This work was supported in part by Green Network of Excellence (GRENE) project from the Ministry of Education, Culture, Sport, and Technology (MEXT) in Japan. The authors are also grateful to the technicians of the Sialon Unit for their help in the phosphors synthesis, to MANA for its help in EDS measurements and to K. Nakagawa for the help in the CL system.

1.样品<ol><li>荧光粉合成<ol><li>设计产品，确定基于所述预期的化学反应的起始材料和它们的重量。准确控制原料原料粉末14-20。 </li><li>粉碎并用手在玛瑙研钵它们混合。取决于原料粉末的质量，以获得尽可能均匀地混合混合15-30分钟。包装粉末混合物到氮化硼坩埚中。 注:执行步骤1.1.1-1.1.2中在惰性气体下的手套箱中，以非常低的氧浓度作为最终产物或原料粉末在空气中是不稳定的。 </li><li>火在用石墨加热器的气体加压烧结炉的粉末混合物。以恒定的加热速率加热所述样品。引入到室中的预先确定的氮气（纯度为99.999％），并同时提高了温度为所需的值。 注意:保持同样的条件，sinte期间<html>环。根据材料14-20的加热温度和持续时间是不同的。 </li><li>烧成后，切断电源，并让样品冷却下来炉内。手工压碎以及在玛瑙研钵中烧结粉末，直至获得细颗粒。 </li></ol></li><li>横截面<ol><li>混合150毫克与300毫克的树脂和30毫克硬化剂的荧光体。倒入硅酮模具中，在60℃下烘烤30分钟在真空中从混合物蒸发氧气。 </li><li>放入硅模具和烘烤再次在100℃下60分钟在空气中，以制造粉末嵌入式芯片。在加热过程中，最粉末在底部沉积，由于高的材料密度。 </li><li>抛光由手持圈和氩离子截面抛光的装置的芯片的底面的面，以产生镜面。成型粉末的更高的量允许粉末的内部结构的更好的观察。 </li></ol></li></ol>jove_title"&gt; 2。阴极发光<ol><li>样品和设置准备 注意:作为CL是非接触技术，存在用于测量本身没有特别的要求。制备将取决于测量的目标。因此，对于定量测量，可以优选把大量的粉末的碳上的磁带，或者制成一个膜。定性测量，分离的颗粒的调查可通过将粉末少量在碳胶带，或分散的粉末在乙醇中，佛光普照一种常规铜微电网用于TEM中的溶液受到青睐。 <ol><li>调整样品载物台的高度对齐与参考级（12mm）中的样品的顶部。 </li><li>插入样品台到腔室。插入电子枪和样品之间的椭圆面反射镜。确保样品不接触椭圆面反射镜，以防止污染的镜像或打破它。 </li><li>补凉ING探测器油藏液体N 2。打开探测器上。等到探测器温度马厩开始CL测量。用于测量的理想的温度为110 K。注:温度可在软件进行检查。 </li></ol></li><li> CL测量 注意:电子束的条件，特别是电子束能量和束电流，被选中。这些条件应在样品的预期的发光强度，观察到的充电，发光退化和在深度分析的利益的函数来选择。 <ol><li>要采取SEM和/或CL谱电子束位置。重点以衬托出定义的形状和矫正散光以获得清晰锐利的图像的图像。调整阶段的高度和工作距离。校正用的x，放大的图像上ýstigmators散光。启动CL采集软件。 </li><li>优化镜位置与样品高度得到的发光光谱强度最强。要执行它，点击"实时测量"，并选择软件"连续模式"。设置反射镜中的单色仪作为"前侧"，以分散的光发送到CCD，并采取快速的CL谱。慢慢地改变反射镜的位置和样本高度同时保持SE影象聚焦并提高发光强度。 </li><li>对于大面积的发光光谱，点击"实时测量"图标，并选择上的软件"一次性模式"。为了将发射的光发送到CCD配置的光检测系统。取决于样品，选择光栅，狭缝宽度和测量收集时间，以获得最合适的强度/光谱分辨率。 </li><li>对于CL单色影像，点击"图片测量"图标，并选择软件上的"PMT探测器"。设置镜单色一的"后侧"，以分散的光发送到PMT检测，并插入的狭缝。根据不同的样品，选择分辨率，放大的，可取的收集波长和时间。冻结图像，并将其发送给软件。 </li><li>对于本地CL分析，先取SE或CL图像。点击"测量"图标，选择取图像上谱的位置。配置的光检测系统，以便将发射的光发送到CCD，然后采取的CL谱。 </li><li>对于CL时间的演化，点击"时间相关测量"图标，并选择软件上的"CCD"。为了将发射的光发送到CCD检测器配置的光检测系统。根据不同的软件，选择光谱和2测量之间的时间的数字，例如360光谱每10秒。 </li></ol></li></ol>

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The authors have nothing to disclose.

