The authors wish to acknowledge the competitive faculty-initiated collaboration (FIC) grant from KAUST.

1.准备镨掺杂的SrTiO 3粉<ol><li>为了制备将10克锶0.95镨0.05的TiO 3粉末，权衡的SrCO 3粉末（7.53407克）的TiO 2纳米粉末（4.28983克），和Pr的化学计量的量2 O 3的烧结的块状（0.44299克）反应后对于 x = 0.05: </li></ol><img alt="式（1）" fo:content-width="5in" src="/files/ftp_upload/52869/52869eq1.JPG" width="550" /><ol start="2"><li>研磨称重镨2 O 3的烧结团块用玛瑙研钵和研杵微粒。 </li><li>将称取的SrCO 3粉末和TiO 2纳米粉末添加到镨2 O 3和继续研磨并用玛瑙研钵和研杵直到目视均匀的粉末达到混合。 </li><li>加载研磨粉末成玻璃罐混合使用湍流器进行30分钟至均匀第Ë混合物。 </li><li>加载所得混合粉放入一个精心清洗和抛光不锈钢模具（直径为1英寸）并夹持其两个不锈钢柱塞之间。 </li><li>冷压机使用约1吨载荷下按粉末。 </li><li>通过将管芯上的中空不锈钢圆筒，并用推入杆从顶部推柱塞和沉淀出弹出冷压球团。一旦从模具中冷压球团（生坯）的喷射，通过轻轻覆盖用小一块透明胶带的颗粒和通过翻录磁带除去一薄层清洗上的粒料的圆周表面上的任何污染。 </li><li>将沉淀垂直氧化铝舟填充商购的SrTiO 3粉末作为氧化铝舟和冷压球团之间的屏障。 </li><li>将船的管式炉，升温至1300℃，在3小时，并保持在该温度下15小时。允许粒料冷却至室温炉内当煅烧结束。这个步骤被称为"煅烧过程"之后。 </li><li>使用玛瑙研钵和杵研磨颗粒和负载所得粉末成玻璃瓶用于使用​​湍流器进一步混合。 </li><li>加载粉末放入不锈钢管芯和冷负荷下的约3吨挤压。 </li><li>在3小时重复步骤1.9一次在1400℃，并保持在该温度20小时。 </li><li>磨用玛瑙研钵和杵沉淀。 </li><li>重复步骤1.11，1.12，和1.13一次为固态反应达到完全。 </li></ol> 2.制备多晶硅散货镨掺杂的SrTiO 3陶瓷<ol><li>权衡1.6克所制备粉末（为一个盘2毫米厚和12.7毫米直径）。 </li><li>制备圆形graphoil件，以覆盖顶部和底部INTErface在石墨模具的夹持粉末和石墨柱塞。另外，制备另一矩形graphoil片以覆盖石墨模具的内壁。 </li><li>加载所制备粉末放入石墨模具（12.7毫米内径）和夹持相同大小的两个石墨柱塞之间的粉末。钻一个2毫米孔中的石墨模具的长度的中间，并且从模具的外表面，以约2mm的内表面的温度读数。 注意:调节模外其余的石墨柱塞的长度和定位夹持粉末汽缸，其中所述孔被放置以获得精确的温度读数的中心。石墨柱塞的表面需要对工件的加工过程中被精心整平。任何未对准可导致在烧结粒料的期间放电等离子烧结的开裂。 </li><li>冷压使用压在安装前的火花粉末轻轻（负载&lt;200千克）等离子体烧结板的腔室内部。使用顶部和底部的柱塞和新闻界级之间平面抛光不锈钢支撑板，以避免损坏石墨柱塞。 </li><li>裹一块石墨毡模具周围的绝缘和石墨丝固定。设计上感到通过切割一矩形片在温度读数孔被放置在模具中的毡的石墨的窗口。 </li><li>放置在放电等离子烧结室中的装载石墨模具和柱塞。移动阶段到最终位置。 </li><li>聚焦和对准上冲模的温度读取孔的高温计目标圆。确保高温计的发射率设置被设置为石墨。 </li><li>关闭室，并把7.7千牛负荷（约60兆帕）的样品。真空和吹扫该室用Ar三次和离开腔室6帕的动态真空下。 </li><li>通过增加电流（手动或使用增加温度程序）。使用一个250分钟-1（相当于约300-400℃，分-1），优化样本。这是该放电等离子烧结过程中最重要的步骤。 </li><li>通过手动调节电流或使用程序将温度保持在1500℃下进行5分钟。在5分钟保持期结束时，关断电流并快速松开7.7千牛顿负荷，以避免在冷却开裂的样品。让样品冷却至室温的室内。 </li><li>轻轻模具采用冷新闻稿散装颗粒从石墨。这是通过把石墨模具上的空心钢筒和喷射颗粒和使用的钢从顶部推入杆的石墨柱塞完成。 </li><li>除去对粒料用一把锋利的剃刀片顶面和底面以及所述圆周表面上的graphoil。 </li><li>使用粗糙的砂纸（400格）下来0.3-0.5毫米每边以保证擦亮样本彻底清除graphoil的。清洁用丙酮样品。 </li></ol>散装陶瓷3.电子表征及热传输特性<ol><li>确定所述陶瓷盘，ρ的密度，采用阿基米德法。 </li><li>测量样品的重量，W 干 ，然后将样品浸没在水中，的重量W 湿 ，在一个稳定的密度测量系统，并从计算阿基米德密度</li></ol><img alt="公式（2）" fo:content-width="2.1in" src="/files/ftp_upload/52869/52869eq2.JPG" width="260" />其中ρ 水是水在测量温度下的密度（ 例如，等于1克厘米-3，在300°K）。14 <ol start="2"><li>测量样品，D的热扩散率，使用下一个75毫升分钟-1流量的Ar的瞬时激光闪光技术。测量厚度样本，L的，准确首先使用数字微米。 注意:具有不同尺寸和形状（ 例如，圆盘12.7毫米直径或正方形10×10 平方毫米磁盘）和厚度平行面的样品毫米之间在0.5和5可以很容易地测量。 <ol><li>在激光闪光热扩散技术中，照射一个面样品的由短（约1毫秒）的激光脉冲和记录由红外线检测器的温度上升的相反面。然后从样品的厚度，并使用帕克方程式15的温度上升-时间分布计算热扩散通过激光闪光接口软件</li></ol></li></ol><img alt="公式3" fo:content-width="1.9in" src="/files/ftp_upload/52869/52869eq3.JPG" width="220" />其中L是磁盘和叔1/2的厚度的其他S的最大温升的一半时间IDE样品。 注意:帕克模型15假定绝热样品和瞬时脉冲加热，其他模型已被提出，多年来，占在测量各种损失，如热损失，有限脉冲持续时间，非均匀脉冲加热和非均质的理想条件结构。我们已经使用了考恩模型16与脉冲校正是最先进的方法之一。应当指出的是，为了最大化从正面发射的热能的量和以最大化由IR检测器观察到的信号中，样品表面必须高度发光。通常这需要一个薄的石墨涂层到样品表面上的应用程序。的2％-5％的热扩散率的测定不确 ​​定度的存在，从尺寸的确定而产生。17 <ol start="3"><li>用金刚石锯成矩形棒切盘沉淀，2×2×10毫米3，导电性和塞贝克系数的测量以及一个正方形盘，4×4×1.5 mm 3的高温比热和一个薄的矩形片，8×5×1毫米3对霍尔测量。 </li><li>测量的比热的样品，C 磷 ，在平坦和镜面抛光方片（4×4×1.5 立方毫米）使用差示扫描量热法（DSC）在氩气流下18 <ol><li>使用的5 K.分钟-1向上的加热速率40℃下等温保持10分钟，以使样品达到热平衡之后20K的分钟-1的加热速率高达500℃，用一个精确的冷却速度它紧随其后。氩气气流下进行测量（50毫升分钟-1建议）。 </li></ol></li></ol>注意:由于用于分析的方法的灵敏度，进行三次测量，以确定热容量<html>包括（1）的基线测量中减去背景，（2）测定用标准物质的比热（如蓝宝石）与已知的中c p，和样品的比热（3）的测量。保证样品是平的，镜面抛光，以使与测量坩埚底部的理想接触（铂/铑锅与Al在这项工作中使用2 O 3坩埚）。在DSC阶段的确切结构详情的DSC技术给他人，并用于测量样品的确切说明的比较可以在各种来源中找到。19 <ol start="5"><li>计算出的高温热传导从热扩散率，d时，比热，C P，以及密度的测量值的样本，κ，ρ用 20 </li></ol>/52869/52869eq4.JPG"WIDTH ="200"/&gt; <ol start="6"><li>金板的2×2×10mm的3片切来自样品的探针接触点（4接触），以减轻的接触电阻的问题。 <ol><li>为了溅射金仅在所需的接触区域，环绕的2×2×10mm的3样品一个苏格兰胶带作为模版来使用。离开2×2mm的2面未覆盖。用剃刀刀片，切出2非常小的孔（大约1毫米直径）中的2×10 平方毫米面沿着由探针距离分开的线的中间。 </li><li>使用台式黄金溅射装置溅射一〜200纳米厚的金膜。21 </li></ol></li><li>测量样品的电输送特性，即导电性和塞贝克系数）随温度22,23的功能。 <ol><li>使用四端子法测量电导率。衡量对SAM塞贝克系数E设定使用的温度和电压的测量通过两个中间热电偶"探针"。测量使用数字显微镜这两个探针之间的距离。上电输运测量的更多细节可以在其他地方被发现。22,23 </li></ol></li><li>测量霍尔载流子浓度作为温度上使用物理性质测量系统的8×5×1毫米3的样品的功能。24 </li></ol>

