CN109023313A - 一种提高BiFeO3薄膜磁电耦合效应的退火方法 - Google Patents

一种提高BiFeO3薄膜磁电耦合效应的退火方法 Download PDF

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CN109023313A
CN109023313A CN201811097686.5A CN201811097686A CN109023313A CN 109023313 A CN109023313 A CN 109023313A CN 201811097686 A CN201811097686 A CN 201811097686A CN 109023313 A CN109023313 A CN 109023313A
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张丰庆
王玲续
郭晓东
刘慧莹
范素华
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Abstract

本发明公开了一种提高BiFeO3薄膜磁电耦合效应的退火方法。以化学溶液沉积法结合层层退火工艺，以ITO/glass为基体制备BiFeO3薄膜，薄膜的奇数层采用低温退火，偶数层采用高温退火。利用高低温退火相结合的方式一方面可以保证偶数层可以形成较大的晶粒，增强铁电性能，另外一方面可以保证奇数层的晶粒粒径小于62nm，有利用薄膜磁性的提高。利用这种退火方式提高了BiFeO3薄膜的磁电耦合效应。

Description

一种提高BiFeO3薄膜磁电耦合效应的退火方法
技术领域
本发明涉及电子信息材料领域，尤其涉及一种提高BiFeO3薄膜磁电耦合效应的退火方法。
背景技术
BiFeO3是一种集铁电性和磁性于一体的单相多铁材料，室温下具有铁电有序和反铁磁有序，且铁电性和磁性之间存在耦合效应。BiFeO3的铁电性源于其晶体结构，室温下的BiFeO3属于R3c空间群，为三方扭曲的菱方钙钛矿结构，其晶体结构在立方结构基础上沿[111]方向拉伸，使铁氧八面体（FeO6）以[111]轴为中心发生扭曲，从而在该方向出现一定程度的自发极化，其理论剩余极化强度可达100μC/cm2以上。BFO的磁性来源于过渡金属Fe3 +，其相邻的两个(111)面内磁矩的反向平行造成G型反铁磁有序，但该结构在长程调制作用下表现为摆线形螺旋磁有序结构，周期为62nm，在周期内磁极化几乎可以完全抵消，从而导致BiFeO3宏观上表现为弱磁性。由于BiFeO3理论上具有较好的铁磁性能，使得BiFeO3在信息存储、传感器和微机电系统等多功能器件中有潜在的应用价值，从而不断吸引着各国研究人员的目光。但是BiFeO3的性能目前还不能满足微电子器件应用的要求，特别是铁电性和铁磁性相互制约，为此如何同时提高BiFeO3的铁电性和铁磁性是亟需解决的问题。
BiFeO3薄膜的铁电性来自于晶粒的铁电畴，因此晶粒越大铁电畴越多，铁电性越好；而BiFeO3有周期为 62 nm 的螺旋调制结构，当制备的BiFeO3尺寸小于 62 nm 时，磁性必然会增强。因此，为了同时提高BFO薄膜的磁电耦合效应（铁磁性能），我们提出了一种提高BiFeO3薄膜磁电耦合效应的退火方法。
发明内容
本发明采用化学溶液沉积法，结合层层退火工艺制备BiFeO3薄膜，薄膜的制备过程主要分为三个阶段，即前驱体溶液的配制阶段，湿膜的制备阶段，热处理成膜阶段，以ITO/glass为基体。
具体方案如下：
（1）BiFeO3薄膜前驱体溶液配制：首先用电子天平按照各溶质的摩尔计量比进行称量，硝酸铁与硝酸铋的摩尔比为1：1:1；用移液管量取体积比为1:3的乙二醇和冰乙酸作为溶剂，将上述溶质和溶液置于磁力搅拌器上搅拌8小时，直至溶质全部溶解，待溶液搅拌均匀后，量取与硝酸铋摩尔比为1:1的乙酰丙酮作为螯合剂加入其中，在磁力搅拌器上匀速搅拌12小时，得到暗红色半透明溶液。最后再补充乙二醇和冰乙酸，最后所得溶液浓度为0.3mol/L， pH值在0.3-0.4，得到制备BiFeO3薄膜样品所需的前驱体溶液。
（2）将所制备的BiFeO3溶液静置24小时，把前驱体溶液均匀旋涂在预处理过氧化铟锡/玻璃（ITO/glass）的基体上。
（3）湿膜烘干：将涂膜结束的薄膜样品快速转移到150-200℃的电热板上120s烘干，使所制备湿膜中的部分有机溶剂得以挥发，从而得到所要求薄膜的干膜。
（4）预处理：将前期所制备的干模置于快速退火炉中，奇数层薄膜样品的预处理温度为300℃，偶数层薄膜样品的预处理温度为400℃，保温时间100-200s，使得薄膜样品中的有机成分进一步去除，因预处理的温度较低，不足以提供薄膜形核和生长所需要的能量，因此，预处理结束后得到非晶态的薄膜样品。
（5）最终退火：这一过程和预处理过程相类似，只是温度不同。奇数层薄膜样品的退火温度为400-500℃，偶数层薄膜样品的退火温度为650-750℃，保温时间都为300-500s，得到晶态薄膜样品。
（6）将湿膜的制备和热处理成膜两个阶段重复，从而制得所需厚度的薄膜样品，最终制备的薄膜层数为16层。
本发明的效益是，与现有每层都选择相同的退火工艺相比，这种退火方式保证了奇数层纳米晶粒形成，特别是粒径小于62 nm的晶粒，有利用薄膜磁性的提高；而高温退火可以保证偶数层晶粒的发育，利用铁电畴的发育，有利用铁电性的提高，这种退火方式提高了BiFeO3薄膜的磁电耦合效应。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合具体实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅用以解释本发明，并不用于限定本发明。
实施例1
按照上述工艺将所制备的干模置于快速退火炉中，奇数层薄膜样品的预处理温度为300℃，偶数层薄膜样品的预处理温度为400℃，保温时间150s。将热解的薄膜进行退火处理，奇数层薄膜样品的退火温度为400℃，偶数层薄膜样品的退火温度为650℃，保温时间都为400s，得到晶态薄膜样品。将湿膜的制备和热处理成膜两个阶段重复，从而制得所需厚度的薄膜样品，制备的薄膜最终层数为16层。
实施例2
按照上述工艺将所制备的干模置于快速退火炉中，奇数层薄膜样品的预处理温度为300℃，偶数层薄膜样品的预处理温度为400℃，保温时间150s。将热解的薄膜进行退火处理，奇数层薄膜样品的退火温度为450℃，偶数层薄膜样品的退火温度为700℃，保温时间都为400s，得到晶态薄膜样品。将湿膜的制备和热处理成膜两个阶段重复，从而制得所需厚度的薄膜样品，制备的薄膜最终层数为16层。
实施例3
按照上述工艺将所制备的干模置于快速退火炉中，奇数层薄膜样品的预处理温度为300℃，偶数层薄膜样品的预处理温度为400℃，保温时间150s。将热解的薄膜进行退火处理，奇数层薄膜样品的退火温度为500℃，偶数层薄膜样品的退火温度为750℃，保温时间都为400s，得到晶态薄膜样品。将湿膜的制备和热处理成膜两个阶段重复，从而制得所需厚度的薄膜样品，制备的薄膜最终层数为16层。
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，根据本发明的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之内。
表1实施例性能指标
性能 铁电性(2Pr) 磁性(2Mc)
实施例1 98μC/cm2 0.15emμ/g
实施例2 80μC/cm2 0.21emμ/g
实施例3 102μC/cm2 0.18emμ/g

