这项研究是由香港中文大学通过直接拨款4053077及4441179、研资局具竞争性的专用研究资助、402812及14304314及卓越 AoE/P-02/12。

1. 干涉光刻的设置
注: 干涉光刻用于制造周期阵列12。图 1所示的示意图设置如下:
<ol><li>将 325 nm 激光从 HeCd 多模激光器集中到 13X UV 物镜上, 并通过50微米的基于针孔的空间滤波器进行模式清洗。</li>
	<li>将两个2.5 厘米直径的虹膜30厘米分开, 进一步过滤发散光的中心区域。第二个虹膜后, 光束直径等于2.5 厘米, 并随着距离的增长非常缓慢, 这是 < 3 厘米在1米距离从第二个虹膜。假定光线几乎是准直的。 注意: 在肉眼检查时, 第二虹膜的输出应该是均匀的。</li>
	<li>将准直光束转向劳埃德的镜面干涉仪。劳埃德的设置包含一个棱镜为基础的样本持有人和一个5.04 厘米的镜子定位垂直于它。直接和反射的照明一起创建一个稳定的驻波沿样品表面的模式。棱镜作为一种减反射装置。 注意: 常设波浪的期间 P 可以被写作为: <img alt="Equation 9" src="/files/ftp_upload/56735/56735eq9.jpg"> </img>, λ = 325 毫微米和α是事件角度关于样品法线, 如图 1所示。通过旋转劳埃德的设置, 可以调整事件的角度。</li>
</ol>2. 周期性阵列准备
注: 样品是根据制造商建议的标准程序编制的。所有的程序都是在室温下进行的。
<ol><li>使用1厘米2玻璃基板。在超声波浴中, 用甲醇和丙酮清洁玻璃10分钟, 然后在200摄氏度的热板上预焙1小时以去除污垢。</li>
	<li>自旋涂层的玻璃基板与5毫微米厚粘附层和 100 nm 厚负 SU-8 光刻胶与双速自旋涂布机。<ol>
<li>用伽玛丁内稀释 SU-8 光刻胶, 其比例为 1:5 (v/v), 使厚度可以控制在自旋涂层后接近 100 nm。</li>
		<li>在玻璃基板上分配3-5 滴 (0.2 毫升) 的附着力溶液, 并在十年代和3600转每分钟 600 rpm 旋转, 连续的1分钟。</li>
		<li>重复步骤2.2.2 与 5-7 (0.3 毫升) 滴稀释 SU-8 从步骤2.2.1 以相同的速度。 注: 附着力层提高了玻璃基板和光刻胶之间的附着力, 使光刻胶在显影过程中不会脱落。SU-8 层厚度由自旋涂布机的浓度和速度控制。</li>
	</ol>
</li>
	<li>焙样品在65°c 和95°c 烤盘为1分钟每。这里不推荐使用烤箱。</li>
	<li>将样品转移到干涉仪中的棱镜上。添加一滴折射率匹配油 (n = 1.45), 以附加样品在棱镜上。把它尽可能靠近镜子。 注: 由于油的表面张力, 试样附着在棱镜表面。油的折射率选择与棱镜和玻璃基片相同, 以消除干涉的反反射。</li>
	<li>对于二维正方形晶格, 用相同曝光时间但正交方向公开两次样品;即, 暴露样品, 然后旋转它的90°第二次曝光。当光刻胶暴露在325纳米光, 它 crosslinks, 不能被 SU-8 开发人员溶解。 注: 可通过调整曝光时间来控制阵列的直径 D。</li>
	<li>硬烤样品在65°c 和95°c 2 分钟, 以防止薄膜开裂。</li>
	<li>将整个样品浸入显影液中2分钟, 连续搅拌以溶解未暴露区域。</li>
	<li>将样品浸泡在异丙醇中1分钟, 冲洗残留物, 然后用压缩空气将其烘干。然后生成一个 nanohole 数组。</li>
</ol>3. 金膜沉积和光发射涂层
<ol><li>将样品附着在带双双面胶带的射频磁控溅射沉积系统样品架上, 用于金膜沉积。</li>
	<li>用涡轮分子泵将腔体向下泵入 2x10-6乇基压, 然后再用 6x10-3乇超高纯度氩气填充。</li>
	<li>使用5厘米直径 99.9% Au 目标, 并在样品和目标之间放置一个快门。使用低功耗 (50 W) 降低沉积速率以及表面粗糙度。随着快门关闭, 预先溅射目标10分钟, 以清除污垢。</li>
	<li>打开快门, 在室温下处理沉积物20分钟。薄膜厚度为100毫微米定期存放, 以确保等离子系统是光学上厚, 没有传输。</li>
	<li>一旦样品准备就绪, 旋转涂层的发光材料, 如有机染料或量子点在金属表面形成薄层的电介质。<ol>
<li>对于参考9中使用的苯乙烯8染料, 将聚乙烯醇聚合物 (PVA) 的苯乙烯8和500µg 的20µg 溶解在甲醇的5毫升内。</li>
		<li>在样品上分配3-5 滴 (0.2 毫升) 染料溶液, 并在十年代和 3600 rpm 的 600 rpm 上连续旋转1分钟。厚度估计为 80 nm。 注: 水溶性或不溶性聚合物可作为锚固材料使用, 取决于发射材料的类型。然而, 聚合物应该是非发射的, 这样它就不会干扰光致发光测量。推荐聚乙烯醇聚合物 (PVA) 溶解水溶性染料, 如罗丹明6G 和苯乙烯8。</li>
	</ol>
</li>
</ol>4. 测定细菌衰变率的反射率测量