<ol>
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Jpn. 114, 102 (2006).</li><li>Wang, N., He, H., Ba, Y., Wan, C., Koumoto, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thermoelectric+Properties+of+Nb-doped+SrTiO3+Ceramics+Enhanced+by+Potassium+Titanate+Nanowires+Addition.">Thermoelectric Properties of Nb-doped SrTiO3 Ceramics Enhanced by Potassium Titanate Nanowires Addition.</a> J. Ceram. Soc. Jpn. 118, 1098 (2010).</li><li>Ohta, S., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Large+Thermoelectric+Performance+of+Heavily+Nb-doped+SrTiO3+Epitaxial+Film+at+High+Temperature.">Large Thermoelectric Performance of Heavily Nb-doped SrTiO3 Epitaxial Film at High Temperature.</a> Appl. Phys. Lett. 87, 092108 (2005).</li><li>Kovalevsky, A., Yaremchenko, A., Populoh, S., Weidenkaff, A., Frade, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Enhancement+of+Thermoelectric+Performance+in+Strontium+Titanate+by+Praseodymium+Substitution.">Enhancement of Thermoelectric Performance in Strontium Titanate by Praseodymium Substitution.</a> J. Appl. Phys. 113, 053704 (2013).</li><li>Kovalevsky, A. V., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Towards+a+High+Thermoelectric+Performance+in+Rare-Earth+Substituted+SrTiO3:+Effects+Provided+by+Strongly-Reducing+Sintering+Conditions.">Towards a High Thermoelectric Performance in Rare-Earth Substituted SrTiO3: Effects Provided by Strongly-Reducing Sintering Conditions.</a> Phys. Chem. 16, 26946 (2014).</li><li>Dawson, J. A., Tanaka, I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Local+Structure+and+Energetics+of+Pr-+and+La-Doped+SrTiO3+Grain+Boundaries+and+the+Influence+on+Core–Shell+Structure+Formation.">Local Structure and Energetics of Pr- and La-Doped SrTiO3 Grain Boundaries and the Influence on Core–Shell Structure Formation.</a> J. Phys. Chem. C. 118, 25765-25778 (2014).</li><li>Mehdizadeh Dehkordi, A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=New+Insights+on+the+Synthesis+and+Electronic+Transport+in+Bulk+Polycrystalline+Pr-doped+SrTiO3&#8722;&#948;.">New Insights on the Synthesis and Electronic Transport in Bulk Polycrystalline Pr-doped SrTiO3&#8722;&#948;.</a> Appl. Phys. Lett. 117, 055102 (2015).</li></ol>

