这项研究是在太平洋西北国家实验室 (PNNL) 进行的, 该实验由能源部巴特利纪念研究所根据合同编号进行管理。DE-AC05-76RL01830。

这里所描述的实验要求使用的氢气是无嗅的, 无色的, 从而无法检测到人类的感官。氢气是高度易燃和燃烧与几乎无形的蓝色火焰, 可以形成爆炸性混合物在存在的氧气。高压力超过6.9 兆帕增加额外的爆炸危险, 必须适当规划, 以准备任何测试。这种储存的能量意味着严重的安全隐患, 因此, 在进行这样的试验之前, 必须进行尽职调查、规划和安全评估, 以确保减轻这些危险。这里的实验是按照美国机械工程师协会 (ASME) 认证的压力容器中的适当的安全预防措施进行的, 并在适当的通风条件下将爆裂盘设置为34.5 兆帕。
1. 制备高分子板材
<ol><li>将洗涤剂应用于 EDPM 聚合物板材, 使用非磨料海绵, 在水下冲洗约3分钟, 以除去在制造和运输过程中应用的油和滑石粉。</li>
	<li>干燥的聚合物板材在烘干烤箱在材料的工作温度的 85%, 大约75°c 为 EPDM, 大约72小时驱动任何水剩余从洗涤。</li>
	<li>关闭烤箱, 并允许聚合物板材材料冷却到室温内的烤箱。</li>
	<li>用指向聚合物片顶部的箭头标记钣金件的一角。这支箭将有助于确定在样品券产生的方向的工作表, 确保从聚合物片切割样品将始终如一的相同的方向。</li>
	<li>在室温、湿度控制环境下, 在摩擦学试验之前, 将聚合物板材贮存在室温下, 温度接近25% 相对湿度。</li>
</ol>2. 生成和安装样品优惠券
<ol><li>在佩戴无粉手套的同时, 在聚合物薄板的制备过程中, 用箭头在预期的息票区域标记聚合物板材, 使两个箭头具有相同的方向。</li>
	<li>使用2.222 厘米直径圆形模具和槌, 戳出一个样品券围绕箭头标记。</li>
	<li>松开在原位摩擦上固定样品钳的六角帽螺钉, 从样品夹最容易接近的拐角处卸下六角帽螺钉和精密弹簧。</li>
	<li>滑动样品券到样品夹, 注意确保样品是面向的箭头指向面向下和朝向背面的钳, 这是最接近背面板的摩擦。</li>
	<li>更换精密弹簧和六角帽螺钉在样品钳的空角, 并着手收紧所有四的六角帽螺钉的钳, 直到舒适, 使弹性体样品压缩10% 的原始高度。假设一个0.318 厘米的样本高度, 10% 的压缩可以达到通过使用 0.287 cm 标尺块之间的两个板块的夹具。</li>
</ol>3. 准备就地摩擦
<ol><li>在摩擦的墙和样品雪橇之间放置一个2.413 厘米的量规块, 直接位于驱动螺钉的下方。请确保数据收集框已关闭, 然后按顺时针方向旋转驱动器链以返回示例雪橇, 这样, 雪橇的边缘就会从摩擦壁2.413 厘米。</li>
	<li>用软布或不起毛的纸巾轻轻擦拭柜台表面的钢球, 并在大约30秒内用丙酮等适当的溶剂, 直到柜台表面表面没有任何碎屑。</li>
	<li>滑动青铜计数器表面载体和青铜重量, 总正常载荷为 7.5 N, 垂直于试样雪橇的导轨上, 允许计数器球滑入孔内并在聚合物样品上休息。</li>
