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>

<ol>
	<li>Munir, Z. A., Anselmi-Tamburini, U., Ohyanagi, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+effect+of+electric+field+and+pressure+on+the+synthesis+and+consolidation+of+materials:+A+review+of+the+spark+plasma+sintering+method.">The effect of electric field and pressure on the synthesis and consolidation of materials: A review of the spark plasma sintering method.</a> J. Mater. Sci. 41 (3), 763-777 (2006).</li><li>Chen, W., Anselmi-Tamburini, U., Garay, J. E., Groza, J. R., Munir, Z. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Fundamental+investigations+on+the+spark+plasma+sintering/synthesis+process:+I.+Effect+of+dc+pulsing+on+reactivity.">Fundamental investigations on the spark plasma sintering/synthesis process: I. Effect of dc pulsing on reactivity.</a> Mater. Sci. Eng. A. 394 (1-2), 132-138 (2005).</li><li>Holland, T. B., Anselmi-Tamburini, U., Mukherjee, A. K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electric+fields+and+the+future+of+scalability+in+spark+plasma+sintering.">Electric fields and the future of scalability in spark plasma sintering.</a> Scr. Mater. 69 (2), 117-121 (2013).</li><li>Wan, J., Duan, R., Mukherjee, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Spark+plasma+sintering+of+silicon+nitride/silicon+carbide+nanocomposites+with+reduced+additive+amounts.">Spark plasma sintering of silicon nitride/silicon carbide nanocomposites with reduced additive amounts.</a> Scr. Mater. 53 (6), 663-667 (2005).</li><li>Carney, C. M., Mogilvesky, P., Parthasarathy, T. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Oxidation+Behavior+of+Zirconium+Diboride+Silicon+Carbide+Produced+by+the+Spark+Plasma+Sintering+Method.">Oxidation Behavior of Zirconium Diboride Silicon Carbide Produced by the Spark Plasma Sintering Method.</a> J. Amer. Ceram. Soc. 92 (9), 2046-2052 (2009).</li><li>Dupeux, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Production+of+Oriented+Two-Phase+Bicrystals+by+Diffusion+Bonding+Technique.">Production of Oriented Two-Phase Bicrystals by Diffusion Bonding Technique.</a> J. Cryst. Growth. 66, 169-178 (1984).</li><li>Castro, R., 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=.">.</a> Sintering: mechanisms of convention nanodensification and field assisted processes. 35, (2012).</li><li>Byeon, S. C., Hong, K. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electric+field+assisted+bonding+of+ceramics.">Electric field assisted bonding of ceramics.</a> Mater. Sci. Eng. A. 287 (2), 159-170 (2000).</li><li>Wang, J., Conrad, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Contribution+of+the+space+charge+to+the+grain+boundary+energy+in+yttria-stabilized+zirconia.">Contribution of the space charge to the grain boundary energy in yttria-stabilized zirconia.</a> J. Mater. Sci. 49 (17), 6074-6080 (2014).</li><li>Fujimoto, M., Kingery, W. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Microstructures+of+SrTiO3+Internal+Boundry+Layer+Capacitors+During+and+After+Processing+and+Resultant+Electrical+Properties.">Microstructures of SrTiO3 Internal Boundry Layer Capacitors During and After Processing and Resultant Electrical Properties.</a> J. Amer. Ceram. Soc. 68 (4), 169-173 (1985).</li><li>Mitsuma, T., 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=Structures+of+a+&#931;+=+9,+[110]/{221}+symmetrical+tilt+grain+boundary+in+SrTiO3.">Structures of a &#931; = 9, [110]/{221} symmetrical tilt grain boundary in SrTiO3.</a> Journal of Materials Science. 46 (12), 4162-4168 (2011).</li><li>Ikuhara, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Grain+Boundary+and+Interface+Structures+in+Ceramics.">Grain Boundary and Interface Structures in Ceramics.</a> J. Ceram. Soc. Jpn. 109 (7), S110-S120 (2001).</li><li>Hutt, S., Kienzle, O., Ernst, F., Ruhle, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Processing+and+Structure+of+Grain+boundaries+in+Strontium+Titanate.">Processing and Structure of Grain boundaries in Strontium Titanate.</a> Z. Metallkd. 92 (2), 105-109 (2001).</li><li>Takahisa, Y., Ikuhara, Y., Sakuma, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Current-voltage+characteristics+across+45&#9702;+symmetric+tilt+boundary+in+highly+donor-doped+SrTiO3+bicrystal.">Current-voltage characteristics across 45&#9702; symmetric tilt boundary in highly donor-doped SrTiO3 bicrystal.</a> J. Mater. Sci. Lett. 20, 1827-1829 (2001).</li><li>Hill, A., Wallach, E. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Modelling+Solid+State+Diffusion+Bonding.">Modelling Solid State Diffusion Bonding.</a> Acta Metall. 37 (9), 2425-2437 (1989).</li><li>Sato, Y., 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=Non-linear+current-voltage+characteristics+related+to+native+defects+in+SrTiO3+and+ZnO+bicrystals.">Non-linear current-voltage characteristics related to native defects in SrTiO3 and ZnO bicrystals.</a> Sci. Technol. Adv. Mater. 4 (6), 605-611 (2003).</li><li>Hirose, S., Nishimura, H., Niimi, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Resistance+switching+effect+in+Nb-doped+SrTiO[sub+3]+(100)+bicrystal+with+(100)+&#8764;45&#176;+twist+boundary.">Resistance switching effect in Nb-doped SrTiO[sub 3] (100) bicrystal with (100) &#8764;45&#176; twist boundary.</a> J. App. Phys. 106 (4), 043711-043716 (2009).</li><li>Hutt, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Doctoral Thesis. , (2002).</li><li>Brunner, D., Taeri-Baghbadrani, S., Sigle, W., Ruhle, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Suprising+Results+of+a+Studay+on+the+Plasticity+in+Strontium+Titanate.">Suprising Results of a Studay on the Plasticity in Strontium Titanate.</a> J. Amer. Ceram. Soc. 84 (5), 1161-1163 (2001).</li><li>Gumbsch, P., Taeri-Baghbadrani, S., Brunner, D., Sigle, W., Ruhle, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Plasticity+and+an+inverse+brittle-to-ductile+transition+in+strontium+titanate.">Plasticity and an inverse brittle-to-ductile transition in strontium titanate.</a> Phys. Rev. Lett. 87 (8), 085501-085504 (2001).</li><li>Taeri, S., Brunner, D., Sigle, W., Ruhle, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Deformation+Behavior+of+Strontium+Titanate+between+Room+Temperature+and+1800K+under+Ambient+Pressure.">Deformation Behavior of Strontium Titanate between Room Temperature and 1800K under Ambient Pressure.</a> Z. Metallkd. 95, 433-446 (2004).</li><li>Takahashi, K., Ohtomo, A., Kawasaki, M., Koinuma, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Advanced+Processing+and+Characterization+of+SrTiO3+Single+Crystals+and+Bicrystals+for+High+Tc+Superconducting+Film+Substrate.">Advanced Processing and Characterization of SrTiO3 Single Crystals and Bicrystals for High Tc Superconducting Film Substrate.</a> Mater. Sci. Eng. B. 41, 152-156 (1996).</li><li>Rhodes, W. H., Kingery, W. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Dislocation+Dependence+of+Cationic+Diffusion+in+SrTiO3.">Dislocation Dependence of Cationic Diffusion in SrTiO3.</a> J. Amer. Ceram. Soc. 49 (10), 521-526 (1966).</li><li>Yamamoto, T., Hayashi, K., Ikuhara, Y., Sakuma, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Grain+Boundary+Structure+and+Electrical+Properties+in+Nb-Doped+SrTiO&lt;sub&gt;3&lt;/sub&gt;+Bicrystals.">Grain Boundary Structure and Electrical Properties in Nb-Doped SrTiO&lt;sub&gt;3&lt;/sub&gt; Bicrystals.</a> Key Eng. Mater. 181-182, 225-230 (2000).</li><li>Fitting, L., Thiel, S., Schmehl, A., Mannhart, J., Muller, D. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Subtleties+in+ADF+imaging+and+spatially+resolved+EELS:+A+case+study+of+low-angle+twist+boundaries+in+SrTiO3.">Subtleties in ADF imaging and spatially resolved EELS: A case study of low-angle twist boundaries in SrTiO3.</a> Ultramicroscopy. 106 (11-12), 1053-1061 (2006).</li><li>Hughes, L. 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...

