Name: the evolution of silica nanoparticle-polyester coatings on surfaces exposed to sunlight
Uploaded: 2016-10-11T14:00:00.000+00:00
Duration: 10 min 27 s
Description: Watch this Scientific Journal Video about The Evolution of Silica Nanoparticle-polyester Coatings on Surfaces Exposed to Sunlight at JoVE.com

Funding from the Australian Research Council Industrial Transformation Research Hubs Scheme (Project Number IH130100017) is gratefully acknowledged. Authors gratefully acknowledge the RMIT Microscopy and Microanalysis Facility (RMMF) for providing access to the characterisation instruments. This research was also undertaken on the Infrared Microscopectroscopy beamline at the Australian Synchrotron, Victoria, Australia.

<html> 1.钢铁样品<ol><li>从商业供应商获得厚度为1毫米的钢试样。 注:样品涂覆有聚酯或聚酯涂覆有二氧化硅纳米粒子。 </li><li>样品暴露在罗克汉普顿，澳大利亚昆士兰州的阳光:收集了总共5年的时间后，一年期和五年期的时间间隔采样。切样片到用打孔器直径1厘米的圆形光盘。 </li><li>前表面表征，用双蒸水漂洗样品，然后干燥用氮气（99.99％）。保持在所有样品中的气密容器以防止任何空气污染物吸附到表面上（ 图1）。 </li></ol><img alt="图1" src="/files/ftp_upload/54309/54309fig1.jpg" /> 图1的金属圆盘制备聚酯系涂料。将样品储存在容器中，直到需要。OM /文件/ ftp_upload / 54309 / 54309fig1large.jpg"目标="_空白"&gt;点击此处查看该图的放大版本。 2.表面的化学和理化性质<ol><li>利用X射线光电子能谱法分析表面化学。 <ol><li>执行使用在150瓦操作的单色X射线源（铝Kα，hν= 1486.6电子伏特）的X射线光电子光谱法（XPS） 注意:利用X射线束的光点大小为400微米的直径。 </li><li>在样品板负载的样品。放置样品板到的XPS真空室，然后泵室中。等待室中的真空达到约1×10 -9毫巴。 </li><li>在光电子能谱软件，按"洪水枪"的选项涌入样品低能电子抵消表面充电。 </li><li>按"插入"&gt;"点"&gt;"点"插入一个分析POIN吨。 注意:这将是在其中进行分析的位置。启用自动高度函数来获得收购的最佳高度。 </li><li>按"插入"&gt;"频谱"&gt;"多光谱"来扫描添加到这一点。 注意:这将打开一个周期表的窗口;通过点击它以突出显示它选择一个元素。 </li><li>设立试验后，按"播放"命令进行扫描。 </li><li>按"曲线拟合"命令，然后按"添加峰"和"适合所有级别"命令来解决高分辨率光谱，化学性质不同的物种。 注:此步骤将收购雪莉算法消除背景和高斯-洛伦兹拟合解卷积光谱19。 </li><li>选择所有高清晰度和调查谱。按"Shift键充电"选项，使用hydroca纠正谱的C 1s峰（结合能285.0 eV）的作为参考的rbon组件。 </li><li>后电荷修正，按"导出"选项生成的峰面积的基础上，元件的相对原子浓度的数据表。 </li></ol></li><li>表面化学 注:红外光谱（IR）光束线在澳大利亚同步加速器如下使用衰减全反射红外显微光谱（ATR-IR）分析表面化学: <ol><li>关于显微镜的阶段负荷样品。打开"开始视频辅助测量"或"开始测量没有3D"选项。打开"可见"模式。使用目标集中在样品表面。按"快照/概览"采取所需的图像。 注:0.5毫米厚的CaF 2板可以用作背景。 </li><li>在ATR目标更改为样本。小心地移动舞台放置一个45°的多反射GERmanium水晶（4折射率）1-2毫米以上的表面。实况视频窗口上单击鼠标右键。按"开始测量"&gt;"更改测量参数。"选择选项"不要使用现有的BG所有职位"。 注意:这将选择不采取背景光谱对每个测量点。 </li><li>绘制视频屏幕上的地图来选择感兴趣的区域。按下一个红色的方形孔，然后选择"光圈"&gt;"更改光圈"。更改实际的"刀锋光圈"设置X = 20微米和Y = 20微米。 </li><li>在新尺寸的方形孔径右键点击并进入"光圈"&gt;"设置所有光圈选定的孔径。"按"测量"图标启动扫描。保存数据。 注:戈晶体的折射率为4，所以为20μm×20μm的孔将定义为5μm×5μm的光点尺寸。氏S步进将允许通过20微米，其对应于5微米5微米的光斑通过横跨4,000-850厘米，最大波数范围的晶体用20的孔径设定FTIR制图- 1。 </li><li>使用光谱软件打开主文件。选择对红外光谱目标峰。感兴趣的峰值单击鼠标右键。选择"集成"&gt;"集成"。它将允许创建二维伪彩色图</li></ol></li><li>表面润湿性测量 注意:使用装备有纳米分配器19的接触角测角器进行润湿的测量。 <ol><li>在舞台上放置样品。使针的底部会出现大约四分之一的方式在实时视频窗口屏幕朝下调整微量组件的位置。 </li><li>利用Z轴直到样品和表面之间的距离提高样品是约5毫米。移动至注射器，直到DOUB的液滴乐蒸馏水接触的表面上。移动注射器到原来的位置。 </li><li>按"运行"命令，记录水滴在表面上影响了使用它与硬件集成在一个黑白CCD摄像机20秒的时间。 </li><li>按下"停止"命令来获得一系列图像。 </li><li>按"接触角"命令来测量获得的图像接触角。重复该接触角测量在每个样品三个随机的位置。 </li></ol></li></ol> 3.表面形貌的可视化<ol><li>光学仿形测量。 注:该仪器是白光垂直扫描干涉模式下工作。 <ol><li>在显微镜的阶段处的样品。 注:确保有物镜和舞台之间有足够的间隙（ 例如 ，"15毫米）。 </li><li>专注于表面使用5×目标通过控制Z轴直到条纹出现在屏幕上。按"自动"命令优化力度。按"测量"命令开始扫描。保存主文件。 </li><li>重复步骤3.1.2为20×和50×的目标。 </li><li>此前统计分析粗糙，按下"删除倾斜"选项去除表面波纹度。按"轮廓"选项来分析粗糙度参数。点击"3DI"选项生成使用兼容的软件20倍光学分析文件的三维图像。 </li></ol></li><li>原子力显微镜<ol><li>上钢盘将样品。将钢盘到磁持有人。 </li><li>在轻敲模式21进行AFM扫描。机械负载磷掺杂的硅探针为0.9牛顿/米，具有8毫微米半径约20千赫表面成像的共振频率前端曲率的弹簧常数。 </li> &lt;LI&gt;手动调整悬臂的激光反射。选择"自动调整"命令，然后按"调"命令来调整AFM悬臂达到制造商报告的最佳共振频率。 </li><li>重点在表面上。移动靠近样品表面的提示。点击命令搞搞表面上的针尖。 </li><li>输入"1赫兹"到扫描速度框。选择扫描区域。按"运行"命令来执行扫描。至少重复扫描的每个的每个条件的五个样品的十个方面。 </li><li>选择找平选项处理所得的地形数据。保存主文件。 </li><li>打开兼容的AFM软件。加载AFM主文件。按"平"命令删除面的倾斜。按"平滑化"命令删除背景。 </li><li>按"统计参数分析"生成的统计粗糙度21。 </li></ol></l我&gt; </ol> 4.统计分析<ol><li>表达在平均值和其标准偏差方面的结果。使用配对Student的双尾T-测试，以评估结果的一致性进行统计的数据处理。集合P -值在&lt;0.05指示统计显着性水平。 </li></ol>

