我们感谢教授马克·阿贝（UGA）为碳酸盐在这项工作中使用的钡提供的近红外成像设备和Rasik Raythatha博士（苏威高性能化学品）。我们承认以赛亚·诺里斯（UGA本科）和Terra布莱文斯（北奥科尼高中），谁帮助测试合成方法的努力。

1，准备CaCuSi 4 O 10 <ol><li> CaCuSi 4 O 10的熔体通量合成<ol><li>称出的CaCO 3，SiO 2的，和Cu 2 CO 3（OH）2在2点08分01秒的摩尔比：SiO 2的，0.1470克的碳酸钙 ，0.3196克（5.319毫摩尔）的0.1331克（1.330毫摩尔）（ 0.6648毫摩尔的Cu 2 CO 3）（OH）2。此外，掂量出焊剂成分（按重量计12.5％）。0.0375克的Na 2 CO 3的0.0125克氯化钠，并0.0250克的Na 2 B 4 O 7 10H 2 O。这些材料加入到一个干净的玛瑙研钵。 </li><li>手磨为〜5分钟用玛瑙杵直到混合物变成均匀的浅绿色粉末（ 图1a和图2a）。这种混合物转移到一个干净，干燥的铂金坩埚。 </li><li>加热在炉中的坩埚中，以875℃（2℃/ min的升温速率），保持在875℃下进行16小时，然后冷却至室温（速率为0.8℃/分钟）。 </li><li>从坩埚中取出晶体，轻轻地用杵粉碎他们。 </li><li>让该晶体在50ml的1M HCl水溶液中浸泡过夜，以除去熔融焊剂。 </li><li>过滤和结晶用去离子水冲洗，以完全消除任何剩余的熔助焊剂。 注意：该材料应磨成更细的粉末的粉末X射线衍射（PXRD）分析（ 图5）。它也可被表征通过光学显微镜（ 图3），扫描电子显微镜（SEM）（ 图4），和近红外照相（ 图8）。 </li></ol></li><li> CaCuSi 4 O 10的固相合成<ol><li>称出的CaCO 3，SiO 2的和CuO在1点04分01秒的摩尔比：0.1331克（1.330毫摩尔）的CaCO 3，0.3196克（5.319毫摩尔）的SiO 2，和0.1058克氧化铜（1.330毫摩尔）并加入到一个干净的玛瑙研钵。 </li><li>用1-2毫升丙酮和手磨用玛瑙杵〜5分钟挫伤粉末混合物。传送所产生的浅灰色粉末（ 图1b和2b）中放入铂坩埚中。 </li><li>加热的箱式炉中的坩埚，以1020℃，以5℃/分钟的升温速率，保持16小时，然后冷却至室温</li><li>掏出使用聚四氟乙烯（PTFE）刮刀的松动，淡蓝灰色粉末。 注：该产品的特点可以用光学显微镜（ 图3），扫描电镜（ 图4），PXRD（图5），和近红外照相（ 图8）。 </li></ol></li></ol> BaCuSi 4 O 10 2。合成<ol><li> BaCuSi 4 O 10的熔体通量合成 <ol><li>称出的BaCO 3，SiO 2的和CuO在1点04分01秒的摩尔比：0.2085克的BaCO 3（1.057毫摩尔），0.2539克的SiO 2（4.226毫摩尔），并0.0840克氧化铜（1.056毫摩尔）。此外，称出的磁通成分（按重量计12.5％）：0.0765克的PbO。这些材料加入到一个干净的玛瑙研钵。 </li><li>手磨为〜5分钟用玛瑙杵直到混合物变成均匀的浅灰色粉末（ 图1C和2C）。这种混合物转移到一个干净，干燥的铂金坩埚。 </li><li>加热在炉中的坩埚中，以950℃（2℃/ min的升温速率），保持在950℃下放置24小时，然后慢慢冷却到700℃（速率为0.1℃/分钟），并最后冷却至室温。 </li><li>从坩埚中取出晶体，轻轻地用杵粉碎他们。 </li><li>让该晶体在50毫升的1M含水HNO 3浸泡过夜，以除去熔融焊剂。 </li><li>过滤和结晶用去离子水冲洗，充分去除熔体通量的其余部分。注：此马terial应磨成细粉末的PXRD分析（ 图6）。它也可被表征通过光学显微镜（ 图3）和近红外照相（ 图8）。 </li></ol></li><li> BaCuSi 4 O 10的固相合成<ol><li>称出的BaCO 3，SiO 2的和CuO在1点04分01秒的摩尔比：0.2085克的BaCO 3（1.057毫摩尔），0.2539克的SiO 2（4.226毫摩尔），并0.0840克氧化铜（1.056毫摩尔），并加入到一个干净的玛瑙研钵。 </li><li>用1-2毫升丙酮和手磨用玛瑙杵〜5分钟挫伤粉末混合物。传送所产生的浅灰色粉末（ 图1d和 2d）放入铂坩埚中。 </li><li>加热的箱式炉中的坩埚中，以960℃，以5℃/分钟的升温速率和保持16小时，然后冷却至室温。 </li><li>掏出使用聚四氟乙烯（PTFE）抹刀松蓝色粉末。注意：该产品的特征在于通过光学显微镜（ 图3），PXRD（图6），和近红外照相（ 图8）。 </li></ol></li></ol> CaCuSi 4 O 10 3。剥离<ol><li>充的50ml圆底烧瓶中，用0.50克CaCuSi 4 O 10的40毫升去离子水和玻璃涂覆的磁性搅拌棒。 </li><li>附加一个水冷式冷凝器的烧瓶中。加热反应至85℃，以400rpm两周磁力搅拌。 </li><li>从热源取下，使溶液沉降原状过夜，然后通过0.4微米的膜过滤器过滤上清液。真空干燥该固体。注意：该产品是一种淡蓝色的粉末，可以表征通过光学显微镜（ 图3），PXRD（图5），透射电子显微镜（TEM）（ 图7），和近红外照相（ 图URE 8）。 </li></ol> BaCuSi 4 O 10 4。剥离<ol><li>充电50毫升塑料离心管中0.14克BaCuSi 4 O 10和20毫升N-乙烯基吡咯烷酮。 </li><li>用离心管浸入冰/水浴中，超声处理用探针超声波发生器以40％的幅度（17瓦）1小时。 </li><li>让分散体沉降不受干扰过夜，然后倒出上清液到新的离心管中。 </li><li>用离心机降速为10,286 XG。倒出上清液，留下纳米片在离心管的底部。 </li><li>重悬这种材料在20毫升的水，浴超声几分钟。以分离出粉末，过滤通过0.4微米滤膜过滤并真空干燥固体。注意：该产品是一种淡蓝色的粉末，可以表征通过光学显微镜（ 图3），PXRD（图6），透射电子显微镜（ 图7 </sTRONG&gt;）和近红外摄影（ 图8）。 </li></ol> 5，油墨的制备<ol><li>驱散〜0.10克CaCuSi 4 O 10纳米片在5毫升去离子水中超声浴〜10分钟。注意：该油墨（ 图9）可用于涂装，印刷等 见图10为一个有代表性的例子，其中将油墨施加到纸用刷子。 </li></ol> 6，近红外感光成像<ol><li>采用红光（ 例如用红色发光二极管阵列），照顾，以消除光的任何其他来源照射样品。 </li><li>拍摄用修改图像中的近红外区域的摄像机。使用f止损设置f/22时为0.5秒的曝光时间。 </li></ol>

