技术领域technical field
本发明涉及一种锂离子电池及制备技术领域，尤其涉及一种负极浆料、负极浆料的制备方法以及使用该负极浆料制作的负极片及锂离子电池。The invention relates to the technical field of a lithium ion battery and its preparation, in particular to a negative electrode slurry, a method for preparing the negative electrode slurry, and a negative electrode sheet and a lithium ion battery made using the negative electrode slurry.
背景技术Background technique
锂离子电池因能够实现多次充放电、可以对外界环境实现大倍率放电、无记忆效应、节约能源等诸多独特优点而被人们利用，来代替传统电池无法循环使用、不环保、浪费能源等一系列问题。但是目前锂电池普遍存在锂离子电池大电流充放电时电池极化严重，倍率放电性能较差、低温环境下放电量少，使用寿命短等一系列问题。这是因为以传统石墨为负极材料的锂电池中碳的嵌锂和脱锂性能不佳，使充电过程中金属锂表面不均匀，造成“锂枝晶”。所以寻找新型的负极材料，改善传统石墨负极材料的缺陷成为锂离子电池的研究热点。Lithium-ion batteries are used by people because they can be charged and discharged multiple times, can discharge at a large rate to the external environment, have no memory effect, save energy, and many other unique advantages. They are used to replace traditional batteries that cannot be recycled, are not environmentally friendly, and waste energy. series of questions. However, at present, lithium batteries generally have a series of problems such as severe battery polarization when charging and discharging lithium-ion batteries at high currents, poor rate discharge performance, low discharge capacity in low temperature environments, and short service life. This is because the carbon in lithium batteries using traditional graphite as the negative electrode material has poor lithium insertion and delithiation performance, which makes the surface of metal lithium uneven during charging, resulting in "lithium dendrites". Therefore, looking for new negative electrode materials and improving the defects of traditional graphite negative electrode materials has become a research hotspot for lithium-ion batteries.
硬碳材料由于具有相互交错的层状结构，锂离子在硬碳中具有比传统石墨更多的嵌入和脱出通道，因此具有比石墨更高的充放电速度和更优良的低温性能，同时大量微孔的存在，也使得硬碳具有比石墨更高的可逆比容量，是一种非常富有潜力的负极材料。然而，正是由于具有大量交错层状结构及锂离子脱嵌通道，使得硬碳材料的首次充放电的不可逆容量大大增加，主要原因是大量的锂与电解液在材料表面反应生成的固体电解质SEI膜所致。因此，改善硬碳负极材料首次充放电效率低的缺陷，成为硬碳负极材料的一个开发热点。Due to the interlaced layered structure of hard carbon materials, lithium ions have more intercalation and extraction channels in hard carbon than traditional graphite, so they have higher charge and discharge speeds and better low-temperature performance than graphite. The existence of pores also makes hard carbon have a higher reversible specific capacity than graphite, which is a very potential negative electrode material. However, it is precisely because of the large number of interlaced layered structures and lithium ion deintercalation channels that the irreversible capacity of the first charge and discharge of hard carbon materials is greatly increased, mainly due to the solid electrolyte SEI formed by the reaction of a large amount of lithium and electrolyte on the surface of the material. caused by the membrane. Therefore, improving the defect of low initial charge and discharge efficiency of hard carbon negative electrode materials has become a development hotspot of hard carbon negative electrode materials.
发明内容Contents of the invention
本发明要解决的技术问题是针对以上问题，提供一种负极浆料及负极浆料的制备方法，采用本发明的负极浆料制备的锂离子电池能够实现超高倍率充放电，且低温环境下放电量性能好，充放电速率及容量密度高，负极材料首次充放电效率高，具有高循环寿命；The technical problem to be solved in the present invention is to provide a negative electrode slurry and a preparation method of the negative electrode slurry in view of the above problems. The lithium ion battery prepared by using the negative electrode slurry of the present invention can realize ultra-high rate charge and discharge, and can be discharged in a low temperature environment. Good power performance, high charge and discharge rate and capacity density, high initial charge and discharge efficiency of negative electrode materials, and high cycle life;
本发明还提供了一种采用上述负极浆料的负极片；The present invention also provides a negative electrode sheet using the above negative electrode slurry;
另外，本发明还提供了一种利用上述负极片的锂离子电池。In addition, the present invention also provides a lithium ion battery using the above negative electrode sheet.
