Name: characterization of nanocrystal size distribution using raman spectroscopy with a multi-particle phonon confinement model
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This work was part of the research programme of the Foundation for Fundamental Research on Matter (FOM), which is part of the Netherlands Organisation for Scientific Research (NWO). Authors of this work thank M. J. F. van de Sande for skillful technical assistance, M. A. Verheijen for TEM images, and the group of Tom Gregorkiewicz for PL measurements.

1.规划实验<ol><li>合成或获得的利息13（ 图1a）的纳米晶体。 </li><li>通过确保在基片材料不具有在纳米晶体（图1a）的喇曼光谱重叠峰避免与背景信号的任何混淆。 </li><li>打开拉曼光谱设置的激光。等待足够的时间（约15分钟）的激光强度稳定。 </li><li>测量纳米材料的散装参考待分析12（图1b），以下在步骤2中从散装材料的峰值位置中所述的测量步骤，估计相对移位12。 </li><li>估算所需要的激光功率使用上要被测量的纳米晶体不同的功率拉曼测量。开始具有最低可能的功率的测量，以获得足够的信号（峰强度的对比率背景噪声应至少50），而且如果需要增加激光功率，只要该纳米晶体拉曼峰值保持相同12,13的位置和形状。 </li></ol>利息的纳米2.拉曼光谱<ol><li>加载与纳米晶体的粉末沉积在衬底导入测量室在样品上。 注意:基板尺寸不是关键的（可从毫米到数十厘米），只要它适合于样品支架阶段。的粉末或薄膜的厚度应至少为几十纳米到具有从拉曼光谱仪可检测的信号。对于平面基板保持台，只需放置在光学元件（ 图1b）的衬底。 <ol><li>确保"激光"和"激活"灯都关了，为了从操作激光的不必要的照明是安全的开门之前。如果这些灯不关，执行步骤的操作20.5和2.6。在"联锁"的牌子始终岿然不动。 </li><li>按"盖松开"，并打开测量室的门，并把样品到样品架台（ 图1b）。 </li></ol></li><li>样品的调整的聚焦被测量，以获得最高可能的信号。 <ol><li>选择50X的目标和重点纳米晶粉（ 图1b）的表面上。 </li><li>使用样本保持器的z方向操纵带来下焦点的样品。检查聚焦图像的清晰度从计算机屏幕上的直播相机视图。 </li><li>关闭测量室的门。 </li><li>通过点击从Renishaw的软件的"快门离"钮去掉快门，并让被测定激光光线照到样品。观察到"激光"和"积极"的迹象，现在绿色闪烁，呈红色闪烁，分别。在从S实时图像creen，激光器将是可见的（图1c）。 </li><li>从实时图像，微调使用滚轮机器人，直到最小的激光点，这是最好的重点，是在实时图像上观察到的样品聚焦。 </li></ol></li><li>从Renishaw的分析软件设置测量如下所述（ 图1d）。 <ol><li>从"测量"选择新的光谱采集选项。 </li><li>从弹出窗口，设置测量范围从150至700厘米-的1，设置时间测量为30秒，获得作为2×的总数，和激光功率的0.5％的比例（在测量过程中使用的25毫瓦的激光）。接受的参数插入，窗口将被关闭。 </li><li>通过点击菜单栏上的收购开始按钮开始测量。在测量过程中的"激光"和"活动"指示灯将保持上。 </li></ol></li><li>不要打开测量室时，这些灯是作为激光在操作和正在执行的测量。 </li><li>经过测量完成后，把快门按一下"快门"按钮，从雷尼绍软件。观察到，"激光"和"活动"的关灯。按"盖松开"，然后打开测量室的门。 </li><li>前服用样品流出，降低样品架台与z操纵器，直到有测定样本和放大透镜的表面，以去除样品之间的安全距离。然后，将样品返回到其容器。 </li><li>关闭激光。 </li><li>保存在雷尼绍软件格式，".wxd"中的数据，并在文本文件格式，名为".txt"。后者将用于实验数据的分析。 </li></ol> 3.尺寸Distribut离子测定利息的纳米晶的<ol><li>打开测量为纳米晶体测量的文本文件，和体参考。 </li><li>前绘图数据，但使用三次样条平滑它们，将数据标准化为1处于它们的最高峰的位置，以具有相对峰位移的良好比较。 </li><li>积在硅纳米晶体和硅基准数据，确定参考硅的峰值位置，并估计偏移的量，如果有的话，从521厘米-1的实际峰值位置12然后保存处理的硅纳米晶体的数据作为.TXT文件中。 </li><li>启动拟合程序。 <ol><li>对于装修过程中，请在图2F所示为一个分析程序，如数学拟合函数。 </li><li>导入规格化和校正数据作为输入使用"导入"命令非线性拟合模型。 </li><li>确保间隔对偏斜度为0.1〜1.0，且平均尺寸间隔为2纳米至20纳米之间。 </li><li>如果需要的话，插入下测得的峰的附加的峰使用拟合函数，并重复步骤3.4.2和3.4.3以适合其他子分发（多个）。 </li><li>按"Shift + Enter"来执行拟合程序。 </li><li>在此之后，插入所获得的值的平均大小以及在图2b中所示的预先定义的通用分布函数的偏度。 </li><li>在此之后，插入所获得的值的平均大小，D 0，偏度，σ，在图2b中所示的预先定义的一般分布函数。 </li><li>设置的积分的下边界为1纳米。设置集成的上限任何尺寸不表现出在拉曼光谱的任何变化（20纳米的硅NCS）12到。 </li><li>整合在图2b的分布函数</stron克&gt;作为纳米晶体的大小，使用的积分函数定义一个数据分析，并通过设置的较低和较高的尺寸为整体的边界（1-20纳米的硅NCS）绘图程序的功能。剧情Φ（D）对丁给大小分布。可替换地，发现了一组Φ（D）的值的D（表示的Si-NC的，例如，从1至20纳米，具有1纳米的增量）和情节Φ（D）中对丁，的每个值是尺寸分布。 </li><li>如果多模态粒度分布存在，首先定义要安装用于进行其它尺寸分布的峰值。然后，通过首先找到的测定数据的反卷积后获得（与大小分布确定过程）各峰的面积，然后计算每个峰的面积比相对于估计不同尺寸分布的其体积分数相对于彼此总的拉曼峰值。 </li></ol></li></ol>