<ol>
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埃及蓝颜料的制备方法，主要是CaCuSi 4 O 10和SiO 2的混合物，是一个充分研究的过程中4,13-21。众多的报告程序可以被归类为熔融焊剂或固态反应。的熔融焊剂的方法的两个主要优点是，它允许较低的反应温度（&lt;900℃），并允许CaCuSi 4 O 10晶体的成核和从熔融玻璃相20成长。磁通分量通常是碱金属盐（ 如的Na 2 CO 3）或硼酸酯化合物（ 例如硼砂）。相比较而言，固态合成中省略了磁通，但需要较高的温度（〜1000℃）的Ca，氧化铜之间的反应，和SiO 2的来源，以达到完成。 虽然汉蓝颜料的合成是没有得到很好的研究作为埃及蓝4,22-25，B的制备aCuSi 4 O 10所示相似的熔融焊剂和具有两个不同的固态路线：（1）一氧化铅焊剂应被使用，并且（2）该反应的温度必须更紧密，因为替代钡铜的Si-O相的控制可以形成（ 如 BaCuSi 2 O 6）。 这些点在本文所描述的详细过程和结果说明。首先，对于所有的方法，起始原料应研磨成光滑的粉末（ 图1a-d）由5-20微米的颗粒（通过SEM; 图2a-d）所示 。接着，在CaCuSi 4 O 10和BaCuSi 4 O 10导致高度结晶的产品，其特征是强烈的蓝色着色（ 图3a和3c）的制备中使用的显著量通量（以重量计12.5％），比较大粒径（ 图4a </strong&gt;）和强的PXRD图样（ 图5a和图6a）。该减弱的分离产率（〜70％）从这些制剂通过熔融反应混合物在坩埚的附着引起的。相比之下，CaCuSi 4 O 10和BaCuSi 4 O 10制备的固态路线展览较不强烈着色（ 图3b和3d）和较小的颗粒尺寸（ 图4b）。作为合成时，这些产品是粉末，可以是分离的，近乎定量的产率。因此，对于这两个CaCuSi 4 O 10和BaCuSi 4 O 10，通量和反应温度的重要性的优势不能被夸大。 值得注意的是，CaCuSi 4 O 10和BaCuSi 4 O 10的剥离下简单的水溶液条件下发生。在CaCuSi 4 O 10的情况下，该反应是在室温相当慢温度（≥6周看到任何明显的去角质），但它成为在80℃（大量脱落，2周后）合成有用的。相比之下，BaCuSi 4 O 10的剥离是缓慢的，即使在80℃，因此，我们采用一个更大的能量输入在超声波的形式。这些反应是有两点需要说明高度可靠。对于CaCuSi 4 O 10， 使用玻璃涂覆的搅拌棒是很重要的;如果一个标准的PTFE涂层的搅拌棒时，我们发现，聚四氟乙烯副产品污染CaCuSi 4 O 10纳米片的产品。为BaCuSi 4 O 10，重要的是，使反应停止前的纳米片成为退化来控制超声波的功率和时间。 的纳米片制品的透射电子显微镜（TEM）表明，这些非常薄的材料具有横向尺寸范围从几百纳米到几个麦克风RONS。一般来说，这些横向尺寸相关联的三维起始材料的微晶尺寸。在以前的工作中，原子力显微镜，惟证实这些纳米片12的单层厚度（〜1.2 nm）的地形测绘。粉的照片CaCuSi 4 O 10和BaCuSi 4 O 10纳米片样品（ 图3E-H）表明，它们的颜色比的起始原料，纳米结构的直接结果的那么强烈。 附加信息是通过PXRD（ 图5和6），它揭示了沿（001）面，并沿{00升 }系列的所有纳米片样品择优取向基底切割提供的。这些特征反映了这些的时候，下拉式浇铸在基板高度各向异性的纳米材料的堆积排列。此外，CaCuSi 4 O 10的〜9的特性近红外荧光在约950纳米10纳米和BaCuSi 4 O 10中示出的所有8个样本的NIR照片（ 图8）。 CaCuSi 4 O 10的溶液处理可以通过简单地制备CaCuSi 4 O 10纳米片的胶态分散体（ 图9）作为油墨使用来实现。该油墨然后可以通过旋涂法，喷涂法，喷墨印刷12，或仅仅刷牙（ 图10）被施加到基材上。重要的是，CaCuSi 4 O 10的近红外发光特性被保留在这个过程中的所有阶段。这些新的可能性突出CaCuSi 4 O 10纳米片和传统的利用埃及的蓝色颜料，即是具有挑战性的合并成一个光滑的漆非常细微的材料之间的对比。

