这项工作是由德国研究基金会（DFG）（CH 943/2-1合同）成立。笔者想感谢沃尔夫冈迪图斯和斯特凡Paetel的Zentrum酒店献给Sonnenenergie和Wasserstoff-Forschung巴登 - 符腾堡州准备对这项工作的CIGS吸收层。

1。 CIGS层沉积<ol><li>溅射沉积500纳米到3mm厚的钠钙玻璃基板（SLG），钼（背接触层）。 </li><li>合作蒸发2微米的铜铟镓硒联多级CIGS工艺24。沫背接触层上沉积所得到的铜铟镓硒是图1中所示。 </li><li>测量CIGS层的组成组合物，用X-射线荧光光谱仪（XRF）。将得到的铜铟镓硒组合物示于表1。 </li></ol> 2。网站特定的样品制备APT分析<ol><li>剪切的TEM沫网格分为两半，以便取得一排的几个标签，即购买试样的支持。到一个保持器和锥形的标签的端部安装的TEM半网格通过电解在5重量。 ％的NaOH到顶端直径小于2微米。这个过程可以是合理控制使用立体。然后安装到另一架吨电解电网帽子是优化顺序FIB，透射电子显微镜（TEM），电子背散射衍射和APT表征。 </li><li>穆勒分两期进入CIGS薄膜使用FIB底切（ 图2a）。的组块的左侧的第一自由裁切。 </li><li>显微附加的组块通过离子束诱导化学气相沉积法沉积的Pt焊接。然后，使最终的自由相反的站点和升降机的自由站立的块（ 图2b）。 </li><li>现在切TEM莫半格尖锐的针（直径2-3微米），有一个良好的联合提取块楔形。安装大块引脚上的使用PT沉积（ 图2c）。自由切割，最终得到钼针的顶端上只有一小部分（约2微米）的chunk。之后电网架安装颠倒，莫引脚和安装一块铂之间填补了国内空白。追求其它块的相同的程序。欲了解更多详细信息，电梯过程中，读者可以查阅以下引用18,25。 </li><li>将网格直立和清洁的chunk（选铂焊缝稀释剂在网站上）的横截面，通过使用低加速电压和电子束电流（5 kV和&lt;50 pA的），在FIB中。因此，人们得到表面光滑，少污染由于GA +注入EBSD测量，这是需要的，。 </li><li>从EBSD测量截面上进行选择一个GB的兴趣。对GB的方向优选垂直于相对于分析在原子探针（z轴）方向的减少，这是描述中更详细地讨论的一部分的局部放大的效果26。与GB的一个适当的区域突出显示在图2d。 </li><li>执行在区域选择步骤2.6）中，以形成一个锋利的尖的GB的环形铣削。的曲率半径应足够小（&lt;100 nm）的进一步的TEM investigat离子。为了达到这个目标，减少的的环形铣刀图案一步的步骤（ 图2e）的内径，并且伴随着可视化的二次电子（SE）的前端成形。因此，可以纠正光束变化或调整铣图案，删除违规尖上像涟漪或材料来自不同溅射产量，阴影效果等的再沉积。 </li><li>本地化的前端通过使用TEM工具（参见图2f）的顶点相对于晶界的精确位置，知道CIGS晶界与其它材料（如超耐热合金）相比，在SEM中是不可见的。 </li><li>精确了解其中GB是位于的APT尖内，标本转移到FIB和继续磨样品位于GB最大200纳米以下的尖端的顶点。在这个阶段，在非常低的千伏（5千伏）和低电流（&lt;50 pA的）进行铣削。事实上，我们的目标不仅是本地化的GB接近吨Ø先端尖，还能最大限度地减少GA +的伤害，在此过程中的APT尖。伴随地的低千伏铣削的，可视化的形状，在SEM中的APT前端控制的物质的量应被删除从尖端的顶点（ 图2g）。 </li><li>再次转入试样的TEM检查GB尖的顶点的位置。使试样的概览图像（ 图2h），能够获得精确的了解GB位置时，试样直径的演变和半柄角。这是必要的，以便获得最佳的APT数据重建。此外，使用低倍率和减少曝光时间，以减少电子束引起的损害和C的污染，这可能会导致在APT测量较高的故障率。 </li></ol> 3。一个的CAMECA LEAP 3000X HR系统APT分析<ol><li>在亚太保持装入标本呃。然后，装入标本冰球的四个转盘之一。 </li><li>插入传送带含有试样的冰球负载锁内部和开始抽装载锁定。当负载锁内的真空度〜10 -7乇时，插入圆盘传送带内的缓冲室。 </li><li>在等待CA。 1小时来恢复缓冲室中的真空度（约7×10 -9乇），将试样从缓冲室主要分析室。这是与水平转移的棒，其中的手动操作装置。 </li><li>内的APT，凉爽下降到60 K的温度在开始测量之前，这样低的温度将在分析过程中，避免在试样表面的原子的扩散。这里我们注意到，60 K是设定温度，而不是真正的上APT尖测量，这应该是较高的，由于激光热处理试样的温度。凯洛格等人所提出的27日 ，温TURE可以估算考虑到相对充电状态比。不幸的是，在这项工作中的真实温度的提示无法计算主要是未知的，因为这一领域的CIGS材料蒸发。 </li><li> APT实验进行了使用绿色激光，其波长约532 nm和12皮秒的脉冲长度的激光模式。 </li></ol> 4。 APT数据重建<ol><li>打开RHIT文件（原始数据后直接获得APT测量）与CAMECA的综合可视化和分析软件（IVAS 3.6.2）28一般用来重建三维地图。 </li><li>执行重建三维地图使用以下八个步骤28： <ol><li>第1步-这是一个只读窗格，让所有的性质和内容的详细信息，选定研究的设置 。 </li><li>第2步- 选择离子的序列范围 。本步骤定义离子序列范围相对标本电压被选中的重建数据。 </li><li>第3步- 选择探测器的投资回报率 。此步骤可为机会，以去除离子探测器外的投资回报率（黑色椭圆探测器事件直方图）。 </li><li>步骤4 - TOF改正 。此步骤中计算的电压， - 飞行时间（TOF），分析检测器的平面性（“碗校正”）修正。 </li><li>第5步- 大众校准 。在质谱分析测得的峰值位置进行校准与已知的同位素/充电状态。 </li><li>第6步- 远程离子分配 。在此步骤中的质谱峰在指定元素同位素的范围。 </li><li>步骤7 - 重建 。此步骤适用于三种重建方法，对采集的数据之一：电压法，柄角法或尖剖面法。最后一个是在目前的研究中，重建我们的三维地图。此方法需要一个扫描电镜（SEM）或透射电子显微镜图像的钛p等示于图2g和图2小时 。在任何点的重建尖端的曲率半径被定义了一系列的SEM图像中定义的点之间的线性内插。 </li><li>第8步- 确认 。在此步骤中，将转换为“重建”选项卡中创建预览保存的分析。 </li></ol></li></ol>