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The authors have nothing to disclose.

聚酯涂料已被广泛地用于保护钢基质从上未涂布表面将发生因水分和污染物的积累的腐蚀。的聚酯涂料的应用可以保护钢免受腐蚀;然而这些涂料的长期效力，如果它们暴露于高水平的潮湿条件下的紫外光，损害作为在热带气候发生。二氧化硅纳米粒子可被施加到聚酯的表面以改善这些环境内的这些涂层的坚固性，对这些含二氧化硅的涂层材料的环境因素然而效果，到现在为止，未知的，特别是关于在其微的变化 - 和纳米表面形貌。 在许多情况下，底层表面的润湿性可提供一个指示，以任何表面降解是否已经发生。接触角测量，但是，不提供关于可能已发生的表面（ 图2）上的物理和化学结构变化的任何细节。 XPS和ATR-FTIR是技术，允许在碳含量和羰基（C = O）的功能分布的变化来确定。 在这项研究中获得的结果表明，阳光照射引起的聚酯涂料的降解。这种退化拟议机制如图9 22,23中给出。酯基可通过暴露于紫外光从根本上降低以形成自由基-COO·，-H 2 C·，-O·， - CO·。在降解过程，CO和CO 2的产生。 <img alt="图9" src="/files/ftp_upload/54309/54309fig9.jpg" /> 图9.拟聚酯的紫外光催化降解。在暴露在阳光下时，酯基团存在于聚酯形成自由基形成稳定的醇，醛，具有消除一氧化碳和二氧化碳的羧酸基团。 <a href="http://ecsource.jove.com/files/ftp_upload/54309/54309fig9large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> 除了涂层的化学降解，观察到在涂料的表面形貌的改变，但仅在纳米级。在以前的研究中，也报道紫外线照射有显著改性聚合物表面24-26的表面形貌的纳米级。这里，人们发现，在表面拓扑结构已通过球状纳米结构（ 图6和7）的形成改变。 XPS可以提供​​洞察的百万分之一的水平在表面化学变化。由于该技术的高灵敏度，样品污染可以容易地检测到的，这可能会导致偏置的结果。在制备样品的XPS分析的最重要的步骤是，以确保样品不放出气体或含有可能损坏仪器的真空系统中的任何颗粒。为了防止这种情况的发生，样品应用氮气进行清洗和任何测量之前脱气。这种技术只提供了一个表面的整体化学超过几百微米的，并且仅揭示了表面化学至〜10nm的深度。所得高分辨率光谱允许确定存在于表面上的不同的化学物质。 XPS是对可能发生的表面的化学修饰的调查的重要工具。一种替代技术来XPS是能量分散X射线光谱（EDX）27。 ATR-IR显微镜要求的良好接触的ATR晶体和表面之间存在是因为小分机的被分析发生超出晶体的渐逝波的ension。 ATR-IR显微镜空间解析表面的分子和结构的组合物。在ATR晶体的污染也可能导致要获得的低信号或偏置的结果。之前的任何实验，清洁用纯异丙醇结晶，以确保任何交叉污染不会发生是重要的。另外，ATR晶体的折射率必须大于该样品的显著高。使用ATR法的红外（IR）光谱是能够被应用到可以使用的发送方法进行分析的化学或生物系统。 ATR-IR已被广泛用于监测真核细胞的发展。拉曼显微光谱是通过该表面的化学不均匀性可以被确定28的替代方法。 水接触角测角是一种技术，根据该杨氏方程，确定的固体S的疏水性urface。当使用这种技术，样品应适当地存储，使得能够避免任何污染物的吸附。该技术的一个限制是，它被限制为平坦的表面。如果不是这种情况下，在液/固/气界面的曲率将被扭曲和不确定的。这种技术被广泛用于指示可能在表面上发生的任何化学变化，并确定疏水和亲水官能团的存在。所述的Wilhelmy板方法是一种替代（但不太容易地进行）技术用于估计表面可湿性29的程度。 光学表面分析提供了一种非破坏性和非接触式测量。该技术的最关键的一步需要用户开始以限定焦平面和防止物镜和样品表面之间的接触，以最低倍率的测量。光学分析只允许的可视化在微观尺度表面形貌。原子力显微镜具有检查的表面的从纳米到分子级的地形的能力。原子力显微镜的操作需要特定的技能相比，光学谱进行分析更长的时间。目前的研究提供了一个极好的例子，A​​FM能够检测表面形貌的也不明显使用光学分析变化。替代技术光学分析和AFM是触笔分析和扫描电子显微镜，其也可以提供表面结构27,30的量化。 一组这些表面表征技术可用于研究的聚合物和金属表面化学和地形特征。光学分析和原子力显微镜可以用于检查表面微米和纳米尺度的地形变化。表面化学特性的技术，包括红外显微镜和X射线坡toelectron光谱可用于横向检查表面化学均匀性。

Environmental corrosion of metals in the environment is both prevalent and costly1-3. A recent study conducted by the Australasian Corrosion Association (ACA) reported that corrosion of metals resulted in a yearly cost of $982 million, which was directly associated with the degradation of assets and infrastructure through metallic corrosion within the water industry4. From an international perspective, the World Corrosion Organization estimated that metallic corrosion was responsible for a direct cost of $3.3 trillion, over 3% of the world's GDP5. The process of galvanizing as a corrosion preventative method has been widely used to increase the lifespan of steel material6. In humid and subtropical climates, however, water tends to condense into small pockets or grooves within the surface of the galvanized steel, leading to the acceleration of corrosion rates through pit corrosion7,8. Thermosetting polymer coatings based on polyesters have been developed to coat the galvanized steel substrata increasing their ability to withstand humid weathering conditions for items such as satellite dishes, garden furniture, air-conditioning units or agricultural construction equipment9-11. Unfortunately polymer coatings on steel surfaces have been found to be considerably adversely affected by the presence of high levels of ultraviolet (uv) radiation12-14. Coatings comprised of silica nanoparticles (SiO2) spread over a polymer layer have been widely used with a view to increasing their corrosion-, wear-, tear- and degradation-resistance15,16. The tendency of the protective polymeric coatings to form pores and cracks can be reduced by incorporating nanoparticles (NPs), which contribute to the passive obstruction of corrosion initiation17,18. Also, the mechanical stability of the protective polymeric layer can be improved by NPs inclusion. However, these coatings act as passive physical barriers and, in comparison to the galvanization approach, cannot inhibit corrosion propagation actively.
An in-depth understanding of the effect that high-levels of ultraviolet light exposure under humid conditions upon these metal coatings is yet to be obtained. In this paper, a wide range of surface analytical techniques, including X-ray photoelectron spectroscopy (XPS), attenuated total reflection infrared micro-spectroscopy (ATR IR), contact angle goniometry, optical profiling and atomic force microscopy (AFM) will be employed to examine the changes in the surface of steel coatings prepared from polyester- and silica nanoparticle-coated polyester (silica nanoparticles/polyester) after exposure to sunlight. Furthermore, the aim of this work is to give a concise, practical overview of the overall characterization techniques to examine weathered samples.

