这项工作得到斯洛伐克研究和发展局根据合同编号的支持。APVV-16-0079 和 APVV-15-0621, 赠款维加 1/0182/16 和维加 2/0082/17 和 Palacký大学的内部 IGA 赠款 (IGA_PrF_2018_002)。我们感谢 R. Rüffer (ESRF, 格勒诺布尔) 为同步辐射实验提供帮助。

1. 镁的制备
注: 为了演示 NFS 与穆斯堡尔光谱的广泛诊断能力, 设计了适当的镁成分, 即 (Fe3Co1)76钼8铜1B15 (在 .%)。该系统显示了从铁磁向顺磁态过渡到结晶开始的磁场。此外, 晶粒在第一结晶过程中出现, 形成 bcc-铁, Co 相。因为钴在 bcc 格子的某些原子位置替换铁, 偏差在各自超精细相互作用发生。
<ol><li>熔体的制备 注: 穆斯堡尔光谱和 NFS 扫描的地方原子安排通过超精细相互作用的57Fe 核是存在于调查样本。这稳定的核素的自然丰盈在所有 Fe 同位素之中是, 然而仅2.19%。为了减少原位NFS 实验的采集时间, 57铁同位素的相对含量应提高到约50%。<ol>
<li>采用石英玻璃坩埚 (直径为15毫米的圆柱形), 用氮化硼覆盖其内壁, 以避免硅从墙壁中对其含量进行可能的污染, 并插入0.4050 克高浓缩57Fe (~ 95%) 和0.5267 克标准电解纯铁 (纯度 99.95%) 到这个坩埚。该混合物的总质量为0.9317 克, 保证了 50% 57Fe 的同位素富集。 注: 由于稳定的57Fe 同位素的高价格, 优化其数量到尽可能低的质量。大约500毫克57Fe 应该是足够保证熔化的整体重量到大约 1.5 g。这是制备设备的低技术极限。</li>
		<li>将0.3245 克电解 Co (99.85%)、0.0184g 铜 (99.8%)、0.2222 克钼 (99.95%) 和0.0470 克晶体 B (99.95%) 加入同一个石英玻璃坩埚中。混合物的总质量是 1.5438 g, 并且粉末的意欲的构成是 (Fe3Co1)76钼8铜1B15。</li>
		<li>在保护氩 (4N8) 气氛下, 在石英玻璃坩埚中通过感应加热熔化所获得的标准电解材料混合物, 以避免氧化, 并使用90-120 赫的射频场。 注: 射频场确保坩埚中各元件的混合。当熔体形成时, 它们的混合在涡流的帮助下进一步进行。允许足够的时间融化粉末混合物, 形成液体。目视检查是足够的, 没有必要测量产生的液体的温度。</li>
		<li>从坩埚中取出所获得的小锭。目视检查其表面的任何痕迹的出现。如果存在, 通过机械抛光去除。</li>
	</ol></li>
	<li>带状状试样的制备
	<ol>
<li>使用用于平面流铸件的装置。图 1显示了这样一个设备的示例。 注: 石英管内的熔体被 Ar 流排出到在空气中旋转的淬火轮上。不需要特殊的大气条件下, 淬火车轮的操作 (如真空或惰性气体环境) 的这一组成的熔融。</li>
		<li>由于钢锭的重量小 (~ 1.5 克), 选择一个具有喷嘴直径为0.8 毫米圆孔的石英管。把钢锭放进去, 用感应加热熔化。保持熔化的温度在 1,280-1, 295 °c。</li>
		<li>将冷却轮的表面速度调整到40米/秒。</li>
		<li>在环境条件下,即空气中, 将熔体铸造在旋转淬火轮上。 注: 产生的丝带约 1.5-2 毫米宽, 25-27 µm 厚, 5 米长。丝带的空气边, 在生产期间被暴露对周围的空气大气, 是光学上发亮的 (光泽), 而相反轮子边, 与淬火轮子直接地接触, 是垫 (沉闷)。这些微妙的丝带质量是由熔体的低质量造成的。因此, 由于单个元素的输入质量低, 验证所生产的淬火带的最终化学成分是很重要的。</li>
	</ol></li>
	<li>验证色带的最终化学成分
	<ol>
<li>准备几个 (多达五) 短片的丝带, 每个有约0.70 毫克的质量. 从所生产的丝带的不同部分, 沿其长度选择。</li>
		<li>将每条丝带溶解在1毫升的浓缩中 (67%)HNO3酸, 充水达到50毫升的溶液总容积。</li>
		<li>用电感耦合等离子体 (ICP) 光学发射光谱法测定钼和 B 的含量。使用仪器手册中提供的外部校准方法。用以下波长记录信号: Mo 在203.844 毫微米和204.598 毫微米, 并且 B 在249.773 毫微米。</li>
		<li>火焰原子吸收光谱法测定铁、钴、铜的含量。使用仪器手册中提供的外部校准方法, 并选择这些波长: Fe 在248.3 毫微米, Co 在240.7 毫微米, 并且铜在324.7 毫微米。</li>
	</ol></li>
	<li>生产带的结构表征
	<ol>
<li>通过在布拉格-布伦塔诺几何中执行 X 射线衍射 (XRD) 检查产生的色带的非晶性;使用波长为 0.154056 nm 的铜阳极, 记录 2Θ20-100°的衍射模式, 0.05°和采集时间为一点。 注: 非晶态试样的 XRD diffractogram 特征是像图 2所示的宽反射峰。没有窄线表明存在的晶粒应该存在。</li>
		<li>准备小块的生产丝带, 总质量约3-5 毫克, 并把它们放入一个石墨坩埚的 DSC 设备。 注: 长度约2毫米的小块可以用剪刀从丝带上剪下来。</li>
