CN112501717A - 一种LaAlO3纳米纤维的制备方法及其产品和应用 - Google Patents
一种LaAlO3纳米纤维的制备方法及其产品和应用 Download PDFInfo
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Abstract
本发明公开了一种纳米纤维的制备方法,包括以下步骤:a、将0.1458~0.4374份硝酸镧和0.1263~0.3789份硝酸铝溶解在5~15份N,N‑二甲基甲酰胺中,再加入0.825~2.475份聚乙烯吡咯烷酮,获得静电纺丝前驱体溶液;b、静电纺丝法制备La(NO3)2/Al(NO3)3/PVP前驱体纤维;c、烘干并在730~850℃烧结,得到LaAlO3纳米纤维。本发明还公开了所得LaAlO3纳米纤维以及其在超级电容器电极中应用。本发明所制得的LaAlO3纳米纤维粗细均匀且连续,直径为50~80nm,纤维尺寸大大缩小,增大了比表面积,有利于提升LaAlO3纤维材料的电化学性能。
Description
技术领域
本发明涉及纤维制法及应用,具体为一种LaAlO3纳米纤维的制备方法及其产品和应用。
背景技术
随着地球环境的日益恶化以及人类对能源需求的不断增加,人们对高性能化学动力源的需求也变得越来越迫切。超级电容器是一种介于充电电池与传统电容器之间的高性能电化学储能设备,它有着容量大、能量密度高、使用寿命长等诸多优点。LaAlO3是一种典型的钙钛矿结构材料,具有介电常数小,化学稳定性好,能隙宽,比表面积大,热稳定性好等诸多优点,所以被广泛应用于电子器件、催化、污水处理等领域,作为一种潜在的超级电容器电极材料目前对其电化学性能的研究鲜有发表。并且,现有的制备工艺还存在制备时间长、合成温度高、对能源消耗大、对人体和环境不友好等诸多缺点。。
发明内容
发明目的:为了克服现有技术中存在的不足,本发明的目的是提供一种简单方便、热处理温度适中、所用原料对人体对环境危害均较低的LaAlO3纳米纤维的制备方法,本发明的另一目的是提供一种比容量高、循环稳定性好的LaAlO3纳米纤维,本发明的再一目的是提供一种LaAlO3纳米纤维在超级电容器电极中的应用。
技术方案:本发明所述的一种LaAlO3纳米纤维的制备方法,包括以下步骤:
a、将0.1458~0.4374份硝酸镧和0.1263~0.3789份硝酸铝溶解在5~15份N,N-二甲基甲酰胺(DMF)中,再向其中加入0.825~2.475份聚乙烯吡咯烷酮(PVP),获得静电纺丝前驱体溶液;PVP用于增加液体的导电性,使其在高压电场力的作用下能够被拉成丝;
b、通过静电纺丝法制备La(NO3)2/Al(NO3)3/PVP前驱体纤维;
c、将所得纤维烘干并在730~850℃烧结,降温后得到LaAlO3纳米纤维。
步骤b中,静电纺丝的电压为10~30kV,溶液注射速度为0.1~0.6ml/h。静电纺丝的收丝筒转速为80~300r/min,接收距离为5~25cm。静电纺丝的温度为0~40℃。
步骤c中的烘干温度为50~120℃,烘干时间为2~24h。升温速率为0.5~5℃/min,烧结温度为700~850℃,烧结时间为2~4h,降温速率为0.5~5℃/min。
当原料的配比确定时,若PVP的重量份数不在0.825~2.475份的区间内,则无法成功制得LaAlO3纳米纤维。
上述LaAlO3纳米纤维的制备方法所制得的LaAlO3纳米纤维,直径为50~80nm,连续且粗细均匀。
LaAlO3纳米纤维能够在超级电容器电极中应用,LaAlO3纳米纤维制备成超级电容器电极后,具有比容量可达140F/g,循环次数可达10000次。
制备原理:La(NO3)3+Al(NO3)3+O2→LaAlO3+NO2+NO。
静电纺丝法是一种特殊的制备工艺,溶液在高压电场力的作用下被拉成纤维状的细丝,利用静电纺丝法制备出的纳米纤维其直径可以达到纳米级,使之比表面积远大于传统制备方法制备出的材料,同时静电纺丝法制备出的纤维材料由于其特殊的结构不仅增大材料的比表面积,还提高了电子的传输效率,从而可以提高材料的电化学性能。
有益效果:本发明和现有技术相比,具有如下显著性特点:
1、所制得的LaAlO3纳米纤维粗细均匀且连续,直径为50~80nm,根据纳米效应,纤维尺寸大大缩小,增大了比表面积,有利于提升LaAlO3纤维材料的电化学性能;
2、由于LaAlO3纳米纤维具有特殊的一维线性结构,不仅增大材料的比表面积,还提高了电子的传输效率,从而可以提高材料的电化学性能;