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The authors have nothing to disclose.

首先讨论的焦点是协议中的关键步骤。为了不具有与所关注的材料重叠的峰，它使用另一种类型的衬底材料中提到的步骤1.2是很重要的。例如，如果硅的NC感兴趣，不使用硅衬底的拉曼测量。 图 1中，例如，硅的NC上合成有机玻璃基板，其具有完全平面信号大致围绕感兴趣的范围内， 即 480-530厘米- 1。除了测量堆积的参考信号来估计纳米晶体相关的峰值的移位中提到的?...

半导体纳米晶体提请注意为他们的电子和光学特性可以通过简单地改变它们的范围大小相比，他们各自的激子玻尔半径进行调整。1这些独特的大小相关的功能，使这些纳米晶体相关的各种技术应用。例如，载体乘法效果，观察到当一个高能量光子被的CdSe，Si和葛的纳米晶体吸收，可以在频谱变换在太阳能电池应用的概念被使用; 2 - 4或尺寸相关的光发射PBS-NC的和Si-NC的所用的光可以使用发光二极管（LED）的应用程序。5,6-对纳米晶体尺寸分布的精确知识和控制，因此将发挥上的可靠性的决定因素的作用，这些技术的应用程序基于所述性能在纳米晶体。 常用技术的尺寸d纳米晶体的istribution和形态学分析可以被列为X射线衍射（XRD），透射电子显微镜（TEM），光致发光光谱（PL）和拉曼光谱。 X射线衍射是一种结晶技术，揭示了分析材料的形态信息。从衍射峰的扩大，估计该纳米晶体的大小是可能的，但是7，从而获得清晰的数据通常是耗时的。此外，X射线衍射只能使平均纳米晶体尺寸分布的计算。在多模态粒度分布的存在，大小分析用X射线衍射可以是误导性的，导致错误的解释。 TEM是一个功能强大的技术，使纳米晶体成像8虽然TEM能够揭示在多模态粒度分布各自的分布的存在下，制样问题始终努力的测量之前要花费。此外，工作在密密麻麻纳米晶体合奏不同尺寸是由于个别纳米成像的困难挑战。光致发光光谱（PL）是光学分析技术，和光学活性的纳米晶体可以诊断。从尺寸相关发射得到的纳米晶体的尺寸分布。9由于间接带隙的纳米颗粒，大纳米晶体是不受到限制效应，和缺陷富含小的纳米晶体的差的光学性能不能由PL和观察到的大小来检测分布仅限于纳米晶体具有良好的光学性能。虽然这些上述技术都有其自身的优点，他们都没有满足的期望的能力（即，速度快，非破坏性，并可靠）从和理想化大小分析技术。 的纳米晶体的尺寸分布分析的另一种手段是拉曼光谱。拉曼光谱是广泛使用在大多数实验室的，而且它是一个快速和非破坏性技术。此外，在大多数情况下，是不需要的样品制备。拉曼光谱是一种振动分析的材料的技术，它可用于获得不同的形态（晶体或无定形）的信息，和大小相关的信息（从出现在频谱的声子模式的尺寸相关的移） 10拉曼光谱的独特之处在于，虽然尺寸依赖性变化观察到作为移位的频谱，声子峰的形状（扩大，不对称）给出了关于纳米晶体尺寸分布的形状的信息。因此，在原则上是可能的，以提取必要的信息 ，即，平均尺寸和形状因子，从拉曼光谱得到纳米晶体分析的尺寸分布。在多模态粒度分布的情况下的子分布，也可以单独通过deconvolu识别化实验拉曼光谱。 在文献中，这两种理论通常称为建模纳米晶体尺寸分布上的拉曼光谱的形状的效果。债券极化模式（BPM）11描述了从规模内的所有债券的贡献纳米晶体的极化。单粒子声子约束模型（PCM）10使用尺寸相关的物理变量， 即 ，晶体动量，声子频率和分散性，并限制的程度，以限定纳米晶体的拉曼光谱具有特定的大小。由于这些物理变量取决于大小，PCM的可明确地公式化为纳米晶体尺寸的函数的解析表示可以被定义。因此投射在一个通用尺寸分布函数此表达式将能够考虑尺寸分布的PCM内的效果，它可以用来确定nanocr从实验拉曼光谱ystal尺寸分布。12

