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CN110029315A - 一种超晶格材料及其制备方法和应用 - Google Patents

一种超晶格材料及其制备方法和应用 Download PDF

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CN110029315A
CN110029315A CN201910354441.4A CN201910354441A CN110029315A CN 110029315 A CN110029315 A CN 110029315A CN 201910354441 A CN201910354441 A CN 201910354441A CN 110029315 A CN110029315 A CN 110029315A
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ferrimagnetic
substrate
crystal lattice
material layer
dimensional material
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CN110029315B (zh
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金立川
贾侃成
张岱南
张怀武
钟智勇
杨青慧
唐晓莉
白飞明
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University of Electronic Science and Technology of China
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Abstract

本发明涉及超晶格磁光材料技术领域，尤其涉及一种超晶格材料及其制备方法和应用。根据实施例的记载，本发明提供的超晶格材料同时具有亚铁石榴石材料较好的磁性能和石墨烯等二维半导体材料良好的光电吸收特性，测试得到的磁光克尔效应数据表明，本发明所述的超晶格材料在2500Oe磁场下的饱和磁光克尔角为13mdeg，相比较未插入二维材料的非超晶格亚铁磁性薄膜材料，其磁光克尔角提高了2.5倍，实现了磁光效应的增强。

Description

一种超晶格材料及其制备方法和应用
技术领域
本发明涉及超晶格磁光材料技术领域，尤其涉及一种超晶格材料及其制备方法和应用。
背景技术
随着磁光信息存储技术的发展，传统的信息存储材料和器件架构已很难满足小型化和低功耗的存储应用需求。对磁光效应的研究发现具有固有磁矩的物质在外磁场的作用下电磁特性会发生变化，使光波在其内部的传输特性发生改变，光的自由度决定了光携带自旋和轨道角动量两种内禀特性，可作为信息载体，具有能耗低、灵敏度高和量子化输运等特性。因此，光与物质的相互作用是实现纳米光电子器件、高密度数据存储设备和光开关器件的重要科学途径。
因此，目前急需一种磁光效应强的材料。
发明内容
为了解决上述技术问题，本发明提供了一种超晶格材料及其制备方法和应用，所述超晶格材料具有很好的磁光效应。
为了实现上述发明目的，本发明提供以下具体技术方案：
本发明提供了一种超晶格材料，包括基片、在基片上设置的超晶格结构；
所述超晶格结构为[第一亚铁磁性薄膜/二维材料层/第二亚铁磁性薄膜]n，n≥1；
所述第一亚铁磁性薄膜、二维材料层和第二亚铁磁性薄膜依次层叠设置；
所述二维材料层的材料为石墨烯、拓扑绝缘体、过渡金属硫系化合物和黑磷中的一种或几种；
