CN114512651A - 一种硅酸钛锂颗粒原位碳包覆方法及复合产物 - Google Patents
一种硅酸钛锂颗粒原位碳包覆方法及复合产物 Download PDFInfo
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- SWAIALBIBWIKKQ-UHFFFAOYSA-N lithium titanium Chemical compound [Li].[Ti] SWAIALBIBWIKKQ-UHFFFAOYSA-N 0.000 title claims abstract description 64
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 58
- 238000000576 coating method Methods 0.000 title claims abstract description 25
- 239000002245 particle Substances 0.000 title claims abstract description 21
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 17
- 239000002131 composite material Substances 0.000 title description 5
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 36
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000000725 suspension Substances 0.000 claims abstract description 9
- 230000032683 aging Effects 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004094 surface-active agent Substances 0.000 claims abstract description 6
- 239000012298 atmosphere Substances 0.000 claims abstract description 5
- 239000003054 catalyst Substances 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 4
- 238000010000 carbonizing Methods 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract 4
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 1
- 239000011248 coating agent Substances 0.000 abstract description 12
- 239000005011 phenolic resin Substances 0.000 abstract description 7
- 238000003763 carbonization Methods 0.000 abstract description 6
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 abstract description 4
- 229920001568 phenolic resin Polymers 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 238000000498 ball milling Methods 0.000 abstract 1
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 10
- 239000010410 layer Substances 0.000 description 10
- 229910052744 lithium Inorganic materials 0.000 description 10
- 230000004048 modification Effects 0.000 description 7
- 238000012986 modification Methods 0.000 description 7
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 6
- 229910001416 lithium ion Inorganic materials 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 5
- 239000012299 nitrogen atmosphere Substances 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 229910052912 lithium silicate Inorganic materials 0.000 description 4
