Name: elemental-sensitive detection of the chemistry in batteries through soft x-ray absorption spectroscopy and resonant inelastic x-ray scattering
Uploaded: 2018-04-17T15:00:00.000+00:00
Duration: 7 min 55 s
Description: Watch this Scientific Journal Video about Elemental-sensitive Detection of the Chemistry in Batteries through Soft X-ray Absorption Spectroscopy and Resonant Inelastic X-ray Scattering at JoVE.com

劳伦斯伯克利国家实验室 (LBNL) 的高级光源 (ALS) 由美国能源部科学办公室主任, 根据合同编号支持。DE-AC02-05CH11231。Q.L. 感谢中国奖学金理事会 (CSC) 在中国111项目的基础上进行合作, 提供财务支持。B13029。R.Q. 感谢 LBNL LDRD 计划的支持。西西杰克森感谢 ALS 博士奖学金的支持。

1. 实验计划
注意: 虽然 sXES 可以用实验室设备进行, 但 sXAS 和 RIXS 是基于同步辐射的实验, 需要访问同步加速器设备的 beamtime。在不同的设施中, 申请 beamtime 和运行实验的程序可能不同, 但它们都遵循类似的基本程序。
<ol><li>检查光束线目录 (例如、https://als.lbl.gov/beamlines/) 的设施网站, 或与负责有关光束线的科学家联系, 以确定科学需要的适当光束线.</li>
	<li>通过在线提交系统在 https://als.lbl.gov/users/user-guide/上提交 beamtime 的建议, 光束线先进的光源 (ALS)。 注: beamtime 的建议将根据同步辐射设施的政策进行审查, 成功的提案的作者将被通知为实验性调度的设施。</li>
	<li>安全控制, 根据设备的要求完成必要的安全培训。报告化学品、样品和试验所需的特殊设备, 并进行检查以保证安全。</li>
	<li>到达 beamtime 前的设施, 以获得关于实验设置和示例加载的基本想法, 特别是作为新用户的设施/光束线。</li>
</ol>2. 样品准备
<ol><li>综合了自由和同胞材料的样品, 电化学循环到不同的电荷状态 (SOC)。</li>
	<li>
对空气敏感样品执行以下步骤:
	<ol>
<li>处理空气敏感的样品, 不暴露空气,即打开样品容器, 并用剪刀和镊子将样品切割成一个在惰性气体环境下拟合实验系统的尺寸。</li>
		<li>在惰性气体环境下使用双面导电胶带, 将合适尺寸的样品装在样品持有者上。 注: 如果要测量碳或氧的边缘, 使用软金属如铟粘附粉末样品, 以避免导电胶带中有机化合物的背景 C 和 O 信号。</li>
	</ol>
</li>
	<li>
对非空气敏感样品执行以下步骤:
	<ol>
<li>切割样品以匹配实验系统的特定样品持有者。</li>
		<li>使用双面导电胶带将合适尺寸的样品装入样品持有者。在收集功率样品的碳和氧信号时使用铟箔。</li>
	</ol>
</li>
	<li>对于原位示例, 请使用通常实现软 x 射线膜的特定单元格准备原位示例。在进入实验系统之前, 检查电气连接和电池完整性。 注意: 有关就地单元格的详细信息超出了此工作的范围, 但可以在以前的出版物35、36、37中找到。</li>
</ol>3. 装载和定位样品
注: 由于超高真空对软 x 射线光谱学实验的要求, 试样加载通常在进入主实验室之前, 通过缓冲真空室进行多个步骤。
<ol><li>停止真空泵, 在样品 loadlock 和主实验室之间关闭真空阀, 并排气样品 loadlock, 通常直接连接到带有 N2气体的实验系统。</li>
	<li>使用自制的样品采集器或大镊子抓取样品持有人, 并加载到 loadlock。</li>
	<li>开始抽 loadlock。等待, 直到真空压力表显示足够低的真空, 以打开 loadlock 到主实验室, 通常大约在10中旬-7乇。</li>
	<li>打开 loadlock 和主腔之间的阀门。使用转移臂将样品持有人转移到主室的主机械手上。</li>
	<li>打开主实验室与光束线之间的阀门。通过观察可见光荧光的参考样品来确定光斑。</li>
	<li>通过改变实验实验站的样本机械手的坐标, 将试样定位到光斑上。</li>
</ol>4. 设置 X 射线能量和分辨率
<ol><li>通过计算机程序或手动调节旋钮更改光束线单色仪的狭缝值, 以控制入射 X 射线光束的能量分辨率。</li>
	<li>将入射光束能量设置为访问感兴趣元素的吸收边缘所需的值,例如, 290 ev 用于 C k, 530 ev 用于 O k 边缘38。</li>
