This work is supported by an agreement with Syracuse University awarded by the Syracuse Center of Excellence in Energy and Environmental Systems with funding under prime award number DE-EE0006031 from the US Department of Energy and matching funding under award number 53367 from the New York State Energy Research and Development Authority (NYSERDA), contract 61736 from NYSERDA, and an award from Empire State Development's Division of Science, Technology and Innovation (NYSTAR) through the Syracuse Center of Excellence, under award number #C120183. This work is supported by the National Science Foundation Graduate Research Fellowship Program under Grant No. 1247399.

1.燃烧计算<ol><li>分析选择的燃料。在这里，选择甲烷作为基准燃料，但原则是转移到其他烃类燃料。 </li><li>与1摩尔甲烷作为燃料，平衡公式（1）为化学计量燃烧来获得等式（2）。 <img alt="式（1）" src="/files/ftp_upload/54638/54638eq1.jpg" /> <img alt="公式（2）" src="/files/ftp_upload/54638/54638eq2.jpg" /></li><li>通过空气的质量除以甲烷的质量计算化学计算如等式3为甲烷燃烧的燃料-空气比（F / A 化学计量）。来计算，该分子是甲烷倍摩尔数甲烷的摩尔质量（16·G·摩尔-1），分母是氧倍摩尔的氧的摩尔质量数（32·G·摩尔-1）加的氮倍摩尔数氮的摩尔质量（28·G·摩尔-1）。 <img alt="公式3"SRC ="/文件/ ftp_upload / 54638 / 54638eq3.jpg"/&gt; </li><li>为了改变当量比（方程4），变化或者空气流量，燃料流量或同时两者。通常情况下，固定量之一并改变另一个。确定是否修复无论是对燃烧器的燃料或空气的流量。对于本实验，修正燃料流量在10升/分钟，并允许空气流速在此设置而变化。 <img alt="公式4" src="/files/ftp_upload/54638/54638eq4.jpg" /></li><li>随着燃料流速F，固定（10升/分），F / A 坚忍 。计算的（0.0583），并考虑到当量比的定义，计算出空气流量，一个，对于每个要测试的当量比。公式（5）提供了计算的气流速度在升/分的每个当量比的一个直接的方法和结果示为1的化学计量当量比。 <img alt="公式5" src="/files/ftp_upload/54638/54638eq5.jpg" /> 注:上FLAMM能力的限制（或爆炸上限）是最丰富的当量比即可以在不存在催化剂的骤冷火焰中燃烧。更高的当量比可以通过使用催化剂来获得，但仅非催化燃烧在本文中描述。查阅文献，评估选择的燃料燃烧上限。 </li></ol> 2.燃烧特性实验装置<ol><li>选择基于在步骤1.5中得到的流速为甲烷和空气质量流量控制器（微型燃料电池）。选择MFC大小时要小心，以确保MFC不会在其范围的低端测试期间（&lt;满刻度值的10％）运行。对于这个特定的情况下，使用40升/分和200升/分钟的MFC分别为甲烷和空气。 </li><li>通过铜管连接微型燃料电池的甲烷和空气罐。 </li><li>按照规定设置甲烷和空气罐为MFC适当的压力调节器由制造商。在这种情况下，将压力设置为138千帕（20磅）。 </li><li>校准微型燃料电池，以确保准确的流量。 </li><li>构造燃烧室。在这个实验中，制定了燃烧室914毫米长着168毫米出口直径。 <ol><li>钻头端口燃烧废气分析和沿着燃烧室的长度热电偶放置。所需的确切数目和间隔取决于火焰的尺寸和实验的目的。对于这种设置，第一空间5热电偶置于最靠近燃烧区域隔开7mm左右。空间的最后6热电偶除了14毫米。使用相同的间距排气口。 </li><li>经由端口孔插入的K型热电偶入燃烧室。对准热电偶尖端在燃烧室的中心。尺寸端口孔，以适应热电偶和高温金属套圈和螺母以防止泄漏密封。 </li></ol></li><li>康涅狄格州等的K型热电偶直接向数据采集模块。 </li><li>通过USB驱动器连接数据采集模块到计算机。 </li><li>燃料MFC的后立即和刚好在燃烧器之前附着在铜管路径的单向阀。定向阀，使流只能移动从MFC路程。该单向阀是一个重要的安全功能，以防止闪回。 </li><li>检查前后MFC设置有泄漏后铜管。使用用毛笔应用肥皂水管道检测泄漏的泄漏会产生气泡。 </li><li>通过铜管连接燃烧室和燃烧器的质量流量控制器。 </li><li>完成燃烧室设置后，选择测试排气口之一。连接该端口延伸到GC分析端口铜管。 </li><li>选择注射器从燃烧室拉排气然后将它推入GC进行分析。