为了解决上述问题，本发明采用以下技术方案：一种负极浆料，其特征在于：所述负极浆料包括以下重量配比的组份：硬碳和石墨混合料91-95%，导电炭黑1-3%，聚偏氟乙烯4-6%，另加上述物料总配重0.1-0.3%的草酸。In order to solve the above problems, the present invention adopts the following technical solutions: a negative electrode slurry, characterized in that: the negative electrode slurry includes the following components in weight ratio: hard carbon and graphite mixture 91-95%, conductive carbon black 1-3%, polyvinylidene fluoride 4-6%, plus oxalic acid with a total weight of 0.1-0.3% of the above materials.
以下是本发明的进一步改进：The following are further improvements of the present invention:
所述硬碳和石墨混合料中硬碳占混合料总重量比为10-18%。The hard carbon in the hard carbon and graphite mixture accounts for 10-18% of the total weight of the mixture.
进一步改进：Further improvements:
所述硬碳为微米级颗粒，其比表面为3-5m2/g。The hard carbon is micron-sized particles with a specific surface area of 3-5m2 /g.
进一步改进：Further improvements:
所述负极浆料包括以下重量配比的组份：硬碳和石墨混合料94%，导电炭黑1.5%，聚偏氟乙烯4.5%，另加上述物料总配重0.2%的草酸。The negative electrode slurry includes the following components by weight: 94% hard carbon and graphite mixture, 1.5% conductive carbon black, 4.5% polyvinylidene fluoride, plus 0.2% oxalic acid with the total weight of the above materials.
进一步改进：Further improvements:
一种负极浆料的制备方法，包括如下步骤：A preparation method of negative electrode slurry, comprising the steps of:
1）、真空烘干步骤，取上述重量配比的硬碳和石墨混合料、导电炭黑、聚偏氟乙烯和前述物质总重量0.2%的草酸，作为负极浆料的原料，真空烘干；1) In the vacuum drying step, take the hard carbon and graphite mixture, conductive carbon black, polyvinylidene fluoride and oxalic acid with a total weight of 0.2% of the above-mentioned substances in the above weight ratio, as the raw material of the negative electrode slurry, and vacuum dry;
2）、溶胶步骤，取与上述原料重量相等的N-甲基吡咯烷酮作为溶剂，将1）中的聚偏氟乙烯溶于其中，高速搅拌；2), the sol step, taking N-methylpyrrolidone equal to the weight of the above raw materials as a solvent, dissolving the polyvinylidene fluoride in 1) in it, and stirring at a high speed;
3）、向步骤2）中制备的胶液中加入导电炭黑，低速搅拌，得到混合料；3) Add conductive carbon black to the glue prepared in step 2), and stir at a low speed to obtain a mixture;
4）、向步骤3）中的混合料中先加入硬碳，低速搅拌，得到混合料；4), first add hard carbon to the mixture in step 3), and stir at a low speed to obtain the mixture;
5）、向步骤4）中的混合料中加入石墨，低速搅拌，得到混合料；5), add graphite to the mixture in step 4), and stir at a low speed to obtain the mixture;
6）、向步骤5）中的混合料中加入草酸，低速搅拌，得到混合料；6), add oxalic acid to the mixture in step 5), and stir at a low speed to obtain the mixture;
7）、将步骤5）得到的混合料真空保压，制得负极浆料。7) Vacuum-press the mixture obtained in step 5) to prepare negative electrode slurry.
进一步改进：Further improvements:
步骤2）中溶胶过程中，先不开循环水，当温度达到 50℃，再打开循环水，搅拌完成时，胶液无明显结块；搅拌时间为3～4h。Step 2) During the sol process, do not turn on the circulating water first, and then turn on the circulating water when the temperature reaches 50°C. When the stirring is completed, there is no obvious agglomeration of the glue; the stirring time is 3 to 4 hours.