通过对塞隆荧光低能耗CL表征这些代表性的例子，我们已经表明了荧光粉调查强大和快速的技术如何能。通过测量当地的CL测量和制图，以在样品制备的灵活性优势，CL与其他技术相结合，我们可以更准确地归因于发光的起源，明确的增长机制，并确定应用程序最适合的荧光粉。这些结果主要是可以实现的，由于在电子显微镜的改进和光检测器，这增强了测量收集时间，灵敏度和空间分辨率。 既赛隆荧光体和CL字段不自然不限于本文所提出的各个方面。在下文中，为了扩大的讨论中，我们将分别讨论关于他们多一点点。 在箱体O˚F塞隆荧光，用自己优异的发光和稳定性，他们正在被越来越多的用于照明应用。然而，它们也显示非常有趣的机械，热，磁，超导，电气，电子和光学性质，这可以通过改变它们的组合物来调节。因此，它们也在广泛的应用，例如抗反射涂层，太阳能吸收剂，热反射镜，有色颜料，可见光驱动光催化剂，透明窗口和装甲，或荧光探针用于生物医学成像29找到。我们可以预见，他们将发挥在许多能源和环境相关方面的关键角色，如高效收获太阳能，实现氢经济，减少了环境污染，节约自然资源， 等等。然而，大量的工作仍然需要继续改进它们的性能，同时降低其生产成本，如decreASING烧结温度或限制使用的稀土离子。它可以通过寻找新颖赛隆荧光体，和澄清的对性能的组合物和生长条件的作用来实现。我们已经看到，CL能起到为实现这些目标发挥重要作用。但是，最近的新方法也透露非常有前途的可能性。这些方法中的两个是时间飞行二次离子质谱法（TOF-SIMS）及单粒子的诊断。 TOF-SIMS是能够以高灵敏度，这使得不仅在痕量检测物种中，而且在氧化状态31的差异空间上解决整个质谱。单粒子诊断由在一个复杂的混合物作为微小单晶单个发光颗粒的治疗，并调查由超分辨率单晶X射线衍射装置和单粒子荧光的光学和结构特性31。 <p类="jove_content"&gt;至于低能量CL表征，在本文中，我们已主要集中在使用的CL为赛隆荧光体，而CL也可以用于其他的材料，如半导体，纳米结构，有机材料，和陶瓷。另一方面，虽然CL为光电子材料的定性表征的宝贵的技术，它也诱导定量测量一些注意事项。事实上，CL结果不仅取决于激励的条件下，电子束电流和电子能量，也取决于研究的材料25的量。因此，这些参数的微小变化可能显著改变发光强度。此外，电子束辐照可以提高损伤样本的可能性。它可能会引起强度的急剧变化，或诱导的新的发光中心，这可能影响定量CL测量的可靠性的创建/活化。 CL的材料茶发展racterization是，将密切相关的在电子束显微镜的改进和光检测器。因此，现在有可能要执行的TEM。它允许一个更高的空间分辨率和的发光变化原位观察伴随有引起电子束诱导原子位移微观结构变化的发光变化的直接观察，例如32-34。此外，通过加入与该光学检测器同步的在列波束阻断的，它是现在可以使用电子束在脉冲模式，其允许执行衰减轮廓测量到的电子显微镜35。它也可以认为使用脉冲电子束辐照可以降低电子束诱发的损害，这将提高定量测量的可靠性和在电子束敏感材料表征帮助。这些2实施例说明如何分析CL可能在将来得到改善。&lt;/ P&gt;

