Name: high-pressure, high-temperature deformation experiment using the new generation griggs-type apparatus
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这项研究是献给哈利. 格林教授的记忆, 没有他, 这一切都是不可能的。我们还感谢 Jörg Renner 和 Sébastien 桑切斯在设计和实施该设备方面的影响, 以及安德烈 k. 古斯塔夫·克隆博格、凯勒 w 莲 III 和三名匿名审评员进行了卓有成效的讨论和评论。我们感谢 1月 Tullis 教我们和许多学生的基础和许多有用的技巧, 固体介质变形实验。这项研究由紧急救济 RHEOLITH (赠款 290864)、Labex 伏尔泰 (ANR-10-LABX-100-01)、Equipex PlaneX (ANR-11-EQPX-0036) 和情报局德尔夫 (ANR-12-JS06-0003) 提供资金。

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作者没有什么可透露的。

最初, 格雷型装置的设计是为了尽可能缓慢地进行变形实验, 以接近于其他技术的地质应变率,即, 超过几周, 数月甚至几年9。因此, 格雷型实验可以运行, 只要电源和水冷却功能, 特别是一夜没有操作员是需要的。如前所述, 格雷机还可以探索岩石圈中所遇到的压力和温度的大部分范围。然而, 这种技术目前受到一些限制, 可能会降低应力确定的准确性。
格雷型实验的成功依赖于几个关键点, 主要包括热电偶鞘的质量、填料环的形状和剪切活塞的对准 (仅用于一般剪切实验)。事实上, 热电偶线应该是很好的绝缘彼此和从限制介质 (NaCl)。否则, 温度记录可以通过接触样品室外的两根导线进行修改, 导致温度急剧升高 (这可能会破坏压力容器), 或者热电偶可能破裂, 实验失败。.每个填料环的顶面 (σ1和σ3) 应该是平坦和足够大 (大约半毫米)。这是必要的, 以避免任何铅泄漏在压力增加。对于一般剪切试验, 顶部和底部的剪切活塞应完全对准, 这样在实验过程中不会发生非对称变形。如果没有, 样品可能会接触到的限制介质通过夹克泄漏, 造成可能的污染和样品失败。此外, 如果不及早停止变形活塞, 一般剪切试验中可能会出现这样的夹克泄漏。铂金夹克在没有任何断裂的情况下变形的能力可能会因实验而异。然而, 虽然剪切变形已经达到了超过伽玛 = 7 在2毫米厚度的样品 (一个例子是在 Heilbronner 和 Tullis24), 伽玛 = 5 是常规应用的一个良好的成功率和显着更高的剪切通过降低试样厚度可以达到应变。
目前, 格雷压力机受摩擦效应的影响, 降低了应力测量的准确度, 特别是当 "命中点" 由曲线拟合定义时。大部分摩擦力发生在变形活塞通过σ1填料环、铅片和围介质 (NaCl) 推进时。在变形阶段的 "运行" 步骤 (图 9) 中, 也可以从应力-时间曲线中看到这一点, 而且在命中点后加载过程中也是如此。当弹性行为不依赖于试样刚度时, 加载曲线的斜率随试样强度的增加而增大, 格雷型装置。这主要是由于非弹性试样应变, 而σ1活塞推动通过铅。事实上, 屈服应力条件前的载荷曲线斜率并不代表样品的纯弹性载荷, 而是包括摩擦和一些试样变形/压实的不同组分的组合。不幸的是, 这种类型的行为是难以重现的, 因为它取决于样品强度, 这是在高温低, 和摩擦引起的误差, 强烈变化, 从3到 9%18。一些其他较弱的材料, 如铟, 铋或锡已被使用, 而不是铅19, 但它们总是导致一些泄漏的压力高于 1 GPa。另外, 虽然公里尺度对象和非常缓慢的应变率 (10-15-10-12 s-1) 需要考虑为地质目的, 格雷类型仪器象任何其他变形仪器-在样品大小方面是有限的 (最大.格雷压力机直径为8毫米) 和应变率 (最小 10-8 s-1)。这些地质条件确实需要不切实际的力量和不切实际的试验时间。然而, 变形试验与地质环境之间的这一不可避免的差距可能会被数值模型部分取代, 前提是实验室的机械定律通过推断是完全有效的。这肯定需要开发更准确的高压装置, 至少与气体压力介质类型的设备 (即, 1 MPa) 一样好。
目前, 只有气体介质设备的精度足以进行流变实验, 而现有的大多数机械定律都来自于 0.3 GPa 的围压。应力测量的高精度主要依赖于承受围压的内部负载单元的存在, 与外部的压力容器的存在形成对比的是, 它与一个仅承受房间压强的外在压力, 以及它与气体压船的结合, 允许应用一个不能像它一样转移到固体介质中的压力机的特定设计。今天, 固体介质设备只使用外部负载单元--其中一些甚至没有任何负载单元--来测量微分应力, 导致分辨率差, 并且由于摩擦力而大幅高估。
在格雷型装置中, 熔融盐组件的使用可以显著减少试样周围的摩擦力 (系数为 3)。但如前所述, 它也引起了进一步的问题, 而应力测量的准确度仍然比百德新仪器低10倍。另一种方法将包括实现内部负载单元, 或类似的东西, 以摆脱在格雷压力机的摩擦效应。考虑到 "常规" 负载单元的大小和容量, 如在工业中发现的, 在压力容器的取样室中加入其中一些似乎不切实际。它们无法维持围压和高容量的负载单元 (最大 200 kN), 例如格雷型仪器中高压实验所需的, 而且它们太大, 不能包含在样品室中。然而, 有一种可能意味着将样本柱的基底活塞作为内部负载单元25, 但前提是它的变形可以精确测量 (安德烈 k. 古斯塔夫·克隆博格, 个人通信)。这需要在基板下面有一个房间来适应特定的负载单元, 这在新的格雷类型设备 (图 1) 中已经被预期。但今天, 在固体介质变形装置中, 这种内部载荷细胞仍有待实现。