<ol>
	<li>Stanbery, B. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Copper+indium+selenides+and+related+materials+for+photovoltaic+devices.">Copper indium selenides and related materials for photovoltaic devices.</a> Crit. Rev. Solid State. 27, 73-117 (2002).</li><li>Kemell, M., Ritala, M., Leskel&#228;, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thin+film+deposition+methods+for+CuInSe2+solar+cells.">Thin film deposition methods for CuInSe2 solar cells.</a> Crit. Rev. Solid State. 30, 1-31 (2005).</li><li>Kazmerski, L. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Solar+photovoltaics+R&amp;D+at+the+tipping+point:+a+2005+technology+overview.">Solar photovoltaics R&amp;D at the tipping point: a 2005 technology overview.</a> J. Electron Spectrosc. 150 (2-3), 105-135 (2006).</li><li>Sadewasser, S., Glatzel, T., Schuler, S., Nishiwaki, S., Kaigawa, R., Lux-Steiner, M. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Kelvin+probe+force+microscopy+for+the+nano+scale+characterization+of+chalcopyrite+solar+cell+materials+and+devices.">Kelvin probe force microscopy for the nano scale characterization of chalcopyrite solar cell materials and devices.</a> Thin Solid Films. 431-432, 257-261 (2003).</li><li>Jiang, C. S., Noufi, R., AbuShama, J. A., Ramanathan, K., Moutinho, H. R., Pankow, J., Al-Jassim, M. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Local+built-in+potential+on+grain+boundary+of+Cu(In,Ga)Se2+thin-films.">Local built-in potential on grain boundary of Cu(In,Ga)Se2 thin-films.</a> Appl. Phys. Lett. 84, 3477-1-3477-3 (2004).</li><li>Abou-Ras, D., Koch, C. T., K&#252;stner, V., van Aken, P. A., Jahn, U., Contreras, M. A., Caballero, R., Kaufmann, C. A., Scheer, R., Unold, T., Schock, H. W. <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+types+in+chalcopyrite-type+thin+films+and+their+correlations+with+film+texture+and+electrical+properties.">Grain-boundary types in chalcopyrite-type thin films and their correlations with film texture and electrical properties.</a> Thin Solid Films. 517, 2545-2549 (2009).</li><li>Nichterwitz, M., Abou-Ras, D., Sakurai, K., Bundesmann, J., Unold, T., Scheer, R., Schock, H. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Influence+of+grain+boundaries+on+current+collection+in+Cu(In,Ga)Se2+thin-film+solar+cells.">Influence of grain boundaries on current collection in Cu(In,Ga)Se2 thin-film solar cells.</a> Thin Solid Films. 517, 2554-2557 (2009).</li><li>Abou-Ras, D., Schorr, S., Schock, H. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Grain+sizes+and+grain+boundaries+in+chalcopyrite-type+thin+films.">Grain sizes and grain boundaries in chalcopyrite-type thin films.</a> J. Appl. Cryst. 40, 841-848 (2007).</li><li>Niles, D. W., Al-Jassim, M., Ramanathan, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Direct+observation+of+Na+and+O+impurities+at+grain+surfaces+of+CuInSe2+thin+films.">Direct observation of Na and O impurities at grain surfaces of CuInSe2 thin films.</a> J. Vac. Sci. Technol. A. 17, 291-296 (1998).</li><li>Rockett, A., Granath, K., Asher, S., Al Jassim, M. M., Hasoon, F., Matson, R., Basol, B., Kapur, V., Britt, J. S., Gillespie, T., Marshall, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Na+incorporation+in+Mo+and+CuInSe2+from+production+processes.">Na incorporation in Mo and CuInSe2 from production processes.</a> Sol. Energy. 59, 255-264 (1999).</li><li>Heske, C., Eich, D., Fink, R., Umbach, E., Kakar, S., van Buuren, T., Bostedt, C., Terminello, L. J., Grush, M. M., Callcott, T. A., Himpsel, F. J., Ederer, D. L., Perera, R. C. C., Riedl, W., Karg, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Localization+of+Na+impurities+at+the+buried+CdS/Cu(In,+Ga)Se2+heterojunction.">Localization of Na impurities at the buried CdS/Cu(In, Ga)Se2 heterojunction.</a> Appl. Phys. Lett. 75, 2082-2084 (1999).</li><li>Braunger, D., Hariskos, D., Bilger, G., Rau, U., Schock, H. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Influence+of+Na+on+the+growth+of+polycrystalline+Cu(In,Ga)Se2+thin+films.">Influence of Na on the growth of polycrystalline Cu(In,Ga)Se2 thin films.</a> Thin Solid Films. 361, 161-166 (2000).</li><li>Cerezo, A., Godfrey, T. J., Sijbrandij, S. J., Smith, G. D. W., Warren, P. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Performance+of+an+energy-compensated+three-dimensional+atom+probe.">Performance of an energy-compensated three-dimensional atom probe.</a> Rev. Sci. Instrum. 69, 49-58 .</li><li>Blavette, D., Bostel, A., Sarrau, J. M., Deconihout, B., Menand, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=An+atom-probe+for+three+dimensional+tomography.">An atom-probe for three dimensional tomography.</a> Nature. 363, 432-435 (1993).</li><li>Gault, B., Vurpillot, F., Vella, A., Gilbert, M., Menand, A., Blavette, D., Deconihout, B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Design+of+a+femtosecond+laser+assisted+tomographic+atom+probe.">Design of a femtosecond laser assisted tomographic atom probe.</a> Rev. Sci. Instrum. 77, 043705-1-043705-8 (2006).</li><li>Kelly, T. F., Miller, M. K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Atom+probe+tomography.">Atom probe tomography.</a> Rev. Sci. Instrum. 78, 031101-1-031101-20 (2007).</li><li>Thompson, K., Lawrence, D., Larson, D. J., Olson, J. D., Kelly, T. F., Gorman, B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=In+situ+site-specific+specimen+preparation+for+atom+probe+tomography.">In situ site-specific specimen preparation for atom probe tomography.</a> Ultramicroscopy. 107 (2-3), 131-139 (2007).