近来，越来越多的注意力投向环境问题，特别是能源生产和消费。为了回答这些社会需求，能源生产必须是"绿色"，这意味着，减少了从传统渠道能耗或开发新的环保材料。发光二极管（LED）和场发射显示器（FED）已经得到显著注意，由于其紧凑性，改进的性能和更低的功耗相比，实际的显示，如水银气体放电荧光灯或等离子体显示器1-5。用于LED和FED光源的关键因素是高效率的荧光体。稀土掺杂的磷光体是由一个主晶格和稀土掺杂剂，其可在光子激发（紫外线（UV），蓝光），电子（电子束）或电场发光的无机材料。为高效率的荧光体的要求是:1）高CONVER锡永效率与不同的激发源; 2）具有较低的热淬火稳定性好; 3）高色纯度全色彩的重现性。然而，只有磷光体的数量非常有限可目前满足这些最低要求。目前使用的氧化物系荧光体具有在可见光光谱低的吸收，而基于硫化物的那些具有低的化学和热稳定性。此外，它们显示出在电子或环境气氛中，这限制了器件的寿命劣化。因为它们的色纯度和效率是有限的，这使得它们难以被用于实现高显色指数（CRI）的发光装置。因此，需要新的荧光粉的探索。 稀土掺杂的氮化物和氧氮化物（赛隆）荧光体被认为是良好的候选者与基于其稳定化学键的结构突出的热稳定性和化学稳定性。斯托克斯位移成为一个强大的拉小ttice并将其引导到一个高转换效率和荧光体6-9的小的热淬火。在一般情况下，二价的稀土离子，如铕2+或镱2+和Ce 3+的发光归因于5D-4F电子跃迁，并包括一个宽频带的带由于主晶格峰值位置变化到5d轨道和晶体场之间的强相互作用。由于它们的特性，波长可调的发光是通过改变稀土离子的化学性质和它们的浓度在主晶格（ 图1）获得的。因此，赛隆荧光体可用于实现高CRI白光LED使用蓝绿色，红色磷光体系统和应用程序中的UV-的FED。 尽管塞隆荧光是有希望的材料，做了大量的工作，如寻找新的结构和降低成本的生产仍然需要。此外，由于困难罪的优化方面tering条件，塞隆荧光往往含有第二相18-20。 这种局部结构的调查重要的是要了解的烧结机制，优化烧结条件等，以改善赛隆荧光体的光学性质。这些目标可以通过低能量阴极（CL）技术来实现。 CL是在其中的电子照射在荧光体引起的光子发射的现象。相反的光致发光（PL），它是由光子激发诱导，激发区域通常是在毫米波和选择性激励的顺序提高特定发射过程中，电子束的激励在纳米尺度和激活所有存在于材料中的发光机制，这可能会允许不同阶段具有不同的发光特性10-12检测。此外，入射电子不仅可以产生CL信号而且各种信号，如反射电子，俄歇或X射线，其提供对材料不同的信息。因此，也可以得到的结构，化学或电性能。这些技术在一个更好的理解赛隆荧光体14-20的局部结构的起源的CL结果相结合。 CL调查可通过不同类型的电子束源13的手段来进行。现在，扫描电子显微镜（SEM）是执行CL测量最常用的系统。在下文中，我们将主要讨论这个系统。如见于图2，CL测量是通过使用一种电子源（SEM）的光收集器（光纤和单色器）和一个检测系统进行的。检测系统包括一个电荷耦合器件（CCD）和一个光电倍增管（PMT），它们分别是平行检测模式和序列检测模式的。在一般情况下，从样品收集的光由狭缝调节，然后通过单色光栅分散。当样品的收集的光被分散到CCD（平行检测模式），每个发射波长同时检测。当由狭缝（串行检测模式）选择的分散的光的特定波长，它的强度由光电倍增管记录以形成单色图像。 在本文中，我们主要强调的塞隆荧光的特性使用低能量的CL，代表性，Si掺杂的AlN 14，22，钙掺杂（镧，铈）铝（SI 6-Z 系的Al z）（ N 10-Z O z）中（z〜1）（JEM）15，硅/ EU掺杂的AlN 16，17和Ce掺杂的La 5的Si 3 O 12 N材料。采用氩离子束（CP法）截面抛光方法是观察层状结构，由于以较少的表面损伤更广泛的抛光区域的有效方法。它已经为磷光体的局部结构的调查进行。 CL的与其他基于电子技术和发光稳定性的调查的相关性也将被示出。

