Name: in situ neutron powder diffraction using custom-made lithium-ion batteries
Uploaded: 2014-11-10T15:00:00
Description: Watch this Scientific Journal Video about In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries at JoVE.com

We thank AINSE Ltd for providing support through the research fellowship and postgraduate award scheme.

1.需要电池组件在施工前注：钒可以被常规用于NPD的实验，它是被密封的一端，而在另一公开的全钒管。因此几乎从钒NPD的数据没有信号。 <ol><li>切下一块锂金属箔的向尺寸相匹配的钒罐的容积。例如，切一块约120×35毫米，9毫米口径的钒即可。此外，使用更薄的锂箔，以尽量减少中子吸收，并指出，厚度小于125微米可能难以处理而不会撕裂。 </li><li>预选择分离器的类型可?...

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Power Sources. 236, 163-168 (2013).</li><li>Doeff, M. 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=Characterization+of+electrode+materials+for+lithium+ion+and+sodium+ion+batteries+using+synchrotron+radiation+techniques.">Characterization of electrode materials for lithium ion and sodium ion batteries using synchrotron radiation techniques.</a> J. Visualized Exp. , 50591-50594 (2013).</li></ol>

当设计和现场试验执行，或者用“翻车”中子衍射细胞或另一种设计方案中，有一个数字，必须小心地控制，以确保成功的实验方面。这些包括仔细选择的类型和细胞组分的量，以确保所制得的电极和最终构建的细胞都是高质量的，选择合适的衍射条件，规划的电化学循环的步骤可以预先进行，终于了解什么产生的数据也并不能告诉一个约的材料正在调查中。 细胞成?...

