This work was supported by the National Natural Science Foundation of China (Grant No. 11374245), the NIH under Grant No. P41-EB2182, the Natural Science Foundation of Fujian Province, China (Grant No. 2013J01163), and the Open Research Fund of the State Key Laboratory of Acoustics, Chinese Academy of Science (Grant No. SKLA201306).

1.样品制备注意:所希望的大小的PZT-4陶瓷样品可以从许多的PZT陶瓷制造商可以直接订购。一个也可以由使用金刚石切割机更大的PZT陶瓷块切取试样，然后repole恢复通过切割和抛光depoling引起样品。这里，样品形状为具有3 mm与10mm之间的每个维度的平行六面。尺寸较大的样品是没有必要的，但如果样本太小精度可能受到影响。 <ol><li>擦亮长方体样品的表面上有机玻璃磁盘使用的 Al 2 O 3粉末。 <ol><li>首先，由杆和样品加热至60℃胶样品使用非常薄的蜡层的金属棒状的底表面。然后冷却到室温。紧密地配合在杆成具有较大外径的金属圆筒，使气缸和样品的底表面可以是抛光的TOG醚来保证抛光样品表面的平整度。 </li><li>湿用水瓶玻璃板然后撒上6微米的 Al 2 O 3粉末到潮湿的表面。将样品支架与粘在其上板样品并进行圆周运动研磨样品表面平坦。清洗有机玻璃板，彻底的样品架。 </li><li>洒3微米的 Al 2 O 3粉末在潮湿玻璃板并重复进行再次研磨，使样品表面会更光滑。洗干净的一切。 </li><li>由该组件加热至60℃以熔化蜡取下样品保持器的。清洁用丙酮样品表面上的剩余蜡。 </li><li>抛光用同样的步骤样品的所有6个表面上。 </li></ol></li><li>测量样品的使用微米尺寸和记录结果。这里，在图1所示的PZT-4样品的尺寸如下:● </EM&gt; X =4.461毫米，L Y =6.073毫米和l Z =4.914毫米。 </li><li>使用数字分析天平测量样品的质量。 </li><li>由体积除以质量，以获得质量密度ρ。 </li></ol> 2.脉冲回波超声测量注:在本文中， <img alt="15式" src="/files/ftp_upload/53461/image015.jpg" />和<img alt="16式" src="/files/ftp_upload/53461/image016.jpg" />代表第i行第 j以恒定电场和恒定电位移，分别弹性刚度张量的列元素; <img alt="17式" src="/files/ftp_upload/53461/image017.jpg" />和<img alt="18式" src="/files/ftp_upload/53461/image018.jpg" />代表第i行第 j在恒定电弹性柔顺张量的列元素场和恒定电位移，分别; ÐIJ表示第i行第 j压电应变张量的列元素; ËIJ表示第i行第 j压电应力张量的列元素; <img alt="21式" src="/files/ftp_upload/53461/image021.jpg" />和<img alt="式（22）" src="/files/ftp_upload/53461/image022.jpg" />代表第i行第 j 个夹紧和自由介电常数柱元件，分别。所有的基体材料常数是福格特符号。 <ol><li>打开脉冲接收器。将模式设置为的P / E为脉冲回波测量。 </li><li>连接一个纵波换能器（15兆赫）和一个数字示波器的脉冲接收器。 </li><li>把换能器到所述样品表面沿x方向的一些耦合润滑脂在两者之间。注意，偏振可怕ction被定义为z轴。 </li><li>按数字示波器的控制面板上的光标键;按侧面菜单按钮，垂直条，然后旋转通用旋钮一个光标线移动到第一回波信号的最高峰。 </li><li>按SELECT键，然后旋转通用旋钮另一个光标线移动到相应的峰值在第二回波信号。 </li><li>在标有Δ的地方读取数值:在屏幕上，这是飞行的往返时间， <img alt="23式" src="/files/ftp_upload/53461/image023.jpg" />沿x轴的纵波脉冲。 </li><li>沿x方向计算纵波速度， <img alt="24式" src="/files/ftp_upload/53461/image024.jpg" />通过除以两倍的样品的厚度（往返距离） <img alt="27式" src="/files/ftp_upload/53461/image027.jpg" /> ，然后确定弹性常数<im克ALT ="式29"SRC ="/文件/ ftp_upload / 53461 / image029.jpg"/&gt;使用下式: <img alt="30式" src="/files/ftp_upload/53461/image030.jpg" /> ，其中ρ是样品的密度。 </li><li>用剪力波换能器（5兆赫）重复2.3-2.5并且使用公式确定剪切波速<img alt="33式" src="/files/ftp_upload/53461/image033.jpg" /> ，其中<img alt="34式" src="/files/ftp_upload/53461/image034.jpg" />是的飞行为沿x方向的剪力波的往返时间。确定剪切弹性不变<img alt="35式" src="/files/ftp_upload/53461/image035.jpg" />使用下式<img alt="36式" src="/files/ftp_upload/53461/image036.jpg" /> 。 </li><li>计算弹性常数<img alt="37式" src="/files/ftp_upload/53461/image037.jpg" />使用下式: <img alt="38式" src="/files/ftp_upload/53461/image038.jpg" /> 。这是用于与∞ 米对称PZT的样品配方。&lt;/ LI&gt; <li>放置一个剪切换能器（5兆赫）到样品的Z表面。