CN108807185A - 溶液制备氧化物界面电子气的方法 - Google Patents
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Abstract
本发明公开了一种溶液制备氧化物界面电子气的方法,用于解决现有方法制备氧化物界面电子气质量差的技术问题。技术方案是首先对单晶衬底进行预处理,再配置氧化物前驱体溶液,进而通过化学旋涂和高真空退火工艺的控制,形成氧化物与钛酸锶衬底的异质结构,并在界面产生二维电子气效应。通过调节薄膜材料结构、结晶度以及薄膜与衬底间界面性质,实现了高电子迁移率的二维电子气的制备。所制备的氧化物界面电子气质量高,其霍尔迁移率在190cm2V‑1s‑1~5113cm2V‑1s‑1范围内。本发明采用溶液旋涂方法制备氧化物界面电子气,具有质量高、耗能低、操作简单的特点。
Description
技术领域
本发明属于表面科学和微电子技术领域,特别涉及一种溶液制备氧化物界面电子气的方法。
背景技术
由于复杂氧化物界面具有丰富的电、光和磁等性能,并伴随着脉冲激光沉积、分子束外延等先进薄膜生长技术的发展,使氧化物界面的研究引起人们广泛的兴趣。其中,最经典的发现是A.Ohtomo和H.Y.Hwang通过脉冲激光沉积技术,在同为钙钛矿结构的SrTiO3和LaAlO3界面处发现了奇特的金属导电行为,且界面存在高的电子迁移率,即二维电子气。这种具有强关联特性的氧化物界面成为了半导体器件中应用广泛的功能单元,如纳米尺度效应管、新型量子霍尔系统和高Tc超导体,具有应用到下一代电子器件上的潜力。然而,在低温2K时,这种同钙钛矿结构的LaAlO3/SrTiO3二维电子气的电子迁移率一般在1000cm2V-1s-1左右,载流子浓度在1013~1014cm-2的范围。最近几年,根据文献1“Nature Communications,2394(4):1371;2013”发现异构的尖晶石/钙钛矿结构的Al2O3/SrTiO3界面二维电子气,在低温2K时,其电子迁移率可以达到1.4×105cm2V-1s-1,要高于之前报道的所有以SrTiO3为衬底的界面体系。在以往的研究中,如文献2“Journal of Applied Physics,117:095303;2015”和文献3“Journal of Applied Physics,118:115303;2015”,制备Al2O3/SrTiO3界面主要利用脉冲激光沉积和分子束外延等方法,但这些方法技术都涉及了相对高的能量和非平衡态的生长条件,在高能激光的轰击下SrTiO3衬底表面容易引入缺陷,更易发生原子扩散,从而降低了二维电子气的质量。
发明内容
为了克服现有方法制备氧化物界面电子气质量差的不足,本发明提供一种溶液制备氧化物界面电子气的方法。该方法首先对单晶衬底进行预处理,再配置氧化物前驱体溶液,进而通过化学旋涂和高真空退火工艺的控制,形成氧化物与钛酸锶衬底的异质结构,并在界面产生二维电子气效应。通过调节薄膜材料结构、结晶度以及薄膜与衬底间界面性质,实现了高电子迁移率的二维电子气的制备。所制备的氧化物界面电子气质量高,其霍尔迁移率在190cm2V-1s-1~5113cm2V-1s-1范围内。本发明采用溶液旋涂方法制备氧化物界面电子气,具有质量高、耗能低、操作简单的特点。
本发明解决其技术问题所采用的技术方案:一种溶液制备氧化物界面电子气的方法,其特点是包括以下步骤:
步骤一、将大小为3×5~5×5mm的(001)晶面的钛酸锶单晶衬底依次用去离子水、无水乙醇、离子水和无水乙醇超声清洗5~20min,用以NH4·F为缓冲液的HF酸腐蚀,其NH4·F与HF的比为0.5~5:0.8~4,腐蚀时间为35~70s,酸腐蚀后的钛酸锶单晶衬底置于空气氛围的管式炉中950~1000℃煅烧,升温速率2~5℃/min,保温时间1~3小时,得到以TiO2为终止面的钛酸锶单晶衬底。
步骤二、称取九水合硝酸铝、草酸铝、高氯酸铝或十六水合硫酸铝的铝酸化合物加入到乙醇、丙酮或N,N-二甲基甲酰胺溶剂中,在磁力搅拌下搅拌24小时使其充分溶解,再加入聚乙烯吡咯烷酮,铝盐和聚乙烯吡咯烷酮、DMF的用量范围比是铝盐:PVP:DMF的重量比=0.5~5:0.2~1:2.5~10g,在35℃~50℃恒温搅拌下形成Al的前驱体溶液。
步骤三、初始PVP-Al/SrTiO3薄膜的制备:将钛酸锶单晶衬底置于加热台上80~120℃预热5min,再将经过处理的钛酸锶单晶衬底置于匀胶机中,滴加前驱体溶液于钛酸锶单晶衬底上,依次以转速为1000~3000r/min,时间为10~30s进行低速旋涂,以转速为8000~9900r/min,,时间为30~60s进行高速旋涂,获得PVP-Al/SrTiO3薄膜。
步骤四、将步骤三中得到的PVP-Al/SrTiO3薄膜先置于空气氛围的马弗炉中400~500℃预处理,恒温时间2~5小时,再将经过预处理的PVP-Al/SrTiO3薄膜置于1×10-4Pa~1×10-3Pa的高真空腔中600~900℃高温退火,升温速率控制在1~5℃/min,保温时间5~60min,即得Al2O3/SrTiO3界面二维电子气。
本发明的有益效果是:该方法首先对单晶衬底进行预处理,再配置氧化物前驱体溶液,进而通过化学旋涂和高真空退火工艺的控制,形成氧化物与钛酸锶衬底的异质结构,并在界面产生二维电子气效应。通过调节薄膜材料结构、结晶度以及薄膜与衬底间界面性质,实现了高电子迁移率的二维电子气的制备。所制备的氧化物界面电子气质量高,其霍尔迁移率在190cm2V-1s-1~5113cm2V-1s-1范围内。本发明采用溶液旋涂方法制备氧化物界面电子气,具有质量高、耗能低、操作简单的特点。
下面结合附图和具体实施方式对本发明作详细说明。
附图说明
图1是本发明溶液制备氧化物界面电子气的方法的流程图。
图2是实施例1中(001)晶面的SrTiO3衬底预处理之后的原子力图。
图3是实施例1中Al2O3/SrTiO3二维电子气截面的高倍透射电镜图及选区衍射图。
具体实施方式
以下实施例参照图1-3。
实施例1:步骤一、将大小为3×5mm的(001)晶面的钛酸锶单晶衬底依次用去离子水、无水乙醇、离子水和无水乙醇超声清洗5min,用以NH4·F为缓冲液的HF酸腐蚀,其NH4·F与HF的比为0.5:0.8,腐蚀时间为35s,酸腐蚀后的钛酸锶单晶衬底置于空气氛围的管式炉中950℃煅烧,升温速率2℃/min,保温时间1小时,得到以TiO2为终止面的钛酸锶单晶衬底。
步骤二、称取九水合硝酸铝、草酸铝、高氯酸铝或十六水合硫酸铝的铝酸化合物加入到乙醇、丙酮或N,N-二甲基甲酰胺溶剂中,在磁力搅拌下搅拌24小时使其充分溶解,再加入聚乙烯吡咯烷酮,铝盐和聚乙烯吡咯烷酮、DMF的用量范围比是铝盐:PVP:DMF的重量比=0.5:0.2:2.5,在35℃恒温搅拌下形成Al的前驱体溶液。
步骤三、初始PVP-Al/SrTiO3薄膜的制备:将钛酸锶单晶衬底置于加热台上80℃预热5min,再将经过处理的钛酸锶单晶衬底置于匀胶机中,滴加前驱体溶液于钛酸锶单晶衬底上,依次以转速为1000r/min,时间为10s进行低速旋涂,以转速为8000r/min,,时间为30s进行高速旋涂,获得PVP-Al/SrTiO3薄膜。