<table><tbody><tr><td>polyester-coated steel&lt;br/&gt; silica nanoparticle-polyester coated steel substrata</td><td>BlueScope Steel</td><td></td><td>Samples provided by company</td></tr><tr><td>Millipore PetriSlide&lt;sup&gt;TM&lt;/sup&gt;&amp;nbsp;</td><td>Fisher Scientific</td><td>PDMA04700</td><td>Storing samples</td></tr><tr><td>Thermo Scientific&lt;sup&gt;TM&lt;/sup&gt; K-alpha&lt;br/&gt; X-ray Photoelectron Spectrometer</td><td>Thermo Fisher Scientific, Inc.</td><td>IQLAADGAAFFACVMAHV</td><td>Acquire XPS spectra</td></tr><tr><td>Avantage Data System</td><td>Thermo Fisher Scientific, Inc.</td><td>IQLAADGACKFAKRMAVI</td><td>Analyse XPS spectra</td></tr><tr><td>A Bruker Hyperion 2000 microscope&amp;nbsp;</td><td>Bruker Corporation</td><td></td><td>Synchrotron integrated instrument</td></tr><tr><td>Bruker Opus v. 7.2</td><td>Bruker Corporation</td><td></td><td>ATR-IR analysis software</td></tr><tr><td>Contact angle goniometer, FTA1000c</td><td>First Ten &amp;Aring;ngstroms Inc., VA, USA</td><td></td><td>Measuring the wettability of surfaces</td></tr><tr><td>FTA v. 2.0</td><td>First Ten &amp;Aring;ngstroms Inc., VA, USA</td><td></td><td>Anaylyzing water contact angle</td></tr><tr><td>Optical profiler, Wyko NT1100&amp;nbsp;</td><td>Bruker Corporation</td><td></td><td>Measure surface topography</td></tr><tr><td>Innova atomic force microscope&amp;nbsp;</td><td>Bruker Corporation</td><td></td><td>Measure surface topography</td></tr><tr><td>Phosphorus doped silicon probes, MPP-31120-10</td><td>Bruker Corporation</td><td></td><td>AFM probes</td></tr><tr><td>Gwyddion software</td><td>http://gwyddion.net/</td><td></td><td>Software used to measure optical profiling and AFM data</td></tr></tbody></table>

the evolution of silica nanoparticle-polyester coatings on surfaces exposed to sunlight

金属表面的腐蚀是在环境中普遍存在，并在许多领域，包括军事，交通，航空，建筑，食品等行业，除其他外的极大关注。聚酯和含有聚酯和二氧化硅纳米粒子的涂层（SiO 2的纳米颗粒）已经被广泛地用于保护钢基质免受腐蚀。在这项研究中，我们利用X射线光电子能谱，衰减全反射红外微光谱，水接触角的测量，光分析和原子力显微镜，以提供深入了解暴露于阳光下如何导致在微米和纳米级的完整性的改变的涂层。使用光学轮廓检测在表面微地形无显著变化，然而，使用原子力显微镜进行检测统计学显著纳米变化到表面。 X射线光电子能谱分析和衰减全反射红外微光谱数据表明，已通过暴露于紫外线光发生酯基的降解以形成COO·，-H 2 C·，-O·， - CO·自由基。在降解过程，CO和CO 2的也被生产。

