CN105098168A - 一种动力型锂电池负极材料的制备方法 - Google Patents
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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Abstract
本发明涉及一种动力型锂电池负极材料的制备方法，包括如下步骤：将按照重量份计的改性钛酸锂80～100份、乙炔黑10～20份和PVDF？10～20份混合均匀，再加入10～20份有机溶剂，混合均匀后，即得；本发明制得得到的钛酸锂在做为负极材料时放电容量明显优于同类产品，而且经过多次放电后，其放电容量损失不大；通过对油酸进行了硫化改性，可以有效地使钛酸锂在与其它的石墨烯、氧化钛材料进行混合时，更好地形成空隙结构，有利于提高烧结过程中制备得到的阴极材料的空隙率，提高放电容量；加入松油醇，提高了放电容量，加入硅烷偶联剂，提高了阴极材料的电容量保持性能，在多次运行后，电容量没有发生了较为明显的下降。
Description
技术领域
本发明涉及锂电池生生产工艺技术领域，具体是指一种动力型锂电池负极材料的制备方法。
背景技术
随着能源的紧缺和世界环保方面的压力，大容量动力蓄电池逐渐形成动力电源的主体，其中作为绿色蓄电池的锂电池，因不会造成二次污染且不具有记忆效应等，逐渐成为动力电源市场应用的首选。动力型锂电池具有能量高、电池电压高、工作温度范围宽、贮存寿命长、具备高功率承受力、自放电率很低、重量轻、绿色环保、无记忆效应等优点，主要应用于混合动力车、电动汽车、电动自行车、以及未来太阳能LED路灯储能设备等方面。环境适应性好、高比能、高安全性和轻量化动力型锂电池正在成为目前国内外研究热点和未来发展方向。现有的锂电池经过多次放电后，放电容量损失较大，大大降低了电池的性能以及使用寿命。
发明内容
本发明的目的在于针对现有动力型锂电池的上述缺陷，提出一种以改性钛酸锂来制作的负极材料，来解决现有锂电池经过多次放电后放电容量损失较大的缺陷。
本发明的技术方案包括：
一种动力型锂电池负极材料的制备方法，包括如下步骤：将按照重量份计的改性钛酸锂80～100份、乙炔黑10～20份和PVDF10～20份混合均匀，再加入10～20份有机溶剂，混合均匀后，即得；
所述的改性钛酸锂的制备方法，包括如下步骤：
第1步、按重量份计，取氢氧化锂15～20份、偏钛酸8～15份、松油醇3～6份，加入170～350份的去离子水，加热至50～60℃，保持3～5小时，得到悬浮液；
第2步、在悬浮液中加入油酸10～20重量份、氢化蓖麻油2～4份、5～12份的石墨烯、二氧化钛2～4份、过氧化二苯甲酰2～4份、硅烷偶联剂5～20份、表面活性剂5～10重量份，搅拌均匀，加热至50～60℃，保持1～2小时，得到改性悬浮液；
第3步、将改性悬浮液用微滤膜过滤，所得的颗粒在1100～1200℃下烧结5～8小时，冷却至室温即可。
所述的第1步中，油酸是经过硫化改性的。
所述的有机溶剂选自N-甲基-2-吡咯烷酮、四氢呋喃、二甲基亚砜、酰胺类溶剂、酯类溶剂或内酯类溶剂；所述的酰胺类溶剂选自二甲基乙酰胺或二甲基甲酰胺；所述的酯类溶剂选自磷酸三甲酯或磷酸三乙酯等；所述的内酯类溶剂选自γ-丁内酯。
所述的表面活性剂是脂肪酸甘油酯。
所述的硅烷偶联剂是KH550。
有益效果
本发明制得得到的钛酸锂在做为负极材料时放电容量明显优于同类产品，而且经过多次放电后，其放电容量损失不大；通过对油酸进行了硫化改性，可以有效地使钛酸锂在与其它的石墨烯、氧化钛材料进行混合时，更好地形成空隙结构，有利于提高烧结过程中制备得到的阴极材料的空隙率，提高放电容量；加入松油醇，提高了放电容量，加入硅烷偶联剂，提高了阴极材料的电容量保持性能，在多次运行后，电容量没有发生了较为明显的下降。
具体实施方式
实施例1
一种动力型锂电池负极材料的制备方法，步骤：将改性钛酸锂90Kg、乙炔黑15Kg和PVDF15Kg混合均匀，再加入20Kg有机溶剂N-甲基-2-吡咯烷酮，混合均匀后，即得；
