CN115548311A - 氟掺杂TiO2(B)/rGO复合材料及其制备方法和应用 - Google Patents
氟掺杂TiO2(B)/rGO复合材料及其制备方法和应用 Download PDFInfo
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- 239000011737 fluorine Substances 0.000 title claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims abstract description 14
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 12
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 12
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Abstract
本发明公开了一种氟掺杂TiO2(B)/rGO复合材料及其制备方法和应用,将氧化石墨烯加入醋酸溶液中,搅拌后加入乙醇酸、钛酸四丁酯和氟化铵,然后移入反应釜,于200℃下反应24h。得到的灰色沉淀,经乙醇和水分别洗涤离心后烘干;最后将灰色沉淀于400℃,升温速度2℃/min,N2气氛下煅烧2h后,得到F‑TiO2(B)/rGO。本发明的氟掺杂TiO2(B)/rGO复合材料用作锂电池负极,得到的锂电池具有很高的比容量和循环稳定性,在电流密度2 A/g时充放电500圈,容量稳定在202.3 mAh/g,表现出优异的倍率放电性能。即使在电流密度为5 A/g时其充放电容量也能稳定在191.7 mAh/g。
Description
技术领域
本发明属于锂电池负极材料技术领域,具体涉及一种氟掺杂TiO2(B)/rGO复合材料及其制备方法和应用。
背景技术
锂离子电池作为一种高效储能器件被广泛应用于人类生活和生存活动中。而随着3C产品的广泛普及和纯电动新能源汽车的推广,人们对电池在使用过程中的安全性和使用寿命提出了越来越高的要求。目前商业化使用的负极材料主要为石墨,其嵌锂电位低,在反复充放电过程中容易形成锂枝晶,刺穿隔膜而引发电池短路。同时石墨负极还存在倍率性能差,循环寿命短等问题。
TiO2由于其结构稳定、含量丰富、成本低、安全性高等特点,作负极材料为被应用于储能器件中。其中TiO2(B)具有三维通道,有利于Li+的传输。同时TiO2(B)的理论容量高达335 mAh/g,约为其他TiO2晶相的两倍。因此,TiO2(B)已成为锂离子电池中最有前途的钛基负极材料。
发明内容
本发明公开了一种氟掺杂TiO2(B)/rGO复合材料F-TiO2(B)/rGO,将其用作锂电池负极,得到的锂电池具有很高的比容量和循环稳定性。
为实现上述目的,本发明采用如下技术方案:
一种氟掺杂TiO2(B)/rGO复合材料的制备方法包括以下步骤:
(1)将0.04g氧化石墨烯加入20mL醋酸溶液中,搅拌均匀后加入2g乙醇酸、1.6mL钛酸四丁酯和0.174g氟化铵,搅拌均匀后,移入反应釜进行反应,得到的灰色沉淀经无水乙醇和水分别洗涤离心后烘干;
(2)将步骤(1)烘干后的灰色沉淀于400℃,升温速度2℃/min,N2气氛下煅烧2h后,得到F-TiO2(B)/rGO,即氟掺杂TiO2(B)/rGO复合材料。
进一步地,步骤(1)中反应条件为:在200℃下反应24h。
本发明的掺杂F的TiO2(B)在所有扩散路径上的能垒都低于纯TiO2(B),导致锂在所有扩散路径上都发生了大规模扩散。同时,在醋酸溶剂中,NH4F被分解提供F-,F-通过电子吸引优先与Ti4+结合,形成少量晶核,并生长成纳米棒,因此,F-会诱导形成TiO2(B)纳米棒,缩短了锂离子的传输距离,导致了优异的界面动力学。此外,氧化石墨烯的作用:i) TiO2(B)纳米棒均匀生长在还原氧化石墨烯纳米片表面,避免了纳米材料的过度聚集。ii) 氧化石墨烯纳米片形成了导电网络,增强了材料的导电性。
本发明还公开了上述氟掺杂TiO2(B)/rGO复合材料的制备方法在锂电池负极材料中的应用:锂离子电池组装:按质量比F-TiO2(B)/rGO:乙炔黑:PVDF=7:2:1混合研磨后均匀地涂在铜箔上做负极,参比电极和对电极均为金属锂,电解质由1M LiPF6的EC+EMC+DMC(EC/EMC/DMC =1/1/1 vol%)。所有组装均在手套箱里进行。
本发明的优点:本发明的制备方法简单,成本廉价,重现性好,性能优异,将氟掺杂TiO2(B)/rGO复合材料用作锂离子电池负极材料时,在电流密度0.2 A/g时充放电100圈,容量稳定在249.4 mAh/g。同时表现出优异的倍率放电性能,即使在电流密度为5 A/g时其充放电容量也能稳定在191.7 mAh/g。
附图说明
图1为实施例1的氟掺杂TiO2(B)/rGO复合材料的XRD、扫描电镜与透射电镜分析图;
图2为实施例1的氟掺杂TiO2(B)/rGO复合材料的的电化学性能图;
