Name: spark plasma sintering apparatus used for the formation of strontium titanate bicrystals
Uploaded: 2017-02-09T15:00:00.000+00:00
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Description: Watch this Scientific Journal Video about Spark Plasma Sintering Apparatus Used for the Formation of Strontium Titanate Bicrystals at JoVE.com

LH非常感谢在加州大学戴维斯分校1148897.批准号:电子显微镜表征和SPS处理由美国国家科学基金会研究生研究奖学金的财政支持由美国加利福尼亚大学的实验室费用奖项是财政支持（＃12-LR-238313）。 在分子铸造工作是由科学，基础能源科学办公室的办公室，能源合同号DE-AC02-05CH11231美国能源部的支持。

1.样品单晶钛酸锶的制备注:单晶STO与抛光至镜面（100）表面提供。 <ol><li>第STO成5×5毫米2采用金刚石线锯件。 </li><li>超声波清洗试样在50-60赫兹连续在每个15分钟丙酮，异丙醇和甲醇浴。 </li><li>从甲醇浴除去STO以立即放置在200℃的温度下保持热板上。清洗后加热样品防止酒精蒸发形成的斑点。 </li><li>将样品在缓冲氢氟酸（pH值= 4）十分钟，一6:氟化铵和49％的氢氟酸1溶液。 22该解决方案蚀刻STO，形成主要是（100） 的 TiO 2表面终止。如果该单晶的光学平面侧具有彩虹铜绿，样品被过度蚀刻，并应Ñ催产素被使用。 </li><li>在蚀刻剂溶液10分钟后，冲洗去离子（DI）水的样品，然后在异丙醇中。用干燥清洁室内空气。 </li></ol> 2.通过放电等离子烧结设备形成双晶注:对于5×5毫米2晶体使用直径30毫米石墨模具。如果小于30毫米使用直径的模头，该双晶灾难性接合时骨折。由所述SPS装置产生最佳的芯片尺寸以及压力是高度依赖于晶体的尺寸。 <ol><li>放置石墨纸30毫米圆上用直径为30毫米的石墨柱塞。石墨纸可防止STO从在实验过程中结合到石墨柱塞。 </li><li>栈中的两处5×5 平方毫米的STO单晶其置于向内以形成双晶边界光学平坦的表面。居中在石墨纸和柱塞的顶部堆叠。 </li><li>旋转顶级单哭飞虱围绕&lt;100&gt;轴到选定的取向差角。 &lt;100&gt;轴垂直于晶体的光学平面。 </li><li>滑到柱塞和晶体石墨模具。将石墨纸的每秒30毫米直径的圆，然后在30毫米直径的柱塞在堆叠STO晶体。 </li><li>叠合并的柱塞和模上在SPS装置石墨隔板（ 图1）。 </li><li>适用的3千牛顿的单轴力使用z轴控制按钮，以减少接触电阻。整个实验中，用户必须通过z轴控制按钮保持在3千牛顿的力。 </li><li>在小孔，在图1所示插入k型热电偶插入石墨模具。热电偶通过模具到样品延伸。 </li><li>设置使用真空按钮的SPS设备约10帕的室压力。 </li><li>通过程序仪器有限公司选择债券的温度，时间和升温速率ntrol软件（ 见表1）。用于粘合的温度和时间，可使用70-80℃/分钟的加热速率和50℃/ min的冷却速率。 </li><li>设置12秒时，使用仪器烧结按钮2秒关闭直流脉冲。一旦程序设置为运行的〜4 V A脉冲偏压和〜550 A的直流电以增量施加到样品。 </li><li>按下机器上的启动按钮。 </li><li>在程序结束时，取出样本。双晶形成后，将样品会出现灰黑色由于所述SPS装置的还原环境。 </li><li>在1200℃进行140小时的温度下使用高温炉，在此过程中不应用压力，退火和再氧化在空气中的样品。根据赫特等人做了以前的工作退火参数选择。在其中形成在高真空13双晶。退火后，将样品揭示了灰白色的颜色和被氧化。 </li></ol><ol><li>用金刚石导线截面双晶看到成5X1毫米2个部分。 </li><li>波兰截面样品金刚石研磨膜。在金刚石研磨膜中的砂砾尺寸逐渐从9微米减小到0.1微米。更改为更小的粒度一旦划痕在表面均匀。使用逆时针方向压盘运动为9微米到6微米的研磨膜。使用逆时针方向压板运动带摆动样本头6微米至0.1微米的抛光膜。 </li><li>波兰截面样品用于使用垫布2分钟胶体二氧化硅。