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low-energy cathodoluminescence for (oxy)nitride phosphors

氮化物和氮氧化合物（赛隆）磷光体为紫外和可见光发射应用的良好候选。高性能，稳定性好，它们的发射性质的灵活性可以通过控制其成分和掺杂物来实现。然而，大量的工作仍需要改善其性能，并降低了生产成本。一种可行的方法是，以优化其生长参数，并找到新的荧光粉关联与当地的结构和化学环境的赛隆颗粒的发光特性。对于这样的目的，在低电压阴极（CL）的显微镜是一种强大的技术。作为激发源使用电子允许检测大多数的发光中心，空间和深入揭示其发光分布，直接比较CL结果与其他基于电子技术，以及ST在调查其发光性能的稳定性RESS。对于磷光体表征这种优点将通过低能量的CL上几个赛隆荧光体调查的例子加以强调。

发光分布不仅横向而且深入。这种核-表面分布是通过改变电子能量与CL观察到的，因为它改变所述入射电子21的穿透深度。然而，穿透深度对于每一种材料而异，电子能量和穿透深度之间的对应关系是非线性的，并可能引入一些额外的效果，如高能量光子的距离更深的区域通过材料本身的重吸收。因此，它可能是优选的直接观察到通过截面观察核 - 表面分布。在荧光体粉末的情况下，这样的观察可以通过截面抛光的颗粒捕集到树脂和抛光的粉末 - 树脂复合材料，例如来实现。因为该颗粒随机分布在树脂中，切割方向是不可控的。然而，颗粒的高量的llows切割足够的颗粒进行这样的分析有效。 为了说明这一点，我们已经调查Si掺杂AlN粉末的发光分布。 图5a示出了掺杂有0.0％和Si 1.6％的AlN粉末的发光光谱。未掺杂的AlN的发射包括在350 2频带和380nm处的，而AlN的在350nm处具有一个带1.6％掺杂有在280nm明确肩。在350和380纳米带被归因于Al空位-氧复合物（0:N -V Al）的 ，而在与受硅形成的SiO蒸汽22的O型纯化的AlN 280nm处的肩部， 图5b和5c示出了发光在280nm为作为烧结和拍摄的图像横截面掺杂有分别的Si 1.6％，氮化铝粉末。 280 nm发射是沿着从作为烧结试样的CL图像颗粒不均匀，较亮的区域似乎是在面值边缘ticles，但粒子的形态及其分布可能使这些意见不那么明显。不过，从横截面样品的CL像，它清晰地显示了280 nm发射主要定位在所述颗粒的表面上，这表明的AlN颗粒实际上是由一富硅层和表面纯化可进行包衣。 在塞隆荧光局部组成的变化会显着影响发光性能。因此，在不同的主机晶格或在不同的位点相同的稀土类离子可以给出不同的排放15,18-20。但是，不幸的是，在烧结过程中的局部差异，如温度的分布或原料的比例，或颗粒的表面的局部氧化，预计，导致沿颗粒和/或在组合物中的变化几个阶段的共存。这样的效果可能不是二rectly与观察到的结构和化学表征技术。因此，为了调查荧光体的局部发光特性是重要的。在用SEM的电子束的大小和位置的精确控制，有可能不仅从一个纳米级区域获取的CL谱，而且，以获得发光中心的高分辨率的CL图像。 （镧，铈）铝（SI 6-Z 系的Al z）（N 10-Z O z）中（z〜1）（JEM）是一种强烈的蓝色荧光，适用于一般照明。已经发现，通过以Ca取代（镧，铈），红移和CL峰的加宽发生根据钙掺杂。有人认为，钙是影响铈3+的晶场分裂。然而，这样的解释，仅基于发光光谱，是误导，由横截面局部分析所揭示。15 图6示出了横秒TIONAL SE（CS-SE），在300纳米（红），430纳米（蓝）和540纳米（绿）和局部发光光谱在5kV为掺杂有0 JEM荧光粉采取组合的CS-CL图像（A，B， c）和0.69（D，E，F）的。钙％，分别为。它必须被注意的是，这些波长是在为了减少几个波段存在频带的情况下，重叠的选择。对于CA-未掺杂样品的CS-CL图像，JEM颗粒由相互聚集许多颗粒。在430nm处的发光几乎均匀地与一些明亮区域，并在300毫微米某些局部区域的分布。另一方面，在晶界显示较暗发射。本地CL分析表明频谱形状是在任何位置相对可比，从430至450纳米和光谱强度与图像的一致的频带的移位。对于钙掺杂CS-CL的形象，有430和540纳米之间显著的差异。亚微米贴片沿大宝清晰地出现在300和540 nm的亮较深晶粒边界区域的颗粒rtion，而430 nm发射在颗粒的另一部分的局部。当地分析，在430 nm的明亮区域（3点）所采取的CL光谱由在440nm乐队，在对钙掺杂样品观察到的可比性。亮区在540nm，嵌在相同的粒子，（点1和4）在480-490纳米的显示的频带。在300纳米（2点）和暗晶界区（点5）小亮的区域在480nm处显示在肩部440纳米带，偶尔在发射波长310 nm。根据文献和XRD分析，我们可以在属性约430nm的JEM 22和480 nm的α-SiAlON的23中心，以铈3+ 3+铈乐队。较暗的宽的发射是起源于铈3+在β型塞隆，并且在310纳米至赛隆主体材料。这些结果表明，该红移和根据钙掺杂的CL峰的加宽可能不能归因以铈3+的晶场分裂钙引起的变化如最初想象的，但更多的不同阶段，在同一颗粒内的共存和β-SiAlON的逐步转变为α型塞隆与钙掺杂。 虽然不同的发射中心的观察和其分布是通过利用低能量的CL可能的，它可能是不够充分了解发光中心的性质。在这样的情况下，有必要到CL测量与其他技术相结合。由于入射电子可以产生CL旁其它信号，也能够通过调查与不同的电子束技术相同的区域直接关联与电的，化学或结构特性的光发射。因此，CL具有高分辨率TEM（HRTEM）和EBIC的相关已用于表征缺陷，例如位错或堆垛层错。至于浓度/组合物的变化，CL的用TEM，EDS或俄歇能谱的组合可导致更好地理解本发光的来源的。 这里，我们通过研究Si掺杂AlN粉末的发光说明这个方面。 图7示出在CS-CL和CS-EDS图像（A，B）和本地光谱（C，D）掺杂有4.0％的Si的AlN颗粒掺杂。在CS-CL图像摄于350纳米，而CS-EDS图像由Si和Al分布的叠加。在CS-CL图像示出了在颗粒的中心暗细长结构。在明亮的地区采取局部发光光谱包括在与肩部350纳米的280，380和460 nm的巅峰强者的。但是，也有在与位置这些不同的带之间的比率清晰的变化。区示出在350nm的明亮的发射（点1）示出了更高的280 nm发射和较小460nm发射相比于m泉带在350纳米，而较暗的细长贴片（点2）示出了一个更小的280纳米发射和更高460nm发射相比，在350处的主带。 460纳米源于Si容纳在氮化铝24的缺陷。 EDS图像和本地光谱表明较暗细长区域显示出更小的Al和更高的Si组合物相比于颗粒的其余部分。