图3为对比例1的氟掺杂TiO2(B)材料的的电化学性能图;
图4为对比例2的TiO2(B)材料的的电化学性能图;
图5为对比例2的TiO2(B)材料的扫描电镜图。
具体实施方式
为了使本发明所述的内容更加便于理解,下面结合具体实施方式对本发明所述的技术方案做进一步的说明,但是本发明不仅限于此。
实施例1
一种氟掺杂TiO2(B)/rGO复合材料的制备方法包括以下步骤:
(1)将0.04g氧化石墨烯加入20mL醋酸溶液中,搅拌均匀后加入2g乙醇酸、1.6mL钛酸四丁酯和0.174g氟化铵,搅拌均匀后,移入反应釜,在200℃下反应24h,得到的灰色沉淀经无水乙醇和水分别洗涤离心后烘干;
(2)将步骤(1)烘干后的灰色沉淀于400℃,升温速度2℃/min,N2气氛下煅烧2h后,得到F-TiO2(B)/rGO,即氟掺杂TiO2(B)/rGO复合材料。
上述氟掺杂TiO2(B)/rGO复合材料的制备方法在锂电池负极材料中的应用:锂离子电池组装:按质量比F-TiO2(B)/rGO:乙炔黑:PVDF=7:2:1混合研磨后均匀地涂在铜箔上做负极,参比电极和对电极均为金属锂,电解质由1M LiPF6的EC+EMC+DMC (EC/EMC/DMC =1/1/1 vol%)。所有组装均在手套箱里进行。
对比例1
一种氟掺杂TiO2(B)材料的制备方法包括以下步骤:
(1)将0.04g氧化石墨烯加入20mL醋酸溶液中,搅拌均匀后加入2g乙醇酸、1.6mL钛酸四丁酯,搅拌均匀后,移入反应釜,在200℃下反应24h,得到的灰色沉淀经无水乙醇和水分别洗涤离心后烘干;
(2)将步骤(1)烘干后的灰色沉淀于400℃,升温速度2℃/min,N2气氛下煅烧2h后,得到F-TiO2(B),即氟掺杂TiO2(B)材料。
对比例2
一种TiO2(B)材料的制备方法包括以下步骤:
(1)在20mL醋酸溶液中加入2g乙醇酸、1.6mL钛酸四丁酯,搅拌均匀后,移入反应釜,在200℃下反应24h,得到的灰色沉淀经无水乙醇和水分别洗涤离心后烘干;
(2)将步骤(1)烘干后的灰色沉淀于400℃,升温速度2℃/min,N2气氛下煅烧2h后,得到TiO2(B),即TiO2(B)材料。图5为对比例2的TiO2(B)材料的扫描电镜图,没有进行F掺杂,其形貌为堆积的块状结构。
图1为实施例1的氟掺杂TiO2(B)/rGO复合材料的XRD、扫描电镜与透射电镜分析图。从XRD图中看出,所得样品的衍射峰与TiO2(B)标准峰位(JCPDS 46-1238)相吻合,说明制备的TiO2(B)是纯相。从SEM图中看出,样品是由纳米片堆积而成的网状结构。TiO2(B)纳米棒均匀地分散在还原氧化石墨烯纳米片的表面。从TEM图中看出,TiO2(B)纳米棒的晶格条纹清晰可见,说明TiO2(B)纳米棒具有较高的结晶度,其值分别为0.62和0.31 nm,分别对应于TiO2(B) 的(001)和(002)晶面。
图2为氟掺杂TiO2(B)/rGO复合材料的的电化学性能图,在电流密度0.2 A/g时充放电100圈,容量稳定在249.4 mAh/g,表现出优异的倍率放电性能。即使在电流密度为5 A/g时其充放电容量也能稳定在191.7 mAh/g。
图3为氟掺杂TiO2(B)材料的的电化学性能图,在电流密度0.2 A/g时充放电100圈,容量稳定在198.9 mAh/g。在电流密度为5 A/g时其充放电容量也能稳定在155.1 mAh/g。
图4为TiO2(B)材料的的电化学性能图,在电流密度0.2 A/g时充放电100圈,容量稳定在168.9mAh/g。在电流密度为5 A/g时其充放电容量也能稳定在131.2 mAh/g。
以上所述仅为本发明的较佳实施例,凡依本发明申请专利范围所做的均等变化与修饰,皆应属本发明的涵盖范围。
Claims (5)
1.一种氟掺杂TiO2(B)/rGO复合材料的制备方法,其特征在于:包括以下步骤:
(1)将氧化石墨烯加入醋酸溶液中,搅拌均匀后加入乙醇酸、钛酸四丁酯和氟化铵,搅拌均匀后,移入反应釜进行反应,得到的灰色沉淀经无水乙醇和水分别洗涤离心后烘干;
(2)将步骤(1)烘干后的灰色沉淀于400℃,升温速度2℃/min,N2气氛下煅烧2h后,得到F-TiO2(B)/rGO,即氟掺杂TiO2(B)/rGO复合材料。
2.根据权利要求1所述的氟掺杂TiO2(B)/rGO复合材料的制备方法,其特征在于:步骤(1)中所述氧化石墨烯的质量为0.04g,乙醇酸的质量为2g,钛酸四丁酯的体积为1.6mL,氟化铵的质量为0.174g。
3.根据权利要求1所述的氟掺杂TiO2(B)/rGO复合材料的制备方法,其特征在于:步骤(1)中反应条件为:在200℃下反应24h。
4.一种如权利要求1-3任一项所述的制备方法制得的氟掺杂TiO2(B)/rGO复合材料。
5.一种如权利要求4所述的氟掺杂TiO2(B)/rGO复合材料在锂电池负极中的应用,其特征在于:按质量比氟掺杂TiO2(B)/rGO复合材料:乙炔黑:PVDF=7:2:1混合研磨后均匀地涂在铜箔上做锂电池负极。
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