	<li>使用六角键和两个青铜螺钉, 将线性可变差动变压器 (LVDT) 测量臂重新连接到青铜计数器表面支架上, 使 LVDT 的自由浮动气缸靠在手臂上。</li>
	<li>调整夹持 LVDT 的钳位, LVDT 在零点附近测量, 然后拧紧夹具以确保 LVDT 到位。</li>
	<li>将摩擦组件降低到压力容器中, 确保容器顶部法兰上的热电偶套管降低到摩擦和容器壁之间的间隙。</li>
	<li>包装密封 o 形环, 共两个半层的聚四氟乙烯胶带。这是通过包装聚四氟乙烯胶带, 使每一个额外的包装重叠约一半的程序圈, 直到绕 o 形环直径两次。然后将 o 形环的直径包装成最后一次, 不加任何重叠。一旦 o 形环被包裹, 把它放在凹槽中的压力容器的唇。</li>
	<li>考虑到接线标签, 重新连接摩擦马达的五个电源线、四个负载单元的数据线和五个 LVDT 的数据线。</li>
</ol>4. 密封压力容器
<ol><li>降低压力容器的顶部法兰, 将其关闭, 注意将顶部法兰轻轻地放到聚四氟乙烯包裹密封 o 形环上。</li>
	<li>将螺栓插入到制造商以升序指示的顶部法兰上的编号孔中, 直到手指紧固为止。</li>
	<li>使用手动十六进制键, 扭矩的法兰螺栓升序, 以手紧, 重复, 直到螺栓不能再收紧。</li>
	<li>从120毫微米开始, 并增加 40 nm 增量, 使用扭矩扳手扭矩的法兰螺栓以升序为每 ~ 40 Nm 增量, 直到它们被扭转到 280 nm。</li>
</ol>5. 灌装压力容器
<ol><li>压力容器密封后, 将气体配件连接到高压釜盖上, 将低压 (0.55 兆帕) 氩气的压力容器冲洗约1小时, 直到容器中的氧含量降到 10 ppm 以下, 使用氧气传感器探测到压力容器的输出。</li>
	<li>慢慢地 (< 0.25 兆帕/秒) 用氢气将容器冲洗至6.9 兆帕, 然后慢慢地将气体排放到大气压。重复冲洗过程两次。</li>
	<li>在冲洗压力容器后, 缓慢地 (< 0.25 兆帕) 填充压力容器, 氢气高达13.75 兆帕, 允许容器休息10分钟, 使容器内气体的温度 equilibrates 室温。</li>
	<li>将容器装满20.7 兆帕, 再等10分钟。</li>
	<li>把船上的目标 27.6 MPa 和关闭所有阀门。</li>
	<li>在开始实验之前, 允许聚合物样品在氢气中浸泡至少12小时, 以便完全渗透。</li>
</ol>6. 运行实验
<ol><li>双检查所有进出压力容器的直通导线是否正确连接到连接到摩擦控制箱的标签线束, 然后打开摩擦。</li>
	<li>在摩擦软件设置实验时间到1小时以 0.1 cm/s 速度以 0.140 cm 的路径长度。这对应于距离大约 3.5 m。</li>
	<li>对负载单元进行包装, 并确保 LVDT 在摩擦软件中报告适当的深度, 应接近0毫米。</li>
	<li>开始实验。</li>
</ol>7. 后实验
<ol><li>实验完成后, 将氢气的压力容器慢慢排出大约0.35 兆帕, 确保压力容器温度不会降到0摄氏度以下。</li>
	<li>最后, 在大气压下用氩气冲洗压力容器容积10分钟, 以确保容器内没有剩余的氢气。</li>
</ol>