进一步改进：Further improvements:
步骤3）-步骤5）中搅拌时间为1 h。The stirring time in step 3)-step 5) is 1 h.
进一步改进：Further improvements:
步骤5）中真空度为-0.09Mpa，保压时间为1h。Step 5) The medium vacuum degree is -0.09Mpa, and the holding time is 1h.
一种负极片，所述负极片包括负极集流体，负极集流体的上下表面上均匀涂布有负极浆料，负极浆料涂布的单面面密度为5.41-6.41mg/cm2。A negative electrode sheet, the negative electrode sheet includes a negative electrode current collector, the upper and lower surfaces of the negative electrode current collector are uniformly coated with negative electrode slurry, and the density of one side coated with the negative electrode slurry is 5.41-6.41 mg/cm2 .
一种锂离子电池，包括正极片、负极片、隔膜和铝塑复合膜，其中正极片和负极片交替排列，而隔膜位于正极片和负极片之间，铝塑复合膜包裹住正极片、负极片和隔膜，正负极极片极耳均采用全极耳设计。A lithium-ion battery comprising a positive electrode sheet, a negative electrode sheet, a diaphragm and an aluminum-plastic composite film, wherein the positive electrode sheet and the negative electrode sheet are arranged alternately, and the separator is located between the positive electrode sheet and the negative electrode sheet, and the aluminum-plastic composite film wraps the positive electrode sheet, the negative electrode The tabs and diaphragms, the tabs of the positive and negative poles are designed with full tabs.
本发明采用上述技术方案的负极浆料制备的锂离子电池具有以下技术效果：The present invention adopts the lithium-ion battery prepared by the negative electrode slurry of the above-mentioned technical scheme to have the following technical effects:
1、电池能够10C-30C高倍率放电，且20C/1C放电容量可达到95%，30C/1C放电容量可达到90%以上；1. The battery can be discharged at a high rate of 10C-30C, and the discharge capacity of 20C/1C can reach 95%, and the discharge capacity of 30C/1C can reach more than 90%;
2、电池可大倍率快速充电，5C快速充电后，10C和20C高倍率放电容量释放率均高达98%以上；2. The battery can be quickly charged at a high rate. After 5C fast charge, the release rate of 10C and 20C high rate discharge capacity is as high as 98%;
3、电池能够在-20℃— -40℃放电，-20℃放电容量可达常温放电容量的90%以上，且在-40℃放电容量可达额定容量的81%；3. The battery can be discharged at -20°C - -40°C, the discharge capacity at -20°C can reach more than 90% of the normal temperature discharge capacity, and the discharge capacity at -40°C can reach 81% of the rated capacity;
4、电池10C充10C放电持续循环200周，容量保持率达92%以上；4. The battery can be charged at 10C and discharged at 10C continuously for 200 cycles, and the capacity retention rate is over 92%;
5、负极材料首次充放电效率可达87%以上；5. The first charge and discharge efficiency of the negative electrode material can reach more than 87%;
6、性能稳定，可超高倍率充放电，耐低温性能良好，可应用于汽车启停电源领域，具有广泛的应用前景。6. It has stable performance, can be charged and discharged at an ultra-high rate, and has good low temperature resistance. It can be used in the field of automobile start-stop power supply, and has broad application prospects.
附图说明Description of drawings
附图1为电芯极片的结构示意图；Accompanying drawing 1 is the structural representation of cell pole piece;
附图2软包电池的结构示意图；Accompanying drawing 2 is the schematic structural diagram of the pouch battery;
附图3为铝壳电池的结构示意图；Accompanying drawing 3 is the structural representation of aluminum case battery;
附图4为负极极片SEM图；Accompanying drawing 4 is the SEM figure of negative pole sheet;
附图5为1C充电不同倍率放电曲线对比图；Accompanying drawing 5 is the comparative chart of 1C charging different rate discharge curves;
附图6为5C充电不同倍率放电曲线对比图；Accompanying drawing 6 is a comparison chart of 5C charge and discharge curves at different rates;
附图7为不同温度下1C放电曲线对比图。Accompanying drawing 7 is the comparative chart of 1C discharge curve under different temperature.
