Name: simple methods for the preparation of non-noble metal bulk-electrodes for electrocatalytic applications
Uploaded: 2017-06-21T15:00:00
Description: Watch this Scientific Journal Video about Simple Methods for the Preparation of Non-noble Metal Bulk-electrodes for Electrocatalytic Applications at JoVE.com

我们感谢B. Konkena und W. Schuhmann进行有价值的科学讨论。化学工业（Liebig授予U.-PA）和Deutsche Forschungsgemeinschaft（Emmy Noether授予U-PA，AP242 / 2-1）的财务支持。

1.高温合成Fe 4.5 Ni 4.5 S 8 注意：本文所述的合成Fe 4.5 Ni 4.5 S 8的方法从文献中采用。 8,10所报告的加热斜坡的严格应用对于防止相位杂质的形成和二氧化硅安瓿的缺陷是非常重要的。 <ol><li>在研钵中充分混合铁（1.66g，29.8mmol），镍（1.75g，29.8mmol）和硫（1.70g，53.1mmol），并将混合物转移到二氧化硅安瓿（直径...

<ol>
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X-ray, neutron, M&#246;ssbauer, and magnetic studies of pentlandite and the &#960; phases &#960;(Fe, Co, Ni, S), Co8MS8, and Fe4Ni4MS8 (M = Ru, Rh, Pd).</a> J Solid State Chem. 16 (1-2), 97-116 (1976).</li><li>Kullerud, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thermal+stability+of+pentlandite.">Thermal stability of pentlandite.</a> The Canadian Mineralogist. 7 (3), 353-366 (1963).</li><li>Siracusano, S., 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=An+electrochemical+study+of+a+PEM+stack+for+water+electrolysis.">An electrochemical study of a PEM stack for water electrolysis.</a> Int J Hydrogen Energy. 37 (2), 1939-1946 (2012).</li></ol>

在真空密封的安瓿中进行Fe 4.5 Ni 4.5 S 8的合成，以防止在合成过程中材料的氧化。在合成过程中，温度控制是获得纯产品的关键。第一，非常缓慢的加热步骤从而防止硫的过热，这可能由于高硫压而导致安瓿的破裂。更重要的是通过缓慢加热样品来防止相位杂质如单硫化物固溶体（mss）。在700°C的后续退火步骤确保了系统的平衡。随后，在1100℃退火，最终导致形成一个纯?...

波动的可再生能源如太阳能和风能的储存由于化石燃料逐渐褪色和随后的替代能源需求而具有重大的社会利益。在这方面，由于清洁的燃烧过程，氢气是分子能量储存解决方案的有希望的可持续候选者。 1此外，氢气可用作燃料或用作更复杂燃料（ 如甲醇）的起始原料。使用碳中和资源轻松合成氢的首选方法是使用可持续能量进行电化学还原水。 目前，已知铂及其合金是显示低过电位，快速反应速率和高电流密度下的操作的析氢反应（HER）的最有效的电催化剂。 2然而，由于其高价格和低自然丰度，需要非金属催化剂。在大量替代的非贵重过渡金属催化剂中， 3种特别是过渡金属二硫属元素（MX 2 ; M =金属; X = S，Se）已被证明具有高的HER活性。 4，5，6，7在这方面，我们最近提出了Fe 4.5 Ni 4.5 S 8作为高度耐用和活跃的“岩石”HER电催化剂。这种天然丰富的材料在酸性条件下是稳定的，并且具有良好定义的催化活性表面的高固有电导率。 8 虽然已经报道了许多具有高HER活性的材料，但是电极制备通常伴随着多个问题， 例如重现性和令人满意的稳定性（&gt; 24小时）。 Additionally，由于本体上过渡金属基催化剂的固有导电性通常较高，所以电极制备需要纳米结构的催化剂以允许有效的电子转移。然后将这些催化剂转化成含有粘合剂如Nafion和催化剂的催化剂油墨。之后，墨水滴涂在惰性电极表面（ 如玻璃碳）上。虽然在低电流密度下相当稳定，但是在高电流密度下通常观察到催化剂在电极载体上的增加的接触电阻和平均粘附性。因此，需要更多的制备方法和电极材料是显而易见的。 该方案提出了使用散装材料的高耐用性和成本效益的电极的新型制备方法。这种电极的先决条件是低的本征材料电阻。 Fe 4.5 Ni 4.5 S 8填充此标准，可以通过密封硅胶安瓿中的简单高温合成从元件中获得。使用粉末X射线衍射（PXRD），差示扫描量热法（DSC），扫描电子显微镜（SEM）和能量色散X射线光谱（EDX），获得的材料的特征在于其结构，形态和组成。将合成的材料加工成两种类型的体电极，即“岩石”和“颗粒”电极。然后使用标准电化学测试和通过气相色谱（GC）进行的H 2定量来研究两种电极类型的性能。介绍了两种类型电极的性能与常用滴涂实验相比较。

