Name: writing and low-temperature characterization of oxide nanostructures
Uploaded: 2014-07-18T15:00:00.000+00:00
Duration: 6 min 43 s
Description: Watch this Scientific Journal Video about Writing and Low-Temperature Characterization of Oxide Nanostructures at JoVE.com

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).

1。LAO / STOヘテロ構造を取得<ol><li> TiO 2の終端のSTO基板上にパルスレーザー堆積法により成長したLAOの3.4単位の細胞からなる酸化物ヘテロ構造を得る。試料の成長の詳細は参考文献22に記載されている。 </li></ol>サンプルの2。フォトリソグラフィー処理チップキャリアへの配線キャンバスのためのボンディングパッドと、LAO / STO界面に電気接点を作成します。個々の処理ステップを以下に詳細に説明する。 <ol><li>スピン、フォトレジスト<ol><li>次いで、30秒間4,000 rpmで、5秒間600 rpmで試料上にフォトレジストをスピン。フォトレジスト層は約2μmの厚さになります。 1分間95℃でサンプルを焼く。 </li></ol></li><li> 5 MW / cm 2のドーズ量で100秒間、320 nmの光でマスクアライナを用いてフォトレジストを公開します。 </li><li>フォトレジスト現像FOにおけるフォトレジストを開発rは1分。 </li><li>イオンミリング<ol><li>フォトレジストで覆われていない領域に15物質のナノメートル（LAOとSTO）を除去するのAr +イオンミルを使用してください。入ってくるのAr +イオンビームに対して垂直な方向に22.5°の角度でサンプルを置きます。のAr +エッチング速度が較正されていない場合は、材料の正確な量が除去されることを保証するために、キャリブレーションの実行を行う。 AFMまたは同等profilmetryを用いたエッチング深さを決定する。 </li></ol></li><li> TiとAuとのDCスパッタリング<ol><li>デポジットさ4nmのTi、次いで25nmのAuを試料上にAuが露出STO層と電気的に接触するようになっている。スパッタ圧力範囲は2-6×10 -7トルであり、スパッタリングは、RTでのサンプルで行われる。シャッターを10分間にTiをプリスパッタ100W、[開くシャッターが閉鎖され、50Wで1分間、完了すると、100Wで20秒すぐにプリスパッタ金をスパッタしてのサンプルに30秒間のAuスパッタ50 W·カリ希望のTiとAuの厚さを生成するために時間をフィブラート。 </li></ol></li><li>離昇<ol><li>サンプルの表面からフォトレジストを除去するアセトン/ IPA、超音波洗浄を使用してください。 </li></ol></li><li>第2層<ol><li>ステップ4（ すなわち 、イオンミリングを除く）を除く第二のリソグラフィプロセスは、個々のボンディングパッドに金ワイヤ接続を作成するために使用される。 2つのパターンが、彼らは電気的短絡を生じないことを保証するために十分に整列させる必要があります。 </li></ol></li><li>プラズマ洗浄。 <ol><li> IPCバレルエッチャーは、パターン溝にフォトレジスト残渣を除去するために使用される。 1分間100 Wと1トルのアルゴンで使用される機器</li></ol></li></ol> 3。ワイヤボンド書き込みのために準備するためのサンプル<ol><li> 28使用可能なピンとチップ·キャリア（ 図2A）に、LAO / STOサンプルをマウントします。 </li><li>ワイヤボンド構造</li></ol>注：電気Cを作るために、ワイヤボンダーを使用して、試料上のボンディングパッドとチップキャリアとの間のonnections。電気接点とチップキャリアとの間で1ミル（25ミクロン）金ワイヤを取り付けます。ナノ構造を書く 4。ナノ構造をお書きください。 <ol><li>導電性ナノ構造（ 図3A）の非公式スケッチを作成します。 </li><li>スケーラブルベクターグラフィックス（SVG）エディタ（ 図3B）を開きます。 <ol><li>テンプレートを使用するか、AFM像と一致するようにウィンドウのサイズを定義します。 </li><li> SVGエディタにサンプルのAFM像をロードします。 </li><li>原子間力顕微鏡の画像に重ねたナノ構造要素を作成します。 </li></ol></li><li>ナノリソグラフィプログラムにSVGファイルをロードします。 </li><li>導電性ナノ構造体を作成するために、リソグラフィ·ソフトウェアを実行します。 <ol><li>ナノ構造を消去するために、ナノ構造、およびV チップ =-10Vを作成するには、V チップ = +10 Vを使用してください。 </li><li> 20に至るまでの速度で、C-AFMの先端を移動2ミクロン/秒0ナノメートル/秒。 </li></ol></li></ol> 5。デバイスを冷却し、測定を行う<ol><li>すべての白のライトをオフにして、赤色フィルタ/光源を使用しています。 </li><li>原子間力顕微鏡システムからサンプルを抽出します。 </li><li>希釈冷凍機（A）にサンプルをロードします。 </li><li>試料が冷却される温度（B）対抵抗を測定します。 </li><li>低温（℃）で輸送特性を測定します。 </li></ol>