岩石变形是最重要的地质过程之一。它强烈地助长了人为时间尺度的现象, 如地震或山体滑坡, 同时也影响了大地行星上固体外壳的大规模运动, 包括地球上的板块构造1。例如, 根据壳状岩石圈的流变性, 它定义了地壳和亚固溶体地幔的强度 (1200 °c), 板块构造和相关特征的方案可能会有显著变化<img alt="Equation" src="/files/ftp_upload/56841/56841eq1.jpg"> 2,3 ,4,5。一方面, 需要有一个强大的最上层地幔和/或下部地壳, 以维持山脉或稳定俯冲带6。但另一方面, 数值模型也表明, 如果岩石圈太强, 板块边界不能从地幔对流中发展, 从而导致在金星7上观察到的刚性盖子行为。因此, 岩石流变学所规定的岩石圈强度直接控制着活动行星的板块状行为。
半个多世纪以来, 岩石流变学研究在高温 (> 300 °c), 产生了最先进的技术, 主要是不同的压力范围, 他们可以达到。这包括在相对较低的压力下 (< 0.5 GPa)、固态介质格雷型设备9、10、11在中间到高压 (0.5-5 gpa) 中的气中百德比型设备8 , 以及变形-直径仪器12,13 (DDia:20 gpa) 或金刚石铁砧细胞在非常高压14 (由超过 100 GPa)。因此, 在深部地球上遇到的压力和温度现在可以通过实验来实现。然而, 岩石变形也依赖于需要测量精度高、精度较高的微分应力, 从而可以形成本构关系。多亏了它的气体限制介质, 帕特森的仪器今天是唯一能够进行应力测量的技术, 具有足够的精度 (1 兆帕), 以推断数据超过6级的应变率, 但它只能探索变形在低压力下的过程。相反, 固体介质装置可以在高压下使岩石变形, 但应力测量精度较低。虽然格雷型仪器15、16的压力精度估计为30兆帕斯卡, 但基于同步加速器的 DDia 产生的机械定律的误差超过了 # 100 MPa17。在格雷型设备中, 在帕特森一15中, 应力测量也可能被高估36%。在高压力和高温下进行精确精确的应力测量, 这仍然是地球科学中的一大挑战。
除了在压力可能超过 5 GPa 的深层俯冲板之外, 格雷型设备目前是研究压力 (< 4 gpa) 和温度 (1200 °c) 中的变形过程的更合适的技术, 在很大程度上是<img alt="Equation" src="/files/ftp_upload/56841/56841eq1.jpg">岩石圈.在此基础上, 在1990进行了重大的努力, 以改善应力测量, 特别是减少摩擦效应, 在示例11,18周围使用共晶盐混合物作为围介质。这样的熔融盐组件提高了应力测量的准确度, 将误差从30减至10兆帕斯卡15,19, 但应用此类程序集时遇到其他缺点。它们的成功率低得多, 执行非同轴 (剪切) 实验的难度很大, 更复杂的样品组装。此外, 应力测量的准确度仍然比低压帕特森型设备低十倍。这些问题限制了格雷型装置对流变过程的定量化, 目前在研究变形过程及其相关显微结构方面的应用更为普遍。因此需要一种新的方法来在高岩石圈压力下进行流变量化。
本文详细介绍了采用新设计的固体介质格雷型装置进行高压变形实验的 "常规" 程序。在在ISTO (奥尔良、法国) 和存在 (法国巴黎) 实施的新的 "格雷" 实验室框架内, 主要目的是详细说明议定书的每一步, 以便所有领域的科学家能够决定仪器是否适合或不符合他们的学习目的。还讨论了这种先进技术的关键步骤和局限性, 以及新的方法和可能的未来发展。
新型格雷型装置
基于活塞缸技术, 格雷型设备以前是由 David t 格雷在1960的9中设计的, 然后由哈利 w 绿色在1980的11中进行修改 (主要是为了在变形过程中获得更高的压力。实验)。在这两种情况下, 格雷设备的特点是金属框架, 包括: 1) 三水平压台安装在垂直列, 2) 一个主液压缸 (围压 ram) 悬浮到中间板和 3) 变形齿轮箱和活塞/执行器固定在上部压板的顶部 (图 1)。"约束" ram 和变形执行器分别连接到独立活塞, 将力传递到压力容器内的试样组件。有了这样的容器, 变形可以达到2或 5 GPa 的限制压力, 这取决于样品装配的仪器和直径。
由于电阻炉, 样品温度增加焦耳效应 (高达≈1300°c20), 而压力容器是水冷的顶部和底部。在格林的设计中, 格雷设备还包括一个端负荷系统, homogenizes 压力容器中的预应力 (图 1)。这允许在更高的压力下实现变形实验 (最高 5 GPa), 特别是在压力容器中使用一个小孔。有关格雷新闻的详细信息, 读者可参考 Rybacky et 等对修改后的格雷设备设计的优秀描述。19。
由于de 奥尔良(ISTO、法国) 和高等师范学校高等 de 巴黎(法国巴黎) 之间的密切协作, 新一代格雷型设备直接基于 H 的设计。.w 绿色11, 但已进行了一些改进, 以符合欧洲高压试验安全标准。在这台新的压力机, 限制和变形执行器由伺服控制的液压注射器泵驱动, 使有可能在高压下进行恒定负载或恒定位移实验 (高达 5 GPa)。使用油压传感器、负载单元 (最大 200 kN) 和位移传感器 (图 1) 分别对围 (静压) 压力、力和位移进行监测。压力容器是由内部碳化钨 (WC) 芯插入1°圆锥钢环和预应力使用带状缠绕技术21。对于传输力, 压力容器和试样总成位于 WC-可移动活塞之间, 其中包括变形活塞 (σ1)、限制活塞 (σ3)、端部负载活塞和底板 (图 1)。与压力容器的顶部和底部的常规冷却一起, 水流经钢容器周围的碳化钨核心在6毫米直径孔, 以更好地冷却 (图 1)。硅油流量也冷却了围压液压缸。此外, 奥尔良中的变形装置采用较大的试样尺寸, 直径可达8毫米, 因此 1) 的显微组织可以更好地开发, 2) 格雷出版社和帕特森出版社分享一个共同的样本维度, 用于未来的比较。这需要增加压力容器中 WC 孔的直径 (27 毫米, 而不是1英寸, 即25.4 毫米), 从而将最大可达到的压力降低到 3 GPa。
本文介绍了用新的格雷型装置进行实验的过程, 包括用氧化铝活塞 (图 2A和 2B) 组成常规的固体盐试样组件的所有部件的描述. ), 以及连续的步骤来生产它们并将它们引入压力容器中。这个描述在大部分跟随了在许多岁月被开发的惯例由教授 1月 Tullis 并且同事在布朗大学 (罗德岛, 美国)。所得到的样品装配是完全适当的, 以执行共轴 (纯剪切) 或非同轴 (一般剪切) 变形实验的整个范围的压力和温度的格雷型设备。虽然纯剪切实验通常需要一定长度的芯钻样本 (通常是试样直径的≈2倍), 但一般剪切变形通常适用于45°到活塞轴的区域切割 (图 2B)。样品材料可以是核心样品的切片或选择晶粒尺寸的细粒粉。所有零件都包裹在一个金属箔和套在铂管焊接 (或折叠平) 两侧。通常使用 s 型 (Pt90%Rd10%合金) 或 K 型 (镍合金) 热电偶对温度进行监视, 但仅在此处描述了使用莫来石2孔护套管制备 s 型热电偶的方法 (图 2C)。