所述第一亚铁磁性薄膜和二维材料层之间为异质结结构；所述二维材料层和第二亚铁磁性薄膜之间为异质结结构。
优选的，所述拓扑绝缘体为Bi2Te3、Bi2Se3和Bi0.9Te0.1中的一种或几种。
优选的，所述第一亚铁磁性薄膜和第二亚铁磁性薄膜的材料独立地为石榴石型铁氧体；
所述石榴石型铁氧体为钇铁石榴石、铥铁石榴石和镥铋铁石榴石中的一种或几种。
优选的，所述第一亚铁磁性薄膜和第二亚铁磁性薄膜的厚度独立地为1nm～10μm。
优选的，所述二维材料层为原子层；所述原子层的层数≥1。
优选的，所述基片的材料为钆镓石榴石、硅单晶、砷化镓或氮化镓。
本发明还提供了上述技术方案所述超晶格材料的制备方法，包括以下步骤：
在基片上依次层叠生长第一亚铁磁性薄膜、二维材料层和第二亚铁磁性薄膜，得到超晶格材料。
优选的，生长所述第一亚铁磁性薄膜和第二亚铁磁性薄膜的方法独立地为脉冲激光沉积法、液相外延或磁控溅射。
优选的，生长所述二维材料层的方法为湿法转移法、分子束外延法或化学气相沉积法。
本发明还提供了上述技术方案所述的超晶格材料或由上述技术方案所述的制备方法制备得到的超晶格材料在磁光信息存储、光信息处理、光纤通信和量子信息领域中的应用。
本发明提供了一种超晶格材料，包括基片、在基片上设置的超晶格结构；所述超晶格结构为[第一亚铁磁性薄膜/二维材料层/第二亚铁磁性薄膜]n，n≥1；所述第一亚铁磁性薄膜、二维材料层和第二亚铁磁性薄膜依次层叠设置；所述二维材料层的材料为石墨烯、拓扑绝缘体、过渡金属硫系化合物和黑磷中的一种或几种；所述第一亚铁磁性薄膜和二维材料层之间为异质结结构；所述二维材料层和第二亚铁磁性薄膜之间为异质结结构。本发明在第一亚铁磁性薄膜和第二亚铁磁性薄膜之间设置二维材料层可以增强亚铁磁性薄膜的基态自旋轨道耦合作用，改善其带间磁光吸收性能。利用所述超晶格材料进行信息处理时，当入射光进入亚铁磁性薄膜内部，光波的传播特性，如偏振面、相位或散射特性会发生变化，对已经写入信息的亚铁磁性薄膜就可以通过透射或发射光波的特性变化将所需要的信息读出，具有更好的灵敏度和低功耗。根据实施例的记载，本发明所述的超晶格材料同时具有亚铁石榴石材料较好的磁性能和石墨烯等二维半导体材料具有良好的光电吸收特性两方面优点，测试得到的磁光克尔效应数据表明，本发明所述的超晶格材料在2500Oe的磁场下的饱和磁光克尔角为13mdeg，相比较未插入二维材料的非超晶格亚铁磁性薄膜材料，其磁光克尔角提高了2.5倍，实现了磁光效应的增强。与传统磁性存储材料相比，超晶格材料具有利用磁光效应进行信息处理的特点，并具有更好的灵敏度和低功耗特性；与传统磁光材料相比，亚铁石榴石/二维原子晶体超晶格材料具有优异的的光吸收特性等优势，本发明提供的超晶格材料将在磁光信息存储，光信息处理，光纤通信和量子信息领域有极大的应用前景。
附图说明
图1为本发明所述的超晶格材料的结构侧视图；
图2为实施例1制备得到的超晶格材料的扫描电子显微镜图；
图3为实施例1制备得到的超晶格材料和对比例1制备得到的超晶格材料的磁光克尔信号增强图；
图4为实施例1制备得到的超晶格材料和对比例1制备得到的超晶格材料的核磁共振线宽展宽图；
图5为实施例1制备得到的超晶格材料和对比例1制备得到的超晶格材料的阻尼增强图。
具体实施方式
本发明提供了一种超晶格材料，包括基片、在基片上设置的超晶格结构；
所述超晶格结构为[第一亚铁磁性薄膜/二维材料层/第二亚铁磁性薄膜]n，n≥1；
所述第一亚铁磁性薄膜、二维材料层和第二亚铁磁性薄膜依次层叠设置；
所述二维材料层的材料为石墨烯、拓扑绝缘体、过渡金属硫系化合物和黑磷中的一种或几种；
所述第一亚铁磁性薄膜和二维材料层之间为异质结结构；所述二维材料层和第二亚铁磁性薄膜之间为异质结结构。