注意: 偏振和角度分辨反射率光谱学的设置如图 2所示。它包括一个量角器与三个自转阶段为独立地改变样品取向 (阶段 1) 和检测角度 (阶段 2) 并且样品方位角 (阶段 3)。
<ol><li>使用来自石英灯的宽带白光作为光源。首先一对多模光纤束, 然后瞄准它由一对共线面对面物镜 (5X 和 60X)。通过改变样品方向, 在不同入射角度照射样品上的光束。在样品前后放置一对入射偏光片和检测分析仪进行极化依赖性测量。 注: 面对面目标充当透镜系统, collimates 和扩展多模光纤中的白色光源。</li>
	<li>使用多模光纤从样品中收集镜面反射, 连接到光谱仪和用于光谱学的 CCD 探测器。</li>
	<li>仔细对齐设置, 以确保采样方向阶段和检测旋转阶段都是同心的, i. e., 它们的旋转轴是共线的。</li>
	<li>用扁金胶片校准安装。用已知的 Au 介电函数, 测量不同入射角的反射谱, 并与菲涅尔方程计算的理论反射谱进行比较。这两组数据应与不到5% 的错误一致。</li>
	<li>一旦安装就绪, 测量的线性极化, p 或 s, 反射光谱的样品在不同的入射角。入射角的步长为 0.5°, 波长分辨率为 0.66 nm。为了在多个入射角度下采集光谱, 给出了机械运动、快门控制、数据采集、背景减法等自动化控制程序。 注意: 这个步骤是通过计算完成的。该程序可根据要求提供。如有需要, 请向相应的作者发送一封电子邮件给源代码。</li>
	<li>等高线图的反射率与波长和入射角, 以获得等离子系统的色散关系的模式识别和衰减率的确定。 注意: 采样方位角是在布里渊区域中定位位置。例如, 对于方形格子样本, 旋转样品方位, 使其周期之一与入射平面平行, 这就定义了Γ X 方向。通过45°旋转样本来定义Γ M 方向。</li>
	<li>如果在45°上对入射平面设置了入射极化, 并且分析仪位于 45°, 则测量正交或交叉极化反射率映射。</li>
	<li>提取 p 极化和正交反射光谱, 并配合使用9,12,13, 在讨论中所述的许可证的衰变率。</li>
</ol>5. 测定发射功率比的光致发光测量方法
注意: 角度和偏振分辨光致发光设置如图 3所示。
<ol><li>用 514 nm 氩离子或633纳米 HeNe 激光器取代宽带光源。使用一个全宽半最大 (FWHM) 小于 5 nm 的激光线滤波器来清洗激光光谱, 并放置一个半波板来控制激光束的偏振态。量角器和检测单元保持不变。在检测单元前放置一个凹槽过滤器, 以去除激光线, 从而掩埋发光。 注: 激光波长取决于发射材料的类型。更高的光子能量需要激发更短的发射波长的材料。</li>
	<li>测量 Eq 的发射功率比. (2) & (3), 进行两种类型的测量: 检测和事件扫描。事件和检测扫描之间的相互作用有助于<img alt="Equation 10" src="/files/ftp_upload/56735/56735eq10.jpg">确定、 <img alt="Equation 11" src="/files/ftp_upload/56735/56735eq11.jpg"> </img>、 <img alt="Equation 12" src="/files/ftp_upload/56735/56735eq12.jpg">和. <img alt="Equation 13" src="/files/ftp_upload/56735/56735eq13.jpg"> </img></li>
	<li>对于事件扫描, 可连续更改事件角度, 但根据样本的正常情况修正检测角度。 注意: 这个步骤是通过计算完成的。这种配置有选择地激发传入的许可证, 这是入射角度的依赖, 同时监测在所选检测角度下的发射变化。换言之, 当入射角度满足 Eq 中的相位匹配方程时, 发射量增加. (1)。<ol>
<li>轮廓绘制了入射扫描映射的波长和入射角度的光致发光谱。测量不同检测角度的映射, 但发现相对强度相同。因此, 事件扫描探讨了传入许可证对发射的影响或简单的激励增强, 使我们能够测量<img alt="Equation 10" src="/files/ftp_upload/56735/56735eq10.jpg">和. <img alt="Equation 11" src="/files/ftp_upload/56735/56735eq11.jpg"> </img></li>
	</ol>
</li>
	<li>对于检测扫描, 根据样本的正常情况修正入射角度, 但改变检测角度。 注意: 这个步骤是通过计算完成的。<ol>
<li>同样, 轮廓图的光致发光光谱与波长和检测角度产生的检测扫描映射。随着许可证辐射阻尼的产生, 其发射强度与检测角度有关。因此, 在恒定激励下, 当检测角度满足 Eq 时, 发射量增加. (1)。这种配置探讨了发射增强, 并允许我们确定<img alt="Equation 12" src="/files/ftp_upload/56735/56735eq12.jpg">不同α的顺序, 只要它有明确的检测角度依赖性。</li>
	</ol>
</li>
</ol>