与在图5中观察到的结果相比较，我们可以假设，通过增加Si量成的AlN，Si和AlN的，其诱导塞隆相的形成之间发生副反应。 一种材料在设备中使用的两个重要参数是在压力下的材料的高性能和稳定性。事实上，在压力下的材料特性的劣化会降低其使用寿命，这在工业上不可行的。因此，对于电子束刺激的设备，诸如阴极射线管（CRT）或FED，它是正具完整开发电子束辐射抗性磷光体和/或了解电子束诱发的机制，以防止或减少这种影响。发光降解可以通过不同的机制，例如吸附/脱附，或在表面上，创建或缺陷活化等 25-27充电发生。尽管这些强度变化CL结果的定量分析复杂化，它们可以被用来研究光电器件的寿命。 为了说明这一点，我们有发光光谱和两个蓝色发光荧光粉的变阵，掺铈拉5的Si 3 O 12 N和Si / EU掺杂的AlN。 图8a显示了铈掺杂拉5硅化学发光光谱在5千伏3 O 12 N和Si / EU掺杂的AlN 20秒照射后。两种样品显示出强烈的蓝光发射:对于CE掺杂香格里拉&lt;带位置和强度子&gt; 5的Si 3 O 12 N分别为456 nm和3,270厘泊，而对硅/铕共掺杂AlN的是466纳米〜3100厘泊。先验，这些2个样品之间的主要区别是发射的广泛性，由于掺铈的La 5的Si 3 O 12 N的发射是由于几个频带的共存大。因此，似乎两种材料都适合作为用于FED的蓝色发光荧光体，而且我们必须考虑的标准为制造成本，与其它磷光体的相容性或电子束辐射下发光性能的稳定性，以确定最合适的。 图8b示出了在5千伏的掺铈的La 5的Si 3 O 12 N和Si /铕掺杂的AlN发光强度的电子束照射期间的演变。对于CE掺杂拉5的Si 3 O 12 N，强度从5分钟到3,270 CPS 450和95厘泊的60分钟减少。即，下3600秒5千伏的照射，强度降低了初始强度的95％以上。为硅/铕掺杂的AlN，则强度降低，60分钟3100至2500厘泊，即该初始强度的20％的下降。这些结果清楚地表明，在Si /铕掺杂的AlN比掺铈的La 5的Si好得多候选3 O 12 N是由于其较高的稳定性。 <img alt="图1" src="/files/ftp_upload/54249/54249fig1.jpg" /> 图1:掺杂稀土的赛隆荧光体的发光不同的磷光体的照片下可见（a）和紫外（B）光。 （ 三 ）在不同的主晶格的Eu 2+的归一化化学发光光谱。 <a href="http://ecsource.jove.com/files/ftp_upload/54249/54249fig1large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> 页面="1"&gt; <img alt="图2" src="/files/ftp_upload/54249/54249fig2.jpg" /> 图2:CL的安装 （ 一 ）的SEM用化学发光体系的照片，与插入椭圆面反射镜的照片。 （ 二 ）光探测系统原理映像。 <a href="http://ecsource.jove.com/files/ftp_upload/54249/54249fig2large.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/54249/54249fig3.jpg" /> 图3: 赛隆荧光体的制备 （ 一 ）的起始粉末，重量和烧结条件测定。 （b）将所述原料粉末; （c）该粉末混合物的烧结; （ 四 ）前和破碎后烧结粉末。目标="_空白"&gt;点击此处查看该图的放大版本。 <img alt="图4" src="/files/ftp_upload/54249/54249fig4.jpg" /> 图 4: 横截面制备 （a）用在混合物中的树脂和固化剂，并蒸发空气中的粉末的混合。 （ 二 ）倒入一个硅胶模具和暖气。 （c）以方便圈和氩离子截面抛光的筹码抛光。 （ 四 ）测量截面积打磨。 <a href="http://ecsource.jove.com/files/ftp_upload/54249/54249fig4large.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/54249/54249fig5.jpg" /> 图 5: 在Si掺杂的AlN核壳分布 （ 一 ）<html>氮化铝粉末的发光光谱在5kV掺杂有Si的1.6％。 （B - C）在5千伏和作为烧结（b）和掺杂了Si的1.6％，横截面（C）氮化铝粉末，分别为280纳米的拍摄CL图片<a href="http://ecsource.jove.com/files/ftp_upload/54249/54249fig5large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图6" src="/files/ftp_upload/54249/54249fig6.jpg" /> 图6: 钙掺杂JEM荧光体的局部分析的CS-SE，在300纳米（红），430纳米（蓝）和540纳米（绿）和局部发光光谱组合的CS-CL图像在5kV采取JEM荧光粉掺有0（A，b，C）和0.69（D，E，F）的。钙％，分别为。ig6large.jpg"目标="_空白"&gt;点击此处查看该图的放大版本。 <img alt="图7" src="/files/ftp_upload/54249/54249fig7.jpg" /> 图7:掺4.0％Si掺杂的AlN粒子的Si掺杂的AlN CS-CL和CS-EDS图像（A，C）和当地光谱（B，D） 的CL和EDS对比 <a href="http://ecsource.jove.com/files/ftp_upload/54249/54249fig7large.jpg" target="_blank">请点击这里查看更大的版本这个数字。</a> <img alt="图8" src="/files/ftp_upload/54249/54249fig8.jpg" /> 图8:两个蓝色荧光粉的发光稳定性 （ 一 ）铈掺杂的La 5的Si 3 O 12 N和化学发光光谱在5千伏20秒照射后的Si / EU掺杂的AlN。 （ 二 </str翁&gt;）在5千伏电子束辐照过程中铈掺杂的La 5的Si 3 O 12 N和Si / EU掺杂AlN的发光强度的演变。 <a href="http://ecsource.jove.com/files/ftp_upload/54249/54249fig8large.jpg" target="_blank">请点击此处查看该图的放大版本。</a>