<table><tbody><tr><td>Griggs-type apparatus</td><td>Sanchez Technologies (Corelab)</td><td>TRI-X 6/1500 SD</td><td>Solid-medium Griggs-type deformation apparatus</td></tr><tr><td></td><td>Sanchez Technologies (Corelab)</td><td>Stigma pumps 1000/300 and 100/1500</td><td>hydraulic syringe pumps to apply pressure</td></tr><tr><td>Arbor press</td><td>Schiltz</td><td>PA.WZ.5000.530</td><td>Arbor press required to insert the sample assembly into the pressure vessel</td></tr><tr><td>Low-speed saw</td><td>Presi</td><td>Mecatome T180</td><td>Law-speed saw to cut alumina piston and mullite sheath</td></tr><tr><td></td><td>Presi</td><td>LR02033</td><td>Diamond saw blade</td></tr><tr><td>40 tons hydraulic press</td><td>CompaC</td><td>APA 9040EH1-D</td><td>40-ton hydraulic press to press salt/lead pieces and extract the sample</td></tr><tr><td>Pressure vessel (and pistons)</td><td>STRECON</td><td>vessel A4071&amp;nbsp;</td><td>Inner tungsten-carbide core inserted into a 1&amp;deg; conical steel ring and pre-stressed using the strip winding technique</td></tr><tr><td></td><td>STRECON</td><td>Deformation piston</td><td>Tungsten carbide piston to apply deformation</td></tr><tr><td></td><td>STRECON</td><td>Confining piston</td><td>Tungsten carbide piston to apply confining pressure</td></tr><tr><td></td><td>STRECON</td><td>End-load piston</td><td>Tungsten carbide piston to pre-stress the pressure vessel</td></tr><tr><td>PUK U3</td><td>Lampert</td><td>PUK 5 welding microscope</td><td>Fine welding system to weld the thermocouple and platinum jacket</td></tr><tr><td>Cooling system Ultracool</td><td>Lauda</td><td>UC 4 E1 PI5 SR BSP &amp;deg;C</td><td>Cooler for the pressure vessel</td></tr><tr><td></td><td>Lauda</td><td>Proline RP850</td><td>Cooler for the confining/end-load ram</td></tr><tr><td>Leath</td><td>Schneider electric</td><td>Eurotherm 2704</td><td>Temperature controller</td></tr><tr><td>Milling machine</td><td>Enerpac</td><td>P-142</td><td>Hand pump to lift up the confining/end-load ram</td></tr><tr><td></td><td>HBM</td><td>1-P3TCP/2000 bar</td><td>Pressure transducer</td></tr><tr><td></td><td>HBM</td><td>1-P3TCP/500 bar</td><td>Pressure transducer</td></tr><tr><td></td><td>HBM</td><td>WA/10 mm</td><td>Displacement transducer</td></tr><tr><td></td><td>HBM</td><td>WA/50 mm</td><td>Displacement transducer</td></tr><tr><td></td><td>HBM&amp;nbsp;</td><td>1-C2/200 kN</td><td>Load cell</td></tr><tr><td></td><td>Geoscience instrument</td><td></td><td>Graphite furnace: graphite tube inserted between two pyrophyllite sleeves (custom-made)</td></tr><tr><td></td><td>McDanel</td><td>MRD028330018858</td><td>Mullite Round Double Bore Tubing</td></tr><tr><td></td><td>Morgan Advanced Materials</td><td>WH-Feuerfestkitt</td><td>Ceramic glue</td></tr><tr><td></td><td>PRECIS</td><td>T90 L</td><td>Lathe</td></tr><tr><td></td><td>NSK</td><td>EM-255</td><td>Diamond tool to parallelize alumina piston using the lathe</td></tr><tr><td></td><td>Mecanelec</td><td>CDM &amp;ndash; IP 1 &amp;ndash; 5L/mn</td><td>Flow meter for water cooling (pressure vessel)</td></tr><tr><td></td><td>Hedland</td><td>H602A-0005-F1</td><td>Flow meter for oil cooling (confining/end-load ram)</td></tr><tr><td></td><td>Legris</td><td>S&amp;eacute;rie 21</td><td>double-self-sealing coupler for tube of the water cooling system</td></tr><tr><td></td><td>Corelab</td><td>Falcon</td><td>Software to monitor the hydraulic syringe pumps</td></tr><tr><td></td><td>HBM</td><td>CatmanEasy-HP</td><td>Software to record data</td></tr><tr><td></td><td>Schneider electric</td><td>Eurotherm itools</td><td>Software to set programs for the temperature controller</td></tr><tr><td></td><td>VWR</td><td>410-0114</td><td>Ceramic mortar</td></tr><tr><td></td><td>VWR</td><td>231-2322</td><td>Microspatule</td></tr><tr><td></td><td>VWR</td><td>459-0206</td><td>Ceramic recipient</td></tr><tr><td></td><td>VWR</td><td>AnalaR NORMAPUR 27810.364</td><td>Sodium Chloride 99.9% purity</td></tr><tr><td></td><td>VWR</td><td>Barnstead/Thermoline 48000 furnace</td><td>Benchtop Muffle furnace for melting lead</td></tr><tr><td></td><td>DP/Pr&amp;eacute;cision</td><td>Custom made</td><td>Tools needed to produce the salt and lead pieces</td></tr><tr><td></td><td>Cincinnati</td><td>TYPE PE-5</td><td>Milling machine</td></tr><tr><td></td><td>Memmert</td><td>UNB 400</td><td>Oven to stock salt powder and salt pieces</td></tr><tr><td></td><td>Otelo</td><td>Otelo 65220023</td><td>Tubing cutter for Platinum</td></tr><tr><td></td><td>Otelo</td><td>BAITER 51600202</td><td>File tool</td></tr><tr><td></td><td>Otelo</td><td>VADIUM 65172600</td><td>Diagional micro-cutter</td></tr><tr><td></td><td>Otelo</td><td>VADIUM 65172620</td><td>Flat needle nose micro-pliers</td></tr><tr><td></td><td>SAM</td><td>EMP-13J</td><td>Round screw hollow punch</td></tr><tr><td></td><td>Professional Platic</td><td>Chemfluor MFA Tube</td><td>Minitube for isolating thermocouple wires</td></tr><tr><td></td><td>Radiospar</td><td>RS 370-6717</td><td>S-type flat pin thermocouple connector</td></tr><tr><td></td><td>LEMER</td><td></td><td>Lead (bulk)</td></tr><tr><td></td><td>Goodfellow</td><td>FP301305</td><td>Polyt&amp;eacute;trafluoro&amp;eacute;thyl&amp;egrave;ne - Film ; 0.15 mm thickness</td></tr><tr><td></td><td>Heraeus</td><td>81128696</td><td>Pure Platinum wire</td></tr><tr><td></td><td>Heraeus</td><td>81128743</td><td>Platinum90%/Rhodium10% wire</td></tr><tr><td></td><td>Alfa Aesar</td><td>M11C056</td><td>Nickel foil 0.025 thickness annealed 99.5%</td></tr><tr><td></td><td>DP/precision</td><td></td><td>Tools to produce the salt pieces and lead piece (custom-made)</td></tr><tr><td></td><td>Polyco Bodyguards</td><td>GL890</td><td>Blue Nitrile Medical Examination gloves</td></tr></tbody></table>