对于这个实验中，使用一个25毫升注射器。 </li><li>放置在与排气口连接到GC铜管线一个三通阀。双向阀的一端连接到GC中，第二到排气口和第三至25毫升注射器。铜管连接到三通阀。用注射器从室吸燃烧废气，然后将其推入GC进行分析。 </li><li>连接阀到GC和注射器3路。驱动注射器推杆，以确保手术成功。 注意:安装的简化示意图如图1所示。 </li></ol><img alt="图1" src="/files/ftp_upload/54638/54638fig1.jpg" /> 图1的燃烧特性的实验装置示意图。燃烧特性的实验装置示意图，显示燃料，空气和排气流量（黑色箭头）和数据流（红色箭头）。单向阀用于防止回火。 <aHREF ="https://www.jove.com/files/ftp_upload/54638/54638fig1large.jpg"目标="_空白"&gt;点击此处查看该图的放大版本。 3.燃烧特性试验<ol><li>在测试之前，推针筒柱塞在完全打开的排气口侧的三通阀。 </li><li>打开第一空气MFC到86.5升/分钟的流速。 </li><li>打开甲烷的MFC上的10升/分钟的流速。这产生1.10预混当量比，稍微富混合物，这是更容易点燃。 </li><li>打开热电偶上通过计算机模块，开始记录数据。 </li><li>用丁烷打火机点燃在燃烧室的端部的混合物。点火后，火焰应该在燃烧器前稳定。 </li><li>通过从86.5升/分钟的初始值调节空气的流速缓慢，以所需的值调整量比。小心不要太快移动或去flammab之外ility限制这将导致火焰熄灭。 </li><li>记录在数据文件中的温度读数温度稳定后，热电偶。 </li><li>再次，拉针筒柱塞以从排气口抽取燃烧废气。 </li><li>抽取燃烧废气后，打开阀门到GC侧三通和关闭排气口侧。 </li><li>推针筒柱塞，直到它完全关闭并且所有的排气的已发送到GC。 </li><li>直到所有连接端口到GC铜管的残余气体的去除重复步骤3.8-3.10。铜管的内部容积相比，注射器的体积将指示多少次的一个简单的分析步骤3.8-3.10需要重复。 </li><li>在油管删除所有剩余气体后提取用于分析的最终排气样。推废气入GC和转动的GC分析模式7,17。 </li><li>记录通过保存的数据GC在GC分析数据。 </li><li>直到所有想要当量比进行测试，重复步骤3.1-3.13。 </li></ol> 4.模型燃烧废气的发展<ol><li>画出燃烧废气种体积百分数来观察的趋势。 </li><li>确定模型燃烧废气截止浓度值。在开发初期MT-FFC分析模型燃烧废气的燃料，仅部件中出现显著比例（&gt; 1％）被包括在模型中的燃料。 </li><li>为模型的燃料仅选择产生在排气显著氢气和一氧化碳（每个组件&gt; 1％）的那些等价比率。 </li><li>记录每个排气组件会议4.3的标准的体积百分比。 </li></ol> 5.燃料电池测试设置<ol><li>确定流率范围为每种气体。乘以从用t的GC分析的结果所获得的体积百分比他总计每个燃料电池内所需的模型燃烧废气的流速。 </li><li>评估流速为每个燃烧排气物种的范围，以确定每个物种的最大和最小流量。 </li><li>根据在步骤2.1中描述的相同的原则选择流量计。 </li><li>通过经由铜管连接流量计的气罐构建测试装置。 </li><li>设置气体压力调节器，以用于流量计的规定值。 </li><li>放置的单向阀在使用可燃性气体的每个流量计下游的铜管路径。 </li><li>连接所有流量计出境口岸在一起，通过铜管和多方面的。 </li><li>上设置具有内部直径只比所述燃料电池的外部直径大的钢管内的微管式SOFC。密封燃料电池用陶瓷粘合剂的钢管。 </li><li>具有微管式SOFC的钢管连接到一块陶瓷耐火米aterial保持在炉中的燃料电池。 </li><li>利用与连接到微管式SOFC用在阳极2线和阴极2线的电流收集和电压感测线的4探针技术10,11。确保线不会相互交叉创建短裤。 </li><li>把四根导线连接到恒电位仪10,11的四个探头。 </li><li>稳压器连接到计算机10,11。 </li><li>放置一个热电偶在与尖端接触微管式SOFC电解质10,11的外部的炉中。 </li><li>附加热电偶线到数据采集模块。 </li><li>通过USB端口连接数据采集模块到计算机。 注: 图2是示出了MT-FFC测试设置的简化示意图。与开发的模型的燃料和用于控制模型燃料流至燃料电池建立的设置，测试可根据常规˚F继续UEL电池测试方法。这些方法是公建立在文献中和在此将不再重复。 </li></ol><img alt="图2" src="/files/ftp_upload/54638/54638fig2.jpg" /> 的H 2，CO，CO 2 图2微管状火焰辅助燃料电池测试设置示意图。流动N 2（黑色箭头）与一个MFC和一个单向阀，以防止回火调节。从SOFC在炉内的电子流（绿线）的电位和回向SOFC。热电偶数据和电化学数据流由红色箭头表示。 <a href="https://www.jove.com/files/ftp_upload/54638/54638fig2large.jpg" target="_blank">请点击此处查看该图的放大版本。</a>

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The authors have nothing to disclose.

