Name: determination of aggregate surface morphology at the interfacial transition zone (itz)
Uploaded: 2019-12-16T15:00:00
Description: Watch this Scientific Journal Video about Determination of Aggregate Surface Morphology at the Interfacial Transition Zone ITZ at JoVE.com

作者感谢国家重点研发项目（2017YFB0309904）、国家自然科学基金（授权号51508090和51808188）、973计划（2015CB655100）、国家重点实验室的财政支持。高性能土木工程材料 （2016CEM005）。同时，对江苏省建筑科学研究院和高性能土木工程材料国家重点实验室的资助项目表示高度赞赏。

1. 用单个陶瓷颗粒制备模型混凝土
<ol><li>模具制备<ol>
<li>使用刷子清洁模具（25 毫米 x 25 毫米 x 25 毫米），并确保模具的内表面无杂质。</li>
		<li>使用另一个刷子均匀地将柴油涂抹在模具的内表面，以便更容易脱模。 注：在这里，我们没有使用普通模具进行砂浆或混凝土制备。由于陶瓷颗粒直径约15毫米，因此使用长度约30毫米的立方塑料模具进行样品制备。确保塑料模具的尺寸大于陶瓷颗粒...

<ol>
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采用X-CT技术粗略确定陶瓷粒子的几何中心，以确保分析的表面通过粒子的赤道。因此，可以避免高估由2D伪影引起的ITZ厚度。因此，获得结果的准确性在很大程度上取决于被检查表面的平坦度。通常，较长的磨削和抛光时间有助于表面充分光滑，以便进行测试。然而，由于水泥膏和陶瓷颗粒之间的硬度不同，长时间的磨削和抛光时间往往在两个阶段之间产生高度差异，在获得的B...

在中观尺度上，水泥基材料可视为由水泥膏、聚合体和界面过渡区（ITZ）组成的三相复合材料，它们之间的1、2。ITS通常被视为一个薄弱环节，因为它增加的孔隙度可以作为入侵物种3，4的通道，或为裂缝生长5，6，7，8，9，10，11提供更容易的途径。因此，对精确描述ITZ的特性进行评价和预测水泥基材料的宏观性能是十分感兴趣的。
为了研究ITZ，对它微观结构特征、形成机制和影响因子12、13、14的研究都采用了实验和数值方法。各种技术已经结合为ITZ表征，包括：机械测试，运输测试，汞入侵孔隙测量（MIP）测试15，16和纳米缩进17。人们普遍认为，IT主要是由墙体效应引起的，以及水膜、微出血、单侧生长和凝胶辛斯18。
随着近二十年来数字图像处理方法（DIP）的发展，可以定量确定信息源的形态特征（如体积分数、厚度和孔隙梯度）。基于使用带背散电子探测器（BSE）的扫描电子显微镜（SEM）对平面部分的检查，通过立体理论20，从2D结果中得出ITZ的三维（3D）特征。与SEM-BSE技术一样，纳米缩进技术也基于对抛光表面的检查，但它更侧重于现有阶段21的弹性模量。然而，在SEM-BSE分析和纳米缩进试验中，由于被检查的横截面很少从总表面22穿过正常方向，因此对ITZ厚度可能被高估。然而，结合荧光3D共聚焦显微镜，可以消除对ITZ的高估，获得真正的ITZ孔隙度和无水水泥含量。
以往对影响因素的研究主要集中在水泥膏上，忽略了骨料的作用及其表面质地24、25、26。由于聚合的形状和形态特性已经广泛描述的基础上，从SEM或X射线计算机断层扫描（X-CT）27，28的数字切片的定量分析。然而，还没有开展以聚合表面纹理对伊茨区域形成影响的研究。
本文根据SEM-BSE图像的定量分析和K-means聚类算法，提出了一种研究聚合表面形态对ITZ微观结构形成的影响的协议。以球形陶瓷颗粒作为粗骨料制备模型混凝土样品。X-CT 用于在将样品减半之前大致确定颗粒在不透明水泥基质中的相对位置。对获得SEM-BSE图像的处理后，观察到了单聚合周围ITZ的不均匀分布。此外，还定义了描述像素级别的聚合表面纹理的索引表面粗糙度 （SR）。K-均值聚类算法最初用于信号处理领域，现在广泛用于图像聚类29，30，被引入建立表面粗糙度（SR）和孔隙度梯度（SL）之间的关系。

