書き込みおよび酸化物ナノ構造の低温特性評価
Summary
Oxide nanostructures provide new opportunities for science and technology. The interfacial conductivity between LaAlO3 and SrTiO3 can be controlled with near-atomic precision using a conductive atomic force microscopy technique. The protocol for creating and measuring conductive nanostructures at LaAlO3/SrTiO3 interfaces is demonstrated.
Abstract
Oxide nanoelectronics is a rapidly growing field which seeks to develop novel materials with multifunctional behavior at nanoscale dimensions. Oxide interfaces exhibit a wide range of properties that can be controlled include conduction, piezoelectric behavior, ferromagnetism, superconductivity and nonlinear optical properties. Recently, methods for controlling these properties at extreme nanoscale dimensions have been discovered and developed. Here are described explicit step-by-step procedures for creating LaAlO3/SrTiO3 nanostructures using a reversible conductive atomic force microscopy technique. The processing steps for creating electrical contacts to the LaAlO3/SrTiO3 interface are first described. Conductive nanostructures are created by applying voltages to a conductive atomic force microscope tip and locally switching the LaAlO3/SrTiO3 interface to a conductive state. A versatile nanolithography toolkit has been developed expressly for the purpose of controlling the atomic force microscope (AFM) tip path and voltage. Then, these nanostructures are placed in a cryostat and transport measurements are performed. The procedures described here should be useful to others wishing to conduct research in oxide nanoelectronics.
Introduction
酸化物ヘテロ構造1-5は、両方の科学的に興味深いとアプリケーション4に潜在的に有用である創発物理現象が顕著多種多様性を示す。特に、ランタンアルミ3（LAO）とのSrTiO 3（STO）6との間のインターフェースは、絶縁導電性、7超伝導、強誘電体のような8、9および強磁性挙動を示すことができる。 2006年には、ティールら LAO層の厚さは4単位セル（4uc）の臨界厚さが増加するように鋭利な絶縁体-金属転移が存在することを示した10。それは、その後3uc-LAO/STO構造は導電性の原子間力顕微鏡（C-AFM）プローブ11を局所的に制御することができるヒステリシス転移を示すことが示された。
このようにLaAlO 3 /たSrTiO 3のような酸化物界面の特性は、導電性の有無に依存する界面で電子が。これらの電子は、ゲート10バック、トップゲート電極12,13を用いて制御することができ、表面14は、強誘電体層15,16およびc-AFMリソグラフィー11を吸着。のc-AFMリソグラフィーのユニークな特徴は、非常に小さいナノスケールの特徴を作成することができることである。
二次元閉じ込めと組み合わせた電気頂ゲーティングは、多くの場合、III-V族半導体量子ドット17を作成するために使用される。代替的に、準一次元半導体ナノワイヤーは、電気的近接によってゲート制御することができる。これらの構造体を製造するための方法は、時間がかかり、一般に不可逆である。対照的に、C-AFMリソグラフィー技術は、ナノ構造は、一つの実験のために作成し、次いで（ホワイトボードと同様に）「消去」することができるという意味で、可逆的である。消去しながら、一般的には、C-AFMの書き込みは、AFMチップに印加される正の電圧を用いて行われる負電圧を用いて行われる。特定の構造を作成するために必要な時間は、デバイスの複雑さに依存するが、通常30分未満であり;そのほとんどの時間を過ごしたキャンバスを消去する。典型的な空間分解能は約10ナノメートルであるが、適切なチューニングを2ナノメートルは18作成できる限り小さくしています。
ナノスケールの製造手順の詳細は以下の通りである。ここで提供される詳細は、同様の実験が興味の研究者が行うことを可能にするのに十分であるべきである。ここで説明する方法は、半導体内の電子のナノ構造を作成するために使用される従来のリソグラフィの手法に比べて多くの利点を有する。
ここで説明するC-AFMリソグラフィー法は、走査型陽極酸化19、ディップペンナノリソグラフィー20、圧電パターニングを含む走査プローブベースのリソグラフィの努力、はるかに広いクラスの一部である21など。新規な酸化物界面を用いて結合されたここに記載のc-AFM技術は、物理的性質の前例のない様々な最高精度の電子構造のいくつかを生成することができる。
Protocol
Representative Results
Discussion
Successful creation of nanostructures depends on several critical steps. It is important that the LAO/STO samples are grown with a thickness that is known to be at the boundary between the insulating and conductive phase. (Details of sample growth fall outside the scope of this paper, but are crucial for overall success.) Second, it is important to have relative humidity within the range 25-45% for successful c-AFM writing. Values below 25% are unlikely to produce conductive nanostructures, while too high humidity will generally produce uncontrollably large features. Also, temperature control of the AFM is important if the c-AFM tip needs to achieve precise registry over long periods of time. Once the nanostructures are created, they must be placed in a vacuum environment if experiments lasting longer than a few hours are to be performed. For the experiments described here, the structure is created and within minutes transferred to a vacuum environment.