high-pressure, high-temperature deformation experiment using the new generation griggs-type apparatus

为了在很大的深度处理地质过程, 最好在高压下 (> 0.5 GPa) 和高温 (> 300 °c) 测试岩石变形。然而, 由于目前的固体压力介质装置的低应力分辨率, 高分辨率测量目前仅限于气体压力介质中低压变形实验。本文介绍了新一代固体介质活塞缸 ("格雷型") 装置。能够执行高达 5 GPa 的高压变形实验, 并为适应内部负载单元而设计, 这种新型仪器为高压流变学的建立提供了技术基础。本文提供了以视频为基础的程序详细文档 (使用 "常规" 的固态盐组件) 进行高压、高温实验, 采用新设计的格雷型装置。此外, 还给出了一个在700°c、1.5 GPa 和 10-5 s-1中变形的卡拉拉大理石试样的代表性结果。相关的应力-时间曲线说明了格雷型实验的所有步骤, 从增加压力和温度到试样淬火等变形停止。并结合未来的发展, 讨论了格雷装置的关键步骤和局限性。

图 9显示了由新一代格雷型设备在卡拉拉大理石 (8 mm 长核心样品) 的纯剪切 (共轴) 变形过程中产生的应力-时间曲线的示例, 其应变速率为 10-5 s-1, 温度为700°c 和 1.5 GPa 的围压。在这样的实验中, 压力和温度都首先增加 alternatingly, 主要是防止 NaCl 融化。熔融氯化钠对样品具有很强的腐蚀性, 可能不可逆转地损坏热电偶。沿着不断增加的压力和温度的步骤-这里称为 "泵浦阶段" (图 9) –铅片具有防止样品变形的功能, 将应力从σ1转移到σ3。和相反, 在示例组件中保持或多或少的均衡应力状态。
当目标压力和温度达到时, 可以采用 "热压" 的时期。尽管可选, 这一步骤 (通常为24小时) 可能需要在变形前烧结样品粉末, 如果适用。σ1活塞/执行器然后被推进变形样品, 导致所谓的 "变形阶段"。后者的特点是, 微分应力的陡向温和增加 (σ1 -σ3), 这是由于摩擦引起 1) 填料环和 2) 在σ1活塞和铅片之间的接触面增加当σ1正通过引线移动时。此 "运行" 部分应具有足够的持续时间, 以便通过曲线拟合 (图 9) 精确确定命中点 (σ1活塞和顶部氧化铝活塞之间的接触)。为此, 在开始推进σ1之前, 必须在σ1活塞和氧化铝活塞之间有显著的引线厚度 (≥2毫米)。当接近顶部氧化铝活塞时, 铅的挤压速度快于薄试样厚度, 导致铅中的应变硬化, 并促进渐进应力增加, 直到σ1活塞推上样品柱。应力曲线然后急剧上升到屈服应力条件, 理论上定义从弹性到塑性行为的转变 (图 9)。根据需要定义微分应力, 实验的命中点随后从 "弹性" 曲线和 "运行" 曲线的扩展之间的交集中推断出来 (图 9)。
当变形最终停止时, 温度会迅速下降 (≈300摄氏度/分钟) 以保持显微组织。在 "样品淬火" 过程中, 一定会产生大量的压力, 但在这一下降之后, σ1和σ3活塞在液压公羊 (≈ 5 MPa/分钟) 的压力下缓慢地向后移动。这是限制卸荷裂缝形成的必要条件, 虽然有些裂缝是不可避免的。实验后, 应力-时间曲线随后被修正, 以产生从命中点起变形试样的应力应变曲线 (参见图 9中的插入)。这些修正包括 1) 设备的刚度/扩展和 2) 由填料环和引线片引起的摩擦力15,19。图 10还显示了实验后示例程序集的两个示例, 一个包含卡拉拉大理石的核心样本 (图 10A和10B), 另一个是橄榄粉烧结的第二个, 然后在900摄氏度的一般剪切中变形。和 1.2 GPa 使用前格雷型设备23 (图 10C和10D)。
<img alt="Figure 1" class="xfigimg" src="/files/ftp_upload/56841/56841fig1.jpg"> 图 1: 新一代格雷型设备.现在可在格雷奥尔良(ISTO、法国) 和高等师范学校高等 de 巴黎(巴黎, 法国) 提供的新型仪器的示意图。当试样装配位于压力容器内时, 独立的注射器泵通过液压公羊和活塞/执行器来应用高围压和差动应力。通过电阻石墨炉从组件下方注入低电压/高电流电流 (见侧面视图), 温度增加。为保持碳化钨 (WC) 模具, 压力容器也冷却的水流从底部到顶部通过冷却板/箱和容器本身。<a href="https://cloudflare-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/56841/56841fig1large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 2" class="xfigimg" src="/files/ftp_upload/56841/56841fig2.jpg"> 图 2: 示例程序集.构成示例程序集的片断的详细视图。σ1活塞, σ3活塞和基板也显示-其中的一部分, 在透明度-以找到每一块的位置, 关于格雷型设备。A)同轴实验的示例程序集。B)示例程序集的分解视图, 可用于 "同轴" (白色) 或 "常规剪切" 示例 (绿色)。铅片和下盐片以透明度显示。C) 3D 视图, 用于在实验期间监视温度的莫来石2孔护套 S 型热电偶。WC = 碳化钨。<a href="https://cloudflare-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/56841/56841fig2large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 3" class="xfigimg" src="/files/ftp_upload/56841/56841fig3.jpg"> 图 3: 冷压从 NaCl 粉中的外、内盐片所需的工具.A) 3D 在冲压过程中的视图 (三十年代14吨) 和提取外盐件 (左), 以及相关工具组件的缩放绘图 (右)。B) 3D 在冲压过程中的视图 (三十年代6吨) 和提取内盐片 (左), 以及相关工具组件 (右) 的缩放绘图。有些部分以透明度显示。<a href="https://cloudflare-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/56841/56841fig3large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 4" class="xfigimg" src="/files/ftp_upload/56841/56841fig4v2.jpg"> 图 4: 钻下外层盐片所需的工具.A) 3D 视图 (顶部) 和 (底部) 钻孔。B)缩放工具的绘图 (3D、顶部和侧面视图) (仅显示一个部件)。<a href="https://cloudflare-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/56841/56841fig4large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 5" class="xfigimg" src="/files/ftp_upload/56841/56841fig5.jpg"> 图 5: 生产白金夹克所需的工具.A) 3D 视图 (左) 和缩放绘图 (右) 用于生产铂杯的工具。通过推上10毫米直径的铂盘, 其外部部分弯曲超过1毫米的厚度成一个杯子形状, 使它可以适应和被焊接在一起与8毫米直径白金夹克。B) 3D 视图 (顶部) 和缩放绘图 (底部), 用于将铂金杯焊接至铂金夹克 (仅显示顶部部分的一半)。<a href="https://cloudflare-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/56841/56841fig5large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 6" class="xfigimg" src="/files/ftp_upload/56841/56841fig6.jpg"> 图 6: 生成引线片所需的工具.A) 3D 在冲压过程中 (4 吨三十年代) 的熔融铅 (50 克) 的视图。组件 #2 以透明显示。B) 3D 视图在提取引线片断期间 (尺寸显示在左上图中)。C)缩放工具组件的绘图。<a href="https://cloudflare-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/56841/56841fig6large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 7" class="xfigimg" src="/files/ftp_upload/56841/56841fig7v2.jpg"> 图 7: 将基活塞固定在压力容器上的夹具.3D. 压力容器、基活塞和夹具 (顶部) 的视图, 以及一个夹具顶部和底部的缩放图, 包括3D 视图 (底部)。<a href="https://cloudflare-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/56841/56841fig7large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 8" class="xfigimg" src="/files/ftp_upload/56841/56841fig8.jpg"> 图 8: 水泵和冷却系统的水力学.