<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 border="0" cellpadding="0" cellspacing="0" width="1429">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Strontium titanate single crystal (100)</td>
			<td style="width:187px;">MTI Corporation</td>
			<td style="width:427px;">STOa101005S1-JP</td>
			<td style="width:443px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Buffered oxide etch, hyrofluoric acid 6:1</td>
			<td style="width:187px;">JT Baker</td>
			<td style="width:427px;">&#160;MBI 1178-03</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Scanning electron microscope (SEM)</td>
			<td style="width:187px;">FEI</td>
			<td>Model: 430 NanoSEM</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">SPS apparatus&#160;</td>
			<td>Sumitomo Coal Mining Co</td>
			<td>Model: Dr. Sinter 5000 SPS Apparatus</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">High Temperature Furnace</td>
			<td>Thermolyne</td>
			<td>Model: 41600</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Ultrasonic Cleaner</td>
			<td>Bransonic</td>
			<td>Model: 221</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Mechanical polisher</td>
			<td style="width:187px;">Allied High Tech Products</td>
			<td>15-2100-TEM</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Diamond lapping film</td>
			<td style="width:187px;">3M</td>
			<td>660XV&#160;</td>
			<td>1 um to 9 um Grit Size</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Diamond lapping film</td>
			<td style="width:187px;">3M</td>
			<td style="width:427px;">661X</td>
			<td>0.5 um to 0.1 um Grit Size</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Colloidal silica</td>
			<td style="width:187px;">Allied High Tech Products</td>
			<td>180-20000</td>
			<td>.05 um Grit Size</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Sputter coater</td>
			<td style="width:187px;">QuorumTech</td>
			<td>Model: Q150RES</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Focused ion beam (FIB) instrument&#160;</td>
			<td style="width:187px;">FEI</td>
			<td>Model: Scios dual-beamed focused ion beam (FIB) instrument&#160;</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Nanomill TEM specimen preparation system</td>
			<td style="width:187px;">Fischione Instruments</td>
			<td>Model: 1040</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Transmission electron microscope (TEM)&#160;</td>
			<td style="width:187px;">JEOL</td>
			<td>Model: JEM2500 SE&#160;</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Scanning transmission electron microscope (STEM)</td>
			<td style="width:187px;">FEI</td>
			<td>Model: TEAM 0.5&#160;</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?...