连续倒胶体二氧化硅与上逆时针运动压板和摆动样本头垫。 </li><li>除去样品前十五秒钟，停浇胶体二氧化硅和倒DI水到台板。倒入去离子水十五秒，取出样品，并立即冲洗样品在去离子水中1分钟。如果此过程不遵循，胶体二氧化硅将粘合样品的表面和扫描电子显微镜（SEM）在掩盖晶界。 </li><li>一旦样品被抛光至光学平滑表面，超声波清洁样品连续在每个15分钟丙酮，异丙醇和甲醇浴。 </li><li>从甲醇浴除去STO以立即放置在200℃的温度下保持热板上。清洗后加热样品防止酒精蒸发形成的斑点。 </li><li>摩样品抛光面高达上使用胶体石墨样本存根。 </li><li>溅射涂层样品表面与碳的2-3纳米。使用的碳涂布机下列参数:0.2纳米/脉冲，0.2 A /脉冲电流步率，40 A的脉冲电流，2秒脉冲长度，以及最多50个脉冲的脉冲分辨率。 </li></ol> 4.清洁FIB铜网<ol><li>将铜网FIB为每个1小时，丙酮，然后异丙醇浴。 </li><li>等离子体清洁铜FIB格10分钟。 </li></ol> 5.制备透射电子显微镜（TEM），通过聚焦离子束（FIB）装置薄片注:FIB准备使用的所有参数都打印或从FIB设备软件的下拉菜单中选择。 <ol><li>放在FIB设备STO样品和铜网FIB。该阶段是7毫米。 </li><li>找到的沿着两个单晶， 即 ，晶界之间的界面的感兴趣区域。 </li><li>选择图案对话框。在图案的控制，与应用性能的Ce-DEP面选择矩形图案的工具。将C-DEP注气。存款C的15×2×2微米3保护层阿尔邦使用以5.0千伏，13.0 nA的的电流的电压的电子束，和0°的倾斜角。收回C-DEP。 </li><li>选择图案对话框。在图案的控制，与应用程序属性W-DEP选择矩形图案的工具。将W-DEP注气。存15×2×2微米3使用离子束在30.0千伏，0.3 nA的的电流的电压钨的保护层，以及52°的倾斜角。收回W-DEP。 </li><li>选择图案对话框。在图案的控制，与应用性能硅选择正规的横截面图案化模具。使用22×25×15微米3的底部图案和的22×27×15微米3为顶图案在30.0千伏，30.0 nA的的电流，并经由离子束的52°的倾斜角的电压。的图案将创建在保护层两侧的沟槽磨。 </li><li>选择图案对话框。在图案控制，选择清洁横截面图案化模具与应用性能硅。使用22×3×60微米3在30.0千伏的电压的顶部和底部图案，并通过离子束1.0 NA的电流。倾斜角为53.5°的底部图案和50.5°的顶部图案。图案清除从由经常截面图案化产生的结壳图案的沟槽薄片的表面上。 </li><li>切J-模式为使用与应用性能硅矩形图案工具的样本。使用2微米的宽度在30.0千伏的电压，并通过离子束1.0 NA的电流。 </li><li>选择简易电梯对话框。将显微公园的位置。降低显微并通过使用在5.4中详述的处理的钨焊接附着样品到铜FIB电网。 </li><li>使用在5.7中详述的步骤，用离子束以一个电压μcut一个U模式，从原来的J-图案继续进行，在样品中30.0千伏和1.0 NA的电流。 </li><li>通过大样上方的显微提起薄片。 </li><li>旋转显微180°，所以在晶界不再平行于离子束，但在垂直于离子束。 </li><li>钨用在5.4与30.0千伏的电压，离子束和0.3的NA的电流详述的步骤焊接薄片到铜FIB网格。 </li><li>切使用在5.7与30.0千伏的电压，离子束和1.0 NA的电流详述的步骤的薄片的显微。 </li><li>重复5.3的详细步骤。淀积碳的使用电子束以5.0千伏，13.0 nA的的电流的电压的15×2×4微米3保护层，和0°的倾斜角。 </li><li>重复5.4的详细步骤。钨的使用离子束在30.0千伏，0.3 nA的的电流的电压存款15×2×8微米3保护层，以及52°的倾斜角。 </li><li>同离子束，细使用30.0千伏电压和0.5 nA的的系统减少电流，0.3 Na和0.1 nA的样品以约200纳米。在此阶段，清洁截面图案被使用，并且将样品倾斜到52±±1.5°的角度。 </li><li>与离子束，细样品使用5.0千伏的电压和77.0 Pa的电流电子透明度。在此阶段，一个矩形图案用于为52±3°的倾斜角。 </li><li>在500伏特的电压和150微安的电流清洗试样移除的FIB招致非晶损坏。 </li><li>在扫描透射电子显微镜（STEM）的TEM架和刀片保持器处TEM样品。选择"捕获"，图像采样晶界。 </li></ol>