这里讨论的协议是以往的燃烧特性的研究和燃料电池测试之间的重要桥梁。燃料重整和燃料电池测试使用燃烧的已DFFC设置10-15已应用数年。然而，在DFFCs燃烧过程的表征主要涉及原位火焰组合物16的特性，并使用MS 8。作为DFFC是开放的环境中，排气组合物由主要是水和CO 2，而不是所需要的排气的表征。为了开发最近FFC概念的过程用于在部分封闭的腔室表征燃?...

固体氧化物燃料电池（SOFC）的革新已报道在近年来随着技术的不断发展。在众多的优势，固体氧化物燃料电池已经成为众所周知的高燃油效率，低排放和燃油适中灵活性相对于其他基于燃发电技术1。此外，固体氧化物燃料电池是可伸缩的，可用于高燃油效率，即使在小尺度。不幸的是，在当前的氢基础设施的限制已经创建需要一种通常低效的燃料重整系统。最近的发展是微型管状火焰辅助燃料电池（MT-FFC）在笔者的前期工作2的报道。所述MT-FFC是建立在原有的火焰直接型燃料电池（DFFC），其提供热量和燃料通过燃烧3重整的好处的火焰辅助燃料电池（FFC）的第一个例子。该DFFC设置放在与火焰直接接触到开放环境ENVIR一个SOFConment。火焰的部分氧化较重烃类燃料来创建的 H 2和CO，它可以直接用较少潜在相比纯甲烷或其它较重的烃可以使用在固体氧化物燃料电池为碳焦化。另外，该火焰提供以使固体氧化物燃料电池，以它的工作温度所需要的热能。原来的DFFC最近发生的变化通过移动SOFC出火焰区和窜燃烧废气的SOFC创建FFC 2。不像DFFC，燃烧发生在一个部分封闭的腔室（而不是环境温度），以便可以控制燃料与空气的比值和排气，可直接供给到燃料电池不完全燃烧的发生。 FFCS具有其他优势，包括高燃料利用率和电机效率高相比DFFCs 2。 作为一个新兴的研究领域，需要的实验技术，可以评估MT-FF的潜力CS为未来的发电应用。这些技术需要部分氧化，或富燃料燃烧，并已被鉴定为产生的 H 2和CO，也被称为合成气的一种方式的排气分析，用CO 2和H 2 O沿合成气可以直接在燃料电池发电中使用。富燃料燃烧废气的分析已经很好地建立在近年来已进行了理论上4，计算5,6-和实验7用于许多不同的目的。许多理论和计算研究都依赖于化学平衡分析（CEA），以评估燃烧产物品种是积极有利的，和化学动力学模型反应机理。虽然这些方法非常有用，许多新兴技术都在实验技术的研究和开发过程中依赖。实验技术通常依赖于ANA利用燃烧废气的裂解任一气体色谱仪（GC）7或质谱仪（MS）8。无论在GC线/注射器或MS探针插入燃烧废气和测量以评估物种的浓度。实验技术的应用在小规模发电的区域已经屡见不鲜。一些实例包括已开发了单室固体氧化物燃料电池7,9和DFFCs 10-15操作微燃烧器。在宽范围的操作条件，包括不同的温度，流速和当量比发生燃烧废气的分析。 在DFFC研究，燃料和氧化剂的区域可以是部分预混合或非预混，与燃烧器开放以保证完全燃烧的环境。与需要分析火焰组合物中，MS已经在许多情况下用于DFFC研究和燃烧分析16。的FFC的最近发展通过在部分封闭的环境依靠预混合燃烧与燃烧器，以防止燃料的完全氧化而不同。其结果是，需要在从漏气自由受控环境燃烧废气的分析。为此目的开发的实验技术依赖于用于微燃烧室研究与在不同当量比的燃烧排气的GC分析较早的技术。 GC分析导致燃烧废气组合物的表征（ 即 ，每个排气组分包括二氧化碳的体积％，H 2 O，N 2 等 ）该分析允许根据由测得的比率分离气体的混合GC创造未来FFC研究的典范富燃料燃烧废气。 分析富燃料燃烧废气，发展模式富燃料燃烧废气和应用协议ING的SOFC测试排气建立在本文中。共同的挑战和限制对这些技术进行讨论。