</li><li>Cadel, E., Barreau, N., Kessler, J., Pareige, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Atom+probe+study+of+sodium+distribution+in+polycristalline+Cu(In,Ga)Se2+thin+film.">Atom probe study of sodium distribution in polycristalline Cu(In,Ga)Se2 thin film.</a> Acta Material. 58, 2634-2637 (2010).</li><li>Schlesiger, R., Oberdorfer, C., W&#252;rz, R., Greiwe, G., Stender, P., Artmeier, M., Pelka, P., Spaleck, F., Schmitz, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Design+of+a+laser-assisted+tomographic+atom+probe+at+M&#252;nster+University.">Design of a laser-assisted tomographic atom probe at M&#252;nster University.</a> Rev. Sci. Instr. 81, 043703 (2010).</li><li>Cojocaru-Mir&#233;din, O., Choi, P., Abou-Ras, D., Schmidt, S. S., Caballero, R., Raabe, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Characterization+of+grain+boundaries+in+Cu(In,Ga)Se2+films+using+atom-probe+tomography.">Characterization of grain boundaries in Cu(In,Ga)Se2 films using atom-probe tomography.</a> IEEE J. Photovolt. 1 (2), 207-212 (2011).</li><li>Cojocaru-Mir&#233;din, O., Choi, P., Wuerz, R., Raabe, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Atomic-scale+characterization+of+the+CdS/CuInSe2+interface+in+thin-film+solar+cells.">Atomic-scale characterization of the CdS/CuInSe2 interface in thin-film solar cells.</a> Appl. Phys. Lett. 98, 103504-1-103504-3 (2011).</li><li>Couzinie-Devy, F., Cadel, E., Barreau, N., Arzel, L., Pareige, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Atom+probe+study+of+Cu-poor+to+Cu-rich+transition+during+Cu(In,Ga)Se2+growth.">Atom probe study of Cu-poor to Cu-rich transition during Cu(In,Ga)Se2 growth.</a> Appl. Phys. Lett. 99, 232108-1-232108-3 (2011).</li><li>Voorwinden, G., Jackson, P., Kniese, R., Powalla, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=In-line+Cu(In,Ga)Se2+co-evaporation+process+on+30+cm+x+30+cm+substrates+with+multiple+deposition+stages.">In-line Cu(In,Ga)Se2 co-evaporation process on 30 cm x 30 cm substrates with multiple deposition stages.</a> , 2115-2118 (2007).</li><li>Miller, M. K., Russell, K. F., Thompson, K., Alvis, R., Larson, D. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Review+of+atom+probe+FIB-based+specimen+preparation+methods.">Review of atom probe FIB-based specimen preparation methods.</a> Microscopy Microanal. 13 (6), 428-436 (2007).</li><li>J, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Modeling+image+distortions+in+3DAP.">Modeling image distortions in 3DAP.</a> Microscopy and Microanalysis. 10 (3), 384-390 (2008).</li><li>Kellog, G. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Determining+the+field+emitter+temperature+during+laser+irradiation+in+the+pulsed+laser+atom+probe.">Determining the field emitter temperature during laser irradiation in the pulsed laser atom probe.</a> J. Appl. Phys. 52, 5320 (1981).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> IVASTM 3.6.2 User Guide 2012. , (2012).</li><li>Persson, C., Zunger, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Compositionally+induced+valence-band+offset+at+the+grain+boundary+of+polycrystalline+chalcopyrites+creates+a+hole+barrier.">Compositionally induced valence-band offset at the grain boundary of polycrystalline chalcopyrites creates a hole barrier.</a> Appl. Phys. Lett. 87, 211904-1-211904-3 (2005).</li><li>Zhang, S. B., Wei, S. -. H., Zunger, A., Katayama-Yoshida, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Defect+physics+of+the+CuInSe2+chalcopyrite+semiconductor.">Defect physics of the CuInSe2 chalcopyrite semiconductor.</a> Phys. Rev. B. 57, 9642-9656 (1998).</li><li>Cahn, J. W., Johnson, W. C., Blakely, J. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Interfacial Segregation. , 3-23 (1979).</li><li>Miller, M. K., Jayaram, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Some+factors+affecting+analysis+in+atom+probe.">Some factors affecting analysis in atom probe.</a> Surf. Sci. 266, 458-462 (1992).</li><li>Wuerz, R., Eicke, A., Kessler, F., Paetel, S., Efimenko, S., Schlegel, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=CIGS+thin-film+solar+cells+and+modules+on+enamelled+steel+substrates.">CIGS thin-film solar cells and modules on enamelled steel substrates.</a> Sol. Energy. 100, 132-137 (2012).</li><li>De Geuser, F., Lefebvre, W., Danoix, F., Vurpillot, F., Forbord, B., Blavette, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=An+improved+reconstruction+procedure+for+the+correction+of+local+magnification+effects+in+three-dimensional+atom-probe.">An improved reconstruction procedure for the correction of local magnification effects in three-dimensional atom-probe.</a> Surf. Interf. Anal. 39, 268-272 (2007).</li><li>Kingham, D. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+post-ionization+of+field+evaporated+ions:+A+theoretical+explanation+of+multiple+charge+states.">The post-ionization of field evaporated ions: A theoretical explanation of multiple charge states.</a> Surf. Sci. 116, 273-301 (1982).</li><li>Letellier, 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> Etude des joints de grains et interphases dans les superalliages Astroloy par microscopie electronique et tomographie atomique [dissertation]. , (1994).</li><li>Hoummada, I., Mangelinck, K., Chow, D., Lee, J., Bernardini, <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Original+methods+for+diffusion+measurements+in+polycrystalline+thin-films.">Original methods for diffusion measurements in polycrystalline thin-films.</a> Defect and Diffusion Forum. 322, 129-150 (2012).</li></ol>