3、将该材料应用于超级电容器电极材料时,具有比容量高、循环稳定性好以及使用寿命较长等诸多优点;
4、LaAlO3纤维的制备方法简单方便,热处理温度适中,所用原料对人体对环境危害均较低。
附图说明
图1是本发明实施例1的LaAlO3纳米纤维的XRD图;
图2是本发明实施例1的LaAlO3纳米纤维的SEM图;
图3是本发明实施例1的LaAlO3纳米纤维的循环伏安曲线图;
图4是本发明实施例1的LaAlO3纳米纤维的充放电图;
图5是本发明实施例1的LaAlO3纳米纤维的长循环图;
图6是本发明对比例1的LaCoO3纳米纤维的充放电图;
图7是本发明对比例2的LaAlO3纳米纤维的充放电图。
具体实施方式
以下各实施例中,硝酸镧的纯度为99.9%,硝酸铝的纯度为99%,DMF的纯度为99%,PVP的平均分子量为1300000。PVP的平均分子量对能否纺成纤维有很大影响,如果改变则无法纺出纤维。
实施例1
一种用于超级电容器的LaAlO3纳米纤维的制备方法,包含以下步骤:
a、0.2916g硝酸镧和0.2526g硝酸铝依次溶解在10g DMF中,再向其中加入1.65gPVP,从而得到静电纺丝所需纺丝液;
b、通过静电纺丝法制备La(NO3)2/Al(NO3)3/PVP前驱体纤维,电压为18kV,溶液注射速度为0.5ml/h,收丝筒转速为100r/min,接收距离为20cm,静电纺丝的温度为25℃;
c、将所得La(NO3)2/Al(NO3)3/PVP前驱体纤维在80℃烘干12h后,在箱式电阻炉中,以5℃/min的升温速率升温到750℃进行烧结2h,再以1℃/min的降温速率冷却,得到LaAlO3纳米纤维。
将实施例1所制得的LaAlO3纳米纤维进行XRD检测、微观形貌和性能分析。由图1可以看出,所有的峰都可以根据LaAlO3的JCPDS卡进行索引(PDF#31-0022),即该样品为单一的LaAlO3。LaAlO3纳米纤维的扫描电子显微镜图如图2所示,结果表明,合成的样品为纳米级,呈明显纤维状结构,纤维直径为50-80nm。LaAlO3纳米纤维的循环伏安曲线图如图3所示,在10mV和100mV的扫面速率下,图形没有明显的变化,表明具有良好的倍率性能。LaAlO3纳米纤维的充放电图如图4所示,可以看出将LaAlO3纳米纤维制备成电极后有着较高的比电容,比电容经计算可达140F/g。LaAlO3纳米纤维的长循环图如图5所示,可以看出将LaAlO3纳米纤维制备成电极后有着良好的循环性能,循环次数可达10000圈。
实施例2
一种用于超级电容器的LaAlO3纳米纤维的制备方法,包含以下步骤:
a、0.1458g硝酸镧和0.1263g硝酸铝依次溶解在5g DMF中,再向其中加入0.825gPVP,从而得到静电纺丝所需纺丝液;
b、通过静电纺丝法制备La(NO3)2/Al(NO3)3/PVP前驱体纤维,电压为10kV,溶液注射速度为0.1ml/h,收丝筒转速为80r/min,接收距离为5cm,静电纺丝的温度为0℃;
c、将所得La(NO3)2/Al(NO3)3/PVP前驱体纤维在50℃烘干2h后,在箱式电阻炉中中,以0.5℃/min的升温速率升温到700℃进行烧结2h,再以0.5℃/min的降温速率冷却,得到LaAlO3纳米纤维。
实施例3
一种用于超级电容器的LaAlO3纳米纤维的制备方法,包含以下步骤:
a、0.4374g硝酸镧和0.3789g硝酸铝依次溶解在15g DMF中,再向其中加入2.475gPVP,从而得到静电纺丝所需纺丝液;
b、通过静电纺丝法制备La(NO3)2/Al(NO3)3/PVP前驱体纤维,电压为30kV,溶液注射速度为0.6ml/h,收丝筒转速为300r/min,接收距离为25cm,静电纺丝的温度为40℃;
c、将所得La(NO3)2/Al(NO3)3/PVP前驱体纤维在120℃烘干24h后,在箱式电阻炉中中,以5℃/min的升温速率升温到850℃进行烧结4h,再以5℃/min的降温速率冷却,得到LaAlO3纳米纤维。
实施例4
一种用于超级电容器的LaAlO3纳米纤维的制备方法,包含以下步骤:
a、0.2187g硝酸镧和0.18945g硝酸铝依次溶解在7.5g DMF中,再向其中加入1.2375g PVP,从而得到静电纺丝所需纺丝液;
b、通过静电纺丝法制备La(NO3)2/Al(NO3)3/PVP前驱体纤维,电压为20kV,溶液注射速度为0.2ml/h,收丝筒转速为150r/min,接收距离为18cm,静电纺丝的温度为10℃;