<table border="0" cellpadding="0" cellspacing="0" width="758">
	<tbody>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">Gas chromotograph</td>
			<td style="width:111px;">SRI Instruments, Inc.</td>
			<td style="width:129px;">SRI 8610C</td>
			<td style="width:303px;"></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">K type thermocouples</td>
			<td style="width:111px;">Omega</td>
			<td style="width:129px;">KQXL-116G-6</td>
			<td>Custom length</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">K type thermocouple extension wire</td>
			<td style="width:111px;">Omega</td>
			<td style="width:129px;">EXTT-K-20-SLE-100</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">Mass flow controller</td>
			<td style="width:111px;">Omega</td>
			<td style="width:129px;">FMA5427</td>
			<td style="width:303px;">0-40 L/min (N2) 
			Used for methane</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">Mass flow controller</td>
			<td style="width:111px;">Omega</td>
			<td style="width:129px;">FMA5443</td>
			<td style="width:303px;">0-200 L/min (N2) 
			Used for air</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">Mass flow controller</td>
			<td style="width:111px;">Omega</td>
			<td style="width:129px;">FMA5402A</td>
			<td style="width:303px;">0-10 mL/min (N2) 
			Used for CO</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">Mass flow controller</td>
			<td style="width:111px;">Brooks Instrument</td>
			<td style="width:129px;">SLA5850</td>
			<td style="width:303px;">200 SCCM (Propane) 
			Used for CO2</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">Mass flow controller</td>
			<td style="width:111px;">Brooks Instrument</td>
			<td style="width:129px;">SLA5850</td>
			<td style="width:303px;">5 L/min (Air) 
			Used for N2</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">Mass flow controller</td>
			<td style="width:111px;">Brooks Instrument</td>
			<td style="width:129px;">SLA5850</td>
			<td style="width:303px;">500 SCCM (N2) 
			Used for H2</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">Regulator</td>
			<td style="width:111px;">Harris Products Group</td>
			<td style="width:129px;">HP721-125-350-F</td>
			<td style="width:303px;">Methane tank</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">Regulator</td>
			<td style="width:111px;">Harris Products Group</td>
			<td style="width:129px;">HP702-050-590-E</td>
			<td>Air tank</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">Regulator</td>
			<td style="width:111px;">Airgas</td>
			<td style="width:129px;">Y11-SR145B</td>
			<td>CO tank</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">Regulator</td>
			<td style="width:111px;">Harris Products Group</td>
			<td style="width:129px;">HP702-050-320-E</td>
			<td>CO2 tank</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">Regulator</td>
			<td style="width:111px;">Airgas</td>
			<td style="width:129px;">Y12-215B</td>
			<td>N2 tank</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">Regulator</td>
			<td style="width:111px;">Harris Products Group</td>
			<td style="width:129px;">HP702-015-350-D</td>
			<td>H2 tank</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">Methane, Compressed , 
			Ultra high purity</td>
			<td style="width:111px;">Airgas</td>
			<td style="width:129px;">UN1971</td>
			<td style="width:303px;">Extremely Flammable</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">Air, Compressed, 
			Ultra pure</td>
			<td style="width:111px;">Airgas</td>
			<td style="width:129px;">UN1002</td>
			<td style="width:303px;">Not classified as hazardous to health.</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">CO, Compressed, 
			Ultra high purity</td>
			<td style="width:111px;">Airgas</td>
			<td style="width:129px;">UN1016</td>
			<td style="width:303px;">Toxic by inhalation, Extremely flammable</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">CO2, Compressed, 
			Research grade</td>
			<td style="width:111px;">Airgas</td>
			<td style="width:129px;">UN1013</td>
			<td style="width:303px;">Asphyxiant in high 
			concentrations</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">&#160;N2, Compressed, 
			Ultra high purity</td>
			<td style="width:111px;">Airgas</td>
			<td style="width:129px;">UN1066</td>
			<td style="width:303px;">Not classified as hazardous to health.</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">H2, Compressed, 
			Ultra high purity</td>
			<td style="width:111px;">Airgas</td>
			<td style="width:129px;">UN1049</td>
			<td style="width:303px;">Extremely flammable, 
			burns with invisible flame</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">Source meter</td>
			<td style="width:111px;">Tektronix, Inc.</td>
			<td style="width:129px;">Keithley 2420</td>
			<td style="width:303px;">Connects to computer 
			via USB</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">Horizontal split tube furnace</td>
			<td style="width:111px;">MTI Corportation</td>
			<td style="width:129px;">OTF-1200X</td>
			<td style="width:303px;"></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">Data acquisition</td>
			<td style="width:111px;">National Instruments</td>
			<td style="width:129px;">NI cDAQ-9172</td>
			<td style="width:303px;">Connects to computer 
			via USB</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">Thermocouple input</td>
			<td style="width:111px;">National Instruments</td>
			<td style="width:129px;">NI 9211</td>
			<td>Connects to cDAQ-9172</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Computer control for Mass Flow Controllers</td>
			<td style="width:111px;">National Instruments</td>
			<td style="width:129px;">NI 9263</td>
			<td style="width:303px;">Connects to cDAQ-9172 
			Computer control for Mass Flow Controllers</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">Testing software</td>
			<td style="width:111px;">National Instruments</td>
			<td style="width:129px;">LabVIEW 8.6</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:43px;width:216px;">Ceramabond</td>
			<td style="width:111px;">Aremco</td>
			<td>552-VFG</td>
			<td>1 Pint</td>
		</tr>
	</tbody>
</table>

combustion characterization and model fuel development for micro-tubular flame-assisted fuel cells