	<li>连接 X 射线束通量 (I-0) 显示器的信号电缆, 通常是光束路径中的一个干净的金网。</li>
	<li>修正了光束线单色仪的机构, 并在波荡间隙收集束流强度。为最大可能的光束通量确定特定的波荡间隙值。 注: 由于 sXAS 需要一个大的能量范围为不同的边缘, 一个优化的波荡隙, 以获得最大可能的光束通量往往是必要的。</li>
</ol>5. 收集 sXAS 数据
注: 通过记录采样电流 (泰) 和 channeltron 或光电二极管 (TFY) 的信号强度, 收集总收益 sXAS 数据。部分屈服信号通常通过门控 channeltron 和固态探测器收集。由于 RIXS 系统是在这里介绍的, 并且 RIXS 包括所有种类的部分荧光率 (PFY) 信号, 包括 PFY 和逆 PFY (iPFY), 在本次会议中只描述了泰和 TFY 数据收集的典型协议。
<ol><li>将样品连接到当前放大器, 并将采样电流信号 (泰) 送到计算机计数器。</li>
	<li>打开 channeltron 或光电二极管的电源和控制器, 将 TFY 信号送到计算机计数器。</li>
	<li>启动 LabVIEW sXAS 数据采集 grogram BL 控制主到达软件界面 (图 2), 然后单击菜单按钮扫描 |单电机扫描(图 2)。</li>
	<li>单击菜单按钮扫描安装程序(图 3), 设置事件 (光束线) X 射线光子的扫描范围, 以匹配感兴趣的 sXAS 边缘, 例如, 为 C K 边缘提供 280-300 eV. </li>
	<li>单击按钮开始扫描(图 3), 在扫描入射 X 射线光子能量时, 记录 (i) 泰 (ii) TFY 和 (iii) I-0 通道同时进行的强度信号。 注意: 在入射 X 射线光子能量上, 通常会有几个 eV 的小位移。在收集电池材料样品之前, 要进行校准, 收集一个或多个典型参考样品的 sXAS 数据。</li>
</ol>6. 收集 sXES 和 RIXS 数据
注: 由于 sXES 技术上是在非共振 (高) 能量范围内的 RIXS 切割, 所以数据收集设备和过程基本上是相同的。
<ol><li>收集 sXAS 首先定义励磁能量范围和校准能量值 (参考协议步骤 5)。</li>
	<li>打开 sXES/RiXS 系统光谱仪探测器的电源, 并冷却软 x 射线探测器, 以减少背景噪音, 每个制造商的建议。</li>
	<li>启动 LabVIEW sXES/RiXS 数据采集 grogram BL 控制主以到达软件接口 (图 4)。</li>
	<li>单击菜单按钮马达(图 4) 设置光谱仪的光学参数, 以便探测器覆盖感兴趣的元素和边缘的能量范围 (图 5)。</li>
	<li>单击菜单按钮扫描(图 4) |CCD 仪器扫描(图 6)。</li>
	<li>单击菜单按钮扫描安装程序(图 6), 以设置事件 (光束线) X 射线光子能量的扫描范围。如果收集 sXES, 将其设置为大约 20-30 eV 以上的 sXAS 吸收边缘的单一值;否则, 如果收集 RiXS, 将入射 X 射线 (光束线) 能量设置为覆盖 sXAS 吸收边缘的范围。</li>
	<li>选择图标应用宇宙射线滤镜(图 6), 从原始 RIXS 2D 图像中取出宇宙射线信号, 一旦从光谱仪探测器采集到它们。</li>
	<li>单击按钮开始扫描(图 6) 以收集荧光信号, 它们由光栅衍射和能量解析, 以2D 图像的形式由探测器上的每个激发能量组成。</li>
</ol>7. sXAS 数据处理
注: 实验数据, 包括 sXAS 以及 sXES 和 RiXS, 都是在伊戈尔 Pro 程序中处理的。
<ol><li>将 sXAS 泰和 TFY 信号正常化为同时收集的 I-0 信号。</li>
	<li>计算参考样品所收集的 sXAS 与标准之间的能量误差;根据计算出的能量误差来校准 sXAS 信号。</li>
</ol>8. sXES 和 RIXS 数据处理
<ol><li>通过对沿角度调整的发射-能量通道的光子计数进行汇总, 将原始2D 图像的强度综合起来, 生成单个 sXES 或 RIXS 谱。</li>
	<li>将集成的 1D RIXS 频谱正常化为在数据收集过程中实时监视的入射光束流量, 以及收集时间 (以秒为单位)。</li>
	<li>按颜色缩放格式绘制规范化的1D 频谱。</li>
	<li>对于 RiXS 数据, 对每个激发能量重复步骤 8.1-8.3, 在发射能量通道上获得一系列 1D RiXS 谱;然后, 将所有颜色缩放的 1D RIXS 光谱一对一地叠加成2D 图像图, 用一个轴沿励磁能量, 另一轴显示发射能量通道。</li>
	<li>使用 sXAS 校准, 通常通过参考样本 (参见协议步骤 7.2) 校准 sXES 频谱或 RIXS 映射的励磁能量值。</li>
	<li>选择一组点 (x = 通道号、 y = 能量值) 沿 RIXS 地图上的弹性特征, 其中激发和发射能量相同;用点集进行线性曲线拟合, 达到每通道的形式能量值;根据关系, 缩放从通道到能量的x轴。</li>
</ol>