鲜艳的色彩被撬开整个古代世界。即使在今天，我们仍然可以看到由各大文化创造颜料和染料的遗体。值得注意的是，两个最有名的合成蓝色色素有着相似的化学组成和结构，尽管已开发的广泛的不同的时间和地点。两个埃及蓝，CaCuSi 4 O 10，和韩青，BaCuSi 4 O 10的有色成分，属于碱土铜四硅系列，ACuSi 4 O 10（A =钙，锶，钡）1，以及在大gillespite组，ABSI 4 O 10（B =铁，铜，铬）2,3。 除了传统颜料的应用，目前在这些材料科学的兴趣在他们强大的近红外（NIR）发射特性中心。这个排放来源于铜离子在平面正方形协调;这些离子由四面体连结三维晶体结构内升硅酸盐部分，并将所得的层交替与碱土离子4-6。最近的技术亮点包括近红外成像识别文化遗产文物7,8，ACuSi 4 O 10的镧系元素掺杂埃及和汉蓝色颜料，以提高近红外反射特性，并打开新的能量传递途径9,10，使用ACuSi 4 O 10作为光学传感器11，和CaCuSi 4 O 10的剥离成单层纳米片12的活性物质。 尤其是，最后的例子提供了一种纳米结构CaCuSi 4 O 10，以便它可以被处理为胶态分散体，而不是作为固体颗粒12。因为胶态分散体与溶液加工技术兼容（ 例如旋涂，喷墨印刷，层-层沉积化），这种提前开启，范围从防伪油墨，以生物医学成像新的应用领域。在这方面的贡献所示的实验方案将使研究人员来自不同背景的准备，检定和使用CaCuSi 4 O 10和BaCuSi 4 O 10纳米片的工作。