可充电锂离子电池为现代电子设备提供便携的能量，并在高能应用中非常重要，如电动汽车，并为大规模可再生能源发电的储能装置。3-7仍然存在一些挑战，实现普遍使用的可充电电池中的车辆与大型存储，包括能量密度和安全性。 原位方法中的用途的探测原子和分子级的电池功能操作期间正变得越来越普遍，获得了在这些实验中的信息可以直接的方法来改进现有的电池材料， 例如 ，通过确定可能的故障机制，8-10和通过揭示晶体结构可以考虑为下一代的材料。11 原位 NPD的主要目标是探测电池内部组件的晶体结构演变作为充电/放电的功能。为了测量晶体结构演变的组件必须是结晶，其重点是晶体有序电极等的研究。它是在该电荷载流子（锂）插入/抽出而这种变化之后的NPD的电极。 原位 NPD提供了可能性“跟踪”不仅反应机理和晶格参数的电极的演进，也插入/抽出从电极锂。基本上在锂离子电池的电荷载流子可以遵循。这使电池功能的锂为中心的视图，并且在只有少数的研究最近已经证明11-13 NPD是一种理想的技术，研究含有锂的材料和锂离子电池。这是因为，NPD的依赖于中子束和样品之间的相互作用。不像X射线粉末衍射（XRD），其中，所述相互作用的X射线辐射主要是与样品中的电子，从而线性地原子序数而变化，在NPD的相互作用是由导致更复杂的和明显的随机变异原子序数中子核的相互作用介导的。因此， 在原位 NPD是用于锂离子电池材料研究特别有希望的，由于多种因素，如NPD的朝锂原子在较重的元素的存在下的敏感性，中子与所述电池的非破坏性的相互作用，以及高穿透深度的中子使商用设备中使用的尺寸的整个电池中的电池组件的块状晶体结构的检查。因此， 原位 NPD是用于锂离子电池的研究，这些优势的结果是特别有用的。尽管如此， 在现场 NPD实验的电池研究界的摄取是有限的，仅占25出版物罪CE 1998年14所述的吸收有限是采用原位 NPD为电池研究的第一份报告，由于一些主要实验的障碍，如需要占很大的非相干中子散射横氢在电解质溶液和隔膜部在电池中，这是不利的NPD的信号。这通常是通过用与氘（2H）电解质溶液并用备用的无氢或较差的材料代替隔板克服15的另一个障碍是，需要有足够的样品中的中子束，一个要求，即往往需要使用的较厚的电极而这又限制了最大充电/可施加到电池放电速率。一个更实际关注的是相对小一些世界范围内的中子衍射仪相对于X射线衍射仪，其能力- 例如时间和角分辨率。随着新的中子diffractomeTER值都来网上和上述障碍克服， 就地 NPD实验种植数量。 有两个选项进行原位 NPD的实验中，使用商业或定制细胞。商业的细胞已被证明以显示结构的信息，包括锂的含量和分布在电极上的演变。8-11,16-20但是，使用商用单元限制了可以研究那些已经市售的电极的数量，并且其中厂家或选择研究设施从事生产商用型细胞尚未未商业化的材料。商用型电池的生产依赖于足量的电极材料用于制作电池的情况，典型的公斤的量级和显著高于电池的研究中使用，它可以是一个障碍，细胞产量更高。商业细胞TYpically设有两个电极中的充电/放电是进化和两个电极的演化会在所得的衍射图案被捕获。这是因为，中子束高度穿透性和能穿透单个锂离子电池（ 例如 ，18650细胞的整个体积）。两个电极的演变可以使数据的分析变得复杂，但是，如果两个电极的足够的布拉格反射被观测到，这些可使用全粉图案的方法来模拟。但是，定做半电池可以构造在其中一个电极是锂，且应在充电/放电结构上不发生变化，因此，作为一个（或另一个）内部标准。只留下一个应该表现出结构性变化，简化了数据分析电极。也必须小心，以确保所有感兴趣的电极反射不与其他组件的反射发生在细胞结构变化的重叠。广告定做的细胞的优势在于，组件可以被交换，以改变在衍射图案反射位置。此外，定制的细 ​​胞使得研究者的选项，在原则上，改善信号对噪声的比率，并调查所取得在较小规模的研究批次，由此允许更大的各种材料的原位 NPD的研究材料。 到目前为止，已经在原位的NPD的研究已经6的电化学电池设计为报告，其中包括三个圆柱形设计，14,15,21,22 2的硬币型电池的设计23-26和袋的单元设计。12,27第一圆柱形电池设计中使用限于非常低的充电/由于大量的电极材料使用的放电速率。14,21的翻转的设计，下面15详细描述的，修改后的版本的原始筒状细胞的22克服了许多的与T有关的问题他第一圆柱形设计，并且可以用于可靠地相关联的电极材料的结构与其电化学。硬币电池设计用于原位 NPD还允许相似量的电极材料被探测相对于该翻转单元，同时具有在施工，适用的充电率和成本方面的细微差别。15具体地，币形电池类型最近有报道使用的Ti-Zn系合金作为外壳材料（零矩阵），它产生没有信号在NPD的图案已经被建造。26这类似于以下描述的翻车设计的使用钒罐。能够影响适用的充电/放电率（和偏振）的关键因素是电极的厚度，其中典型地较厚的电极需要低电流的应用。小区设计，现在变得更流行的是小袋的细胞与并联连接的多个个体的细胞，或片材的片材看得太被卷在一个类似的方式的锂离子电池中的移动电子设备中找到的建筑。12,27这种细胞是矩形（袋），其可以在更高的充电/放电率比翻车或硬币型函数细胞。在这项工作中，我们把重点放在&#39;翻车&#39;单元设计，显示单元建设，使用，以及使用电池了一定的成效。 该电极准备翻车设计的电池实际上是类似的电极制备用于传统纽扣电池使用到。该电极可浇铸到集电体通过刮刀，具有最大的不同之处在于，电极需要跨越尺寸大于35×120-150毫米。这可能难以均匀地涂布与每一个电极的材料。在集电体上的集电体，隔板和锂金属箔与电极的层布置，轧制，并插入到钒罐。电解液使用d为的LiPF 6，在锂离子电池用氘代碳酸乙烯酯和氘代碳酸二甲酯是最常用的一种盐。此细胞已被成功地用于在四个报告的研究和在下文中更详细地描述。15,28-30