步骤四、将步骤三中得到的PVP-Al/SrTiO3薄膜先置于空气氛围的马弗炉中400℃预处理,恒温时间2小时,再将经过预处理的PVP-Al/SrTiO3薄膜置于1×10-4Pa的高真空腔中600℃高温退火,升温速率控制在1℃/min,保温时间5min,即得Al2O3/SrTiO3界面二维电子气。
该产品中Al2O3薄膜的厚度大概在70nm,并且γ相的Al2O3薄膜是沿SrTiO3基底的(001)晶面择优生长。
将得到的Al2O3/SrTiO3二维电子气进行电输运特性测试,其电阻在15K和300K时分别为0.42Ω和78.0Ω,载流子浓度保持不变为3.1×1015cm-2,霍尔电子迁移率分别为4924.4cm2V-1s-1和38.0cm2V-1s-1。本实施例制备的氧化物界面电子气,具有质量高、耗能低、操作简单的特点。
从图2中可以看出,(001)晶面的SrTiO3衬底经过预处理达到了原子级别的平整度。
图3中可以看出,Al2O3/SrTiO3电子气截面形成了高质量的氧化物异质结。
实施例2:步骤一、将大小为4×5mm的(001)晶面的钛酸锶单晶衬底依次用去离子水、无水乙醇、离子水和无水乙醇超声清洗10min,用以NH4·F为缓冲液的HF酸腐蚀,其NH4·F与HF的比为3:4,腐蚀时间为50s,酸腐蚀后的钛酸锶单晶衬底置于空气氛围的管式炉中990℃煅烧,升温速率3℃/min,保温时间2小时,得到以TiO2为终止面的钛酸锶单晶衬底。
步骤二、称取九水合硝酸铝、草酸铝、高氯酸铝或十六水合硫酸铝的铝酸化合物加入到乙醇、丙酮或N,N-二甲基甲酰胺溶剂中,在磁力搅拌下搅拌24小时使其充分溶解,再加入聚乙烯吡咯烷酮,铝盐和聚乙烯吡咯烷酮、DMF的用量范围比是铝盐:PVP:DMF的重量比=3:0.5:6,在40℃恒温搅拌下形成Al的前驱体溶液。
步骤三、初始PVP-Al/SrTiO3薄膜的制备:将钛酸锶单晶衬底置于加热台上100℃预热5min,再将经过处理的钛酸锶单晶衬底置于匀胶机中,滴加前驱体溶液于钛酸锶单晶衬底上,依次以转速为2000r/min,时间为20s进行低速旋涂,以转速为9000r/min,时间为45s进行高速旋涂,获得PVP-Al/SrTiO3薄膜。
步骤四、将步骤三中得到的PVP-Al/SrTiO3薄膜先置于空气氛围的马弗炉中450℃预处理,恒温时间3小时,再将经过预处理的PVP-Al/SrTiO3薄膜置于1×10-4Pa的高真空腔中750℃高温退火,升温速率控制在3℃/min,保温时间35min,即得Al2O3/SrTiO3界面二维电子气。
该产品中Al2O3薄膜的厚度大概在50nm,并且γ相的Al2O3薄膜是沿SrTiO3基底的(001)晶面择优生长。
将得到的Al2O3/SrTiO3二维电子气进行电输运特性测试,其电阻在15K和300K时分别为42Ω和530Ω,载流子浓度保持不变为7.5×1014cm-2,霍尔电子迁移率分别为4210.4cm2V-1s-1和10.0cm2V-1s-1。
本实施例制备的氧化物界面电子气,具有质量高、耗能低、操作简单的特点。
实施例3:步骤一、将大小为5×5mm的(001)晶面的钛酸锶单晶衬底依次用去离子水、无水乙醇、离子水和无水乙醇超声清洗20min,用以NH4·F为缓冲液的HF酸腐蚀,其NH4·F与HF的比为5:4,腐蚀时间为70s,酸腐蚀后的钛酸锶单晶衬底置于空气氛围的管式炉中1000℃煅烧,升温速率5℃/min,保温时间3小时,得到以TiO2为终止面的钛酸锶单晶衬底。