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A., van Benthem, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Formation+of+SrTiO3+bicrystals+using+spark+plasma+sintering+techniques.">Formation of SrTiO3 bicrystals using spark plasma sintering techniques.</a> Scr. Mater. 118, 9-12 (2016).</li></ol>

We have nothing to disclose.

被选择的1200℃的接合温度最大化扩散由于温度的微小变化可以大大地影响所有扩散接合机制的动力学。 1200℃的温度是脆韧转变温度范围STO之外。然而，样品在该温度下进行脆性断裂。申通快递双晶的灾难性故障并不出乎意料，因为申通快递有〜1200℃，0.5％的延展性。此外，该样品在140兆帕的整个加热过程中的压力保持和STO在该加热过程，其中具有0％延性21通过其脆性阶段过渡。经由所述SPS装置单晶从而成功扩散接合就必须材料的温度依赖性塑性行为的深入了解。 两个双晶用800℃的粘合温度和20分钟的接合时间而形成的。该双晶与4˚的标称取向差下退火50小时，显示出的接合界面馏分2.2倍比45°标称取向误差的双晶，退火140小时以上。退火时间超过50小时时没有透露扩散接合质量的任何显著改善。退火温度和时间分别根据其中形成在高真空炉中，类似于所述SPS设备11中的双晶以前的工作选择。以确定是否有所述退火工艺对这些双晶的扩散接合产生影响，扩散键长计算，结果为在1200℃140小时23的温度下0.27纳米。所选的退火参数，因此，只有在双晶的扩散接合的影响有限。该分析进一步支持当一个双晶的具有45°的扭曲取向误差的扩散接合是不成功为退火期间所使用的相同的参数。 而选定的退火参数没有显著影响扩散接合时，取向差角确有明显的影响。高角度取向差角创建两个半晶体之间一个较大的结构失配，这阻碍了交叉扩散，降低界面粘合。为高取向差角，粘合温度和时间必须以具有更大的成功接合界面分数增加。 经由SPS处理技术双晶的形成比常规热压方法发生在显著加速时间尺度和适中温度范围。在常规扩散接合SPS法之间的处理参数这种差异也可见于粉末压块和复合材料的形成。如上所述，双晶经由常规扩散接合方法形成的在温度超过1400℃的时间尺度从3至20小时11 24更大的形成。使用SPS仪器，扩散接合发生在800℃下用次尺度从20至90分钟的温度。所述SPS技术是则与常规方法相比双晶的迅速扩散接合有用的。形成双晶的SPS仪器还允许在有选择的取向差晶界传质机理的实验观察。这一实验观察会提供更深入地了解了支撑技术，SPS机制。 在本体STO双晶微裂纹防止以往的机械的TEM薄片制备。机械减薄过程导致了TEM薄片的断裂由于微裂纹在整个批量蔓延。因此，使用了TEM薄片的FIB制备。传统的FIB升IFT出薄片，其中，所述晶界平行于离子束，导致沿界面平面（ 图5a）优惠铣削。 FIB的制备技术随后被修改。首先，碳和钨的初始保护层的厚度选择成，在升降出步骤结束时，在保护层研磨程。如果保护层太厚，并保持整个变薄过程中，发生了钨的重新沉积和遮蔽TEM分析。