所述的改性钛酸锂的制备方法，步骤如下：取氢氧化锂18Kg、偏钛酸12Kg、松油醇4Kg，加入300Kg的去离子水，加热至55℃，保持4小时，得到悬浮液；在悬浮液中加入油酸17Kg、氢化蓖麻油3Kg、10Kg的石墨烯、二氧化钛3Kg、过氧化二苯甲酰3Kg、KH550硅烷偶联剂15Kg、脂肪酸甘油酯8Kg，搅拌均匀，加热至55℃，保持2小时，得到改性悬浮液；将改性悬浮液用微滤膜过滤，所得的颗粒在1150℃下烧结7小时，冷却至室温即可。
实施例2
所述的第1步中，油酸是经过硫化改性的，改性方法是：在装有搅拌装置的三口瓶中，加入50g油酸，在不断搅拌下，逐滴加入15g一氯化硫(S2Cl2)，控制反应温度在40℃以下，滴加完毕后，继续反应2小时，往反应物中慢慢加入约100ml的多硫化钠溶液，搅拌反应充分后，分去水层，再加入少许还原铁粉，除去反应体系中的游离硫，过滤，得到油状物，即可。
一种动力型锂电池负极材料的制备方法，步骤：将改性钛酸锂90Kg、乙炔黑15Kg和PVDF15Kg混合均匀，再加入20Kg有机溶剂N-甲基-2-吡咯烷酮，混合均匀后，即得；
所述的改性钛酸锂的制备方法，步骤如下：取氢氧化锂18Kg、偏钛酸12Kg、松油醇4Kg，加入300Kg的去离子水，加热至55℃，保持4小时，得到悬浮液；在悬浮液中加入油酸17Kg、氢化蓖麻油3Kg、10Kg的石墨烯、二氧化钛3Kg、过氧化二苯甲酰3Kg、KH550硅烷偶联剂15Kg、脂肪酸甘油酯8Kg，搅拌均匀，加热至55℃，保持2小时，得到改性悬浮液；将改性悬浮液用微滤膜过滤，所得的颗粒在1150℃下烧结7小时，冷却至室温即可。
对照例1
与实施例1的区别在于：改性钛酸锂的制备方法中未加入松油醇。
一种动力型锂电池负极材料的制备方法，步骤：将改性钛酸锂90Kg、乙炔黑15Kg和PVDF15Kg混合均匀，再加入20Kg有机溶剂N-甲基-2-吡咯烷酮，混合均匀后，即得；
所述的改性钛酸锂的制备方法，步骤如下：取氢氧化锂18Kg、偏钛酸12Kg，加入300Kg的去离子水，加热至55℃，保持4小时，得到悬浮液；在悬浮液中加入油酸17Kg、氢化蓖麻油3Kg、10Kg的石墨烯、二氧化钛3Kg、过氧化二苯甲酰3Kg、KH550硅烷偶联剂15Kg、脂肪酸甘油酯8Kg，搅拌均匀，加热至55℃，保持2小时，得到改性悬浮液；将改性悬浮液用微滤膜过滤，所得的颗粒在1150℃下烧结7小时，冷却至室温即可。
对照例2
与实施例1的区别在于：改性钛酸锂的制备方法中未加入硅烷偶联剂。
一种动力型锂电池负极材料的制备方法，步骤：将改性钛酸锂90Kg、乙炔黑15Kg和PVDF15Kg混合均匀，再加入20Kg有机溶剂N-甲基-2-吡咯烷酮，混合均匀后，即得；
所述的改性钛酸锂的制备方法，步骤如下：取氢氧化锂18Kg、偏钛酸12Kg、松油醇4Kg，加入300Kg的去离子水，加热至55℃，保持4小时，得到悬浮液；在悬浮液中加入油酸17Kg、氢化蓖麻油3Kg、10Kg的石墨烯、二氧化钛3Kg、过氧化二苯甲酰3Kg、脂肪酸甘油酯8Kg，搅拌均匀，加热至55℃，保持2小时，得到改性悬浮液；将改性悬浮液用微滤膜过滤，所得的颗粒在1150℃下烧结7小时，冷却至室温即可。
电池极片材料的性能表征
将制得的负极材料，混合成糊状，在铜箔上涂成厚度为100μm的均匀膜，通过实施例1中的方法压片后制成负极片。以商品化的LiCo0极片为正极，电解液由电解质LiPF6和碳酸乙烯酯/1，2-二甲基碳酸酯按照体积比1：1的混合溶液组成，以聚丙烯微孔膜为隔膜，装配成电池进行试验，在2.8～3.4V，在室温下以20mA/g的恒定电流进行充放电，进行充放电性能测试，结果如下表所示
| 实施例1 | 实施例2 | 对照例1 | 对照例2 | |
| 首次放电容量 mAh/g | 177.5 | 184.6 | 159.8 | 165.2 |
| 30次循环后放电容量 mAh/g | 158.2 | 168.4 | 108.6 | 112.3 |