c、将所得La(NO3)2/Al(NO3)3/PVP前驱体纤维在100℃烘干12h后,在箱式电阻炉中中,以2℃/min的升温速率升温到800℃进行烧结3h,再以2℃/min的降温速率冷却,得到LaAlO3纳米纤维。
实施例5
一种用于超级电容器的LaAlO3纳米纤维的制备方法,包含以下步骤:
a、0.3645g硝酸镧和0.31575g硝酸铝依次溶解在12.5g DMF中,再向其中加入2.0625g PVP,从而得到静电纺丝所需纺丝液;
b、通过静电纺丝法制备La(NO3)2/Al(NO3)3/PVP前驱体纤维,电压为25kV,溶液注射速度为0.4ml/h,收丝筒转速为200r/min,接收距离为15cm,静电纺丝的温度为15℃;
c、将所得La(NO3)2/Al(NO3)3/PVP前驱体纤维在90℃烘干8h后,在箱式电阻炉中中,以3℃/min的升温速率升温到780℃进行烧结2.5h,再以3℃/min的降温速率冷却,得到LaAlO3纳米纤维。
对比例1
一种LaCoO3纳米纤维的制备方法,包括以下步骤:
a、0.8747g硝酸镧和0.5879g硝酸钴依次溶解在10g DMF中,再向其中加入1g PVP,从而得到静电纺丝所需纺丝液;
b、通过静电纺丝法制备La(NO3)2/Co(NO3)3/PVP前驱体纤维,电压为15kV,溶液注射速度为0.5ml/h,收丝筒转速为100r/min,接收距离为20cm,静电纺丝的温度为25℃;
c、将所得La(NO3)2/Al(NO3)3/PVP前驱体纤维在80℃烘干12h后,在箱式电阻炉中,以5℃/min的升温速率升温到700℃进行烧结2h,再以1℃/min的降温速率冷却,得到LaAlO3纳米纤维。
图6是本对比例所制得的LaCoO3纳米纤维的充放电图,将其与实施例1中的LaAlO3纳米纤维进行比较,可以看出,实施例1所制得的LaAlO3纳米纤维的比容量更大。
对比例2
a、0.2916g硝酸镧和0.2526g硝酸铝依次溶解在10g DMF中,再向其中加入2g PVP,从而得到静电纺丝所需纺丝液;
b、通过静电纺丝法制备La(NO3)2/Al(NO3)3/PVP前驱体纤维,电压为18kV,溶液注射速度为0.5ml/h,收丝筒转速为100r/min,接收距离为20cm,静电纺丝的温度为25℃;
c、将所得La(NO3)2/Al(NO3)3/PVP前驱体纤维在80℃烘干12h后,在箱式电阻炉中,以5℃/min的升温速率升温到750℃进行烧结2h,再以1℃/min的降温速率冷却,得到LaAlO3纳米纤维。
图7是本对比例所制得的LaAlO3纳米纤维的充放电图,经计算可以得出比容量仅剩70F/g,将其与实施例1中的LaAlO3纳米纤维进行比较,可以看出增加PVP的量会对材料的电化学性能造成不利的影响。
Claims (9)
1.一种LaAlO3纳米纤维的制备方法,其特征在于,包括以下步骤:
(a)将0.1458~0.4374份硝酸镧和0.1263~0.3789份硝酸铝溶解在5~15份N,N-二甲基甲酰胺中,再向其中加入0.825~2.475份聚乙烯吡咯烷酮,获得静电纺丝前驱体溶液;
(b)通过静电纺丝法制备La(NO3)2/Al(NO3)3/PVP前驱体纤维;
(c)将所得纤维烘干并在730~850℃烧结,降温后得到LaAlO3纳米纤维。
2.根据权利要求1所述的一种LaAlO3纳米纤维的制备方法,其特征在于:所述步骤(b)中,静电纺丝的电压为10~30kV,溶液注射速度为0.1~0.6ml/h。
3.根据权利要求1所述的一种LaAlO3纳米纤维的制备方法,其特征在于:所述步骤(b)中,静电纺丝的收丝筒转速为80~300r/min,接收距离为5~25cm。
4.根据权利要求1所述的一种LaAlO3纳米纤维的制备方法,其特征在于:所述步骤(b)中静电纺丝的温度为0~40℃。
5.根据权利要求1所述的一种LaAlO3纳米纤维的制备方法,其特征在于:所述步骤(c)中的烘干温度为50~120℃,烘干时间为2~24h。
6.根据权利要求1所述的一种LaAlO3纳米纤维的制备方法,其特征在于:所述步骤(c)中的升温速率为0.5~5℃/min,烧结温度为700~850℃,烧结时间为2~4h,降温速率为0.5~5℃/min。
7.根据权利要求1~6任一所述的一种LaAlO3纳米纤维的制备方法所制得的LaAlO3纳米纤维。
8.根据权利要求7所述的LaAlO3纳米纤维,其特征在于:直径为50~80nm。
9.根据权利要求7所述的LaAlO3纳米纤维在超级电容器电极中的应用。
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