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The authors have nothing to disclose.

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 &#8220;writing test&#8221; 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 &#8220;cutting&#8221; 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.

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。

<table><tbody><tr><td>Equipment</td><td></td><td></td><td></td></tr><tr><td>Contact Aligner</td><td>Karl-Suss</td><td>MA6</td><td></td></tr><tr><td>Spinner</td><td>Solitec</td><td>5110C</td><td></td></tr><tr><td>Ion Mill</td><td>Commonwealth Scientific</td><td>8C</td><td></td></tr><tr><td>Sputtering System</td><td>Leybold-Heraeus</td><td>Z-650</td><td></td></tr><tr><td>Barrel Etcher</td><td>Branson/IPC</td><td>3000C</td><td></td></tr><tr><td>Wire Bonder</td><td>Westbond</td><td>7700E</td><td></td></tr><tr><td>AFM</td><td>Asylum Research</td><td>MFP-3D</td><td></td></tr><tr><td>Dilution Refrigerator</td><td>Quantum Design</td><td>P850</td><td></td></tr><tr><td>Ultrasonic Wash Machine</td><td>Fisher Scientific</td><td>15-335-6</td><td></td></tr><tr><td>Current Amplifier</td><td>Femto</td><td>DLPCA-200</td><td></td></tr><tr><td>Materials</td><td></td><td></td><td></td></tr><tr><td>LaAlO&lt;sub&gt;3&lt;/sub&gt;/SrTiO&lt;sub&gt;3&lt;/sub&gt;</td><td>Prof. Chang-Beom Eom</td><td></td><td>5 mm x 1 mm with ~3.4 unit cells of LAO (See Reference 18)</td></tr><tr><td>Photoresist</td><td>AZ Electronic Materials</td><td>P4210</td><td></td></tr><tr><td>Developer</td><td>AZ Electronic Materials</td><td>400K</td><td></td></tr><tr><td>Acetone</td><td>Fisher Scientific</td><td>A929SK-4</td><td></td></tr><tr><td>Isopropyl Alcohol</td><td>Fisher Scientific</td><td>A459-1</td><td></td></tr><tr><td>Deionized Water</td><td>Fisher Scientific</td><td>23-290-065</td><td></td></tr><tr><td>Gold Wire</td><td>DuPont</td><td>5771</td><td>1 mm diameter</td></tr><tr><td>Chip Carrier</td><td>NTK Technologies</td><td>IRK28F1-5451D</td><td></td></tr></tbody></table>

writing and low-temperature characterization of oxide nanostructures

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.