Watch this Scientific Journal Video about Low-energy Cathodoluminescence for OxyNitride Phosphors at JoVE.com

Low-energy Cathodoluminescence for OxyNitride Phosphors

的（氧）氮化物荧光粉优良的化学及发光稳定性目前它作为一种很有前途的替代目前使用的硫化和氧化荧光粉。在本文中，我们提出调查使用低能量的阴极（CL）本地发光性能的方式。

低能量的阴极射线（氧）氮化物荧光粉

Nitride and oxynitride (Sialon) phosphors are good candidates for the ultraviolet and visible emission applications. High performance, good stability and ...

low-energy-cathodoluminescence-for-oxy-nitride-phosphors

Research

JoVE Journal

Chemistry

Low-energy Cathodoluminescence for (Oxy)Nitride Phosphors

10.6K 次观看.  University of Tsukuba. 的（氧）氮化物荧光粉优良的化学及发光稳定性目前它作为一种很有前途的替代目前使用的硫化和氧化荧光粉。在本文中，我们提出调查使用低能量的阴极（CL）本地发光性能的方式。 

视频: Low-energy Cathodoluminescence for OxyNitride Phosphors

Fabricating Nanogaps by Nanoskiving

There are several methods of fabricating nanogaps with controlled spacings, but the precise control over the sub-nanometer spacing between two electrodes-and generating them in practical quantities-is still challenging. The preparation of nanogap electrodes using nanoskiving, which is a form of edge lithography, is a fast, simple and powerful technique. This method is an entirely mechanical process which does not include any photo- or electron-beam lithographic steps and does not require any special equipment or infrastructure such as clean rooms. Nanoskiving is used to fabricate electrically addressable nanogaps with control over all three dimensions; the smallest dimension of these structures is defined by the thickness of the sacrificial layer (Al or Ag) or self-assembled monolayers. These wires can be manually positioned by transporting them on drops of water and are directly electrically-addressable; no further lithography is required to connect them to an electrometer.

The fabrication of electrically addressable, high-aspect-ratio (> 1000:1) metal nanowires separated by gaps of single nanometers using either sacrificial layers of aluminum and silver or self-assembled monolayers as templates is described. These nanogap structures are fabricated without a clean room or any photo- or electron-beam lithographic processes by a form of edge lithography known as nanoskiving.

制造由Nanoskiving Nanogaps的

There are several methods of fabricating nanogaps with controlled spacings, but the precise control over the sub-nanometer spacing between two ...

科研

化学

Polymalic Acid-based Nano Biopolymers for Targeting of Multiple Tumor Markers: An Opportunity for Personalized Medicine?

Tumors with similar grade and morphology often respond differently to the same treatment because of variations in molecular profiling. To account for this diversity, personalized medicine is developed for silencing malignancy associated genes. Nano drugs fit these needs by targeting tumor and delivering antisense oligonucleotides for silencing of genes. As drugs for the treatment are often administered repeatedly, absence of toxicity and negligible immune response are desirable. In the example presented here, a nano medicine is synthesized from the biodegradable, non-toxic and non-immunogenic platform polymalic acid by controlled chemical ligation of antisense oligonucleotides and tumor targeting molecules. The synthesis and treatment is exemplified for human Her2-positive breast cancer using an experimental mouse model. The case can be translated towards synthesis and treatment of other tumors.

An example of a nano drug based on polymalic acid is presented towards the rational design of personalized medicine that is applicable to cancer. It describes the synthesis of a nano drug to treat Her2-positive human breast cancer in a nude mouse.

聚苹果酸为基础的生物聚合物纳米靶向的多种肿瘤标志物:用于个性化医疗的机会？

Tumors with similar grade and morphology often respond differently to the same treatment because of variations in molecular profiling. To account for this ...

Gyroid Nickel Nanostructures from Diblock Copolymer Supramolecules

Nanoporous metal foams possess a unique combination of properties - they are catalytically active, thermally and electrically conductive, and furthermore, have high porosity, high surface-to-volume and strength-to-weight ratio. Unfortunately, common approaches for preparation of metallic nanostructures render materials with highly disordered architecture, which might have an adverse effect on their mechanical properties. Block copolymers have the ability to self-assemble into ordered nanostructures and can be applied as templates for the preparation of well-ordered metal nanofoams. Here we describe the application of a block copolymer-based supramolecular complex - polystyrene-block-poly(4-vinylpyridine)(pentadecylphenol) PS-b-P4VP(PDP) - as a precursor for well-ordered nickel nanofoam. The supramolecular complexes exhibit a phase behavior similar to conventional block copolymers and can self-assemble into the bicontinuous gyroid morphology with two PS networks placed in a P4VP(PDP) matrix. PDP can be dissolved in ethanol leading to the formation of a porous structure that can be backfilled with metal. Using electroless plating technique, nickel can be inserted into the template&#39;s channels. Finally, the remaining polymer can be removed via pyrolysis from the polymer/inorganic nanohybrid resulting in nanoporous nickel foam with inverse gyroid morphology.

This article describes the preparation of well-ordered nickel nanofoams via electroless metal deposition onto nanoporous templates obtained from self-assembled diblock copolymer based supramolecules.

Gyroid镍纳米结构的嵌段共聚物超分子

Nanoporous metal foams possess a unique combination of properties - they are catalytically active, thermally and electrically conductive, and furthermore, ...

Au-Interaction of Slp1 Polymers and Monolayer from Lysinibacillus sphaericus JG-B53 - QCM-D, ICP-MS and AFM as Tools for Biomolecule-metal Studies