<html>已被经受暴露于阳光下一个或五年涂覆的钢样品收集，与水的接触角测量进行了决定曝光是否已导致在所述表面的表面疏水性的改变（ 图2 ）。 <img alt="图2" src="/files/ftp_upload/54309/54309fig2.jpg" /> 图2.润湿与聚酯或二氧化硅纳米微粒/聚酯涂料（硅胶/聚酯）在五年内暴露于阳光的表面的变化 （A）的测角的图像示出用于测量表面的平衡接触角水滴。 （B）的水接触角作为曝光时间的函数（*表示P &lt;0.05，相比其相应的控制（年0））。数据代表平均值±标准偏差。ource.jove.com/files/ftp_upload/54309/54309fig2large.jpg"目标="_空白"&gt;点击此处查看该图的放大版本。 它被发现的聚酯涂覆基质的润湿性没有改变的暴露在阳光下的结果，但是在二氧化硅纳米微粒/聚酯涂覆的样品，暴露一年后，被发现是1.3疏水性比更大倍未曝光的样品。采用XPS和ATR-FTIR进行这些样品的进一步分析。 XPS的一个优点是，这种技术允许在表面下约10nm深度要确定一个表面的元素组成。人们发现，Si的含量在该深度已经从约2％，在5年的曝光周期提高到15％。这种增加可以归因于空气中的污染物的吸附。的XPS谱表示在聚酯涂覆基质一个检测铁（Fe）压脚提升1至5年的接触（ 图3），并且有已经在5年的曝光时间后的聚酯包覆的样品中的碳含量略有下降。无显著变化是在硅（Si）中发现，在二氧化硅纳米微粒/聚酯涂覆基质的铁（Fe）和碳（C）的水平。 XPS不，但是，允许要确定的聚合物涂层的特定功能。其结果，同步来源的ATR-IR被用来确定在10微米为已被暴露在阳光下的试样的深度在化学官能的变化，特别是已在羰基的数目发生了变化。我们发现羰基的数目五年后曝光的同时在聚酯和二氧化硅纳米微粒/聚酯涂覆的样品降低。 <img alt="图3" src="/files/ftp_upload/54309/54309fig3.jpg" /> 图3.元素组成瓦里（PE），聚酯通货膨胀和二氧化硅纳米颗粒/聚酯涂料（PE +的SiO 2）五年以上暴露在阳光下的使用XPS确定。（A）代表XPS宽光谱和O的1秒的高分辨率光谱，C 1和的硅2P前和曝光后的聚酯涂料。 （B）的三要素（硅，铁和C）（原子分数）的浓度测定为暴露以确定下高水平潮湿条件下的阳光照射的表面涂层的组合物的变化的时间的函数。 <a href="http://ecsource.jove.com/files/ftp_upload/54309/54309fig3large.jpg" target="_blank">请此处查看该图的放大版本。</a> <img alt="图4" src="/files/ftp_upload/54309/54309fig4.jpg" /> 图4代表性的ATR-FTIR光谱三年后ENVIR的用于对钢表面涂层的羰基改变的测量onmental曝光。变化羰基的分布是由于酯基的紫外线诱导击穿。 <a href="http://ecsource.jove.com/files/ftp_upload/54309/54309fig4large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> 光学分析和原子力显微镜进一步用于研究的基质的在微米和纳米尺度的表面形貌。聚酯和二氧化硅纳米微粒/聚酯涂覆样品的微观地形演化示于图5中 。可以看出，这两个涂层的表面变得比原来的基质粗糙，曝光的一年后，然而，这增加了被发现，但有统计学显著（p&gt; 0.05）。 <img alt="图5" src="/files/ftp_upload/54309/54309fig5.jpg" /> 图5. MICR邻规模上超过钢五年曝光期间聚酯和二氧化硅纳米颗粒/聚酯涂料地形的变化。（A）曝光前后钢化涂料的代表光学分析图像。 （B）的图表表示在两涂层的平均粗糙度的环境暴露时间的函数的增加（*表示P &lt;0.05，与它的相应的控制（年0）相比较）。数据表示平均值±标准差。 <a href="http://ecsource.jove.com/files/ftp_upload/54309/54309fig5large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> 所述基质的进一步分析突出了纳米级表面形貌被显著改变作为紫外线灯照射的结果（ 图6，7和8）。原来的纳米二氧化硅/聚酯涂料光滑在纳米级，然而，曝光后，发现这些两种涂层已经形成的球状结构。五年后曝光的，发现表面表现出显著更高的平均粗糙度比原始基质，范围从40 - 47纳米（P &lt;0.05）。 <img alt="图6" src="/files/ftp_upload/54309/54309fig6.jpg" /> 图6.纳米超过五年期暴露钢聚酯涂料地形的变化。代表原子力显微照片及其相应的表面轮廓，突出了聚合物涂层的地形变化。 <a href="http://ecsource.jove.com/files/ftp_upload/54309/54309fig6large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图7" src="/files/ftp_upload/54309/54309fig7.jpg" /> 图7.纳米二氧化硅nanopa地形变化<html> rticle /聚酯涂料在5年的曝光时间。代表原子力显微照片及其相应的表面轮廓，突出了聚合物涂层的地形变化，尽管纳米二氧化硅保护层的存在。 <a href="http://ecsource.jove.com/files/ftp_upload/54309/54309fig7large.jpg" target="_blank">请点击此处查看大图这个数字。</a> <img alt="图8" src="/files/ftp_upload/54309/54309fig8.jpg" /> 聚酯和二氧化硅纳米微粒/聚酯涂层对钢作为曝光时间的函数的图8的平均纳米级表面粗糙度。表面涂层增加平均粗糙度与暴露的时间（*表示P &lt;0.05显著，与其相应的对照组比较（ 0年））。数据代表平均值±标准偏差。目标="_空白"&gt;点击此处查看该图的放大版本。

Watch this Scientific Journal Video about The Evolution of Silica Nanoparticle-polyester Coatings on Surfaces Exposed to Sunlight at JoVE.com

The Evolution of Silica Nanoparticle-polyester Coatings on Surfaces Exposed to Sunlight

两种类型的表面，涂覆有二氧化硅纳米颗粒的层的聚酯涂层钢板及聚酯，进行了研究。两面暴露在阳光下，将其发现导致在表面的化学性质和纳米形貌实质性的变化。

表面上的纳米硅聚酯涂料暴露在阳光下的演变

Corrosion of metallic surfaces is prevalent in the environment and is of great concern in many areas, including the military, transport, aviation, ...