<table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always">
	<tbody>
		<tr>
			<td>Auto Sputter Coater</td>
			<td>Cressington</td>
			<td>108 Auto/SE</td>
			<td></td>
		</tr>
		<tr>
			<td>Automatic polishing machine</td>
			<td>Buehler</td>
			<td>Phoenix4000</td>
			<td></td>
		</tr>
		<tr>
			<td>Brush</td>
			<td>Huoniu</td>
			<td>3#</td>
			<td></td>
		</tr>
		<tr>
			<td>Cement</td>
			<td>China United Cement Corporation</td>
			<td>P.I. 42.5</td>
			<td></td>
		</tr>
		<tr>
			<td>Cement paste mixer</td>
			<td>Wuxi Construction and Engineering</td>
			<td>NJ160</td>
			<td></td>
		</tr>
		<tr>
			<td>Ceramic particle</td>
			<td>Haoqiang</td>
			<td>&#934;15 mm</td>
			<td></td>
		</tr>
		<tr>
			<td>Cling film</td>
			<td>Miaojie</td>
			<td>65300</td>
			<td></td>
		</tr>
		<tr>
			<td>Cold mounting machine</td>
			<td>Buehler</td>
			<td>Cast N&#39; Vac 1000</td>
			<td></td>
		</tr>
		<tr>
			<td>Conductive tape</td>
			<td>Nissin Corporation</td>
			<td>7311</td>
			<td></td>
		</tr>
		<tr>
			<td>Cup</td>
			<td>Buehler</td>
			<td>20-8177-100</td>
			<td></td>
		</tr>
		<tr>
			<td>Cutting machine</td>
			<td>Buehler</td>
			<td>Isomet 4000</td>
			<td></td>
		</tr>
		<tr>
			<td>Cylindrical plastic mold</td>
			<td>Buehler</td>
			<td>20-8151-100</td>
			<td></td>
		</tr>
		<tr>
			<td>Diamond paste</td>
			<td>Buehler</td>
			<td>00060210, 00060190, 00060170</td>
			<td></td>
		</tr>
		<tr>
			<td>Diesel oil</td>
			<td>China Petroleum</td>
			<td>0#</td>
			<td></td>
		</tr>
		<tr>
			<td>Electronic balance</td>
			<td>Setra</td>
			<td>BL-4100F</td>
			<td></td>
		</tr>
		<tr>
			<td>Epoxy resin</td>
			<td>Buehler</td>
			<td>20-3453-128</td>
			<td></td>
		</tr>
		<tr>
			<td>Hardener</td>
			<td>Buehler</td>
			<td>20-3453-032</td>
			<td></td>
		</tr>
		<tr>
			<td>High precision cutting machine</td>
			<td>Buehler</td>
			<td>2215</td>
			<td></td>
		</tr>
		<tr>
			<td>Image J</td>
			<td>National Institutes of Health</td>
			<td>1.52o</td>
			<td></td>
		</tr>
		<tr>
			<td>Isopropyl alcohol</td>
			<td>Sinopharm</td>
			<td>M0130-241</td>
			<td></td>
		</tr>
		<tr>
			<td>Matlab</td>
			<td>MathWorks</td>
			<td>R2014a</td>
			<td></td>
		</tr>
		<tr>
			<td>Paper</td>
			<td>Deli</td>
			<td>A4</td>
			<td></td>
		</tr>
		<tr>
			<td>Plastic box</td>
			<td>Beichen</td>
			<td>3630</td>
			<td></td>
		</tr>
		<tr>
			<td>Plastic mold</td>
			<td>Youke</td>
			<td>a=b=c=25mm</td>
			<td></td>
		</tr>
		<tr>
			<td>Polished flannelette</td>
			<td>Buehler</td>
			<td>242150, 00242050, 00242100</td>
			<td></td>
		</tr>
		<tr>
			<td>Release agent</td>
			<td>Buehler</td>
			<td>20-8186-30</td>
			<td></td>
		</tr>
		<tr>
			<td>Scanning Electron Microscopy</td>
			<td>FEI</td>
			<td>Quanta 250</td>
			<td></td>
		</tr>
		<tr>
			<td>Scrape knife</td>
			<td>Jinzheng Building Materials</td>
			<td>CD-3</td>
			<td></td>
		</tr>
		<tr>
			<td>SiC paper</td>
			<td>Buehler</td>
			<td>P180, P320, P1200</td>
			<td></td>
		</tr>
		<tr>
			<td>Ultrasonic cleaner</td>
			<td>Zhixin</td>
			<td>DLJ</td>
			<td></td>
		</tr>
		<tr>
			<td>Vacuum box</td>
			<td>Heheng</td>
			<td>DZF-6020</td>
			<td></td>
		</tr>
		<tr>
			<td>Vacuum drying oven</td>
			<td>ZK</td>
			<td>ZK30</td>
			<td></td>
		</tr>
		<tr>
			<td>Vibrating table</td>
			<td>Jianyi</td>
			<td>GZ-75</td>
			<td></td>
		</tr>
		<tr>
			<td>Wooden stick</td>
			<td>Buehler</td>
			<td>20-8175</td>
			<td></td>
		</tr>
		<tr>
			<td>X-ray Computed Tomography</td>
			<td>YXLON</td>
			<td>Y.CT PRECISION S</td>
			<td></td>
		</tr>
	</tbody>
</table>

determination of aggregate surface morphology at the interfacial transition zone (itz)