		<li>在 Ar 气氛下, 在50-700 摄氏度的温度范围内, 执行 DSC 实验, 温度斜坡为 10 K/分钟。</li>
		<li>确定结晶 Tx1的起始温度, 这是在 DSC 曲线上最显著峰值的扭结处进行的。 注: 结晶 Tx1的起始温度在图 3中用箭头表示。</li>
		<li>选择了五的退火温度, 覆盖 DSC 上的预结晶和结晶区, 进一步进行原位退火。 注: 在我们的情况下, 适当的温度是 370, 410, 450, 510 和550°c, 如图 3所示。</li>
	</ol></li>
	<li>原位退火<ol>
<li>准备五组7厘米长的片 (总长度) 的淬火丝带。各自的丝带应该是至少 1 cm 长。</li>
		<li>对于原位退火, 使用炉 (图 4)。设置目标温度, 并等待15分钟的稳定。 注: 炉体设计保证了等温退火的最小起效时间。该炉由两部分组成: 上、下圆形大型镀镍铜块, 作为温度均质体。Kanthal 一条带热的块, 温度调节和稳定的高动态。目标温度是在步骤1.4.5 中确定的。</li>
		<li>将带状件插入到疏散和热稳定区。要做到这一点, 在两个方块之间打开一个7-10 毫米的缝隙, 并将丝带直接滑入加热区的中心。</li>
		<li>立即关闭缺口。这样, 试样的温度在 0.1 K 的差值内达到5秒的炉膛温度。</li>
		<li>在真空下进行370、410、450、510和550摄氏度的退火, 以防止表面氧化。</li>
		<li>退火后, 取下加热的丝带, 放在真空系统内的冷基板上。这保证了样品的快速冷却到室温。 注: 热处理后的缎带诱导结构的变化, 最终导致结晶的最初无定形材料。</li>
	</ol></li>
</ol>2. 调查方法
<ol><li>
穆斯堡尔光谱 注: 使用的铁丰富到约50% 在57Fe 生产的研究 MG 确保足够短的采集时间的原位NFS 实验。另一方面, 有效厚度的丝带明显增加。这就造成了与传统透射几何实验中记录的吸收穆斯堡尔谱线极高的展宽有关的问题。这就是为什么要考虑穆斯堡尔光谱的表面敏感技术。即转换电子穆斯堡尔光谱分析 (CEMS) 和转换 X 射线穆斯堡尔光谱分析 (CXMS) 可以应用。虽然 CEMS 扫描地下区域到大约200毫微米的深度, CXMS 提供信息从更深的区域延伸到大约5-10 µm。<ol>
<li>为 CEMS/CXMS 实验准备样品;用6-8 块1厘米长的丝带做一个样品。</li>
		<li>将丝带并排连接到铝架上, 形成紧凑面积约 1 x 1 厘米2;在丝带的两端使用胶带;所有丝带必须放在他们的空气两侧向上。 注: 确保缎带与持有人之间有电接触, 样品的中心部分 (约 8 x 10 毫米2) 从任何表面污染中清除,例如胶带的残留物。</li>
		<li>将铝持有者与样品插入 CEMS/CXMS 探测器。</li>
		<li>在测量之前, 用检测气体的流彻底清洗内部检测器体积, 以排出所有残余空气。允许10-15 分钟完成此过程。</li>
		<li>用针阀将气体流量通过检测器调整到3毫升/分。</li>
		<li>将高电压连接到探测器: 典型值为 CEMS 约1.2 伏, CXMS 高约200伏。</li>
		<li>使用装有57Co/Rh 放射源的恒定加速度光谱仪记录 CEMS 和 CXMS 穆斯堡尔谱。根据说明书在室温下使用气体检测仪操作光谱仪。</li>
		<li>分别用4和 Ar + ch4气体混合物填充气体探测器, 完成对转换电子和 X 射线的检测。在两种情况下, 将 CH4的数量保持在10%。</li>
		<li>重复步骤2.1.2 到2.1.8 的车轮侧的调查的丝带。</li>
		<li>使用薄 (12.5 µm) α Fe 箔对仪器进行速度校准14 。</li>
		<li>评价 CEMS/CXMS 谱;在校准α-Fe 箔的室温穆斯堡尔谱上引用获得的异构体移位值。 注: 获得的穆斯堡尔谱可以通过任何合适的拟合代码进行评估, 例如由煨软件24。</li>
	</ol>
</li>
	<li>
Nfs
	<ol>
<li>在同步加速器上使用合适的核磁共振光束线完成 NFS 实验。一个可能的选择: ID 18 在欧洲同步辐射设施 (ESRF) 在格勒诺布尔, 法国。25
</li>
		<li>将光子光束的能量调至14.413 凯文, 带宽为1兆伏特。</li>
		<li>在真空炉内放置被调查的镁的大约6毫米长的丝带。</li>
		<li>在样品的连续加热过程中记录 NFS 时间域模式, 温度可达700摄氏度, 斜坡为 10 K/分钟. 在整个原位退火过程中, 使用1分钟的时间间隔来获取实验数据。 注意: NFS 实验的传输几何可以确保从样本的批量获取有关超精细交互的信息。</li>
		<li>使用合适的软件 (如www.nrixs.com) 评估 NFS 实验数据。 注意: 在一次原位实验中, 通常会记录多达100个 NFS 时间域模式。在 CONUSS 软件包26、27的评估过程中, 考虑应用一个名为休伯特的特殊自由软件, 它可以在半自动模式28中评估如此巨大的数据量。</li>
	</ol>
</li>
</ol>