<p class="jove_content"&gt;什么都没有透露。</p&gt;

在当前的工作中，我们提出了铜铟镓硒的随机HAGB中，化合物半导体材料，用于光伏应用APT结果。此外，我们还表明，APT结合互补的技术，如EBSD和TEM是一个功能强大的工具来阐明的CIGS太阳能电池的结构组成性能关系。不幸的是，APT和EDX / EELS在TEM之间的相关性是不可能的，因为首先，EDX / EELS有没有足够的分辨率来检测低Na和O浓度晶界其次，EDX / EELS是不敏感的所有元素，尤其是娜和O <p class="jove_c...

<html>超过二十年的，因为他们的效率高，抗辐射，长期稳定，一直在开发基于铜矿结构的化合物半导体沉积Cu（In，Ga）的硒（CIGS）作为吸收材料的薄膜太阳能电池性能和低的生产成本1-3。可以制造这些太阳能电池中，只有很少的材料消耗，由于CIGS吸收层的良好的光学性能，即，直接带隙和高吸收系数1,2。足以产生高的光吸收体膜的厚度只有几微米。由于电极的光生电荷载流子的扩散路径比较短，CIGS吸收体，可以以多晶形式。铜的最大效率（铟，镓）硒（CIGS）太阳能电池迄今取得的20.4％，这是所有薄膜太阳能电池中的最高值。 ove_content“&gt;为进一步建立的CIGS薄膜光伏技术，既降低生产成本和提高太阳能电池的效率是必不可少的，后者是强烈地依赖于CIGS吸收层的微观结构和化学组成的内部接口，在吸收塔内的特定的晶界（GBS），发挥了举足轻重的作用，因为它们可能影响运输的光生载流子。 CIGS太阳能电池方面尚未解决的主要问题之一是的良性性质CIGS GBS， 即多晶的CIGS吸收薄膜产量优秀的电池效率，尽管高密度的晶界和晶格缺陷。 几位作者研究金紫荆星章CIGS薄膜太阳能级就其电学性能5,6，性格和取向差7-9以及杂质分离10-13。但是，没有明确的联系这些properti之间ES可以成立至今。特别是，有相当大的缺乏有关本地的化学组成和晶界的杂质含量。 在过去的二十年中，原子探针断层扫描（APT）已成为一个有前途的纳米分析技术14-17。直到最近，APT的太阳能电池的研究已经在很大程度上限制在样品制备过程中的困难，并使用传统的脉冲电压的原子探针分析半导体材料的能力有限。这些限制已经在很大程度上克服的发展“升出法的基础上，聚焦离子束（FIB）铣18台 ，并引进脉冲激光APT 16。已经发表了多篇论文关于APT表征CIGS太阳能电池19-23，这是大力鼓励作进一步调查。 本文给出了如何学习内部I指引nterfaces在铜铟镓硒薄膜太阳能电池由原子探针层析成像技术。