ここに示された結果は、ナノ構造のこのクラスによって示されることができ、詳細23-26の他の箇所に記載されているトランスポートの動作の代表である。この例では、ナノワイヤキャビティは、3.3単位セルLAO / STOヘテロ構造から（ 図4）を構築した。実験11」をカットする&quot;ナノワイヤーによって決定された（緑で表示）導電性パスは、幅広い一般的には10nmである。先端書き込み速度はそのまま各セグメントの先端速度と電圧は、リソグラフィのフロントパネル（ 図4B）から独立して設定可能です。 「仮想電極は、「界面接点とそのインタフェースは、ナノ構造の導電性の高い電気的な接続があることを確認してください。 ナノ構造が書き込まれた後、希釈冷凍機に転送される。 550 nmで以下光への曝露は、不要な光伝導が生成されますので、IMPですortant暗闇の中、または赤色の「暗室」は、光（ 図5A）を用いてデバイスを転送します。電気的接続はRTで行う必要があり、かつ低温での電気接続を変更するときに最も半導体ナノ構造と同様に、細心の注意を払うべきである。デバイスは静電放電に供されている場合は、最も可能性の高い絶縁性となるであろう。注目すべきことに、デバイス機能」は、サイクリング」300 Kの温度にし、再び冷却することによって回収することができる。 クールダウン中は、温度の関数として、2端子抵抗を監視するためのルーチン、さらには4端子抵抗である。交流電流は、トランスインピーダンス増幅器を使用して測定している間、これらの測定のために交流電圧（典型的には1〜7mV）は、一方の電極に低周波数（&lt;10ヘルツ）で適用される。復調にロックすると、フィルタリングは、家庭が開発し、ロックインアンプを使用して実行されます。交流のCurrent温度の関数（ 図5B）のように監視される。 装置は、希釈冷凍機（50 m·K）でのベース温度に冷却されると、四端子輸送測定（ 図5C）が行われる。デバイスの両端の電圧を同時に測定している間、これらの測定では、電流は、装置の主要なチャネルを介して供給されます。代わりに、ロックインアンプで測定する、完全な電流 - 電圧（IV）トレースを測定する。この方法は、より多くの情報が含まれており、差動伝導が数値微分を介して算出することができる。特定のデバイスについては、差動伝導はサイドゲート電圧V SGの関数として測定される。このゲートは装置の化学ポテンシャルを変化させることができる。装置を通る輸送はクーロンブロッケードが小さな値のために行われ、STROれる領域を示す、強力な非単調な依存性を示すV SGの大きな値のため、超伝導ngの。デバイスのこのクラスの物理的解釈についての詳細は他の箇所に記載する。 <img alt="図1" src="/files/ftp_upload/51886/51886fig1highres.jpg" /> 図1フォトリソグラフィ処理ステップステップ1：スピンフォトレジスト。ステップ2：マスクアライナーを用いてフォトレジストを公開します。ステップ3：フォトレジストを開発しています。ステップ4：イオンミリング。ステップ5：DCは、TiとAuを堆積させるスパッタリング。ステップ6：リフトオフ。ステップ7：第二の層を堆積させる。ステップ8：プラズマ洗浄。 <img alt="図2" src="/files/ftp_upload/51886/51886fig2highres.jpg" /> 図2。リソグラフィでパターンLAO / STOヘテロ構造のイメージ。チップキャリアに接合さ5mm x 5mmのサンプル線を示す（A）の画像。（B）<html>ボンディングパッドとキャンバスの1を示す光学像。（C）単独のキャンバスのクローズアップ。 <a href="https://www-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/51886/51886fig2highres.jpg" target="_blank">この図の拡大版を表示するには、こちらをクリックしてください。</a> <img alt="図3" src="/files/ftp_upload/51886/51886fig3highres.jpg" /> 図3。LAO / STOナノ構造の（A）非公式なデザイン。（B）は 、オープンソースのスケーラブルベクターグラフィックス（SVG）エディタを使用してナノ構造体の正確なレイアウト。 <img alt="図4" src="/files/ftp_upload/51886/51886fig4highres.jpg" /> 図4のC-AFMのパターニングのための（A）リソグラフィ、フロントパネル（B）3Dシミュレータからのスクリーンの位置とC-AFMチップの電圧を示す。w.jove.com/files/ftp_upload/52058/52058fig4large.jpg &quot;ターゲット=&quot; _blank &quot;&gt;この図の拡大版を表示するには、こちらをクリックしてください。 <img alt="図5" src="/files/ftp_upload/51886/51886fig5highres.jpg" /> の関数としてのデバイスの四端子微分コンダクタンスの図5（A）LAO / STOナノ構造は、希釈冷凍機に挿入される。試料耐性の（B）モニタリングがmKで50 300 Kから冷却される。（C）モニタリングデバイス（V4t）全体の​​サイドゲート電圧VSGと電圧。強度グラフは、ジーメンス（S）の単位で表示され、電圧はボルト（V）単位で表示されている。