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

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

Investigation of Early Plasma Evolution Induced by Ultrashort Laser Pulses

Early plasma is generated owing to high intensity laser irradiation of target and the subsequent target material ionization. Its dynamics plays a significant role in laser-material interaction, especially in the air environment1-11.
Early plasma evolution has been captured through pump-probe shadowgraphy1-3 and interferometry1,4-7. However, the studied time frames and applied laser parameter ranges are limited. For example, direct examinations of plasma front locations and electron number densities within a delay time of 100 picosecond (ps) with respect to the laser pulse peak are still very few, especially for the ultrashort pulse of a duration around 100 femtosecond (fs) and a low power density around 1014 W/cm2. Early plasma generated under these conditions has only been captured recently with high temporal and spatial resolutions12. The detailed setup strategy and procedures of this high precision measurement will be illustrated in this paper. The rationale of the measurement is optical pump-probe shadowgraphy: one ultrashort laser pulse is split to a pump pulse and a probe pulse, while the delay time between them can be adjusted by changing their beam path lengths. The pump pulse ablates the target and generates the early plasma, and the probe pulse propagates through the plasma region and detects the non-uniformity of electron number density. In addition, animations are generated using the calculated results from the simulation model of Ref. 12 to illustrate the plasma formation and evolution with a very high resolution (0.04 ~ 1 ps).
Both the experimental method and the simulation method can be applied to a broad range of time frames and laser parameters. These methods can be used to examine the early plasma generated not only from metals, but also from semiconductors and insulators.

An experimental method to examine the early plasma evolution induced by ultrashort laser pulses is described. Using this method, high quality images of early plasma are obtained with high temporal and spatial resolutions. A novel integrated atomistic model is used to simulate and explain the mechanisms of early plasma.

超短激光脉冲诱导的等离子体演化早期的调查

Early plasma is generated owing to high intensity laser irradiation of target and the subsequent target material ionization. Its dynamics plays a ...