<table><tbody><tr><td>Raman Spectroscopy</td><td>Renishaw</td><td>In Via</td><td>Equipped with 514 nm Ar ion laser</td></tr><tr><td>Wire 3.0</td><td>Renishaw</td><td></td><td>Raman spectroscopy record tool</td></tr><tr><td>Mathematica</td><td>Wolfram</td><td></td><td>For fitting function and size determination</td></tr><tr><td>Substrate</td><td></td><td></td><td>Plexiglass (to avoid signal coincidence with Si-NCs)</td></tr><tr><td>Si wafer</td><td></td><td></td><td>Reference to Si-NC peak position</td></tr><tr><td>Photoluminescence Spectroscopy</td><td></td><td></td><td>334 nm Ar laser. For optical size distribution.</td></tr><tr><td>Transmission Electron Microscopy</td><td></td><td></td><td>Beam intensity 300 kV. For nanocrystal size and morphology determination.</td></tr></tbody></table>

characterization of nanocrystal size distribution using raman spectroscopy with a multi-particle phonon confinement model

纳米晶体的尺寸分布的分析是它们的大小依赖特性的处理和优化的关键要求。用于大小分析的常用技术是透射电子显微镜（TEM），X射线衍射（XRD）和光致发光光谱（PL）。这些技术，然而，不适合于分析在同一时间以快速，非破坏性的纳米晶体尺寸分布和可靠的方式。我们在这一工作的目的是表明半导体纳米晶体是受尺寸相关声子限制效应的该大小分布，利用拉曼光谱法可以定量估计在非破坏性的，快速和可靠的方式。此外，混合的大小分布可以分别探测，和它们各自的体积比可以使用这种技术来估计。为了分析的粒度分布，我们已形式化的单粒子的PCM和p的解析表达式rojected它到通用分布函数将表示分析纳米晶体的尺寸分布。作为一个模型的实验中，我们已经分析的自由站立的硅纳米晶体（硅NCS）与多模态粒度分布的粒度分布。估计的大小分布是在用TEM和PL结果非常一致，揭示了模型的可靠性。

对于使用拉曼光谱作为一种尺寸的分析工具，模型来提取所需的测量拉曼光谱的大小相关的信息。 图2总结了分析多粒子声子约束模型12全尺寸相关声子约束功能 （图2 c）的投影到一个通用尺寸分布函数（ 图2b），其被选择为对数正态分布函数。给定的幅度（图2 d）中，全宽半值（图2 e）和</str...