In this publication the gold sorption behavior of surface layer (S-layer) proteins (Slp1) of Lysinibacillus sphaericus JG-B53 is described. These biomolecules arrange in paracrystalline two-dimensional arrays on surfaces, bind metals, and are thus interesting for several biotechnical applications, such as biosorptive materials for the removal or recovery of different elements from the environment and industrial processes. The deposition of Au(0) nanoparticles on S-layers, either by S-layer directed synthesis 1 or adsorption of nanoparticles, opens new possibilities for diverse sensory applications. Although numerous studies have described the biosorptive properties of S-layers 2-5, a deeper understanding of protein-protein and protein-metal interaction still remains challenging. In the following study, inductively coupled mass spectrometry (ICP-MS) was used for the detection of metal sorption by suspended S-layers. This was correlated to measurements of quartz crystal microbalance with dissipation monitoring (QCM-D), which allows the online detection of proteinaceous monolayer formation and metal deposition, and thus, a more detailed understanding on metal binding.
The ICP-MS results indicated that the binding of Au(III) to the suspended S-layer polymers is pH dependent. The maximum binding of Au(III) was obtained at pH 4.0. The QCM-D investigations enabled the detection of Au(III) sorption as well as the deposition of Au(0)-NPs in real-time during the in situ experiments. Further, this method allowed studying the influence of metal binding on the protein lattice stability of Slp1. Structural properties and protein layer stability could be visualized directly after QCM-D experiment using atomic force microscopy (AFM). In conclusion, the combination of these different methods provides a deeper understanding of metal binding by bacterial S-layer proteins in suspension or as monolayers on either bacterial cells or recrystallized surfaces.

Au-Interaction of Slp1 Polymers and Monolayer from Lysinibacillus sphaericus JG-B53 - QCM-D, ICP-MS and AFM as Tools for Biomolecule-metal Studies

To obtain basic information on the sorption and recycling of gold from aqueous systems the interaction of Au(III) and Au(0) nanoparticles on S-layer proteins were investigated. The sorption of protein polymers was investigated by ICP-MS and that of proteinaceous monolayers by QCM-D. Subsequent AFM enables the imaging of the nanostructures.

SLP1聚合物和单层从金交互<em&gt; Lysinibacillus球形</em&gt; JG-B53 - QCM-D，ICP-MS和原子力显微镜的工具生物分子金属研究

In this publication the gold sorption behavior of surface layer (S-layer) proteins (Slp1) of Lysinibacillus sphaericus JG-B53 is described. These ...

Synthesis of Cd-free InP/ZnS Quantum Dots Suitable for Biomedical Applications

Fluorescent nanocrystals, specifically quantum dots, have been a useful tool for many biomedical applications. For successful use in biological systems, quantum dots should be highly fluorescent and small/monodisperse in size. While commonly used cadmium-based quantum dots possess these qualities, they are potentially toxic due to the possible release of Cd2+ ions through nanoparticle degradation. Indium-based quantum dots, specifically InP/ZnS, have recently been explored as a viable alternative to cadmium-based quantum dots due to their relatively similar fluorescence characteristics and size. The synthesis presented here uses standard hot-injection techniques for effective nanoparticle growth; however, nanoparticle properties such as size, emission wavelength, and emission intensity can drastically change due to small changes in the reaction conditions. Therefore, reaction conditions such temperature, reaction duration, and precursor concentration should be maintained precisely to yield reproducible products. Because quantum dots are not inherently soluble in aqueous solutions, they must also undergo surface modification to impart solubility in water. In this protocol, an amphiphilic polymer is used to interact with both hydrophobic ligands on the quantum dot surface and bulk solvent water molecules. Here, a detailed protocol is provided for the synthesis of highly fluorescent InP/ZnS quantum dots that are suitable for use in biomedical applications.

In this protocol, the synthesis of Cd-free InP/ZnS quantum dots (QDs) is detailed. InP-based QDs are gaining popularity due to the toxicity of Cd2+ ions that may be released through nanoparticle degradation. After synthesis, QDs are solubilized in water using an amphiphilic polymer for use in biomedical applications.

镉免费的InP /硫化锌量子点的合成适合生物医学应用

Fluorescent nanocrystals, specifically quantum dots, have been a useful tool for many biomedical applications. For successful use in biological systems, ...

A Protocol for the Production of Gliadin-cyanoacrylate Nanoparticles for Hydrophilic Coating

This article presents a protocol for the production of protein-based nanoparticles that changes the hydrophobic surface to hydrophilic by a simple spray coating. These nanoparticles are produced by the polymerization reaction of alkyl cyanoacrylate on the surface of cereal protein (gliadin) molecules. Alkyl cyanoacrylate is a monomer that instantly polymerizes at RT when it is applied to the surface of materials. Its polymerization reaction is initiated by the trace amounts of weakly basic or nucleophilic species on the surface, including moisture. Once polymerized, the polymerized alkyl cyanoacrylates show a strong affinity with the object materials because nitrile groups are in the backbone of poly (alkyl cyanoacrylate). Proteins also work as initiator for this polymerization because they contain amine groups that can initiate the polymerization of cyanoacrylate. If aggregated protein is used as an initiator, protein aggregate is surrounded by the hydrophobic poly(alkyl cyanoacrylate) chains after the polymerization reaction of alkyl cyanoacrylate. By controlling the experimental condition, particles in the nanometer range are produced. The produced nanoparticles readily adsorb to the surface of most materials including glass, metals, plastics, wood, leather, and fabrics. When the surface of a material is sprayed with the produced nanoparticle suspension and rinsed with water, the micellar structure of nanoparticle changes its conformation, and the hydrophilic proteins are exposed to the air. As a result, the nanoparticle-coated surface changes to hydrophilic.

This article presents a protocol for the production of protein-based nanoparticles that changes the hydrophobic surface to hydrophilic. The produced nanoparticle is an assembly of gliadin-cyanoacrylate diblock copolymers. Spray coating with the produced nanoparticle changes the surface of target material to a hydrophilic surface.

一种醇溶蛋白氰基丙烯酸酯纳米粒子为亲水涂料生产协议

This article presents a protocol for the production of protein-based nanoparticles that changes the hydrophobic surface to hydrophilic by a simple spray ...