附图8为10C充放电循环曲线图。Accompanying drawing 8 is 10C charging and discharging cycle graph.
具体实施方式detailed description
实施例1，一种负极浆料，包括固体物料及液体物料，所述固体物料包括以下重量配比的组份：硬碳和石墨混合料94%，导电炭黑1.5%，聚偏氟乙烯4.5%，另加固体物料总配重0.1-0.3%的草酸，优选为0.2%。Embodiment 1, a kind of negative electrode slurry, comprises solid material and liquid material, and described solid material comprises the component of following weight ratio: hard carbon and graphite mixture 94%, conductive carbon black 1.5%, polyvinylidene fluoride 4.5% %, plus 0.1-0.3% oxalic acid with a total weight of solid material, preferably 0.2%.
所述液体物料为有机溶剂，优选为N-甲基吡咯烷酮。The liquid material is an organic solvent, preferably N-methylpyrrolidone.
所述负极浆料的固含量为50%（即固体物料占总浆料的比重）。The solid content of the negative electrode slurry is 50% (that is, the proportion of solid materials in the total slurry).
所述硬碳和石墨混合料中硬碳占混合料总重量比为15%。The hard carbon in the hard carbon and graphite mixture accounts for 15% of the total weight of the mixture.
所述硬碳为微米级颗粒，其比表面为3-5m2/g。The hard carbon is micron-sized particles with a specific surface area of 3-5m2 /g.
一种负极浆料的制备方法，包括如下步骤：A preparation method of negative electrode slurry, comprising the steps of:
1）、取重量配比为94%的硬碳和石墨混合料、1.5%的导电炭黑、4.5%的聚偏氟乙烯和前述物质总重量0.2%的草酸，作为负极浆料的原料，真空烘干，去除水分；1) Take 94% hard carbon and graphite mixture by weight, 1.5% conductive carbon black, 4.5% polyvinylidene fluoride, and 0.2% oxalic acid in the total weight of the aforementioned substances as raw materials for the negative electrode slurry, vacuum drying to remove moisture;
2）、取与上述原料重量相等的N-甲基吡咯烷酮作为溶剂，将步骤1）中的聚偏氟乙烯溶于其中，采用双行星搅拌（高速搅拌）3～4h；2) Take N-methylpyrrolidone equal to the weight of the above raw materials as a solvent, dissolve the polyvinylidene fluoride in step 1) in it, and use double planetary stirring (high-speed stirring) for 3 to 4 hours;
溶胶过程中，先不开循环水，当温度达到 50℃，再打开循环水，搅拌完成时，胶液无明显结块；During the sol process, do not turn on the circulating water first, and then turn on the circulating water when the temperature reaches 50°C. When the stirring is completed, there is no obvious agglomeration of the glue;
3）、向步骤2）中制备的胶液中加入导电炭黑，低速搅拌1h，得到混合料；3) Add conductive carbon black to the glue prepared in step 2), and stir at a low speed for 1 hour to obtain a mixture;
4）、向步骤3）中的混合料中先加入硬碳，低速搅拌1h；4) Add hard carbon to the mixture in step 3) and stir for 1 hour at low speed;
再加入石墨，低速搅拌1h；Then add graphite and stir at low speed for 1 h;
最后加入草酸，低速搅拌1h；Finally, add oxalic acid and stir for 1 hour at low speed;
最后真空-0.09Mpa以下保压1h，得到负极浆料。Finally, keep the pressure under vacuum-0.09Mpa for 1h to obtain the negative electrode slurry.
一种负极片，包括负极集流体和上述负极浆料，负极集流体为具有导电涂层覆盖的集流体，涂层厚度为1-2um。A negative electrode sheet includes a negative electrode current collector and the above negative electrode slurry, the negative electrode current collector is a current collector covered with a conductive coating, and the thickness of the coating is 1-2um.
负极浆料均匀涂布在负极集流体的上下表面上，浆料在负极集流体上的单面面密度为5.85mg/cm2。The negative electrode slurry was evenly coated on the upper and lower surfaces of the negative electrode current collector, and the density of the slurry on one side of the negative electrode current collector was 5.85 mg/cm2 .