Watch this Scientific Journal Video about Characterization of Nanocrystal Size Distribution using Raman Spectroscopy with a Multi-particle Phonon Confinement Model at JoVE.com

Characterization of Nanocrystal Size Distribution using Raman Spectroscopy with a Multi-particle Phonon Confinement Model

我们展示了如何使用拉曼光谱法采用一种解析定义的多声子粒子约束模型，以确定以定量方式的半导体纳米晶体的尺寸分布。得到的结果与像透射电子显微镜和光致发光光谱的其它大小分析技术非常吻合。

使用拉曼光谱与多颗粒的声子坐月子型号纳米大小分布的特征

Analysis of the size distribution of nanocrystals is a critical requirement for the processing and optimization of their size-dependent properties. The ...

characterization-nanocrystal-size-distribution-using-raman

Universidad San Sebastian

Research

JoVE Journal

Engineering

13.4K 次观看.  Eindhoven University of Technology. 我们展示了如何使用拉曼光谱法采用一种解析定义的多声子粒子约束模型，以确定以定量方式的半导体纳米晶体的尺寸分布。得到的结果与像透射电子显微镜和光致发光光谱的其它大小分析技术非常吻合。 

视频: Characterization of Nanocrystal Size Distribution using Raman Spectroscopy with a Multi-particle Phonon Confinement Model

Measurement of Scattering Nonlinearities from a Single Plasmonic Nanoparticle

Plasmonics, which are based on the collective oscillation of electrons due to light excitation, involve strongly enhanced local electric fields and thus have potential applications in nonlinear optics, which requires extraordinary optical intensity. One of the most studied nonlinearities in plasmonics is nonlinear absorption, including saturation and reverse saturation behaviors. Although scattering and absorption in nanoparticles are closely correlated by the Mie theory, there has been no report of nonlinearities in plasmonic scattering until very recently. 
Last year, not only saturation, but also reverse saturation of scattering in an isolated plasmonic particle was demonstrated for the first time. The results showed that saturable scattering exhibits clear wavelength dependence, which seems to be directly linked to the localized surface plasmon resonance (LSPR). Combined with the intensity-dependent measurements, the results suggest the possibility of a common mechanism underlying the nonlinear behaviors of scattering and absorption. These nonlinearities of scattering from a single gold nanosphere (GNS) are widely applicable, including in super-resolution microscopy and optical switches. 
In this paper, it is described in detail how to measure nonlinearity of scattering in a single GNP and how to employ the super-resolution technique to enhance the optical imaging resolution based on saturable scattering. This discovery features the first super-resolution microscopy based on nonlinear scattering, which is a novel non-bleaching contrast method that can achieve a resolution as low as l/8 and will potentially be useful in biomedicine and material studies.

Saturable and reverse saturable scattering were discovered in isolated plasmonic particles and adopted as a novel non-bleaching contrast method in super-resolution microscopy. Here the experimental procedures of detecting and extracting nonlinear scattering are explained in detail, as well as how to enhance resolution with the aid of saturated excitation microscopy.

从单电浆纳米粒子散射非线性测量

Plasmonics, which are based on the collective oscillation of electrons due to light excitation, involve strongly enhanced local electric fields and thus ...

科研

工程学

Resonance Raman Spectroscopy of Extreme Nanowires and Other 1D Systems

This paper briefly describes how nanowires with diameters corresponding to 1 to 5 atoms can be produced by melting a range of inorganic solids in the presence of carbon nanotubes. These nanowires are extreme in the sense that they are the limit of miniaturization of nanowires and their behavior is not always a simple extrapolation of the behavior of larger nanowires as their diameter decreases. The paper then describes the methods required to obtain Raman spectra from extreme nanowires and the fact that due to the van Hove singularities that 1D systems exhibit in their optical density of states, that determining the correct choice of photon excitation energy is critical. It describes the techniques required to determine the photon energy dependence of the resonances observed in Raman spectroscopy of 1D systems and in particular how to obtain measurements of Raman cross-sections with better than 8% noise and measure the variation in the resonance as a function of sample temperature. The paper describes the importance of ensuring that the Raman scattering is linearly proportional to the intensity of the laser excitation intensity. It also describes how to use the polarization dependence of the Raman scattering to separate Raman scattering of the encapsulated 1D systems from those of other extraneous components in any sample.

The paper describes a method for producing extreme nanowires by melt infiltration into carbon nanotubes and how 1D systems may be characterized and investigated using Resonance Raman Spectroscopy to determine vibrational and optical excitation energies.