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 150000002641 lithium Chemical class 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 229910052596 spinel Inorganic materials 0.000 description 3
- 239000011029 spinel Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 210000001787 dendrite Anatomy 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
本发明公开了一种对硅酸钛锂颗粒进行原位均匀碳包覆的方法,步骤为:将硅酸钛锂颗粒分散在一定量水中,加入少量表面活性剂搅拌均匀,形成悬浮液。分别加入乙醇、间苯二酚、甲醛和少量催化剂搅拌均匀,搅拌后室温下无干扰静置老化一段时间;经过离心、洗涤、干燥后得到酚醛树脂包覆的前驱体;将所得前驱物在氮气或惰性气氛下碳化,得到均匀碳包覆的硅酸钛锂材料。本发明中酚醛树脂在硅酸钛锂颗粒表面原位生成,碳化后可实现颗粒表面均匀碳包覆。本发明适用于不同尺寸的硅酸钛锂颗粒表面碳包覆。该包覆工艺不需要复杂和昂贵的球磨混料设备,过程简单,易操作,有利于商业化。
Description
技术领域
本发明属于锂离子电池材料技术领域,尤其涉及一种对负极材料硅酸钛锂颗粒表面进行原位均匀碳包覆的方法及复合产物。
背景技术
随着“双碳”目标和5G时代的到来,人们对电动汽车和便携式电子设备的需求与日俱增,由此产生的对高能量密度、高功率密度、长循环寿命和高安全性能的锂离子电池的需求也愈加旺盛。与传统的铅酸电池、镍氢电池相比,目前商业化的锂离子电池有着高能量密度、长循环寿命、安全性能好和环境友好等优点,已经成为便携式电子产品和电动汽车的首选电池储能技术。
现阶段锂离子电池负极材料主要采用基于嵌入反应的石墨和尖晶石型钛酸锂,但是石墨的工作电势较低,大电流充放电和长时间循环易导致锂枝晶在电极表面沉积形成刺穿隔膜,带来可怕的安全隐患。尖晶石型钛酸锂虽然不易形成锂枝晶,而且稳定性好,但是理论比容量较低,充放电电势较高,极大限制了锂离子电池的能量密度提升。
新型聚阴离子型锂离子电池负极材料硅酸钛锂,不仅理论比容量高(308mAh g-1),还具有合适的充放电平台(约0.3V)。因此,可以在一定程度上解决钛酸锂比容量较低和充放电平台过高的缺点,与石墨相比安全性也更高。但是硅酸钛锂较低的电导率和充放电过程中出现的晶粒粉化现象严重限制了其电化学性能的发挥。
发明内容
发明目的:本发明的第一目的在于提供一种有效提高硅酸钛锂循环稳定性能和倍率性能的碳包覆改性制备方法。
本发明的第二目的在于提供利用所述制备方法得到的碳包覆硅酸钛锂复合材料;该复合材料电导率、循环稳定性和倍率性能都得到了极大的提高。
技术方案:本发明的硅酸钛锂颗粒原位碳包覆方法,包括如下步骤:
步骤1、将硅酸钛锂分散在一定量水中,加入表面活性剂,搅拌或超声分散均匀,形成悬浮液;
步骤2、往悬浮液中依次加入乙醇、间苯二酚、甲醛和催化剂,搅拌均匀;
步骤3、将步骤2所得混合物在室温下无干扰静置老化;
步骤4、将步骤3所得产物离心、洗涤、干燥得到前驱物;
步骤5、将前驱物在惰性气氛下碳化,煅烧,冷却后得到所述的碳包覆硅酸钛锂材料。
进一步地,步骤1中,所述表面活性剂为十六烷基三甲基溴化铵;所述硅酸钛锂与十六烷基三甲基溴化铵的质量比为1:0.5~1。
进一步地,步骤2中,所述间苯二酚的加入量,按照硅酸钛锂与间苯二酚的质量比为1:0.2~0.5。
进一步地,步骤2中,所述甲醛的加入量,按照硅酸钛锂与甲醛的质量比为1∶2~5。
进一步地,步骤2中,所述催化剂为氨水;所述氨水的加入量,按照硅酸钛锂与氨水的质量比为1∶1~5。
进一步地,步骤3中,所述无干扰静置老化的时间为6~12h。
进一步地,步骤4中,所述干燥条件为60℃,干燥时间为6~12h。
进一步地,步骤5中,所述惰性气氛为氩气或氮气气氛。
进一步地,步骤5中,所述煅烧温度为700~1000℃,煅烧时间为2~5h。
反应原理如下:
本发明利用表面活性剂的吸附耦合作用,将间苯二酚和甲醛反应生成的酚醛树脂原位吸附在硅酸钛锂的表面形成均匀致密的包覆层。将所得产物碳化后,前驱体酚醛树脂中苯环中6个sp2杂化的碳原子构成的六元环状π-π共轭结构被保留下来,形成高石墨化度碳层。碳层中的共轭结构极大促进了电子和离子的传输,使得硅酸钛锂具备出色的电化学性能。
有益效果:与现有技术相比,本发明具有如下显著优点:
(1)本发明引入的聚合物碳源在硅酸钛锂颗粒表面原位生成,高温碳化后可以在硅酸钛锂表面实现均匀碳包覆。
(2)本发明引入的碳源含有大量的共轭结构,因此经过碳化后形成的碳包覆层具有极高的电子电导率。
(3)本发明通过控制其他变量,只改变反应物浓度就可以在硅酸钛锂表面包覆几纳米到上百纳米厚度不等的均匀碳层。
(4)本发明引入的碳包覆改性制备方法极大的提高了硅酸钛锂的电导率、循环稳定性能和倍率性能。
附图说明
图1为本发明实施例1碳包覆改性制备的硅酸钛锂的工艺流程图;
图2为本发明实施例1碳包覆改性制备的硅酸钛锂的X-射线衍射图谱;
图3为本发明实施例1碳包覆改性制备的硅酸钛锂在不同放大倍数下的扫描电镜图;
图4为本发明实施例1碳包覆改性制备的硅酸钛锂在不同放电倍率下的性能图。