<table border="0" cellpadding="0" cellspacing="0" width="1426">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:347px;">Name of Material/ Equipment</td>
			<td style="width:159px;">Company</td>
			<td style="width:119px;">Catalog Number</td>
			<td style="width:801px;">Comments/Description</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Slurry Preparation</td>
			<td style="width:159px;"></td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">PVDF</td>
			<td style="width:159px;">MTI Corporation</td>
			<td style="width:119px;">EQ-Lib-PVDF</td>
			<td>http://www.mtixtl.com/PVDFbinderforLi-ionbatteryelectrodes80g/bag-EQ-Lib-PVDF.aspx</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Active Electrode Material</td>
			<td style="width:159px;">Researcher makes*</td>
			<td style="width:119px;"></td>
			<td>This is dependent on the electrode under investigation, typically made in-house by the researcher and varies every time</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Carbon black</td>
			<td style="width:159px;">MTI Corporation</td>
			<td style="width:119px;">EQ-Lib-SuperC65</td>
			<td>http://www.mtixtl.com/TimicalSUPERC65forLithium-IonBatteries80g/bag-EQ-Lib-SuperC65.aspx</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">NMP</td>
			<td style="width:159px;">MTI Corporation</td>
			<td style="width:119px;">EQ-Lib-NMP</td>
			<td>http://www.mtixtl.com/N-Methyl-2-pyrrolidoneNMPsolventforPVDF 
			250g/bottleLib-NMP.aspx</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;">Magnetic stirrer</td>
			<td style="width:159px;">IKA</td>
			<td style="width:119px;">C-MAG HS 7 IKAMAG</td>
			<td>http://www.ika.in/owa/ika/catalog.product_detail?iProduct=3581200</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:347px;"></td>
			<td style="width:159px;"></td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Electrode Fabrication</td>
			<td style="width:159px;"></td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;">Doctor blade (notch bar)</td>
			<td style="width:159px;">DPM Solutions Inc.</td>
			<td style="width:119px;">100, 200, 300 &#38; 400 micron&#160; 4-Sided Notch Bar</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Al or Cu current collectors</td>
			<td style="width:159px;">MTI Corporation</td>
			<td style="width:119px;">EQ-bcaf-15u-280</td>
			<td>http://www.mtixtl.com/AluminumFoilforBatteryCathodeSub 
			strate-EQ-bcaf-15u-280.aspx</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Vacuum Oven</td>
			<td style="width:159px;">Binder</td>
			<td style="width:119px;">e.g. VD 53</td>
			<td>http://www.binder-world.com/en/vacuum-drying-oven/vd-series/vd-53/</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Flat-plate press</td>
			<td style="width:159px;">MTI Corporation</td>
			<td style="width:119px;">EQ-HP-88V-LD</td>
			<td>http://www.mtixtl.com/25THydraulicFlat 
			HotPress-EQ-HP-88V.aspx</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:347px;"></td>
			<td style="width:159px;"></td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Roll-over cell construction</td>
			<td style="width:159px;"></td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">V can</td>
			<td style="width:159px;"></td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">electrode on Al/Cu</td>
			<td style="width:159px;">MTI Corporation</td>
			<td style="width:119px;">EQ-bcaf-15u-280</td>
			<td>http://www.mtixtl.com/AluminumFoilforBatteryCathodeSub 
			strate-EQ-bcaf-15u-280.aspx</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;">polyethylene-based or PVDF membrane</td>
			<td style="width:159px;">MTI Corporation</td>
			<td style="width:119px;">EQ-bsf-0025-400C</td>
			<td>http://www.mtixtl.com/separatorfilm-EQ-bsf-0025-400C.aspx</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">LiPF6</td>
			<td style="width:159px;">Sigma-Aldrich</td>
			<td style="width:119px;">450227</td>