其次，在TEM薄片被附着到显微操纵的前端之后，在微操作被旋转180°。该旋转导致晶界，成为垂直于离子束，从而防止优惠减薄（ 图5b）。最后，电梯出处理后，碳和钨的保护层沉积在新取向的TEM薄片的表面上。这些修改常规FIB公关eparation技术带领到一个干净的TEM薄片通过HAADF-STEM使原子分辨率的成像。 对于在800℃下贴合90分钟标称45°的扭曲晶界的双晶HRTEM和HAADF-STEM显微图显示出与没有第二相的原子解决晶界结构。空间分辨EELS揭示在晶界芯内的钛协调变化，表明相比于本体中的氧空位浓度的增加。这些结果与文献报道于低角度扭曲晶粒边界25一致。这些实验的进一步分析别处26所述。 在这项研究中，STO双晶成功地合成了使用SPS设备的第一次。具有0°扭转取向，4℃，并在适度的粘合温度和时间高压形成45°进行双晶秤相比，在常规粘合发现这些参数。通过SPS设备双晶的形成提供了一个机会，以定量测定电场对选定的晶界的核心结构的影响，以及加热速度。

<html>放电等离子烧结（SPS）是其中应用高的单轴压力，脉冲直流电引线的粉末的快速致密化压块1的技术。这种技术也导致由各种材料，包括氮化硅/碳化硅，硼化锆/碳化硅或碳化硅的成功形成复合结构，没有额外的烧结助剂需要2，3，4，5。这些复合结构通过常规热压已经过去有挑战性的合成。同时通过SPS技术高的单向压力和快速升温速率的应用提高粉末和复合材料的整理，的现象，造成文献2,3辩论这种增强致密化，类="外部参照"&gt; 6，7。此外，还存在对于电场在晶界形成的影响只有有限的信息和晶界芯8,9的所得原子结构。这些芯结构确定的SPS烧结材料的功能特性，包括高电压电容器的电击穿和陶瓷氧化物10的机械强度和韧性。因此，了解基本晶界结构的SPS加工参数，如施加的电流的函数，是必需的材料的整体物理性能的操作。系统地阐明支撑SPS的基本物理机制的一种方法是特定晶界结构， 即 ，双晶的形成。一个双晶是由两个单晶，然后将它们的操作创建diffu锡永的具体取向差角度保税11。此方法提供了一种可控制的方式来研究的基本晶界芯结构作为处理参数的函数，掺杂剂浓度，并且杂质偏析12，13，14。 扩散接合是依赖于四个参数:温度，时间，压力，和键合气氛15。钛酸锶的常规扩散接合（的SrTiO 3，STO）双晶通常发生在低于1兆帕的压力下，温度范围为1,400-1,500℃的范围内，和时间尺度从3至20小时13，14，16，17。在这项研究中，接合在一个SPS装置以在C显著较低的温度和时间尺度达到omparison常规方法。对于多晶材料，降低温度和时间尺度通过SPS显著限制晶粒长大，从而通过其微操纵提供了物质属性的有利控制。 所述SPS的装置，对于一个5×5 平方毫米的样品，施加140兆帕的最小压力。内的常规扩散接合温度范围，哈特等人。当粘结压力超过10兆帕18日报道STO瞬间断裂。然而，STO具有温度依赖性可塑性的行为，表示连接压力可在特定的温度超过10兆帕。以上1200℃和低于700℃，STO具有一些延展性，在其中强调大于120兆帕可以在没有样品的瞬时断裂被应用。在中间温度范围的700-1,200°C，申通快递在s脆性和经验瞬时断裂秀发大于10兆帕。在800℃，STO具有应力断裂小于200兆帕19，20，21之前轻微变形。因此，粘合温度为经由SPS装置的STO双晶的形成必须根据材料的塑性行为进行选择。