The authors have nothing to disclose.

在这个协议中，我们已经提出，为了成功地批量制备多晶硅镨掺杂的SrTiO 3陶瓷具有改进的电子和热电性能的综合战略的步骤。该协议的主要步骤包括:（i）固态合成掺杂的SrTiO 3粉末在空气中在常压下与放电等离子体烧结法的能力（ⅱ）利用致密所制备的粉末成高密度散装陶瓷，并在同一时间，以进一步掺杂有镨的样品的晶界。据证实，通过施加高的SPS加热速度（300-400℃，分-1...

氧化物热电被证明是有前途的候选高温热电应用，从稳定性和成本的观点，以电子输运性质。之间的n型氧化物热电，高度掺杂的钛酸锶（STO）已经引起了人们的注意，因为它有趣的电子特性。然而，大的总热导率（κ〜12瓦米-1 K -1，在300°K的单结晶）1和低载流子迁移率（μ〜6cm 2的V -1秒-1，在300°K的单结晶） 1不利地影响热电性能是由优点的一个无量纲的数字计算，ZT =α2σT/κ，其中α是塞贝克系数，σ电导率，T为绝对温度以开尔文，以及κ的总热导率。这里我们定义的分子作为功率因数，PF =α263;吨。为了使该氧化物热电材料与其他高温热电（例如SiGe合金）进行竞争，在功率因数和/或减少晶格热导率更明显的增加是必需的。 为了提高STO的热电性能的大多数实验研究主要集中在热导率通过应变场和声子的质量波动散射的降低。这些尝试包括:（i）单或双掺杂锶2+和/或Ti 4+的网站，如相对于主要的努力这个方向，自然超晶格Ruddlesden -波普尔结构的2,3（二）合成为了通过加入纳米第二相绝缘的SrO层，4和（iii）复合工程进一步降低热导率不过5，直到最近，无增强策略已报道substantially增加这些氧化物热电功率因数。散装单和多晶的STO所报告的最大功率因数（PF）的值被限制于PF &lt;1.0 W M -1 K -1的上限。 各种合成方法和处理技术已经被用于实现上述尝试的想法。粉末合成途径包括传统的固态反应，6溶胶-凝胶，水热7，图8和燃烧合成，9而常规烧结，6热压10和最近放电等离子体烧结12顷之间用于将粉末压实成普通技术散装陶瓷。然而，对于一个类似的掺杂剂（ 例如，La）的和掺杂浓度，将得到的块状陶瓷表现出范围的电子和热传输性能。这在很大程度上是由于钛酸锶&lt;的强烈过程相关的缺陷化学子&gt; 3，这导致合成依赖特性。只有少数报告的优化合成和加工参数，以造福热电运输。值得一提的是，由于非常小的声子平均中的SrTiO 3自由程（升pH值 〜2在300K纳米），11纳米结构是不是一个可行的选择的散装STO陶瓷在TE性能主要是通过减少的改善的晶格热导率。 最近，我们报导优点在非均匀掺Pr的SrTiO 3陶瓷从同时提高热电功率因数始发热电数字超过30％的改善，并降低热导率。12,13在此详细的视频协议中，我们提出与讨论我们的综合战略，这些编制的步骤镨掺杂STO陶瓷具有改进的电子和热电性能。