至尊纳米线和其他维系统的共振拉曼光谱

This paper briefly describes how nanowires with diameters corresponding to 1 to 5 atoms can be produced by melting a range of inorganic solids in the ...

High Resolution Phonon-assisted Quasi-resonance Fluorescence Spectroscopy

High resolution optical spectroscopy methods are demanding in terms of either technology, equipment, complexity, time or a combination of these. Here we demonstrate an optical spectroscopy method that is capable of resolving spectral features beyond that of the spin fine structure and homogeneous linewidth of single quantum dots (QDs) using a standard, easy-to-use spectrometer setup. This method incorporates both laser and photoluminescence spectroscopy, combining the advantage of laser line-width limited resolution with multi-channel photoluminescence detection. Such a scheme allows for considerable improvement of resolution over that of a common single-stage spectrometer. The method uses phonons to assist in the measurement of the photoluminescence of a single quantum dot after resonant excitation of its ground state transition. The phonon&#39;s energy difference allows one to separate and filter out the laser light exciting the quantum dot. An advantageous feature of this method is its straight forward integration into standard spectroscopy setups, which are accessible to most researchers.

The manuscript describes a method of phonon-assisted quasi-resonant fluorescence spectroscopy that incorporates both laser-limited resolution and photoluminescence (PL) spectroscopy. This method utilizes optical phonons to provide linewidth-limited resolution spectra of atom-like semiconductor structures in the energy domain. The method is also easily realized with a single spectrometer optical spectroscopy setup.

高分辨率声子辅助准共振荧光光谱仪

High resolution optical spectroscopy methods are demanding in terms of either technology, equipment, complexity, time or a combination of these. Here we ...

Characterization of Ultra-fine Grained and Nanocrystalline Materials Using Transmission Kikuchi Diffraction

One of the challenges in microstructure analysis nowadays resides in the reliable and accurate characterization of ultra-fine grained (UFG) and nanocrystalline materials. The traditional techniques associated with scanning electron microscopy (SEM), such as electron backscatter diffraction (EBSD), do not possess the required spatial resolution due to the large interaction volume between the electrons from the beam and the atoms of the material. Transmission electron microscopy (TEM) has the required spatial resolution. However, due to a lack of automation in the analysis system, the rate of data acquisition is slow which limits the area of the specimen that can be characterized. This paper presents a new characterization technique, Transmission Kikuchi Diffraction (TKD), which enables the analysis of the microstructure of UFG and nanocrystalline materials using an SEM equipped with a standard EBSD system. The spatial resolution of this technique can reach 2 nm. This technique can be applied to a large range of materials that would be difficult to analyze using traditional EBSD. After presenting the experimental set up and describing the different steps necessary to realize a TKD analysis, examples of its use on metal alloys and minerals are shown to illustrate the resolution of the technique and its flexibility in term of material to be characterized.

This paper provides a detailed method to characterize the microstructure of ultra-fine grained and nanocrystalline materials using a scanning electron microscope equipped with a standard electron backscatter diffraction system. Metal alloys and minerals presenting refined microstructures are analyzed using this technique, showing the diversity of its possible applications.

超细晶和纳米晶材料的表征采用透射菊池衍射

One of the challenges in microstructure analysis nowadays resides in the reliable and accurate characterization of ultra-fine grained (UFG) and ...

Liquid-cell Transmission Electron Microscopy for Tracking Self-assembly of Nanoparticles

Drying a nanoparticle dispersion is a versatile way to create self-assembled structures of nanoparticles, but the mechanism of this process is not fully understood. We have traced the trajectories of individual nanoparticles using liquid-cell transmission electron microscopy (TEM) to investigate the mechanism of the assembly process. Herein, we present the protocols used for liquid-cell TEM studies of the self-assembly mechanism. First, we introduce the detailed synthetic protocols used to produce uniformly sized platinum and lead selenide nanoparticles. Next, we present the microfabrication processes used to produce liquid cells with silicon nitride or silicon windows and then describe the loading and imaging procedures of the liquid-cell TEM technique. Several notes are included to provide helpful tips for the entire process, including how to manage the fragile cell windows. The individual motions of nanoparticles tracked by liquid-cell TEM revealed that changes in the solvent boundaries caused by evaporation affected the self-assembly process of nanoparticles. The solvent boundaries drove nanoparticles to primarily form amorphous aggregates, followed by flattening of the aggregates to produce a 2-dimensional (2D) self-assembled structure. These behaviors are also observed for different nanoparticle types and different liquid-cell compositions.