一种锂离子电池，如图1-3所示，包括正极片、负极片、隔膜和铝塑复合膜（或铝壳），其中正极片和负极片交替排列，而隔膜位于正极片和负极片之间，铝塑复合膜（或铝壳）包裹住正极片、负极片和隔膜，正极极耳及负极极耳均采用全极耳设计。A lithium-ion battery, as shown in Figure 1-3, includes a positive electrode sheet, a negative electrode sheet, a separator, and an aluminum-plastic composite film (or aluminum shell), in which the positive electrode sheet and the negative electrode sheet are arranged alternately, and the separator is located between the positive electrode sheet and the negative electrode sheet. Between them, the aluminum-plastic composite film (or aluminum shell) wraps the positive electrode, negative electrode and separator, and the positive electrode tab and the negative electrode tab are all designed with full tabs.
本实施例通过上述步骤制得负极片，通过叠片（或卷绕）的方式作出方形的电芯体，制造而成的电芯体再经过封装、干燥及注液、化成和分容等工序而制造成方形的电池。In this example, the negative electrode sheet is prepared through the above steps, and a square cell body is made by stacking (or winding), and the manufactured cell body is then packaged, dried, liquid injected, formed, and volume divided. And manufactured into a square battery.
本发明中的负极浆料采用硬碳搭配石墨作为活性材料。由于硬碳材料为无序乱层结构，拥有较石墨材料更多的锂离子传递通道，因此其充放电速率及容量密度更高。借助硬碳良好的倍率充放电和低温性能，实现了电池的30C超高倍率大电流放电性能和可快速充满电的性能，改善了石墨负极低温放电性能差的缺陷。The negative electrode slurry in the present invention adopts hard carbon and graphite as active materials. Since the hard carbon material has a disordered disordered layer structure, it has more lithium ion transfer channels than the graphite material, so its charge and discharge rate and capacity density are higher. With the help of hard carbon's good rate charge and discharge and low temperature performance, the battery's 30C ultra-high rate high current discharge performance and fast full charge performance have been realized, and the defect of poor low temperature discharge performance of the graphite negative electrode has been improved.
但是硬碳材料首次效率不高，比表面越大，首次效率损失越严重。因此，本发明采用的硬碳比表面为3-5m2/g。同时搭配石墨材料，使得首次效率可达87%以上，改善了首次效率低的问题。选择的硬碳占总重量比例为10%-18%，同时兼顾了电池首次效率，以及复合材料的电子电导率和离子迁移速率，保证了其最佳导电嵌锂性能。However, the initial efficiency of hard carbon materials is not high, and the larger the specific surface area, the more serious the initial efficiency loss. Therefore, the specific surface area of the hard carbon used in the present invention is 3-5m2 /g. At the same time, with graphite materials, the first-time efficiency can reach more than 87%, which improves the problem of low first-time efficiency. The selected hard carbon accounts for 10%-18% of the total weight, while taking into account the initial efficiency of the battery, as well as the electronic conductivity and ion migration rate of the composite material, to ensure its best conductive lithium intercalation performance.
实施例2-5，与实施例1不同的是负极浆料配比参数，表1为本发明中实施例1-5的负极浆料配比参数表，其中各实施例的制备方法均与实施例1相同，故此处不再进行一一详述，具体参数值见下表：Embodiment 2-5, different from embodiment 1 is negative electrode slurry proportioning parameter, and table 1 is the negative electrode slurry proportioning parameter table of embodiment 1-5 in the present invention, and wherein the preparation method of each embodiment is all with implementation Example 1 is the same, so it will not be described in detail here, and the specific parameter values are shown in the table below:
表1 各实施例负极配料比例Table 1 The ratio of negative electrode ingredients in each embodiment
采用本发明的组分及制备方法制备而成的锂离子电池具有超高倍率放电和耐低温的性能。The lithium ion battery prepared by adopting the component and the preparation method of the invention has the performance of super high rate discharge and low temperature resistance.
经试验，实施例1为最优实施例，以实施例1中制备的锂离子电池为例，其性能参见图4-8。After testing, Example 1 is the best example. Taking the lithium-ion battery prepared in Example 1 as an example, its performance is shown in Figures 4-8.