记录飞行的往返时间， <img alt="39式" src="/files/ftp_upload/53461/image039.jpg" />沿使用数字示波器的z方向上的横波。计算的声速<img alt="40式" src="/files/ftp_upload/53461/image040.jpg" />使用下式: <img alt="41式" src="/files/ftp_upload/53461/image041.jpg" /> ，并确定的弹性常数<img alt="42式" src="/files/ftp_upload/53461/image042.jpg" />使用下式: <img alt="43式" src="/files/ftp_upload/53461/image043.jpg" /> 。 </li></ol> 3.测量介电常数的温度依赖性<ol><li>适用的导电银漆薄层到在x方向上用刷子将样品的两个表面。涂料可以以使相同样品可以在开路条件用于RUS测量以后很容易地擦去。 </li><li> CONNECT阻抗分析器控制计算机并开启两个。 </li><li>设置的启动和停止的阻抗分析仪的频率分别为10兆赫和40兆赫，对于频率扫描。因为介电常数&gt;&gt; 1这个PZT样品，计算出其介电常数<img alt="44式" src="/files/ftp_upload/53461/image044.jpg" />使用平行板近似<img alt="45式" src="/files/ftp_upload/53461/image045.jpg" /> ，其中所述电容<img alt="46式" src="/files/ftp_upload/53461/image046.jpg" />在35兆赫被测量，A是电极面积，t是试样的厚度。 </li><li>在16048A适配器连接到阻抗分析仪的四端子对端口。 </li><li>按阻抗分析仪显示校准菜单的CAL键。 </li><li>将适配器按键显示适配器设置在开始菜单，然后选择4TP 1M。 </li><li>连接LCUR和LPOT项在16048A inals至04294-61001的HPOT和HCUR终端。其他终端保持在开路状态。 </li><li>按SET OFUP键，显示适配器设置菜单。 </li><li>按PHASE COMP [ - ]键启动相位补偿数据测量。当完成相位补偿数据测量，软键标签变为PHASE COMP [DONE]。 </li><li>连接在16048A要在04294-61001的LCUR，LPOT，HPOT和HCUR终端LCUR，LPOT，HPOT和HCUR终端。 </li><li>按LOAD [ - ]键开始测量。当加载完成数据测量，软键标签更改为LOAD [DONE]。 </li><li>夹具连接到阻抗分析仪，并保持在开路状态。 </li><li>按CAL键，然后按软键灯具COMPEN显示灯具补偿菜单。 </li><li>按下OPEN [ - ]键启动开路数据测量。当负载数据测量完成，在SOFT键标签变为打开[ON]。 </li><li>短夹具通过将铜线的正和负引线之间。 </li><li>按短[ - ]键启动短路数据测量。当负载数据测量完成后，软键标签更改为短[ON]。 </li><li>修正了一个100Ω电阻夹具。按软键LOAD RESIST然后定义值，输入100，然后按键X1。 </li><li>按LOAD键。当加载完成数据测量，软键标签更改为LOAD [ON]。现在校准完毕。 </li><li>把样品在夹具上，然后把整个组装成低温试验箱，并关闭大门。 </li><li>按阻抗分析器面板上的键MEAS，并且选择<img alt="47式" src="/files/ftp_upload/53461/image047.jpg" /> 。 </li><li>使用控制计算机设置腔室温度至20℃。 </li><li>打开安装在连接到计算机的电子表格软件阻抗分析器来读取和从阻抗分析器记录数据。 </li><li>读取使用在计算机中的软件的电容数据和测量结果保存到文件中。 </li><li>与按室的控制面板上的UP键5℃的温度下步骤改变该室的温度。箱内温度后，在每个温度升高，重复步骤3.23变得稳定。 </li><li>确定夹紧介电常数的温度依赖性<img alt="公式3" src="/files/ftp_upload/53461/image003.jpg" />基于使用在35兆赫，在该电容变为几乎与频率无关的电容值的并联电容式。 </li><li>重置启动和停止的频率为1千赫兹和10千赫兹，分别。 </li><li>重复步骤3.21-3.24测量样品的低频电容的温度依赖性。保存测量结果。 </li><li>确定自由昼夜的温度依赖性ectric不变<img alt="48式" src="/files/ftp_upload/53461/image048.jpg" />使用低频电容在1千赫。 </li><li>删除使用丙酮的样品表面上的导电的银涂料。 </li><li>应用导电银漆沿极化z方向上的两个示例的表面。 </li><li>重复步骤3.3-3.28。确定被夹紧和自由介电常数的温度依赖性， <img alt="49式" src="/files/ftp_upload/53461/image049.jpg" />和<img alt="50式" src="/files/ftp_upload/53461/image050.jpg" /> 。 </li></ol>在室温和模式识别4.共振频率测量<ol><li>测量的共振频率。 <ol><li>把样品中的发送和RUS系统，仅在样品（ 图2）的相对的角接触的接收换能器之间。注意，触点软弹簧加载，并且施加的压力是非常二极管灯T，刚够举行的地方样本。因此，没有损害是由接触引起的。 </li><li>打开动态共振系统（ 图2）和连接到它的计算机上。 </li><li>运行动态共振系统的控制接口。设置开始频率f 1时，停止频率f 2和数据点的总数被收集Ñ。请选择N，使得（F 1 - F 2）/ N小于0.1千赫，以确保频率分辨率。对于此示例， 在设定f 1 = 200千赫，F 2 = 450 kHz和N = 8,192。 </li><li>测量在室温下该频率范围内的样品的共振谱和频谱保存到文件中。 </li><li>测量结果到一个文件中导出ASCII数据。 </li><li>有数据绘图软件打开ASCII数据。数据矩阵的第一列和第二列代表respo的实部和虚部NSE，分别为。 </li></ol></li><li>确定测量共振频率通讯模式。 <ol><li>积频率-幅度曲线（ 图3）。该峰对应于谐振样品的频率。 </li><li>计算使用测量室温全套张量常数的共振频率。的值<img alt="公式6" src="/files/ftp_upload/53461/image006.jpg" /> ， <img alt="公式7" src="/files/ftp_upload/53461/image007.jpg" /> ， <img alt="10式" src="/files/ftp_upload/53461/image010.jpg" />在步骤2.4-2.8进行了测定。的值<img alt="公式3" src="/files/ftp_upload/53461/image003.jpg" />和<img alt="公式4" src="/files/ftp_upload/53461/image004.jpg" />在步骤3.25和3.31进行了测定。由公式确定剪切压电常数e 15: <img alt="51式" src="/files/ftp_upload/53461/image051.jpg" /> 。估计初始输入VAL统一电力<img alt="52式" src="/files/ftp_upload/53461/image052.jpg" /> ， <img alt="53式" src="/files/ftp_upload/53461/image053.jpg" /> ， 电子 31和电子 33的基础上，使用组合技术从几个样品测量材料常数。用于计算的各模式的谐振频率的方程在参考文献被给予。 6。 </li><li>比较所计算的共振频率与实测以确定所测量的共振频率对应的模式。 </li><li>有所不同的猜测值<img alt="71式" src="/files/ftp_upload/53461/image071.jpg" /> ， <img alt="公式9" src="/files/ftp_upload/53461/image009.jpg" /> ， 电子 31和电子 33迭代地最小化所计算的和测量的谐振频率之间的总全局误差。在达到所需的精度时，迭代停止。 </li></ol></li></ol> 5.共振光谱Measurement在较高温度和全套材料常数的温度依赖性的测定<ol><li>测量样品的共振频率在较高的温度。 <ol><li>把样品架组装成一个空气炉（ 图4）。使用两个高温同轴电缆导线通过在炉壁上的孔的组件连接到RUS系统。 </li><li>仅在样品的对角放置在样品中的发射和接收换能器中已经在炉内，与接点之间。 </li><li>把热电偶样品实际温度读数附近。热电偶连接到温度计的炉外。 </li><li>关闭炉门。 </li><li>转动RUS系统的控制接口上。设置的启动和停止的频率，以分别为200千赫和450千赫，和数据点到8,192的数目。 </li><li>运行RUS系统测量软件，测量共振FRE样品的下以及结果保存到文件中。 </li><li>增加试样的温度与ΔT= 5℃的步骤。重复5.1.6达到所需的温度，直到。给保存在不同的名称每个文件。 注意:温度上限是由连接导线和换能器来确定。这里，RUS单元具有200℃的温度上限。 </li></ol></li><li>确定全套材料常数的温度依赖性。 <ol><li>重复步骤4.1.5，对于每一个数据集在不同的温度和4.1.6 4.2.1。 </li><li>识别每个谐振频率的模式。使用在温度T确定为下一个温度T +ΔT的基准模式。 </li><li>适合与各模式对应到一个简单的函数测得的共振频率的温度依赖性（例如，线性或二次函数），使用绘图软件。 </li><li>确定从适合的全套材料常数使用该解决RUS向后问题自写的计算机程序（ 图5， 图6）在每个温度泰德共振频率。 注意:识别模式的共振频率作为输入参数数值计算。从共振频率确定材料常数的过程发现的偏差函数的局部极小的非线性最小二乘问题<img alt="54式" height="30" src="/files/ftp_upload/53461/image054.jpg" width="135" /> ，其中<img alt="式（55）" src="/files/ftp_upload/53461/image055.jpg" />是计算的共振频率， <img alt="56式" src="/files/ftp_upload/53461/image056.jpg" />是从测得的结果的拟合共振频率，而w i是加权因子。从测得的谐振频率未知材料常数的计算中的计算机代码被写基于文伯格 - Mauquardt（L实现LM算法时，M）算法8，并在MINPACK 9一些FORTRAN子程序被称为。 </li></ol></li><li>检查的全套材料常数自洽。 <ol><li>计算自由介电常数<img alt="48式" src="/files/ftp_upload/53461/image048.jpg" />和<img alt="50式" src="/files/ftp_upload/53461/image050.jpg" />从反演结果与直接测量的人对它们进行比较（ 图7）10。 </li><li>查所获得的数据集以确定它们是否服从热力学稳定性的条件下，例如， <img alt="58式" src="/files/ftp_upload/53461/image058.jpg" />对于PZT情况。 </li><li>使用比较D 15-计算出的值<img alt="59式" src="/files/ftp_upload/53461/image059.jpg" />和<img alt="60式" src="/files/ftp_upload/53461/image060.jpg" />和d 33的值计算运用<img alt="61式" src="/files/ftp_upload/53461/image061.jpg" />和<img alt="62式" src="/files/ftp_upload/53461/image062.jpg" /> 。 注意:这些关系将对于不同的对称性不同，但原理是相同的。通常，如果相对误差是预测和测量量之间小于5％，结果将被视为自洽11。在一些公开的数据，当数量是使用不同的公式计算出4,11甚至符号将是错误的。 </li></ol></li></ol>