步骤二、称取九水合硝酸铝、草酸铝、高氯酸铝或十六水合硫酸铝的铝酸化合物加入到乙醇、丙酮或N,N-二甲基甲酰胺溶剂中,在磁力搅拌下搅拌24小时使其充分溶解,再加入聚乙烯吡咯烷酮,铝盐和聚乙烯吡咯烷酮、DMF的用量范围比是铝盐:PVP:DMF的重量比=5:1:10,在50℃恒温搅拌下形成Al的前驱体溶液。
步骤三、初始PVP-Al/SrTiO3薄膜的制备:将钛酸锶单晶衬底置于加热台上120℃预热5min,再将经过处理的钛酸锶单晶衬底置于匀胶机中,滴加前驱体溶液于钛酸锶单晶衬底上,依次以转速为3000r/min,时间为30s进行低速旋涂,以转速为9900r/min,,时间为60s进行高速旋涂,获得PVP-Al/SrTiO3薄膜。
步骤四、将步骤三中得到的PVP-Al/SrTiO3薄膜先置于空气氛围的马弗炉中500℃预处理,恒温时间5小时,再将经过预处理的PVP-Al/SrTiO3薄膜置于1×10-3Pa的高真空腔中900℃高温退火,升温速率控制在5℃/min,保温时间60min,即得Al2O3/SrTiO3界面二维电子气。
该产品中Al2O3薄膜的厚度大概在62nm,并且γ相的Al2O3薄膜是沿SrTiO3基底的(111)晶面择优生长。
将得到的Al2O3/SrTiO3二维电子气进行电输运特性测试,其电阻在15K和300K时分别为55Ω和775Ω,载流子浓度保持不变为1.1×1016cm-2,霍尔电子迁移率分别为190cm2V- 1s-1和5113cm2V-1s-1。
本实施例制备的氧化物界面电子气,具有质量高、耗能低、操作简单的特点。
Claims (1)
1.一种溶液制备氧化物界面电子气的方法,其特征在于包括以下步骤:
步骤一、将大小为3×5~5×5mm的(001)晶面的钛酸锶单晶衬底依次用去离子水、无水乙醇、离子水和无水乙醇超声清洗5~20min,用以NH4·F为缓冲液的HF酸腐蚀,其NH4·F与HF的比为0.5~5:0.8~4,腐蚀时间为35~70s,酸腐蚀后的钛酸锶单晶衬底置于空气氛围的管式炉中950~1000℃煅烧,升温速率2~5℃/min,保温时间1~3小时,得到以TiO2为终止面的钛酸锶单晶衬底;
步骤二、称取九水合硝酸铝、草酸铝、高氯酸铝或十六水合硫酸铝的铝酸化合物加入到乙醇、丙酮或N,N-二甲基甲酰胺溶剂中,在磁力搅拌下搅拌24小时使其充分溶解,再加入聚乙烯吡咯烷酮,铝盐和聚乙烯吡咯烷酮、DMF的用量范围比是铝盐:PVP:DMF的重量比=0.5~5:0.2~1:2.5~10,在35℃~50℃恒温搅拌下形成Al的前驱体溶液;
步骤三、将钛酸锶单晶衬底置于加热台上80~120℃预热5min,再将经过处理的钛酸锶单晶衬底置于匀胶机中,滴加前驱体溶液于钛酸锶单晶衬底上,依次以转速为1000~3000r/min,时间为10~30s进行低速旋涂,以转速为8000~9900r/min,,时间为30~60s进行高速旋涂,获得PVP-Al/SrTiO3薄膜;
步骤四、将步骤三中得到的PVP-Al/SrTiO3薄膜先置于空气氛围的马弗炉中400~500℃预处理,恒温时间2~5小时,再将经过预处理的PVP-Al/SrTiO3薄膜置于1×10-4Pa~1×10- 3Pa的高真空腔中600~900℃高温退火,升温速率控制在1~5℃/min,保温时间5~60min,即得Al2O3/SrTiO3界面二维电子气。
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