由图4可知，负极材料中的硬碳均匀分散在石墨中。It can be seen from Figure 4 that the hard carbon in the negative electrode material is uniformly dispersed in the graphite.
由图5可知，该电池能够20C-30C高倍率放电，20C/1C放电容量可达95%，且30C/1C放电容量比值达到90%以上。It can be seen from Figure 5 that the battery can be discharged at a high rate of 20C-30C, the 20C/1C discharge capacity can reach 95%, and the 30C/1C discharge capacity ratio can reach more than 90%.
由图6可知，5C快速充电后10C和20C高倍率放电容量释放率均高达98%以上。It can be seen from Figure 6 that after 5C fast charging, the 10C and 20C high-rate discharge capacity release rates are as high as 98%.
由图7可知，低温-20℃1C放电容量可达常温放电容量的92.5%，-40℃仍可放出81%电量。It can be seen from Figure 7 that the low temperature -20°C 1C discharge capacity can reach 92.5% of the normal temperature discharge capacity, and -40°C can still discharge 81% of the electricity.
由图8可知，本发明电池10C快速充放电持续循环200周，容量保持率达92%以上。It can be seen from FIG. 8 that the battery 10C of the present invention has a continuous cycle of rapid charge and discharge for 200 cycles, and the capacity retention rate is over 92%.
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610616819.XACN106169559A (en) | 2016-08-01 | 2016-08-01 | A kind of cathode size, the preparation method of cathode size and use the negative plate and lithium ion battery that this cathode size makes |
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610616819.XACN106169559A (en) | 2016-08-01 | 2016-08-01 | A kind of cathode size, the preparation method of cathode size and use the negative plate and lithium ion battery that this cathode size makes |
| Publication Number | Publication Date |
|---|---|
| CN106169559Atrue CN106169559A (en) | 2016-11-30 |
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610616819.XAPendingCN106169559A (en) | 2016-08-01 | 2016-08-01 | A kind of cathode size, the preparation method of cathode size and use the negative plate and lithium ion battery that this cathode size makes |
| Country | Link |
|---|---|
| CN (1) | CN106169559A (en) |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109742339A (en)* | 2018-12-14 | 2019-05-10 | 江苏海四达电源股份有限公司 | A kind of high-energy-density ultralow temperature high-safety polymer lithium ion battery and preparation method thereof |
| CN113471404A (en)* | 2020-03-15 | 2021-10-01 | 深圳格林德能源集团有限公司 | Inorganic ceramic coating negative plate of lithium ion battery and manufacturing method thereof |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103441305A (en)* | 2013-08-27 | 2013-12-11 | 深圳市贝特瑞新能源材料股份有限公司 | Power and energy storage lithium-ion battery and preparation method thereof |
| CN104577042A (en)* | 2014-12-23 | 2015-04-29 | 山东精工电子科技有限公司 | Lithium ion battery negative electrode paste and preparation method |
| CN104900904A (en)* | 2015-05-25 | 2015-09-09 | 深圳市斯盛能源股份有限公司 | Lithium ion secondary battery |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103441305A (en)* | 2013-08-27 | 2013-12-11 | 深圳市贝特瑞新能源材料股份有限公司 | Power and energy storage lithium-ion battery and preparation method thereof |
| CN104577042A (en)* | 2014-12-23 | 2015-04-29 | 山东精工电子科技有限公司 | Lithium ion battery negative electrode paste and preparation method |
| CN104900904A (en)* | 2015-05-25 | 2015-09-09 | 深圳市斯盛能源股份有限公司 | Lithium ion secondary battery |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109742339A (en)* | 2018-12-14 | 2019-05-10 | 江苏海四达电源股份有限公司 | A kind of high-energy-density ultralow temperature high-safety polymer lithium ion battery and preparation method thereof |
| CN113471404A (en)* | 2020-03-15 | 2021-10-01 | 深圳格林德能源集团有限公司 | Inorganic ceramic coating negative plate of lithium ion battery and manufacturing method thereof |
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| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | Application publication date:20161130 | |
| RJ01 | Rejection of invention patent application after publication |