atom probe tomography studies on the cu(in,ga)se2 grain boundaries

与已有技术相比，原子探针断层扫描是一个独特的技术，能够在纳米级，并在三维空间中的化学特性的内部接口。事实上，APT具有高灵敏度（ppm级）和高空间分辨率（子纳米）。 在这里做了相当大的努力准备包含所需的晶界结构与已知的APT尖。事实上，特定于站点的样品制备使用聚焦离子束，电子背散射衍射和透射电子显微镜相结合，提出了这项工作。这种方法允许选择晶界已知的结构和位置，铜（铟，镓）硒薄膜薄膜加以研究，原子探针断层扫描。 最后，我们讨论了使用原子探针断层扫描技术来研究晶界（铜铟，镓）硒薄膜太阳能电池的优点和缺点。

图3示出的侧视图（XZ片）元素的地图随机高角度GB（HAGB）28.5° - &lt;511&gt;通过位点特异性制备方法在图2中选择的幼崽 。使用APT，共分离的钠，钾，和O在CIGS HAGB的直接映射。最有可能在这些杂质扩散到吸收层的沉积过程中在〜600℃的CIGS层的SLG衬底 图4a示出了铜，地，镓和硒的浓度分布横跨GB 如图3所示。铜，铟，镓，...

Watch this Scientific Journal Video about Atom Probe Tomography Studies on the CuIn,GaSe2 Grain Boundaries at JoVE.com

Atom Probe Tomography Studies on the CuIn,GaSe2 Grain Boundaries

在这项工作中，我们描述了使用的原子探针层析成像技术研究中的CIGS型太阳能电池的吸收层的晶粒边界。这里也提出一种新颖的方法来准备包含所需的晶界结构与已知的原子探针提示。

原子探针层析成像研究在Cu（铟，镓）硒<sub&gt; 2</sub&gt;晶界

Compared with the existent techniques, atom probe tomography is a unique technique able to chemically characterize the internal interfaces at the ...

atom-probe-tomography-studies-on-the-cuingase2-grain-boundaries

Research

JoVE Journal

Engineering

Atom Probe Tomography Studies on the Cu(In,Ga)Se2 Grain Boundaries

12.6K 次观看.  Max-Planck-Institut für Eisenforschung GmbH. 在这项工作中，我们描述了使用的原子探针层析成像技术研究中的CIGS型太阳能电池的吸收层的晶粒边界。这里也提出一种新颖的方法来准备包含所需的晶界结构与已知的原子探针提示。

视频: Atom Probe Tomography Studies on the CuIn,GaSe2 Grain Boundaries

Scanning-probe Single-electron Capacitance Spectroscopy

The integration of low-temperature scanning-probe techniques and single-electron capacitance spectroscopy represents a powerful tool to study the electronic quantum structure of small systems - including individual atomic dopants in semiconductors. Here we present a capacitance-based method, known as Subsurface Charge Accumulation (SCA) imaging, which is capable of resolving single-electron charging while achieving sufficient spatial resolution to image individual atomic dopants. The use of a capacitance technique enables observation of subsurface features, such as dopants buried many nanometers beneath the surface of a semiconductor material1,2,3. In principle, this technique can be applied to any system to resolve electron motion below an insulating surface.
As in other electric-field-sensitive scanned-probe techniques4, the lateral spatial resolution of the measurement depends in part on the radius of curvature of the probe tip. Using tips with a small radius of curvature can enable spatial resolution of a few tens of nanometers. This fine spatial resolution allows investigations of small numbers (down to one) of subsurface dopants1,2. The charge resolution depends greatly on the sensitivity of the charge detection circuitry; using high electron mobility transistors (HEMT) in such circuits at cryogenic temperatures enables a sensitivity of approximately 0.01 electrons/Hz&frac12; at 0.3 K 5.

Scanning-probe single-electron capacitance spectroscopy facilitates the study of single-electron motion in localized subsurface regions. A sensitive charge-detection circuit is incorporated into a cryogenic scanning probe microscope to investigate small systems of dopant atoms beneath the surface of semiconductor samples.

扫描探针单电子电容谱

The integration of low-temperature scanning-probe techniques and single-electron capacitance spectroscopy represents a powerful tool to study the ...