图5为本发明实施例2碳包覆改性制备的硅酸钛锂的在不同放大倍数下的透射电镜图;
图6为本发明实施例3碳包覆改性制备的硅酸钛锂的在不同放大倍数下的透射电镜图;
图7为本发明实施例4碳包覆改性制备的硅酸钛锂的在不同放大倍数下的透射电镜图。
具体实施方式
下面结合附图对本发明的技术方案作进一步说明。
实施例1
本发明的流程如图1所示:
A、称取1g硅酸钛锂和0.5g十六烷基三甲基溴化铵,分散于蒸馏水中超声均匀,形成悬浮液;
B、往溶液中加入20ml乙醇、0.2g间苯二酚、2ml甲醛和1ml起催化作用的氨水搅拌均匀,制得混合物;
C、将混合物在室温下无干扰静置6h老化;
D、将所得产物离心、洗涤后,在60℃干燥6h后得到前驱体;
E、将所得前驱体在氮气气氛下700℃煅烧2h,冷却后获得所述的碳包覆改性硅酸钛锂。
图2为碳包覆硅酸钛锂的X-射线衍射谱图,从图2中可以看出碳包覆后的硅酸钛锂结晶性良好;图3为碳包覆后的硅酸钛锂在不同放大倍数下的扫描电镜图,从图3可以看出碳层均匀包覆在硅酸钛锂颗粒的表面;图4为碳包覆和未经包覆处理的的硅酸钛锂电极在不同放电电流密度下的容量对比图,从图4可以看出碳包覆后的硅酸钛锂在不同电流密度下比容量明显高于纯相硅酸钛锂,说明均匀碳包覆提高了硅酸钛锂大电流下的放电能力。
实施例2
A、称取1g硅酸钛锂和0.6g十六烷基三甲基溴化铵,分散于蒸馏水中超声均匀,形成悬浮液;
B、往溶液中加入25ml乙醇、0.3g间苯二酚、3ml甲醛和2ml起催化作用的氨水搅拌均匀,制得混合物;
C、将混合物在室温下无干扰静置8h老化;
D、将所得产物离心、洗涤后,在60℃干燥8h后得到前驱体;
E、将所得前驱体在氮气气氛下800℃煅烧3h,冷却后获得所述的碳包覆改性硅酸钛锂。
图5为碳包覆改性硅酸钛锂的透射电镜图,从图5a可以看出酚醛树脂碳化后在硅酸钛锂颗粒表面形成了均匀包覆的碳层,从图5b中可以看出碳层厚度约为3nm。
实施例3
A、称取1g硅酸钛锂和0.8g十六烷基三甲基溴化铵,分散于蒸馏水中超声均匀,形成悬浮液;
B、往溶液中加入30ml乙醇、0.4g间苯二酚、4ml甲醛和3ml起催化作用的氨水搅拌均匀,制得混合物;
C、将混合物在室温下无干扰静置10h老化;
D、将所得产物离心、洗涤后,在60℃干燥10h后得到前驱体;
E、将所得前驱体在氮气气氛下900℃煅烧3h,冷却后获得所述的碳包覆改性硅酸钛锂。
图6为碳包覆改性硅酸钛锂的透射电镜图,从图6a可以看出酚醛树脂碳化后在硅酸钛锂的表面形成了均匀包覆的碳层,从图6b中可以看出碳层厚度约为9nm。
实施例4
A、称取1g硅酸钛锂和1g十六烷基三甲基溴化铵,分散于蒸馏水中超声均匀,形成悬浮液;
B、往溶液中加入30ml乙醇、0.5g间苯二酚、5ml甲醛和5ml起催化作用的氨水搅拌均匀,制得混合物;
C、将混合物在室温下无干扰静置12h老化;
D、将所得产物离心、洗涤后,在60℃干燥12h后得到前驱体;
E、将所得前驱体在氮气气氛下1000℃煅烧5h,冷却后获得所述的碳包覆改性硅酸钛锂。
图7为碳包覆改性硅酸钛锂的透射电镜图,从图7a可以看出酚醛树脂碳化后在硅酸钛锂的表面形成了均匀包覆的碳层,从图7b中可以看出碳层厚度约为20nm。
Claims (10)
1.一种硅酸钛锂颗粒原位碳包覆方法,其特征在于,包括如下步骤:
步骤1、将硅酸钛锂分散在一定量水中,加入表面活性剂,搅拌或超声分散均匀,形成悬浮液;
步骤2、往悬浮液中依次加入乙醇、间苯二酚、甲醛和催化剂,搅拌均匀;
步骤3、将步骤2所得混合物在室温下无干扰静置老化;
步骤4、将步骤3所得产物离心、洗涤、干燥得到前驱物;
步骤5、将前驱物在惰性气氛下碳化,煅烧,冷却后得到所述的碳包覆硅酸钛锂材料。
2.根据权利要求1所述的硅酸钛锂颗粒原位碳包覆方法,其特征在于,步骤1中,所述表面活性剂为十六烷基三甲基溴化铵;所述硅酸钛锂与十六烷基三甲基溴化铵的质量比为1:0.5~1。
3.根据权利要求1所述的硅酸钛锂颗粒原位碳包覆方法,其特征在于,步骤2中,所述间苯二酚的加入量,按照硅酸钛锂与间苯二酚的质量比为1:0.2~0.5。
4.根据权利要求1所述的硅酸钛锂颗粒原位碳包覆方法,其特征在于,步骤2中,所述甲醛的加入量,按照硅酸钛锂与甲醛的质量比为1∶2~5。
5.根据权利要求1所述的硅酸钛锂颗粒原位碳包覆方法,其特征在于,步骤2中,所述催化剂为氨水;所述氨水的加入量,按照硅酸钛锂与氨水的质量比为1∶1~5。
6.根据权利要求1所述的硅酸钛锂颗粒原位碳包覆方法,其特征在于,步骤3中,所述无干扰静置老化的时间为6~12h。
7.根据权利要求1所述的硅酸钛锂颗粒原位碳包覆方法,其特征在于,步骤4中,所述干燥条件为60℃,干燥时间为6~12h。
8.根据权利要求1所述的硅酸钛锂颗粒原位碳包覆方法,其特征在于,步骤5中,所述惰性气氛为氩气或氮气气氛。
9.根据权利要求1所述的硅酸钛锂颗粒原位碳包覆方法,其特征在于,步骤5中,所述煅烧温度为700~1000℃,煅烧时间为2~5h。
10.一种采用权利要求1~9中任一项所述方法制备得到碳包覆改性硅酸钛锂复合物。
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CN103985876A (zh) * | 2014-05-15 | 2014-08-13 | 中国科学院化学研究所 | 利用酚醛树脂对锂离子电池电极材料进行原位可控包覆的方法 |
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