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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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...

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 border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>SrCO3 Powder, 99.9%</td>
			<td>Sigma Aldrich</td>
			<td>472018</td>
			<td></td>
		</tr>
		<tr>
			<td>TiO2 Nanopowder, 99.5%</td>
			<td>Sigma Aldrich</td>
			<td>718467</td>
			<td></td>
		</tr>
		<tr>
			<td>Pr2O3 Sintered Lumps, 99.9%</td>
			<td>Alfa Aesar</td>
			<td>35663&#160;</td>
			<td></td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Name of&#160; Equipment</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Spark Plasma Sintering&#160;</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&#160; 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 ...

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

9.7K 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.