科研

工程学

The Measurement of Unsteady Surface Pressure Using a Remote Microphone Probe

Microphones are widely applied to measure pressure fluctuations at the walls of solid bodies immersed in turbulent flows. Turbulent motions with various characteristic length scales can result in pressure fluctuations over a wide frequency range. This property of turbulence requires sensing devices to have sufficient sensitivity over a wide range of frequencies. Furthermore, the small characteristic length scales of turbulent structures require small sensing areas and the ability to place the sensors in very close proximity to each other. The complex geometries of the solid bodies, often including large surface curvatures or discontinuities, require the probe to have the ability to be set up in very limited spaces. The development of a remote microphone probe, which is inexpensive, consistent, and repeatable, is described in the present communication. It allows for the measurement of pressure fluctuations with high spatial resolution and dynamic response over a wide range of frequencies. The probe is small enough to be placed within the interior of typical wind tunnel models. The remote microphone probe includes a small, rigid, and hollow tube that penetrates the model surface to form the sensing area. This tube is connected to a standard microphone, at some distance away from the surface, using a "T" junction. An experimental method is introduced to determine the dynamic response of the remote microphone probe. In addition, an analytical method for determining the dynamic response is described. The analytical method can be applied in the design stage to determine the dimensions and properties of the RMP components.

Here, we present a protocol to measure, with high spatial resolution, the unsteady surface pressure in turbulent flows. This method demonstrates the construction of a remote microphone probe (RMP) and the determination of its frequency-dependent, complex transfer function. An analytical determination of the dynamic response is presented and validated.

非定常表面压力的使用远程麦克风探头测量

Microphones are widely applied to measure pressure fluctuations at the walls of solid bodies immersed in turbulent flows. Turbulent motions with various ...

Microfluidic Imaging Flow Cytometry by Asymmetric-detection Time-stretch Optical Microscopy (ATOM)

Scaling the number of measurable parameters, which allows for multidimensional data analysis and thus higher-confidence statistical results, has been the main trend in the advanced development of flow cytometry. Notably, adding high-resolution imaging capabilities allows for the complex morphological analysis of cellular/sub-cellular structures. This is not possible with standard flow cytometers. However, it is valuable for advancing our knowledge of cellular functions and can benefit life science research, clinical diagnostics, and environmental monitoring. Incorporating imaging capabilities into flow cytometry compromises the assay throughput, primarily due to the limitations on speed and sensitivity in the camera technologies. To overcome this speed or throughput challenge facing imaging flow cytometry while preserving the image quality, asymmetric-detection time-stretch optical microscopy (ATOM) has been demonstrated to enable high-contrast, single-cell imaging with sub-cellular resolution, at an imaging throughput as high as 100,000 cells/s. Based on the imaging concept of conventional time-stretch imaging, which relies on all-optical image encoding and retrieval through the use of ultrafast broadband laser pulses, ATOM further advances imaging performance by enhancing the image contrast of unlabeled/unstained cells. This is achieved by accessing the phase-gradient information of the cells, which is spectrally encoded into single-shot broadband pulses. Hence, ATOM is particularly advantageous in high-throughput measurements of single-cell morphology and texture &#8211; information indicative of cell types, states, and even functions. Ultimately, this could become a powerful imaging flow cytometry platform for the biophysical phenotyping of cells, complementing the current state-of-the-art biochemical-marker-based cellular assay. This work describes a protocol to establish the key modules of an ATOM system (from optical frontend to data processing and visualization backend), as well as the workflow of imaging flow cytometry based on ATOM, using human cells and micro-algae as the examples.

Microfluidic Imaging Flow Cytometry by Asymmetric-detection Time-stretch Optical Microscopy ATOM

This protocol describes the implementation of an asymmetric-detection time-stretch optical microscopy system for single-cell imaging in ultrafast microfluidic flow and its applications in imaging flow cytometry.

微流控成像流式细胞仪通过不对称检测时间延伸光学显微镜（ATOM）

Scaling the number of measurable parameters, which allows for multidimensional data analysis and thus higher-confidence statistical results, has been the ...

In Situ Monitoring of the Accelerated Performance Degradation of Solar Cells and Modules: A Case Study for Cu(In,Ga)Se2 Solar Cells

The levelized cost of electricity (LCOE) of photovoltaic (PV) systems is determined by, among other factors, the PV module reliability. Better prediction of degradation mechanisms and prevention of module field failure can consequently decrease investment risks as well as increase the electricity yield. An improved knowledge level can for these reasons significantly decrease the total costs of PV electricity. 
In order to better understand and minimize the degradation of PV modules, the occurring degradation mechanisms and conditions should be identified. This should preferably happen under combined stresses, since modules in the field are also simultaneously exposed to multiple stress factors. Therefore, two 'Combined Stress test with in situ measurement' setups have been designed and constructed. These setups allow the simultaneous use of humidity, temperature, illumination, and electrical biases as independently controlled stress factors on solar cells and minimodules. The setups also allow real-time monitoring of the electrical properties of these samples. This protocol presents these setups and describes the experimental possibilities. Moreover, results obtained with these setups are also presented: various examples about the influence of both deposition and degradation conditions on the stability of thin film Cu(In,Ga)Se2 (CIGS) as well as Cu2ZnSnSe4 (CZTS) solar cells are described. Results on the temperature dependency of CIGS solar cells are also presented.