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			<td height="21" style="height:21px;width:317px;">Name of Material/ Equipment</td>
			<td style="width:161px;">Supplier</td>
			<td style="width:119px;">Catalog Number</td>
			<td style="width:527px;">Comments/Description</td>
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		<tr height="25">
			<td height="25" style="height:25px;">Sodium carbonate (Na2CO3)</td>
			<td style="width:161px;">Sigma Aldrich&#160;</td>
			<td style="width:119px;">S7795</td>
			<td>bioXtra, &#8805; 99.0 %</td>
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		<tr height="25">
			<td height="25" style="height:25px;">Calcium carbonate (CaCO3)</td>
			<td style="width:161px;">Sigma Aldrich&#160;</td>
			<td style="width:119px;">C4830</td>
			<td>bioXtra, &#8805; 99.0 %</td>
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		<tr height="44">
			<td height="44" style="height:44px;">Barium carbonate (BaCO3)</td>
			<td style="width:161px;">Solvay Performance Chemicals</td>
			<td style="width:119px;"></td>
			<td>Research sample: Electronic-grade purity, nanocrystalline</td>
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			<td height="25" style="height:25px;">Copper (II) carbonate basic (Cu2CO3(OH)2)&#160;&#160;</td>
			<td style="width:161px;">Sigma Aldrich&#160;</td>
			<td style="width:119px;">207896</td>
			<td>Reagent grade</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Copper (II) oxide (CuO)&#160;</td>
			<td style="width:161px;">Sigma Aldrich&#160;</td>
			<td style="width:119px;">450812</td>
			<td>99.99 % trace metals base</td>
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		<tr height="25">
			<td height="25" style="height:25px;">Silicon dioxide (SiO2)</td>
			<td style="width:161px;">Sigma Aldrich&#160;</td>
			<td style="width:119px;">S5631</td>
			<td>~99 %, particle size 0.5-10 &#956;m (approx. 80% between 1-5 &#956;m)</td>
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		<tr height="26">
			<td height="26" style="height:26px;">Sodium tetraborate decahydrate (Na4B4O7.10H2O)</td>
			<td style="width:161px;">Sigma Aldrich&#160;</td>
			<td style="width:119px;">S9640</td>
			<td>ACS &#8805; 99.5 %</td>
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		<tr height="21">
			<td height="21" style="height:21px;">Sodium chloride (NaCl)&#160;</td>
			<td style="width:161px;">Sigma Aldrich&#160;</td>
			<td style="width:119px;">S9888</td>
			<td>ACS &#8805; 99.0 %</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Lead (II) oxide (PbO)&#160;</td>
			<td style="width:161px;">Sigma Aldrich&#160;</td>
			<td style="width:119px;">402982</td>
			<td>ACS &#8805; 99.0 %</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">N-Vinylpyrrolidinone (C6H9NO)</td>
			<td style="width:161px;">Sigma Aldrich&#160;</td>
			<td style="width:119px;">V3409</td>
			<td>contains sodium hydroxide as inhibitor, ACS &#8805; 99.0 %</td>
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		<tr height="21">
			<td height="21" style="height:21px;width:317px;">Box Furnace</td>
			<td style="width:161px;">Fisher Scientific</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:317px;">Box Furnace</td>
			<td style="width:161px;">Carbolite</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:317px;">Bath Sonicator</td>
			<td style="width:161px;">Branson</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:317px;">Ultrasonicator</td>
			<td style="width:161px;">Qsonica</td>
			<td style="width:119px;"></td>
			<td>Q700 Sonicator</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:317px;">Camera</td>
			<td style="width:161px;">custom modification of Nikon D3000 camera</td>
			<td style="width:119px;">n/a</td>
			<td>Xnite Nikon D3000 camera with a Nikkor 18-200 mm lens and a Xnite 830 filter&#160;</td>
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		<tr height="21">
			<td height="21" style="height:21px;width:317px;">Light Source</td>
			<td style="width:161px;">Excled Ltd.</td>
			<td style="width:119px;">PAR64</td>
			<td>LED Colour Beamer</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:317px;">Light Microscope</td>
			<td>Leica</td>
			<td style="width:119px;"></td>
			<td>mz6 Stereomicroscope with Spot Idea camera and Software</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:317px;">Powder X-Ray Diffractometer</td>
			<td>Bruker&#160;</td>
			<td style="width:119px;"></td>
			<td>D8-Advance diffractometer (Co-K&#945; radiation source)</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:317px;">Transmission Electron Microscope</td>
			<td>FEI Technai</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:317px;">Scanning Electron Microscope</td>
			<td>FEI</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:317px;">Membrane filters</td>
			<td style="width:161px;">Millipore</td>
			<td style="width:119px;">HTTP04700</td>
			<td>Isopore Membrane filter with 0.4 &#181;m pore size</td>
		</tr>
	</tbody>
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exfoliation of egyptian blue and han blue, two alkali earth copper silicate-based pigments

在古老的过去与现代连接的可视化例子中，我们描述CaCuSi 4 O 10和BaCuSi 4 O 10，历史悠久的埃及蓝色和汉蓝颜料的着色组分的制备和剥落。这些材料的散装形式通过两个合成的熔融焊剂和固态航线，这提供了对产品的微晶尺寸一定的控制。熔融焊剂过程是耗费时间的，但它会产生相对大的晶体，在较低的反应温度。相比较而言，固相法是更快但需要较高的反应温度，并产生更小的微晶。一旦在热水中搅拌，CaCuSi 4 O 10自发地去除角质成单层纳米片，其特点是TEM和PXRD。 BaCuSi 4 O 10，另一方面，需要超声处理在有机溶剂中实现剥离。近红外成像说明，无论是散装和CaCuSi 4 O 10和BaCuSi 4 O 10纳米片的形式是强大的近红外线发射器。因为它们提供了一种新的方式来处理，检定和胶体形式处理这些物质的水性CaCuSi 4 O 10和BaCuSi 4 O 10纳米片分散体是有用的。