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作者没有什么可透露的。

现有的用于高分子材料摩擦学测试的前向原位技术要求样品暴露在高压氢气上, 然后减压使用商用摩擦进行测试。15,24,25本协议中的测试方法旨在允许在高压环境下对聚合物样品的摩擦学性能进行测试,原位。通过对以上所述的高分子材料 (如三元乙丙橡胶试样的加压) 进行测试, 本协议允许对在氢输送基础设施组件?...

近年来, 在车辆和固定动力源中, 氢气作为潜在的零排放或近零排放燃料的兴趣一直很大。由于氢气存在于室温下的低密度气体中, 大多数应用都使用某种形式的压缩氢气作为燃料。1,2使用压缩高压氢气的潜在缺点与基础结构2、3、4和车载应用程序5中发现的许多材料不兼容, 其中兼容性问题与反复压力和温度循环相结合。一个纯净的氢环境是已知的损害金属成分, 包括某些钢和钛通过不同的机制, 包括氢化物形成, 膨胀, 表面起泡和脆化。2,6,7,8在压电陶瓷中使用的锆钛酸铅 (PZT) 等非金属元件也被证明易受降解, 因为氢不相容效应, 如表面起泡和铅迁移。9,10,11,12虽然以前曾研究过氢暴露造成的损害的这些例子, 但在氢环境中聚合物组分的相容性最近才引起关注。13,14,15,16这主要是由于金属部件在核和石油和天然气应用中提供结构完整性, 而聚合物成分通常充当屏障或密封。17,18,19,20因此, 在诸如聚四氟乙烯 (PTFE) 阀座和丁腈橡胶 (丁腈橡胶) O 形环等元件内的高分子材料的摩擦和磨损特性成为其功能能力的重要因素。
在氢基础设施的情况下, 诸如阀门、压缩机和储罐等部件含有与金属表面接触的高分子材料。聚合物和金属表面之间的摩擦相互作用导致每个表面的磨损。两个相互作用表面的摩擦和磨损之间的关系的科学被称为摩擦学。聚合物的弹性模量和强度比金属低, 因此高分子材料的摩擦学性能与金属材料有很大的不同。因此, 在与金属表面摩擦接触后, 聚合物表面往往表现出更大的磨损和损伤。21,22在氢基础设施应用中, 快速压力和温度循环导致聚合物与金属表面反复相互作用, 增加了聚合物组分摩擦和磨损的可能性。量化这一损害可能是挑战前现场由于可能爆炸减压的聚合物样品后减压, 可能会导致非摩擦学损伤。23此外, 许多商业聚合物产品含有许多填充剂和添加剂, 如氧化镁 (氧化镁), 它们可能通过氢与氢气产生负面作用, 进一步使原位分析的磨损在这些材料.24,25
由于摩擦磨损对聚合物材料损伤的判别复杂度为原位, 因此需要直接研究非金属材料的摩擦特性原位在可能存在于氢传递基础结构中的高压氢环境中。在本议定书中, 我们演示了一种测试方法, 用于在高压氢环境中利用专门构建的原位摩擦来量化聚合物材料的摩擦和磨损特性。26我们还提供使用原位摩擦和乙烯丙二烯单体 (三元乙丙橡胶) 获得的具有代表性的数据, 这是一种常见的聚合物密封和阻隔材料。使用下面的协议生成具有代表性数据的三元乙丙橡胶材料是以60.96 厘米见方的0.3175 厘米厚的方形板材购买的, 并由供应商报告其硬度等级为60A。