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Alloy. Compounds. 638, 398-404 (2015).</li><li>Miglierini, M., Pavlovi&#269;, M., Proch&#225;zka, V., Hatala, T., Schumacher, G., R&#252;ffer, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Evolution+of+structure+and+local+magnetic+fields+during+crystallization+of+HITPERM+glassy+alloys+studied+by+in+situ+diffraction+and+nuclear+forward+scattering+of+synchrotron+radiation.">Evolution of structure and local magnetic fields during crystallization of HITPERM glassy alloys studied by in situ diffraction and nuclear forward scattering of synchrotron radiation.</a> Phys. Chem. Chem. Phys. 17 (42), 28239-28249 (2015).</li><li>Miglierini, M. B., Proch&#225;zka, V., Khodaei, M., Petaccia, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nanocrystallization+of+Metallic+Glasses+Followed+by+in+situ+Nuclear+Forward+Scattering+of+Synchrotron+Radiation.">Nanocrystallization of Metallic Glasses Followed by in situ Nuclear Forward Scattering of Synchrotron Radiation.</a> X-ray Characterization of Nanomaterials by Synchrotron Radiation. , 7-29 (2017).</li><li>Miglierini, M., Mat&#250;&#353;, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Structural+Modifications+of+Metallic+Glasses+Followed+by+Techniques+of+Nuclear+Resonances.">Structural Modifications of Metallic Glasses Followed by Techniques of Nuclear Resonances.</a> Pure Appl. Chem. 89 (4), 405-417 (2017).</li><li>&#381;&#225;k, T., Jir&#225;skov&#225;, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=CONFIT:+M&#246;ssbauer+spectra+fitting+program.">CONFIT: M&#246;ssbauer spectra fitting program.</a> Surf. Interf. Anal. 38 (4), 710-714 (2006).</li><li>R&#252;ffer, R., Chumakov, A. I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nuclear-resonance+beamline+at+ESRF.">Nuclear-resonance beamline at ESRF.</a> Hyperfine Interact. (1-4), 589-604 (1996).</li><li>Sturhahn, W., Gerdau, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Evaluation+of+time-differential+measurements+of+nuclear-resonance+scattering.">Evaluation of time-differential measurements of nuclear-resonance scattering.</a> of X-rays Phys. Rev. B. 49 (14), 9285-9294 (1994).</li><li>Sturhahn, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=CONUSS+and+PHOENIX:+Evaluation+of+nuclear+resonant+scattering+data.">CONUSS and PHOENIX: Evaluation of nuclear resonant scattering data.</a> Hyperfine Interact. 125 (1-4), 149-172 (2000).</li><li>Vrba, V., Proch&#225;zka, V., Smr&#269;ka, D., Miglierini, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Advanced+Approach+to+the+Analysis+of+a+Series+of+in-situ+Nuclear+Forward+Scattering+Experiments.">Advanced Approach to the Analysis of a Series of in-situ Nuclear Forward Scattering Experiments.</a> Nucl. Instr. Meth. Phys. Res. A. 847, 111-116 (2017).</li><li>Miglierini, M., Gren&#232;che, J. -. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=M&#246;ssbauer+Spectrometry+of+Fe(Cu)MB-Type+Nanocrystalline+Alloys:+I.+The+Fitting+Model+for+the+M&#246;ssbauer+Spectra.">M&#246;ssbauer Spectrometry of Fe(Cu)MB-Type Nanocrystalline Alloys: I. The Fitting Model for the M&#246;ssbauer Spectra.</a> J. Phys.: Condens. Matter. 9 (10), 2303-2319 (1997).</li><li>M&#252;lhaupt, G., R&#252;ffer, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Properties+of+synchrotron+radiation.">Properties of synchrotron radiation.</a> Hyperfine Int. 123 (1-8), 13-30 (1999).</li><li>R&#252;ffer, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nuclear+resonance+scattering.">Nuclear resonance scattering.</a> C. R. Physique. 9 (5-6), 595-607 (2008).</li><li>Seto, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Condensed+matter+physics+using+nuclear+resonant+scattering.">Condensed matter physics using nuclear resonant scattering.</a> J. Phys. Soc. Jpn. 82 (2), 021016 (2013).</li><li>Machala, L., Proch&#225;zka, V., Miglierini, M., Sharma, V. K., Maru&#353;&#225;k, Z., Wille, H. -. C. h., Zbo&#345;il, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Direct+Evidence+of+Fe(V)+and+Fe(IV)+Intermediates+during+Reduction+of+Fe(VI)+to+Fe(III):+A+Nuclear+Forward+Scattering+of+Synchrotron+Radiation+Approach.">Direct Evidence of Fe(V) and Fe(IV) Intermediates during Reduction of Fe(VI) to Fe(III): A Nuclear Forward Scattering of Synchrotron Radiation Approach.</a> Phys. Chem. Chem. Phys. 17 (34), 21787-21790 (2015).</li></ol>