In Situ Monitoring of the Accelerated Performance Degradation of Solar Cells and Modules: A Case Study for CuIn,GaSe2 Solar Cells

Two &#39;Combined Stress test with in situ measurement&#39; setups, which allow real-time monitoring of accelerated degradation of solar cells and modules, were designed and constructed. These setups allow the simultaneous use of humidity, temperature, electrical biases, and illumination as independently controlled stress factors. The setups and various experiments executed are presented.

就地太阳能电池和模块加速性能退化的监测: 铜 (in, Ga) Se2太阳能电池的实例研究

The levelized cost of electricity (LCOE) of photovoltaic (PV) systems is determined by, among other factors, the PV module reliability. Better prediction ...

Fabrication of Magnetic Nanostructures on Silicon Nitride Membranes for Magnetic Vortex Studies Using Transmission Microscopy Techniques

Electron and x-ray magnetic microscopies allow for high-resolution magnetic imaging down to tens of nanometers. However, the samples need to be prepared on transparent membranes which are very fragile and difficult to manipulate. We present processes for the fabrication of samples with magnetic micro- and nanostructures with spin configurations forming magnetic vortices suitable for Lorentz transmission electron microscopy and magnetic transmission x-ray microscopy studies. The samples are prepared on silicon nitride membranes and the fabrication consists of a spin coating, UV and electron-beam lithography, the chemical development of the resist, and the evaporation of the magnetic material followed by a lift-off process forming the final magnetic structures. The samples for the Lorentz transmission electron microscopy consist of magnetic nanodiscs prepared in a single lithography step. The samples for the magnetic x-ray transmission microscopy are used for time-resolved magnetization dynamic experiments, and magnetic nanodiscs are placed on a waveguide which is used for the generation of repeatable magnetic field pulses by passing an electric current through the waveguide. The waveguide is created in an extra lithography step.

A protocol for the fabrication of magnetic micro- and nanostructures with spin configurations forming magnetic vortices suitable for transmission electron microscopy (TEM) and magnetic transmission x-ray microscopy (MTXM) studies is presented.

用透射显微技术制备氮化硅薄膜磁性纳米结构的研究

Electron and x-ray magnetic microscopies allow for high-resolution magnetic imaging down to tens of nanometers. However, the samples need to be prepared ...

Fabrication of Robust Nanoscale Contact between a Silver Nanowire Electrode and CdS Buffer Layer in Cu(In,Ga)Se2 Thin-film Solar Cells

Silver nanowire transparent electrodes have been employed as window layers for Cu(In,Ga)Se2 thin-film solar cells. Bare silver nanowire electrodes normally result in very poor cell performance. Embedding or sandwiching silver nanowires using moderately conductive transparent materials, such as indium tin oxide or zinc oxide, can improve cell performance. However, the solution-processed matrix layers can cause a significant number of interfacial defects between transparent electrodes and the CdS buffer, which can eventually result in low cell performance. This manuscript describes how to fabricate robust electrical contact between a silver nanowire electrode and the underlying CdS buffer layer in a Cu(In,Ga)Se2 solar cell, enabling high cell performance using matrix-free silver nanowire transparent electrodes. The matrix-free silver nanowire electrode fabricated by our method proves that the charge-carrier collection capability of silver nanowire electrode-based cells is as good as that of standard cells with sputtered ZnO:Al/i-ZnO as long as the silver nanowires and CdS have high-quality electrical contact. The high-quality electrical contact was achieved by depositing an additional CdS layer as thin as 10 nm onto the silver nanowire surface.

Fabrication of Robust Nanoscale Contact between a Silver Nanowire Electrode and CdS Buffer Layer in CuIn,GaSe2 Thin-film Solar Cells

In this protocol, we describe the detailed experimental procedure for the fabrication of a robust nanoscale contact between a silver nanowire network and CdS buffer layer in a CIGS thin-film solar cell.

在 Cu(In、Ga)Se2薄膜太阳能电池中制造银纳米线电极与 CdS 缓冲层之间的强健纳米级接触

Silver nanowire transparent electrodes have been employed as window layers for Cu(In,Ga)Se2 thin-film solar cells. Bare silver nanowire electrodes ...

Visualization of Failure and the Associated Grain-Scale Mechanical Behavior of Granular Soils under Shear using Synchrotron X-Ray Micro-Tomography

The rapid development of X-ray imaging techniques with image processing and analysis skills has enabled the acquisition of CT images of granular soils with high-spatial resolutions. Based on such CT images, grain-scale mechanical behavior such as particle kinematics (i.e., particle translations and particle rotations), strain localization and inter-particle contact evolution of granular soils can be quantitatively investigated. However, this is inaccessible using conventional experimental methods. This study demonstrates the exploration of the grain-scale mechanical behavior of a granular soil sample under triaxial compression using synchrotron X-ray micro-tomography (&#956;CT). With this method, a specially fabricated miniature loading apparatus is used to apply confining and axial stresses to the sample during the triaxial test. The apparatus is fitted into a synchrotron X-ray tomography setup so that high-spatial resolution CT images of the sample can be collected at different loading stages of the test without any disturbance to the sample. With the capability of extracting information at the macro scale (e.g., sample boundary stresses and strains from the triaxial apparatus setup) and the grain scale (e.g., grain movements and contact interactions from the CT images), this procedure provides an effective methodology to investigate the multi-scale mechanics of granular soils.