液压系统的方案, 包括阀门 (V), 电阀 (EV) 和油箱 (T) –变形泵 (紫色)、围泵 (橙色)、压力容器 (浅蓝色) 的冷却系统和围/端负载 ram (黄色) 的冷却系统。<a href="https://cloudflare-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/56841/56841fig8large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 9" class="xfigimg" src="/files/ftp_upload/56841/56841fig9.jpg"> 图 9: 代表性结果.用新一代格雷型装置进行变形试验的应力-时间曲线实例。本实验是在卡拉拉大理石的核心样品 (8 毫米长) 上进行的, 同轴地700摄氏度, 1.5 GPa, 应变率为10 -5s-1。这一结果说明了格雷型实验的后续步骤, 其中包括 1) 一个 "抽放阶段", 以增加压力和温度, 2) 一个 "热压阶段" 烧结样品, 如果适用, 3) 一个 "变形阶段" 变形的样品, 和 4)"淬火阶段", 以减少压力和温度。在变形过程中, σ1活塞首先通过引线 ("运行" 步骤) 向前推进, 然后推上氧化铝活塞以正确地变形试样 (从命中点起), 从而产生弹性然后塑性行为 (见文本)。在修正了应力-时间曲线从摩擦和刚度/延伸的设备, 一个应力-应变曲线产生了从命中点 (插入)。σ1 = 由σ1活塞应用的应力;σ3 = 由σ3活塞应用的应力;P = 围 (等静) 压力;T = 温度。σ1-σ3 = 微分应力。<a href="https://cloudflare-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/56841/56841fig9large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 10" class="xfigimg" src="/files/ftp_upload/56841/56841fig10.jpg"> 图 10: 抽取示例.A)在图 9中描述的实验之后提取的示例程序集的下部部分。B)在新的格雷型设备中, 在700°c 和 1.5 GPa 的纯剪切变形后, 卡拉拉大理石 (仍然包裹在其白金夹克中) 的样品。C)下部分样品组件, 其中包含一个烧结橄榄粉样品, 然后在一般剪切900°c 和 1.2 GPa 上变形, 与前格雷型装置23。D)橄榄石样品和氧化铝剪切活塞 (仍然包裹在铂金夹克) 后从样品组装提取。TC = 热电偶。<a href="https://cloudflare-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/56841/56841fig10large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>

Watch this Scientific Journal Video about High-pressure, High-temperature Deformation Experiment Using the New Generation Griggs-type Apparatus at JoVE.com

High-pressure, High-temperature Deformation Experiment Using the New Generation Griggs-type Apparatus

岩石变形需要在高压下进行量化。本文介绍了一种新设计的固体介质格雷型装置的变形实验过程。这为未来的流变学研究提供了技术基础, 其压力可达 5 GPa。

新一代格雷型装置高压高温变形试验

In order to address geological processes at great depths, rock deformation should ideally be tested at high pressure (&#62; 0.5 GPa) and high temperature ...

high-pressure-high-temperature-deformation-experiment-using-new

Research

Education

JoVE Core

JoVE Journal

Mechanical Engineering

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Unit 1

Deflection of Beams

SCIENTISTS IN ACTION

18.7K 次观看.  Université d’Orléans. 岩石变形需要在高压下进行量化。本文介绍了一种新设计的固体介质格雷型装置的变形实验过程。这为未来的流变学研究提供了技术基础, 其压力可达 5 GPa。

视频: High-pressure, High-temperature Deformation Experiment Using the New Generation Griggs-type Apparatus

Simulation of the Planetary Interior Differentiation Processes in the Laboratory

A planetary interior is under high-pressure and high-temperature conditions and it has a layered structure. There are two important processes that led to that layered structure, (1) percolation of liquid metal in a solid silicate matrix by planet differentiation, and (2) inner core crystallization by subsequent planet cooling. We conduct high-pressure and high-temperature experiments to simulate both processes in the laboratory. Formation of percolative planetary core depends on the efficiency of melt percolation, which is controlled by the dihedral (wetting) angle. The percolation simulation includes heating the sample at high pressure to a target temperature at which iron-sulfur alloy is molten while the silicate remains solid, and then determining the true dihedral angle to evaluate the style of liquid migration in a crystalline matrix by 3D visualization. The 3D volume rendering is achieved by slicing the recovered sample with a focused ion beam (FIB) and taking SEM image of each slice with a FIB/SEM crossbeam instrument. The second set of experiments is designed to understand the inner core crystallization and element distribution between the liquid outer core and solid inner core by determining the melting temperature and element partitioning at high pressure. The melting experiments are conducted in the multi-anvil apparatus up to 27 GPa and extended to higher pressure in the diamond-anvil cell with laser-heating. We have developed techniques to recover small heated samples by precision FIB milling and obtain high-resolution images of the laser-heated spot that show melting texture at high pressure. By analyzing the chemical compositions of the coexisting liquid and solid phases, we precisely determine the liquidus curve, providing necessary data to understand the inner core crystallization process.