作者没有什么可透露的。

前现场穆斯堡尔效应实验描述了在应用热处理后, 在所研究的 MG 中遇到的稳态情况。每种光谱都是在室温下连续数小时收集的。因此, 最初的非晶态结构的演化是作为退火条件的函数来遵循的。由于穆斯堡尔光谱对共振核作用下的超精细相互作用很敏感, 所以可以揭示温度升高引起的结构和/或磁性修正的微弱细节。然而, 当临时改变的条件 (如温度升高) 的影响已经完成时, 在环境条件下检查被调查的样品。
就地NFS 实验研究了在不同温度下的动态模态中的 MG。这打开一个定性地新的洞察到兴趣系统的行为, 一个镁在这种情况下。值得注意的是, NFS 数据是在一分钟内获取的。这使得实时检查超精细交互的演化。这几乎是不可能的常规穆斯堡尔光谱分析。然而, 我们应该承认, 得到的参数是平均的每分钟的时间间隔内的数据记录。然而, 在如此短的时间跨度内, 个别参数的可能变化可以被认为是微不足道的。
穆斯堡尔光谱和 NFS 都通过超精细相互作用探测铁共振原子的局部邻域。因此, 有关结构安排和磁性显微结构的信息同时可用。当研究诸如 NCA 等复杂系统时, 这一点尤为重要。正如我们已经证明的, 它不仅可以遵循磁性过渡从铁磁到顺磁安排, 但也随之而来的结构转换,即结晶。nanograins 的形成可以在稳态和瞬态条件下进行检验。此外, 他们的详细描述, 以识别不同数量的外国原子在一个 bcc 结构的个别格子站点也是可行的。
通过常规穆斯堡尔谱光谱学进行的原位实验提供了有关材料的稳态状态的信息, 包括稳定和亚稳态。这意味着我们可以调查在初始 (淬火) 材料和最终产品中的局部结构以及磁性安排。后者通过纳米在适当的热处理之后获得, 但在环境条件下测量。然而,原位穆斯堡尔光谱在能量领域提供了信息。因此, 所得到的光谱直接关系到所研究材料的状态, 更便于评价和解释。
另一方面,原位NFS 方法适用于研究相变过程中发生的瞬态过程。由于材料的排列信息是在时间域中记录的量子节拍中编码的, 因此对 NFS 模式的评估是一项具有挑战性的任务。通过对原位穆斯堡尔效应实验所得结果的合理利用, 可以较好地解决这一问题。因此, 这两种方法的结合使得对所研究系统的稳态和瞬态状态进行检验。
这两种技术都是互补的, 从获得的结果的角度来看, 以及它们的实现条件。获得的经验也可以有效地用于研究与结构和/或磁性过渡相关的其他问题。作为一个典型的例子, 在温度处理过程中, 铁 (VI) 到铁 (III) 氧化物的固态还原中, 中间相的存在有不同的价态, 可以提到33。