<ol>
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作者声明他们没有竞争的财政利益。

在本协议中, 有几个关键步骤。首先, 机械稳定性是样品制备的关键。劳埃德设置产生的驻波对两个光照光束的相位差很敏感。因此, 在曝光时间内的任何振动都会降低 nanohole 的均匀性和边缘锐度。强烈建议在无振动环境下操作,例如, 具有隔振支承的光学工作台。此外, 高功率激光器也希望减少振动, 因为它减少曝光时间相应。其次, 必须正确选择步骤1.1 中的针孔。孔的大小应该足够小, 以执...

表面等离子体介导荧光 (SPMF) 最近得到了相当关注1,2,3,4,5,6。当光发射器靠近等离子系统时, 能量可以在发射器和表面等离子极化激元 (许可证) 之间传输。一般情况下, 强等离子场可以强烈增强2发射器的激发。同时, 由于许可证所制造的大密度的状态, 产生了众所周知的珀尔效应3, 排放率也在增加。这两个过程在生产 SPMF 方面携手并进。由于 SPMF 已经在固态照明1、4、能量采集5和生物检测6中激发了大量应用, 目前正在进行密集的调查。特别是, 从许可证到发射器的能量传输速率的知识, 反之亦然,即激发和耦合率, 是非常重要的。然而, 激励和排放过程通常是纠缠在一起的, 这方面的研究还是缺乏的。例如, 大多数研究只确定了激发效率比, 这简单地比较了排放与和不许可证7。激发率的确切的测量仍然是缺掉的。另一方面, 传统的时间分辨技术 (如荧光寿命光谱学) 通常用于研究发射过程的动力学, 但它们无法将耦合率从总衰变率8中分离出来。在这里, 我们描述如何通过结合速率方程模型和时间耦合模式理论9,10来确定它们。值得注意的是, 我们发现, 激发和耦合速率可以用可测量的数量来表示, 这可以通过执行角度和极化分辨反射率和光致发光光谱来获得。我们将首先概述配方, 然后详细描述仪器。这种方法完全是基于频域的, 它不需要任何时间分辨的附件, 如超快激光器和时间相关的单光子计数器, 这是昂贵的, 有时难以实现8,11. 我们预计这项技术将成为确定光发射器和谐振腔之间的励磁和耦合速率的有利技术。
本文介绍了周期性系统中的 SPMF。对于一个周期性的等离子系统, 在这种情况下, 可以产生类似于许可证的直接激发和发射, 其特征是激发效率η和自发发射速率Γr, 发射器可以通过传入的许可证激发并通过传出许可证衰变。换句话说, 在共振激励下, 会产生传入的许可证, 以创建强大的等离子场, 使发射器充满活力。一旦发射器兴奋, 他们的能量就可以转移到传出的许可证, 随后 radiatively 消散到远场, 从而产生增强的排放量。他们定义了 SPMF。对于简单的两能级发射器, 励磁指的是电子从地面向激发态的过渡, 而发射则定义了电子衰变回基态, 伴随着波长定义的光子发射。由兴奋和地面状态之间的能量区别。SPMF 的激发和发射条件, 满足已知的相位匹配方程, 激发传入和传出许可证9
<img alt="Equation 1" src="/files/ftp_upload/56735/56735eq1.jpg">(1)
其中εa和εm是电介质和金属的介电常数, θ和φ是事件和方位角, P 是数组的周期, λ是激发或发射波长, m 和 n 是整数, 指定的顺序许可证.对于励磁, 激光束在平面内的 wavevector 将是布拉格分散到动量匹配的传入许可证和θ和φ一起定义指定的事件配置, 以刺激的许可证, 以提高电子吸收在励磁波长λ前。同样, 对于发射, 传出的许可证将反向布拉格分散, 以匹配的光线, 现在的角度代表可能的发射通道在发射波长λem。然而, 人们注意到, 由于发射器可以将他们的能量耦合到矢量传播<img alt="Equation 2" src="/files/ftp_upload/56735/56735eq2.jpg">许可证与它有相同<img alt="Equation 3" src="/files/ftp_upload/56735/56735eq3.jpg">的大小, 但不同的方向, 许可证可以通过不同的组合 (m, n) 到远场后的 Eq. (1)。
利用速率方程模型和时间耦合模理论 (许可证), 我们发现, 激发率Γex,即能量传递率从从的到发射器, 可以表示为9,12,13
<img alt="Equation 4" src="/files/ftp_upload/56735/56735eq4.jpg">(2)
在没有传入许可证的情况下, η是上述直接励磁速率, γ是许可证<img alt="Equation 5" src="/files/ftp_upload/56735/56735eq5.jpg">的总衰减率, γabs和γrad是许可证的欧姆吸收和辐射衰减率,<img alt="Equation 6" src="/files/ftp_upload/56735/56735eq6.jpg">是具有和没有传入许可证的光致发光功率比。另一方面, 耦合速率Γc(即从发射器到许可证的能量传递速率) 可以写为:
<img alt="Equation 7" src="/files/ftp_upload/56735/56735eq7.jpg">(3)
γr是<img alt="Equation 8" src="/files/ftp_upload/56735/56735eq8.jpg">直接发射速率, 是αth介导衰变与直接端口之间的光致发光功率比, γradα和γ是α端口的辐射衰减率.和总衰变率。我们将看到, 虽然所有的细菌衰变率都可以用反射率光谱学来衡量, 但发射功率比可以通过光致发光光谱学来确定。有关配方的详细资料, 请参阅9、10。

