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，获取LAO / STO异质<ol><li>获得氧化物异质结构由老挝3.4单位细胞对TiO 2结尾的STO基片脉冲激光沉积生长的。样品成长之详情载于文献22中描述。 </li></ol> 2，光刻样品的处理建立电接触到老挝/ STO界面，与焊盘布线画布到芯片载体。各个处理步骤的详细说明如下。 <ol><li>旋光刻胶<ol><li>旋转光致抗蚀剂上的样品，在600 rpm离心5秒，然后在4,000 rpm下进行30秒。光致抗蚀剂层将约2微米厚。烤的试样在95℃下1分钟。 </li></ol></li><li>使用掩模对准器320处的光线为100秒为5毫瓦/厘米2的剂量曝光光致抗蚀剂。 </li><li>开发在光致抗蚀剂显影剂的光致抗蚀剂FO中R 1分钟。 </li><li>离子铣削<ol><li>使用氩离子磨到不属于光致抗蚀剂的区域去除材料的15纳米（LAO和STO）。将样品在一个22.5°的角度，以垂直于进入的氩离子束的方向。如果氩离子刻蚀速率未校准，进行校准运行，以确保材料的正确金额被删除。利用原子力显微镜或等效profilmetry确定蚀刻深度。 </li></ol></li><li> Ti和Au，直流溅射<ol><li>存款4纳米钛，那么25纳米金上的样品，以使使金与暴露STO层电接触。溅射压力的范围为2-6×10 -7乇，溅射发生与样品在室温下。预溅射钛为10分钟，使用快门关闭，在100 W，然后打开快门和溅射20秒，在100瓦特完成后，立即在50瓦的预溅射金为1分钟，然后溅射金为30秒至样品在50 W·卡利BRATE以产生所需的Ti和Au的厚度的时间。 </li></ol></li><li>剥离<ol><li>用丙酮/异丙醇超声洗涤以从样品表面除去光致抗蚀剂。 </li></ol></li><li>第二层<ol><li>第二光刻工艺，不含步骤4（ 即 ，不包括离子铣削），是用来建立金线连接到各个键合焊盘。这两个图案必须很好对齐，以确保它们不会产生电气短路。 </li></ol></li><li>等离子清洗。 <ol><li>一个IPC桶式蚀刻来除去在图案沟槽中的光致抗蚀剂残余物。用在100 W和1乇氩气1分钟仪器</li></ol></li></ol> 3，焊线样品来准备写作<ol><li>与28引脚可挂载老挝/ STO样品在芯片载体（ 图2A）。 </li><li>焊线结构</li></ol>注:使用引线键合机，使电ç在样品上键合焊盘和芯片载体之间onnections。附1密耳（25微米）金线的电气触点和芯片载体之间。写纳米结构 4。写纳米结构<ol><li>建立一个非正式的导电纳米结构（ 图3A）的草图。 </li><li>打开可伸缩矢量图形（SVG）的编辑器（ 图3B）。 <ol><li>使用模板或定义窗口的大小以匹配原子力显微镜图像。 </li><li>装入样品的AFM图像到SVG编辑器。 </li><li>建立覆盖在原子力显微镜图像上纳米结构的元素。 </li></ol></li><li>加载SVG文件到纳米光刻方案。 </li><li>运行光刻软件创建一个导电纳米结构。 <ol><li>使用V 提示 = +10 V创建的纳米结构，和V 提示 = -10 V擦除纳米结构。 </li><li>将C-AFM针尖的速度范围从200毫微米/秒至2微米/秒。 </li></ol></li></ol> 5，冷却设备和进行测量<ol><li>关闭所有的白灯，并使用红色滤镜/光源。 </li><li>从AFM系统提取样品。 </li><li>样品装入稀释制冷机（A）。 </li><li>测量电阻与温度（B）作为样品冷却。 </li><li>在低温下（C）测量传输特性。 </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.

氧化物异质1-5表现出了显着各种各样的突发物理现象这都是有趣的科学和应用4可能有用。特别是， 铝酸镧（LAO）和钛酸锶（STO）6之间的界面上可以显示出绝缘性，导电，超导7，铁电状8和9铁磁行为。在2006年，Thiel 等人发现10，有一个锐利的绝缘体-金属转变为LAO层的厚度增加时，为4的单元电池（4UC）的临界厚度。据事后证明3uc-LAO/STO结构表现出了可以在本地用导电原子力显微镜（C-AFM）探针11被控制的迟滞过渡。 氧化接口，如铝酸镧/ 钛酸锶的属性取决于传导的存在或不存在电子界面处。这些电子可以通过顶部栅电极12,13，背门10被控制，表面吸附物14，铁电层15,16和c-AFM光刻11。的C-AFM平版印刷的独特的特点是非常小的纳米级功能可以被创建。 电顶部门控，并结合2维限制，通常被用来创建在III-V族半导体17的量子点。备选地，准一维半导体纳米线可以电由接近门控。该方法用于制备这些结构是耗时的且通常不可逆的。与此相反，在C-原子力显微镜光刻技术是可逆的，即纳米结构可以为一个实验被创建，然后在"擦除"（类似白板）。通常，C-​​AFM写作与施加在针尖正电压进行的，而，擦除使用负电压被执行。创建特定结构所需的时间依赖于该设备的复杂性，但通常不超过30分钟;大部分时间都花在擦除画布。典型的空间分辨率约为10纳米，但2纳米可以创建18用适当的调整功能小。 纳米级的制造步骤的详细说明如下。这里所提供的细节，应足以允许类似的实验，以通过感兴趣的研究人员进行。这里所描述的方法具有超过用于在半导体制造的电子的纳米结构的传统光刻方法的许多优点。 这里所描述的C-AFM光刻方法是一个更广泛的类的扫描探针为基础的光刻技术的努力，包括扫描阳极氧化19，蘸笔纳米光刻20，压电图案的一部分21，依此类推。这里所描述的C-原子力显微镜技术，再加上使用的新型氧化物界面，可以产生一些最精密的电子结构与前所未有的各种物理性能。

<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.