Watch this Scientific Journal Video about Writing and Low-Temperature Characterization of Oxide Nanostructures at JoVE.com

Writing and Low-Temperature Characterization of Oxide Nanostructures

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.

書き込みおよび酸化物ナノ構造の低温特性評価

Oxide nanoelectronics is a rapidly growing field which seeks to develop novel materials with multifunctional behavior at nanoscale dimensions.  Oxide ...

writing-and-low-temperature-characterization-of-oxide-nanostructures

Universidad San Sebastian

Research

JoVE Journal

Engineering

9.9K ビュー.  University of Pittsburgh. 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.

ビデオ: Writing and Low-Temperature Characterization of Oxide Nanostructures

Angle-resolved Photoemission Spectroscopy At Ultra-low Temperatures

The physical properties of a material are defined by its electronic structure. Electrons in solids are characterized by energy (&omega;) and momentum (k) and the probability to find them in a particular state with given &omega; and k is described by the spectral function A(k, &omega;). This function can be directly measured in an experiment based on the well-known photoelectric effect, for the explanation of which Albert Einstein received the Nobel Prize back in 1921. In the photoelectric effect the light shone on a surface ejects electrons from the material. According to Einstein, energy conservation allows one to determine the energy of an electron inside the sample, provided the energy of the light photon and kinetic energy of the outgoing photoelectron are known. Momentum conservation makes it also possible to estimate k relating it to the momentum of the photoelectron by measuring the angle at which the photoelectron left the surface. The modern version of this technique is called Angle-Resolved Photoemission Spectroscopy (ARPES) and exploits both conservation laws in order to determine the electronic structure, i.e. energy and momentum of electrons inside the solid. In order to resolve the details crucial for understanding the topical problems of condensed matter physics, three quantities need to be minimized: uncertainty* in photon energy, uncertainty in kinetic energy of photoelectrons and temperature of the sample.
In our approach we combine three recent achievements in the field of synchrotron radiation, surface science and cryogenics. We use synchrotron radiation with tunable photon energy contributing an uncertainty of the order of 1 meV, an electron energy analyzer which detects the kinetic energies with a precision of the order of 1 meV and a He3 cryostat which allows us to keep the temperature of the sample below 1 K. We discuss the exemplary results obtained on single crystals of Sr2RuO4 and some other materials. The electronic structure of this material can be determined with an unprecedented clarity.

The overall goal of this method is to determine the low-energy electronic structure of solids at ultra-low temperatures using Angle-Resolved Photoemission Spectroscopy with synchrotron radiation.

超低温での角度分解光電子分光

The physical properties of a material are defined by its  electronic structure. Electrons in solids are characterized by energy (&omega;)  and momentum ...

工学

Fabrication of Nano-engineered Transparent Conducting Oxides by Pulsed Laser Deposition

Nanosecond Pulsed Laser Deposition (PLD) in the presence of a background gas allows the deposition of metal oxides with tunable morphology, structure, density and stoichiometry by a proper control of the plasma plume expansion dynamics. Such versatility can be exploited to produce nanostructured films from compact and dense to nanoporous characterized by a hierarchical assembly of nano-sized clusters. In particular we describe the detailed methodology to fabricate two types of Al-doped ZnO (AZO) films as transparent electrodes in photovoltaic devices: 1) at low O2 pressure, compact films with electrical conductivity and optical transparency close to the state of the art transparent conducting oxides (TCO) can be deposited at room temperature, to be compatible with thermally sensitive materials such as polymers used in organic photovoltaics (OPVs); 2) highly light scattering hierarchical structures resembling a forest of nano-trees are produced at higher pressures. Such structures show high Haze factor (&gt;80%) and may be exploited to enhance the light trapping capability. The method here described for AZO films can be applied to other metal oxides relevant for technological applications such as TiO2, Al2O3, WO3 and Ag4O4.