<table border="0" cellpadding="0" cellspacing="0" style="width:817px;" width="818">
	<tbody>
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			<td height="21" style="height:21px;width:319px;">Control program</td>
			<td style="width:213px;">National Instruments</td>
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		</tr>
	</tbody>
</table>

determination of the excitation and coupling rates between light emitters and surface plasmon polaritons

我们开发了一种独特的方法来测量光发射器和表面等离子极化激元 (许可证) 产生的金属周期阵列, 而不涉及时间分辨技术的励磁和耦合速率。我们已经制定了数量, 可以用简单的光学测量测量。本文将详细介绍基于角度和偏振分辨反射率和光致发光光谱的仪器。我们的方法是有趣的, 因为它的简单性, 这需要常规光学和几个机械阶段, 因此是高负担得起的大多数研究实验室。

在图 4a8的嵌入中给出了一个 Au 周期阵列的例子。平面观扫描电镜图像表明, 该样品为2D 方形圆孔阵列, 周期为 510 nm, 孔深 280 nm, 孔径为 140 nm。沿Γ X 方向进行的 p 偏振反射率映射如图 4a所示。虚线是由相匹配方程计算的 Eq. (1) 表明 (m =-1, n = 0) 许可证是兴奋的。
当?...

Watch this Scientific Journal Video about Determination of the Excitation and Coupling Rates Between Light Emitters and Surface Plasmon Polaritons at JoVE.com

Determination of the Excitation and Coupling Rates Between Light Emitters and Surface Plasmon Polaritons

本协议描述了用于确定由周期性阵列引起的光发射器和类似于极化激元的表面等离子体的激发和耦合速率的仪器。

光发射器与表面等离子体极化激元的激发和耦合速率的测定

We have developed a unique method to measure the excitation and coupling rates between the light emitters and surface plasmon polaritons (SPPs) arising ...

determination-excitation-coupling-rates-between-light-emitters

Research

JoVE Journal

Engineering

6.7K 次观看.  Sun Yat-sen University. 本协议描述了用于确定由周期性阵列引起的光发射器和类似于极化激元的表面等离子体的激发和耦合速率的仪器。

视频: Determination of the Excitation and Coupling Rates Between Light Emitters and Surface Plasmon Polaritons