Simple Methods for the Preparation of Non-noble Metal Bulk-electrodes for Electrocatalytic Applications

The rock material pentlandite with the composition Fe4.5Ni4.5S8 was synthesized via high temperature synthesis from the elements. The structure and composition of the material was characterized via powder X-ray diffraction (PXRD), M&#246;ssbauer spectroscopy (MB), scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and energy dispersive X-ray spectroscopy (EDX). Two preparation methods of pentlandite bulk electrodes are presented. In the first approach a piece of synthetic pentlandite rock is directly contacted via a wire ferrule. The second approach utilizes pentlandite pellets, pressed from finely ground powder, which is immobilized in a Teflon casing. Both electrodes, whilst being prepared by an additive-free method, reveal high durability during electrocatalytic conversions in comparison to common drop-coating methods. We herein showcase the striking performance of such electrodes to accomplish the hydrogen evolution reaction (HER) and present a standardized method to evaluate the electrocatalytic performance by electrochemical and gas chromatographic methods. Furthermore, we report stability tests via potentiostatic methods at an overpotential of 0.6 V to explore the material limitations of the electrodes during electrolysis under industrial relevant conditions.

A facile preparation method of electrodes using the bulk material Fe4.5Ni4.5S8 is presented. This method provides an alternative technique to conventional electrode fabrication and describes prerequisites for unconventional electrode materials including a straightforward electrocatalytic testing method.

用于制备用于电催化应用的非贵金属体电极的简单方法

The rock material pentlandite with the composition Fe4.5Ni4.5S8 was synthesized via high temperature synthesis from the elements. The structure and ...

Controlled Photoredox Ring-Opening Polymerization of O-Carboxyanhydrides Mediated by Ni/Zn Complexes

Here, we describe an effective protocol that combines photoredox Ni/Ir catalysis with the use of a Zn-alkoxide for efficient ring-opening polymerization, allowing for the synthesis of isotactic poly(&#945;-hydroxy acids) with expected molecular weights (&#62;140 kDa) and narrow molecular weight distributions (Mw/Mn &#60; 1.1). This ring-opening polymerization is mediated by Ni and Zn complexes in the presence of an alcohol initiator and a photoredox Ir catalyst, irradiated by a blue LED (400 - 500 nm). The polymerization is performed at a low temperature (-15 &#176;C) to avoid undesired side reactions. The complete monomer consumption can be achieved within 4 - 8 hours, providing a polymer close to the expected molecular weight with narrow molecular weight distribution. The resulted number-average molecular weight shows a linear correlation with the degree of polymerization up to 1000. The homodecoupling 1H NMR study confirms that the obtained polymer is isotactic without epimerization. This polymerization reported herein offers a strategy for achieving rapid, controlled O-carboxyanhydrides polymerization to prepare stereoregular poly(&#945;-hydroxy acids) and its copolymers bearing various functional side-chain groups.

Controlled Photoredox Ring-Opening Polymerization of O-Carboxyanhydrides Mediated by Ni/Zn Complexes

A protocol for the controlled photoredox ring-opening polymerization of O-carboxyanhydrides mediated by Ni/Zn complexes is presented.

镍/锌配合物介导的O-Carboxyanhydrides 的控制 Photoredox 环开聚合

Here, we describe an effective protocol that combines photoredox Ni/Ir catalysis with the use of a Zn-alkoxide for efficient ring-opening polymerization, ...

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 ...

Luminescence Lifetime Imaging of O2 with a Frequency-Domain-Based Camera System

We describe a method to image dissolved oxygen (O2), in 2D at high spatial (&#60; 50-100 &#181;m) and temporal (&#60; 10 s) resolution. The method employs O2 sensitive luminescent sensor foils (planar optodes) in combination with a specialized camera system for imaging luminescence lifetime in the frequency-domain. Planar optodes are prepared by dissolving the O2-sensitive indicator dye in a polymer and spreading the mixture on a solid support in a defined thickness via knife coating. After evaporation of the solvent, the planar optode is placed in close contact with the sample of interest - here demonstrated with the roots of the aquatic plant Littorella uniflora. The O2 concentration-dependent change in the luminescence lifetime of the indicator dye within the planar optode is imaged via the backside of the transparent carrier foil and aquarium wall using a special camera. This camera measures the luminescence lifetime (&#181;s) via a shift in phase angle between a modulated excitation signal and emission signal. This method is superior to luminescence intensity imaging methods, as the signal is independent of the dye concentration or intensity of the excitation source, and solely relies on the luminescence decay time, which is an intrinsically referenced parameter. Consequently, an additional reference dye or other means of referencing are not needed. We demonstrate the use of the system for macroscopic O2 imaging of plant rhizospheres, but the camera system can also easily be coupled to a microscope.

Luminescence Lifetime Imaging of O2 with a Frequency-Domain-Based Camera System

We describe the use of a novel, frequency-domain luminescence lifetime camera for mapping 2D O2 distributions with optical sensor foils. The camera system and image analysis procedures are described along with the preparation, calibration and application of sensor foils for visualizing the O2 microenvironment in the rhizosphere of aquatic plants.

使用基于频率域的摄像机系统的 O2的发光寿命成像

We describe a method to image dissolved oxygen (O2), in 2D at high spatial (&#60; 50-100 &#181;m) and temporal (&#60; 10 s) resolution. The method employs ...