本文提出了一种综合方法，说明围绕聚合的界面过渡区（ITZ）分布不均，以及聚合表面形态对性指标的形成的影响。首先，用球形陶瓷颗粒在水泥基质的中央部分制备一个模型混凝土样品，作为普通混凝土/砂浆中使用的粗骨。固化至设计年龄后，通过X射线计算机断层扫描样品，以确定陶瓷颗粒在水泥基质中的相对位置。选择三个位置：在聚合上方、聚合侧和聚合下方。经过一系列处理后，使用 SEM-BSE 检测器扫描样品。利用数字图像处理方法（DIP）对结果图像进行进一步处理，以获得ITZ的定量特性。基于数字图像的像素层次，对表面形态进行了特征化。此后，采用K-值聚类法来说明表面粗糙度对ITZ形成的影响。

对位于聚合方、聚合侧和聚合下方的 ITZ 区域的孔隙分布进行了比较，如图432所示。上表面上方的 ITZ 孔隙度似乎小于骨量侧面或上方，表明其密度较高，而聚合下方的 ITZ 始终由于微出血而最多孔。图 432显示，即使围绕相同的聚合，分布也是不均匀的。
为了研究聚合曲面形态的影响，手动捕获?...

Watch this Scientific Journal Video about Determination of Aggregate Surface Morphology at the Interfacial Transition Zone ITZ at JoVE.com

Determination of Aggregate Surface Morphology at the Interfacial Transition Zone ITZ

本文提出了一种说明集面形态学对ITZ微观结构的影响的协议。通过数字图像处理对SEM-BSE图像进行了定量分析，获得了ITZ的孔隙度梯度，并进一步采用了K-均值聚类算法，建立了孔隙梯度与表面粗糙度的关系。

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 ...

我们提出了一个方案，用于研究聚合表面形态对水泥材料中个别过渡区的形成的影响。将实验方法与数据处理方法相结合，说明集料表面粗糙度对伊茨形成的影响。首先成型模型混凝土。用电子天平称重1000克水泥和350克水，然后用湿毛巾擦拭5升混合锅，以滋润它。将水和水泥加入锅中，放在搅拌器上，将其提升至搅拌位置。在 65 rpm 下混合 90 秒，让混合物静止 30 秒。在锅内壁的糊状中刮。然后在 130 rpm 下再混合 60 秒。从搅拌机中取出锅，将陶瓷颗粒放入糊状物中，然后用手将其与水泥糊彻底混合。用新鲜的水泥糊半填充模具，将陶瓷颗粒放在糊状物的顶部，用糊状物填充模具的其余部分。用刮刀擦掉多余的水泥糊，在振动桌上振动模具一分钟。用保鲜膜密封模具表面，防止水分蒸发。在固化室中固化样品 24 小时，然后从模具中取出试样，并在相同的环境条件下固化 28 天。使用 X 射线计算机断层扫描试样，以获得一叠切片，并大致选择陶瓷颗粒看起来最大的切片。将陶瓷粒子的边界与圆拟合，并确定圆的中心为粒子的几何中心。使用切割机通过陶瓷颗粒的几何中心将试样切成两部分。然后将两部分浸入异丙醇中三天，以去除未绑定的水并终止内部水化。确保每 24 小时更换一次异丙基溶液。在40摄氏度的温度下，在真空烘箱中干燥两部分7天。要凝固微观结构，请用手指涂抹两个圆柱形塑料模具的内表面，并涂上脱模膏。将一块样品放入每个模具中，表面朝下检查。在纸杯中，重50克低粘度环氧树脂，加入5克硬质，然后手动搅拌混合物两分钟。将模具与纸杯一起放入冷安装机中。启动机器上的真空，将环氧树脂倒入模具中，直到与每个样品合并。将模具在机器中保持 24 小时，使环氧树脂更硬。第二天，拆下每个模具的底部并挤出样品。将其存放在真空烘干炉中。准备就绪后，在文本手稿中描述的自动抛光机上用碳化硅纸和酒精研磨样品。然后将法兰绒连接到机器的转盘上，以 150 rpm 的速度用三、一和 0.25 微米的金刚石糊抛光样品。每次研磨和抛光步骤后，用酒精清除超声波清洁剂中的碎屑。完成后，将每个样品存放在塑料盒中，表面朝上检查，将样品存放在真空干炉中。在真空环境中，在表面上喷洒一层薄薄的金箔，用自动溅射涂布机进行检查。将胶带条放在样品侧面，连接测试表面和相反表面，然后将样品放在测试台上，测试面朝上。将样品移动到区域 1 上，然后真空 SEM 并更改为反散射电子模式。将放大倍数设置为 1000 倍，并仔细调整亮度和对比度。沿聚合边界的方向将镜头移动到另一个位置，然后拍摄另一个图像。获取至少 15 张图像进行统计分析。然后在区域二和三上重复成像过程。成像后，使用图像 J 对图像进行最佳拟合和三次三分之一中位数滤镜三次的预处理，以降低噪声并增强不同相位的边界。手动捕获陶瓷粒子的边界，然后从原始图像中剪切此部分。通过设置不同的阈值和分割图像以与原始值进行比较，大致确定孔相的上阈值。获取图像其余部分的灰度分布。选择曲线的两个大致线性部分，略高于预定的上限阈值，并适合线性曲线的这两个部分。交点将设置在此图像的确切上限阈值。使用此值执行分段，并将二进制图像与原始灰度图像进行比较，以确定最终阈值。然后将灰度图像转换为二进制图像，白色表示孔相，黑色表示实心相。比较了上述、在聚合面和以下的 ITZ 区域的孔隙分布。上表面上方的孔隙度小于聚集体侧面或上方的孔隙度，而集料下方的 ITZ 由于微漂白而是最多孔的。通过将手动捕获的不规则边界与直线和圆弧进行拟合，对聚集表面形态进行了调查。直线似乎更适合所选边界。计算了定义的表面粗糙度和孔隙度梯度参数，并应用K-means聚类算法将散射点细分为两个组，即粗糙度组和平滑组。随着孔隙度梯度的减小，表面粗糙度增加。对粗糙光滑的组值的孔隙分布进行平均和比较，几乎在每一个距离，ITZ在光滑表面周围的孔隙度明显低于粗糙表面周围的孔隙度，证明地表形态确实在 ITZ 的形成中起着重要作用。应选择正确的研磨和抛光工艺，以获得足够光滑的表面，以便进行 BSE 检查。根据对采用高斯混合物模型的BSE测量的定量分析，还可以确定水泥材料中不同相的体积分数。BSE是多相材料成分定量分析的有力技术。