the-evolution-silica-nanoparticle-polyester-coatings-on-surfaces

Nanyang Technological University

Research

JoVE Journal

Engineering

9.5K 次观看.  Swinburne University of Technology. 两种类型的表面，涂覆有二氧化硅纳米颗粒的层的聚酯涂层钢板及聚酯，进行了研究。两面暴露在阳光下，将其发现导致在表面的化学性质和纳米形貌实质性的变化。 

视频: The Evolution of Silica Nanoparticle-polyester Coatings on Surfaces Exposed to Sunlight

Preparation of Silica Nanoparticles Through Microwave-assisted Acid-catalysis

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle diameters ranging from 30-250 nm by varying the reaction conditions. Through the selection of a microwave compatible solvent, silicic acid precursor, catalyst, and microwave irradiation time, these microwave-assisted methods were capable of overcoming the previously reported shortcomings associated with synthesis of silica nanoparticles using microwave reactors. The siloxane precursor was hydrolyzed using the acid catalyst, HCl. Acetone, a low-tan &#948; solvent, mediates the condensation reactions and has minimal interaction with the electromagnetic field. Condensation reactions begin when the silicic acid precursor couples with the microwave radiation, leading to silica nanoparticle sol formation. The silica nanoparticles were characterized by dynamic light scattering data and scanning electron microscopy, which show the materials&#39; morphology and size to be dependent on the reaction conditions. Microwave-assisted reactions produce silica nanoparticles with roughened textured surfaces that are atypical for silica sols produced by St&#246;ber&#39;s methods, which have smooth surfaces.

Silica nanoparticles were prepared using acid-catalysis of a siloxane precursor and microwave-assisted synthetic techniques resulting in the controlled growth of nanomaterials ranging from 30-250 nm in diameter. The growth dynamics can be controlled by varying the initial silicic acid concentration, time of the reaction, and temperature of reaction.

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle ...

科研

化学

Stabilizing Hepatocellular Phenotype Using Optimized Synthetic Surfaces

Currently, one of the major limitations in cell biology is maintaining differentiated cell phenotype. Biological matrices are commonly used for culturing and maintaining primary and pluripotent stem cell derived hepatocytes. While biological matrices are useful, they permit short term culture of hepatocytes, limiting their widespread application. We have attempted to overcome the limitations using a synthetic polymer coating. Polymers represent one of the broadest classes of biomaterials and possess a wide range of mechanical, physical and chemical properties, which can be fine-tuned for purpose. Importantly, such materials can be scaled to quality assured standards and display batch-to-batch consistency. This is essential if cells are to be expanded for high through-put screening in the pharmaceutical testing industry or for cellular based therapy. Polyurethanes (PUs) are one group of materials that have shown promise in cell culture. Our recent progress in optimizing a polyurethane coated surface, for long-term culture of human hepatocytes displaying stable phenotype, is presented and discussed.

This article will focus on developing polymer coated surfaces for long-term, stable culture of stem cell derived human hepatocytes.

稳定肝细胞表型采用优化合成表面

Currently, one of the major limitations in cell biology is maintaining differentiated cell phenotype. Biological matrices are commonly used for culturing ...

Experimental Protocol to Investigate Particle Aerosolization of a Product Under Abrasion and Under Environmental Weathering

The present article presents an experimental protocol to investigate particle aerosolization of a product under abrasion and under environmental weathering, which is a fundamental element to the approach of nanosafety-by-design of nanostructured products for their durable development. This approach is basically a preemptive one in which the focus is put on minimizing the emission of engineered nanomaterials' aerosols during the usage phase of the product's life cycle. This can be attained by altering its material properties during its design phase without compromising with any of its added benefits. In this article, an experimental protocol is presented to investigate the nanosafety-by-design of three commercial nanostructured products with respect to their mechanical solicitation and environmental weathering. The means chosen for applying the mechanical solicitation is an abrasion process and for the environmental weathering, it is an accelerated UV exposure in the presence of humidity and heat. The eventual emission of engineered nanomaterials is studied in terms of their number concentration, size distribution, morphology and chemical composition. The purpose of the protocol is to study the emission for test samples and experimental conditions which are corresponding to real life situations. It was found that the application of the mechanical stresses alone emits the engineered nanomaterials' aerosols in which the engineered nanomaterial is always embedded inside the product matrix, thus, a representative product element. In such a case, the emitted aerosols comprise of both nanoparticles as well as microparticles. But if the mechanical stresses are coupled with the environmental weathering, the experimental protocol reveals then the eventual deterioration of the product, after a certain weathering duration, may lead to the emission of the free engineered nanomaterial aerosols too.

In this article, an experimental protocol to investigate particle aerosolization of a product under abrasion and under environmental weathering is presented. Results on the emission of engineered nanomaterials, in the form of aerosols are presented. The specific experimental set-up is described in detail.

实验协议来调查产品的粒子雾化在耐磨和环境下风化

The present article presents an experimental protocol to investigate particle aerosolization of a product under abrasion and under environmental ...