Characterization of Surface Modifications by White Light Interferometry: Applications in Ion Sputtering, Laser Ablation, and Tribology Experiments

In materials science and engineering it is often necessary to obtain quantitative measurements of surface topography with micrometer lateral resolution. From the measured surface, 3D topographic maps can be subsequently analyzed using a variety of software packages to extract the information that is needed.
In this article we describe how white light interferometry, and optical profilometry (OP) in general, combined with generic surface analysis software, can be used for materials science and engineering tasks. In this article, a number of applications of white light interferometry for investigation of surface modifications in mass spectrometry, and wear phenomena in tribology and lubrication are demonstrated. We characterize the products of the interaction of semiconductors and metals with energetic ions (sputtering), and laser irradiation (ablation), as well as ex situ measurements of wear of tribological test specimens.
Specifically, we will discuss:
<ol class="lroman">
	<li>Aspects of traditional ion sputtering-based mass spectrometry such as sputtering rates/yields measurements on Si and Cu and subsequent time-to-depth conversion.</li>
	<li>Results of quantitative characterization of the interaction of femtosecond laser irradiation with a semiconductor surface. These results are important for applications such as ablation mass spectrometry, where the quantities of evaporated material can be studied and controlled via pulse duration and energy per pulse. Thus, by determining the crater geometry one can define depth and lateral resolution versus experimental setup conditions.</li>
	<li>Measurements of surface roughness parameters in two dimensions, and quantitative measurements of the surface wear that occur as a result of friction and wear tests.</li>
</ol>
Some inherent drawbacks, possible artifacts, and uncertainty assessments of the white light interferometry approach will be discussed and explained.

White light microscope interferometry is an optical, noncontact and quick method for measuring the topography of surfaces. It is shown how the method can be applied toward mechanical wear analysis, where wear scars on tribological test samples are analyzed; and in materials science to determine ion beam sputtering or laser ablation volumes and depths.

白光干涉表面改性中的应用离子溅射，激光烧蚀，与摩擦学实验表征

In materials science and engineering it is often necessary to obtain quantitative measurements of surface topography with micrometer lateral resolution. ...

科研

工程学

Design, Fabrication, and Experimental Characterization of Plasmonic Photoconductive Terahertz Emitters

In this video article we present a detailed demonstration of a highly efficient method for generating terahertz waves. Our technique is based on photoconduction, which has been one of the most commonly used techniques for terahertz generation 1-8. Terahertz generation in a photoconductive emitter is achieved by pumping an ultrafast photoconductor with a pulsed or heterodyned laser illumination. The induced photocurrent, which follows the envelope of the pump laser, is routed to a terahertz radiating antenna connected to the photoconductor contact electrodes to generate terahertz radiation. Although the quantum efficiency of a photoconductive emitter can theoretically reach 100%, the relatively long transport path lengths of photo-generated carriers to the contact electrodes of conventional photoconductors have severely limited their quantum efficiency. Additionally, the carrier screening effect and thermal breakdown strictly limit the maximum output power of conventional photoconductive terahertz sources. To address the quantum efficiency limitations of conventional photoconductive terahertz emitters, we have developed a new photoconductive emitter concept which incorporates a plasmonic contact electrode configuration to offer high quantum-efficiency and ultrafast operation simultaneously. By using nano-scale plasmonic contact electrodes, we significantly reduce the average photo-generated carrier transport path to photoconductor contact electrodes compared to conventional photoconductors 9. Our method also allows increasing photoconductor active area without a considerable increase in the capacitive loading to the antenna, boosting the maximum terahertz radiation power by preventing the carrier screening effect and thermal breakdown at high optical pump powers. By incorporating plasmonic contact electrodes, we demonstrate enhancing the optical-to-terahertz power conversion efficiency of a conventional photoconductive terahertz emitter by a factor of 50 10.

We describe methods for the design, fabrication, and experimental characterization of plasmonic photoconductive emitters, which offer two orders of magnitude higher terahertz power levels compared to conventional photoconductive emitters.

电浆光电导太赫兹发射器的设计，制造和实验表征

In this video article we present a detailed demonstration of a highly efficient method for generating terahertz waves. Our technique is based on ...