We describe the experimental method to deposit nanostructured oxide thin films by nanosecond Pulsed Laser Deposition (PLD) in the presence of a background gas. By using this method Al-doped ZnO (AZO) films, from compact to hierarchically structured as nano-tree forests, can be deposited.

パルスレーザー蒸着法によるナノエンジニアリング透明導電性酸化物の作製

Nanosecond Pulsed  Laser Deposition (PLD) in the presence of a background gas allows the deposition  of metal oxides with tunable morphology, structure, ...

Fabrication of Spatially Confined Complex Oxides

Complex materials such as high Tc superconductors, multiferroics, and colossal magnetoresistors have electronic and magnetic properties that arise from the inherent strong electron correlations that reside within them. These materials can also possess electronic phase separation in which regions of vastly different resistive and magnetic behavior can coexist within a single crystal alloy material. By reducing the scale of these materials to length scales at and below the inherent size of the electronic domains, novel behaviors can be exposed. Because of this and the fact that spin-charge-lattice-orbital order parameters each involve correlation lengths, spatially reducing these materials for transport measurements is a critical step in understanding the fundamental physics that drives complex behaviors. These materials also offer great potential to become the next generation of electronic devices 1-3. Thus, the fabrication of low dimensional nano- or micro-structures is extremely important to achieve new functionality. This involves multiple controllable processes from high quality thin film growth to accurate electronic property characterization. Here, we present fabrication protocols of high quality microstructures for complex oxide manganite devices. Detailed descriptions and required equipment of thin film growth, photo-lithography, and wire-bonding are presented.

We describe the use of pulsed laser deposition (PLD), photolithography and wire-bonding techniques to create micrometer scale complex oxides devices. The PLD is utilized to grow epitaxial thin films. Photolithography and wire-bonding techniques are introduced to create practical devices for measurement purposes.

空間的に閉じ込められた複合酸化物の作製

Complex materials such as high Tc superconductors, multiferroics, and colossal magnetoresistors have electronic and magnetic properties that arise from ...

Atomically Defined Templates for Epitaxial Growth of Complex Oxide Thin Films

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain such surfaces are described. The first approach is the preparation of single terminated perovskite SrTiO3 (001) and DyScO3 (110) substrates. Wet etching was used to selectively remove one of the two possible surface terminations, while an annealing step was used to increase the smoothness of the surface. The resulting single terminated surfaces allow for the heteroepitaxial growth of perovskite oxide thin films with high crystalline quality and well-defined interfaces between substrate and film. In the second approach, seed layers for epitaxial film growth on arbitrary substrates were created by Langmuir-Blodgett (LB) deposition of nanosheets. As model system Ca2Nb3O10- nanosheets were used, prepared by delamination of their layered parent compound HCa2Nb3O10. A key advantage of creating seed layers with nanosheets is that relatively expensive and size-limited single crystalline substrates can be replaced by virtually any substrate material.

Various procedures are outlined to prepare atomically defined templates for epitaxial growth of complex oxide thin films. Chemical treatments of single crystalline SrTiO3 (001) and DyScO3 (110) substrates were performed to obtain atomically smooth, single terminated surfaces. Ca2 Nb3 O10- nanosheets were used to create atomically defined templates on arbitrary substrates.

複合酸化物薄膜のエピタキシャル成長のために原子的に定義されたテンプレート

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain ...