在本发明中，所述基片的材料优选为钆镓石榴石、硅单晶砷化镓或氮化镓，更优选为钆镓石榴石；所述基片的厚度优选为500μm。
在本发明中，所述n≥1，优选为2～10，更优选为4～6。
在本发明中，所述第一亚铁磁性薄膜和第二亚铁磁性薄膜的材料独立地优选为石榴石型铁氧体；所述石榴石型铁氧体优选为钇铁石榴石、铥铁石榴石和镥铋铁石榴石中的一种或几种；当所述石榴石型铁氧体为上述具体选择中的两种以上时，本发明对所述具体物质的配比没有任何特殊的限定。所述第一亚铁磁性薄膜和第二亚铁磁性薄膜的厚度独立地优选为1nm～10μm，更优选为10～500nm。
在本发明中，所述二维材料层的材料优选为石墨烯、拓扑绝缘体、过渡金属硫系化合物和黑磷中的一种或几种；所述拓扑绝缘体优选为Bi2Te3、Bi2Se3和Bi0.9Te0.1中的一种或几种；所述过渡金属硫系化合物优选为二硫化钼。当所述二维材料层的材料为上述具体选择中的两种以上时，本发明对所述具体物质的配比没有任何特殊的限定，按任意配比进行混合即可。所述二维材料层优选原子层；所述原子层的层数≥1，优选为2～10，更优选为4～6。
本发明还提供了上述技术方案所述的超晶格材料的制备方法，包括以下步骤：
在基片上依次层叠生长第一亚铁磁性薄膜、二维材料层和第二亚铁磁性薄膜，得到超晶格材料。
在本发明中，若无特殊说明，所有原料组分均为本领域技术人员熟知的市售产品。
在本发明中，所述基片在生长第一亚铁磁性薄膜前，优选对所述基片进行预处理；所述预处理优选为依次用丙酮、酒精和去离子水进行清洗；所述清洗在超声的条件下进行；本发明对所述超声条件没有任何特殊的限定。
在本发明中，生长所述第一亚铁磁性薄膜的方法优选为脉冲激光沉积法、液相外延或磁控溅射，更优选为脉冲激光沉积法。
当生长所述第一亚铁磁性薄膜的方法为液相外延时，所述液相外延的过程优选为准确称量高纯第一亚铁磁性薄膜的材料，研磨混合后置于铂坩埚中，熔化，得到均匀熔体；将清洗后的基片放入所述均匀熔体中，进行液相外延后，清洗，得到第一亚铁磁性薄膜；所述熔化优选为先在1000～1100℃下熔化12～24h后，降温至950～1000℃，搅拌8～12h；更优选为先在1040～1060℃下熔化15～20h后，降温至960～980℃，搅拌10h；所述液相外延的温度优选为950℃，基片的转速优选为120rpm，所述液相外延的时间优选为10s～2min。
当生长所述第一亚铁磁性薄膜的方法为磁控溅射时，所述磁控溅射的氧气分压优选为1～10Pa，更优选为5Pa；所述磁控溅射的基片温度优选为700～800℃，更优选为750℃；所述磁控溅射的功率优选为20～100W，更优选为35W。
当生长所述第一亚铁磁性薄膜的方法为脉冲激光沉积法，所述脉冲激光沉积法的靶基距优选为7cm；所述脉冲激光沉积优选在氧气气氛下进行，所述氧气气氛的气压优选为0.5～1.5Pa，更优选为1.0Pa；所述脉冲激光沉积的温度优选为700～800℃，更优选为750℃；升温速率优选为8～12℃/min，更优选为10℃/min；所述脉冲激光沉积的时间优选为15～25min，更优选为20min；所述脉冲激光沉积的激光能量优选为250～350mJ，更优选为300mJ；激光频率优选为4～10Hz，更优选为5Hz。
所述脉冲激光沉积法的过程优选为在脉冲激光沉积腔体内放入基片，设置靶基距；在≤10-6Pa的真空环境下，将基片加热到700～800℃后；在腔体内通入氧气；然后，打开并设置激光器参数；打开基片挡板，进行沉积，沉积完成后关闭基片挡板；最后，以4～6℃/min的速率将基片温度降至室温，得到第一亚铁磁性薄膜。
在本发明中，生长所述二维材料层的方法优选为湿法转移、分子束外延、化学气相沉积；