			<td>http://www.sigmaaldrich.com/catalog/product/aldrich/450227?lang=en&#38;region=AU</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">deuterated dimethyl carbonate</td>
			<td style="width:159px;">Cambridge Isotopes</td>
			<td style="width:119px;">DLM-3903-PK&#160;</td>
			<td>http://shop.isotope.com/productdetails.aspx?id=10032379&#38;itemno=DLM-3903-PK</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">deuterated ethylene carboante</td>
			<td style="width:159px;">CDN Isotopes</td>
			<td style="width:119px;">D-5489</td>
			<td>https://www.cdnisotopes.com/as/products/specifications/D-5489.php?ei=YWVraWmjoJ1i0lZ7nkr0RpwHr 
			Hxc9ornu14O4WUtZKbZWZrcq6j55 
			G0lOab3Wi0dMZ7xc+0Yse1leWVtZ 
			LnrGKvta7v591o4JrnkbRowHt/r</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Li metal foil</td>
			<td style="width:159px;">MTI Corporation</td>
			<td style="width:119px;">Lib-LiF-30M</td>
			<td>http://www.mtixtl.com/Li-Foil-30000mmL-35mmW-0.17mm 
			Th.aspx</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Rubber stopper cut to size</td>
			<td style="width:159px;">generic eraser</td>
			<td style="width:119px;"></td>
			<td>cut a generic eraser to size</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">dental wax</td>
			<td style="width:159px;">Ainsworth Dental</td>
			<td>AIW042</td>
			<td>http://www.ainsworthdental.com.au/catalogue/Ainsworth-Modelling-Wax-500g.html</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Copper wire (insulated)</td>
			<td style="width:159px;">generic</td>
			<td style="width:119px;"></td>
			<td>sheathed Cu wire that can be cut to size</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Aluminium rod (&#60;2mm diameter)</td>
			<td style="width:159px;">generic</td>
			<td style="width:119px;"></td>
			<td>cut to size as required</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Glovebox</td>
			<td style="width:159px;">Mbraun</td>
			<td style="width:119px;">UNILab</td>
			<td>http://www.mbraun.com/products/glovebox-workstations/unilab-glovebox/</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Scissors&#160;</td>
			<td style="width:159px;">generic</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Soldering iron</td>
			<td style="width:159px;">generic</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:347px;"></td>
			<td style="width:159px;"></td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">In situ NPD</td>
			<td style="width:159px;"></td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Appropriate neutron diffractometer</td>
			<td style="width:159px;">ANSTO</td>
			<td style="width:119px;">Wombat</td>
			<td>http://www.ansto.gov.au/ResearchHub/Bragg/Facilities/Instruments/Wombat/</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Potentiostat/galvanostat</td>
			<td style="width:159px;">Autolab</td>
			<td style="width:119px;">PGSTAT302N</td>
			<td>http://www.ecochemie.nl/Products/Echem/NSeriesFolder/PGSTAT302N</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Connections to battery from potentiostat/galvanostat</td>
			<td style="width:159px;">generic</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Training of NPD instrument and use</td>
			<td style="width:159px;"></td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:347px;"></td>
			<td style="width:159px;"></td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Data analysis</td>
			<td style="width:159px;"></td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Data visualisation and peak fitting, .e.g. LAMP suite</td>
			<td style="width:159px;">ILL</td>
			<td style="width:119px;">LAMP</td>
			<td>http://www.ill.eu/instruments-support/computing-for-science/cs-software/all-software/lamp/</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Rietveld analysis software, e.g. GSAS</td>
			<td style="width:159px;">APS</td>
			<td style="width:119px;">GSAS</td>
			<td>https://subversion.xray.aps.anl.gov/trac/EXPGUI</td>
		</tr>
	</tbody>
</table>