The high-pressure and high-temperature experiments described here mimic planet interior differentiation processes. The processes are visualized and better understood by high-resolution 3D imaging and quantitative chemical analysis.

模拟行星内部分化过程中的实验室

A planetary interior is under high-pressure and high-temperature conditions and it has a layered structure. There are two important processes that led to ...

科研

工程学

Metal-silicate Partitioning at High Pressure and Temperature: Experimental Methods and a Protocol to Suppress Highly Siderophile Element Inclusions

Estimates of the primitive upper mantle (PUM) composition reveal a depletion in many of the siderophile (iron-loving) elements, thought to result from their extraction to the core during terrestrial accretion. Experiments to investigate the partitioning of these elements between metal and silicate melts suggest that the PUM composition is best matched if metal-silicate equilibrium occurred at high pressures and temperatures, in a deep magma ocean environment. The behavior of the most highly siderophile elements (HSEs) during this process however, has remained enigmatic. Silicate run-products from HSE solubility experiments are commonly contaminated by dispersed metal inclusions that hinder the measurement of element concentrations in the melt. The resulting uncertainty over the true solubility and metal-silicate partitioning of these elements has made it difficult to predict their expected depletion in PUM. Recently, several studies have employed changes to the experimental design used for high pressure and temperature solubility experiments in order to suppress the formation of metal inclusions. The addition of Au (Re, Os, Ir, Ru experiments) or elemental Si (Pt experiments) to the sample acts to alter either the geometry or rate of sample reduction respectively, in order to avoid transient metal oversaturation of the silicate melt. This contribution outlines procedures for using the piston-cylinder and multi-anvil apparatus to conduct solubility and metal-silicate partitioning experiments respectively. A protocol is also described for the synthesis of uncontaminated run-products from HSE solubility experiments in which the oxygen fugacity is similar to that during terrestrial core-formation. Time-resolved LA-ICP-MS spectra are presented as evidence for the absence of metal-inclusions in run-products from earlier studies, and also confirm that the technique may be extended to investigate Ru. Examples are also given of how these data may be applied.

We present a procedure to determine the metal-silicate partitioning of siderophile elements, emphasizing techniques that suppress the formation of metal inclusions in experiments for the noble metals. The results of these experiments are used to demonstrate the effect of core-formation on the highly siderophile element composition of the mantle.

金属硅酸盐分区在高压和高温:实验方法和协议，以抑制高亲铁元素元素夹杂物

Estimates of the primitive upper mantle (PUM) composition reveal a depletion in many of the siderophile (iron-loving) elements, thought to result from ...

化学

High-Sensitivity Nuclear Magnetic Resonance at Giga-Pascal Pressures: A New Tool for Probing Electronic and Chemical Properties of Condensed Matter under Extreme Conditions

Nuclear Magnetic Resonance (NMR) is one of the most important techniques for the study of condensed matter systems, their chemical structure, and their electronic properties. The application of high pressure enables one to synthesize new materials, but the response of known materials to high pressure is a very useful tool for studying their electronic structure and developing theories. For example, high-pressure synthesis might be at the origin of life; and understanding the behavior of small molecules under extreme pressure will tell us more about fundamental processes in our universe. It is no wonder that there has always been great interest in having NMR available at high pressures. Unfortunately, the desired pressures are often well into the Giga-Pascal (GPa) range and require special anvil cell devices where only very small, secluded volumes are available. This has restricted the use of NMR almost entirely in the past, and only recently, a new approach to high-sensitivity GPa NMR, which has a resonating micro-coil inside the sample chamber, was put forward. This approach enables us to achieve high sensitivity with experiments that bring the power of NMR to Giga-Pascal pressure condensed matter research. First applications, the detection of a topological electronic transition in ordinary aluminum metal and the closing of the pseudo-gap in high-temperature superconductivity, show the power of such an approach. Meanwhile, the range of achievable pressures was increased tremendously with a new generation of anvil cells (up to 10.1 GPa), that fit standard-bore NMR magnets. This approach might become a new, important tool for the investigation of many condensed matter systems, in chemistry, geochemistry, and in physics, since we can now watch structural changes with the eyes of a very versatile probe.

Nuclear magnetic resonance is one of the most important spectroscopic tools. Here, the development of a new approach under high pressure, currently up to 10.1 GPa, is presented. This opens a new window into condensed matter physics and chemistry, where high-pressure research is of great importance.

高灵敏度核磁共振的千兆帕斯卡压力:一种新的工具，用于极端条件下探测电子和化工凝聚态的性质

Nuclear Magnetic Resonance (NMR) is one of the most important techniques for the study of condensed matter systems, their chemical structure, and their ...

A Method for Studying the Temperature Dependence of Dynamic Fracture and Fragmentation

The dynamic fracture of a body is a late-stage phenomenon typically studied under simplified conditions, in which a sample is deformed under uniform stress and strain rate. This can be produced by evenly loading the inner surface of a cylinder. Due to the axial symmetry, as the cylinder expands the wall is placed into a tensile hoop stress that is uniform around the circumference. While there are various techniques to generate this expansion such as explosives, electromagnetic drive, and existing gas gun techniques they are all limited in the fact that the sample cylinder must be at room temperature. We present a new method using a gas gun that facilitates experiments on cylinders from 150 K to 800 K with a consistent, repeatable loading. These highly diagnosed experiments are used to examine the effect of temperature on the fracture mechanisms responsible for failure, and their resulting influence on fragmentation statistics. The experimental geometry employs a steel ogive located inside the target cylinder, with the tip located about halfway in. A single stage light gas gun is then used to launch a polycarbonate projectile into the cylinder at 1,000 m/sec-1. The projectile impacts and flows around the rigid ogive, driving the sample cylinder from the inside. The use of a non-deforming ogive insert allows us to install temperature control hardware inside the rear of the cylinder. Liquid nitrogen (LN2) is used for cooling and a resistive high current load for heating. Multiple channels of upshifted photon Doppler velocimetry (PDV) track the expansion velocity along the cylinder enabling direct comparison to computer simulations, while High speed imaging is used to measure the strain to failure. The recovered cylinder fragments are also subject to optical and electron microscopy to ascertain the failure mechanism.

