，流量为8slpm，氮气的压力为6bar，流量为15slpm，送粉速度为30g/min，喷涂距离为250mm。The pressure of the oxygen is 20bar, the flow is 600slpm, the pressure of hydrogen is 7bar, the flow is 40slpm, the pressure of the auxiliary gas methane is 2bar, the flow is 8slpm, the pressure of nitrogen is 6bar, the flow is 15slpm, and the powder feeding speed is 30g/ min, the spraying distance is 250mm.
对比例3Comparative Example 3
本实施例与实施例1的锂离子电池正极极片及其制备方法基本相同，不同的是，在所述的制备方法的步骤(1)中，不添加石墨粉，其余不变。具体的：This embodiment is basically the same as the lithium ion battery positive electrode piece and the preparation method thereof in Embodiment 1, the difference is that in step (1) of the preparation method, no graphite powder is added, and the rest remain unchanged. specific:
所述锂离子电池正极极片的制备方法包括下述步骤：The preparation method of the lithium ion battery positive pole piece comprises the following steps:
(1)在合浆缸中依次加入12份PVDF和45份极性溶剂NMP，保持合浆缸为真空状态，打胶50min，然后加入3份石墨烯粉体和0.3份镍粉；继续打胶2h，得到混合液；(1) Add 12 parts of PVDF and 45 parts of polar solvent NMP into the mixing cylinder in turn, keep the mixing cylinder in a vacuum state, and glue for 50 minutes, then add 3 parts of graphene powder and 0.3 parts of nickel powder; continue to glue 2h to obtain a mixed solution;
(2)将上述混合液2.5倍重量的正极活性物质加入到上述混合液中搅拌混合，然后加入极性溶剂NMP调节浆料粘度至7000mPa·s，该过程中保持合浆缸为真空状态；(2) the positive active material of above-mentioned mixed solution 2.5 times of weight is added in above-mentioned mixed solution and stirred and mixed, then add polar solvent NMP to adjust slurry viscosity to 7000mPa s, keep mixing cylinder in vacuum state in this process;
(3)将上述浆料低速匀浆，然后均匀涂布在正极集流体的正反两面，在110℃的温度下烘烤15s后，以甲烷作为辅助气体，采用超音速火焰喷涂的方式将铝粉喷涂到正极集流体表面的涂层上，得到正极极片；(3) Homogenize the above slurry at a low speed, and then evenly coat it on both sides of the positive electrode current collector. After baking at a temperature of 110 ° C for 15 s, use methane as an auxiliary gas, and use supersonic flame spraying to spray aluminum. The powder is sprayed on the coating on the surface of the positive electrode current collector to obtain a positive electrode sheet;
所述超音速火焰喷涂的喷涂参数为，采用氧气作为助燃气，氢气作为燃气，氮气作为送粉气体；The spraying parameters of the supersonic flame spraying are that oxygen is used as auxiliary gas, hydrogen is used as fuel gas, and nitrogen is used as powder feeding gas;
所述氧气的压力为20bar，流量为600slpm，氢气的压力为7bar，流量为40slpm，辅助气体甲烷的压力为2bar，流量为8slpm，氮气的压力为6bar，流量为15slpm，送粉速度为30g/min，喷涂距离为250mm。The pressure of the oxygen is 20bar, the flow is 600slpm, the pressure of hydrogen is 7bar, the flow is 40slpm, the pressure of the auxiliary gas methane is 2bar, the flow is 8slpm, the pressure of nitrogen is 6bar, the flow is 15slpm, and the powder feeding speed is 30g/ min, the spraying distance is 250mm.
相关测试：Related tests:
1、将实施例中制备得到的正极极片采用剥离强度专用胶带固定，测试极片的剥离强度，测试仪拉伸，剥离正极极片的长度为50mm，将测试的剥离强度记录到表1中。1. The positive pole piece prepared in the embodiment is fixed with a special tape for peel strength, the peel strength of the pole piece is tested, the tester is stretched, and the length of the peeled positive pole piece is 50mm, and the peel strength of the test is recorded in Table 1 .
2、采用四探针法测试实施例中制备得到的正极极片的电阻率，将测试结果记录到表1中。2. The resistivity of the positive electrode pieces prepared in the examples was tested by the four-probe method, and the test results were recorded in Table 1.
表1：Table 1:
基于上述试验数据可以看出，本发明提供的多元复合导电层具有优异的导电性能。采用本发明提供的多元复合导电层的锂离子电池正极极片也具有良好的加工性。Based on the above test data, it can be seen that the multi-component composite conductive layer provided by the present invention has excellent electrical conductivity. The lithium ion battery positive pole piece using the multi-component composite conductive layer provided by the present invention also has good processability.
以上显示和描述了本发明的基本原理、主要特征和本发明的特点。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的范围内。本发明要求保护的范围由所附的权利要求书及其等效物界定。The above shows and describes the basic principles, main features and characteristics of the present invention. Those skilled in the art should understand that the present invention is not limited by the above-mentioned embodiments, and the descriptions in the above-mentioned embodiments and the description are only to illustrate the principle of the present invention. Without departing from the spirit and scope of the present invention, the present invention will have Various changes and modifications are intended to fall within the scope of the claimed invention. The claimed scope of the present invention is defined by the appended claims and their equivalents.
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| CN105441857A (en)* | 2015-11-25 | 2016-03-30 | 广州有色金属研究院 | Method for carrying out high velocity oxy-fuel spraying on surface of roller of lithium battery pole piece rolling machine |
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