<table border="0" cellpadding="0" cellspacing="0" width="1228">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Iron, powder</td>
			<td style="width:309px;">Sigma-Aldrich, http://www.sigmaaldrich.com</td>
			<td style="width:115px;">12310-500G-R</td>
			<td style="width:495px;"></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:311px;">Nickel, powder</td>
			<td style="width:309px;">Sigma-Aldrich, http://www.sigmaaldrich.com</td>
			<td>203904-25G</td>
			<td style="width:495px;">H: 351-372-317-412; 
			P: 281-273-308-313-302+352</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Sulfur, powder</td>
			<td style="width:309px;">Sigma-Aldrich, http://www.sigmaaldrich.com</td>
			<td style="width:115px;">13803-1KG-R</td>
			<td>H: 315</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Silver Epoxy Glue EC 151 L</td>
			<td style="width:309px;">Polytec PT, http://www.polytec-pt.de/de/</td>
			<td style="width:115px;">161010-1</td>
			<td>-</td>
		</tr>
		<tr height="84">
			<td height="84" style="height:84px;width:311px;">Two Component Epoxy Glue Uhu Plus Endfest</td>
			<td>Uhu, http://www.uhu.com</td>
			<td style="width:115px;">-</td>
			<td style="width:495px;">&#160;H: 315-319-317-411; 
			&#160;P: 101-102-261-272-280-302+352-333+313-362-363-305+351+338-337+313</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:311px;">Sulfuric Acid &#62;95%</td>
			<td style="width:309px;">VWR, https://ru.vwr.com</td>
			<td style="width:115px;">231-639-5</td>
			<td style="width:495px;">H: 290-314; 
			S: (1/2)-26-30-45</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">PTFE Tube</td>
			<td style="width:309px;">-</td>
			<td style="width:115px;">-</td>
			<td>Prepare 8 cm long peaces</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Iron Sleeves</td>
			<td style="width:309px;">-</td>
			<td style="width:115px;">-</td>
			<td>Connect to the copper wire</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Copper Wire</td>
			<td style="width:309px;">-</td>
			<td style="width:115px;">-</td>
			<td>-</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Lapping Film 3&#181;m, 215.9 x 279 mm</td>
			<td style="width:309px;">3M, http://3mpro.3mdeutschland.de</td>
			<td style="width:115px;">60-0700-0232-8</td>
			<td>Polish with a small amount of water</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Lapping Film 1&#181;m, 215.9 x 279 mm</td>
			<td style="width:309px;">3M, http://3mpro.3mdeutschland.de</td>
			<td style="width:115px;">60-0700-0266-6</td>
			<td>Polish with a small amount of water</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Sand Paper 20 &#181;m, SiC</td>
			<td style="width:309px;">-</td>
			<td style="width:115px;">-</td>
			<td>-</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Sand Paper 14 &#181;m, SiC</td>
			<td style="width:309px;">-</td>
			<td style="width:115px;">-</td>
			<td>-</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Dremel Model 225</td>
			<td>Dremel, https://www.dremeleurope.com</td>
			<td style="width:115px;">2615022565</td>
			<td>Use grinding pulley wheel for cutting&#160;</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Hand Made Pellet Press</td>
			<td style="width:309px;">Hand Made</td>
			<td style="width:115px;">-</td>
			<td>-</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Stirring Plate</td>
			<td style="width:309px;">-</td>
			<td style="width:115px;">-</td>
			<td>-</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:311px;">GAMRY Reference 600</td>
			<td style="width:309px;">GAMRY Instruments, https://www.gamry.com</td>
			<td style="width:115px;">-</td>
			<td>-</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Gero Furnace 30-3000&#176;C</td>
			<td>http://www.carbolite-gero.de</td>
			<td style="width:115px;">-</td>
			<td>-</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Quartz glass ampule</td>
			<td style="width:309px;">Hand Made</td>
			<td style="width:115px;">-</td>
			<td>-</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Vacuum pump</td>
			<td style="width:309px;">-</td>
			<td style="width:115px;">-</td>
			<td>-</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:311px;">Hydraulic press</td>
			<td style="width:309px;">-</td>
			<td style="width:115px;">-</td>
			<td>-</td>
		</tr>
	</tbody>
</table>

simple methods for the preparation of non-noble metal bulk-electrodes for electrocatalytic applications

通过元素的高温合成，合成组成为Fe 4.5 Ni 4.5 S 8的岩石材料。材料的结构和组成通过粉末X射线衍射（PXRD），Mössbauer光谱（MB），扫描电子显微镜（SEM），差示扫描量热法（DSC）和能量色散X射线光谱（EDX）表征。介绍了两种制备五面体电极的方法。在第一种方法中，一片合成的五面体岩石通过电线套圈直接接触。第二种方法是使用固定在特氟龙套管中的细磨粉末压制的镍盐颗粒。两种电极在通过无添加剂方法制备时，与普通的滴涂方法相比，在电催化转化过程中显示出高的耐久性。我们在这里展示了这样的电极的惊人的性能来完成水电罗氏进化反应（HER），并提出了一种通过电化学和气相色谱法评估电催化性能的标准化方法。此外，我们在0.6V的超电势下通过恒电位法报告稳定性测试，以探索在工业相关条件下的电解期间电极的材料限制。

由于存在突出的（111），（311），（222），（331）和（511）反射，通过粉末X射线衍射实验证实具有Pentlandite结构的Fe 4.5 Ni 4.5 S 8的成功合成（ 图1a ）。然而，在反应期间适当的温度控制是获得相纯物质的关键。值得注意的是，当将混合物以较高的加热速率（例如20℃/分钟）加热到700℃时，已经观察到单硫化物固溶体（mss），?...

Watch this Scientific Journal Video about Simple Methods for the Preparation of Non-noble Metal Bulk-electrodes for Electrocatalytic Applications at JoVE.com

Simple Methods for the Preparation of Non-noble Metal Bulk-electrodes for Electrocatalytic Applications

提出了使用大块材料Fe 4.5 Ni 4.5 S 8的电极的简便制备方法。该方法提供了常规电极制造的替代技术，并描述了非常规电极材料的先决条件，包括直接的电催化测试方法。

用于制备用于电催化应用的非贵金属体电极的简单方法

The rock material pentlandite with the composition Fe4.5Ni4.5S8 was synthesized via high temperature synthesis from the elements. The structure and ...

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