工程学

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 ...

Advanced Compositional Analysis of Nanoparticle-polymer Composites Using Direct Fluorescence Imaging

The fabrication of polymer-nanoparticle composites is extremely important in the development of many functional materials. Identifying the precise composition of these materials is essential, especially in the design of surface catalysts, where the surface concentration of the active component determines the activity of the material. Antimicrobial materials which utilize nanoparticles are a particular focus of this technology. Recently swell encapsulation has emerged as a technique for inserting antimicrobial nanoparticles into a host polymer matrix. Swell encapsulation provides the advantage of localizing the incorporation to the external surfaces of materials, which act as the active sites of these materials. However, quantification of this nanoparticle uptake is challenging. Previous studies explore the link between antimicrobial activity and surface concentration of the active component, but this is not directly visualized. Here we show a reliable method to monitor the incorporation of nanoparticles into a polymer host matrix via swell encapsulation. We show that the surface concentration of CdSe/ZnS nanoparticles can be accurately visualized through cross-sectional fluorescence imaging. Using this method, we can quantify the uptake of nanoparticles via swell encapsulation and measure the surface concentration of encapsulated particles, which is key in optimizing the activity of functional materials.

Here we present a reliable method to monitor the incorporation of nanoparticles into a polymer host matrix via swell encapsulation. We show that the surface concentration of cadmium selenide quantum dots can be accurately visualized through cross-sectional fluorescence imaging.

纳米粒子 - 聚合物复合材料使用直接荧光成像的先进成分分析

The fabrication of polymer-nanoparticle composites is extremely important in the development of many functional materials. Identifying the precise ...

TiO2-coated Hollow Glass Microspheres with Superhydrophobic and High IR-reflective Properties Synthesized by a Soft-chemistry Method

This manuscript proposes a soft-chemistry method to develop superhydrophobic and highly IR-reflective hollow glass microspheres (HGM). The anatase TiO2 and a superhydrophobic agent were coated on the HGM surface in one step. TBT and PFOTES were selected as the Ti source and the superhydrophobic agent, respectively. They were both coated on the HGM, and after the hydrothermal process, the TBT turned to anatase TiO2. In this way, a PFOTES/TiO2-coated HGM (MCHGM) was prepared. For comparison, PFOTES single-coated HGM (F-SCHGM) and TiO2 single-coated HGM (Ti-SCHGM) were synthesized as well. The PFOTES and TiO2 coatings on the HGM surface were demonstrated through X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive detector (EDS) characterizations. The MCHGM showed a higher contact angle (153&#176;) but a lower sliding angle (16&#176;) than F-SCHGM, with a contact angle of 141.2&#176; and a sliding angle of 67&#176;. In addition, both Ti-SCHGM and MCHGM displayed similar IR reflectivity values, which were about 5.8% higher than the original HGM and F-SCHGM. Also, the PFOTES coating barely changed the thermal conductivity. Therefore, F-SCHGM, with a thermal conductivity of 0.0479 W/(m&#183;K), was quite like the original HGM, which was 0.0475 W/(m&#183;K). MCHGM and Ti-SCHGM were also similar. Their thermal conductivity values were 0.0543 W/(m&#183;K) and 0.0543 W/(m&#183;K), respectively. The TiO2 coating slightly increased the thermal conductivity, but with the increase in reflectivity, the overall heat-insulation property was enhanced. Finally, since the IR-reflecting property is provided by the HGM coating, if the coating is fouled, the reflectivity decreases. Therefore, with the superhydrophobic coating, the surface is protected from fouling, and its lifetime is also prolonged.

TiO2-coated Hollow Glass Microspheres with Superhydrophobic and High IR-reflective Properties Synthesized by a Soft-chemistry Method

This manuscript proposes a soft-chemistry method to synthesize superhydrophobic, TiO2-coated hollow glass microspheres (HGM) with high IR-reflective properties.

二氧化钛<sub&gt; 2</sub与由软化学法合成的超疏水性和高IR反射属性&gt;涂覆的空心玻璃微球

This manuscript proposes a soft-chemistry method to develop superhydrophobic and highly IR-reflective hollow glass microspheres (HGM). The anatase TiO2 ...

Deposition of Porous Sorbents on Fabric Supports

A microwave deposition technique for silanes, previously described for production of oleophobic fabrics, is adapted to provide a fabric support material that can be subsequently treated by dip coating. Dip coating with a sol preparation provides a supported porous layer on the fabric. In this case, the porous layer is a porphyrin functionalized sorbent system based on a powdered material that has been demonstrated previously for the capture and conversion of phosgene. A representative coating is applied to cotton fabric at a loading level of 10 mg/g. This coating has minimal impact on water vapor transport through the fabric (93% of the support fabric rate) while significantly reducing transport of 2-chloroethyl ethyl sulfide (CEES) through the material (7% of support fabric rate). The described approaches are suitable for use with other fabrics providing amine and hydroxyl groups for modification and can be used in combination with other sol preparations to produce varying functionality.