Combustion based power generation has been accomplished for many years through a number of heat engine systems. Recently, a move towards small scale power generation and micro combustion as well as development in fuel cell research has created new means of power generation that combine solid oxide fuel cells with open flames and combustion exhaust. Instead of relying upon the heat of combustion, these solid oxide fuel cell systems rely on reforming of the fuel via combustion to generate syngas for electrochemical power generation. Procedures were developed to assess the combustion by-products under a wide range of conditions. While theoretical and computational procedures have been developed for assessing fuel-rich combustion exhaust in these applications, experimental techniques have also emerged. The experimental procedures often rely upon a gas chromatograph or mass spectrometer analysis of the flame and exhaust to assess the combustion process as a fuel reformer and means of heat generation. The experimental techniques developed in these areas have been applied anew for the development of the micro-tubular flame-assisted fuel cell. The protocol discussed in this work builds on past techniques to specify a procedure for characterizing fuel-rich combustion exhaust and developing a model fuel-rich combustion exhaust for use in flame-assisted fuel cell testing. The development of the procedure and its applications and limitations are discussed.

燃烧特性室应当在期望当量比为空气的逆流进入测试期间的腔室或其他空气泄漏测试之前进行检查。在开室燃烧过程被称为是几乎同量异序。其结果是，燃烧室内的压力可能不足以确保无来自外部环境的空气是回流入从室排气口或其它渗漏点燃烧室。有几个实验技术，以确认没有逆流发生。首先，对于一个非催化燃烧器，富-可燃性限值是公建立了许多燃料18,19。?...

Watch this Scientific Journal Video about Combustion Characterization and Model Fuel Development for Micro-tubular Flame-assisted Fuel Cells at JoVE.com

Combustion Characterization and Model Fuel Development for Micro-tubular Flame-assisted Fuel Cells

A protocol for creating a model fuel-rich combustion exhaust is developed through combustion characterization and is applied for micro-tubular flame-assisted fuel cell testing and research.

燃烧特性参数和模型燃料开发的微型管状火焰辅助燃料电池

Combustion based power generation has been accomplished for many years through a number of heat engine systems. Recently, a move towards small scale power ...

combustion-characterization-model-fuel-development-for-micro-tubular

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Unit 1

Alkanes and Cycloalkanes

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9.5K 次观看.  Syracuse University. A protocol for creating a model fuel-rich combustion exhaust is developed through combustion characterization and is applied for micro-tubular flame-assisted fuel cell testing and research.

视频: Combustion Characterization and Model Fuel Development for Micro-tubular Flame-assisted Fuel Cells

Probing and Mapping Electrode Surfaces in Solid Oxide Fuel Cells

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen 1-7. The performance of SOFCs and the rates of many chemical and energy transformation processes in energy storage and conversion devices in general are limited primarily by charge and mass transfer along electrode surfaces and across interfaces. Unfortunately, the mechanistic understanding of these processes is still lacking, due largely to the difficulty of characterizing these processes under in situ conditions. This knowledge gap is a chief obstacle to SOFC commercialization. The development of tools for probing and mapping surface chemistries relevant to electrode reactions is vital to unraveling the mechanisms of surface processes and to achieving rational design of new electrode materials for more efficient energy storage and conversion2. Among the relatively few in situ surface analysis methods, Raman spectroscopy can be performed even with high temperatures and harsh atmospheres, making it ideal for characterizing chemical processes relevant to SOFC anode performance and degradation8-12. It can also be used alongside electrochemical measurements, potentially allowing direct correlation of electrochemistry to surface chemistry in an operating cell. Proper in situ Raman mapping measurements would be useful for pin-pointing important anode reaction mechanisms because of its sensitivity to the relevant species, including anode performance degradation through carbon deposition8, 10, 13, 14 ("coking") and sulfur poisoning11, 15 and the manner in which surface modifications stave off this degradation16. The current work demonstrates significant progress towards this capability. In addition, the family of scanning probe microscopy (SPM) techniques provides a special approach to interrogate the electrode surface with nanoscale resolution. Besides the surface topography that is routinely collected by AFM and STM, other properties such as local electronic states, ion diffusion coefficient and surface potential can also be investigated17-22. In this work, electrochemical measurements, Raman spectroscopy, and SPM were used in conjunction with a novel test electrode platform that consists of a Ni mesh electrode embedded in an yttria-stabilized zirconia (YSZ) electrolyte. Cell performance testing and impedance spectroscopy under fuel containing H2S was characterized, and Raman mapping was used to further elucidate the nature of sulfur poisoning. In situ Raman monitoring was used to investigate coking behavior. Finally, atomic force microscopy (AFM) and electrostatic force microscopy (EFM) were used to further visualize carbon deposition on the nanoscale. From this research, we desire to produce a more complete picture of the SOFC anode.