<ol>
	<li>Armand, M., Tarascon, 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=Building+better+batteries.">Building better batteries.</a> Nature. 451 (7179), 652-657 (2008).</li><li>Yang, Z., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrochemical+energy+storage+for+green+grid.">Electrochemical energy storage for green grid.</a> Chem Rev. 111 (5), 3577-3613 (2011).</li><li>Dunn, B., Kamath, H., Tarascon, 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=Electrical+energy+storage+for+the+grid:+a+battery+of+choices.">Electrical energy storage for the grid: a battery of choices.</a> Science. 334 (6058), 928-935 (2011).</li><li>Ellis, B. L., Lee, K. T., Nazar, L. F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Positive+Electrode+Materials+for+Li-Ion+and+Li-Batteries.">Positive Electrode Materials for Li-Ion and Li-Batteries.</a> Chemistry of Materials. 22 (3), 691-714 (2010).</li><li>Goodenough, J. B., Kim, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Challenges+for+Rechargeable+Li+Batteries.">Challenges for Rechargeable Li Batteries.</a> Chemistry of Materials. 22 (3), 587-603 (2009).</li><li>Grimaud, A., Hong, W. T., Shao-Horn, Y., Tarascon, 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=Anionic+redox+processes+for+electrochemical+devices.">Anionic redox processes for electrochemical devices.</a> Nat Mater. 15 (2), 121-126 (2016).</li><li>Wanli Yang, R. Q. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Soft+x-ray+spectroscopy+for+probing+electronic+and+chemical+states+of+battery+materials.">Soft x-ray spectroscopy for probing electronic and chemical states of battery materials.</a> Chin. Phys. B. 25 (1), 17104 (2016).</li><li>Yang, W., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Key+electronic+states+in+lithium+battery+materials+probed+by+soft+X-ray+spectroscopy.">Key electronic states in lithium battery materials probed by soft X-ray spectroscopy.</a> Journal of Electron Spectroscopy and Related Phenomena. 190, 64-74 (2013).</li><li>Qiao, R., Yang, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Interactions+at+the+electrode-electrolyte+interfaces+in+batteries+studied+by+quasi-in-situ+soft+x-ray+absorption+spectroscopy.">Interactions at the electrode-electrolyte interfaces in batteries studied by quasi-in-situ soft x-ray absorption spectroscopy.</a> Journal of Electron Spectroscopy and Related Phenomena. , (2017).</li><li>Lin, F., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synchrotron+X-ray+Analytical+Techniques+for+Studying+Materials+Electrochemistry+in+Rechargeable+Batteries.">Synchrotron X-ray Analytical Techniques for Studying Materials Electrochemistry in Rechargeable Batteries.</a> Chem Rev. , (2017).</li><li>Liu, X., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Why+LiFePO4+is+a+safe+battery+electrode:+Coulomb+repulsion+induced+electron-state+reshuffling+upon+lithiation.">Why LiFePO4 is a safe battery electrode: Coulomb repulsion induced electron-state reshuffling upon lithiation.</a> Phys Chem Chem Phys. 17 (39), 26369-26377 (2015).</li><li>Liu, G., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Polymers+with+tailored+electronic+structure+for+high+capacity+lithium+battery+electrodes.">Polymers with tailored electronic structure for high capacity lithium battery electrodes.</a> Adv Mater. 23 (40), 4679-4683 (2011).</li><li>Wu, M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Toward+an+Ideal+Polymer+Binder+Design+for+High-Capacity+Battery+Anodes.">Toward an Ideal Polymer Binder Design for High-Capacity Battery Anodes.</a> Journal of the American Chemical Society. 135 (32), 12048-12056 (2013).</li><li>Wang, L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Rhombohedral+prussian+white+as+cathode+for+rechargeable+sodium-ion+batteries.">Rhombohedral prussian white as cathode for rechargeable sodium-ion batteries.</a> J Am Chem Soc. 137 (7), 2548-2554 (2015).</li><li>Qiao, R., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Distinct+Solid-Electrolyte-Interphases+on+Sn+(100)+and+(001)+Electrodes+Studied+by+Soft+X-Ray+Spectroscopy.">Distinct Solid-Electrolyte-Interphases on Sn (100) and (001) Electrodes Studied by Soft X-Ray Spectroscopy.</a> Advanced Materials Interfaces. 1 (100), (2014).</li><li>Shan, X., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Bivalence+Mn5O8+with+hydroxylated+interphase+for+high-voltage+aqueous+sodium-ion+storage.">Bivalence Mn5O8 with hydroxylated interphase for high-voltage aqueous sodium-ion storage.</a> Nat Commun. 7, 13370 (2016).</li><li>Qiao, R., Chuang, Y. D., Yan, S., Yang, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Soft+x-ray+irradiation+effects+of+Li(2)O(2),+Li(2)CO(3)+and+Li(2)O+revealed+by+absorption+spectroscopy.">Soft x-ray irradiation effects of Li(2)O(2), Li(2)CO(3) and Li(2)O revealed by absorption spectroscopy.</a> PLoS One. 7 (11), 49182 (2012).</li><li>Bak, S. -. M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Na-Ion+Intercalation+and+Charge+Storage+Mechanism+in+2D+Vanadium+Carbide.">Na-Ion Intercalation and Charge Storage Mechanism in 2D Vanadium Carbide.</a> Advanced Energy Materials. , 1700959 (2017).</li><li>Zhuo, Z., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effect+of+excess+lithium+in+LiMn2O4+and+Li1.15Mn1.85O4+electrodes+revealed+by+quantitative+analysis+of+soft+X-ray+absorption+spectroscopy.">Effect of excess lithium in LiMn2O4 and Li1.15Mn1.85O4 electrodes revealed by quantitative analysis of soft X-ray absorption spectroscopy.</a> Applied Physics Letters. 110, 093902 (2017).</li><li>Qiao, R., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Transition-metal+redox+evolution+in+LiNi+0.5+Mn+0.3+Co+0.2+O+2+electrodes+at+high+potentials.">Transition-metal redox evolution in LiNi 0.5 Mn 0.3 Co 0.2 O 2 electrodes at high potentials.</a> Journal of Power Sources. 360, 294-300 (2017).</li><li>Qiao, R., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Revealing+and+suppressing+surface+Mn(II)+formation+of+Na0.44MnO2+electrodes+for+Na-ion+batteries.">Revealing and suppressing surface Mn(II) formation of Na0.44MnO2 electrodes for Na-ion batteries.</a> Nano Energy. 16, 186-195 (2015).