<table><tbody><tr><td>Strontium titanate single crystal (100)</td><td>MTI Corporation</td><td>STOa101005S1-JP</td><td></td></tr><tr><td>Buffered oxide etch, hyrofluoric acid 6:1</td><td>JT Baker</td><td>&amp;nbsp;MBI 1178-03</td><td></td></tr><tr><td>Scanning electron microscope (SEM)</td><td>FEI</td><td>Model: 430 NanoSEM</td><td></td></tr><tr><td>SPS apparatus&amp;nbsp;</td><td>Sumitomo Coal Mining Co</td><td>Model: Dr. Sinter 5000 SPS Apparatus</td><td></td></tr><tr><td>High Temperature Furnace</td><td>Thermolyne</td><td>Model: 41600</td><td></td></tr><tr><td>Ultrasonic Cleaner</td><td>Bransonic</td><td>Model: 221</td><td></td></tr><tr><td>Mechanical polisher</td><td>Allied High Tech Products</td><td>15-2100-TEM</td><td></td></tr><tr><td>Diamond lapping film</td><td>3M</td><td>660XV</td><td>1 &amp;#956;m to 9 &amp;#956;m Grit Size</td></tr><tr><td>Diamond lapping film</td><td>3M</td><td>661X</td><td>0.5 &amp;#956;m to 0.1 &amp;#956;m Grit Size</td></tr><tr><td>Colloidal silica</td><td>Allied High Tech Products</td><td>180-20000</td><td>0.05 &amp;#956;m Grit Size</td></tr><tr><td>Sputter coater</td><td>QuorumTech</td><td>Model: Q150RES</td><td></td></tr><tr><td>Focused ion beam (FIB) instrument&amp;nbsp;</td><td>FEI</td><td>Model: Scios dual-beamed focused ion beam (FIB) instrument&amp;nbsp;</td><td></td></tr><tr><td>Nanomill TEM specimen preparation system</td><td>Fischione Instruments</td><td>Model: 1040</td><td></td></tr><tr><td>Transmission electron microscope (TEM)&amp;nbsp;</td><td>JEOL</td><td>Model: JEM2500 SE&amp;nbsp;</td><td></td></tr><tr><td>Scanning transmission electron microscope (STEM)</td><td>FEI</td><td>Model: TEAM 0.5&amp;nbsp;</td><td></td></tr></tbody></table>

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.