<table><tbody><tr><td>SrCO&lt;sub&gt;3&lt;/sub&gt; Powder, 99.9%</td><td>Sigma Aldrich</td><td>472018</td><td></td></tr><tr><td>TiO&lt;sub&gt;2&lt;/sub&gt; Nanopowder, 99.5%</td><td>Sigma Aldrich</td><td>718467</td><td></td></tr><tr><td>Pr&lt;sub&gt;2&lt;/sub&gt;O&lt;sub&gt;3&lt;/sub&gt; Sintered Lumps, 99.9%</td><td>Alfa Aesar</td><td>35663&amp;nbsp;</td><td></td></tr><tr><td>Spark Plasma Sintering&amp;nbsp;</td><td>Dr. Sinter Lab</td><td>SPS-515S</td><td></td></tr><tr><td>Resistivity/Seebeck Coefficient Measurement System</td><td>Ulvac-Riko</td><td>ZEM-2</td><td></td></tr><tr><td>Laser Flash Thermal Diffusivity Measurement System</td><td>Netzsch</td><td>LFA-457 Microflash</td><td></td></tr><tr><td>Differential Scanning Calorimetry (DSC) System</td><td>Netzsch</td><td>404C Pegasus</td><td></td></tr><tr><td>Physical Property Measurement system (PPMS)</td><td>Quantum Design</td><td></td><td></td></tr><tr><td>Field Emission Scanning Electron Microscope (FE-SEM)</td><td>Hitachi</td><td>SU-6600</td><td></td></tr><tr><td>Energyy-dispersive X-ray Spectroscopy (EDS)</td><td>Oxford Instruments</td><td></td><td></td></tr><tr><td>X-ray Diffractometer</td><td>Rigaku</td><td>Ultima IV</td><td></td></tr><tr><td>Bench-top Sputter Coater</td><td>Denton Vacuum</td><td>Desk II</td><td></td></tr><tr><td>Diamond&amp;nbsp; Wheel Saw</td><td>South Bay Technology</td><td></td><td></td></tr></tbody></table>

synthesis of non-uniformly pr-doped srtio3 ceramics and their thermoelectric properties

We demonstrate a novel synthesis strategy for the preparation of Pr-doped SrTiO3 ceramics via a combination of solid state reaction and spark plasma sintering techniques. Polycrystalline ceramics possessing a unique morphology can be achieved by optimizing the process parameters, particularly spark plasma sintering heating rate. The phase and morphology of the synthesized ceramics were investigated in detail using X-ray diffraction, scanning electron microcopy and energy-dispersive X-ray spectroscopy. It was observed that the grains of these bulk Pr-doped SrTiO3 ceramics were enhanced with Pr-rich grain boundaries. Electronic and thermal transport properties were also investigated as a function of temperature and doping concentration. Such a microstructure was found to give rise to improved thermoelectric properties. Specifically, it resulted in a significant improvement in carrier mobility and the thermoelectric power factor. Simultaneously, it also led to a marked reduction in the thermal conductivity. As a result, a significant improvement (> 30%) in the thermoelectric figure of merit was achieved for the whole temperature range over all previously reported maximum values for SrTiO3-based ceramics. This synthesis demonstrates the steps for the preparation of bulk polycrystalline ceramics of non-uniformly Pr-doped SrTiO3.

为了研究上的SrTiO镨掺杂的效果3晶格，镨的溶解度的SrTiO共收集所制备的粉末和相应散装陶瓷作为镨含量的函数（ 图1）的X射线衍射图案3和次要相（多个）的形成。模式确认的SrTiO 3相的所有所制备的粉末，其中所述的反射可以被索引到一个立方晶格，空间群（ 图1A）的形成。从一个= 3.906对于x = 0（未掺杂）随着Pr含量中索引晶格参数的单调变化证...