科研

工程学

Encapsulation and Permeability Characteristics of Plasma Polymerized Hollow Particles

In this protocol, core-shell nanostructures are synthesized by plasma enhanced chemical vapor deposition. We produce an amorphous barrier by plasma polymerization of isopropanol on various solid substrates, including silica and potassium chloride. This versatile technique is used to treat nanoparticles and nanopowders with sizes ranging from 37 nm to 1 micron, by depositing films whose thickness can be anywhere from 1 nm to upwards of 100 nm. Dissolution of the core allows us to study the rate of permeation through the film. In these experiments, we determine the diffusion coefficient of KCl through the barrier film by coating KCL nanocrystals and subsequently monitoring the ionic conductivity of the coated particles suspended in water. The primary interest in this process is the encapsulation and delayed release of solutes. The thickness of the shell is one of the independent variables by which we control the rate of release. It has a strong effect on the rate of release, which increases from a six-hour release (shell thickness is 20 nm) to a long-term release over 30 days (shell thickness is 95 nm). The release profile shows a characteristic behavior: a fast release (35% of the final materials) during the first five minutes after the beginning of the dissolution, and a slower release till all of the core materials come out.

We have used plasma enhanced chemical vapor deposition to deposit thin films ranging from a few nm to several 100 nm on nano-sized particles of various materials. We subsequently etch the core material to produce hollow nanoshells whose permeability is controlled by the thickness of the shell. We characterize the permeability of these coatings to small solutes and demonstrate that these barriers can provide sustained release of the core material over several days.

等离子体聚合空心颗粒的封装和渗透特征

In this protocol, core-shell nanostructures are synthesized by plasma enhanced chemical vapor deposition. We produce an amorphous barrier by plasma ...

Characterization of Recombination Effects in a Liquid Ionization Chamber Used for the Dosimetry of a Radiosurgical Accelerator

Most modern radiation therapy devices allow the use of very small fields, either through beamlets in Intensity-Modulated Radiation Therapy (IMRT) or via stereotactic radiotherapy where positioning accuracy allows delivering very high doses per fraction in a small volume of the patient. Dosimetric measurements on medical accelerators are conventionally realized using air-filled ionization chambers. However, in small beams these are subject to nonnegligible perturbation effects. This study focuses on liquid ionization chambers, which offer advantages in terms of spatial resolution and low fluence perturbation. Ion recombination effects are investigated for the microLion detector (PTW) used with the Cyberknife system (Accuray). The method consists of performing a series of water tank measurements at different source-surface distances, and applying corrections to the liquid detector readings based on simultaneous gaseous detector measurements. This approach facilitates isolating the recombination effects arising from the high density of the liquid sensitive medium and obtaining correction factors to apply to the detector readings. The main difficulty resides in achieving a sufficient level of accuracy in the setup to be able to detect small changes in the chamber response.

A growing number of radiation therapy devices offer the advantage of delivering the dose through very small beams to the tumor, allowing for increased conformity and higher doses per fraction. Many different detectors can be used for the dosimetry of these small fields. In the present study, the effect of ion recombination is investigated for a liquid ionization chamber using a stereotactic radiation therapy system.

重组的影响在液体电离室表征用于一个电波加速器的剂量学

Most modern radiation therapy devices allow the use of very small fields, either through beamlets in Intensity-Modulated Radiation Therapy (IMRT) or via ...

How to Ignite an Atmospheric Pressure Microwave Plasma Torch without Any Additional Igniters

This movie shows how an atmospheric pressure plasma torch can be ignited by microwave power with no additional igniters. After ignition of the plasma, a stable and continuous operation of the plasma is possible and the plasma torch can be used for many different applications. On one hand, the hot (3,600 K gas temperature) plasma can be used for chemical processes and on the other hand the cold afterglow (temperatures down to almost RT) can be applied for surface processes. For example chemical syntheses are interesting volume processes. Here the microwave plasma torch can be used for the decomposition of waste gases which are harmful and contribute to the global warming but are needed as etching gases in growing industry sectors like the semiconductor branch. Another application is the dissociation of CO2. Surplus electrical energy from renewable energy sources can be used to dissociate CO2 to CO and O2. The CO can be further processed to gaseous or liquid higher hydrocarbons thereby providing chemical storage of the energy, synthetic fuels or platform chemicals for the chemical industry. Applications of the afterglow of the plasma torch are the treatment of surfaces to increase the adhesion of lacquer, glue or paint, and the sterilization or decontamination of different kind of surfaces. The movie will explain how to ignite the plasma solely by microwave power without any additional igniters, e.g., electric sparks. The microwave plasma torch is based on a combination of two resonators &#8212; a coaxial one which provides the ignition of the plasma and a cylindrical one which guarantees a continuous and stable operation of the plasma after ignition. The plasma can be operated in a long microwave transparent tube for volume processes or shaped by orifices for surface treatment purposes.