Fracture and fragmentation are late stage phenomena in dynamic loading scenarios and are typically studied using explosives. We present a technique for driving expansion using a gas gun which uniquely enables control of both loading rate and sample temperature.

为研究动态断裂及破碎的温度敏感性的方法

The dynamic fracture of a body is a late-stage phenomenon typically studied under simplified conditions, in which a sample is deformed under uniform ...

Stress Distribution During Cold Compression of Rocks and Mineral Aggregates Using Synchrotron-based X-Ray Diffraction

We report detailed procedures for performing compression experiments on rocks and mineral aggregates within a multi-anvil deformation apparatus (D-DIA) coupled with synchrotron X-radiation. A cube-shaped sample assembly is prepared and compressed, at room temperature, by a set of four X-ray transparent sintered diamond anvils and two tungsten carbide anvils, in the lateral and the vertical planes, respectively. All six anvils are housed within a 250-ton hydraulic press and driven inward simultaneously by two wedged guide blocks. A horizontal energy dispersive X-ray beam is projected through and diffracted by the sample assembly. The beam is commonly in the mode of either white or monochromatic X-ray. In the case of white X-ray, the diffracted X-rays are detected by a solid-state detector array that collects the resulting energy dispersive diffraction pattern. In the case of monochromatic X-ray, the diffracted pattern is recorded using a two-dimensional (2-D) detector, such as an imaging plate or a charge-coupled device (CCD) detector. The 2-D diffraction patterns are analyzed to derive lattice spacings. The elastic strains of the sample are derived from the atomic lattice spacing within grains. The stress is then calculated using the predetermined elastic modulus and the elastic strain. Furthermore, the stress distribution in two-dimensions allow for understanding how stress is distributed in different orientations. In addition, a scintillator in the X-ray path yields a visible light image of the sample environment, which allows for the precise measurement of sample length changes during the experiment, yielding a direct measurement of volume strain on the sample. This type of experiment can quantify the stress distribution within geomaterials, which can ultimately shed light on the mechanism responsible for compaction. Such knowledge has the potential to significantly improve our understanding of key processes in rock mechanics, geotechnical engineering, mineral physics, and material science applications where compactive processes are important.

We report detailed procedures for compression experiments on rocks and mineral aggregates within a multi-anvil deformation apparatus coupled with synchrotron X-radiation. Such experiments allow quantification of the stress distribution within samples, that ultimately sheds light on compaction processes in geomaterials.

基于同步辐射 x 射线衍射的岩石和矿物团聚体冷压缩应力分布

We report detailed procedures for performing compression experiments on rocks and mineral aggregates within a multi-anvil deformation apparatus (D-DIA) ...

环境科学

A Novel Biaxial Testing Apparatus for the Determination of Forming Limit under Hot Stamping Conditions

The hot stamping and cold die quenching process is increasingly used to form complex shaped structural components of sheet metals. Conventional experimental approaches, such as out-of-plane and in-plane tests, are not applicable to the determination of forming limits when heating and rapid cooling processes are introduced prior to forming for tests conducted under hot stamping conditions. A novel in-plane biaxial testing system was designed and used for the determination of forming limits of sheet metals at various strain paths, temperatures, and strain rates after heating and cooling processes in a resistance heating uniaxial testing machine. The core part of the biaxial testing system is a biaxial apparatus, which transfers a uniaxial force provided by the uniaxial testing machine to a biaxial force. One type of cruciform specimen was designed and verified for the formability test of aluminum alloy 6082 using the proposed biaxial testing system. The digital image correlation (DIC) system with a high-speed camera was used for taking strain measurements of a specimen during a deformation. The aim of proposing this biaxial testing system is to enable the forming limits of an alloy to be determined at various temperatures and strain rates under hot stamping conditions.

This protocol proposes a novel biaxial testing system used on a resistance heating uniaxial tensile test machine in order to determine the forming limit diagram (FLD) of sheet metals under hot stamping conditions.

一种新型双轴试验设备的成形极限的下烫印条件的决定

The hot stamping and cold die quenching process is increasingly used to form complex shaped structural components of sheet metals. Conventional ...

A Novel Method for In Situ Electromechanical Characterization of Nanoscale Specimens

Electrically assisted deformation (EAD) is increasingly being used to improve the formability of metals during processes such as sheet metal rolling and forging. Adoption of this technique is proceeding despite disagreement concerning the underlying mechanism responsible for EAD. The experimental procedure described herein enables a more explicit study compared to previous EAD research by removing thermal effects, which are responsible for disagreement in interpreting previous EAD results. Furthermore, as the procedure described here enables EAD observation in situ and in real time in a transmission electron microscope (TEM), it is superior to existing post-mortem methods that observe EAD effects post-test. Test samples consist of a single crystal copper (SCC) foil having a free-standing tensile test section of nanoscale thickness, fabricated using a combination of laser and ion beam milling. The SCC is mounted to an etched silicon base that provides mechanical support and electrical isolation while serving as a heat sink. Using this geometry, even at high current density (~3,500 A/mm2), the test section experiences a negligible temperature increase (&#60;0.02 &#176;C), thus eliminating Joule heating effects. Monitoring material deformation and identifying the corresponding changes to microstructures, e.g. dislocations, are accomplished by acquiring and analyzing a series of TEM images. Our sample preparation and in situ experiment procedures are robust and versatile as they can be readily utilized to test materials with different microstructures, e.g., single and polycrystalline copper.

A Novel Method for In Situ Electromechanical Characterization of Nanoscale Specimens

Isolating electrical and thermal effects on electrically assisted deformation (EAD) is very difficult using macroscopic samples. Metallic sample micro- and nanostructures together with a custom test procedure have been developed to evaluate the impact of applied current on the formation without joule heating and evolution of dislocations on these samples.

一种新的方法<em&gt;原位</em&gt;纳米级样品的机电表征

Electrically assisted deformation (EAD) is increasingly being used to improve the formability of metals during processes such as sheet metal rolling and ...