We present a unique platform for characterizing electrode surfaces in solid oxide fuel cells (SOFCs) that allows simultaneous performance of multiple characterization techniques (e.g. in situ Raman spectroscopy and scanning probe microscopy alongside electrochemical measurements). Complementary information from these analyses may help to advance toward a more profound understanding of electrode reaction and degradation mechanisms, providing insights into rational design of better materials for SOFCs.

在固体氧化物燃料电池电极表面的探测和测绘

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen ...

科研

工程学

Preparation and Evaluation of Hybrid Composites of Chemical Fuel and Multi-walled Carbon Nanotubes in the Study of Thermopower Waves

When a chemical fuel at a certain position in a hybrid composite of the fuel and a micro/nanostructured material is ignited, chemical combustion occurs along the interface between the fuel and core materials. Simultaneously, dynamic changes in thermal and chemical potentials across the micro/nanostructured materials result in concomitant electrical energy generation induced by charge transfer in the form of a high-output voltage pulse. We demonstrate the entire procedure of a thermopower wave experiment, from synthesis to evaluation. Thermal chemical vapor deposition and the wet impregnation process are respectively employed for the synthesis of a multi-walled carbon nanotube array and a hybrid composite of picric acid/sodium azide/multi-walled carbon nanotubes. The prepared hybrid composites are used to fabricate a thermopower wave generator with connecting electrodes. The combustion of the hybrid composite is initiated by laser heating or Joule-heating, and the corresponding combustion propagation, direct electrical energy generation, and real-time temperature changes are measured using a high-speed microscopy system, an oscilloscope, and an optical pyrometer, respectively. Furthermore, the crucial strategies to be adopted in the synthesis of hybrid composite and initiation of their combustion that enhance the overall thermopower wave energy transfer are proposed.

A protocol for conducting thermopower wave experiments is presented. The synthesis of hybrid composites of a chemical fuel and micro/nanostructured material, manufacturing of a thermopower wave generator, and methods for measuring the corresponding physical phenomena are described.

化学燃料和多壁碳纳米管的混杂复合材料的热电波的研究准备和评估

When a chemical fuel at a certain position in a hybrid composite of the fuel and a micro/nanostructured material is ignited, chemical combustion occurs ...

Characterization of Nanocrystal Size Distribution using Raman Spectroscopy with a Multi-particle Phonon Confinement Model

Analysis of the size distribution of nanocrystals is a critical requirement for the processing and optimization of their size-dependent properties. The common techniques used for the size analysis are transmission electron microscopy (TEM), X-ray diffraction (XRD) and photoluminescence spectroscopy (PL). These techniques, however, are not suitable for analyzing the nanocrystal size distribution in a fast, non-destructive and a reliable manner at the same time. Our aim in this work is to demonstrate that size distribution of semiconductor nanocrystals that are subject to size-dependent phonon confinement effects, can be quantitatively estimated in a non-destructive, fast and reliable manner using Raman spectroscopy. Moreover, mixed size distributions can be separately probed, and their respective volumetric ratios can be estimated using this technique. In order to analyze the size distribution, we have formulized an analytical expression of one-particle PCM and projected it onto a generic distribution function that will represent the size distribution of analyzed nanocrystal. As a model experiment, we have analyzed the size distribution of free-standing silicon nanocrystals (Si-NCs) with multi-modal size distributions. The estimated size distributions are in excellent agreement with TEM and PL results, revealing the reliability of our model.

We demonstrate how to determine the size distribution of semiconductor nanocrystals in a quantitative manner using Raman spectroscopy employing an analytically defined multi-particle phonon confinement model. Results obtained are in excellent agreement with the other size analysis techniques like transmission electron microscopy and photoluminescence spectroscopy.

使用拉曼光谱与多颗粒的声子坐月子型号纳米大小分布的特征

Analysis of the size distribution of nanocrystals is a critical requirement for the processing and optimization of their size-dependent properties. The ...

Printing Fabrication of Bulk Heterojunction Solar Cells and In Situ Morphology Characterization

Polymer-based materials hold promise as low-cost, flexible efficient photovoltaic devices. Most laboratory efforts to achieve high performance devices have used devices prepared by spin coating, a process that is not amenable to large-scale fabrication. This mismatch in device fabrication makes it difficult to translate quantitative results obtained in the laboratory to the commercial level, making optimization difficult. Using a mini-slot die coater, this mismatch can be resolved by translating the commercial process to the laboratory and characterizing the structure formation in the active layer of the device in real time and in situ as films are coated onto a substrate. The evolution of the morphology was characterized under different conditions, allowing us to propose a mechanism by which the structures form and grow. This mini-slot die coater offers a simple, convenient, material efficient route by which the morphology in the active layer can be optimized under industrially relevant conditions. The goal of this protocol is to show experimental details of how a solar cell device is fabricated using a mini-slot die coater and technical details of running in situ structure characterization using the mini-slot die coater.