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A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Properties of Morgan Electroceramic ceramics. Technique publication TP-226. , (2000).</li><li>Migliori, A., Sarrao, J. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Resonant ultrasound spectroscopy. , (1997).</li><li>Zadler, B. J., Le Rousseau, J. H. L., Scales, J. A., Smith, M. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Resonant+ultrasound+spectroscopy:+Theory+and+application.">Resonant ultrasound spectroscopy: Theory and application.</a> Geophys. J. Int. 156, 154-169 (2004).</li></ol>

Authors have nothing to disclose.

这里介绍的RUS技术可以只使用一个样本，它消除了由样品属性的变化来样，这样的自我一致性可以保证测量误差的全套材料常数。该方法可用于任何固体材料具有高品质因数Q，不管他们是压电或没有。所有其他标准表征技术需要多个样品得到充分的数据和难以实现自我一致的数据。 它精确地测量弹性常数是非常重要的<img alt="公式6" src="/files/ftp_upload/53461/image006.jpg" /> ， <img al...

锆钛酸铅（PZT）的压电陶瓷，（1-x）的PbZrO 3 -xPbTiO 3，和其衍生物具有自20世纪50年代1被广泛用于超声换能器，传感器和致动器。许多这些机电装置的在高的温度范围，如在航天和地下测井使用。此外，高功率器件，如治疗超声换能器，压电变压器和声纳投影机，在操作期间经常升温。这种温度上升会改变谐振频率与换能器的焦点，从而导致严重的性能下降。高强度聚焦超声（HIFU）的技术，在临床实践中用于肿瘤的治疗已被使用，使用由PZT陶瓷的超声换能器。在操作过程中，这些换能器的温度会升高，致使PZT谐振器的材料常数的变化，这反过来将改变对HIFU焦点以及输出功率2,3。焦点的转移可能会导致严重的不想要的结果， 即健康组织被破坏，而不是癌组织。另一方面，如果该焦点偏移可以预测，人们可以使用电子设计来校正这种变化。因此，测量压电材料的全套材料特性的温度依赖性是许多机电装置，特别是高功率器件的设计和评价非常重要。 极化的铁电材料是目前已知的最好的压电材料。事实上，几乎所有目前使用的压电材料是铁电材料，包括固溶液PZT陶瓷和（1-x）的铅（镁1/3 Nb的2/3）O 3 -xPbTiO 3（PMN-PT）单晶。阻抗谐振方法的IEEE（电气和电子工程师协会）要求5-7样品drasti卡利以表征的全套材料不同的几何形状常数4。它几乎是不可能获得使用铁电材料在IEEE阻抗谐振方法，因为极化的程度取决于样品几何（边界条件）自洽全套矩阵数据，而样品性质取决于极化水平。以避免由于样品采样变化问题，所有常量应该从一个样品进行测量。 Li等报道了在室温下一个样品的所有常量的成功测量用脉冲回波超声和逆阻抗谱5的组合。不幸的是，这种技术很难在升高的温度，因为它是不可能直接在炉内进行超声测量来执行。也有不能够在高温下工作市售剪切换能器。此外，耦合润滑脂该结合的反能器和样品不能在高温下工作。 在原则上，RUS技术具有以确定压电材料及其温度依赖性的仅使用一个样品6,7的全套材料常数的能力。但也有正常实施RUS技术的几个关键步骤。首先，在室温下的全套张量特性应准确使用脉冲回波和RUS技术的组合来确定。第二，这个房间温度数据集可以被用于预测的谐振频率，并以识别对应的模式匹配所测量的。第三，为从室温升高温度的每个小增量，需要，以便在从所测量的共振谱这个新的温度来检索全套常数针对所测量的共振谱进行频谱重建。然后，使用新的数据集作为新的起点，我们可以<html>另一个小的温度逐步增加的温度下一个温度，以获得全套的常量。继续这一过程将允许我们获得的全套材料常数的温度依赖性。 这里，一个PZT-4压电陶瓷样品用于说明RUS技术的测量程序。该极化PZT-4陶瓷有10个独立的材料常数∞m对称性:5的弹性常数，压电3常量和2的介电常数。由于介电常数不敏感共振频率的变化，它们分别使用相同的样品进行测量。