</li><li>Qiao, R., et al. <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+gradient+Mn(II)+evolution+at+charged+states+in+LiNi0.5Mn1.5O4+electrodes+with+capacity+fading.">Direct evidence of gradient Mn(II) evolution at charged states in LiNi0.5Mn1.5O4 electrodes with capacity fading.</a> Journal of Power Sources. 273, 1120-1126 (2015).</li><li>Wu, J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Modification+of+Transition-Metal+Redox+by+Interstitial+Water+in+Hexacyanometallate+Electrodes+for+Sodium-Ion+Batteries.">Modification of Transition-Metal Redox by Interstitial Water in Hexacyanometallate Electrodes for Sodium-Ion Batteries.</a> Journal of the American Chemical Society. , (2017).</li><li>Liu, X., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Phase+Transformation+and+Lithiation+Effect+on+Electronic+Structure+of+LixFePO4:+An+In-Depth+Study+by+Soft+X-ray+and+Simulations.">Phase Transformation and Lithiation Effect on Electronic Structure of LixFePO4: An In-Depth Study by Soft X-ray and Simulations.</a> Journal of the American Chemical Society. 134 (33), 13708-13715 (2012).</li><li>Liu, X., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Distinct+charge+dynamics+in+battery+electrodes+revealed+by+in+situ+and+operando+soft+X-ray+spectroscopy.">Distinct charge dynamics in battery electrodes revealed by in situ and operando soft X-ray spectroscopy.</a> Nat Commun. 4, 2568 (2013).</li><li>Zhuo, Z., Hu, J., Duan, Y., Yang, W., Pan, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Transition+metal+redox+and+Mn+disproportional+reaction+in+LiMn0.5Fe0.5PO4+electrodes+cycled+with+aqueous+electrolyte.">Transition metal redox and Mn disproportional reaction in LiMn0.5Fe0.5PO4 electrodes cycled with aqueous electrolyte.</a> Applied Physics Letters. 109 (2), 023901 (2016).</li><li>Li, Q., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Quantitative+probe+of+the+transition+metal+redox+in+battery+electrodes+through+soft+x-ray+absorption+spectroscopy.">Quantitative probe of the transition metal redox in battery electrodes through soft x-ray absorption spectroscopy.</a> Journal of Physics D: Applied Physics. 49 (41), 413003 (2016).</li><li>Qiao, R., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Direct+Experimental+Probe+of+the+Ni(II)/Ni(III)/Ni(IV)+Redox+Evolution+in+LiNi0.5Mn1.5O4Electrodes.">Direct Experimental Probe of the Ni(II)/Ni(III)/Ni(IV) Redox Evolution in LiNi0.5Mn1.5O4Electrodes.</a> The Journal of Physical Chemistry C. 119 (49), 27228-27233 (2015).</li><li>Pasta, M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Manganese-cobalt+hexacyanoferrate+cathodes+for+sodium-ion+batteries.">Manganese-cobalt hexacyanoferrate cathodes for sodium-ion batteries.</a> J. Mater. Chem. A. 4 (11), 4211-4223 (2016).</li><li>Jeyachandran, Y. L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Investigation+of+the+Ionic+Hydration+in+Aqueous+Salt+Solutions+by+Soft+X-ray+Emission+Spectroscopy.">Investigation of the Ionic Hydration in Aqueous Salt Solutions by Soft X-ray Emission Spectroscopy.</a> J Phys Chem B. 120 (31), 7687-7695 (2016).</li><li>Jeyachandran, Y. L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ion-Solvation-Induced+Molecular+Reorganization+in+Liquid+Water+Probed+by+Resonant+Inelastic+Soft+X-ray+Scattering.">Ion-Solvation-Induced Molecular Reorganization in Liquid Water Probed by Resonant Inelastic Soft X-ray Scattering.</a> The Journal of Physical Chemistry Letters. 5 (23), 4143-4148 (2014).</li><li>Fuchs, O., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=High-resolution,+high-transmission+soft+x-ray+spectrometer+for+the+study+of+biological+samples.">High-resolution, high-transmission soft x-ray spectrometer for the study of biological samples.</a> Rev Sci Instrum. 80 (6), 063103 (2009).</li><li>Chuang, Y. -. D., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Modular+soft+x-ray+spectrometer+for+applications+in+energy+sciences+and+quantum+materials.">Modular soft x-ray spectrometer for applications in energy sciences and quantum materials.</a> Review of Scientific Instruments. 88 (1), 013110 (2017).</li><li>Qiao, R., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=High-efficiency+in+situ+resonant+inelastic+x-ray+scattering+(iRIXS)+endstation+at+the+Advanced+Light+Source.">High-efficiency in situ resonant inelastic x-ray scattering (iRIXS) endstation at the Advanced Light Source.</a> Review of Scientific Instruments. 88 (3), 033106 (2017).</li><li>Liu, X., Yang, W., Liu, Z. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Recent+Progress+on+Synchrotron-Based+In-Situ+Soft+X-ray+Spectroscopy+for+Energy+Materials.">Recent Progress on Synchrotron-Based In-Situ Soft X-ray Spectroscopy for Energy Materials.</a> Adv Mater. 26 (46), 7710-7729 (2014).</li><li>Guo, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+development+of+in+situ+photon-in/photon-out+soft+X-ray+spectroscopy+on+beamline+7.0.1+at+the+ALS.">The development of in situ photon-in/photon-out soft X-ray spectroscopy on beamline 7.0.1 at the ALS.</a> Journal of Electron Spectroscopy and Related Phenomena. 188, 71-78 (2013).</li><li>Blum, M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Solid+and+liquid+spectroscopic+analysis+(SALSA)-a+soft+x-ray+spectroscopy+endstation+with+a+novel+flow-through+liquid+cell.">Solid and liquid spectroscopic analysis (SALSA)-a soft x-ray spectroscopy endstation with a novel flow-through liquid cell.</a> Review of Scientific Instruments. 80 (12), 123102 (2009).</li><li>Williams, G. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> X-RAY DATA BOOKLET. , (2009).</li><li>Achkar, A. J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Bulk+sensitive+x-ray+absorption+spectroscopy+free+of+self-absorption+effects.">Bulk sensitive x-ray absorption spectroscopy free of self-absorption effects.</a> Physical Review B. 83 (8), 081106 (2011).</li><li>Qiao, R., Chin, T., Harris, S. J., Yan, S., Yang, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Spectroscopic+fingerprints+of+valence+and+spin+states+in+manganese+oxides+and+fluorides.">Spectroscopic fingerprints of valence and spin states in manganese oxides and fluorides.</a> Current Applied Physics. 13 (3), 544-548 (2013).</li></ol>