当生长所述二维材料层的方法为分子束外延时，本发明对所述分子束外延的具体过程没有任何特殊的限定，采用本领域技术人员熟知的过程进行即可。
当生长所述二维材料层的方法为化学气相沉积时，本发明对所述化学气相沉积的具体过程没有任何特殊的限定，采用本领域技术人员熟知的过程进行即可。
当生长所述二维材料层的方法为湿法转移时，所述湿法转移，包括以下步骤：
将双面的铜基二维材料薄膜的一面涂覆PMMA；
将未涂覆PMMA的一面置于三氯化铁溶液表面，腐蚀3分钟后，用三氯化铁溶液冲洗掉未涂覆PMMA的二维材料薄膜后；继续置于三氯化铁溶液表面，腐蚀1小时后，将铜层全部腐蚀掉，使涂覆PMMA的二维材料薄膜漂浮在三氯化铁溶液表面；
用载玻片从下往上将涂覆PMMA的二维材料薄膜捞起来，并放入盛有去离子水的培养皿中(涂覆PMMA的二维材料薄膜漂浮在去离子水表面)；
将生长有第一亚铁磁性薄膜基片从下往上将涂覆PMMA的二维材料薄膜捞起来，使涂覆PMMA的二维材料薄膜位于生长有第一亚铁磁性薄膜基片的中央，干燥(将样品放在吸水的材料上，进行自然风干)，热处理后，用丙酮溶液去除PMMA，得到在第一亚铁磁性薄膜表面生长有二维材料层的基片。
在本发明中，所述热处理的温度优选为100～120℃，更优选为105～115℃，最优选为110℃；所述热处理的时间优选为0.5～1.5h，更优选为0.8～1.2h，最优选为1.0h。在本发明中，所述热处理是为了使二维材料层和第一亚铁磁性薄膜贴合更紧密，并形成异质结。
在本发明中，生长所述第二亚铁磁性薄膜的方法优选为脉冲激光沉积法、液相外延或磁控溅射，更优选为脉冲激光沉积法。
当生长所述第二亚铁磁性薄膜的方法为液相外延时，所述液相外延的过程优选为准确称量高纯第二亚铁磁性薄膜的材料，研磨混合后置于铂坩埚中，熔化，得到均匀熔体；将清洗后的基片放入所述均匀熔体中，进行液相外延后，清洗，得到第二亚铁磁性薄膜；所述熔化优选为先在1000～1100℃下熔化12～24h后，降温至950～1000℃，搅拌8～12h；更优选为先在1040～1060℃下熔化15～20h后，降温至960～980℃，搅拌10h；所述液相外延的温度优选为950℃，基片的转速优选为120rpm，所述液相外延的时间优选为10s～2min。
当生长所述第二亚铁磁性薄膜的方法为磁控溅射时，所述磁控溅射的氧气分压优选为1～10Pa，更优选为5Pa；所述磁控溅射的基片温度优选为700～800℃，更优选为750℃；所述磁控溅射的功率优选为20～100W，更优选为35W。
当生长所述第二亚铁磁性薄膜的方法为脉冲激光沉积法，所述脉冲激光沉积法的靶基距优选为7cm；所述脉冲激光沉积优选在氧气气氛下进行，所述氧气气氛的气压优选为0.5～1.5Pa，更优选为1.0Pa；所述脉冲激光沉积的温度优选为700～800℃，更优选为750℃；升温速率优选为8～12℃/min，更优选为10℃/min；所述脉冲激光沉积的时间优选为15～25min，更优选为20min；所述脉冲激光沉积的激光能量优选为250～350mJ，更优选为300mJ；激光频率优选为4～10Hz，更优选为5Hz。
所述脉冲激光沉积法的过程优选为在脉冲激光沉积腔体内放入基片，设置靶基距；在≤10-6Pa的真空环境下，将基片加热到700～800℃后；在腔体内通入氧气；然后，打开并设置激光器参数；打开基片挡板，进行沉积，沉积完成后关闭基片挡板；最后，以4～6℃/min的速率将基片温度降至室温，得到第二亚铁磁性薄膜。
本发明还提供了上述技术方案所述的超晶格材料或由上述技术方案所述的制备方法制备得到的超晶格材料在磁光信息存储、光信息处理、光纤通信和量子信息领域中的应用。
下面结合实施例对本发明提供的一种超晶格材料及其制备方法和应用进行详细的说明，但是不能把它们理解为对本发明保护范围的限定。
实施例1