化学

Preparation and Reactivity of Gasless Nanostructured Energetic Materials

High-Energy Ball Milling (HEBM) is a ball milling process where a powder mixture placed in the ball mill is subjected to high-energy collisions from the balls. Among other applications, it is a versatile technique that allows for effective preparation of gasless reactive nanostructured materials with high energy density per volume (Ni+Al, Ta+C, Ti+C). The structural transformations of reactive media, which take place during HEBM, define the reaction mechanism in the produced energetic&#160;composites. Varying the processing conditions permits fine tuning of the milling-induced microstructures of the fabricated composite particles. In turn, the reactivity, i.e., self-ignition temperature, ignition delay time, as well as reaction kinetics, of high energy density materials depends on its microstructure. Analysis of the milling-induced microstructures suggests that the formation of fresh oxygen-free intimate high surface area contacts between the reagents is responsible for the enhancement of their reactivity. This manifests itself in a reduction of ignition temperature and delay time, an increased rate of chemical reaction, and an overall decrease of the effective activation energy of the reaction. The protocol provides a detailed description for the preparation of reactive nanocomposites with tailored microstructure using short-term HEBM method. It also describes a high-speed thermal imaging technique to determine the ignition/combustion characteristics of the energetic materials. The protocol can be adapted to preparation and characterization of a variety of nanostructured energetic composites.

This protocol describes the preparation of gasless nanostructured energetic materials (Ni+Al, Ta+C, Ti+C) using the short-term high-energy ball milling (HEBM) technique. It also describes a high-speed thermal imaging method to study the reactivity of mechanically fabricated nanocomposites. These protocols can be extended to other reactive nanostructured energetic materials.

Gaslessナノエネルギー物質の調製と反応性

High-Energy Ball Milling (HEBM) is a ball milling process where a powder mixture placed in the ball mill is subjected to high-energy collisions from the ...

Atomically Traceable Nanostructure Fabrication

Reducing the scale of etched nanostructures below the 10 nm range eventually will require an atomic scale understanding of the entire fabrication process being used in order to maintain exquisite control over both feature size and feature density. Here, we demonstrate a method for tracking atomically resolved and controlled structures from initial template definition through final nanostructure metrology, opening up a pathway for top-down atomic control over nanofabrication. Hydrogen depassivation lithography is the first step of the nanoscale fabrication process followed by selective atomic layer deposition of up to 2.8 nm of titania to make a nanoscale etch mask. Contrast with the background is shown, indicating different mechanisms for growth on the desired patterns and on the H passivated background. The patterns are then transferred into the bulk using reactive ion etching to form 20 nm tall nanostructures with linewidths down to ~6 nm. To illustrate the limitations of this process, arrays of holes and lines are fabricated. The various nanofabrication process steps are performed at disparate locations, so process integration is discussed. Related issues are discussed including using fiducial marks for finding nanostructures on a macroscopic sample and protecting the chemically reactive patterned Si(100)-H surface against degradation due to atmospheric exposure.

We report a protocol for combining the atomic metrology of the Scanning Tunneling Microscope for surface patterning with selective Atomic Layer Deposition and Reactive Ion Etching. Using a robust process involving numerous atmospheric exposures and transport, 3D nanostructures with atomic metrology are fabricated.

アトミックトレーサブルナノ構造作製

Reducing the scale of etched nanostructures below the 10 nm range eventually will require an atomic scale understanding of the entire fabrication process ...

Advanced Experimental Methods for Low-temperature Magnetotransport Measurement of Novel Materials

Novel electronic materials are often produced for the first time by synthesis processes that yield bulk crystals (in contrast to single crystal thin film synthesis) for the purpose of exploratory materials research. Certain materials pose a challenge wherein the traditional bulk Hall bar device fabrication method is insufficient to produce a measureable device for sample transport measurement, principally because the single crystal size is too small to attach wire leads to the sample in a Hall bar configuration. This can be, for example, because the first batch of a new material synthesized yields very small single crystals or because flakes of samples of one to very few monolayers are desired. In order to enable rapid characterization of materials that may be carried out in parallel with improvements to their growth methodology, a method of device fabrication for very small samples has been devised to permit the characterization of novel materials as soon as a preliminary batch has been produced. A slight variation of this methodology is applicable to producing devices using exfoliated samples of two-dimensional materials such as graphene, hexagonal boron nitride (hBN), and transition metal dichalcogenides (TMDs), as well as multilayer heterostructures of such materials. Here we present detailed protocols for the experimental device fabrication of fragments and flakes of novel materials with micron-sized dimensions onto substrate and subsequent measurement in a commercial superconducting magnet, dry helium close-cycle cryostat magnetotransport system at temperatures down to 0.300 K and magnetic fields up to 12 T.