CaCuSi 4 O 10和BaCuSi 4 O 10的描述合成提供约0.5g每批次产品。 CaCuSi 4 O 10的从熔融焊剂和固态合成中的分离产率范围通常为70-75％和90-95％之间。对于BaCuSi 4 O 10中， 分离产率从熔融焊剂和固态合成中通常范围从65-70％和95-99％之间。 所有制备的材料的纹理，以及在其蓝色的强度由于不同的晶粒尺寸的差异，是由低放大倍数的光学显微镜（ 图3a-H）可见。扫描电子显微镜（SEM）照片证实，合成CaCuSi 4的固相法O 10〜产生1-15微米的初级晶体（ 图4b），而熔助焊剂条件导致〜5-50微米CRYST<html>宏家（ 图4a）。粉末X-射线衍射（PXRD）型态的CaCuSi 4 O 10（ 图5a和5c）和BaCuSi 4 O 10（ 图6a和图6c）中展示的组合物和这些产品的相纯度。 代表性的透射型电子显微镜（TEM）图像显示的剥离产品的纳米片的形态（ 图7）。此外，近红外感光成像显示，无论是体积和材料脱落（ 图8）的强发光。一个简单的方法来说明CaCuSi 4 O 10纳米片的加工解决方案是制备水 ​​性油墨（ 图9），适用于喷漆（ 图10）。 hres.jpg“SRC =”/ files/ftp_upload/51686/51686fig1.jpg“/&gt; 图1的手工地面照片的原料。（一 ）CaCuSi 4 O 10熔体通量，（二）CaCuSi 4 O 10固态，（ 三）BaCuSi 4 O 10的熔体流量，以及（d）BaCuSi 4 O 10固态合成。 <a href="https://www.jove.com/files/ftp_upload/51686/51686fig1highres.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图2" fo:content-width="5in" fo:src="/files/ftp_upload/51686/51686fig2highres.jpg" src="/files/ftp_upload/51686/51686fig2.jpg" /> 图2。扫描电镜观察。的手地面图像的起始原料为（A）CaCuSi 4 O 10的熔融焊剂，（ <st荣&gt; B）CaCuSi 4 O 10固态，（ 三）BaCuSi 4 O 10的熔体流量，以及（d）BaCuSi 4 O 10的固态合成。所有样品均涂有金色前成像。 <a href="https://www.jove.com/files/ftp_upload/51686/51686fig2highres.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图3" fo:content-width="5in" fo:src="/files/ftp_upload/51686/51686fig3highres.jpg" src="/files/ftp_upload/51686/51686fig3.jpg" /> 图3光学显微镜。散装CaCuSi 4 O 10通过熔融焊剂（a）和固态（二）程序。散装BaCuSi 4 O 10通过熔融焊剂（c）和固态（ 四）程序。脱落的产品（EH）的（A-<html> d）中，分别。所有图片分享1mm的比例尺显示在面板上（ 一 ）。 <a href="https://www.jove.com/files/ftp_upload/51686/51686fig3highres.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图4" fo:content-width="5in" fo:src="/files/ftp_upload/51686/51686fig4highres.jpg" src="/files/ftp_upload/51686/51686fig4.jpg" /> 图4。扫描电镜观察。散装CaCuSi 4 O 10通过熔融焊剂（a）和固态（二）方法制成的图像。样品喷金前成像。 <a href="https://www.jove.com/files/ftp_upload/51686/51686fig4highres.jpg" target="_blank">请点击此处查看该图的放大版本。</a> 686/51686fig5highres.jpg“宽度=”500“/&gt; 图5粉末X-射线衍射：CaCuSi 4 O 10的模式通过熔融焊剂（a）和固态（ 三）方法批量CaCuSi 4 O 10。星号表示二氧化硅杂质。图案的脱落CaCuSi 4 O 10，（b）和（D），从（a）和（c）分别制备。 <a href="https://www.jove.com/files/ftp_upload/51686/51686fig5highres.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图6" fo:content-width="5in" src="/files/ftp_upload/51686/51686fig6highres.jpg" width="500" /> 图6粉末X-射线衍射：BaCuSi 4 O 10模式批量BaCuSi 4 O 10通过熔融焊剂（ <str翁&gt; a）和固态（ 三）方法。星号表示二氧化硅杂质。图案的脱落BaCuSi 4 O 10，（b）和（D），从（a）和（c）分别制备。 <a href="https://www.jove.com/files/ftp_upload/51686/51686fig6highres.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图7" fo:content-width="5in" fo:src="/files/ftp_upload/51686/51686fig7highres.jpg" src="/files/ftp_upload/51686/51686fig7.jpg" /> 图7。透射电子显微镜。脱落CaCuSi 4 O 10从散装CaCuSi 4 O 10通过熔融焊剂（a）或固态（二）制作方法得出的代表性图像。脱落BaCuSi 4 O 10从散装派生的代表图像BaCuSi 4 O 10通过熔融焊剂（c）或固态（D）的方法进行。 <a href="https://www.jove.com/files/ftp_upload/51686/51686fig7highres.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图8" fo:content-width="5in" fo:src="/files/ftp_upload/51686/51686fig8highres.jpg" src="/files/ftp_upload/51686/51686fig8.jpg" /> 图8。近红外成像，发光的制备熔体通量（a）和固态（二）程序批量CaCuSi 4 O 10。散装BaCuSi 4 O 10的发光通过熔融焊剂（c）和固态（ 四）程序编制。发光的（ 广告 ）时，脱落的产品（EH）分别。粉末样品所包含的玻璃小瓶中，并在entirË组样品进行成像一次。 <a href="https://www.jove.com/files/ftp_upload/51686/51686fig8highres.jpg" target="_blank">请点击此处查看此图的放大版本。</a> <img alt="图9" fo:content-width="5in" fo:src="/files/ftp_upload/51686/51686fig9highres.jpg" src="/files/ftp_upload/51686/51686fig9.jpg" /> 图9。照片在一个小瓶CaCuSi 4 O 10纳米片的油墨。 <img alt="图10" fo:content-width="5in" fo:src="/files/ftp_upload/51686/51686fig10highres.jpg" src="/files/ftp_upload/51686/51686fig10.jpg" /> 图10。近红外成像。一个基本的绘画与CaCuSi 4 O 10纳米片的油墨，说明了两者的简单应用程序及其发光性能。

Watch this Scientific Journal Video about Exfoliation of Egyptian Blue and Han Blue, Two Alkali Earth Copper Silicate-based Pigments at JoVE.com

