CN110289352A - 低铁电极化翻转电压的四方相铁酸铋薄膜及其制备方法 - Google Patents
低铁电极化翻转电压的四方相铁酸铋薄膜及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种低铁电极化翻转电压的四方相铁酸铋薄膜及其制备方法，该制备方法包括以下步骤：S1：在LaAlO3衬底上采用脉冲激光沉淀法制备Ce0.04Ca0.96MnO3底电极；S2：在Ce0.04Ca0.96MnO3底电极上采用脉冲激光沉淀法制备四方相La0.15Bi0.85FeO3薄膜。该制备方法通过La掺杂去降低四方相铁酸铋薄膜的矫顽场从而降低其铁电极化翻转电压，可以在未来实际运用上减少电能的损耗以及减小能耗成本，对于未来BiFeO3薄膜进行低能耗应用具有十分重要的意义。
Description
技术领域
本发明涉及半导体薄膜材料技术领域，特别是涉及一种低铁电极化翻转电压的四方相铁酸铋薄膜及其制备方法。
背景技术
多铁材料是一类兼具铁电性(反铁电性)和铁磁性(反铁磁性)的多功能材料，可实现电和磁之间的相互调控，有望用于高密度、低功耗、高速、长寿的磁电耦合存储器件。铁酸铋(BiFeO3)是目前研究最热的多铁材料之一，其兼具铁电性和反铁磁性，铁电居里温度(～1100K)和反铁磁尼尔温度(～653K)均远高于室温。根据第一性原理计算和实验证明四方相BiFeO3本身具有很大的剩余极化，约为150μC/cm2，因此具有很大的应用前景，但因四方相BiFeO3的极化翻转电压较大，阻碍了其在新一代电子器件的未来应用。
目前，有部分研究通过调整BiFeO3的在基片上的生长取向来减小BiFeO3的翻转电压。但是通过文献调研发现，如何去降低四方相BiFeO3薄膜的翻转电压的研究中有待更近一步的研究。
发明内容
基于此，本发明的目的在于，提供一种低铁电极化翻转电压的四方相铁酸铋薄膜的制备方法，该制备方法制得的四方相铁酸铋薄膜铁电极化翻转电压小，具有良好的应用前景。
本发明的目的是通过以下技术方案实现的：一种低铁电极化翻转电压的四方相铁酸铋薄膜的制备方法，包括以下步骤：
S1：在LaAlO3衬底上采用脉冲激光沉淀法制备Ce0.04Ca0.96MnO3底电极；
S2：在Ce0.04Ca0.96MnO3底电极上采用脉冲激光沉淀法制备四方相La0.15Bi0.85FeO3薄膜。
相比于现有技术，本发明通过制备掺杂15％La的BFO薄膜，减小了其铁电极化翻转所需要的电压，从社会和经济角度出发，通过La掺杂去降低BiFeO3薄膜的矫顽场可以在未来实际运用上减少电能的损耗以及减小能耗成本，可见其对于未来BiFeO3薄膜进行低能耗应用具有十分重要的意义。
进一步地，步骤S1中，采用脉冲激光沉淀法使激光轰击Ce0.04Ca0.96MnO3靶材，让Ce0.04Ca0.96MnO3原子沉积到LaAlO3衬底的(001)晶面上制备出厚度为10nm的底电极。
优选地，步骤S1在温度为700～705℃、氧压为15～15.5Pa的条件下进行。
进一步地，步骤S2中，在底电极Ce0.04Ca0.96MnO3上采用脉冲激光沉淀法使激光轰击La0.15Bi0.85FeO3靶材，得到四方相La0.15Bi0.85FeO3薄膜。
优选地，步骤S2在温度为640～645℃、氧压为15～15.5Pa的条件下进行。
优选地，步骤S3制得的La0.15Bi0.85FeO3薄膜厚度为5～25nm。La0.15Bi0.85FeO3薄膜厚度小于5nm则可能导致薄膜在基片上分布不均匀，而超过25nm会释放混合相，因此制备La0.15Bi0.85FeO3薄膜时应将其厚度控制在5～25nm范围内，以保证制得的La0.15Bi0.85FeO3薄膜仅含有四方相。
本发明还提供一种低铁电极化翻转电压的四方相铁酸铋薄膜，其通过上述制备方法制备而成。该四方相铁酸铋薄膜铁电极化翻转电压较低，具有良好的低能耗应用前景。