This movie shows how an atmospheric plasma torch can be ignited by microwaves with no additional igniters and provides a stable and continuous plasma operation suitable for plenty of applications.

如何点燃常压微波等离子体炬没有任何额外的点火器

This movie shows how an atmospheric pressure plasma torch can be ignited by microwave power with no additional igniters. After ignition of the plasma, a ...

Capillary-based Centrifugal Microfluidic Device for Size-controllable Formation of Monodisperse Microdroplets

Here, we demonstrate a simple method for the rapid production of size-controllable, monodisperse, W/O microdroplets using a capillary-based centrifugal microfluidic device. W/O microdroplets have recently been used in powerful methods that enable miniaturized chemical experiments. Therefore, developing a versatile method to yield monodisperse W/O microdroplets is needed. We have developed a method for generating monodisperse W/O microdroplets based on a capillary-based centrifugal axisymmetric co-flowing microfluidic device. We succeeded in controlling the size of microdroplets by adjusting the capillary orifice. Our method requires equipment that is easier-to-use than with other microfluidic techniques, requires only a small volume (0.1-1 &#181;l) of sample solution for encapsulation, and enables the production of hundreds of thousands number of W/O microdroplets per second. We expect this method will assist biological studies that require precious biological samples by conserving the volume of the samples for rapid quantitative analysis biochemical and biological studies.

Here, we demonstrate a simple production method for size-controllable, monodisperse, water-in-oil (W/O) microdroplets using a capillary-based centrifugal microfluidic device. This method requires only a small sample volume and enables high-yield production. We expect this method will be useful for rapid biochemical and cellular analyses.

基于毛细管的离心微流体装置单分散微滴的大小可控的形成

Here, we demonstrate a simple method for the rapid production of size-controllable, monodisperse, W/O microdroplets using a capillary-based centrifugal ...

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 ...

An Atmospheric Pressure Plasma Setup to Investigate the Reactive Species Formation

Non-thermal atmospheric pressure (&#39;cold&#39;) plasmas have received increased attention in recent years due to their significant biomedical potential. The reactions of cold plasma with the surrounding atmosphere yield a variety of reactive species, which can define its effectiveness. While efficient development of cold plasma therapy requires kinetic models, model benchmarking needs empirical data. Experimental studies of the source of reactive species detected in aqueous solutions exposed to plasma are still scarce. Biomedical plasma is often operated with He or Ar feed gas, and a specific interest lies in investigation of the reactive species generated by plasma with various gas admixtures (O2, N2, air, H2O vapor, etc.) Such investigations are very complex due to difficulties in controlling the ambient atmosphere in contact with the plasma effluent. In this work, we addressed common issues of &#39;high&#39; voltage kHz frequency driven plasma jet experimental studies. A reactor was developed allowing the exclusion of ambient atmosphere from the plasma-liquid system. The system thus comprised the feed gas with admixtures and the components of the liquid sample. This controlled atmosphere allowed the investigation of the source of the reactive oxygen species induced in aqueous solutions by He-water vapor plasma. The use of isotopically labelled water allowed distinguishing between the species originating in the gas phase and those formed in the liquid. The plasma equipment was contained inside a Faraday cage to eliminate possible influence of any external field. The setup is versatile and can aid in further understanding the cold plasma-liquid interactions chemistry.

An experimental setup was created for the helium-operated kHz frequency plasma jet. The setup includes a cage for the plasma power supply and jet and an in-house built reactor to monitor plasma-induced reactive species without the interference of the ambient atmosphere.

大气压等离子体设置调查活性物种形成

Non-thermal atmospheric pressure (&#39;cold&#39;) plasmas have received increased attention in recent years due to their significant biomedical potential. ...

In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films

Combinations of metal oxide semiconductors and gold nanoparticles (AuNPs) have been investigated as new types of materials. The in situ synthesis of AuNPs within the interlayer space of semiconducting layered titania nanosheet (TNS) films was investigated here. Two types of intermediate films (i.e., TNS films containing methyl viologen (TNS/MV2+) and 2-ammoniumethanethiol (TNS/2-AET+)) were prepared. The two intermediate films were soaked in an aqueous tetrachloroauric(III) acid (HAuCl4) solution, whereby considerable amounts of Au(III) species were accommodated within the interlayer spaces of the TNS films. The two types of obtained films were then soaked in an aqueous sodium tetrahydroborate (NaBH4) solution, whereupon the color of the films immediately changed from colorless to purple, suggesting the formation of AuNPs within the TNS interlayer. When only TNS/MV2+ was used as the intermediate film, the color of the film gradually changed from metallic purple to dusty purple within 30 min, suggesting that aggregation of AuNPs had occurred. In contrast, this color change was suppressed by using the TNS/2-AET+ intermediate film, and the AuNPs were stabilized for over 4 months, as evidenced by the characteristic extinction (absorption and scattering) band from the AuNPs.