由熔体快速淬火制备的铁基 mg 代表工业上有吸引力的材料与许多实际应用1。特别是因为它们的磁性能往往优于常规 (多晶硅) 晶体合金2,3。为了更好地从它们的有利参数中获益, 应该知道它们对高温的反应。随着温度的升高, 无定形结构松弛, 最终结晶开始。在某些类型的, 这可能导致其磁性参数的恶化, 因此, 性能较差。然而, 有几个家庭的铁基的铁人与特殊成分4,5,6,7 , 其中新形成的水晶谷物是非常精细的, 通常低于约30毫微米的大小。纳米晶能稳定结构, 从而在宽温度范围8、9保持可接受的磁性参数。这些是所谓的纳米晶合金 (NCA)。
在高温和/或恶劣条件下 (电离辐射、腐蚀等) 的长期性能可靠性要求对其行为和个别物理参数有透彻的了解。由于是无定形的, 分析技术的分类是相当有限的。例如, 衍射方法提供了广泛和无特色的反射, 只能用于验证 amorphicity。
值得注意的是, 有几种, 通常是间接的方法, 提供快速和无损的特性,例如, 磁致伸缩延时线传感原理。该方法提供了结构和应力状态的快速表征, 包括不均匀性的存在。它有利地适用于快速和非破坏性的描述沿镁丝带10,11的整个长度。
更详细的洞察到无序的结构安排可以通过超精细相互作用, 敏感地反映共振原子的局部原子安排来实现。此外, 还可以揭示拓扑和化学短距离阶的变化。在这方面, 在57Fe 核上进行的核磁共振 (NMR) 光谱分析和/或穆斯堡尔光谱分析的方法应该被认为是12,13。前者的方法只对磁偶极子超精细相互作用提供响应, 后者对电四极相互作用也很敏感。因此, 穆斯堡尔分光光度法同时提供了共振铁核14的结构布置和磁态的同时可用信息。
然而, 为了获得合理的统计数据, 穆斯堡尔频谱的获取通常需要几个小时。这一限制应特别考虑到温度依赖性实验的设想。在实验过程中应用的高温导致了研究的15的结构修改。因此, 只有在室温下进行的原位实验, 在一定温度下进行退火, 然后返回到环境条件下, 才能提供可靠的结果。
在热处理过程中, 镁结构的演变是通过分析技术进行的, 这种方法可以快速获取数据, 例如同步辐射 (DSR) 的 X 射线衍射, 差分扫描量热 (DSC), 或磁性测量。虽然现场实验是可能的, 获得的信息涉及结构 (DSR, DSC) 或磁性 (磁性数据) 的特点。然而, 在 DSC (和磁性测量) 的情况下, 在结晶过程中出现的 (纳米) 晶粒的识别是不可能的。另一方面, DSR 数据并不表示所调查系统的磁状态。这种情况的解决方案是利用超精细交互的技术: 同步辐射16的 NFS。它属于一组利用核共振散射过程17的方法。由于从第三代同步辐射获得的辐射极高的光辉,在原位条件下的温度 NFS 实验成为可行的18,19,20,21 ,22,23。
穆斯堡尔光谱和 NFS 都受与57铁核能级之间的核共振有关的物理原理所制约。然而, 虽然前者扫描超精细在能源领域的互动, 后者提供干涉的时间域。这样, 从两种方法得到的结果是等价的和互补的。为了评估 NFS 数据, 必须建立一个合理的物理模型。这项具有挑战性的任务可以通过提供第一个估计的穆斯堡尔光谱的帮助来完成。这两种方法的互补性意味着,原位NFS 检查瞬态状态和穆斯堡尔谱反映了稳定状态,即研究的材料的初始和/或最终状态。
本文详细介绍了这两种不常用的核共振方法的应用: 在这里, 我们将它们应用于在 a (Fe2.85Co1)77钼8铜1中发生的结构修改的调查.B14毫克接触热处理。我们希望这篇文章吸引研究人员的兴趣, 利用这些技术来调查类似的现象, 最终用不同类型的材料。

<table border="0" cellpadding="0" cellspacing="0" width="728">
	<tbody>
		<tr height="30">
			<td height="30" style="height:30px;width:216px;">stable isotope, 57Fe</td>
			<td style="width:147px;">Isoflex USA</td>
			<td style="width:119px;">iron-57</td>
			<td style="width:247px;">metallic form</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">standard eletrolytic Fe, 99.95 %</td>
			<td style="width:147px;">Sigma Aldrich (Merck)</td>
			<td style="width:119px;">1.03819</td>
			<td>fine powder</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">electrolytic Co, 99.85 %</td>
			<td style="width:147px;">Sigma Aldrich (Merck)</td>
			<td style="width:119px;">1.12211</td>
			<td>fine powder</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">electrolytic Cu, 99.8 %</td>
			<td style="width:147px;">Sigma Aldrich (Merck)</td>
			<td style="width:119px;">1.02703</td>
			<td>fine powder</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">electrolytic Mo, 99.95 %</td>
			<td style="width:147px;">Sigma Aldrich (Merck)</td>
			<td style="width:119px;">1.12254</td>
			<td>fine powder</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">crystalline B, 99.95 %</td>
			<td style="width:147px;">Sigma Aldrich (Merck)</td>
			<td style="width:119px;">266620</td>
			<td>crystalline</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">calibration foil for M&#246;ssbauer spectrometry, bcc-Fe</td>
			<td style="width:147px;">GoodFellow</td>
			<td style="width:119px;">564-385-23</td>
			<td>foil 0.0125 mm, purity 99.85 %</td>
		</tr>
		<tr height="44">
			<td height="44" style="height:44px;width:216px;">HNO3 acid, ANALPURE Ultra</td>
			<td style="width:147px;">Analytika Praha, Czech Republic</td>
			<td style="width:119px;">UAc0061a</td>
			<td>concentration 67 %, volume 500 mL</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">spectrometer for atomic absorption spectrometry</td>
			<td style="width:147px;">Perkin Elmer 1100, Germany</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:216px;">spectrometer for optical emmission spectrometry with inductively coupled plasma</td>
			<td style="width:147px;">Jobin Yvon 70 Plus, France</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">X-ray diffractometer</td>
			<td style="width:147px;">Bruker D8 Advance, USA</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">differential scanning calorimeter</td>
			<td style="width:147px;">Perkin Elmer DSC 7, Germany</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
	</tbody>
</table>

methods of ex situ and in situ investigations of structural transformations: the case of crystallization of metallic glasses