为了更好地理解和实施，下面结合附图详细说明本发明。
附图说明
图1为实施例1制得的La0.15Bi0.85FeO3薄膜的形貌图、XRD物相分析图和Phase loop图。
图2为对比实施例1制得的BiFeO3薄膜的形貌图、XRD物相分析图和Phase loop图。
图3为实施例2制得的La0.15Bi0.85FeO3薄膜的形貌图、XRD物相分析图和Phase loop图。
图4为实施例2制得的La0.15Bi0.85FeO3薄膜的(103)晶面的Mapping图。
图5为实施例2制得的La0.15Bi0.85FeO3薄膜的(113)晶面的Mapping图。
图6为对比实施例2制得的BiFeO3薄膜的形貌图、XRD物相分析图和Phase loop图。
图7为对比实施例2制得的BiFeO3薄膜的(103)晶面的Mapping图。
图8为对比实施例2制得的BiFeO3薄膜的(113)晶面的Mapping图。
图9为实施例3制得的La0.15Bi0.85FeO3薄膜的形貌图、XRD物相分析图和Phase loop图。
图10为对比实施例3制得的BiFeO3薄膜的形貌图、XRD物相分析图和Phase loop图。
具体实施方式
实施例1
本实施例的低铁电极化翻转电压的四方相铁酸铋薄膜的制备方法，包括以下步骤：
S1：在温度为700～705℃、氧压为15～15.5Pa的条件下，采用脉冲激光沉淀法(仪器为TSST(Toshiba Samsung Storage Technology)公司的脉冲激光沉积仪)使激光轰击Ce0.04Ca0.96MnO3靶材，让Ce0.04Ca0.96MnO3原子沉积到LaAlO3衬底的(001)晶面上制备出厚度为10nm的底电极；
S2：在底电极Ce0.04Ca0.96MnO3上，在温度为640～645℃、氧压为15～15.5Pa的条件下采用脉冲激光沉淀法使激光轰击La0.15Bi0.85FeO3靶材，得到厚度为5nm的四方相La0.15Bi0.85FeO3薄膜；
S3：将La0.15Bi0.85FeO3的四方相外延薄膜通过原子力显微镜(AFM)和X射线衍射仪(XRD)确定其薄膜中只含有四方相。
S4：利用压电力显微镜(PFM)测得La0.15Bi0.85FeO3四方相外延薄膜的相位回线(Phase loop)，进而得出该薄膜铁电极化翻转所需要的电压。
对比实施例1
本对比实施例的纯BiFeO3的四方相外延薄膜的制备方法，包括以下步骤：
S1：在温度为700～705℃、氧压为15～15.5Pa的条件下，采用脉冲激光沉淀法(仪器为TSST(Toshiba Samsung Storage Technology)公司的脉冲激光沉积仪)使激光轰击Ce0.04Ca0.96MnO3靶材，让Ce0.04Ca0.96MnO3原子沉积到LaAlO3衬底的(001)晶面上制备出厚度为10nm的底电极；
S2：在底电极Ce0.04Ca0.96MnO3上，在温度为640～645℃、氧压为15～15.5Pa的条件下采用脉冲激光沉淀法使激光轰击BiFeO3靶材，得到厚度为5nm的四方相BiFeO3薄膜；
S3：将BiFeO3的四方相外延薄膜通过原子力显微镜(AFM)和X射线衍射仪(XRD)确定其薄膜中只含有四方相；
S4：利用压电力显微镜(PFM)测得BiFeO3四方相外延薄膜的Phase loop，进而得出该薄膜铁电极化翻转所需要的电压。
实施例2
本实施例的低铁电极化翻转电压的四方相铁酸铋薄膜的制备方法，与实施例1基本相同，此处不再赘述；本实施例与实施例1的区别在于：步骤S2制得的四方相La0.15Bi0.85FeO3薄膜厚度为15nm。
对比实施例2
本实施例的纯BiFeO3的四方相外延薄膜的制备方法，与对比实施例1基本相同，此处不再赘述；本实施例与实施例1的区别在于：步骤S2制得的四方相BiFeO3薄膜厚度为15nm。
实施例3