Claims (4)

1.一种提高BiFeO3薄膜磁电耦合效应的退火方法，其特征在于：具体步骤如下：
（1）BiFeO3薄膜前驱体溶液配制：首先用电子天平按照各溶质的摩尔计量比进行称量，硝酸铁与硝酸铋的摩尔比为1：1:1；用移液管量取体积比为1:3的乙二醇和冰乙酸作为溶剂，将上述溶质和溶液置于磁力搅拌器上搅拌8小时，直至溶质全部溶解，待溶液搅拌均匀后，量取与硝酸铋摩尔比为1:1的乙酰丙酮作为螯合剂加入其中，在磁力搅拌器上匀速搅拌12小时，得到暗红色半透明溶液，最后再补充乙二醇和冰乙酸，最后所得溶液浓度为0.3mol/L， pH值在0.3-0.4，得到制备BiFeO3薄膜样品所需的前驱体溶液；
（2）将所制备的BiFeO3溶液静置24小时，把前驱体溶液均匀旋涂在预处理过氧化铟锡/玻璃（ITO/glass）的基体上；
（3）湿膜烘干：将涂膜的薄膜样品快速转移到150-200℃的电热板上120s烘干，使所制备湿膜中的部分有机溶剂得以挥发，得到所要求薄膜的干膜；
（4）预处理：将前期所制备的干膜置于快速退火炉中，奇数层薄膜样品的预处理温度为300℃，偶数层薄膜样品的预处理温度为400℃，保温时间100-200s；
（5）最终退火：奇数层薄膜样品的退火温度为400-500℃，偶数层薄膜样品的退火温度为650-750℃，保温时间都为300-500s，得到晶态薄膜样品；
（6）将湿膜的制备和热处理成膜两个阶段重复，最终制备的薄膜层数为16层。
2.根据权利要求1所述的一种提高BiFeO3薄膜磁电耦合效应的退火方法，奇数层薄膜样品的预处理温度为300℃，偶数层薄膜样品的预处理温度为400℃，保温时间100-200s。
3.根据权利要求1所述的一种提高BiFeO3薄膜磁电耦合效应的退火方法，奇数层薄膜样品的退火温度为400-500℃，偶数层薄膜样品的退火温度为650-750℃，保温时间为300-500s。
4.根据权利要求1所述的一种提高BiFeO3薄膜磁电耦合效应的退火方法，最终制备的薄膜层数为16层。
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