一种超晶格材料：基片材料为钆镓石榴石(GGG)单晶衬底，第一亚铁磁性薄膜的材料为钇铁石榴石(YIG)(60nm)，二维材料层的材料为单层石墨烯，第二亚铁磁性薄膜的材料为钇铁石榴石(YIG)(60nm)；
制备方法：
1)依次用丙酮、酒精和去离子水，在超声的条件下清洗基片材料；
2)在脉冲激光沉积腔体内放入基片，设置靶基距(7cm)；在≤10-6Pa的真空环境下，以10℃/min的升温速率，将基片加热到750℃后；在腔体内通入氧气(气压为1.0Pa)；然后，打开并设置激光器参数(激光能量为300mJ；激光频率为5Hz)；打开基片挡板，沉积20min，沉积完成后关闭基片挡板；最后，以5℃/min的速率将基片温度降至室温，得到钇铁石榴石(YIG)薄膜层(60nm)；
3)将双面的铜基石墨烯薄膜的一面涂覆PMMA；
将未涂覆PMMA的一面置于三氯化铁溶液表面，腐蚀3分钟后，用三氯化铁溶液冲洗掉未涂覆PMMA的石墨烯薄膜后；继续置于三氯化铁溶液表面，腐蚀1小时后，将铜层全部腐蚀掉，使涂覆PMMA的石墨烯薄膜漂浮在三氯化铁溶液表面；
用载玻片从下往上将涂覆PMMA的石墨烯薄膜捞起来，并放入盛有去离子水的培养皿中(涂覆PMMA的石墨烯薄膜漂浮在去离子水表面)；
将生长有钇铁石榴石(YIG)薄膜层的基片从下往上将涂覆PMMA的石墨烯薄膜捞起来，使涂覆PMMA的石墨烯薄膜位于生长有钇铁石榴石(YIG)薄膜层的基片的中央，干燥(将样品放在吸水的材料上，进行自然风干)，热处理后，用丙酮溶液去除PMMA，得到在钇铁石榴石(YIG)薄膜层表面生长有石墨烯薄膜(单层石墨烯)的基片(所述钇铁石榴石(YIG)薄膜层与所述石墨烯薄膜为异质结结构)；
4)在脉冲激光沉积腔体内放入步骤3)得到的基片，设置靶基距(7cm)；在≤10-6Pa的真空环境下，以10℃/min的升温速率，将基片加热到750℃后；在腔体内通入氧气(气压为1.0Pa)；然后，打开并设置激光器参数(激光能量为300mj；激光频率为5Hz)；打开基片挡板，沉积20min，沉积完成后关闭基片挡板；最后，以5℃/min的速率将基片温度降至室温，得到钇铁石榴石(YIG)薄膜层(60nm)，同时最终得到超晶格材料，记为YIG(60nm)/石墨烯/YIG(60nm)。
实施例2
一种超晶格材料：基片材料为钆镓石榴石(GGG)单晶衬底，第一亚铁磁性薄膜的材料为铥铁石榴石(TmIG)(60nm)，二维材料层的材料为单层石墨烯，第二亚铁磁性薄膜的材料为铥铁石榴石(TmIG)(60nm)；
制备方法参考实施例1。
实施例3
一种超晶格材料：基片材料为钆镓石榴石(GGG)单晶衬底，第一亚铁磁性薄膜的材料为镥铋铁石榴石(LuBiIG)(60nm)，二维材料层的材料为单层石墨烯，第二亚铁磁性薄膜的材料为镥铋铁石榴石(LuBiIG)(60nm)；
制备方法参考实施例1。
实施例4
一种超晶格材料：基片材料为钆镓石榴石(GGG)单晶衬底，第一亚铁磁性薄膜的材料为钇铁石榴石(YIG)(60nm)，二维材料层的材料为拓扑绝缘体Bi2Te3(20nm)，第二亚铁磁性薄膜的材料为钇铁石榴石(YIG)(60nm)；
除生长拓扑绝缘体Bi2Te3层以外的其他制备方法参考实施例1；
生长拓扑绝缘体Bi2Te3层的过程(分子束外延)为：在真空度≥10-8Pa的条件下，将基片加热至高于600℃去除基片吸附气体，对高纯固态源材料Bi，Te进行加热，Bi源温度480℃，Te源温度350℃，基片温度450℃下制备得到Bi2Te3二维材料。
实施例5
一种超晶格材料，参考实施例1，区别仅在于将石墨烯膜层替换为二硫化钼(MoS2)膜层(单原子层)。
对比例1
1)依次用丙酮、酒精和去离子水，在超声的条件下清洗基片材料；