夹持介电常数的温度依赖性<img alt="公式3" src="/files/ftp_upload/53461/image003.jpg" />和<img alt="公式4" src="/files/ftp_upload/53461/image004.jpg" />直接从电容测量测定，而游离介电常数OAD / 53461 / image005.jpg"/&gt;和<img alt="公式（2）" src="/files/ftp_upload/53461/image002.jpg" />同时测定被用作数据一致性检查。在恒定电场弹性刚度常数的温度依赖性<img alt="公式6" src="/files/ftp_upload/53461/image006.jpg" /> ， <img alt="公式7" src="/files/ftp_upload/53461/image007.jpg" /> ， <img alt="式（8）" src="/files/ftp_upload/53461/image008.jpg" /> ， <img alt="公式9" src="/files/ftp_upload/53461/image009.jpg" />和<img alt="10式" src="/files/ftp_upload/53461/image010.jpg" />和压电常数的压力ê15，E 31和E 33人通过使用相同的样本RUS技术确定。

<table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always">
	<tbody>
		<tr>
			<td>PZT-4</td>
			<td>TRS</td>
			<td></td>
		</tr>
		<tr>
			<td>paraffin</td>
			<td>MTI Corporation</td>
			<td>8002-74-2</td>
		</tr>
		<tr>
			<td>conductive silver paint</td>
			<td>MG Chemicals</td>
			<td>842-20G</td>
		</tr>
		<tr>
			<td>Al2O3 Powder</td>
			<td>MTI Corporation</td>
			<td></td>
		</tr>
		<tr>
			<td>coupling grease</td>
			<td>Panametrics</td>
			<td></td>
		</tr>
	</tbody>
</table>

characterization of full set material constants and their temperature dependence for piezoelectric materials using resonant ultrasound spectroscopy

在高功率机电装置的操作中，温度上升是不可避免的因机械和电损耗，从而导致的器件性能的劣化。为了评价使用计算机模拟这种劣化，在高温下充分基质材料特性需要作为输入。它是非常困难的测量对铁电体材料，例如数据由于不同的几何形状的样品之间的强烈的各向异性的性质和属性的变化。因为去极化的程度是由IEEE（电气和电子工程师协会）阻抗共振技术，这需要几个样品用完全不同的几何形状得到的边界条件依赖性，数据，通常缺乏自我一致性。谐振超声光谱（RUS）技术允许仅使用一个样品进行测量的全套材料常数，其可以消除由于样品采样variat错误离子。详细RUS过程这里演示使用锆钛酸铅（PZT-4）压电陶瓷样品。在该示例中，材料常数的成套从室温测到120℃。测得的自由介电常数<img alt="式（1）" src="/files/ftp_upload/53461/image001.jpg" />和<img alt="公式（2）" src="/files/ftp_upload/53461/image002.jpg" />分别与基于所测量的全套数据计算那些比较，并且压电常数ð15和d 33分别使用不同的公式还计算。良好的协议是在温度，这证实了RUS获得的数据集的自洽的整个范围内找到。

在反演中使用的LM法算法是一个局部最小取景器。因此，弹性刚度常数的初始值<img alt="公式6" src="/files/ftp_upload/53461/image006.jpg" /> ， <img alt="公式7" src="/files/ftp_upload/53461/image007.jpg" /> ， <img alt="式（8）" src="/files/ftp_upload/53461/image008.jpg" /> ， <img alt="公式9" src="/files/ftp_upload/53461/image009.jpg" />和<img alt="10式" src="/files/ftp_upload/53461/image010.jpg" />和压电常数，E 15，E<...