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			<td height="79" style="height:79px;width:201px;">EPDM Polymer Stock Sheet</td>
			<td style="width:123px;">McMaster-Carr</td>
			<td style="width:117px;">8525T68</td>
			<td style="width:156px;">24&#34; x 24&#34;, 1/8&#34; Thick</td>
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		<tr height="49">
			<td height="49" style="height:49px;width:201px;">Pressure Vessel, Autoclave</td>
			<td style="width:123px;">Fluitron Inc.</td>
			<td style="width:117px;">8308-1788-U</td>
			<td style="width:156px;">5&#34; diameter, 1&#39; height</td>
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		<tr height="43">
			<td height="43" style="height:43px;width:201px;">High Purity Hydrogen Gas</td>
			<td style="width:123px;">Praxair</td>
			<td style="width:117px;">HY4.5</td>
			<td style="width:156px;">Grade 4.5, 5ppm O2, 5 ppm H20</td>
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		<tr height="43">
			<td height="43" style="height:43px;width:201px;">O2 Sensor</td>
			<td style="width:123px;">Advanced Micro Instruments</td>
			<td style="width:117px;">T2</td>
			<td style="width:156px;">0-5ppm min. range, 10,0000ppm max.</td>
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		<tr height="21">
			<td height="21" style="height:21px;width:201px;">Pre-purified Argon Gas</td>
			<td style="width:123px;">Oxarc</td>
			<td style="width:117px;">LCCO-HP818</td>
			<td style="width:156px;">High-purity, 99.998%</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:201px;">Liquid Dishwashing Detergent</td>
			<td style="width:123px;">McMaster-Carr</td>
			<td style="width:117px;">98365T89</td>
			<td style="width:156px;">32 oz pour bottle, lemon scented</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:201px;">Mildew Resistant Sponge</td>
			<td style="width:123px;">McMaster-Carr</td>
			<td style="width:117px;">7309T1</td>
			<td style="width:156px;">6&#34; long x 3 -1/2&#34; Wide x 1&#34; High, yellow</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:201px;">PTFE Pipe Thread Sealant Tape</td>
			<td style="width:123px;">McMaster-Carr</td>
			<td style="width:117px;">4591K12</td>
			<td style="width:156px;">1/2&#34; wide, white color</td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:201px;">Gas Tube Fittings</td>
			<td style="width:123px;">Swagelok</td>
			<td style="width:117px;">SS-400-1-4</td>
			<td style="width:156px;">1/4&#34; OD, stainless steel, male NPT threading</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:201px;">Hammer Driven Die</td>
			<td style="width:123px;">McMaster-Carr</td>
			<td style="width:117px;">3427A22</td>
			<td style="width:156px;">7/8&#34; Hammer driven hole punch</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:201px;">Linear Variable Differential Transformer</td>
			<td style="width:123px;">Omega</td>
			<td style="width:117px;">LD320-2.5&#160;</td>
			<td style="width:156px;">2.5mm, AC output, guided w/spring</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:201px;">Autoclave O-ring Seal</td>
			<td style="width:123px;">Fluitron Inc.</td>
			<td style="width:117px;">A-4511</td>
			<td style="width:156px;">Hastelloy C-276, 5-3/4&#34; OD x 5&#34; ID x 3/8&#34;</td>
		</tr>
		<tr height="105">
			<td height="105" style="height:105px;width:201px;">Torque Wrench</td>
			<td style="width:123px;">McMaster-Carr</td>
			<td style="width:117px;">85555A422</td>
			<td style="width:156px;">Adjustable Torque-Limiting Wrench, Quick-Release, 1/2&#34; Square Drive, 50-250 ft.-lbs. Torque</td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:201px;">Mallet</td>
			<td style="width:123px;">McMaster-Carr</td>
			<td style="width:117px;">5939A11</td>
			<td style="width:156px;">Hard and Extra-Hard Rubber Hammer, 2-1/4 lbs.</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:201px;">iLoad Mini Capacitive Load Sensor</td>
			<td style="width:123px;">Loadstar Sensors</td>
			<td style="width:117px;">MFM-050-050-S*C03</td>
			<td style="width:156px;">50 lb, U Calibration, 0.5% Accuracy, Steel</td>
		</tr>
	</tbody>
</table>

in situ high pressure hydrogen tribological testing of common polymer materials used in the hydrogen delivery infrastructure

众所周知, 高压氢气对压缩机、阀门、软管和驱动器的金属部件产生不利影响。然而, 对高压氢对聚合物密封和阻隔材料的影响的认识相对较少。为了确定在氢燃料输送基础设施的组分中发现的普通高分子材料与高压氢气的相容性, 需要进行更多的研究。因此, 重要的是考虑物理性能的变化, 如摩擦和磨损的就地, 而聚合物暴露在高压氢。在本协议中, 我们提出了一种用自定义内置的就地针平直线往复法测试 28 MPa 高压氢环境中的乙丙二烯单体 (EPDM) 弹性体试样的摩擦磨损性能的方法。摩擦.试验结果表明, 在高压氢气中, 三元乙丙橡胶试样与钢柜台表面的摩擦系数与相似的摩擦系数相比, 在周围的空气。

利用所提出的方法, 在高压氢环境下, 可以测量弹性试样的运动摩擦系数和磨损因数。图 1中提供的代表性数据表明, 在高压氢环境下, 在钢柜台表面下移动三元乙丙基聚合物试样需要更大的力。使用正常力 fN与摩擦力 fK之间的关系, 可以确定三元乙丙橡胶试样与钢球之间的摩擦系数, µ。此数据显示在图 2中, 其中?...