Real-Time DC-dynamic Biasing Method for Switching Time Improvement in Severely Underdamped Fringing-field Electrostatic MEMS Actuators

Mechanically underdamped electrostatic fringing-field MEMS actuators are well known for their fast switching operation in response to a unit step input bias voltage. However, the tradeoff for the improved switching performance is a relatively long settling time to reach each gap height in response to various applied voltages. Transient applied bias waveforms are employed to facilitate reduced switching times for electrostatic fringing-field MEMS actuators with high mechanical quality factors. Removing the underlying substrate of the fringing-field actuator creates the low mechanical damping environment necessary to effectively test the concept. The removal of the underlying substrate also a has substantial improvement on the reliability performance of the device in regards to failure due to stiction. Although DC-dynamic biasing is useful in improving settling time, the required slew rates for typical MEMS devices may place aggressive requirements on the charge pumps for fully-integrated on-chip designs. Additionally, there may be challenges integrating the substrate removal step into the back-end-of-line commercial CMOS processing steps. Experimental validation of fabricated actuators demonstrates an improvement of 50x in switching time when compared to conventional step biasing results. Compared to theoretical calculations, the experimental results are in good agreement.

The robust device design of fringing-field electrostatic MEMS actuators results in inherently low squeeze-film damping conditions and long settling times when performing switching operations using conventional step biasing. Real-time switching time improvement with DC-dynamic waveforms reduces the settling time of fringing-field MEMS actuators when transitioning between up-to-down and down-to-up states.

实时直流偏置的动态法切换时间改善严重欠阻尼边缘化场静电MEMS致动器

Mechanically underdamped electrostatic fringing-field MEMS actuators are well known for their fast switching operation in response to a unit step input ...

Quantification of Hydrogen Concentrations in Surface and Interface Layers and Bulk Materials through Depth Profiling with Nuclear Reaction Analysis

Nuclear reaction analysis (NRA) via the resonant 1H(15N,&#945;&#947;)12C reaction is a highly effective method of depth profiling that quantitatively and non-destructively reveals the hydrogen density distribution at surfaces, at interfaces, and in the volume of solid materials with high depth resolution. The technique applies a 15N ion beam of 6.385 MeV provided by an electrostatic accelerator and specifically detects the 1H isotope in depths up to about 2 &#956;m from the target surface. Surface H coverages are measured with a sensitivity in the order of ~1013 cm-2 (~1% of a typical atomic monolayer density) and H volume concentrations with a detection limit of ~1018 cm-3 (~100 at. ppm). The near-surface depth resolution is 2-5 nm for surface-normal 15N ion incidence onto the target and can be enhanced to values below 1 nm for very flat targets by adopting a surface-grazing incidence geometry. The method is versatile and readily applied to any high vacuum compatible homogeneous material with a smooth surface (no pores). Electrically conductive targets usually tolerate the ion beam irradiation with negligible degradation. Hydrogen quantitation and correct depth analysis require knowledge of the elementary composition (besides hydrogen) and mass density of the target material. Especially in combination with ultra-high vacuum methods for in-situ target preparation and characterization, 1H(15N,&#945;&#947;)12C NRA is ideally suited for hydrogen analysis at atomically controlled surfaces and nanostructured interfaces. We exemplarily demonstrate here the application of 15N NRA at the MALT Tandem accelerator facility of the University of Tokyo to (1) quantitatively measure the surface coverage and the bulk concentration of hydrogen in the near-surface region of a H2 exposed Pd(110) single crystal, and (2) to determine the depth location and layer density of hydrogen near the interfaces of thin SiO2 films on Si(100).

We illustrate the application of 1H(15N,&#945;&#947;)12C resonant nuclear reaction analysis (NRA) to quantitatively evaluate the density of hydrogen atoms on the surface, in the volume, and at an interfacial layer of solid materials. The near-surface hydrogen depth profiling of a Pd(110) single crystal and of SiO2/Si(100) stacks is described.

通过与核反应分析深度剖面的表面和界面层和颗粒材料氢含量的定量

Nuclear reaction analysis (NRA) via the resonant 1H(15N,&#945;&#947;)12C reaction is a highly effective method of depth profiling that quantitatively and ...

Emission Spectroscopic Boundary Layer Investigation during Ablative Material Testing in Plasmatron