in situ neutron powder diffraction using custom-made lithium-ion batteries

锂离子电池被广泛应用于便携式电子装置和被认为是有前途的候选者能量较高的应用，如电动汽车。1,2-然而，许多挑战，如能量密度和电池寿命，需要在此之前尤其要克服电池技术可广泛实施中这样的应用程序。3本研究是具有挑战性的，并且我们概述的方法，以解决利用原位 NPD的探测电极进行电化学循环（充电/放电）在电池中的晶体结构，这些挑战。 NPD的数据帮助确定负责一系列的电极性能的潜在的结构性机制，这些信息可以直接更好的电极和电池的发展。 我们简要回顾一下六类电池设计定做的NPD的实验和细节构造“翻转”电池，我们有方法成功地用在高强度NPD仪，WOMBAT，在澳大利亚核科学和技术组织（ANSTO）。用于细胞结构的设计考虑和材料结合实际的原位 NPD的实验和初始方向的各方面讨论给出关于如何分析这样复杂的现场数据。

我们已经证明了通用性使用文献15,28-30此翻车细胞，在这里我们提出一个例子与李锶0.18 0.66 0.5钛铌0.5 O 3电极。32 之前尝试顺序Rietveld精修（全谱拟合为充电状态的函数），多相模型到第一数据集的一个单一的细化进行，在该数据收集之前，当前的应用程序的原始细胞。几种模式进行了测试，以确定哪个结构参数可以精确地细化。理想?...

Watch this Scientific Journal Video about In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries at JoVE.com

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

我们描述了电极材料采用原位中子衍射（NPD）考试的电化学电池的设计和施工。我们简单地交替在原地 NPD单元设计意见，并讨论了相应的使用这种细胞原位产生的NPD数据的分析方法。

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 ...

Research

JoVE Journal

Engineering

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

Construction and Testing of Coin Cells of Lithium Ion Batteries

钮扣电池锂离子电池的建设和测试

Rechargeable lithium ion batteries have wide applications in electronics, where customers always demand more capacity and longer lifetime.  Lithium ion ...

科研

工程学

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

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. ...

Measuring Material Microstructure Under Flow Using 1-2 Plane Flow-Small Angle Neutron Scattering

测量材料在微流使用1-2面流小角中子散射

A new small-angle neutron scattering (SANS) sample environment optimized for studying the microstructure of complex fluids under simple shear flow is ...

Using Neutron Spin Echo Resolved Grazing Incidence Scattering to Investigate Organic Solar Cell Materials

使用中子自旋回声解决放牧发生率散射调查有机太阳能电池材料

The spin echo resolved grazing incidence scattering (SERGIS) technique has been used to probe the length-scales associated with irregularly shaped ...

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

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 ...

Non-aqueous Electrode Processing and Construction of Lithium-ion Coin Cells

锂离子纽扣电池的非水电极加工和施工

Research into new and improved materials to be utilized in lithium-ion batteries (LIB) necessitates an experimental counterpart to any computational ...

Measuring Spray Droplet Size from Agricultural Nozzles Using Laser Diffraction

从农业喷嘴采用激光衍射测量喷雾的雾滴尺寸

When making an application of any crop protection material such as an herbicide or pesticide, the applicator uses a variety of skills and information to ...

Dielectric RheoSANS &#8212; Simultaneous Interrogation of Impedance, Rheology and Small Angle Neutron Scattering of Complex Fluids

Dielectric RheoSANS ÃƒÆ’Ã‚Â¢ÃƒÂ¢Ã¢â‚¬Å¡Ã‚Â¬ÃƒÂ¢Ã¢â€šÂ¬Ã‚Â Simultaneous Interrogation of Impedance, Rheology and Small Angle Neutron Scattering of Complex Fluids

介电RheoSANS  - 阻抗，流变性和复杂流体的小角中子散射的同时拷问

A procedure for the operation of a new dielectric RheoSANS instrument capable of simultaneous interrogation of the electrical, mechanical and ...

Characterization of Ultra-fine Grained and Nanocrystalline Materials Using Transmission Kikuchi Diffraction

超细晶和纳米晶材料的表征采用透射菊池衍射

One of the challenges in microstructure analysis nowadays resides in the reliable and accurate characterization of ultra-fine grained (UFG) and ...

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

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

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

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