In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films

Here, we present a protocol for the in situ synthesis of gold nanoparticles (AuNPs) within the interlayer space of layered titanate films without the aggregation of AuNPs. No spectral change was observed even after 4 months. The synthesized material has expected applications in catalysis, photo-catalysis, and the development of cost-effective plasmonic devices.

在没有聚集的层状钛酸盐薄膜透明的层间金纳米粒子的原位合成

Combinations of metal oxide semiconductors and gold nanoparticles (AuNPs) have been investigated as new types of materials. The in situ synthesis of AuNPs ...

A Novel Biaxial Testing Apparatus for the Determination of Forming Limit under Hot Stamping Conditions

The hot stamping and cold die quenching process is increasingly used to form complex shaped structural components of sheet metals. Conventional experimental approaches, such as out-of-plane and in-plane tests, are not applicable to the determination of forming limits when heating and rapid cooling processes are introduced prior to forming for tests conducted under hot stamping conditions. A novel in-plane biaxial testing system was designed and used for the determination of forming limits of sheet metals at various strain paths, temperatures, and strain rates after heating and cooling processes in a resistance heating uniaxial testing machine. The core part of the biaxial testing system is a biaxial apparatus, which transfers a uniaxial force provided by the uniaxial testing machine to a biaxial force. One type of cruciform specimen was designed and verified for the formability test of aluminum alloy 6082 using the proposed biaxial testing system. The digital image correlation (DIC) system with a high-speed camera was used for taking strain measurements of a specimen during a deformation. The aim of proposing this biaxial testing system is to enable the forming limits of an alloy to be determined at various temperatures and strain rates under hot stamping conditions.

This protocol proposes a novel biaxial testing system used on a resistance heating uniaxial tensile test machine in order to determine the forming limit diagram (FLD) of sheet metals under hot stamping conditions.

一种新型双轴试验设备的成形极限的下烫印条件的决定

The hot stamping and cold die quenching process is increasingly used to form complex shaped structural components of sheet metals. Conventional ...

New Application of an Atmospheric Pressure Plasma Jet as a Neuro-protective Agent Against Glucose Deprivation-induced Injury of SH-SY5Y Cells

The atmospheric pressure plasma jet (APPJ) has attracted the attention of many researchers from multiple disciplines in recent years because its emissions include multiple types of reactive nitrogen species (RNS) and reactive oxygen species (ROS). Our previous study has shown the cytoprotective effect of the APPJ against oxidative stress-induced injuries. The aim of the present study is to provide a detailed in vitro treatment protocol regarding the neuroprotective applications of helium APPJs on glucose deprivation-induced injury in SH-SY5Y cells. The SH-SY5Y human neuroblastoma-derived cell line was maintained in RPMI 1640 medium supplemented with 15% fetal calf serum. The culture medium was then changed to RPMI 1640 without glucose before APPJ treatment. After a 1 h incubation in a cell incubator, cell viability was determined using Cell Counting Kit 8. The results showed that, compared to the glucose deprivation group, cells treated with APPJ exhibited significantly increased cell viability in a dose-dependent manner, with 8 s/well observed as an optimal dose. Meanwhile, helium flow had no effect on the glucose deprivation-induced cell impairment. Our results indicated that APPJ could be potentially used as a treatment method for the diseases in the central nervous system related to glucose deprivation. This protocol could also be used as a cytoprotective application for other cells with different impairments, but the cell culture and APPJ treatment conditions should be readjusted, and the treatment dose must be relatively low.

A protocol for the neuroprotective application of low-dose atmospheric pressure plasma treatment on glucose deprivation-induced SH-SY5Y injuries.

常压等离子体射流作为神经保护剂抗葡萄糖剥夺诱导 SH-SY5Y 细胞损伤的新应用

The atmospheric pressure plasma jet (APPJ) has attracted the attention of many researchers from multiple disciplines in recent years because its emissions ...