Ablative Thermal Protection Systems (TPS) allowed the first humans to safely return to Earth from the moon and are still considered as the only solution for future high-speed reentry missions. But despite the advancements made since Apollo, heat flux prediction remains an imperfect science and engineers resort to safety factors to determine the TPS thickness. This goes at the expense of embarked payload, hampering, for example, sample return missions. 
Ground testing in plasma wind-tunnels is currently the only affordable possibility for both material qualification and validation of material response codes. The subsonic 1.2MW Inductively Coupled Plasmatron facility at the von Karman Institute for Fluid Dynamics is able to reproduce a wide range of reentry environments. This protocol describes a procedure for the study of the gas/surface interaction on ablative materials in high enthalpy flows and presents sample results of a non-pyrolyzing, ablating carbon fiber precursor. With this publication, the authors envisage the definition of a standard procedure, facilitating comparison with other laboratories and contributing to ongoing efforts to improve heat shield reliability and reduce design uncertainties.
The described core techniques are non-intrusive methods to track the material recession with a high-speed camera along with the chemistry in the reactive boundary layer, probed by emission spectroscopy. Although optical emission spectroscopy is limited to line-of-sight measurements and is further constrained to electronically excited atoms and molecules, its simplicity and broad applicability still make it the technique of choice for analysis of the reactive boundary layer. Recession of the ablating sample further requires that the distance of the measurement location with respect to the surface is known at all times during the experiment. Calibration of the optical system of the applied three spectrometers allowed quantitative comparison. At the fiber scale, results from a post-test microscopy analysis are presented.

Development of new ablative materials and their numerical modeling requires extensive experimental investigation. This protocol describes procedures for material response characterization in plasma flows with the core techniques being non-intrusive methods to track the material recession along with the chemistry in the reactive boundary layer by emission spectroscopy.

烧蚀材料在试验过程中等离子体发生器发射光谱边界层研究

Ablative Thermal Protection Systems (TPS) allowed the first humans to safely return to Earth from the moon and are still considered as the only solution ...

Measurement of Outgassing Rates of Steels

Steels are commonly used materials in the fabrication of vacuum systems because of their good mechanical, corrosion, and vacuum properties. A variety of steels meet the criterion of low outgassing required for high or ultrahigh vacuum applications. However, a given material can present different outgassing rates depending on its manufacturing process or the various pretreatment processes involved during the fabrication. Thus, the measurement of outgassing rates is highly desirable for a specific vacuum application. For this reason, the rate-of-pressure rise (RoR) method is often used to measure the outgassing of hydrogen after bakeout. In this article, a detailed description of the design and execution of the experimental protocol involved in the RoR method is provided. The RoR method uses a spinning rotor gauge to minimize errors that stem from outgassing or the pumping action of a vacuum gauge. The outgassing rates of two ordinary steels (stainless steel and mild steel) were measured. The measurements were made before and after the heat pretreatment of the steels. The heat pretreatment of steels was performed to reduce the outgassing. Extremely low rates of outgassing (on the order of 10&#8722;11 Pa m3 sec&#8722;1 m&#8722;2) can be routinely measured using relatively small samples.

A protocol for the measurement of outgassing rates of hydrogen from ordinary steel vacuum chambers using the rate-of-pressure rise method is presented.

钢的出气率的测量

Steels are commonly used materials in the fabrication of vacuum systems because of their good mechanical, corrosion, and vacuum properties. A variety of ...

Synchrotron X-ray Microdiffraction and Fluorescence Imaging of Mineral and Rock Samples

In this report, we describe a detailed procedure for acquiring and processing&#160;x-ray microfluorescence (&#956;XRF), and Laue and powder microdiffraction two-dimensional (2D) maps at beamline 12.3.2 of the Advanced Light Source (ALS), Lawrence Berkeley National Laboratory. Measurements can be performed on any sample that is less than 10 cm x 10 cm x 5 cm, with a flat exposed surface. The experimental geometry is calibrated using standard materials (elemental standards for XRF, and crystalline samples such as Si, quartz, or Al2O3 for diffraction). Samples are aligned to the focal point of the x-ray microbeam, and raster scans are performed, where each pixel of a map corresponds to one measurement, e.g., one XRF spectrum or one diffraction pattern. The data are then processed using the in-house developed software XMAS, which outputs text files, where each row corresponds to a pixel position. Representative data from moissanite and an olive snail shell are presented to demonstrate data quality, collection, and analysis strategies.

We describe a beamline setup meant to carry out rapid two-dimensional x-ray fluorescence and x-ray microdiffraction mapping of single crystal or powder samples using either Laue (polychromatic radiation) or powder (monochromatic radiation) diffraction. The resulting maps give information about strain, orientation, phase distribution, and plastic deformation.

矿物和岩石样品的同步辐射 x 射线 Microdiffraction 和荧光成像

In this report, we describe a detailed procedure for acquiring and processing&#160;x-ray microfluorescence (&#956;XRF), and Laue and powder ...