作者没有什么可透露的。

提高储能材料性能的艰巨挑战需要先进的工具来直接探测电池化合物在电化学操作过程中的化学演化。软 x 射线核级光谱学, 如 sXAS、sXES 和 RIXS, 是检测在库和同胞中所涉及的阴离子和阳离子的临界价态的一种选择工具。
核心级光谱学技术涉及在偶极子选择规则之后, 核心电子对未占用状态的强烈激发。与硬 X 射线相比, 软 X 射线的低能量使对低 Z 阴离子元素 (如 C、N 和 O K 边)...

开发高性能电池是实现具有环保资源和设备的现代能源应用的关键要求之一。开发高效、低成本、可持续的储能设备已经成为电动汽车和电网的关键, 在这个十年中, 预计的蓄能市场将扩大十倍。无处不在的锂离子电池 (LIB) 技术仍然是高能量密度和高能量存储解决方案1的一个有希望的候选者, 而 Na-离子电池 (同胞) 有望实现绿色电网的低成本稳定存储。应用程序2。但是, 电池技术的总体水平远远低于需要满足这一新阶段的大中型能源存储1,3。
开发高性能储能系统面临的紧迫挑战来自于电池操作的复杂机械和电子特性。广泛的工作重点是材料合成和机械性能。然而, 电池电极中特定元素的化学状态的演变往往是新开发的电池材料的积极辩论。一般而言, 在电荷和放电过程中, 库和同胞都与电子和离子的传输所触发的不断变化的电子元件操作, 从而导致特定元素的氧化和还原 (氧化还原) 反应。电池阴极作为许多性能参数的瓶颈, 在研究和开发中得到了很大的关注4,5。一种实用的电池阴极材料通常是一个3d过渡金属 (TM) 氧化物, 具有特定的离子扩散结构通道。传统上, 氧化还原反应仅限于 TM 元素;然而, 最近的结果表明, 氧气可能被用于可逆电化学循环6。氧化还原机理是了解电化学操作的最关键的信息之一, 因此, 对具有元素灵敏度的电池电极的化学状态进行直接探针是非常可取的。
同步辐射, 软 x 射线光谱学是一种先进的技术, 检测在费米水平附近的电池材料的价电子状态7。由于软 x 射线光子对特定元素和轨道的电子具有很高的灵敏度, 软 x 射线光谱学可以作为电池电极8或电池接口中的临界电子状态的直接探针。9. 此外, 与硬 x 射线相比, 软 x 射线在3d TMs10中的低 Z 元素、例如、C、N、O 和2p到3d激发的能量和覆盖激发上较低。
软 x 射线光谱的激发首先是通过从软 x 射线光子吸收能量, 从一个特定的核心状态到未占用状态的电子跃迁。因此, 这种软 x 射线吸收光谱的强度对应于未占用 (传导带) 状态的密度 (DOS) 与激发的核心孔的存在。X 射线吸收系数可以通过检测在衰变过程中发射的光子或电子的总数量来测量。总电子屈服 (泰) 计数发射电子的总数量, 并且因而是光子在电子出 (PIEO) 检测模式。泰有几纳米的浅探针深度, 因此相对表面敏感, 由于电子的浅逸出深度。然而, 作为光子在光子出 (PIPO) 检测模式, 总荧光率 (TFY) 测量发射光子的总数量在 sXAS 过程中。它的探针深度大约是上百纳米, 比泰深。由于探针深度的不同, 泰与 TFY 的对比可以为材料的表面和体积的比较提供重要的信息。
sXES 是一种 PIPO 技术, 对应于退出状态的衰变, 以填充核心孔, 从而导致 X 射线光子在特征能量下的发射。如果核心电子对离 sXAS 阈值很远的连续电子状态感到兴奋, 它是一个非共振 x 射线荧光过程, 对应于被占领 (价带) 电子到核心孔的衰变,即, sXES 反映 DOS的价带状态。否则, 如果核心电子共振激发到精确的吸收阈值, 则产生的发射谱具有强的激发能量依赖性。对于这种情况, 光谱学实验被称为共振非弹性 x 射线散射 (RIXS)。
由于 sXAS 和 sXES 对应于未占用的 (传导带) 和被占领 (价带) 电子状态, 它们分别提供了有关在电池中参与还原和氧化反应的电子状态的互补信息。电化学操作后的电极11。对于低 Z 元素, 特别是 C12、13、N14和 O15、16、17, sXAS 已被广泛用于研究与电子相对应的临界电子态。传输12,13和化学成分15,16,17。对于3d TMs, tm L 边缘的 sXAS 已成功证明是对 V18、锰19、20、21、22的 tm 氧化还原反应的有效探针, 23, Fe23,24,25,26, Co20,27, 和 Ni20,28。由于 tm L sXAS 功能由定义良好的 multiplet 效果控制, 对不同 TM 氧化的敏感度18,19,20,21,22 ,24,25,26,27, 28 和自旋状态14, 29, TM sXAS 数据可以实现甚至定量LIB 和同胞电极中 TM 氧化还原对的分析27。
与 sXAS 在电池材料研究中的流行就业相比, 由于获得与电池性能有关的有意义的信息10的实验和数据解释的复杂性, RIXS 很少被使用。然而, 由于 RIXS 的化学态选择性极高, RIXS 对电池材料中的化学态演化具有内在的元素敏感性有潜在的敏感性。最近的 sXES 和 RIXS 报告 Jeyachandran et., 已经展示了 RIXS 对特定化学结构的高度敏感性在 sXAS30,31之外的离子溶剂化系统中。随着最近快速发展的高效 RIXS 系统32,33,34, RIXS 迅速从一个基本的物理工具转移到一个强大的电池研究技术, 偶尔成为在电池化合物中阳离子和负离子演化的具体研究的选择工具。
在这项工作中, 介绍了 sXAS、sXES 和 RIXS 实验的详细协议。我们涵盖了实验计划的细节、进行实验的技术程序, 更重要的是对不同光谱技术的数据处理。此外, 在电池材料研究中有三个代表性的结果显示了这三软 x 射线光谱学技术的应用。我们注意到, 这些实验的技术细节在不同的终端站和/或设施中可能是不同的。此外, "原位" 和原位实验由于对软 X 射线光谱学35的超高真空的严格要求, 对采样处理有非常不同的设置过程。但是这里的协议代表了典型的程序, 可以作为在不同实验系统中的软 x 射线光谱学实验的共同参考。

<table><tbody><tr><td>&lt;strong&gt;Material&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>Electrode active materials</td><td>various</td><td></td><td>Synthesized in-house or obtained from various suppliers.</td></tr><tr><td>Lithium foil</td><td>Sigma-Aldrich</td><td>320080</td><td>Anode for half cells. Store and handle in an inert atmosphere glovebox under Ar. (www.sigmaaldrich.com)</td></tr><tr><td>Sodium foil</td><td>Sigma-Aldrich</td><td>282065</td><td>Anode for half cells. Store and handle in an inert atmosphere glovebox under Ar. (www.sigmaaldrich.com)</td></tr><tr><td>Electrolyte solutions</td><td>BASF</td><td>Contact vendor for desired formulations</td><td>http://www.catalysts.basf.com/p02/USWeb-Internet/catalysts/en/content/microsites/catalysts/prods-inds/batt-mats/electrolytes</td></tr><tr><td>Synthetic flake graphite</td><td>Timcal</td><td>SFG-6</td><td>Conductive additive for electrodes. (www.timcal.com)</td></tr><tr><td>Indium foil</td><td>Sigma-Aldrich</td><td>357308</td><td>Used if collecting Carbon and Oxygen signals of power samples</td></tr><tr><td>Argon gas</td><td>Air Products</td><td>Custom order, contact vendors</td><td>Argon used to fill glovebox where to assemble and store air-sensitive samples. (http://www.airproducts.com/products/gases.aspx)</td></tr><tr><td>&lt;strong&gt;Eqiupment&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>CCD</td><td>iKon-L</td><td>DO936N</td><td>Used to capture the emission photons when carrying out the sXES or RiXS experiment (http://www.andor.com/scientific-cameras/ikon-xl-and-ikon-large-ccd-series/ikon-l-936)</td></tr><tr><td>Inert atmosphere glovebox</td><td>MBRAUN</td><td>MB200B</td><td>Used during air-sensitive samples assembly and storage. (http://www.mbraun.com/products/glovebox-workstations/mb200b-mod)</td></tr><tr><td>Battery Charge &amp;amp; Discharge Tester</td><td>Bio-Logic</td><td>VMP3</td><td>Used to electrochemical cycling of battery materials. (https://www.bio-logic.net/en/)</td></tr><tr><td>Swagelok cell</td><td>MTI</td><td>EQ-HSTC</td><td>Used to contain the battery for electrochemical cycling</td></tr><tr><td>Sample holder</td><td>manufactured in lab</td><td></td><td>Used to hold the samples in the experiment</td></tr><tr><td>Hardware tools</td><td>various</td><td></td><td>Including tweezers, scissors (used to assemble samples), tongs (used to transfer sample holders), etc.&amp;nbsp;</td></tr><tr><td>Carbon and Copper tape</td><td>3M</td><td>Custom order, contact vendors</td><td>Used to paste the samples onto sample holders</td></tr><tr><td>Igor Pro</td><td>WaveMetrics</td><td>7.06</td><td>Used to process the experiment data. (https://www.wavemetrics.com/index.html)</td></tr></tbody></table>

elemental-sensitive detection of the chemistry in batteries through soft x-ray absorption spectroscopy and resonant inelastic x-ray scattering