Research

JoVE Journal

Engineering

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

Experimental Measurement of Settling Velocity of Spherical Particles in Unconfined and Confined Surfactant-based Shear Thinning Viscoelastic Fluids

无约束和封闭表面活性剂中球形粒子沉降速度的实验测量 剪切变薄粘性流体

An experimental study is performed to measure the terminal settling velocities of spherical particles in surfactant based shear thinning viscoelastic ...

科研

工程学

Laboratory Drop Towers for the Experimental Simulation of Dust-aggregate Collisions in the Early Solar System

实验室落塔的粉尘聚集在碰撞早期太阳系的实验模拟

For the purpose of investigating the evolution of dust aggregates in the early Solar System, we developed two vacuum drop towers in which fragile dust ...

Taking Advantage of Reduced Droplet-surface Interaction to Optimize Transport of Bioanalytes in Digital Microfluidics

以减少液滴表面的相互作用来优化Bioanalytes运输中的数字微流体

Digital microfluidics (DMF), a technique for manipulation of droplets, is a promising alternative for the development of &#8220;lab-on-a-chip&#8221; ...

Ambient Method for the Production of an Ionically Gated Carbon Nanotube Common Cathode in Tandem Organic Solar Cells

对于一个以离子门控碳纳米管共阴极的串联有机太阳能电池的生产环境法

A method of fabricating organic photovoltaic (OPV) tandems that requires no vacuum processing is presented. These devices are comprised of two ...

How to Ignite an Atmospheric Pressure Microwave Plasma Torch without Any Additional Igniters

如何点燃常压微波等离子体炬没有任何额外的点火器

This movie shows how an atmospheric pressure plasma torch can be ignited by microwave power with no additional igniters. After ignition of the plasma, a ...

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

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 ...

The Measurement of Unsteady Surface Pressure Using a Remote Microphone Probe

非定常表面压力的使用远程麦克风探头测量

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

Emission Spectroscopic Boundary Layer Investigation during Ablative Material Testing in Plasmatron

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 ...

Preparation of Liquid-exfoliated Transition Metal Dichalcogenide Nanosheets with Controlled Size and Thickness: A State of the Art Protocol

与尺寸可控液体剥离的过渡金属二硫属化物纳米片和厚度的制备：艺术议定书的国家

We summarize recent advances in the production of liquid-exfoliated transition metal dichalcogenide (TMD) nanosheets with controlled size and thickness. ...

Orientational Transition in a Liquid Crystal Triggered by the Thermodynamic Growth of Interfacial Wetting Sheets

由界面润湿片的热力学生长触发的液晶中的定向转变

In liquid crystal (LC) physical chemistry, molecules near the surface play a great role in controlling bulk orientation. Thus far, mainly to achieve ...