The protocol describes procedures to acquire high-spatial resolution computed tomography (CT) images of a granular soil during triaxial compression, and to apply image processing techniques to these CT images to explore the grain-scale mechanical behavior of the soil under loading.

使用同步加速器 X 射线微断层扫描技术，在剪切下对颗粒土壤的故障和相关的颗粒级机械性能进行可视化

The rapid development of X-ray imaging techniques with image processing and analysis skills has enabled the acquisition of CT images of granular soils ...

Improving the Combustion Performance of a Hybrid Rocket Engine using a Novel Fuel Grain with a Nested Helical Structure

A technique to improve the combustion performance of a hybrid rocket engine using a novel fuel grain structure is presented. This technique utilizes the different regression rates of acrylonitrile butadiene styrene and paraffin-based fuels, which increase the exchanges of both matter and energy by swirl flow and recirculation zones formed at the grooves between the adjacent vanes. The centrifugal casting technique is used to cast the paraffin-based fuel into an acrylonitrile butadiene styrene substrate made by three-dimensional printing. Using oxygen as the oxidizer, a series of tests were conducted to investigate the combustion performance of the novel fuel grain. In comparison to paraffin-based fuel grains, the fuel grain with a nested helical structure, which can be maintained throughout the combustion process, showed significant improvement in the regression rate and great potential in improvement of combustion efficiency.

A technique utilizing a solid fuel grain with a novel nested helical structure to improve the combustion performance of a hybrid rocket engine is presented.

使用具有嵌套的 Helical 结构的新颖燃料颗粒提高混合火箭发动机的燃烧性能

A technique to improve the combustion performance of a hybrid rocket engine using a novel fuel grain structure is presented. This technique utilizes the ...

Co-localizing Kelvin Probe Force Microscopy with Other Microscopies and Spectroscopies: Selected Applications in Corrosion Characterization of Alloys

Kelvin probe force microscopy (KPFM), sometimes referred to as surface potential microscopy, is the nanoscale version of the venerable scanning Kelvin probe, both of which measure the Volta potential difference (VPD) between an oscillating probe tip and a sample surface by applying a nulling voltage equal in magnitude but opposite in sign to the tip-sample potential difference. By scanning a conductive KPFM probe over a sample surface, nanoscale variations in surface topography and potential can be mapped, identifying likely anodic and cathodic regions, as well as quantifying the inherent material driving force for galvanic corrosion.
Subsequent co-localization of KPFM Volta potential maps with advanced scanning electron microscopy (SEM) techniques, including back scattered electron (BSE) images, energy dispersive spectroscopy (EDS) elemental composition maps, and electron backscattered diffraction (EBSD) inverse pole figures can provide further insight into structure-property-performance relationships. Here, the results of several studies co-localizing KPFM with SEM on a wide variety of alloys of technological interest are presented, demonstrating the utility of combining these techniques at the nanoscale to elucidate corrosion initiation and propagation.
Important points to consider and potential pitfalls to avoid in such investigations are also highlighted: in particular, probe calibration and the potential confounding effects on the measured VPDs of the testing environment and sample surface, including ambient humidity (i.e., adsorbed water), surface reactions/oxidation, and polishing debris or other contaminants. Additionally, an example is provided of co-localizing a third technique, scanning confocal Raman microscopy, to demonstrate the general applicability and utility of the co-localization method to provide further structural insight beyond that afforded by electron microscopy-based techniques.

Kelvin probe force microscopy (KPFM) measures surface topography and differences in surface potential, while scanning electron microscopy (SEM) and associated spectroscopies can elucidate surface morphology, composition, crystallinity, and crystallographic orientation. Accordingly, the co-localization of SEM with KPFM can provide insight into the effects of nanoscale composition and surface structure on corrosion.

开尔文探针力显微镜与其他显微镜和光谱学共定位：合金腐蚀表征中的选定应用

Kelvin probe force microscopy (KPFM), sometimes referred to as surface potential microscopy, is the nanoscale version of the venerable scanning Kelvin ...

Application of Deep Learning-Based Medical Image Segmentation via Orbital Computed Tomography

Recently, deep learning-based segmentation models have been widely applied in the ophthalmic field. This study presents the complete process of constructing an orbital computed tomography (CT) segmentation model based on U-Net. For supervised learning, a labor-intensive and time-consuming process is required. The method of labeling with super-resolution to efficiently mask the ground truth on orbital CT images is introduced. Also, the volume of interest is cropped as part of the pre-processing of the dataset. Then, after extracting the volumes of interest of the orbital structures, the model for segmenting the key structures of the orbital CT is constructed using U-Net, with sequential 2D slices that are used as inputs and two bi-directional convolutional long-term short memories for conserving the inter-slice correlations. This study primarily focuses on the segmentation of the eyeball, optic nerve, and extraocular muscles. The evaluation of the segmentation reveals the potential application of segmentation to orbital CT images using deep learning methods.

Application of Deep Learning-Based Medical Image Segmentation via Orbital Computed Tomography

An object segmentation protocol for orbital computed tomography (CT) images is introduced. The methods of labeling the ground truth of orbital structures by using super-resolution, extracting the volume of interest from CT images, and modeling multi-label segmentation using 2D sequential U-Net for orbital CT images are explained for supervised learning.