A Uniaxial Compression Experiment with CO2-Bearing Coal Using a Visualized and Constant-Volume Gas-Solid Coupling Test System

Injecting carbon dioxide (CO2) into a deep coal seam is of great significance for reducing the concentration of greenhouse gases in the atmosphere and increasing the recovery of coalbed methane. A visualized and constant-volume gas-solid coupling system is introduced here to investigate the influence of CO2 sorption on the physical and mechanical properties of coal. Being able to keep a constant volume and monitor the sample using a camera, this system offers the potential to improve instrument accuracy and analyze fracture evolution with a fractal geometry method. This paper provides all steps to perform a uniaxial compression experiment with a briquette sample in different CO2 pressures with the gas-solid coupling test system. A briquette, cold-pressed by raw coal and sodium humate cement, is loaded in high-pressure CO2, and its surface is monitored in real-time using a camera. However, the similarity between the briquette and the raw coal still needs improvement, and a flammable gas such as methane (CH4) cannot be injected for the test. The results show that CO2 sorption leads to peak strength and elastic modulus reduction of the briquette, and the fracture evolution of the briquette in a failure state indicates fractal characteristics. The strength, elastic modulus, and fractal dimension are all correlated with CO2 pressure but not with a linear correlation. The visualized and constant-volume gas-solid coupling test system can serve as a platform for experimental research about rock mechanics considering the multifield coupling effect.

A Uniaxial Compression Experiment with CO2-Bearing Coal Using a Visualized and Constant-Volume Gas-Solid Coupling Test System

This protocol demonstrates how to prepare a briquette sample and conduct a uniaxial compression experiment with a briquette in different CO2 pressures using a visualized and constant-volume gas-solid coupling test system. It also aims to investigate changes in terms of coal&#8217;s physical and mechanical properties induced by CO2 adsorption.

使用可视化和恒定体积气体-固体耦合测试系统使用 CO2轴承煤的单轴压缩实验

Injecting carbon dioxide (CO2) into a deep coal seam is of great significance for reducing the concentration of greenhouse gases in the atmosphere and ...

Conducting Elevated Temperature Normal and Combined Pressure-Shear Plate Impact Experiments Via a Breech-end Sabot Heater System

A novel approach for conducting normal and/or combined pressure-shear plate impact experiments at test temperatures up to 1000 &#176;C is presented. The method enables elevated temperature plate-impact experiments aimed towards probing dynamic behavior of materials under thermomechanical extremes, while mitigating several special experimental challenges faced while performing similar experiments using the conventional plate impact approach. Custom adaptations are made to the breech-end of a single-stage gas-gun at Case Western Reserve University; these adaptations include a precision-machined extension piece made from SAE 4340 steel, which is strategically designed to mate the existing gun-barrel while providing a high tolerance match to the bore and keyway. The extension piece contains a vertical cylindrical heater-well, which houses a heater assembly. A resistive coil heater-head, capable of reaching temperatures of up 1200 &#176;C, is attached to a vertical stem with axial/rotational degrees of freedoms; this enables thin metal specimens held at the front-end of a heat-resistant sabot to be heated uniformly across the diameter to the desired test temperatures. By heating the flyer plate (in this case, the sample) at the breech-end of the gun-barrel instead of at the target-end, several critical experimental challenges can be averted. These include: 1) severe changes in the alignment of the target plate during heating due to the thermal expansion of the several constituents of the target holder assembly; 2) challenges that arise due to the diagnostics elements, (i.e., polymer holographic gratings, and optical probes) being too close to the heated target assembly; 3) challenges that arise for target plates with an optical window, where crucial tolerances between the sample, bond layer, and window become increasingly difficult to maintain at high temperatures; 4) in the case of combined compression-shear plate impact experiments, the need for high-temperature resistant diffraction gratings for the measurement of transverse particle velocity at the free surface of the target; and 5) limitations imposed on the impact velocity necessary for unambiguous interpretation of the measured free surface velocity versus time profile due to thermal softening and possibly yielding of the bounding target plates.By utilizing the adaptations mentioned above, we present results from a series of reverse geometry normal plate impact experiments on commercial purity aluminum at a range of sample temperatures. These experiments show decreasing particle velocities in the impacted state, which are indicative of material softening (decrease in post-yield flow stress) with increasing sample temperatures.

Here, we present a detailed protocol of a new approach for conducting elevated temperature reverse normal plate impact, and combined pressure-and-shear plate impact. The approach involves the use of a breech-end resistive coil heater to heat a sample held at the front-end of a heat-resistant sabot to the desired temperature.

采用臀端穿甲弹加热系统进行高温常压联合压力-剪切板冲击试验

A novel approach for conducting normal and/or combined pressure-shear plate impact experiments at test temperatures up to 1000 &#176;C is presented. The ...

Sample Preparation and Experimental Design for In Situ Multi-Beam Transmission Electron Microscopy Irradiation Experiments

There is a need to understand materials exposed to overlapping extreme environments such as high temperature, radiation, or mechanical stress. When these stressors are combined there may be synergistic effects that enable unique microstructural evolution mechanisms to activate. Understanding of these mechanisms is necessary for the input and refinement of predictive models and critical for engineering of next generation materials. The basic physics and underlying mechanisms require advanced tools to be investigated. The in situ ion irradiation transmission electron microscope (I&#179;TEM) is designed to explore these principles.
To quantitatively probe the complex dynamic interactions in materials, careful preparation of samples and consideration of experimental design is required. Particular handling or preparation of samples can easily introduce damage or features that obfuscate the measurements. There is no one correct way to prepare a sample; however, many mistakes can be made. The most common errors and things to consider are highlighted within. The I&#179;TEM has many adjustable variables and a large potential experimental space, therefore it is best to design experiments with a specific scientific question or questions in mind.
Experiments have been performed on large number of sample geometries, material classes, and with many irradiation conditions. The following are a subset of examples that demonstrate unique in situ capabilities utilizing the I3TEM. Au nanoparticles prepared by drop casting have been used to investigate the effects of single ion strikes. Au thin films have been used in studies on the effects of multibeam irradiation on microstructure evolution. Zr films have been exposed to irradiation and mechanical tension to examine creep. Ag nanopillars were subjected to simultaneous high temperature, mechanical compression, and ion irradiation to study irradiation induced creep as well. These results impact fields including: structural materials, nuclear energy, energy storage, catalysis, and microelectronics in space environments.

Sample preparation techniques are outlined with specific considerations for in situ ion irradiation TEM experiments. Ion species, energy, and fluence are discussed with methods for how to select and compute them. Finally, procedures for conducting an experiment are described and accompanied by the representative results.

There is a need to understand materials exposed to overlapping extreme environments such as high temperature, radiation, or mechanical stress. When these ...

新一代格雷型装置高压高温变形试验

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