2)在脉冲激光沉积腔体内放入基片，设置靶基距(7cm)；在≤10-6Pa的真空环境下，以10℃/min的升温速率，将基片加热到750℃后；在腔体内通入氧气(气压为1.0Pa)；然后，打开并设置激光器参数(激光能量为300mJ；激光频率为5Hz)；打开基片挡板，沉积20min，沉积完成后关闭基片挡板；最后，以5℃/min的速率将基片温度降至室温，得到钇铁石榴石(YIG)薄膜层(60nm)，得到超晶格材料(记为YIG(120nm))。
测试例
将实施例1得到的超晶格材料进行扫描电子显微镜表征，测试结果如图2所示，由图可知，实施例1制备得到的超晶格材料表面能够看到明显的石墨烯边界形貌，图中左下角具有密集的多边形块状图形区域即为所转移的二维石墨烯材料，右上角平整光滑的表面即为亚铁磁性YIG薄膜区域；
将实施例1和对比例1得到的超晶格材料进行磁光克尔测试，测试结果如图3所示，由图可知，120nm厚YIG薄膜的磁光克尔角在2500Oe的磁场下达到5mdeg后饱和，而在其间插入一层二维石墨烯原子层后，其在2500Oe磁场下的饱和磁光克尔转角增大到13mdeg；
将实施例1和对比例1得到的超晶格材料进行铁磁共振测试，测试结果如图4和图5所示，由图可知，在相同厚度的120nmYIG薄膜内插入一层二维石墨烯原子层后，其铁磁共振峰向低磁场偏移，7～15GHz频率下测试铁磁共振线宽增加，Gilbert阻尼因子增大。
由以上实施例可知，本发明提供的超晶格材料在2500Oe的磁场下的饱和磁光克尔角为13mdeg，相比较未插入二维材料的非超晶格亚铁磁性薄膜材料，其磁光克尔角提高了2.5倍，实现了磁光效应的增强。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (10)

1.一种超晶格材料，包括基片、在基片上设置的超晶格结构；
所述超晶格结构为[第一亚铁磁性薄膜/二维材料层/第二亚铁磁性薄膜]n，n≥1；
所述第一亚铁磁性薄膜、二维材料层和第二亚铁磁性薄膜依次层叠设置；
所述二维材料层的材料为石墨烯、拓扑绝缘体、过渡金属硫系化合物和黑磷中的一种或几种；
所述第一亚铁磁性薄膜和二维材料层之间为异质结结构；所述二维材料层和第二亚铁磁性薄膜之间为异质结结构。
2.如权利要求1所述的超晶格材料，其特征在于，所述拓扑绝缘体为Bi2Te3、Bi2Se3和Bi0.9Te0.1中的一种或几种。
3.如权利要求1所述的超晶格材料，其特征在于，所述第一亚铁磁性薄膜和第二亚铁磁性薄膜的材料独立地为石榴石型铁氧体；
所述石榴石型铁氧体为钇铁石榴石、铥铁石榴石和镥铋铁石榴石中的一种或几种。
4.如权利要求1或3所述的超晶格材料，其特征在于，所述第一亚铁磁性薄膜和第二亚铁磁性薄膜的厚度独立地为1nm～10μm。
5.如权利要求1所述的超晶格材料，其特征在于，所述二维材料层为原子层；所述原子层的层数≥1。
6.如权利要求1所述的超晶格材料，其特征在于，所述基片的材料为钆镓石榴石、硅单晶、砷化镓或氮化镓。
7.权利要求1～6任一项所述的超晶格材料的制备方法，包括以下步骤：
在基片上依次层叠生长第一亚铁磁性薄膜、二维材料层和第二亚铁磁性薄膜，得到超晶格材料。
8.如权利要求7所述的制备方法，其特征在于，生长所述第一亚铁磁性薄膜和第二亚铁磁性薄膜的方法独立地为脉冲激光沉积法、液相外延或磁控溅射。
9.如权利要求7所述的制备方法，其特征在于，生长所述二维材料层的方法为湿法转移法、分子束外延法或化学气相沉积法。
10.权利要求1～6任一项所述的超晶格材料或由权利要求7～9任一项所述的制备方法制备得到的超晶格材料在磁光信息存储、光信息处理、光纤通信和量子信息领域中的应用。
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