We describe the methodology of mechanical exfoliation and deposition of flakes of novel materials with micron-sized dimensions onto substrate, fabrication of experimental device structures for transport experimentation, and the magnetotransport measurement in a dry helium close-cycle cryostat at temperatures down to 0.300 K and magnetic fields up to 12 T.

新規材料の低温磁気伝導測定のための高度な実験方法

Novel electronic materials are often produced for the first time by synthesis processes that yield bulk crystals (in contrast to single crystal thin film ...

Growth and Electrostatic/chemical Properties of Metal/LaAlO3/SrTiO3 Heterostructures

The quasi 2D electron system (q2DES) that forms at the interface between LaAlO3 (LAO) and SrTiO3 (STO) has attracted much attention from the oxide electronics community. One of its hallmark features is the existence of a critical LAO thickness of 4 unit-cells (uc) for interfacial conductivity to emerge. Although electrostatic mechanisms have been proposed in the past to describe the existence of this critical thickness, the importance of chemical defects has been recently accentuated. Here, we describe the growth of metal/LAO/STO heterostructures in an ultra-high vacuum (UHV) cluster system combining pulsed laser deposition (to grow the LAO), magnetron sputtering (to grow the metal) and X-ray photoelectron spectroscopy (XPS). We study step by step the formation and evolution of the q2DES and the chemical interactions that occur between the metal and the LAO/STO. Additionally, magnetotransport experiments elucidate on the transport and electronic properties of the q2DES. This systematic work not only demonstrates a way to study the electrostatic and chemical interplay between the q2DES and its environment, but also unlocks the possibility to couple multifunctional capping layers with the rich physics observed in two-dimensional electron systems, allowing the fabrication of new types of devices.

Growth and Electrostatic/chemical Properties of Metal/LaAlO3/SrTiO3 Heterostructures

We fabricate metal/LaAlO3/SrTiO3 heterostructures using a combination of pulsed laser deposition and in situ magnetron sputtering. Through magnetotransport and in situ X-ray photoelectron spectroscopy experiments, we investigate the interplay between electrostatic and chemical phenomena of the quasi two-dimensional electron gas formed in this system.

成長と静電/化学特性の金属/そこで3/SrTiO3ヘテロ構造

The quasi 2D electron system (q2DES) that forms at the interface between LaAlO3 (LAO) and SrTiO3 (STO) has attracted much attention from the oxide ...

Bulk and Thin Film Synthesis of Compositionally Variant Entropy-stabilized Oxides

Here, we present a procedure for the synthesis of bulk and thin film multicomponent (Mg0.25(1-x)CoxNi0.25(1-x)Cu0.25(1-x)Zn0.25(1-x))O (Co variant) and (Mg0.25(1-x)Co0.25(1-x)Ni0.25(1-x)CuxZn0.25(1-x))O (Cu variant) entropy-stabilized oxides. Phase pure and chemically homogeneous (Mg0.25(1-x)CoxNi0.25(1-x)Cu0.25(1-x)Zn0.25(1-x))O (x = 0.20, 0.27, 0.33) and (Mg0.25(1-x)Co0.25(1-x)Ni0.25(1-x)CuxZn0.25(1-x))O (x = 0.11, 0.27) ceramic pellets are synthesized and used in the deposition of ultra-high quality, phase pure, single crystalline thin films of the target stoichiometry. A detailed methodology for the deposition of smooth, chemically homogeneous, entropy-stabilized oxide thin films by pulsed laser deposition on (001)-oriented MgO substrates is described. The phase and crystallinity of bulk and thin film materials are confirmed using X-ray diffraction. Composition and chemical homogeneity are confirmed by X-ray photoelectron spectroscopy and energy dispersive X-ray spectroscopy. The surface topography of thin films is measured with scanning probe microscopy. The synthesis of high quality, single crystalline, entropy-stabilized oxide thin films enables the study of interface, size, strain, and disorder effects on the properties in this new class of highly disordered oxide materials.