能源储存已成为当今可持续能源应用的一个限制因素, 包括电动汽车和基于挥发性太阳能和风力来源的绿色电网。开发高性能电化学储能解决方案的迫切需求,即电池, 依靠学院和工业界的基本理解和实际发展。开发成功的电池技术所面临的巨大挑战源于不同的能源存储应用的不同要求。能量密度、功率、稳定性、安全性和成本参数都必须在电池中平衡, 以满足不同应用的要求。因此, 需要开发和优化基于不同材料和机制的多电池技术。能够直接探测各种电池材料中化学反应的尖锐工具, 对于推进该领域超越常规的试错方法至关重要。在这里, 我们提出了软 x 射线吸收光谱 (sXAS)、软 x 射线发射光谱 (sXES) 和共振非弹性 x 射线散射 (RIXS) 实验的详细协议, 它们是过渡金属固有的元素敏感探针。3d和负离子2p在电池化合物中的状态。通过这些软 x 射线光谱学技术, 我们提供了有关电池材料中关键化学状态的实验技术和演示的详细信息。

示例持有者和粘贴的示例显示在图 1中。图 7是一个典型的 RIXS 图像, 在特定的励磁能量中收集, 光谱仪设置为感兴趣的边缘。此处显示的图像是在电池电极材料上收集的, 林妮0.33Co0.33锰0.33O2, 其励磁能量为 858 ev, 探测器设置在约 500-900 ev 范围内, 以覆盖 O K、锰 l、Co 和镍 L, 如<strong cla...

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Elemental-sensitive Detection of the Chemistry in Batteries through Soft X-ray Absorption Spectroscopy and Resonant Inelastic X-ray Scattering

软 x 射线吸收光谱和共振非弹性 x 射线散射法检测电池化学成分的元素敏感度

本文提出了软 X 射线吸收光谱 (sXAS) 和共振非弹性 x 射线散射 (RIXS) 的典型实验的协议, 并在电池材料研究中的应用。

Energy storage has become more and more a limiting factor of today's sustainable energy applications, including electric vehicles and green electric grid ...

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12.6K 次观看.  Stanford University. 本文提出了软 X 射线吸收光谱 (sXAS) 和共振非弹性 x 射线散射 (RIXS) 的典型实验的协议, 并在电池材料研究中的应用。

视频: Elemental-sensitive Detection of the Chemistry in Batteries through Soft X-ray Absorption Spectroscopy and Resonant Inelastic X-ray Scattering

Characterization of Electrode Materials for Lithium Ion and Sodium Ion Batteries Using Synchrotron Radiation Techniques

Intercalation compounds such as transition metal oxides or phosphates are the most commonly used electrode materials in Li-ion and Na-ion batteries. During insertion or removal of alkali metal ions, the redox states of transition metals in the compounds change and structural transformations such as phase transitions and/or lattice parameter increases or decreases occur. These behaviors in turn determine important characteristics of the batteries such as the potential profiles, rate capabilities, and cycle lives. The extremely bright and tunable x-rays produced by synchrotron radiation allow rapid acquisition of high-resolution data that provide information about these processes. Transformations in the bulk materials, such as phase transitions, can be directly observed using X-ray diffraction (XRD), while X-ray absorption spectroscopy (XAS) gives information about the local electronic and geometric structures (e.g.&#160;changes in redox states and bond lengths). In situ experiments carried out on operating cells are particularly useful because they allow direct correlation between the electrochemical and structural properties of the materials. These experiments are time-consuming and can be challenging to design due to the reactivity and air-sensitivity of the alkali metal anodes used in the half-cell configurations, and/or the possibility of signal interference from other cell components and hardware. For these reasons, it is appropriate to carry out ex situ experiments (e.g.&#160;on electrodes harvested from partially charged or cycled cells) in some cases. Here, we present detailed protocols for the preparation of both ex situ and in situ samples for experiments involving synchrotron radiation and demonstrate how these experiments are done.

We describe the use of synchrotron X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) techniques to probe details of intercalation/deintercalation processes in electrode materials for Li-ion and Na-ion batteries. Both in situ and ex situ experiments are used to understand structural behavior relevant to the operation of devices

正极材料的同步辐射技术锂离子和钠离子电池表征

Intercalation compounds such as transition metal oxides or phosphates are the most commonly used electrode materials in Li-ion and Na-ion batteries. ...

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 ...

Energy Dispersive X-ray Tomography for 3D Elemental Mapping of Individual Nanoparticles

Energy dispersive X-ray spectroscopy within the scanning transmission electron microscope (STEM) provides accurate elemental analysis with high spatial resolution, and is even capable of providing atomically resolved elemental maps. In this technique, a highly focused electron beam is incident upon a thin sample and the energy of emitted X-rays is measured in order to determine the atomic species of material within the beam path. This elementally sensitive spectroscopy technique can be extended to three dimensional tomographic imaging by acquiring multiple spectrum images with the sample tilted along an axis perpendicular to the electron beam direction.
Elemental distributions within single nanoparticles are often important for determining their optical, catalytic and magnetic properties. Techniques such as X-ray tomography and slice and view energy dispersive X-ray mapping in the scanning electron microscope provide elementally sensitive three dimensional imaging but are typically limited to spatial resolutions of &gt; 20 nm. Atom probe tomography provides near atomic resolution but preparing nanoparticle samples for atom probe analysis is often challenging. Thus, elementally sensitive techniques applied within the scanning transmission electron microscope are uniquely placed to study elemental distributions within nanoparticles of dimensions 10-100 nm.
Here, energy dispersive X-ray (EDX) spectroscopy within the STEM is applied to investigate the distribution of elements in single AgAu nanoparticles. The surface segregation of both Ag and Au, at different nanoparticle compositions, has been observed.