Here we introduce experimental protocols for the real-time observation of a self-assembly process using liquid-cell transmission electron microscopy.

用于跟踪纳米粒子自组装的液体细胞透射电子显微镜

Drying a nanoparticle dispersion is a versatile way to create self-assembled structures of nanoparticles, but the mechanism of this process is not fully ...

化学

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

We demonstrate the use of two nuclear-based analytical methods that can follow the modifications of microstructural arrangement of iron-based metallic glasses (MGs). Despite their amorphous nature, the identification of hyperfine interactions unveils faint structural modifications. For this purpose, we have employed two techniques that utilize nuclear resonance among nuclear levels of a stable 57Fe isotope, namely M&#246;ssbauer spectrometry and nuclear forward scattering (NFS) of synchrotron radiation. The effects of heat treatment upon (Fe2.85Co1)77Mo8Cu1B14 MG are discussed using the results of ex situ and in situ experiments, respectively. As both methods are sensitive to hyperfine interactions, information on structural arrangement as well as on magnetic microstructure is readily available. M&#246;ssbauer spectrometry performed ex situ describes how the structural arrangement and magnetic microstructure appears at room temperature after the annealing under certain conditions (temperature, time), and thus this technique inspects steady states. On the other hand, NFS data are recorded in situ during dynamically changing temperature and NFS examines transient states. The use of both techniques provides complementary information. In general, they can be applied to any suitable system in which it is important to know its steady state but also transient states.

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

Here, we present a protocol to describe ex situ and in situ investigations of structural transformations in metallic glasses. We employed nuclear-based analytical methods which inspect hyperfine interactions. We demonstrate the applicability of M&#246;ssbauer spectrometry and nuclear forward scattering of synchrotron radiation during temperature-driven experiments.

结构转换的原位和原位研究方法: 金属玻璃结晶的实例

We demonstrate the use of two nuclear-based analytical methods that can follow the modifications of microstructural arrangement of iron-based metallic ...

Construction and Operation of a Light-driven Gold Nanorod Rotary Motor System

The possibility to generate and measure rotation and torque at the nanoscale is of fundamental interest to the study and application of biological and artificial nanomotors and may provide new routes towards single cell analysis, studies of non-equilibrium thermodynamics, and mechanical actuation of nanoscale systems. A facile way to drive rotation is to use focused circularly polarized laser light in optical tweezers. Using this approach, metallic nanoparticles can be operated as highly efficient scattering-driven rotary motors spinning at unprecedented rotation frequencies in water.
In this protocol, we outline the construction and operation of circularly-polarized optical tweezers for nanoparticle rotation and describe the instrumentation needed for recording the Brownian dynamics and Rayleigh scattering of the trapped particle. The rotational motion and the scattering spectra provides independent information on the properties of the nanoparticle and its immediate environment. The experimental platform has proven useful as a nanoscopic gauge of viscosity and local temperature, for tracking morphological changes of nanorods and molecular coatings, and as a transducer and probe of photothermal and thermodynamic processes.

Plasmonic gold nanorods can be trapped in liquids and rotated at kHz frequencies using circularly-polarized optical tweezers. Introducing tools for Brownian dynamics analysis and light scatteringspectroscopy leads to a powerful system for research and application in numerous fields of science.

轻型金纳米旋转电机系统的施工与运行

The possibility to generate and measure rotation and torque at the nanoscale is of fundamental interest to the study and application of biological and ...

Assembly and Characterization of Polyelectrolyte Complex Micelles

Polyelectrolyte complex micelles (PCMs), core-shell nanoparticles formed by self-assembly of charged polymers in aqueous solution, provide a powerful platform for exploring the physics of polyelectrolyte interactions and also offer a promising solution to the pressing problem of delivering therapeutic oligonucleotides in vivo. Developing predictive structure-property relationships for PCMs has proven difficult, in part due to the presence of strong kinetic traps during nanoparticle self-assembly. This article discusses criteria for choosing polymers for PCM construction and provides protocols based on salt annealing that enable assembly of repeatable, low-polydispersity nanoparticles. We also discuss PCM characterization using light scattering, small-angle X-ray scattering, and electron microscopy.