本实施例的低铁电极化翻转电压的四方相铁酸铋薄膜的制备方法，与实施例1基本相同，此处不再赘述；本实施例与实施例1的区别在于：步骤S2制得的四方相La0.15Bi0.85FeO3薄膜厚度为25nm。
对比实施例3
本实施例的纯BiFeO3的四方相外延薄膜的制备方法，与对比实施例1基本相同，此处不再赘述；本实施例与实施例1的区别在于：步骤S2制得的四方相BiFeO3薄膜厚度为25nm。
测试结果
测试仪器：形貌图和phase-loop图是美国Asylum Reseach公司的Cypher原子力显微镜(自带压电力显微镜功能模式)所测得；XRD物相分析图是有由PANalytical公司生产的X射线衍射仪所测得。
请参阅图1，其为实施例1制得的La0.15Bi0.85FeO3薄膜的形貌图、XRD物相分析图和Phase loop图。从图1a可以得知厚度为5nm的La0.15Bi0.85FeO3薄膜的生长质量很高，呈现规律的台阶状。图1b则是La0.15Bi0.85FeO3薄膜的普通XRD分析图，从图中可以看到在(001)晶面上只有四方相(Tetragonal phase，XRD图上简写为T)。图1c则是La0.15Bi0.85FeO3薄膜的Phase loop图，从图中可以得出其翻转铁电铁极化所需的电压约为0.8V。
请参阅图2，其对比实施例1制得的BiFeO3薄膜的形貌图、XRD物相分析图和Phaseloop图。从图2a可以得知5nm的BiFeO3薄膜的生长质量很高，呈现规律的台阶状。图2b则是BiFeO3薄膜的普通XRD分析图，从图中可以看到在(001)晶面上只有四方相(Tetragonalphase，XRD图上简写为T)。图2c则是BiFeO3薄膜的Phase loop图，从图中可以得出翻转铁电铁极化所需的电压约为3.5V。
可见，在5nm的相同厚度下比较，四方相的BiFeO3薄膜需要约3.5V的电压去使铁电极化发生翻转，而四方相的La0.15Bi0.85FeO3的薄膜只需要约0.8V的电压去进行极化翻转，即通过La掺杂可有效降低BiFeO3薄膜的极化翻转电压。依据相关La掺杂的文献调研以及实验结果数据，初步认为La掺杂实现了对A位离子Bi3+进行部分取代，其内部晶体结构由类四方相(T-like)转变为纯四方相(T)，这使得铁电极化在面内上的分量减小，从而使得面内极化翻转所需要越过的肖托基势垒减小，这就使得翻转铁电极化所需要的能量更小，故其减小了翻转铁电极化所需要的电压。
请同时参阅图3～5，其中，图3为实施例2制得的La0.15Bi0.85FeO3薄膜的形貌图、XRD物相分析图和Phase loop图，图4为实施例2制得的La0.15Bi0.85FeO3薄膜的(103)晶面的Mapping图，图5为实施例2制得的La0.15Bi0.85FeO3薄膜的(113)晶面的Mapping图。从图3a可以得知厚度为15nm的La0.15Bi0.85FeO3薄膜的生长质量很高，呈现规律的台阶状。图3b则是La0.15Bi0.85FeO3薄膜的普通XRD分析图，从图中可以看到在(001)晶面上只有四方相(Tetragonal phase，XRD图上简写为T)。图4和图5可进一步证明该La0.15Bi0.85FeO3薄膜是单一四方相，不含有其它的相。图3c则是La0.15Bi0.85FeO3薄膜的Phase loop图，从图中可以得出其翻转铁电铁极化所需的电压约为1.5V。
请同时参阅图6～8，其中，图6为对比实施例2制得的BiFeO3薄膜的形貌图、XRD物相分析图和Phase loop图，图7为对比实施例2制得的BiFeO3薄膜的(103)晶面的Mapping图，图8为对比实施例2制得的BiFeO3薄膜的(113)晶面的Mapping图。从图6a可以得知15nm的BiFeO3薄膜的生长质量很高，呈现规律的台阶状。图6b则是BiFeO3薄膜的普通XRD分析图，从图中可以看到在(001)晶面上只有四方相(Tetragonal phase，XRD图上简写为T)。图7和图8可进一步证明该BiFeO3薄膜是单一四方相，不含有其它的相。图6c则是BiFeO3薄膜的Phase loop图，从图中可以得出翻转铁电铁极化所需的电压约为4.5V。