The use of energy dispersive X-ray tomography in the scanning transmission electron microscope to characterize elemental distributions within single nanoparticles in three dimensions is described.

能量色散X射线断层摄影术对个人纳米3D元素映射

Energy dispersive X-ray spectroscopy within the scanning transmission electron microscope (STEM) provides accurate elemental analysis with high spatial ...

Failure Analysis of Batteries Using Synchrotron-based Hard X-ray Microtomography

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent of lithium-ion batteries, researchers have known that the lithium metal anode has the highest theoretical energy density of any anode material. However, rechargeable batteries containing a lithium metal anode are not widely used in consumer products because the growth of lithium dendrites from the anode upon charging of the battery causes premature cell failure by short circuit. Lithium dendrites can also form in commercial lithium-ion batteries with graphite anodes if they are improperly charged. We demonstrate that lithium dendrite growth can be studied using synchrotron-based hard X-ray microtomography. This non-destructive imaging technique allows researchers to study the growth of lithium dendrites, in addition to other morphological changes inside batteries, and subsequently develop methods to extend battery life.

Synchrotron-based hard X-ray microtomography is used to image the electrochemical growth of dendrites from a lithium metal electrode through a solid polymer electrolyte membrane.

电池的使用同步为基础的硬X射线微断层故障分析

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent ...

Detection and Recovery of Palladium, Gold and Cobalt Metals from the Urban Mine Using Novel Sensors/Adsorbents Designated with Nanoscale Wagon-wheel-shaped Pores

Developing low-cost, efficient processes for recovering and recycling palladium, gold and cobalt metals from urban mine remains a significant challenge in industrialized countries. Here, the development of optical mesosensors/adsorbents (MSAs) for efficient recognition and selective recovery of Pd(II), Au(III), and Co(II) from urban mine was achieved. A simple, general method for preparing MSAs based on using high-order mesoporous monolithic scaffolds was described. Hierarchical cubic Ia3d wagon-wheel-shaped MSAs were fabricated by anchoring chelating agents (colorants) into three-dimensional pores and micrometric particle surfaces of the mesoporous monolithic scaffolds. Findings show, for the first time, evidence of controlled optical recognition of Pd(II), Au(III), and Co(II) ions and a highly selective system for recovery of Pd(II) ions (up to ~95%) in ores and industrial wastes. Furthermore, the controlled assessment processes described herein involve evaluation of intrinsic properties (e.g., visual signal change, long-term stability, adsorption efficiency, extraordinary sensitivity, selectivity, and reusability); thus, expensive, sophisticated instruments are not required. Results show evidence that MSAs will attract worldwide attention as a promising technological means of recovering and recycling palladium, gold and cobalt metals.

Because of the importance and extensive use of palladium, gold and cobalt metals in high-technology equipment, their recovery and recycling constitute an important industrial challenge. The metal recovery system described herein is a simple, low-cost means for the effective detection, removal, and recovery of these metals from the urban mine.

检测和钯的回收，从城市矿山黄金和钴金属使用标有纳米货车车轮形的孔隙新型传感器/吸附剂

Developing low-cost, efficient processes for recovering and recycling palladium, gold and cobalt metals from urban mine remains a significant challenge in ...

Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery

We demonstrate a method for electrochemical testing of an aprotic Li-O2 battery. An aprotic Li-O2 battery is made of a Li-metal anode, an aprotic electrolyte, and an O2-breathing cathode. The aprotic electrolyte is a solution of lithium salt with aprotic solvent; and porous carbon is commonly used as the cathode substrate. To improve the performance, an electrocatalyst is deposited onto the porous carbon substrate by certain deposition methods, such as atomic layer deposition (ALD) and wet-chemistry reaction. The as-prepared cathode materials are characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray absorption near edge structure (XANES). A Swagelok-type cell, sealed in a glass chamber filled with pure O2, is used for the electrochemical test on a battery test system. The cells are tested under either capacity-controlled mode or voltage controlled mode. The reaction products are investigated by electron microscopy, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy, and Raman spectroscopy to study the possible pathway of oxygen reduction reaction (ORR) and oxygen evolution reaction (OER). This protocol demonstrates a systematic and efficient arrangement of routine tests of the aprotic Li-O2 battery, including the electrochemical test and characterization of battery materials.

Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery

A protocol for the electrochemical testing of an aprotic Li-O2 battery with the preparation of electrodes and electrolytes and an introduction of the frequently used methods of characterization is presented here.

电化学测试的协议及表征非质子锂的O<sub&gt; 2</sub&gt;电池

We demonstrate a method for electrochemical testing of an aprotic Li-O2 battery. An aprotic Li-O2 battery is made of a Li-metal anode, an aprotic ...

Quantifying X-Ray Fluorescence Data Using MAPS

The quantification of X-ray fluorescence (XRF) microscopy maps by fitting the raw spectra to a known standard is crucial for evaluating chemical composition and elemental distribution within a material. Synchrotron-based XRF has become an integral characterization technique for a variety of research topics, particularly due to its non-destructive nature and its high sensitivity. Today, synchrotrons can acquire fluorescence data at spatial resolutions well below a micron, allowing for the evaluation of compositional variations at the nanoscale. Through proper quantification, it is then possible to obtain an in-depth, high-resolution understanding of elemental segregation, stoichiometric relationships, and clustering behavior.
This article explains how to use the MAPS fitting software developed by Argonne National Laboratory for the quantification of full 2-D XRF maps. We use as an example results from a Cu(In,Ga)Se2 solar cell, taken at the Advanced Photon Source beamline 2-ID-D at Argonne National Laboratory. We show the standard procedure for fitting raw data, demonstrate how to evaluate the quality of a fit and present the typical outputs generated by the program. In addition, we discuss in this manuscript certain software limitations and offer suggestions for how to further correct the data to be numerically accurate and representative of spatially resolved, elemental concentrations.

Here, we demonstrate the use of the X-ray fluorescence fitting software, MAPS, created by Argonne National Laboratory for the quantification of fluorescence microscopy data. The quantified data that results is useful for understanding the elemental distribution and stoichiometric ratios within a sample of interest.

利用地图量化 X 射线荧光数据

The quantification of X-ray fluorescence (XRF) microscopy maps by fitting the raw spectra to a known standard is crucial for evaluating chemical ...