我们演示了采用两种基于核的分析方法, 可以遵循铁基金属玻璃的显微组织安排的修改。尽管它们的非晶性质, 超精细相互作用的识别揭示了微弱的结构修改。为此, 我们使用了两种技术, 利用核共振在稳定的57Fe 同位素的核水平, 即穆斯堡尔光谱和核前向散射 (NFS) 的同步辐射。利用原位试验和原位实验的结果, 讨论了热处理对 (Fe2.85Co1)77钼8铜1B14毫克的影响。由于这两种方法对超精细的相互作用都很敏感, 所以可以随时获得关于结构布置和磁性显微组织的信息。穆斯堡尔分光光度法对在一定条件下 (温度、时间) 退火后的室温下的结构布置和磁性显微结构的变化进行了描述, 从而使该技术检查稳定国家。另一方面, 在动态变化的温度和 nfs 检查瞬态状态时, 会在原位记录 nfs 数据。这两种技术的使用都提供了互补信息。一般情况下, 它们可以应用于任何合适的系统, 其中重要的是要知道它的稳定状态, 而且是瞬态状态。

Watch this Scientific Journal Video about Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses at JoVE.com

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

在这里, 我们提出了一个协议, 以描述原位和原位调查的结构转换在金属玻璃。我们采用了以核为基础的分析方法来检查超精细的相互作用。在温度驱动实验中, 我们证明了穆斯堡尔光谱和同步辐射核前向散射的适用性。

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 ...

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Nanyang Technological University

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

8.4K 次观看.  Slovak University of Technology in Bratislava, Slovakia. 在这里, 我们提出了一个协议, 以描述原位和原位调查的结构转换在金属玻璃。我们采用了以核为基础的分析方法来检查超精细的相互作用。在温度驱动实验中, 我们证明了穆斯堡尔光谱和同步辐射核前向散射的适用性。

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

In-situ Tapering of Chalcogenide Fiber for Mid-infrared Supercontinuum Generation

Supercontinuum generation (SCG) in a tapered chalcogenide fiber is desirable for broadening mid-infrared (or mid-IR, roughly the 2-20 &mu;m wavelength range) frequency combs1, 2 for applications such as molecular fingerprinting, 3 trace gas detection, 4 laser-driven particle acceleration, 5 and x-ray production via high harmonic generation. 6 Achieving efficient SCG in a tapered optical fiber requires precise control of the group velocity dispersion (GVD) and the temporal properties of the optical pulses at the beginning of the fiber, 7 which depend strongly on the geometry of the taper. 8 Due to variations in the tapering setup and procedure for successive SCG experiments-such as fiber length, tapering environment temperature, or power coupled into the fiber, in-situ spectral monitoring of the SCG is necessary to optimize the output spectrum for a single experiment.
	In-situ fiber tapering for SCG consists of coupling the pump source through the fiber to be tapered to a spectral measurement device. The fiber is then tapered while the spectral measurement signal is observed in real-time. When the signal reaches its peak, the tapering is stopped. The in-situ tapering procedure allows for generation of a stable, octave-spanning, mid-IR frequency comb from the sub harmonic of a commercially available near-IR frequency comb. 9 This method lowers cost due to the reduction in time and materials required to fabricate an optimal taper with a waist length of only 2 mm.
	The in-situ tapering technique can be extended to optimizing microstructured optical fiber (MOF) for SCG10 or tuning of the passband of MOFs, 11 optimizing tapered fiber pairs for fused fiber couplers12 and wavelength division multiplexers (WDMs), 13 or modifying dispersion compensation for compression or stretching of optical pulses.14-16

In-situ Tapering of Chalcogenide Fiber for Mid-infrared Supercontinuum Generation

We describe a method for in-situ tapering of As2S3 fibers to achieve efficient mid-infrared supercontinuum generation. By tapering while monitoring the supercontinuum&#x2019;s spectrum, the spectral width can be maximized for a fiber taper. In-situ fiber tapering can be applied to optimize the performance of other fiber-based devices.

原位减量硫系中红外光纤产生超连续谱

Supercontinuum  generation (SCG) in a tapered chalcogenide fiber is desirable for broadening mid-infrared  (or mid-IR, roughly the 2-20 &mu;m wavelength ...

科研

工程学

In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries

Li-ion batteries are widely used in portable electronic devices and are considered as promising candidates for higher-energy applications such as electric vehicles.1,2 However, many challenges, such as energy density and battery lifetimes, need to be overcome before this particular battery technology can be widely implemented in such applications.3 This research is challenging, and we outline a method to address these challenges using in situ NPD to probe the crystal structure of electrodes undergoing electrochemical cycling (charge/discharge) in a battery. NPD data help determine the underlying structural mechanism responsible for a range of electrode properties, and this information can direct the development of better electrodes and batteries.
We briefly review six types of battery designs custom-made for NPD experiments and detail the method to construct the &#8216;roll-over&#8217; cell that we have successfully used on the high-intensity NPD instrument, WOMBAT, at the Australian Nuclear Science and Technology Organisation (ANSTO). The design considerations and materials used for cell construction are discussed in conjunction with aspects of the actual in situ NPD experiment and initial directions are presented on how to analyze such complex in situ data.