Watch this Scientific Journal Video about Characterization of Full Set Material Constants and Their Temperature Dependence for Piezoelectric Materials Using Resonant Ultrasound Spectroscopy at JoVE.co

Characterization of Full Set Material Constants and Their Temperature Dependence for Piezoelectric Materials Using Resonant Ultrasound Spectroscopy

This protocol describes the procedure of measuring the temperature dependence of the full set material constants of piezoelectric materials using resonant ultrasound spectroscopy (RUS).

全套材料常数表征及其温度依赖性的压电材料使用共振超声波谱

During the operation of high power electromechanical devices, a temperature rise is unavoidable due to mechanical and electrical losses, causing the ...

characterization-full-set-material-constants-their-temperature

Universidad de Cartagena UDEC

Research

JoVE Journal

Engineering

9.4K 次观看.  Xiamen University. This protocol describes the procedure of measuring the temperature dependence of the full set material constants of piezoelectric materials using resonant ultrasound spectroscopy (RUS). 

视频: Characterization of Full Set Material Constants and Their Temperature Dependence for Piezoelectric Materials Using Resonant Ultrasound Spectroscopy

Concurrent Quantitative Conductivity and Mechanical Properties Measurements of Organic Photovoltaic Materials using AFM

Organic photovoltaic (OPV) materials are inherently inhomogeneous at the nanometer scale. Nanoscale inhomogeneity of OPV materials affects performance of photovoltaic devices. Thus, understanding of spatial variations in composition as well as electrical properties of OPV materials is of paramount importance for moving PV technology forward.1,2 In this paper, we describe a protocol for quantitative measurements of electrical and mechanical properties of OPV materials with sub-100 nm resolution. Currently, materials properties measurements performed using commercially available AFM-based techniques (PeakForce, conductive AFM) generally provide only qualitative information. The values for resistance as well as Young's modulus measured using our method on the prototypical ITO/PEDOT:PSS/P3HT:PC61BM system correspond well with literature data. The P3HT:PC61BM blend separates onto PC61BM-rich and P3HT-rich domains. Mechanical properties of PC61BM-rich and P3HT-rich domains are different, which allows for domain attribution on the surface of the film. Importantly, combining mechanical and electrical data allows for correlation of the domain structure on the surface of the film with electrical properties variation measured through the thickness of the film.

Organic photovoltaic (OPV) materials are inherently inhomogeneous at the nanometer scale. Nanoscale inhomogeneity of OPV materials affects performance of photovoltaic devices. In this paper, we describe a protocol for quantitative measurements of electrical and mechanical properties of OPV materials with sub-100 nm resolution.

并行定量的导电性和力学性能测试的有机光伏材料利用原子力显微镜

Organic photovoltaic  (OPV) materials are inherently inhomogeneous at the nanometer scale. Nanoscale  inhomogeneity of OPV materials affects performance ...

科研

工程学

Characterization of Electrode Materials for Lithium Ion and Sodium Ion Batteries Using Synchrotron Radiation Techniques

Intercalation compounds such as transition metal oxides or phosphates are the most commonly used electrode materials in Li-ion and Na-ion batteries. During insertion or removal of alkali metal ions, the redox states of transition metals in the compounds change and structural transformations such as phase transitions and/or lattice parameter increases or decreases occur. These behaviors in turn determine important characteristics of the batteries such as the potential profiles, rate capabilities, and cycle lives. The extremely bright and tunable x-rays produced by synchrotron radiation allow rapid acquisition of high-resolution data that provide information about these processes. Transformations in the bulk materials, such as phase transitions, can be directly observed using X-ray diffraction (XRD), while X-ray absorption spectroscopy (XAS) gives information about the local electronic and geometric structures (e.g.&#160;changes in redox states and bond lengths). In situ experiments carried out on operating cells are particularly useful because they allow direct correlation between the electrochemical and structural properties of the materials. These experiments are time-consuming and can be challenging to design due to the reactivity and air-sensitivity of the alkali metal anodes used in the half-cell configurations, and/or the possibility of signal interference from other cell components and hardware. For these reasons, it is appropriate to carry out ex situ experiments (e.g.&#160;on electrodes harvested from partially charged or cycled cells) in some cases. Here, we present detailed protocols for the preparation of both ex situ and in situ samples for experiments involving synchrotron radiation and demonstrate how these experiments are done.

We describe the use of synchrotron X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) techniques to probe details of intercalation/deintercalation processes in electrode materials for Li-ion and Na-ion batteries. Both in situ and ex situ experiments are used to understand structural behavior relevant to the operation of devices

正极材料的同步辐射技术锂离子和钠离子电池表征

Intercalation compounds such as transition metal oxides or phosphates are the most commonly used electrode materials in Li-ion and Na-ion batteries. ...