Exfoliation of Egyptian Blue and Han Blue, Two Alkali Earth Copper Silicate-based Pigments

CaCuSi 4 O 10和BaCuSi 4 O 10的制备和剥落描述。一旦在热水中搅拌，CaCuSi 4 O 10自发地去除角质成单层，而BaCuSi 4 O 10条规定超声在有机溶剂中。近红外（NIR）成像示出这些材料的近红外发射特性，以及这些纳米材料的水分散液对溶液的处理是有用的。

埃及蓝色和汉蓝，两碱地球铜硅酸盐类颜料剥落

In a visualized example of the ancient past connecting with modern times, we describe the preparation and exfoliation of CaCuSi4O10 and BaCuSi4O10, the ...

exfoliation-egyptian-blue-han-blue-two-alkali-earth-copper-silicate

Research

JoVE Journal

Chemistry

15.4K 次观看.  The University of Georgia.  CaCuSi 4 O 10和BaCuSi 4 O 10的制备和剥落描述。一旦在热水中搅拌，CaCuSi 4 O 10自发地去除角质成单层，而BaCuSi 4 O 10条规定超声在有机溶剂中。近红外（NIR）成像示出这些材料的近红外发射特性，以及这些纳米材料的水分散液对溶液的处理是有用的。 

视频: Exfoliation of Egyptian Blue and Han Blue, Two Alkali Earth Copper Silicate-based Pigments

Transport of Surface-modified Carbon Nanotubes through a Soil Column

Carbon nanotubes (CNTs) are widely manufactured nanoparticles, which are being utilized in a number of consumer products, such as sporting goods, electronics and biomedical applications. Due to their accelerating production and use, CNTs constitute a potential environmental risk if they are released to soil and groundwater systems. It is therefore essential to improve the current understanding of environmental fate and transport of CNTs. The transport and retention of CNTs in both natural and artificial media have been reported in literature, but the findings widely vary and are thus not conclusive. There are a number of physical and chemical parameters responsible for variation in retention and transport. In this study, a complete procedure of selected multiwalled carbon nanotubes (MWCNTs) is presented starting from their surface modification to a complete set of laboratory column experiments at critical physical and chemical scenarios. Results indicate that the stability of the commercially available MWCNTs are critical with their attached surface functional group which can also influence the transport and retention of MWCNT through the surrounding medium.

Surface properties of a nanoparticle are important for their interaction with the surrounding medium. Therefore the surface modification of carbon nanotubes can be critical for their transport and retention through porous media. Here, lab scale column experiments are used to understand the possible transport and retention of these nanoparticles.

表面修饰碳纳米管通过土柱运输

Carbon nanotubes (CNTs) are widely manufactured nanoparticles, which are being utilized in a number of consumer products, such as sporting goods, ...

科研

化学

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

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

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

金属硅酸盐分区在高压和高温：实验方法和协议，以抑制高亲铁元素元素夹杂物

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

Chemical Gardens as Flow-through Reactors Simulating Natural Hydrothermal Systems

Here we report experimental simulations of hydrothermal chimney growth using injection chemical garden methods. The versatility of this type of experiment allows for testing of various proposed ocean / hydrothermal fluid chemistries that could have driven reactions toward the origin of life in environments on the early Earth, early Mars, or even other worlds such as the icy moons of the outer planets. We show experiments that include growth of chemical garden structures under anoxic conditions simulating the early Earth, inclusion of trace components of phosphates / organics in the injection solution to incorporate them into the structure, a switch of the injection solution to introduce a secondary precipitating anion, and the measurement of membrane potentials generated by chemical gardens. Using this method, self-assembling chemical garden structures were formed that mimic the natural chimneys precipitated at submarine hydrothermal springs, and these precipitates can be used successfully as flow-through reactors by feeding through multiple successive &#8220;hydrothermal&#8221; injections.

We describe chemical garden formation via injection experiments that allow for laboratory simulations of natural chemical garden systems that form at submarine hydrothermal vents.

化工园为直通式反应器模拟自然热液系统

Here we report experimental simulations of hydrothermal chimney growth using injection chemical garden methods. The versatility of this type of experiment ...

Synthesis and Exfoliation of Discotic Zirconium Phosphates to Obtain Colloidal Liquid Crystals

Due to their abundance in natural clay and potential applications in advanced materials, discotic nanoparticles are of interest to scientists and engineers. Growth of such anisotropic nanocrystals through a simple chemical method is a challenging task. In this study, we fabricate discotic nanodisks of zirconium phosphate [Zr(HPO4)2&#183;H2O] as a model material using hydrothermal, reflux and microwave-assisted methods. Growth of crystals is controlled by duration time, temperature, and concentration of reacting species. The novelty of the adopted methods is that discotic crystals of size ranging from hundred nanometers to few micrometers can be obtained while keeping the polydispersity well within control. The layered discotic crystals are converted to monolayers by exfoliation with tetra-(n)-butyl ammonium hydroxide [(C4H9)4NOH, TBAOH]. Exfoliated disks show isotropic and nematic liquid crystal phases. Size and polydispersity of disk suspensions is highly important in deciding their phase behavior.