Scattering And Absorption of Light in Planetary Regoliths

Theoretical, numerical, and experimental methods are presented for multiple scattering of light in macroscopic discrete random media of densely-packed microscopic particles. The theoretical and numerical methods constitute a framework of Radiative Transfer with Reciprocal Transactions (R2T2). The R2T2 framework entails Monte Carlo order-of-scattering tracing of interactions in the frequency space, assuming that the fundamental scatterers and absorbers are wavelength-scale volume elements composed of large numbers of randomly distributed particles. The discrete random media are fully packed with the volume elements. For spherical and nonspherical particles, the interactions within the volume elements are computed exactly using the Superposition T-Matrix Method (STMM) and the Volume Integral Equation Method (VIEM), respectively. For both particle types, the interactions between different volume elements are computed exactly using the STMM. As the tracing takes place within the discrete random media, incoherent electromagnetic fields are utilized, that is, the coherent field of the volume elements is removed from the interactions. The experimental methods are based on acoustic levitation of the samples for non-contact, non-destructive scattering measurements. The levitation entails full ultrasonic control of the sample position and orientation, that is, six degrees of freedom. The light source is a laser-driven white-light source with a monochromator and polarizer. The detector is a mini-photomultiplier tube on a rotating wheel, equipped with polarizers. The R2T2 is validated using measurements for a mm-scale spherical sample of densely-packed spherical silica particles. After validation, the methods are applied to interpret astronomical observations for asteroid (4) Vesta and comet 67P/Churyumov-Gerasimenko (Figure 1) recently visited by the NASA Dawn mission and the ESA Rosetta mission, respectively.

Numerical and experimental methods are presented for multiple scattering of light in discrete random media of densely-packed particles. The methods are utilized to interpret the observations of asteroid (4) Vesta and comet 67P/Churyumov-Gerasimenko.

行星光的散射和吸收

Theoretical, numerical, and experimental methods are presented for multiple scattering of light in macroscopic discrete random media of densely-packed ...

Accurate Determination of the Equilibrium Surface Tension Values with Area Perturbation Tests

We demonstrate two robust protocols for determining the equilibrium surface tension (EST) values with area perturbation tests. The EST values should be indirectly determined from the dynamic surface tension (DST) values when surface tension (ST) values are at steady-state and stable against perturbations. The emerging bubble method (EBM) and the spinning bubble method (SBM) were chosen, because, with these methods, it is simple to introduce area perturbations while continuing dynamic tension measurements. Abrupt expansion or compression of an air bubble was used as a source of area perturbation for the EBM. For the SBM, changes in the rotation frequency of the sample solution were used to produce area perturbations. A Triton X-100 aqueous solution of a fixed concentration above its critical micelle concentration (CMC) was used as a model surfactant solution. The determined EST value of the model air/water interface from the EBM was 31.5 &#177; 0.1 mN&#183;m-1 and that from the SBM was 30.8 &#177; 0.2 mN&#183;m-1. The two protocols described in the article provide robust criteria for establishing the EST values.

Two protocols for determining the equilibrium surface tension (EST) values using the emerging bubble method (EBM) and the spinning bubble method (SBM) are presented for a surfactant-containing aqueous phase against air.

通过区域扰动测试精确测定平衡表面张力值

We demonstrate two robust protocols for determining the equilibrium surface tension (EST) values with area perturbation tests. The EST values should be ...

Determination of Aggregate Surface Morphology at the Interfacial Transition Zone (ITZ)

Here, we present a comprehensive method to illustrate the uneven distribution of the interfacial transition zone (ITZ) around the aggregate and the effect of aggregate surface morphology on the formation of ITZ. First, a model concrete sample is prepared with a spherical ceramic particle in roughly the central part of the cement matrix, acting as a coarse aggregate used in common concrete/mortar. After curing until the designed age, the sample is scanned by X-ray computed tomography to determine the relative location of the ceramic particle inside the cement matrix. Three locations of the ITZ are chosen: above the aggregate, on the side of the aggregate, and below the aggregate. After a series of treatments, the samples are scanned with a SEM-BSE detector. The resultant images were further processed using a digital image processing method (DIP) to obtain quantitative characteristics of the ITZ. The surface morphology is characterized at the pixel level based on the digital image. Thereafter, K-means clustering method is used to illustrate the effect of surface roughness on ITZ formation.

Determination of Aggregate Surface Morphology at the Interfacial Transition Zone ITZ

Hereby, we proposed a protocol to illustrate the effect of aggregate surface morphology on the ITZ microstructure. The SEM-BSE image were quantitatively analyzed to obtain ITZ's porosity gradient via digital image processing and a K-means clustering algorithm was further employed to establish a relationship between porosity gradient and surface roughness.

在界面过渡区（ITZ）的聚合曲面形态测定

Here, we present a comprehensive method to illustrate the uneven distribution of the interfacial transition zone (ITZ) around the aggregate and the effect ...