In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries

We describe the design and construction of an electrochemical cell for the examination of electrode materials using in situ neutron powder diffraction (NPD). We briefly comment on alternate in situ NPD cell designs and discuss methods for the analysis of the corresponding in situ NPD data produced using this cell.

原位中子衍射用特制的锂离子电池

Li-ion batteries are widely used in portable electronic devices and are considered as promising candidates for higher-energy applications such as electric ...

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 ...

In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films

Combinations of metal oxide semiconductors and gold nanoparticles (AuNPs) have been investigated as new types of materials. The in situ synthesis of AuNPs within the interlayer space of semiconducting layered titania nanosheet (TNS) films was investigated here. Two types of intermediate films (i.e., TNS films containing methyl viologen (TNS/MV2+) and 2-ammoniumethanethiol (TNS/2-AET+)) were prepared. The two intermediate films were soaked in an aqueous tetrachloroauric(III) acid (HAuCl4) solution, whereby considerable amounts of Au(III) species were accommodated within the interlayer spaces of the TNS films. The two types of obtained films were then soaked in an aqueous sodium tetrahydroborate (NaBH4) solution, whereupon the color of the films immediately changed from colorless to purple, suggesting the formation of AuNPs within the TNS interlayer. When only TNS/MV2+ was used as the intermediate film, the color of the film gradually changed from metallic purple to dusty purple within 30 min, suggesting that aggregation of AuNPs had occurred. In contrast, this color change was suppressed by using the TNS/2-AET+ intermediate film, and the AuNPs were stabilized for over 4 months, as evidenced by the characteristic extinction (absorption and scattering) band from the AuNPs.

In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films

Here, we present a protocol for the in situ synthesis of gold nanoparticles (AuNPs) within the interlayer space of layered titanate films without the aggregation of AuNPs. No spectral change was observed even after 4 months. The synthesized material has expected applications in catalysis, photo-catalysis, and the development of cost-effective plasmonic devices.

在没有聚集的层状钛酸盐薄膜透明的层间金纳米粒子的原位合成

Combinations of metal oxide semiconductors and gold nanoparticles (AuNPs) have been investigated as new types of materials. The in situ synthesis of AuNPs ...

In Situ Visualization of the Phase Behavior of Oil Samples Under Refinery Process Conditions

To help address production issues in refineries caused by the fouling of process units and lines, we have developed a setup as well as a method to visualize the behavior of petroleum samples under process conditions. The experimental setup relies on a custom-built micro-reactor fitted with a sapphire window at the bottom, which is placed over the objective of an inverted microscope equipped with a cross-polarizer module. Using reflection microscopy enables the visualization of opaque samples, such as petroleum vacuum residues, or asphaltenes. The combination of the sapphire window from the micro-reactor with the cross-polarizer module of the microscope on the light path allows high-contrast imaging of isotropic and anisotropic media. While observations are carried out, the micro-reactor can be heated to the temperature range of cracking reactions (up to 450 &#176;C), can be subjected to H2 pressure relevant to hydroconversion reactions (up to 16 MPa), and can stir the sample by magnetic coupling. 
Observations are typically carried out by taking snapshots of the sample under cross-polarized light at regular time intervals. Image analyses may not only provide information on the temperature, pressure, and reactive conditions yielding phase separation, but may also give an estimate of the evolution of the chemical (absorption/reflection spectra) and physical (refractive index) properties of the sample before the onset of phase separation.

In Situ Visualization of the Phase Behavior of Oil Samples Under Refinery Process Conditions

This article describes a setup and method for the in situ visualization of oil samples under a variety of temperature and pressure conditions that aim to emulate refining and upgrading processes. It is primarily used for studying isotropic and anisotropic media involved in the fouling behavior of petroleum feeds.

在油样品的相行为在炼油工艺条件的原位可视化

To help address production issues in refineries caused by the fouling of process units and lines, we have developed a setup as well as a method to ...

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 ...

Measuring the Densities of Aqueous Glasses at Cryogenic Temperatures

We demonstrate a method for determining the vitreous phase cryogenic temperature densities of aqueous mixtures, and other samples that require rapid cooling, to prepare the desired cryogenic temperature phase. Microliter to picoliter size drops are cooled by projection into a liquid nitrogen-argon (N2-Ar) mixture. The cryogenic temperature phase of the drop is evaluated using a visual assay that correlates with X-ray diffraction measurements. The density of the liquid N2-Ar mixture is adjusted by adding N2 or Ar until the drop becomes neutrally buoyant. The density of this mixture and thus of the drop is determined using a test mass and Archimedes principle. With appropriate care in drop preparation, management of gas above the liquid cryogen mixture to minimize icing, and regular mixing of the cryogenic mixture to prevent density stratification and phase separation, densities accurate to &#60;0.5% of drops as small as 50 pL can readily be determined. Measurements on aqueous cryoprotectant mixtures provide insight into cryoprotectant action, and provide quantitative data to facilitate thermal contraction matching in biological cryopreservation.

A protocol for determining the vitreous phase densities of micro- to pico-liter size drops of aqueous mixtures at cryogenic temperatures is described.