Watch this Scientific Journal Video about In Situ High Pressure Hydrogen Tribological Testing of Common Polymer Materials Used in the Hydrogen Delivery Infrastructure at JoVE.com

In Situ High Pressure Hydrogen Tribological Testing of Common Polymer Materials Used in the Hydrogen Delivery Infrastructure

介绍了用于氢基础设施服务的聚合物摩擦学性能量化的试验方法, 并讨论了常用弹性体的特性结果。

就地氢气输送基础设施用普通高分子材料的高压氢摩擦学试验

High pressure hydrogen gas is known to adversely affect metallic components of compressors, valves, hoses, and actuators. However, relatively little is ...

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Research

JoVE Journal

Engineering

In Situ High Pressure Hydrogen Tribological Testing of Common Polymer Materials Used in the Hydrogen Delivery Infrastructure

7.5K 次观看.  Pacific Northwest National Laboratory. 介绍了用于氢基础设施服务的聚合物摩擦学性能量化的试验方法, 并讨论了常用弹性体的特性结果。

视频: In Situ High Pressure Hydrogen Tribological Testing of Common Polymer Materials Used in the Hydrogen Delivery Infrastructure

Synthesis and Microdiffraction at Extreme Pressures and Temperatures

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary interiors, design materials with novel properties, understand the mechanical behavior of materials exposed to very high stresses as in explosions or impacts. Synthesis and structural analysis of materials at extreme conditions of pressure and temperature entails remarkable technical challenges. In the laser heated diamond anvil cell (LH-DAC), very high pressure is generated between the tips of two opposing diamond anvils forced against each other; focused infrared laser beams, shined through the diamonds, allow to reach very high temperatures on samples absorbing the laser radiation. When the LH-DAC is installed in a synchrotron beamline that provides extremely brilliant x-ray radiation, the structure of materials under extreme conditions can be probed in situ. LH-DAC samples, although very small, can show highly variable grain size, phase and chemical composition. In order to obtain the high resolution structural analysis and the most comprehensive characterization of a sample, we collect diffraction data in 2D grids and combine powder, single crystal and multigrain diffraction techniques. Representative results obtained in the synthesis of a new iron oxide, Fe4O5 1 will be shown.

The laser heated diamond anvil cell combined with synchrotron micro-diffraction techniques allows researchers to explore the nature and properties of new phases of matter at extreme pressure and temperature (PT) conditions. Heterogeneous samples can be characterized in situ under high pressure by 2D mapping and combined powder, single-crystal and multigrain diffraction approaches.

在极端的压力和温度的合成和Microdiffraction

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary ...

科研

工程学

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 ...

Printing Fabrication of Bulk Heterojunction Solar Cells and In Situ Morphology Characterization

Polymer-based materials hold promise as low-cost, flexible efficient photovoltaic devices. Most laboratory efforts to achieve high performance devices have used devices prepared by spin coating, a process that is not amenable to large-scale fabrication. This mismatch in device fabrication makes it difficult to translate quantitative results obtained in the laboratory to the commercial level, making optimization difficult. Using a mini-slot die coater, this mismatch can be resolved by translating the commercial process to the laboratory and characterizing the structure formation in the active layer of the device in real time and in situ as films are coated onto a substrate. The evolution of the morphology was characterized under different conditions, allowing us to propose a mechanism by which the structures form and grow. This mini-slot die coater offers a simple, convenient, material efficient route by which the morphology in the active layer can be optimized under industrially relevant conditions. The goal of this protocol is to show experimental details of how a solar cell device is fabricated using a mini-slot die coater and technical details of running in situ structure characterization using the mini-slot die coater.