可见，在15nm的相同厚度下比较，四方相的BiFeO3薄膜需要约4.5V的电压去使铁电极化发生翻转，而四方相的La0.15Bi0.85FeO3的薄膜只需要约1.5V的电压去进行极化翻转，即通过La掺杂可有效降低BiFeO3薄膜的极化翻转电压。
请参阅图9，其为实施例3制得的La0.15Bi0.85FeO3薄膜的形貌图、XRD物相分析图和Phase loop图。从图9a可以得知厚度为25nm的La0.15Bi0.85FeO3薄膜的生长质量很高，呈现规律的台阶状。图9b则是La0.15Bi0.85FeO3薄膜的普通XRD分析图，从图中可以看到在(001)晶面上只有四方相(Tetragonal phase，XRD图上简写为T)。图9c则是La0.15Bi0.85FeO3薄膜的Phase loop图，从图中可以得出其翻转铁电铁极化所需的电压约为2.0V。
请参阅图10，其对比实施例3制得的BiFeO3薄膜的形貌图、XRD物相分析图和Phaseloop图。从图2a可以得知25nm的BiFeO3薄膜的生长质量很高，呈现规律的台阶状。图2b则是BiFeO3薄膜的普通XRD分析图，从图中可以看到在(001)晶面上只有四方相(Tetragonalphase，XRD图上简写为T)。图2c则是BiFeO3薄膜的Phase loop图，从图中可以得出翻转铁电铁极化所需的电压约为6.0V。
可见，在25nm的相同厚度下比较，四方相的BiFeO3薄膜需要约6.0V的电压去使铁电极化发生翻转，而四方相的La0.15Bi0.85FeO3的薄膜只需要约2.0V的电压去进行极化翻转，即通过La掺杂可有效降低BiFeO3薄膜的极化翻转电压。
以上所述实施例仅表达了本发明的一种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。
Claims (7)
1.一种低铁电极化翻转电压的四方相铁酸铋薄膜的制备方法，其特征在于：包括以下步骤：
S1：在LaAlO3衬底上采用脉冲激光沉淀法制备Ce0.04Ca0.96MnO3底电极；
S2：在Ce0.04Ca0.96MnO3底电极上采用脉冲激光沉淀法制备四方相La0.15Bi0.85FeO3薄膜。
2.根据权利要求1所述的低铁电极化翻转电压的四方相铁酸铋薄膜的制备方法，其特征在于：步骤S1中，采用脉冲激光沉淀法使激光轰击Ce0.04Ca0.96MnO3靶材，让Ce0.04Ca0.96MnO3原子沉积到LaAlO3衬底的(001)晶面上制备出厚度为10nm的底电极。
3.根据权利要求2所述的低铁电极化翻转电压的四方相铁酸铋薄膜的制备方法，其特征在于：步骤S1在温度为700～705℃、氧压为15～15.5Pa的条件下进行。
4.根据权利要求1所述的低铁电极化翻转电压的四方相铁酸铋薄膜的制备方法，其特征在于：步骤S2中，在底电极Ce0.04Ca0.96MnO3上采用脉冲激光沉淀法使激光轰击La0.15Bi0.85FeO3靶材，得到四方相La0.15Bi0.85FeO3薄膜。
5.根据权利要求4所述的低铁电极化翻转电压的四方相铁酸铋薄膜的制备方法，其特征在于：步骤S2在温度为640～645℃、氧压为15～15.5Pa的条件下进行。
6.根据权利要求1～5任一项所述的低铁电极化翻转电压的四方相铁酸铋薄膜的制备方法，其特征在于：步骤S3制得的La0.15Bi0.85FeO3薄膜厚度为5～25nm。
7.一种低铁电极化翻转电压的四方相铁酸铋薄膜，其特征在于：通过权利要求1～6任一项所述的制备方法制备而成。
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