接合温度，时间，和取向差角都改变，以确定所需的STO双晶（ 表1）的最大可能接合界面部分的最佳参数。接口被认为是"结合"时，晶界不是SEM成像（ 图2a）中可见。 A&#39;非保税"界面时，显示出一个黑暗的图像对比度或空洞出席了边界位置（ 图2b）。黑暗的图像对比度，标志着胶体石墨从FIB安装程序已经由于毛细效应两个STO晶体间扩散。该非接合界面是在双晶的边缘观察到，而接合界面是在双晶的中心观察到的。从边缘到由SPS装置形成的双晶的中心键合行为的变化也出现在通过热压techniqu形成双晶ES 6。 在大部分的双晶的微裂纹形成在所有样品中观察到。为成功地粘合双晶，微裂纹形成不与键合界面干扰。在1200℃的粘结温度，广泛的微裂纹发生时，退火时导致双晶的脆性破坏。因此，在所述SPS装置接合温度保持在低于800℃，以防止灾难性断裂。 对于在600℃的粘合温度700℃0°取向差角和双晶，获得了95％的成功接合界面。在双晶到44.4°的取向差角的增加，需要在800℃，粘合时间90分钟以实现45.8％成功接合界面的粘结温度。高分辨透射电镜（HRTEM）和高角度环形暗场扫描透射电子显微镜（HAADF-STEM）该样品的显微图揭示用无晶间膜或次生相存在（ 图3）的原子突然晶界结构。相比于散装时空间分辨电子能量损失谱（EELS）直接从接口记录表示在钛L 3和L 2的边缘的晶体场分裂，以及在确定边缘强度降低的减少（ 图4） 。 <table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always"><tbody><tr><td>双晶体</td><td>扭转取向（°） </td><td>键温度（℃） </td><td>键时间（min） </td><td>退火温度（℃） </td><td>退火时间（h） </td><td>接合界面±0.3（％） </td></tr><tr><td>一个</td><td> 0 * </td><td> 1200 </td><td> 15 </td><td> 1200 </td><td> 16 </td><td> - </td></tr><tr><td>乙</td><td> 0 </td><td> 600 </td><td> 90 </td><td> 1200 </td><td> 100 </td><td> 92.3 </td></tr><tr><td> C </td><td> 0 </td><td> 700 </td><td> 90 </td><td> 1200 </td><td> 100 </td><td> 99.7 </td></tr><tr><td> ð </td><td> 4.3±0.3 </td><td> 800 </td><td> 20 </td><td> 1200 </td><td> 50 </td><td> 79.2 </td></tr><tr><td> Ë </td><td> 45 * </td><td> 700 </td><td> 60 </td><td> 1200 </td><td> 140 </td><td> 1.3 </td></tr><tr><td> F </td><td> 46.1±0.5 </td><td> 800 </td><td> 20 </td><td> 1200 </td><td> 140 </td><td> 35.4 </td></tr><tr><td> G </td><td> 44.4±0.1 </td><td> 800 </td><td> 90 </td><td> 1200 </td><td> 140 </td><td> 45.8 </td></tr></tbody></table> 表1键合参数和双晶体的后续接口分数。 SPS设备扩散连接参数和STO双晶随后的连接界面分数。的〜4 V A脉冲偏置电压和〜550 A的直流电流，适用于所有实验。键合界面的级分从（1.5±0.4）毫米的平均晶粒边界长度计算的。从不同地区采取了双晶内的这些区域。 <img alt="图1" src="/files/ftp_upload/55223/55223fig1.jpg" /> 图1放电等离子烧结设备。设置为在火花等离子体烧结设备。压力在垂直于双晶界面的应用。 <a href="http://ecsource.jove.com/files/ftp_upload/55223/55223fig1large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图2" src="/files/ftp_upload/55223/55223fig2.jpg" /> 在SPS鸭发现图2.典型的接口paratus形成双晶体。公称 在800℃下进行90分钟的温度下形成的45°的扭曲双晶。 （ 一 ）中定义的"粘合"界面的SEM图像，晶界位置是由一个方位空隙的存在，和所定义的"非粘合"界面（b）的SEM图像推断。图像中观察到的球形珠从抛光残留的二氧化硅。 <a href="http://ecsource.jove.com/files/ftp_upload/55223/55223fig2large.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/55223/55223fig3.jpg" /> 图3.双晶晶界的高分辨率成像。形成在800℃下记录在&lt;100&gt;90分钟带轴的温度下与一个边缘上取向的界面平面标称45°的扭曲双晶边界。 （ <s仲&gt;一）高分辨图像，（B）HRSTEM DF图像，以及（c）两个单结晶，一个在&lt;100&gt;和一个在组成的结构模型&lt;110&gt;带轴取向为{001}界面平面。从预计的结构模型中的实验成像数据的偏差表示与理想单晶原子位置的接口配置的变化。 <a href="http://ecsource.jove.com/files/ftp_upload/55223/55223fig3large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图4" src="/files/ftp_upload/55223/55223fig4.jpg" /> 图4.结构的双晶化学晶界。邻近（a）该钛大号2,3边缘和（b）确定边缘在边界采取的边缘精细结构和45°的扭曲双晶的在800的温度下形成的散装°下90分钟。 <a href="http://ecsource.jove.com/files/ftp_upload/55223/55223fig4large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图5" src="/files/ftp_upload/55223/55223fig5.jpg" /> 图5. FIB铣削在晶双晶界。 （a）用平行于离子束和（b）样品与晶界的晶界样品的纤维蛋白原的TEM薄片垂直于离子束的HRTEM图像。 <a href="http://ecsource.jove.com/files/ftp_upload/55223/55223fig5large.jpg" target="_blank">请点击此处查看该图的放大版本。</a>