A two dimensional model material of discotic zirconium phosphate was developed. The inorganic crystal with lamellar structure was synthesized by hydrothermal, reflux, and microwave-assisted methods. On exfoliation with organic molecules, layered crystals can be converted to monolayers, and nematic liquid crystal phase was formed at sufficient concentration of monolayers.

合成与盘状磷酸盐锆剥落获取胶体液晶

Due to their abundance in natural clay and potential applications in advanced materials, discotic nanoparticles are of interest to scientists and ...

Extraction of Ramie Fiber in Alkali Hydrogen Peroxide System Supported by Controlled-release Alkali Source

This protocol demonstrates a method for ramie fiber extraction by scouring raw ramie in an alkali hydrogen peroxide system supported by a controlled-release alkali source. The fiber extracted from ramie is a type of textile material of great importance. In previous studies, ramie fiber was extracted in an alkali hydrogen peroxide system supported only by sodium hydroxide.However, due to the strong alkalinity of sodium hydroxide, the oxidation reaction speed of hydrogen peroxide was difficult to control and thus resulted in great damage to the treated fiber. In this protocol, a controlled-release alkali source, which is composed of sodium hydroxide and magnesium hydroxide, is used to provide an alkali condition and buffer the pH value of the alkali hydrogen peroxidesystem. The substitution rate of magnesium hydroxide can adjust the pH value of the hydrogen peroxide system and has great influence on the fiber properties. The pH value and oxidation-reduction potential (ORP) value, which represents the oxidation ability of alkali hydrogen peroxide system, were monitored using a pH meter and ORP meter, respectively. The residual hydrogen peroxide content in the alkali hydrogen peroxide system during the extraction process and the chemical oxygen demand (COD) value of wastewater after fiber extraction are tested by KMnO4 titration method. The yield of fiber is measured using a precision electronic balance, and residual gums of fiber are tested by a chemical analysis method. The polymerization degree (PD value) of fiber is tested by an intrinsic viscosity method using the Ubbelohde viscometer. The tensile property of fiber, including tenacity, elongation, and rupture, is measured using a fiber strength instrument. Fourier transform infrared spectroscopy and X-ray diffraction are used to characterize the functional groups and crystal property of fiber. This protocol proves that the controlled-release alkali source can improve the properties of the fiber extracted in an alkali hydrogen peroxide system.

Presented here is a protocol for extraction of ramie fiber in alkali hydrogen peroxide system supported by controlled-release alkali source.

缓释碱源负载碱性过氧化氢体系中苎麻纤维的提取

This protocol demonstrates a method for ramie fiber extraction by scouring raw ramie in an alkali hydrogen peroxide system supported by a ...

Determination of Thermodynamic Properties of Alkaline Earth-liquid Metal Alloys Using the Electromotive Force Technique

A novel electrochemical cell based on a CaF2 solid-state electrolyte has been developed to measure the electromotive force (emf) of binary alkaline earth-liquid metal alloys as functions of both composition and temperature in order to acquire thermodynamic data. The cell consists of a chemically stable solid-state CaF2-AF2 electrolyte (where A is the alkaline-earth element such as Ca, Sr, or Ba), with binary A-B alloy (where B is the liquid metal such as Bi or Sb) working electrodes, and a pure A metal reference electrode. Emf data are collected over a temperature range of 723 K to 1,123 K in 25 K increments for multiple alloy compositions per experiment and the results are analyzed to yield activity values, phase transition temperatures, and partial molar entropies/enthalpies for each composition.

This protocol describes the measurement of the electromotive force of alkaline-earth elements in liquid metal alloys at high temperatures (723-1,123 K) to determine their thermodynamic properties, including activity, partial molar entropy, partial molar enthalpy, and phase transition temperatures, over a wide composition range.

用电动势技术测定碱土金属合金的热力学性质

A novel electrochemical cell based on a CaF2 solid-state electrolyte has been developed to measure the electromotive force (emf) of binary alkaline ...

Reliable Mechanochemistry: Protocols for Reproducible Outcomes of Neat and Liquid Assisted Ball-mill Grinding Experiments

The equilibrium outcomes of ball mill grinding can dramatically change as a function of even tiny variations in the experimental conditions such as the presence of very small amounts of added solvent. To reproducibly and accurately capture this sensitivity, the experimentalist needs to carefully consider every single factor that can affect the ball mill grinding reaction under investigation, from ensuring the grinding jars are clean and dry before use, to accurately adding the stoichiometry of the starting materials, to validating that the delivery of solvent volume is accurate, to ensuring that the interaction between the solvent and the powder is well understood and, if necessary, a specific soaking time is added to the procedure. Preliminary kinetic studies are essential to determine the necessary milling time to achieve equilibrium. Only then can exquisite phase composition curves be obtained as a function of the solvent concentration under ball mill liquid assisted grinding (LAG). By using strict and careful procedures analogous to the ones here presented, such milling equilibrium curves can be obtained for virtually all milling systems. The system we use to demonstrate these procedures is a disulfide exchange reaction starting from the equimolar mixture of two homodimers to obtain at equilibrium quantitative heterodimer. The latter is formed by ball mill grinding as two different polymorphs, Form A and Form B. The ratio R = [Form B] / ([Form A] + [Form B]) at milling equilibrium depends on the nature and concentration of the solvent in the milling jar.