在低温下测量水性玻璃的密度

We demonstrate a method for determining the vitreous phase cryogenic temperature densities of aqueous mixtures, and other samples that require rapid ...

In Situ Monitoring of the Accelerated Performance Degradation of Solar Cells and Modules: A Case Study for Cu(In,Ga)Se2 Solar Cells

The levelized cost of electricity (LCOE) of photovoltaic (PV) systems is determined by, among other factors, the PV module reliability. Better prediction of degradation mechanisms and prevention of module field failure can consequently decrease investment risks as well as increase the electricity yield. An improved knowledge level can for these reasons significantly decrease the total costs of PV electricity. 
In order to better understand and minimize the degradation of PV modules, the occurring degradation mechanisms and conditions should be identified. This should preferably happen under combined stresses, since modules in the field are also simultaneously exposed to multiple stress factors. Therefore, two 'Combined Stress test with in situ measurement' setups have been designed and constructed. These setups allow the simultaneous use of humidity, temperature, illumination, and electrical biases as independently controlled stress factors on solar cells and minimodules. The setups also allow real-time monitoring of the electrical properties of these samples. This protocol presents these setups and describes the experimental possibilities. Moreover, results obtained with these setups are also presented: various examples about the influence of both deposition and degradation conditions on the stability of thin film Cu(In,Ga)Se2 (CIGS) as well as Cu2ZnSnSe4 (CZTS) solar cells are described. Results on the temperature dependency of CIGS solar cells are also presented.

In Situ Monitoring of the Accelerated Performance Degradation of Solar Cells and Modules: A Case Study for CuIn,GaSe2 Solar Cells

Two &#39;Combined Stress test with in situ measurement&#39; setups, which allow real-time monitoring of accelerated degradation of solar cells and modules, were designed and constructed. These setups allow the simultaneous use of humidity, temperature, electrical biases, and illumination as independently controlled stress factors. The setups and various experiments executed are presented.

就地太阳能电池和模块加速性能退化的监测: 铜 (in, Ga) Se2太阳能电池的实例研究

The levelized cost of electricity (LCOE) of photovoltaic (PV) systems is determined by, among other factors, the PV module reliability. Better prediction ...

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

High pressure hydrogen gas is known to adversely affect metallic components of compressors, valves, hoses, and actuators. However, relatively little is known about the effects of high pressure hydrogen on the polymer sealing and barrier materials also found within these components. More study is required in order to determine the compatibility of common polymer materials found in the components of the hydrogen fuel delivery infrastructure with high pressure hydrogen. As a result, it is important to consider the changes in physical properties such as friction and wear in situ while the polymer is exposed to high pressure hydrogen. In this protocol, we present a method for testing the friction and wear properties of ethylene propylene diene monomer (EPDM) elastomer samples in a 28 MPa high pressure hydrogen environment using a custom-built in situ pin-on-flat linear reciprocating tribometer. Representative results from this testing are presented which indicate that the coefficient of friction between the EPDM sample coupon and steel counter surface is increased in high pressure hydrogen as compared to the coefficient of friction similarly measured in ambient air.

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

A test methodology for quantifying tribological properties of polymers used in hydrogen infrastructure service is demonstrated and characteristic results for a common elastomer are discussed.

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 ...

Experimental Procedure for Laboratory Studies of In Situ Burning : Flammability and Burning Efficiency of Crude Oil

A new method for the simultaneous study of the flammability and burning efficiency of fresh and weathered crude oil through two experimental laboratory setups is presented. The experiments are easily repeatable compared to operational scale experiments (pool diameter &#8805;2 m), while still featuring quite realistic in situ burning conditions of crude oil on water. Experimental conditions include a flowing water sub-layer that cools the oil slick and an external heat flux (up to 50 kW/m2) that simulates the higher heat feedback to the fuel surface in operational scale crude oil pool fires. These conditions enable a controlled laboratory study of the burning efficiency of crude oil pool fires that are equivalent to operational scale experiments. The method also provides quantitative data on the requirements for igniting crude oils in terms of the critical heat flux, ignition delay time as a function of the incident heat flux, the surface temperature upon ignition, and the thermal inertia. This type of data can be used to determine the required strength and duration of an ignition source to ignite a certain type of fresh or weathered crude oil. The main limitation of the method is that the cooling effect of the flowing water sub-layer on the burning crude oil as a function of the external heat flux has not been fully quantified. Experimental results clearly showed that the flowing water sub-layer does improve how representative this setup is of in situ burning conditions, but to what extent this representation is accurate is currently uncertain. The method nevertheless features the most realistic in situ burning laboratory conditions currently available for simultaneously studying the flammability and burning efficiency of crude oil on water.

Experimental Procedure for Laboratory Studies of In Situ Burning : Flammability and Burning Efficiency of Crude Oil

Here, we present a protocol to simultaneously study the flammability and burning efficiency of fresh and weathered crude oil under conditions that simulate in situ burning operations on the sea.

原位燃烧试验方法: 原油可燃性和燃烧效率

A new method for the simultaneous study of the flammability and burning efficiency of fresh and weathered crude oil through two experimental laboratory ...