Watch this Scientific Journal Video about Synthesis of Non-uniformly Pr-doped SrTiO3 Ceramics and Their Thermoelectric Properties at JoVE.com

Synthesis of Non-uniformly Pr-doped SrTiO3 Ceramics and Their Thermoelectric Properties

A protocol for the synthesis and processing of polycrystalline SrTiO3 ceramics doped non-uniformly with Pr is presented along with the investigation of their thermoelectric properties.

非均匀掺Pr的SrTiO的合成<sub&gt; 3</sub&gt;陶瓷及其热电性能

We demonstrate a novel synthesis strategy for the preparation of Pr-doped SrTiO3 ceramics via a combination of solid state reaction and spark plasma ...

synthesis-non-uniformly-pr-doped-srtio3-ceramics-their-thermoelectric

Research

JoVE Journal

Chemistry

Synthesis of Non-uniformly Pr-doped SrTiO3 Ceramics and Their Thermoelectric Properties

9.8K 次观看.  Clemson University. A protocol for the synthesis and processing of polycrystalline SrTiO3 ceramics doped non-uniformly with Pr is presented along with the investigation of their thermoelectric properties.

视频: Synthesis of Non-uniformly Pr-doped SrTiO3 Ceramics and Their Thermoelectric Properties

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 ...

科研

工程学

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

Synthesis and Reaction Chemistry of Nanosize Monosodium Titanate

This paper describes the synthesis and peroxide-modification of nanosize monosodium titanate (nMST), along with an ion-exchange reaction to load the material with Au(III) ions. The synthesis method was derived from a sol-gel process used to produce micron-sized monosodium titanate (MST), with several key modifications, including altering reagent concentrations, omitting a particle seed step, and introducing a non-ionic surfactant to facilitate control of particle formation and growth. The resultant nMST material exhibits spherical-shaped particle morphology with a monodisperse distribution of particle diameters in the range from 100 to 150&#160;nm. The nMST material was found to have a Brunauer-Emmett-Teller (BET) surface area of 285 m2g-1, which is more than an order of magnitude higher than the micron-sized MST. The isoelectric point of the nMST measured 3.34 pH units, which is a pH unit lower than that measured for the micron-size MST. The nMST material was found to serve as an effective ion exchanger under weakly acidic conditions for the preparation of an Au(III)-exchange nanotitanate. In addition, the formation of the corresponding peroxotitanate was demonstrated by reaction of the nMST with hydrogen peroxide.

The surfactant mediated sol-gel synthesis of nanosized monosodium titanate is described, along with preparation of the corresponding peroxide modified material. An ion-exchange reaction with Au(III) is also presented.

纳米尺寸钛酸二氢钠的合成和化学反应

This paper describes the synthesis and peroxide-modification of nanosize monosodium titanate (nMST), along with an ion-exchange reaction to load the ...

Epitaxial Growth of Perovskite Strontium Titanate on Germanium via Atomic Layer Deposition

Atomic layer deposition (ALD) is a commercially utilized deposition method for electronic materials. ALD growth of thin films offers thickness control and conformality by taking advantage of self-limiting reactions between vapor-phase precursors and the growing film. Perovskite oxides present potential for next-generation electronic materials, but to-date have mostly been deposited by physical methods. This work outlines a method for depositing SrTiO3 (STO) on germanium using ALD. Germanium has higher carrier mobilities than silicon and therefore offers an alternative semiconductor material with faster device operation. This method takes advantage of the instability of germanium's native oxide by using thermal deoxidation to clean and reconstruct the Ge (001) surface to the 2&#215;1 structure. 2-nm thick, amorphous STO is then deposited by ALD. The STO film is annealed under ultra-high vacuum and crystallizes on the reconstructed Ge surface. Reflection high-energy electron diffraction (RHEED) is used during this annealing step to monitor the STO crystallization. The thin, crystalline layer of STO acts as a template for subsequent growth of STO that is crystalline as-grown, as confirmed by RHEED. In situ X-ray photoelectron spectroscopy is used to verify film stoichiometry before and after the annealing step, as well as after subsequent STO growth. This procedure provides framework for additional perovskite oxides to be deposited on semiconductors via chemical methods in addition to the integration of more sophisticated heterostructures already achievable by physical methods.

