CN108341667B - 一种纳米立方体铁电材料的制备方法 - Google Patents
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Abstract
本发明属于铁电多功能材料领域,一种纳米立方体铁电材料的制备方法,包括两步水热反应过程:(1)在低温条件下形成BNT‑Er/Yb晶核,再在高温超临界条件下制备纳米籽晶Na0.5Bi0.5‑x(Er/Yb)xTiO3(BNT‑Er/Yb);(2)在中温超临界条件下自组装制备纳米立方体铁电材料Na0.5Bi0.5‑x(Er/Yb)xTiO3(BNT‑Er/Yb),式中Er与Yb的原子数量比为1/1‑1/10,其中x=0‑0.05。通过两步水热反应自组装制备纳米立方体铁电材料,避免了传统固相法的高温煅烧,得到纳米立方体铁电材料,呈现增强的荧光和热释电性能,有望在LED照明、红外气体传感器等领域应用。
Description
技术领域
本发明属于铁电多功能材料领域,尤其涉及一种纳米立方体铁电材料的制备方法。
背景技术
稀土元素内层的4f电子容易被激发,能够在4f电子层内或f-d电子层之间发生跃迁,产生从紫外到红外不同波段的吸收和发射荧光光谱。其中稀土元素Er具有丰富的能级结构、能级分布均匀、激发态能级寿命长,Yb经常作为提高上转换发光效率的敏化剂,Er3+/Yb3+共掺杂有望诱导增强的荧光和热释电性能。
钛酸铋钠基无铅压电陶瓷具有优异的电、声、光学性能,具有较低的声子能量,与玻璃态物质相比具有较高的稳定性和机械强度。钛酸铋钠陶瓷有着较强的铁电性能(Pr=38μC/cm2,Ec=73kV/cm),剩余极化较大,能够有效提高稀土离子的光致发光性能,是良好的稀土离子上转换发光基质。
稀土掺杂能够改善铁电陶瓷的电学性能,同时,铁电陶瓷的剩余极化能够诱导增强稀土荧光发射强度。
传统的稀土掺杂荧光粉都是通过高温固相法制备,该方法操作简便,易于工业化应用,但是产物形貌不规则,粒径不均匀,易生成杂相,影响荧光粉的发光性能。与之相对,水热法反应温度低,属于稀薄相生长,有利于快速传质和反应完全,容易制备高纯度的荧光粉;同时,水热合成能够进行原子量级的掺杂,其反应条件易于调节。
发明内容
为解决现有技术存在的固相法产物形貌不规则的缺陷,本发明提供一种纳米立方体铁电材料的制备方法。
为解决上述技术问题,本发明所采用的方案为:一种纳米立方体铁电材料的制备方法,包括两步水热反应过程:
(1)在低温条件下形成BNT-Er/Yb晶核,再在高温超临界条件下制备纳米籽晶Na0.5Bi0.5-x(Er/Yb)xTiO3(BNT-Er/Yb);
(2)在中温超临界条件下自组装制备纳米立方体铁电材料Na0.5Bi0.5-x(Er/Yb)xTiO3(BNT-Er/Yb),式中Er与Yb的原子数量比为1/1-1/10,其中x=0-0.05。
具体地,步骤(1)具体步骤为:按照化学计量比称量NaAc·3H2O、Bi(NO3)3·5H2O、Bi2O3、钛酸正丁酯、TiO2、Er2O3、Yb2O3,放入水热釜中添加去离子水配制成混合液,填充率小于75%,加入十六烷基三甲基溴化铵,加入NaOH形成过饱和溶液,先在120℃水热反应0.5h,诱导形成BNT-Er/Yb晶核;随后升温至240℃水热反应8h,得到BNT-Er/Yb纳米籽晶。
进一步地,所述Bi(NO3)3·5H2O与Bi2O3的摩尔比为1:40-50;所述钛酸正丁酯与TiO2的摩尔比为1:40-50。
具体地,步骤(2)具体步骤为:将步骤(1)得到的含有BNT-Er/Yb纳米籽晶的混合液调节NaOH浓度为6M,加入司本-80和EDTA,在160℃水热反应24h,得到纳米立方体铁电材料BNT-Er/Yb。
作为优先,步骤(1)和(2)中水热反应升降温条件为:升温速率为10℃/min,水热反应结束后降温速率为20℃/min。
有益效果:本发明反应温度低,属于稀薄相生长,有利于快速传质和反应完全,容易制备高纯度的荧光粉;同时,水热合成能够进行原子量级的掺杂,其反应条件易于调节,且通过反应条件的调控、引入籽晶、添加添加剂等可以控制荧光材料的晶体结构和形态,以获得增强的荧光性能。
本发明通过两步水热反应过程自组装制备纳米立方体铁电材料,避免了传统固相法的高温煅烧,得到纳米立方体铁电材料,呈现增强的荧光和热释电性能,有望在LED照明、红外气体传感器等领域获得应用。
附图说明
为了对本发明作更详细的描述,现结合实施例与图简介如下:
图1水热法制备的BNT-Er/Yb的XRD图;