Characterization of Thermal Transport in One-dimensional Solid Materials

The TET (transient electro-thermal) technique is an effective approach developed to measure the thermal diffusivity of solid materials, including conductive, semi-conductive or nonconductive one-dimensional structures. This technique broadens the measurement scope of materials (conductive and nonconductive) and improves the accuracy and stability. If the sample (especially biomaterials, such as human head hair, spider silk, and silkworm silk) is not conductive, it will be coated with a gold layer to make it electronically conductive. The effect of parasitic conduction and radiative losses on the thermal diffusivity can be subtracted during data processing. Then the real thermal conductivity can be calculated with the given value of volume-based specific heat (&#961;cp), which can be obtained from calibration, noncontact photo-thermal technique or measuring the density and specific heat separately. In this work, human head hair samples are used to show how to set up the experiment, process the experimental data, and subtract the effect of parasitic conduction and radiative losses.

The TET (transient electro-thermal) technique is an effective approach developed to measure the thermal diffusivity of solid materials.

在一维固体材料的热传输的特性

The TET (transient electro-thermal) technique is an effective approach developed to measure the thermal diffusivity of solid materials, including ...

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.

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 ...

A Method for Studying the Temperature Dependence of Dynamic Fracture and Fragmentation

The dynamic fracture of a body is a late-stage phenomenon typically studied under simplified conditions, in which a sample is deformed under uniform stress and strain rate. This can be produced by evenly loading the inner surface of a cylinder. Due to the axial symmetry, as the cylinder expands the wall is placed into a tensile hoop stress that is uniform around the circumference. While there are various techniques to generate this expansion such as explosives, electromagnetic drive, and existing gas gun techniques they are all limited in the fact that the sample cylinder must be at room temperature. We present a new method using a gas gun that facilitates experiments on cylinders from 150 K to 800 K with a consistent, repeatable loading. These highly diagnosed experiments are used to examine the effect of temperature on the fracture mechanisms responsible for failure, and their resulting influence on fragmentation statistics. The experimental geometry employs a steel ogive located inside the target cylinder, with the tip located about halfway in. A single stage light gas gun is then used to launch a polycarbonate projectile into the cylinder at 1,000 m/sec-1. The projectile impacts and flows around the rigid ogive, driving the sample cylinder from the inside. The use of a non-deforming ogive insert allows us to install temperature control hardware inside the rear of the cylinder. Liquid nitrogen (LN2) is used for cooling and a resistive high current load for heating. Multiple channels of upshifted photon Doppler velocimetry (PDV) track the expansion velocity along the cylinder enabling direct comparison to computer simulations, while High speed imaging is used to measure the strain to failure. The recovered cylinder fragments are also subject to optical and electron microscopy to ascertain the failure mechanism.

Fracture and fragmentation are late stage phenomena in dynamic loading scenarios and are typically studied using explosives. We present a technique for driving expansion using a gas gun which uniquely enables control of both loading rate and sample temperature.

为研究动态断裂及破碎的温度敏感性的方法

The dynamic fracture of a body is a late-stage phenomenon typically studied under simplified conditions, in which a sample is deformed under uniform ...

Electron Channeling Contrast Imaging for Rapid III-V Heteroepitaxial Characterization

Misfit dislocations in heteroepitaxial layers of GaP grown on Si(001) substrates are characterized through use of electron channeling contrast imaging (ECCI) in a scanning electron microscope (SEM). ECCI allows for imaging of defects and crystallographic features under specific diffraction conditions, similar to that possible via plan-view transmission electron microscopy (PV-TEM). A particular advantage of the ECCI technique is that it requires little to no sample preparation, and indeed can use large area, as-produced samples, making it a considerably higher throughput characterization method than TEM. Similar to TEM, different diffraction conditions can be obtained with ECCI by tilting and rotating the sample in the SEM. This capability enables the selective imaging of specific defects, such as misfit dislocations at the GaP/Si interface, with high contrast levels, which are determined by the standard invisibility criteria. An example application of this technique is described wherein ECCI imaging is used to determine the critical thickness for dislocation nucleation for GaP-on-Si by imaging a range of samples with various GaP epilayer thicknesses. Examples of ECCI micrographs of additional defect types, including threading dislocations and a stacking fault, are provided as demonstration of its broad, TEM-like applicability. Ultimately, the combination of TEM-like capabilities &#8211; high spatial resolution and richness of microstructural data &#8211; with the convenience and speed of SEM, position ECCI as a powerful tool for the rapid characterization of crystalline materials.

The use of electron channeling contrast imaging in a scanning electron microscope to characterize defects in III-V/Si heteroexpitaxial thin films is described. This method yields similar results to plan-view transmission electron microscopy, but in significantly less time due to lack of required sample preparation.