此处显示的结果是代表可以由这个类纳米结构的展示的传输行为，并进行了详细23-26别处所述。在此示例中，纳米线腔已从3.3晶胞LAO / STO异质构造（ 图4）。导电通路（以绿色显示）是典型的10纳米宽，由纳米线确定的"切割"实验11。尖速度和电压为每个段是从光刻前面板（ 图4B）可独立配置的，为的是尖端的写入速度。 "虚拟电极"与界面接触该接口确保有到纳米结构的导电性高的电连接。 纳米结构被写入后，它被转移到稀释制冷机。暴露在光线下或低于550纳米会产生不希望的光电导，所以它是IMPortant到设备在黑暗或有一个红色的"暗室"光（ 图5A）的帮助下转移。电气连接应在室温下进行，并与大多数半导体纳米结构，应十分注意在低温下不断变化的电气连接时服用。如果设备受到静电放电，它最有可能成为绝缘。值得注意的是，该装置的功能可以通过"循环"的温度为300 K和冷却再回收。 时的冷却时间，这是常规监测两个终端电阻，和连四端子电阻作为温度的函数。对于这些测量的交流电压（通常为〜1毫伏）在低频率（&lt;10赫兹）施加到电极中的一个，而将交流电流使用一个跨阻抗放大器测量。锁定在解调和使用家庭开发的锁相放大器进行滤波。交流立方米目前的监测作为温度的（ 图5B）的函数。 一旦设备被冷却到稀释制冷机（50谷）的基部的温度，四端传输执行测量（ 图5C）。对于这些测量，电流是通过该装置的主信道源，而在器件电压被同时测量。代替用锁定放大器，一个完整的电流 - 电压测量（IV）的微量测定。此方法包含更多信息和差分传导可以通过数值微分计算。对于特定的设备中，差分传导被测量为侧栅电压 V SG的函数。此栅极允许改变该装置的化学势。通过该装置的传输显示出强大的非单调的依赖，这表明在该库仑阻塞发生为较小的值，并STRO区域纳克超导较大对V SG值。关于此类设备的物理解释详细情况将在其他地方描述。 <img alt="图1" src="/files/ftp_upload/51886/51886fig1highres.jpg" /> 。图1光刻加工步骤第1步:旋光刻胶。步骤2:使用掩模对准曝光光致抗蚀剂。第3步:开发光致抗蚀剂。步骤4:离子铣削。步骤5:直流溅射法沉积Ti和Au。第6步:剥离。步骤7:沉积第二层。第8步:等离子清洗。 <img alt="图2" src="/files/ftp_upload/51886/51886fig2highres.jpg" /> 图2的光刻图案LAO / STO异质影像。（A）图片显示粘结到芯片载体5mm x 5mm的样品线（B）<html>光学图像显示焊盘与画布之一。（C）特写一个单一的画布。 <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/51886/51886fig2highres.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图3" src="/files/ftp_upload/51886/51886fig3highres.jpg" /> 图3（A）非正式LAO / STO纳米结构的设计（B）纳米结构的采用开源的可伸缩矢量图形（SVG）的编辑器精确布局。 <img alt="图4" src="/files/ftp_upload/51886/51886fig4highres.jpg" /> 图4（A）平版印刷前面板为C-AFM图案（B）从截图3D仿真显示位置和C-AFM针尖电压。w.jove.com/files/ftp_upload/52058/52058fig4large.jpg"目标="_blank"&gt;请点击这里查看该图的放大版本。 <img alt="图5" src="/files/ftp_upload/51886/51886fig5highres.jpg" /> 图5（a）劳/ STO纳米结构被插入稀释制冷机（B）取样电阻的监测，因为它是从300K冷却到50 mK的。设备的四端微分电导（三）监测的一个函数侧栅极电压VSG和两端的电压装置（4T版）。西门子（S）为单位，并显示电压强度图显示在伏（V）为单位。

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.

写作和氧化物纳米结构的低温特性

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

Nanyang Technological University

Research

JoVE Journal

Engineering

9.9K 次观看.  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.

视频: 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.

在极低的温度下角分辨光电子能谱

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

科研

工程学

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.

制备纳米设计的脉冲激光沉积透明导电氧化物

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.

空间密闭的复合氧化物制备

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.

原子定义模板复合氧化物薄膜的外延生长

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.

准备和无气腹纳米结构的反应含能材料

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.

原子纳米结构可追溯制造

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.

对于新材料的低温磁输运测量先进的实验方法

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.

金属/LaAlO 的生长和静电/化学性质3/SrTiO3异

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.

组分变熵稳定氧化物的体积和薄膜合成

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.

通过生长和退火过程中的氧空位控制来调整氧化物性能

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