图2水热法制备的Na0.5Bi0.5-x(Er/Yb)xTiO3(Er/Yb=1/1,x=0.02)的SEM图;
图3水热法制备的BNT-Er/Yb的发射光谱。
具体实施方式
实施例1
按照化学式Na0.5Bi0.5-x(Er/Yb)xTiO3(Er/Yb=1/1,x=0.02)称量计量比的NaAc·3H2O、Bi(NO3)3·5H2O、Bi2O3(Bi(NO3)3·5H2O/Bi2O3=1/40,摩尔比)、钛酸正丁酯、TiO2(钛酸正丁酯/TiO2=1/40,摩尔比,取决于Yb含量)、Er2O3、Yb2O3,放入水热釜中添加去离子水配制成混合液,填充率小于75%,目标产物BNT-Er/Yb的质量为2g。加入十六烷基三甲基溴化铵2.5mg,加入NaOH使其形成16M过饱和溶液,先在120℃水热反应0.5h,随后升温至240℃水热反应8h。
将上述混合液调节NaOH浓度为6M,加入司本-80 60mg、EDTA100mg,在160℃水热反应24h,得到纳米立方体铁电材料Na0.5Bi0.5-x(Er/Yb)xTiO3(Er/Yb=1/1,x=0.02)BNT-Er/Yb。
上述水热反应过程升温速率都为10℃/min,水热反应结束后降温速率都为20℃/min。
实施例2
按照化学式Na0.5Bi0.5-x(Er/Yb)xTiO3(Er/Yb=1/3,x=0.03)称量计量比的NaAc·3H2O、Bi(NO3)3·5H2O、Bi2O3(Bi(NO3)3·5H2O/Bi2O3=1/42,摩尔比)、钛酸正丁酯、TiO2(钛酸正丁酯/TiO2=1/30,摩尔比)、Er2O3、Yb2O3,放入水热釜中添加去离子水配制成混合液,填充率小于75%,目标产物BNT-Er/Yb的质量为2g。加入十六烷基三甲基溴化铵2.5mg,加入NaOH使其形成16M过饱和溶液,先在120℃水热反应0.5h,随后升温至240℃水热反应8h。
将上述混合液调节NaOH浓度为6M,加入司本-80 60mg、EDTA100mg,在160℃水热反应24h,得到纳米立方体铁电材料Na0.5Bi0.5-x(Er/Yb)xTiO3(Er/Yb=1/3,x=0.03)BNT-Er/Yb。
上述水热反应过程升温速率都为10℃/min,水热反应结束后降温速率都为20℃/min。
实施例3
按照化学式Na0.5Bi0.5-x(Er/Yb)xTiO3(Er/Yb=1/5,x=0.04)称量计量比的NaAc·3H2O、Bi(NO3)3·5H2O、Bi2O3(Bi(NO3)3·5H2O/Bi2O3=1/45,摩尔比)、钛酸正丁酯、TiO2(钛酸正丁酯/TiO2=1/25,摩尔比)、Er2O3、Yb2O3,放入水热釜中添加去离子水配制成混合液,填充率小于75%,目标产物BNT-Er/Yb的质量为2g。加入十六烷基三甲基溴化铵2.5mg,加入NaOH使其形成16M过饱和溶液,先在120℃水热反应0.5h,随后升温至240℃水热反应8h。
将上述混合液调节NaOH浓度为6M,加入司本-80 60mg、EDTA100mg,在160℃水热反应24h,得到纳米立方体铁电材料Na0.5Bi0.5-x(Er/Yb)xTiO3(Er/Yb=1/5,x=0.04)BNT-Er/Yb。
上述水热反应过程升温速率都为10℃/min,水热反应结束后降温速率都为20℃/min。
实施例4
按照化学式Na0.5Bi0.5-x(Er/Yb)xTiO3(Er/Yb=1/7,x=0.05)称量计量比的NaAc·3H2O、Bi(NO3)3·5H2O、Bi2O3(Bi(NO3)3·5H2O/Bi2O3=1/50,摩尔比)、钛酸正丁酯、TiO2(钛酸正丁酯/TiO2=1/4220,摩尔比)、Er2O3、Yb2O3,放入水热釜中添加去离子水配制成混合液,填充率小于75%,目标产物BNT-Er/Yb的质量为2g。加入十六烷基三甲基溴化铵2.5mg,加入NaOH使其形成16M过饱和溶液,先在120℃水热反应0.5h,随后升温至240℃水热反应8h。
将上述混合液调节NaOH浓度为6M,加入司本-80 60mg、EDTA100mg,在160℃水热反应24h,得到纳米立方体铁电材料Na0.5Bi0.5-x(Er/Yb)xTiO3(Er/Yb=1/7,x=0.05)BNT-Er/Yb。
上述水热反应过程升温速率都为10℃/min,水热反应结束后降温速率都为20℃/min。
图1是实施例1~4水热法制备的BNT-Er/Yb的XRD图,呈现较纯的三方钙钛矿结构。