电子通道造影的快速III-V异质特征

Misfit dislocations in heteroepitaxial layers of GaP grown on Si(001) substrates are characterized through use of electron channeling contrast imaging ...

Characterization of Nanocrystal Size Distribution using Raman Spectroscopy with a Multi-particle Phonon Confinement Model

Analysis of the size distribution of nanocrystals is a critical requirement for the processing and optimization of their size-dependent properties. The common techniques used for the size analysis are transmission electron microscopy (TEM), X-ray diffraction (XRD) and photoluminescence spectroscopy (PL). These techniques, however, are not suitable for analyzing the nanocrystal size distribution in a fast, non-destructive and a reliable manner at the same time. Our aim in this work is to demonstrate that size distribution of semiconductor nanocrystals that are subject to size-dependent phonon confinement effects, can be quantitatively estimated in a non-destructive, fast and reliable manner using Raman spectroscopy. Moreover, mixed size distributions can be separately probed, and their respective volumetric ratios can be estimated using this technique. In order to analyze the size distribution, we have formulized an analytical expression of one-particle PCM and projected it onto a generic distribution function that will represent the size distribution of analyzed nanocrystal. As a model experiment, we have analyzed the size distribution of free-standing silicon nanocrystals (Si-NCs) with multi-modal size distributions. The estimated size distributions are in excellent agreement with TEM and PL results, revealing the reliability of our model.

We demonstrate how to determine the size distribution of semiconductor nanocrystals in a quantitative manner using Raman spectroscopy employing an analytically defined multi-particle phonon confinement model. Results obtained are in excellent agreement with the other size analysis techniques like transmission electron microscopy and photoluminescence spectroscopy.

使用拉曼光谱与多颗粒的声子坐月子型号纳米大小分布的特征

Analysis of the size distribution of nanocrystals is a critical requirement for the processing and optimization of their size-dependent properties. The ...

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 ...

Applying X-ray Imaging Crystal Spectroscopy for Use as a High Temperature Plasma Diagnostic

X-ray spectra provide a wealth of information on high temperature plasmas; for example electron temperature and density can be inferred from line intensity ratios. By using a Johann spectrometer viewing the plasma, it is possible to construct profiles of plasma parameters such as density, temperature, and velocity with good spatial and time resolution. However, benchmarking atomic code modeling of X-ray spectra obtained from well-diagnosed laboratory plasmas is important to justify use of such spectra to determine plasma parameters when other independent diagnostics are not available. This manuscript presents the operation of the High Resolution X-ray Crystal Imaging Spectrometer with Spatial Resolution (HIREXSR), a high wavelength resolution spatially imaging X-ray spectrometer used to view hydrogen- and helium-like ions of medium atomic number elements in a tokamak plasma. In addition, this manuscript covers a laser blow-off system that can introduce such ions to the plasma with precise timing to allow for perturbative studies of transport in the plasma.

X-ray spectra provide a wealth of information on high temperature plasmas. This manuscript presents the operation of a high wavelength resolution spatially imaging X-ray spectrometer used to view hydrogen- and helium-like ions of medium atomic number elements in a tokamak plasma.

运用X射线成像光谱水晶的使用为高温等离子体诊断

X-ray spectra provide a wealth of information on high temperature plasmas; for example electron temperature and density can be inferred from line ...

Characterization of Ultra-fine Grained and Nanocrystalline Materials Using Transmission Kikuchi Diffraction

One of the challenges in microstructure analysis nowadays resides in the reliable and accurate characterization of ultra-fine grained (UFG) and nanocrystalline materials. The traditional techniques associated with scanning electron microscopy (SEM), such as electron backscatter diffraction (EBSD), do not possess the required spatial resolution due to the large interaction volume between the electrons from the beam and the atoms of the material. Transmission electron microscopy (TEM) has the required spatial resolution. However, due to a lack of automation in the analysis system, the rate of data acquisition is slow which limits the area of the specimen that can be characterized. This paper presents a new characterization technique, Transmission Kikuchi Diffraction (TKD), which enables the analysis of the microstructure of UFG and nanocrystalline materials using an SEM equipped with a standard EBSD system. The spatial resolution of this technique can reach 2 nm. This technique can be applied to a large range of materials that would be difficult to analyze using traditional EBSD. After presenting the experimental set up and describing the different steps necessary to realize a TKD analysis, examples of its use on metal alloys and minerals are shown to illustrate the resolution of the technique and its flexibility in term of material to be characterized.

This paper provides a detailed method to characterize the microstructure of ultra-fine grained and nanocrystalline materials using a scanning electron microscope equipped with a standard electron backscatter diffraction system. Metal alloys and minerals presenting refined microstructures are analyzed using this technique, showing the diversity of its possible applications.