We present detailed procedures to produce experimental equilibrium curves of the phase composition as a function of solvent concentration in a solid state system under milling conditions.

可靠的化学: 整洁和液体辅助球磨机研磨试验的可再生结果协议

The equilibrium outcomes of ball mill grinding can dramatically change as a function of even tiny variations in the experimental conditions such as the ...

Exfoliation and Analysis of Large-area, Air-Sensitive Two-Dimensional Materials

We describe methods for producing and analyzing large, thin flakes of air-sensitive two-dimensional materials. Thin flakes of layered or van der Waals crystals are produced using mechanical exfoliation, in which layers are peeled off a bulk crystal using adhesive tape. This method produces high-quality flakes, but they are often small and can be hard to find, particularly for materials with relatively high cleavage energies such as black phosphorus. By heating the substrate and the tape, two-dimensional material adhesion to the substrate is promoted, and the flake yield can be increased by up to a factor of ten. After exfoliation, it is necessary to image or otherwise analyze these flakes but some two-dimensional materials are sensitive to oxygen or water and will degrade when exposed air. We have designed and tested a hermetic transfer cell to temporarily maintain the inert environment of a glovebox so that air-sensitive flakes can be imaged and analyzed with minimal degradation. The compact design of the transfer cell is such that optical analysis of sensitive materials can be performed outside of a glovebox without specialized equipment or modifications to existing equipment.

A method for exfoliating large thin flakes of air sensitive two-dimensional materials and safely transporting them for analysis outside of a glovebox is presented.

大面积空气敏感二维材料的去角质与分析

We describe methods for producing and analyzing large, thin flakes of air-sensitive two-dimensional materials. Thin flakes of layered or van der Waals ...

Accumulation and Analysis of Cuprous Ions in a Copper Sulfate Plating Solution

Knowledge of the behavior of cuprous ions (monovalent copper ion: Cu(I)) in a copper sulfate plating bath is important for improving the plating process. We successfully developed a method to quantitatively and easily measure Cu(I) in a plating solution and used it for evaluation of the solution. In this paper, a quantitative absorption spectrum measurement and a time-resolved injection measurement of Cu(I) concentrations by a color reaction are described. This procedure is effective as a method to reproduce and elucidate the phenomenon occurring in the plating bath in the laboratory. First, the formation and accumulation process of Cu(I) in solution by electrolysis of a plating solution is shown. The amount of Cu(I) in the solution is increased by electrolysis at higher current values &#8203;&#8203;than the usual plating process. For the determination of Cu(I), BCS (bathocuproinedisulfonic acid, disodium salt), a reagent that selectively reacts with Cu(I), is used. The concentration of Cu(I) can be calculated from the absorbance of the Cu(I)-BCS complex. Next, the time measurement of the color reaction is described. The color reaction curve of Cu(I) and BCS measured by the injection method can be decomposed into an instantaneous component and a delay component. By analysis of these components, the holding structure of Cu(I) can be clarified, and this information is important when predicting the quality of the plating film to be produced. This method is used to facilitate the evaluation of the plating bath in the production line.

Here, accumulation of cuprous ions in a copper sulfate plating solution in a model experiment and an analysis based on quantitative measurements are described. This experiment reproduces the accumulation process of cuprous ions in the plating bath.

硫酸铜镀液中铜离子的积累与分析

Knowledge of the behavior of cuprous ions (monovalent copper ion: Cu(I)) in a copper sulfate plating bath is important for improving the plating process. ...

[(DPEPhos)(bcp)Cu]PF6: A General and Broadly Applicable Copper-Based Photoredox Catalyst

Our group recently reported the use of [(DPEPhos)(bcp)Cu]PF6 as a general copper-based photoredox catalyst which proved efficient to promote the activation of a broad variety of organic halides, including unactivated ones. These can then participate in various radical transformations such as reduction and cyclization reactions, as well as in the direct arylation of several (hetero)arenes. These transformations provide a straightforward access to a range of small molecules of interest in synthetic chemistry, as well as to biologically active natural products. Altogether, [(DPEPhos)(bcp)Cu]PF6 acts as a convenient photoredox catalyst which appears to be an attractive, cheap and complementary alternative to the state-of-the-art iridium- and ruthenium-based photoredox catalysts. Here, we report a detailed protocol for the synthesis of [(DPEPhos)(bcp)Cu]PF6, as well as NMR and spectroscopic characterizations, and we illustrate its use in synthetic chemistry for the direct arylation of (hetero)arenes and radical cyclization of organic halides. In particular, the direct arylation of N-methylpyrrole with 4-iodobenzonitrile to afford&#160;4-(1-methyl-1H-pyrrol-2-yl)benzonitrile and the radical cyclization of N-benzoyl-N-[(2-iodoquinolin-3-yl)methyl]cyanamide to afford natural product luotonin A are detailed. The scope and limitations of this copper-based photoredox catalyst are also briefly discussed.

[DPEPhosbcpCu]PF6: A General and Broadly Applicable Copper-Based Photoredox Catalyst

Detailed and general protocols are presented for the synthesis of [(DPEPhos)(bcp)Cu]PF6, a general copper-based photoredox catalyst, and for its use in synthetic chemistry for the direct arylation of C-H bonds in (hetero)arenes and radical cyclization of organic halides.