This work details the procedures for the growth and characterization of crystalline SrTiO3 directly on germanium substrates by atomic layer deposition. The procedure illustrates the ability of an all-chemical growth method to integrate oxides monolithically onto semiconductors for metal-oxide semiconductor devices.

锗通过原子层沉积钙钛矿型钛酸锶的外延生长

Atomic layer deposition (ALD) is a commercially utilized deposition method for electronic materials. ALD growth of thin films offers thickness control and ...

Spark Plasma Sintering Apparatus Used for the Formation of Strontium Titanate Bicrystals

A spark plasma sintering apparatus was used as a novel method for diffusion bonding of two single crystals of strontium titanate to form bicrystals with one twist grain boundary. This apparatus utilizes high uniaxial pressure and a pulsed direct current for rapid consolidation of material. Diffusion bonding of strontium titanate bicrystals without fracture, in a spark plasma sintering apparatus, is possible at high pressures due to the unusual temperature dependent plasticity behavior of strontium titanate. We demonstrate a method for the successful formation of bicrystals at accelerated time scales and lower temperatures in a spark plasma sintering apparatus compared to bicrystals formed by conventional diffusion bonding parameters. Bond quality was verified by scanning electron microscopy. A clean and atomically abrupt interface containing no secondary phases was observed using transmission electron microscopy techniques. Local changes in bonding across the boundary was characterized by simultaneous scanning transmission electron microscopy and spatially resolved electron energy-loss spectroscopy.

A viable technique for the formation of strontium titanate bicrystals at high pressure and fast heating rate via the spark plasma sintering apparatus is developed.

放电等离子烧结设备中使用的钛酸锶双晶体的形成

A spark plasma sintering apparatus was used as a novel method for diffusion bonding of two single crystals of strontium titanate to form bicrystals with ...

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 ...

Chemical Synthesis of Porous Barium Titanate Thin Film and Thermal Stabilization of Ferroelectric Phase by Porosity-Induced Strain

Barium titanate (BaTiO3, hereafter BT) is an established ferroelectric material first discovered in the 1940s and still widely used because of its well-balanced ferroelectricity, piezoelectricity, and dielectric constant. In addition, BT does not contain any toxic elements. Therefore, it is considered to be an eco-friendly material, which has attracted considerable interest as a replacement for lead zirconate titanate (PZT). However, bulk BT loses its ferroelectricity at approximately 130 &#176;C, thus, it cannot be used at high temperatures. Because of the growing demand for high-temperature ferroelectric materials, it is important to enhance the thermal stability of ferroelectricity in BT. In previous studies, strain originating from the lattice mismatch at hetero-interfaces has been used. However, the sample preparation in this approach requires complicated and expensive physical processes, which are undesirable for practical applications.
In this study, we propose a chemical synthesis of a porous material as an alternative means of introducing strain. We synthesized a porous BT thin film using a surfactant-assisted sol-gel method, in which self-assembled amphipathic surfactant micelles were used as an organic template. Through a series of studies, we clarified that the introduction of pores had a similar effect on distorting the BT crystal lattice, to that of a hetero-interface, leading to the enhancement and stabilization of ferroelectricity. Owing to its simplicity and cost effectiveness, this fabrication process has considerable advantages over conventional methods.

Here, we present a protocol for the synthesis of porous barium titanate (BaTiO3) thin film by a surfactant-assisted sol-gel method, in which self-assembled amphipathic surfactant micelles are used as an organic template.