Watch this Scientific Journal Video about Spark Plasma Sintering Apparatus Used for the Formation of Strontium Titanate Bicrystals at JoVE.com

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

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 ...

spark-plasma-sintering-apparatus-used-for-formation-strontium

Nanyang Technological University

Research

JoVE Journal

Engineering

9.8K 次观看.  University of California, Davis. 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. 

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

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 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.

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 ...

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 ...

High Temperature Fabrication of Nanostructured Yttria-Stabilized-Zirconia (YSZ) Scaffolds by In Situ Carbon Templating Xerogels

We demonstrate a method for the high temperature fabrication of porous, nanostructured yttria-stabilized-zirconia (YSZ, 8 mol% yttria - 92 mol% zirconia) scaffolds with tunable specific surface areas up to 80 m2&#183;g-1. An aqueous solution of a zirconium salt, yttrium salt, and glucose is mixed with propylene oxide (PO) to form a gel. The gel is dried under ambient conditions to form a xerogel. The xerogel is pressed into pellets and then sintered in an argon atmosphere. During sintering, a YSZ ceramic phase forms and the organic components decompose, leaving behind amorphous carbon. The carbon formed in situ serves as a hard template, preserving a high surface area YSZ nanomorphology at sintering temperature. The carbon is subsequently removed by oxidation in air at low temperature, resulting in a porous, nanostructured YSZ scaffold. The concentration of the carbon template and the final scaffold surface area can be systematically tuned by varying the glucose concentration in the gel synthesis. The carbon template concentration was quantified using thermogravimetric analysis (TGA), the surface area and pore size distribution was determined by physical adsorption measurements, and the morphology was characterized using scanning electron microscopy (SEM). Phase purity and crystallite size was determined using X-ray diffraction (XRD). This fabrication approach provides a novel, flexible platform for realizing unprecedented scaffold surface areas and nanomorphologies for ceramic-based electrochemical energy conversion applications, e.g. solid oxide fuel cell (SOFC) electrodes.

High Temperature Fabrication of Nanostructured Yttria-Stabilized-Zirconia YSZ Scaffolds by In Situ Carbon Templating Xerogels

A protocol for fabricating porous, nanostructured yttria-stabilized-zirconia (YSZ) scaffolds at temperatures between 1,000 &#176;C and 1,400 &#176;C is presented.

通过纳米氧化钇稳定的二氧化锆（YSZ）的支架的高温加工<em&gt;原位</em&gt;碳模板干凝胶

We demonstrate a method for the high temperature fabrication of porous, nanostructured yttria-stabilized-zirconia (YSZ, 8 mol% yttria - 92 mol% zirconia) ...