We provide protocols and representative data for designing, assembling, and characterizing polyelectrolyte complex micelles, core-shell nanoparticles formed by polyelectrolytes and hydrophilic charged-uncharged block copolymers.

聚电解质复合微晶体的组装与特性

Polyelectrolyte complex micelles (PCMs), core-shell nanoparticles formed by self-assembly of charged polymers in aqueous solution, provide a powerful ...

Studying Soft-matter and Biological Systems over a Wide Length-scale from Nanometer and Micrometer Sizes at the Small-angle Neutron Diffractometer KWS-2

The KWS-2 SANS diffractometer is dedicated to the investigation of soft matter and biophysical systems covering a wide length scale, from nm to &#181;m. The instrument is optimized for the exploration of the wide momentum transfer Q range between 1x10-4 and 0.5 &#197;-1 by combining classical pinhole, focusing (with lenses), and time-of-flight (with chopper) methods, while simultaneously providing high-neutron intensities with an adjustable resolution. Because of its ability to adjust the intensity and the resolution within wide limits during the experiment, combined with the possibility to equip specific sample environments and ancillary devices, the KWS-2 shows a high versatility in addressing the broad range of structural and morphological studies in the field. Equilibrium structures can be studied in static measurements, while dynamic and kinetic processes can be investigated over time scales between minutes to tens of milliseconds with time-resolved approaches. Typical systems that are investigated with the KWS-2 cover the range from complex, hierarchical systems that exhibit multiple structural levels (e.g., gels, networks, or macro-aggregates) to small and poorly-scattering systems (e.g., single polymers or proteins in solution). The recent upgrade of the detection system, which enables the detection of count rates in the MHz range, opens new opportunities to study even very small biological morphologies in buffer solution with weak scattering signals close to the buffer scattering level at high Q.
In this paper, we provide a protocol to investigate samples with characteristic size levels spanning a wide length scale and exhibiting ordering in the mesoscale structure using KWS-2. We present in detail how to use the multiple working modes that are offered by the instrument and the level of performance that is achieved.

Here, we present a protocol to investigate soft matter and biophysical systems over a wide mesoscopic length scale, from nm to &#181;m that involves the use of the KWS-2 SANS diffractometer at high intensities and an adjustable resolution.

在小角度中子衍射仪KWS-2研究软物质和生物系统在广泛的长度尺度从纳米，微米尺寸

The KWS-2 SANS diffractometer is dedicated to the investigation of soft matter and biophysical systems covering a wide length scale, from nm to &#181;m. ...

生物工程

通过纳米级红外光谱探索多相聚合物系统

Advances in Nanoscale Infrared Spectroscopy to Explore Multiphase Polymeric Systems

Multiphase polymeric systems encompass local domains with dimensions that can vary from a few tens of nanometers to several micrometers. Their composition is commonly assessed using infrared spectroscopy, which provides an average fingerprint of the various materials contained in the volume probed. However, this approach does not offer any details on the arrangement of the phases in the material. Interfacial regions between two polymeric phases, often in the nanoscale range, are also challenging to access. Photothermal nanoscale infrared spectroscopy monitors the local response of materials excited by infrared light with the sensitive probe of an atomic force microscope (AFM). While the technique is suitable for interrogating small features, such as individual proteins on pristine gold surfaces, the characterization of three-dimensional multicomponent materials is more elusive. This is due to a relatively large volume of material undergoing photothermal expansion, defined by the laser focalization onto the sample and by the thermal properties of the polymeric constituents, compared to the nanoscale region probed by the AFM tip. Using a polystyrene (PS) bead and a polyvinyl alcohol (PVA) film, we evaluate the spatial footprint of photothermal nanoscale infrared spectroscopy for surface analysis as a function of the position of PS in the PVA film. The effect of the feature position on the nanoscale infrared images is investigated, and spectra are acquired. Some perspectives on the future advances in the field of photothermal nanoscale infrared spectroscopy are provided, considering the characterization of complex systems with embedded polymeric structures.

作者聚焦:探索多相聚合物系统的纳米级红外光谱进展  

This protocol describes the application of atomic force microscopy and nanoscale infrared spectroscopy to evaluate the performance of photothermal nanoscale infrared spectroscopy in the characterization of three-dimensional multi-polymeric samples.

纳米级红外光谱探索多相聚合物体系的进展

Multiphase polymeric systems encompass local domains with dimensions that can vary from a few tens of nanometers to several micrometers. Their composition ...