Printing Fabrication of Bulk Heterojunction Solar Cells and In Situ Morphology Characterization

Here, we present a protocol to fabricate organic thin film solar cells using a mini-slot die coater and related in-line structure characterizations using synchrotron scattering techniques.

散装异质结太阳能电池的印刷和制作<em&gt;原位</em&gt;形态特征

Polymer-based materials hold promise as low-cost, flexible efficient photovoltaic devices. Most laboratory efforts to achieve high performance devices ...

Spark Plasma Sintering Apparatus Used for the Formation of Strontium Titanate Bicrystals

A spark plasma sintering apparatus was used as a novel method for diffusion bonding of two single crystals of strontium titanate to form bicrystals with one twist grain boundary. This apparatus utilizes high uniaxial pressure and a pulsed direct current for rapid consolidation of material. Diffusion bonding of strontium titanate bicrystals without fracture, in a spark plasma sintering apparatus, is possible at high pressures due to the unusual temperature dependent plasticity behavior of strontium titanate. We demonstrate a method for the successful formation of bicrystals at accelerated time scales and lower temperatures in a spark plasma sintering apparatus compared to bicrystals formed by conventional diffusion bonding parameters. Bond quality was verified by scanning electron microscopy. A clean and atomically abrupt interface containing no secondary phases was observed using transmission electron microscopy techniques. Local changes in bonding across the boundary was characterized by simultaneous scanning transmission electron microscopy and spatially resolved electron energy-loss spectroscopy.

A viable technique for the formation of strontium titanate bicrystals at high pressure and fast heating rate via the spark plasma sintering apparatus is developed.

放电等离子烧结设备中使用的钛酸锶双晶体的形成

A spark plasma sintering apparatus was used as a novel method for diffusion bonding of two single crystals of strontium titanate to form bicrystals with ...

Fabrication of Polymer Microspheres for Optical Resonator and Laser Applications

This paper describes three methods of preparing fluorescent microspheres comprising &#960;-conjugated or non-conjugated polymers: vapor diffusion, interface precipitation, and mini-emulsion. In all methods, well-defined, micrometer-sized spheres are obtained from a self-assembling process in solution. The vapor diffusion method can result in spheres with the highest sphericity and surface smoothness, yet the types of the polymers able to form these spheres are limited. On the other hand, in the mini-emulsion method, microspheres can be made from various types of polymers, even from highly crystalline polymers with coplanar, &#960;-conjugated backbones. The photoluminescent (PL) properties from single isolated microspheres are unusual: the PL is confined inside the spheres, propagates at the circumference of the spheres via the total internal reflection at the polymer/air interface, and self-interferes to show sharp and periodic resonant PL lines. These resonating modes are so-called "whispering gallery modes" (WGMs). This work demonstrates how to measure WGM PL from single isolated spheres using the micro-photoluminescence (&#181;-PL) technique. In this technique, a focused laser beam irradiates a single microsphere, and the luminescence is detected by a spectrometer. A micromanipulation technique is then used to connect the microspheres one by one and to demonstrate the intersphere PL propagation and color conversion from coupled microspheres upon excitation at the perimeter of one sphere and detection of PL from the other microsphere. These techniques, &#181;-PL and micromanipulation, are useful for experiments on micro-optic application using polymer materials.

Protocols for the synthesis of microspheres from polymers, the manipulation of microspheres, and micro-photoluminescence measurements are presented.

用于光学谐振器和激光应用的聚合物微球的制造

This paper describes three methods of preparing fluorescent microspheres comprising &#960;-conjugated or non-conjugated polymers: vapor diffusion, ...