Printing Fabrication of Bulk Heterojunction Solar Cells and In Situ Morphology Characterization

Here, we present a protocol to fabricate organic thin film solar cells using a mini-slot die coater and related in-line structure characterizations using synchrotron scattering techniques.

散装异质结太阳能电池的印刷和制作<em&gt;原位</em&gt;形态特征

Polymer-based materials hold promise as low-cost, flexible efficient photovoltaic devices. Most laboratory efforts to achieve high performance devices ...

Reaction Kinetics and Combustion Dynamics of I4O9 and Aluminum Mixtures

Tetraiodine nonoxide (I4O9) has been synthesized using a dry approach that combines elemental oxygen and iodine without the introduction of hydrated species. The synthesis approach inhibits the topochemical effect promoting rapid hydration when exposed to the relative humidity of ambient air. This stable, amorphous, nano-particle material was analyzed using differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA) and showed an exothermic energy release at low temperature (i.e., 180 &#176;C) for the transformation of I4O9 into I2O5. This additional exothermic energy release contributes to an increase in overall reactivity of I4O9 when dry mixed with nano-aluminum (Al) powder, resulting in a minimum of 150% increase in flame speed compared to Al + I2O5. This study shows that as an oxidizer, I4O9 has more reactive potential than other forms of iodine(V) oxide when combined with Al, especially if I4O9 can be passivated to inhibit absorption of water from its surrounding environment.

Reaction Kinetics and Combustion Dynamics of I4O9 and Aluminum Mixtures

A protocol for measuring flame speeds of a reactive mixture composed of tetraiodine nonoxide (I4O9) and aluminum (Al) is presented. A method for resolving reaction kinetics using differential scanning calorimetry (DSC) is also presented. It was found that I4O9 is 150% more reactive than other iodine(V) oxides.

反应动力学和我燃烧动力学<sub&gt; 4</sub&gt; 0<sub&gt; 9</sub&gt;和铝的混合物

Tetraiodine nonoxide (I4O9) has been synthesized using a dry approach that combines elemental oxygen and iodine without the introduction of hydrated ...

Two-way Valorization of Blast Furnace Slag: Synthesis of Precipitated Calcium Carbonate and Zeolitic Heavy Metal Adsorbent

The aim of this work is to present a zero-waste process for storing CO2 in a stable and benign mineral form while producing zeolitic minerals with sufficient heavy metal adsorption capacity. To this end, blast furnace slag, a residue from iron-making, is utilized as the starting material. Calcium is selectively extracted from the slag by leaching with acetic acid (2 M CH3COOH) as the extraction agent. The filtered leachate is subsequently physico-chemically purified and then carbonated to form precipitated calcium carbonate (PCC) of high purity (&lt;2 wt% non-calcium impurities, according to ICP-MS analysis). Sodium hydroxide is added to neutralize the regenerated acetate. The morphological properties of the resulting calcitic PCC are tuned for its potential application as a filler in papermaking. In parallel, the residual solids from the extraction stage are subjected to hydrothermal conversion in a caustic solution (2 M NaOH) that leads to the predominant formation of a particular zeolitic mineral phase (detected by XRD), namely analcime (NaAlSi2O6&#8729;H2O). Based on its ability to adsorb Ni2+, as reported from batch adsorption experiments and ICP-OES analysis, this product can potentially be used in wastewater treatment or for environmental remediation applications.

A protocol for the parallel production of precipitated calcium carbonate and zeolitic material from blast furnace slag via mineral carbonation and alkaline hydrothermal conversion, respectively, is presented. The performance of the zeolitic material towards nickel adsorption is tested.

高炉矿渣的双向稳定物价:沉淀碳酸钙和沸石重金属吸附剂的合成

The aim of this work is to present a zero-waste process for storing CO2 in a stable and benign mineral form while producing zeolitic minerals with ...

Infrared Degenerate Four-wave Mixing with Upconversion Detection for Quantitative Gas Sensing

We present a protocol for performing gas spectroscopy using infrared degenerated four-wave mixing (IR-DFWM), for the quantitative detection of gas species in the ppm-to-single-percent range. The main purpose of the method is the spatially resolved detection of low-concentration species, which have no transitions in the visible or near-IR spectral range that could be used for detection. IR-DFWM is a nonintrusive method, which is a great advantage in combustion research, as inserting a probe into a flame can change it drastically. The IR-DFWM is combined with upconversion detection. This detection scheme uses sum-frequency generation to move the IR-DFWM signal from the mid-IR to the near-IR region, to take advantage of the superior noise characteristics of silicon-based detectors. This process also rejects most of the thermal background radiation. The focus of the protocol presented here is on the proper alignment of the IR-DFWM optics and on how to align an intracavity upconversion detection system.