The synthesis of high quality bulk and thin film (Mg0.25(1-x)CoxNi0.25(1-x)Cu0.25(1-x)Zn0.25(1-x))O and (Mg0.25(1-x)Co0.25(1-x)Ni0.25(1-x)CuxZn0.25(1-x))O entropy-stabilized oxides is presented.

バルクと組成バリエーション エントロピー安定化酸化物薄膜合成

Here, we present a procedure for the synthesis of bulk and thin film multicomponent (Mg0.25(1-x)CoxNi0.25(1-x)Cu0.25(1-x)Zn0.25(1-x))O (Co variant) and ...

Tuning Oxide Properties by Oxygen Vacancy Control During Growth and Annealing

Electrical, optical, and magnetic properties of oxide materials can often be controlled by varying the oxygen content. Here we outline two approaches for varying the oxygen content and provide concrete examples for tuning the electrical properties of SrTiO3-based heterostructures. In the first approach, the oxygen content is controlled by varying the deposition parameters during a pulsed laser deposition. In the second approach, the oxygen content is tuned by subjecting the samples to annealing in oxygen at elevated temperatures after the film growth. The approaches can be used for a wide range of oxides and nonoxide materials where the properties are sensitive to a change in the oxidation state.
The approaches differ significantly from electrostatic gating, which is often used to change the electronic properties of confined electronic systems such as those observed in SrTiO3-based heterostructures. By controlling the oxygen vacancy concentration, we are able to control the carrier density over many orders of magnitude, even in nonconfined electronic systems. Moreover, properties can be controlled, which are not sensitive to the density of itinerant electrons.

Oxide materials show many exotic properties that can be controlled by tuning the oxygen content. Here, we demonstrate the tuning of oxygen content in oxides by varying the pulsed laser deposition parameters and by performing postannealing. As an example, electronic properties of SrTiO3-based heterostructures are tuned by growth modifications and annealing.

成長・アニール時の酸素空孔制御による酸化物物性の調整

Electrical, optical, and magnetic properties of oxide materials can often be controlled by varying the oxygen content. Here we outline two approaches for ...

書き込みおよび酸化物ナノ構造の低温特性評価

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超低温での角度分解光電子分光

パルスレーザー蒸着法によるナノエンジニアリング透明導電性酸化物の作製

空間的に閉じ込められた複合酸化物の作製

複合酸化物薄膜のエピタキシャル成長のために原子的に定義されたテンプレート

Gaslessナノエネルギー物質の調製と反応性

アトミックトレーサブルナノ構造作製

新規材料の低温磁気伝導測定のための高度な実験方法

成長と静電/化学特性の金属/そこで₃/SrTiO₃ヘテロ構造

バルクと組成バリエーションエントロピー安定化酸化物薄膜合成

成長・アニール時の酸素空孔制御による酸化物物性の調整

書き込みおよび酸化物ナノ構造の低温特性評価

要約

さらに動画を探す

この動画の章

超低温での角度分解光電子分光

パルスレーザー蒸着法によるナノエンジニアリング透明導電性酸化物の作製

空間的に閉じ込められた複合酸化物の作製

複合酸化物薄膜のエピタキシャル成長のために原子的に定義されたテンプレート

Gaslessナノエネルギー物質の調製と反応性

アトミックトレーサブルナノ構造作製

新規材料の低温磁気伝導測定のための高度な実験方法

成長と静電/化学特性の金属/そこで3/SrTiO3ヘテロ構造

バルクと組成バリエーション エントロピー安定化酸化物薄膜合成

成長・アニール時の酸素空孔制御による酸化物物性の調整

成長と静電/化学特性の金属/そこで₃/SrTiO₃ヘテロ構造

バルクと組成バリエーションエントロピー安定化酸化物薄膜合成