从表中可以看出，本发明制得得到的钛酸锂在做为负极材料时，其放电容量明显优于同类产品，而且经过多次放电后，其放电容量损失不大。实施例2中通过对油酸进行了硫化改性，可以有效地使钛酸锂在与其它的石墨烯、氧化钛材料进行混合时，更好地形成空隙结构，有利于提高烧结过程中制备得到的阴极材料的空隙率，提高放电容量；对照例1中由于未加入松油醇，导致了放电容量偏小；对照例2中由于未加入硅烷偶联剂，导致了阴极材料的电容量保持性能不好，在多次运行后，电容量发生了较实施例1和实施例2较为明显的下降。
Claims (5)
1.一种动力型锂电池负极材料的制备方法，其特征在于：所述的负极材料的制备方法，包括如下步骤：将按照重量份计的改性钛酸锂80～100份、乙炔黑10～20份和PVDF10～20份混合均匀，再加入10～20份有机溶剂，混合均匀后，即得；
所述的改性钛酸锂的制备方法，包括如下步骤：
第1步、按重量份计，取氢氧化锂15～20份、偏钛酸8～15份、松油醇3～6份，加入170～350份的去离子水，加热至50～60℃，保持3～5小时，得到悬浮液；
第2步、在悬浮液中加入油酸10～20重量份、氢化蓖麻油2～4份、5～12份的石墨烯、二氧化钛2～4份、过氧化二苯甲酰2～4份、硅烷偶联剂5～20份、表面活性剂5～10重量份，搅拌均匀，加热至50～60℃，保持1～2小时，得到改性悬浮液；
第3步、将改性悬浮液用微滤膜过滤，所得的颗粒在1100～1200℃下烧结5～8小时，冷却至室温即可。
2.根据权利要求1所述的动力型锂电池负极材料的制备方法，其特征在于：所述的第1步中，油酸是经过硫化改性的。
3.根据权利要求1所述的动力型锂电池负极材料的制备方法，其特征在于：所述的有机溶剂选自N-甲基-2-吡咯烷酮、四氢呋喃、二甲基亚砜、酰胺类溶剂、酯类溶剂或内酯类溶剂；所述的酰胺类溶剂选自二甲基乙酰胺或二甲基甲酰胺；所述的酯类溶剂选自磷酸三甲酯或磷酸三乙酯等；所述的内酯类溶剂选自γ-丁内酯。
4.根据权利要求1所述的动力型锂电池负极材料的制备方法，其特征在于：所述的表面活性剂是脂肪酸甘油酯。
5.根据权利要求1所述的动力型锂电池负极材料的制备方法，其特征在于：所述的硅烷偶联剂是KH550。
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| US20130302690A1 (en) * | 2012-05-08 | 2013-11-14 | Korea Institute Of Science And Technology | Method for coating carbon on lithium titanium oxide-based anode active material nanoparticles and carbon-coated lithium titanium oxide-based anode active material nanoparticles produced by the method |
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| WO2012163426A1 (en) * | 2011-06-01 | 2012-12-06 | Westfälische Wilhelms Universität | Electrode material for lithium and lithium ion batteries |
| US20130302690A1 (en) * | 2012-05-08 | 2013-11-14 | Korea Institute Of Science And Technology | Method for coating carbon on lithium titanium oxide-based anode active material nanoparticles and carbon-coated lithium titanium oxide-based anode active material nanoparticles produced by the method |
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