Here, we present a protocol to perform sensitive, spatially resolved gas spectroscopy in the mid-infrared region, using degenerate four-wave mixing combined with upconversion detection.

用于定量气体传感的红外退化四波融合与上转换检测

We present a protocol for performing gas spectroscopy using infrared degenerated four-wave mixing (IR-DFWM), for the quantitative detection of gas species ...

Method Development for Contactless Resonant Cavity Dielectric Spectroscopic Studies of Cellulosic Paper

The current analytical techniques for characterizing printing and graphic arts substrates are largely ex situ and destructive. This limits the amount of data that can be obtained from an individual sample and renders it difficult to produce statistically relevant data for unique and rare materials. Resonant cavity dielectric spectroscopy is a non-destructive, contactless technique which can simultaneously interrogate both sides of a sheeted material and provide measurements which are suitable for statistical interpretations. This offers analysts the ability to quickly discriminate between sheeted materials based on composition and storage history. In this methodology article, we demonstrate how contactless resonant cavity dielectric spectroscopy may be used to differentiate between paper analytes of varying fiber species compositions, to determine the relative age of the paper, and to detect and quantify the amount of post-consumer waste (PCW) recycled fiber content in manufactured office paper.

A protocol for the non-destructive analysis of the fiber content and relative age of paper.

纤维素纸非接触式共振腔电谱研究的方法研究

The current analytical techniques for characterizing printing and graphic arts substrates are largely ex situ and destructive. This limits the amount of ...

Terahertz Imaging and Characterization Protocol for Freshly Excised Breast Cancer Tumors

This manuscript presents a protocol to handle, characterize, and image freshly excised human breast tumors using pulsed terahertz imaging and spectroscopy techniques. The protocol involves terahertz transmission mode at normal incidence and terahertz reflection mode at an oblique angle of 30&#176;. The collected experimental data represent time domain pulses of the electric field. The terahertz electric field signal transmitted through a fixed point on the excised tissue is processed, through an analytical model, to extract the refractive index and absorption coefficient of the tissue. Utilizing a stepper motor scanner, the terahertz emitted pulse is reflected from each pixel on the tumor providing a planar image of different tissue regions. The image can be presented in time or frequency domain. Furthermore, the extracted data of the refractive index and absorption coefficient at each pixel are utilized to provide a tomographic terahertz image of the tumor. The protocol demonstrates clear differentiation between cancerous and healthy tissues. On the other hand, not adhering to the protocol can result in noisy or inaccurate images due to the presence of air bubbles and fluid remains on the tumor surface. The protocol provides a method for surgical margins assessment of breast tumors.

Freshly excised human breast cancer tumors are characterized with terahertz spectroscopy and imaging following fresh tissue handling protocols. Tissue positioning is taken into consideration to enable effective characterization while providing analysis in a timely manner for future intraoperative applications.

新切除乳腺癌肿瘤的Terahertz成像和表征协议

This manuscript presents a protocol to handle, characterize, and image freshly excised human breast tumors using pulsed terahertz imaging and spectroscopy ...

Fabrication and Characterization of Thickness Mode Piezoelectric Devices for Atomization and Acoustofluidics

We present a technique to fabricate simple thickness mode piezoelectric devices using lithium niobate (LN). Such devices have been shown to atomize liquid more efficiently, in terms of &#64258;ow rate per power input, than those that rely on Rayleigh waves and other modes of vibration in LN or lead zirconate titanate (PZT). The complete device is composed of a transducer, a transducer holder, and a &#64258;uid supply system. The fundamentals of acoustic liquid atomization are not well known, so techniques to characterize the devices and to study the phenomena are also described. Laser Doppler vibrometry (LDV) provides vibration information essential in comparing acoustic transducers and, in this case, indicates whether a device will perform well in thickness vibration. It can also be used to &#64257;nd the resonance frequency of the device, though this information is obtained more quickly via impedance analysis. Continuous &#64258;uid atomization, as an example application, requires careful &#64258;uid flow control, and we present such a method with high-speed imaging and droplet size distribution measurements via laser scattering.

Fabrication of piezoelectric thickness mode transducers via direct current sputtering of plate electrodes on lithium niobate is described. Additionally, reliable operation is achieved with a transducer holder and &#64258;uid supply system and characterization is demonstrated via impedance analysis, laser doppler vibrometry, high-speed imaging, and droplet size distribution using laser scattering.

用于原子化和抗波流体的厚度模式压电器件的制造和特性

We present a technique to fabricate simple thickness mode piezoelectric devices using lithium niobate (LN). Such devices have been shown to atomize liquid ...

燃烧特性参数和模型燃料开发的微型管状火焰辅助燃料电池

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