孔隙诱导应变法合成多孔钛酸钡薄膜及铁电相热稳定性

Barium titanate (BaTiO3, hereafter BT) is an established ferroelectric material first discovered in the 1940s and still widely used because of its ...

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 ...

通过射频溅射将 Bi2Te3 和 Sb2Te3 薄膜沉积在玻璃基板上

Fabrication of Bi2Te3 and Sb2Te3 Thermoelectric Thin Films using Radio Frequency Magnetron Sputtering Technique

Through various studies on thermoelectric (TE) materials, thin film configuration gives superior advantages over conventional bulk TEs, including adaptability to curved and flexible substrates. Several different thin film deposition methods have been explored, yet magnetron sputtering is still favorable due to its high deposition efficiency and scalability. Therefore, this study aims to fabricate a bismuth telluride (Bi2Te3) and antimony telluride (Sb2Te3) thin film via the radio frequency (RF) magnetron sputtering method. The thin films were deposited on soda lime glass substrates at ambient temperature. The substrates were first washed using water and soap, ultrasonically cleaned with methanol, acetone, ethanol, and deionized water for 10 min, dried with nitrogen gas and hot plate, and finally treated under UV ozone for 10 min to remove residues before the coating process. A sputter target of Bi2Te3 and Sb2Te3 with Argon gas was used, and pre-sputtering was done to clean the target&#39;s surface. Then, a few clean substrates were loaded into the sputtering chamber, and the chamber was vacuumed until the pressure reached 2 x 10-5 Torr. The thin films were deposited for 60 min with Argon flow of 4 sccm and RF power at 75 W and 30 W for Bi2Te3 and Sb2Te3, respectively. This method resulted in highly uniform n-type Bi2Te3 and p-type Sb2Te3 thin films.

作者聚焦:通过射频磁控溅射实现高性能热电薄膜的进展

The manuscript describes a protocol for radio frequency magnetron sputtering of Bi2Te3 and Sb2Te3 thermoelectric thin films on glass substrates, which represents a reliable deposition method that provides a wide range of applications with the potential for further development.

非均匀掺Pr的SrTiO的合成

摘要

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此视频中的章节

空间密闭的复合氧化物制备

原子定义模板复合氧化物薄膜的外延生长

纳米尺寸钛酸二氢钠的合成和化学反应

锗通过原子层沉积钙钛矿型钛酸锶的外延生长

放电等离子烧结设备中使用的钛酸锶双晶体的形成

金属/LaAlO 的生长和静电/化学性质₃/SrTiO₃异

孔隙诱导应变法合成多孔钛酸钡薄膜及铁电相热稳定性

组分变熵稳定氧化物的体积和薄膜合成

通过生长和退火过程中的氧空位控制来调整氧化物性能

使用射频磁控溅射技术制备Bi₂Te₃ 和Sb₂Te₃ 热电薄膜

非均匀掺Pr的SrTiO的合成

摘要

探索更多视频

此视频中的章节

空间密闭的复合氧化物制备

原子定义模板复合氧化物薄膜的外延生长

纳米尺寸钛酸二氢钠的合成和化学反应

锗通过原子层沉积钙钛矿型钛酸锶的外延生长

放电等离子烧结设备中使用的钛酸锶双晶体的形成

金属/LaAlO 的生长和静电/化学性质3/SrTiO3异

孔隙诱导应变法合成多孔钛酸钡薄膜及铁电相热稳定性

组分变熵稳定氧化物的体积和薄膜合成

通过生长和退火过程中的氧空位控制来调整氧化物性能

使用射频磁控溅射技术制备Bi2Te3 和Sb2Te3 热电薄膜

金属/LaAlO 的生长和静电/化学性质₃/SrTiO₃异

使用射频磁控溅射技术制备Bi₂Te₃ 和Sb₂Te₃ 热电薄膜