It is recommend before writing that a “writing test” be performed on all relevant electrodes. In such a test, two virtual electrodes are first created, and a single nanowire is written while simultaneously monitoring the conductance. A similar test of erasure can be performed by “cutting” the nanowire shortly afterwards. If the nanostructure is decaying rapidly, the issue is most likely due either to the interfacial contacts or the canvas itself. To distinguish between these two effects, a four-terminal measurement of the conductance should be performed, and the two-terminal conductance should be compared with the four-terminal conductance as a function of time. If the two-terminal conductance is decaying more rapidly than the four-terminal conductance, then the issue is related to the electrical contacts to the interface. If the four-terminal conductance is decaying at a comparable rate, then most likely the canvas is not suitable and should be replaced.
There are natural limitations of the current method for creating nanostructures. Specifically, the writing speed for the smallest devices is limited to a few hundred nanometers per second. Speeds far above that value lead to unpredictable results. Use of parallel writing techniques are possible27,28, but are not highly developed and have their own drawbacks. The size of nanostructures that can be created is naturally limited by the scan range of the AFM being used. A high-quality AFM with closed-loop feedback in the two scan directions is highly recommended. Tracking of point-like objects on the sample surface should be performed to monitor temporal drift of the sample.
Once creation of conductive nanostructures at oxide interfaces has been mastered, there are a wide range of experimental directions that can be explored. Using this technique, a wide variety of nanostructures and devices have already been demonstrated, including nanowires18, tunnel barriers29, rectifying junctions30, field-effect transistors18, single-electron transistors31, superconducting nanowires32, nanoscale optical detectors33, and nanoscale THz emitters and detectors34.
Disclosures
The authors have nothing to disclose.
Acknowledgements
The long-standing collaboration with Chang-Beom Eom at the University of Wisconsin-Madison, who provided the LAO/STO samples, is gratefully acknowledged. Video editing assistance from Christopher Solis is greatly appreciated. This work is supported by NSF (DMR-1104191, DMR-1124131), ARO (W911NF-08-1-0317), and AFOSR (FA9550-10-1-0524, FA9550-12-1-0268, FA9550-12-1-0057).
Materials
| Name | Company | Catalog Number | Comments |
| Equipment | |||
| Contact Aligner | Karl-Suss | MA6 | |
| Spinner | Solitec | 5110C | |
| Ion Mill | Commonwealth Scientific | 8C | |
| Sputtering System | Leybold-Heraeus | Z-650 | |
| Barrel Etcher | Branson/IPC | 3000C | |
| Wire Bonder | Westbond | 7700E | |
| AFM | Asylum Research | MFP-3D | |
| Dilution Refrigerator | Quantum Design | P850 | |
| Ultrasonic Wash Machine | Fisher Scientific | 15-335-6 | |
| Current Amplifier | Femto | DLPCA-200 | |
| Materials | |||
| LaAlO3/SrTiO3 | Prof. Chang-Beom Eom | N/A | 5mm x 1mm with ~3.4 unit cells of LAO (See Reference 18) |
| Photoresist | AZ Electronic Materials | P4210 | |
| Developer | AZ Electronic Materials | 400K | |
| Acetone | Fisher Scientific | A929SK-4 | |
| Isopropyl Alcohol | Fisher Scientific | A459-1 | |
| Deionized Water | Fisher Scientific | 23-290-065 | |
| Gold Wire | DuPont | 5771 | 1 mil diameter |
| Chip Carrier | NTK Technologies | IRK28F1-5451D |
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