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 ...

Fused Filament Fabrication (FFF) of Metal-Ceramic Components

Technical ceramics are widely used for industrial and research applications, as well as for consumer goods. Today, the demand for complex geometries with diverse customization options and favorable production methods is increasing continuously. With fused filament fabrication (FFF), it is possible to produce large and complex components quickly with high material efficiency. In FFF, a continuous thermoplastic filament is melted in a heated nozzle and deposited below. The computer-controlled print head is moved in order to build up the desired shape layer by layer. Investigations regarding printing of metals or ceramics are increasing more and more in research and industry. This study focuses on additive manufacturing (AM) with a multi-material approach to combine a metal (stainless steel) with a technical ceramic (zirconia: ZrO2). Combining these materials offers a broad variety of applications due to their different electrical and mechanical properties. The paper shows the main issues in preparation of the material and feedstock, device development, and printing of these composites.

Fused Filament Fabrication FFF of Metal-Ceramic Components

This study shows multi-material additive manufacturing (AM) using fused filament fabrication (FFF) of stainless steel and zirconia.

金属陶瓷元件的熔融长丝制造 (fff)

Technical ceramics are widely used for industrial and research applications, as well as for consumer goods. Today, the demand for complex geometries with ...

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 ...

Radio Frequency Magnetron Sputtering of GdBa2Cu3O7&#8722;&#948;/ La0.67Sr0.33MnO3 Quasi-bilayer Films on SrTiO3 (STO) Single-crystal Substrates

Here, we demonstrate a method of coating ferromagnetic La0.67Sr0.33MnO3 (LSMO) nanoparticles on (001) SrTiO3 (STO) single-crystal substrates by radio frequency (RF) magnetron sputtering. LSMO nanoparticles were deposited with diameters from 10 to 20 nm and heights between 20 and 50 nm. At the same time, (Gd) Ba2Cu3O7&#8722;&#948; ((Gd) BCO) films were fabricated on both undecorated and LSMO nanoparticle decorated STO substrates using RF magnetron sputtering. This report also describes the properties of GdBa2Cu3O7&#8722;&#948;/ La0.67Sr0.33MnO3 quasi-bilayer films structures (e.g., crystalline phase, morphology, chemical composition); magnetization, magneto-transport, and superconducting transport properties were also evaluated.

Radio Frequency Magnetron Sputtering of GdBa2Cu3O7ÃƒÆ’Ã‚Â¢Ãƒâ€¹Ã¢â‚¬Â 'ÃƒÆ’Ã…Â½ Â´/ La0.67Sr0.33MnO3 Quasi-bilayer Films on SrTiO3 STO Single-crystal Substrates

Here, we present a protocol to grow LSMO nanoparticles and (Gd) BCO films on (001) SrTiO3 (STO) single-crystal substrates by radio frequency (RF)-sputtering.

Gdba2cu 3 o7 的射频磁控管散射-/la0.67sr 0.67 mno 3 准双层薄膜上的 srtio 3 (sto) 单晶基板上

Here, we demonstrate a method of coating ferromagnetic La0.67Sr0.33MnO3 (LSMO) nanoparticles on (001) SrTiO3 (STO) single-crystal substrates by radio ...

放电等离子烧结设备中使用的钛酸锶双晶体的形成

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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

非均匀掺Pr的SrTiO的合成

锗通过原子层沉积钙钛矿型钛酸锶的外延生长

通过纳米氧化钇稳定的二氧化锆（YSZ）的支架的高温加工

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

金属陶瓷元件的熔融长丝制造 (fff)

组分变熵稳定氧化物的体积和薄膜合成

Gdba₂cu 3 o7 的射频磁控管散射-/la_0.67sr 0.67 mno 3 准双层薄膜上的 srtio 3 (sto) 单晶基板上