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of lithium-ion (Li-ion) batteries. However, a number of setbacks prevent their integration into commercial devices. The main limiting factor is due to nanoscale phenomena occurring at the electrode/electrolyte interfaces, ultimately leading to degradation of battery operation. These key problems are highly challenging to observe and characterize as these batteries contain multiple buried interfaces. One approach for direct observation of interfacial phenomena in thin film batteries is through the fabrication of electrochemically active nanobatteries by a focused ion beam (FIB). As such, a reliable technique to fabricate nanobatteries was developed and demonstrated in recent work. Herein, a detailed protocol with a step-by-step process is presented to enable the reproduction of this nanobattery fabrication process. In particular, this technique was applied to a thin film battery consisting of LiCoO2/LiPON/a-Si, and has further been previously demonstrated by in situ cycling within a transmission electron microscope.

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

A protocol for the fabrication of electrochemically active LiPON-based solid-state lithium-ion nanobatteries using a focused ion beam is presented.

基于 LiPON 的固态锂离子 Nanobatteries 的聚焦离子束制备方法在原位测试中的研究

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of ...

Detecting the Water-soluble Chloride Distribution of Cement Paste in a High-precision Way

To improve the accuracy of the chloride distribution along the depth of cement paste under cyclic wet-dry conditions, a new method is proposed to obtain a high-precision chloride profile. Firstly, paste specimens are molded, cured, and exposed to cyclic wet-dry conditions. Then, powder samples at different specimen depths are grinded when the exposure age is reached. Finally, the water-soluble chloride content is detected using a silver nitrate titration method, and chloride profiles are plotted. The key to improving the accuracy of the chloride distribution along the depth is to exclude the error in the powderization, which is the most critical step for testing the distribution of chloride. Based on the above concept, the grinding method in this protocol can be used to grind powder samples automatically layer by layer from the surface inward, and it should be noted that a very thin grinding thickness (less than 0.5 mm) with a minimum error less than 0.04 mm can be obtained. The chloride profile obtained by this method better reflects the chloride distribution in specimens, which helps researchers to capture the distribution features that are often overlooked. Furthermore, this method can be applied to studies in the field of cement-based materials, which require high chloride distribution accuracy.

A protocol for obtaining a water-soluble chloride profile by using a high precision milling method is presented.

高精度水泥浆水溶氯分布的检测

To improve the accuracy of the chloride distribution along the depth of cement paste under cyclic wet-dry conditions, a new method is proposed to obtain a ...

Ultrasonic Fatigue Testing in the Tension-Compression Mode

Ultrasonic fatigue testing is one of a few methods which allow investigating fatigue properties in the ultra-high cycle region. The method is based on exposing the specimen to longitudinal vibrations on its resonance frequency close to 20 kHz. With use of this method, it is possible to significantly decrease the time required for the test, when compared to conventional testing devices usually working at frequencies under 200 Hz. It is also used to simulate loading of material during operation in high speed conditions, such as those experienced by components of jet engines or car turbo pumps. It is necessary to operate only in the high and ultra-high cycle region, due to the possibility of extremely high deformation rates, which can have a significant influence on the test results. Specimen shape and dimensions have to be carefully selected and calculated to fulfill the resonance condition of the ultrasonic system; thus, it is not possible to test the full components or specimens of arbitrary shape. Before each test, it is necessary to harmonize the specimen with the frequency of the ultrasonic system to compensate for deviations of the real shape from the ideal one. It is not possible to run a test until a total fracture of the specimen, since the test is automatically terminated after initiation and propagation of the crack to a certain length, when the stiffness of the system changes enough to shift the system out of the resonance frequency. This manuscript describes the process of evaluation of materials' fatigue properties at high-frequency ultrasonic fatigue loading with use of mechanical resonance at a frequency close to 20 kHz. The protocol includes a detailed description of all steps required for a correct test, including specimen design, stress calculation, harmonizing with the resonance frequency, performing the test, and final static fracture.

A protocol for ultrasonic fatigue testing in the high and ultra-high cycle region in axial tension-compression loading mode.

拉伸压缩模式下的超声疲劳试验

Ultrasonic fatigue testing is one of a few methods which allow investigating fatigue properties in the ultra-high cycle region. The method is based on ...

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 ...

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 ...