This report details a microwave-initiated approach for deposition of porphyrin functionalized porous organosilicate sorbents on a cotton fabric and demonstrates reduction in 2-chloroethyl ethyl sulfide (CEES) transport through the fabric resulting from this treatment.

织物支架上多孔吸附剂的沉积

A microwave deposition technique for silanes, previously described for production of oleophobic fabrics, is adapted to provide a fabric support material ...

Preparation of Functional Silica Using a Bioinspired Method

The goal of the protocols described herein is to synthesize bioinspired silica materials, perform enzyme encapsulation therein, and partially or totally purify the same by acid elution. By combining sodium silicate with a polyfunctional bioinspired additive, silica is rapidly formed at ambient conditions upon neutralization. 
The effect of neutralization rate and biomolecule addition point on silica yield are investigated, and biomolecule immobilization efficiency is reported for varying addition point. In contrast to other porous silica synthesis methods, it is shown that the mild conditions required for bioinspired silica synthesis are fully compatible with the encapsulation of delicate biomolecules. Additionally, mild conditions are used across all synthesis and modification steps, making bioinspired silica a promising target for the scale-up and commercialization as both a bare material and active support medium.
The synthesis is shown to be highly sensitive to conditions, i.e., the neutralization rate and final synthesis pH, however tight control over these parameters is demonstrated through the use of auto titration methods, leading to high reproducibility in reaction progression pathway and yield. 
Therefore, bioinspired silica is an excellent active material support choice, showing versatility towards many current applications, not limited to those demonstrated here, and potency in future applications.

Here, we present a protocol to synthesize bioinspired silica materials and immobilize enzymes therein. Silica is synthesized by combining sodium silicate and an amine &#39;additive&#39;, which neutralize at a controlled rate. Material properties and function can be altered either by in situ enzyme immobilization or post-synthetic acid elution of encapsulated additives.

用 Bioinspired 法制备功能性二氧化硅

The goal of the protocols described herein is to synthesize bioinspired silica materials, perform enzyme encapsulation therein, and partially or totally ...

Multiscale Structures Aggregated by Imprinted Nanofibers for Functional Surfaces

Multiscale surface structures have attracted increasing interest owing to several potential applications in surface devices. However, an existing challenge in the field is the fabrication of hybrid micro-nano structures using a facile, cost-effective, and high-throughput method. To overcome these challenges, this paper proposes a protocol to fabricate multiscale structures using only an imprint process with an anodic aluminum oxide (AAO) filter and an evaporative self-aggregation process of nanofibers. Unlike previous attempts that have aimed to straighten nanofibers, we demonstrate a unique fabrication method for multiscale aggregated nanofibers with high aspect ratios. Furthermore, the surface morphology and wettability of these structures on various liquids were investigated to facilitate their use in multifunctional surfaces.

Presented is an easy method to fabricate nano-micro multiscale structures, for functional surfaces, by aggregating nanofibers fabricated using an anodic aluminum oxide filter.

功能表面用印迹纳米纤维聚合的多尺度结构

Multiscale surface structures have attracted increasing interest owing to several potential applications in surface devices. However, an existing ...

Photopatterning Proteins and Cells in Aqueous Environment Using TiO2 Photocatalysis

Organic contaminants adsorbed on the surface of titanium dioxide (TiO2) can be decomposed by photocatalysis under ultraviolet (UV) light. Here we describe a novel protocol employing the TiO2 photocatalysis to locally alter cell affinity of the substrate surface. For this experiment, a thin TiO2 film was sputter-coated on a glass coverslip, and the TiO2 surface was subsequently modified with an organosilane monolayer derived from octadecyltrichlorosilane (OTS), which inhibits cell adhesion. The sample was immersed in a cell culture medium, and focused UV light was irradiated to an octagonal region. When a neuronal cell line PC12 cells were plated on the sample, cells adhered only on the UV-irradiated area. We further show that this surface modification can also be performed in situ, i.e., even when cells are growing on the substrate. Proper modification of the surface required an extracellular matrix protein collagen to be present in the medium at the time of UV irradiation. The technique presented here can potentially be employed in patterning multiple cell types for constructing coculture systems or to arbitrarily manipulate cells under culture.

Photopatterning Proteins and Cells in Aqueous Environment Using TiO2 Photocatalysis

We describe a protocol for modifying cell affinity of a scaffold surface in aqueous environment. The method takes advantage of titanium dioxide photocatalysis to decompose organic film in the photo-irradiated region. We show that it can be used to create microdomains of scaffolding proteins, both ex situ and in situ.

光图案蛋白质和细胞中的水环境中使用二氧化钛<sub&gt; 2</sub&gt;光催化

Organic contaminants adsorbed on the surface of titanium dioxide (TiO2) can be decomposed by photocatalysis under ultraviolet (UV) light. Here we describe ...

表面上的纳米硅聚酯涂料暴露在阳光下的演变

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