图2是实施例1水热法制备的Na0.5Bi0.5-x(Er/Yb)xTiO3(Er/Yb=1/1,x=0.02)的SEM图(实施例2~4产物SEM图基本与实施例1相同),纳米立方体结构有利于增强荧光和热释电性能。
图3是实施例1~4水热法制备的BNT-Er/Yb的荧光发射光谱,在530nm、550nm、660nm和735nm处出现发射峰,分别对应于2H11/2,4S3/2,4F9/2和4I9/2能级到4I15/2能级的跃迁,在绿色光区的550nm的发射峰最强,在红色光区的660nm和735nm的发射峰较弱。水热法制备的纳米立方体铁电材料BNT-Er/Yb呈现增强的荧光和热释电性能,有望在LED照明、红外气体传感器等领域获得应用。
对比例1
按照化学计量比称量NaAc·3H2O、Bi(NO3)3·5H2O、Bi2O3(Bi(NO3)3·5H2O/Bi2O3=1/40,摩尔比)、钛酸正丁酯、二氧化钛(钛酸正丁酯/TiO2=1/40,摩尔比)、Er2O3、Yb2O3,放入水热釜中搅拌均匀配制成水溶液,并向其中加入NaOH、加入司本-80 60mg、EDTA100mg,其中NaOH浓度为12M,在200℃水热反应24h,得到Na0.5Bi0.5-x(Er/Yb)xTiO3(Er/Yb=1/1,x=0.02)BNT-Er/Yb。上述水热反应过程升温速率都为10℃/min,水热反应结束后降温速率都为20℃/min。
经XRD测定,产物存在一定的杂相,产物形貌不均匀。
对比例2
将实施例1步骤(1)中Bi2O3替换成等量的Bi(NO3)3·5H2O(以Bi摩尔量计),其他条件同实施例1。最终制得产物Na0.5Bi0.5-x(Er/Yb)xTiO3(Er/Yb=1/1,x=0.02)BNT-Er/Yb。经测定产物存在杂相,产物形貌不均匀。
对比例3
将实施例1步骤(1)中TiO2替换成等量的钛酸正丁酯(以Ti摩尔量计),其他条件同实施例1,最终制得产物Na0.5Bi0.5-x(Er/Yb)xTiO3(Er/Yb=1/1,x=0.02)BNT-Er/Yb。经测定产物存在杂相,产物形貌不均匀。
对比例4
将实施例1步骤(2)中司本-80及EDTA替换成等量的聚丙烯酰胺,其他条件同实施例1,最终得到产物纳米立方栅栏Na0.5Bi0.5-x(Er/Yb)xTiO3(Er/Yb=1/1,x=0.02)BNT-Er/Yb,产物形貌与实施例1中完全不同。
对比例5
将实施例1中钛酸正丁酯与TiO2摩尔比替换为1/20,其他条件同实施例1,最终得到产品,经XRD检测发现,产物中存在一定的杂相,导致荧光和热释电性能降低。
对比例6
将实施例4中钛酸正丁酯与TiO2摩尔比替换为1/40,其他条件同实施例4,最终得到产品,经XRD检测发现,产物中存在一定的杂相,导致荧光和热释电性能降低。
从实施例1、4、对比例5和6可以说明,证明Yb含量越高,需要提高钛酸正丁酯/TiO2的比例增大,即钛酸正丁酯的量相应增多,才能保证产物的晶相纯度,反之则产品晶相纯度降低。
Claims (2)
1.一种纳米立方体铁电材料的制备方法,其特征在于:包括两步水热反应过程:
(1)在低温条件下形成BNT-Er/Yb晶核,再在高温条件下制备纳米籽晶Na0.5Bi0.5-x(Er/Yb)xTiO3(BNT-Er/Yb);
(2)在中温条件下自组装制备纳米立方体铁电材料Na0.5Bi0.5-x(Er/Yb)xTiO3(BNT-Er/Yb),式中Er与Yb的原子数量比为1/1-1/10,其中x=0-0.05;
步骤(1)具体步骤为:按照化学计量比称量NaAc·3H2O、Bi(NO3)3·5H2O、Bi2O3、钛酸正丁酯、TiO2、Er2O3、Yb2O3,放入水热釜中添加去离子水配制成混合液,填充率小于75%,加入十六烷基三甲基溴化铵,加入NaOH形成过饱和溶液,先在120℃水热反应0.5h,诱导形成BNT-Er/Yb晶核;随后升温至240℃水热反应8h,得到BNT-Er/Yb纳米籽晶;
所述Bi(NO3)3·5H2O与Bi2O3的摩尔比为1:40-50;所述钛酸正丁酯与TiO2的摩尔比为1:40-50;
步骤(2)具体步骤为:将步骤(1)得到的含有BNT-Er/Yb纳米籽晶的混合液调节NaOH浓度为6M,加入司本-80和EDTA,在160℃水热反应24h,得到纳米立方体铁电材料BNT-Er/Yb。
2.如权利要求1所述的一种纳米立方体铁电材料的制备方法,其特征在于,步骤(1)和(2)中水热反应升降温条件为:升温速率为10℃/min,水热反应结束后降温速率为20℃/min。
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