化学

Fabrication of a Dipole-assisted Solid Phase Extraction Microchip for Trace Metal Analysis in Water Samples

This paper describes a fabrication protocol for a dipole-assisted solid phase extraction (SPE) microchip available for trace metal analysis in water samples. A brief overview of the evolution of chip-based SPE techniques is provided. This is followed by an introduction to specific polymeric materials and their role in SPE. To develop an innovative dipole-assisted SPE technique, a chlorine (Cl)-containing SPE functionality was implanted into a poly(methyl methacrylate) (PMMA) microchip. Herein, diverse analytical techniques including contact angle analysis, Raman spectroscopic analysis, and laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) analysis were employed to validate the utility of the implantation protocol of the C-Cl moieties on the PMMA. The analytical results of the X-ray absorption near-edge structure (XANES) analysis also demonstrated the feasibility of the Cl-containing PMMA used as an extraction medium by virtue of the dipole-ion interactions between the highly electronegative C-Cl moieties and the positively charged metal ions.

The fabrication protocol of a dipole-assisted solid phase extraction microchip for the trace metal analysis is presented.

水样中偶极辅助固相萃取Microchip的痕量金属分析的制作

This paper describes a fabrication protocol for a dipole-assisted solid phase extraction (SPE) microchip available for trace metal analysis in water ...

生物工程

Nanoscale Characterization of Liquid-Solid Interfaces by Coupling Cryo-Focused Ion Beam Milling with Scanning Electron Microscopy and Spectroscopy

Physical and chemical processes at solid-liquid interfaces play a crucial role in many natural and technological phenomena, including catalysis, solar energy and fuel generation, and electrochemical energy storage. Nanoscale characterization of such interfaces has recently been achieved using cryogenic electron microscopy, thereby providing a new path to advancing our fundamental understanding of interface processes.
This contribution provides a practical guide to mapping the structure and chemistry of solid-liquid interfaces in materials and devices using an integrated cryogenic electron microscopy approach. In this approach, we pair cryogenic sample preparation which allows stabilization of solid-liquid interfaces with cryogenic focused ion beam (cryo-FIB) milling to create cross-sections through these complex buried structures. Cryogenic scanning electron microscopy (cryo-SEM) techniques performed in a dual-beam FIB/SEM enable direct imaging as well as chemical mapping at the nanoscale. We discuss practical challenges, strategies to overcome them, as well as protocols for obtaining optimal results. While we focus in our discussion on interfaces in energy storage devices, the methods outlined are broadly applicable to a range of fields where solid-liquid interface play a key role.

Cryogenic Focused Ion Beam (FIB) and Scanning Electron Microscopy (SEM) techniques can provide key insights into the chemistry and morphology of intact solid-liquid interfaces. Methods for preparing high quality Energy Dispersive X-ray (EDX) spectroscopic maps of such interfaces are detailed, with a focus on energy storage devices.

通过冷冻聚焦离子束铣削与扫描电子显微镜和光谱学耦合，对液固界面进行纳米级表征

Physical and chemical processes at solid-liquid interfaces play a crucial role in many natural and technological phenomena, including catalysis, solar ...

Screening of Coatings for an All-Solid-State Battery Using In Situ Transmission Electron Microscopy

With the ever-increasing use of Li-ion batteries, especially due to their adoption in electric vehicles, their safety is in prime focus. Thus, the all-solid-state batteries (ASSBs) that use solid electrolytes instead of liquid electrolytes, which reduce the risk of flammability, have been the center stage of battery research for the last few years. However, in the ASSB, the ion transportation through the solid-solid electrolyte-electrode interface poses a challenge due to contact and chemical/electrochemical stability issues. Applying a suitable coating around the electrode and/or electrolyte particles offers a convenient solution, leading to better performance. For this, researchers are screening potential electronic/ionic conductive and nonconductive coatings to find the best coatings with suitable thickness for long-term chemical, electrochemical, and mechanical stability. Operando transmission electron microscopy (TEM) couples high spatial resolution with high temporal resolution to allow visualization of dynamic processes, and thus is an ideal tool to evaluate electrode/electrolyte coatings via studying (de)lithiation at a single particle level in real-time. However, the accumulated electron dose during a typical high-resolution in situ work may affect the electrochemical pathways, evaluation of which can be time-consuming. The current protocol presents an alternative procedure in which the potential coatings are applied on Si nanoparticles and are subjected to (de)lithiation during operando TEM experiments. The high volume changes of Si nanoparticles during (de)lithiation allow monitoring of the coating behavior at a relatively low magnification. Thus, the whole process is very electron-dose efficient and offers quick screening of potential coatings.

Screening of Coatings for an All-Solid-State Battery Using In Situ Transmission Electron Microscopy

Utilizing the volume change of Si nanoparticles during (de)lithiation, the present protocol describes a screening method of potential coatings for all-solid-state batteries using in situ transmission electron microscopy.

软 x 射线吸收光谱和共振非弹性 x 射线散射法检测电池化学成分的元素敏感度

摘要

探索更多视频

此视频中的章节

正极材料的同步辐射技术锂离子和钠离子电池表征

原位中子衍射用特制的锂离子电池

能量色散X射线断层摄影术对个人纳米3D元素映射

电池的使用同步为基础的硬X射线微断层故障分析

检测和钯的回收，从城市矿山黄金和钴金属使用标有纳米货车车轮形的孔隙新型传感器/吸附剂

电化学测试的协议及表征非质子锂的O

利用地图量化 X 射线荧光数据

水样中偶极辅助固相萃取Microchip的痕量金属分析的制作

通过冷冻聚焦离子束铣削与扫描电子显微镜和光谱学耦合，对液固界面进行纳米级表征

使用原位透射电子显微镜筛选全固态电池涂层

软 x 射线吸收光谱和共振非弹性 x 射线散射法检测电池化学成分的元素敏感度

摘要

探索更多视频

此视频中的章节

正极材料的同步辐射技术锂离子和钠离子电池表征

原位中子衍射用特制的锂离子电池

能量色散X射线断层摄影术对个人纳米3D元素映射

电池的使用同步为基础的硬X射线微断层故障分析

检测和钯的回收，从城市矿山黄金和钴金属使用标有纳米货车车轮形的孔隙新型传感器/吸附剂

电化学测试的协议及表征非质子锂的O

利用地图量化 X 射线荧光数据

水样中偶极辅助固相萃取Microchip的痕量金属分析的制作

通过冷冻聚焦离子束铣削与扫描电子显微镜和光谱学耦合，对液固界面进行纳米级表征

使用 原位 透射电子显微镜筛选全固态电池涂层

使用原位透射电子显微镜筛选全固态电池涂层