这项工作是由美国国家科学基金会批准号DMR-1207243，美国国家科学基金会MRSEC程序支持（DMR-0820414），美国能源部批准号：DE-FG02-03ER46054，以及俄勒冈州立大学，金属材料研究所。作者承认了纳米技术实验室在俄亥俄州立大学，以及CY花王和CY陈技术援助。

1.合成和前体的制备<ol><li> [的Et 4 N]的制备[V（CO）6] 23 <ol><li>在氮气手套箱中，切1.88克金属钠到〜40片，并与14.84克蒽的1升三颈圆底烧瓶中混合320毫升无水四氢呋喃（THF）。 注意：这两种金属钠和四​​氢呋喃是高度易燃的。 </li><li>在RT搅拌在氮气氛下的溶液4.5小时，直到NAC 14 H 10被形成深蓝色溶液。 </li><li>冷却该溶液至0℃。 </li><li>在氮气手套箱中，通过加入400毫升无水THF中制备的VCL 3（THF）3的粉红色溶液变成7.48克的VCl 3（THF）3的在500毫升圆底烧瓶中，并在RT搅拌1小时。 </li><li>除去从手套箱的粉红色溶液的VCl 3（THF）3，并冷却至0℃，20分钟。转移到前SOLU经氮气气氛下插管NAC 14 H 10的重刑。均相深紫色溶液立即形成在加入完成之后。 </li><li>从氮中除去，并搅拌15小时。缓慢升温至RT放置在瓶冰桶让冰融化O / N。 </li><li>再次冷却该溶液至0℃，并填充反应烧瓶用一氧化碳。该解决方案将来自深紫变为黄褐色在几分钟之内。 警告：一氧化碳是剧毒。此步骤不应单独进行，一个一氧化碳警报应安装在实验室。 </li><li>搅拌一氧化碳气氛下将溶液在0℃下15小时，然后缓慢温热至室温。 </li><li>除去THF的所有但200毫升真空下。加入500毫升邻2自由水，同时搅拌溶液。 V（CO）6容易被氧化和O 2的存在将导致低收率。 </li><li>过滤所得黄色浆液成的20.8克溴化四乙基铵组成的溶液在200毫升H 2 O（乙醚4 NBR） </li><li>洗涤滤饼用O 2自由水，直到它是无色的。 </li><li>过滤所得[的Et 4 N] [V（CO）6]通过真空过滤的浆液并在真空下干燥。 </li><li>店[的Et 4 N] [V（CO）6]在手套箱冷冻以供将来使用。 </li></ol></li><li> Ⅴ的制备（CO）6 23 <ol><li>油脂的连接点的真空适配器活塞，玻璃双向连接管和冷的手指。放置冷手指在中心颈和一真空接头与活塞中的第三开口。 </li><li>在氩气手套箱中，混合100毫克〔的Et 4 N] [V（CO）6]用1克磷酸中包含磁力搅拌棒的圆底烧瓶中。 </li><li>通过玻璃双向连接桶圆底烧瓶连接到一个三颈圆底烧瓶E在氩气手套箱。 </li><li>从手套箱中取出密封烧瓶制度，建立化学罩。 </li><li>加甲醇至冷手指和搅拌用刮刀-同时加入液氮中直至甲醇被冻结。通过打开旋塞到真空管线，直至压力达到5×10 -2乇抽真空系统。 </li><li>淹没在油浴套的圆底烧瓶至45℃，并开启磁力搅拌。一旦反应开始，所述磷酸会熔化和一个黑蓝色粉末凝结在冷手指。 </li><li>打开真空管线时黑色粉末凝结在圆底烧瓶代替的冷指由于压力过高。收盘前再次泵系统恢复到5×10 -2托。 </li><li>旋转根据需要将反应烧瓶以混合所有的反应物。 </li><li>使反应继续进行，直到在圆底烧瓶中剩余的残余物是白灰色，并且不再冒泡。</li><li>覆铜球团成一个寒冷的安全容器中，冷却用液氮。 </li><li>从指形冷却件用微量除去甲醇。倒入冰镇铜丸进入冷手指转移到手套箱过程中保持低温。 </li><li>转移到氩手套箱前擦净油和凝结水关烧瓶系统。 </li><li>里面的手套箱，取出冷手指从烧瓶系统和用刮刀刮去黑色V（CO）6粉末到一张称重纸上的。 </li><li>商店V（CO）6在氩气氛下一个瓶，并保持低于室温。 </li></ol></li><li> TCNE通过升华纯化<ol><li>购买市售四氰基（TCNE），并储存在冰箱中的化学。 </li><li>拌〜5克TCNE用约0.5克活性炭和研磨带研钵和杵。 </li><li>将TCNE /碳混合物到玻璃船或包裹在微妙的任务湿巾放在底部的烧瓶与真空线。 </li><li>放置冷手指到烧瓶的顶部，并与夹紧密封两个部分组合在一起。 </li><li>加甲醇至冷手指和搅拌用刮刀-同时加入液氮中直至甲醇被冻结。把这个包含TCNE在油浴中加热至70℃的烧瓶的底部。 </li><li>打开真空管线达到10 -4托的压力，然后关闭真空线。 </li><li>偶尔打开真空管线以保持压力。 TCNE凝结在冰冷的手指升华开始。一旦没有更多的TCNE积聚在冷手指升华结束。 </li><li>从指形冷却件用微量除去甲醇。 </li><li>转移到氩手套箱前擦净油和凝结水关烧瓶系统。 </li><li>里面的手套箱，除去寒手指从瓶中系统用刮刀刮去TCNE粉到一张纸重的。 </li><li>申通快递重新纯化TCNE在惰性气氛下低于室温冰箱。 </li></ol></li></ol> 2.设置沉积系统内部的氩气手套箱<ol><li>装配该反应器在氩气手套箱内， 如图1A所示 。 <ol><li>设置到真空泵的连接。 </li><li>由流量计和两行连接到微米阀之间连接一个3路活塞设置气体流的连接。 </li><li>滑动反应器（A部分， 图1B）周围的玻璃加热线圈。 </li><li>包裹有聚四氟乙烯（PTFE）密封条载玻片。 </li><li>从右侧的反应器中，部分A的推载玻片约10cm </li><li>放置在B部分的O型圈和滑入右侧的反应堆。用卡子连接的两片在一起。 </li><li>附加真空管线对A部分的底部连接和压力表连接到顶部连接。 </li><li>放置填充船ED与纯化TCNE到C部分近端，使得TCNE将在反应器的最热的部分坐。 </li><li>脂部分C的连接，并将它推入反应器的左侧。 </li><li>油脂T型船装满V（CO）6和幻灯片的两边成部分B的右端</li><li>每个连接阀微米。一应连接到右侧的T形船及其它到部分C的左侧和在地方夹紧两者。 </li><li>运行测试沉积，以确定该反应区的位置。 </li></ol></li><li>存款V [TCNE]×〜2基板上<ol><li>设置反应加热线圈的温度，从而当在反应器的底部和TCNE船的面积测得接近75℃的反应区设置为一个值接近46℃。设置一个硅油浴的温度升高到10℃。允许温度为至少30分钟稳定。 </li><li>滑动玻璃加热器COI升反应器（A部分， 图1A）左右。 </li><li>包裹有聚四氟乙烯（PTFE）密封条载玻片。安排在覆盖的滑动的顶部的样品的两英寸的空间内。 </li><li>推载玻片到反应器中，以便将样品位于反应区中。交替样品可直接放置在反应器的底部，虽然反应区可在没有一个载玻片被移位。 </li><li>放置在B部分的O型圈和滑入右侧的反应堆。用卡子连接的两片在一起。 </li><li>附加真空管线对A部分的底部连接和压力表连接到顶部连接。 </li><li>把50毫克TCNE入TCNE船和5毫克V（CO）6到T-舟（这些量是适合的75-90分钟的沉积）。 </li><li>该艇TCNE滑入C部分接近尾声，使得TCNE将在应约75℃，反应器的最热的部分坐。 </li><li<html> &gt;黄油C部分的连接，并将其滑入反应器的左侧。 </li><li>油脂T型船和幻灯片两侧成部分B的右端</li><li>流动线滑到右侧的T-船和C部分的左侧边和夹紧到位。组装的建立应该类似于图1A。 </li><li>提高的油浴以覆盖T型船的整个底部。 </li><li>打开真空管线达到30-35毫米汞柱的压力。 </li><li>对于V（CO）6和84标准立方厘米为TCNE设置流速至56标准立方厘米。反应应在反应区的壁中的绿色材料冷凝立即开始。 </li><li>允许反应进行所需的时间长度。该薄膜的厚度是根据反应器内的反应时间和位置， 如图2所示。 </li><li>以停止反应，靠近真空线和关闭加热器和油浴中。 </li></ol></li></ol>ove_title“&gt; 3。清理<ol><li>拆开该系统中的任何命令。 </li><li>浸泡所有的玻璃器皿中，除了至少1-2个小时的基础灌流液加热线圈。 </li><li>冲洗玻璃器皿与水和干的炉中。 </li></ol><img alt="图1" src="/files/ftp_upload/52891/52891fig1.jpg" /> 图1（A）完全组装定制化学气相沉积（CVD）系统。 （ 二）成分的CVD系统的扩展视图。 <a href="https://www.jove.com/files/ftp_upload/52891/52891fig1large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图2" src="/files/ftp_upload/52891/52891fig2.jpg" /> 图2.（A）的反应器中的示出其位置的基板的顶视图。 （B）近似薄膜厚度的反应管，部分是由图1B为75分钟的沉积内侧的位置功能。 <a href="https://www.jove.com/files/ftp_upload/52891/52891fig2large.jpg" target="_blank">请点击此处查看该图的放大版本。</a>

<ol>
	<li>Yoo, J. W., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Spin+injection/detection+using+an+organic-based+magnetic+semiconductor.">Spin injection/detection using an organic-based magnetic semiconductor.</a> Nat. Mater. 9, 638-642 (2010).</li><li>Li, B., 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=Room-temperature+organic-based+spin+polarizer.">Room-temperature organic-based spin polarizer.</a> Appl. Phys. Lett. 99, 153503 (2011).</li><li>Li, B., Kao, C. Y., Yoo, J. W., Prigodin, V. N., Epstein, A. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Magnetoresistance+in+an+All-Organic-Based+Spin+Valve.">Magnetoresistance in an All-Organic-Based Spin Valve.</a> Adv. Mater. 23, 3382-3386 (2011).</li><li>Fang, L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrical+Spin+Injection+from+an+Organic-Based+Ferrimagnet+in+a+Hybrid+Organic-Inorganic+Heterostructure.">Electrical Spin Injection from an Organic-Based Ferrimagnet in a Hybrid Organic-Inorganic Heterostructure.</a> Phys. Rev. Lett. 106, 156602 (2011).</li><li>Yu, H., 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=Ultra-narrow+ferromagnetic+resonance+in+organic-based+thin+films+grown+via+low+temperature+chemical+vapor+deposition.">Ultra-narrow ferromagnetic resonance in organic-based thin films grown via low temperature chemical vapor deposition.</a> Appl. Phys. Lett. 105, 012407 (2014).</li><li>Manriquez, J. M., Yee, G. T., McLean, R. S., Epstein, A. J., Miller, J. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+Room-Temperature+Molecular+Organic+Based+Magnet.">A Room-Temperature Molecular Organic Based Magnet.</a> Science. 252, 1415-1417 (1991).</li><li>Pokhodnya, K. I., Epstein, A. J., Miller, J. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Thin-film V TCNE (x) magnets. Adv. Mater. 12, 410-413 (2000).</li><li>Carlegrim, E., Kanciurzewska, A., Nordblad, P., Fahlman, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Air-stable+organic-based+semiconducting+room+temperature+thin+film+magnet+for+spintronics+applications.">Air-stable organic-based semiconducting room temperature thin film magnet for spintronics applications.</a> Appl. Phys. Lett. 92, 163308 (2008).</li><li>Kao, C. Y., Yoo, J. W., Min, Y., Epstein, A. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Molecular+Layer+Deposition+of+an+Organic-Based+Magnetic+Semiconducting+Laminate.">Molecular Layer Deposition of an Organic-Based Magnetic Semiconducting Laminate.</a> ACS Appl. Mater. Interfaces. 4, 137-141 (2012).</li><li>Miller, J. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Oliver+Kahn+Lecture:+Composition+and+structure+of+the+V+TCNE+(x)+(TCNE+=+tetracyanoethylene)+room-temperature,+organic-based+magnet+-+A+personal+perspective.">Oliver Kahn Lecture: Composition and structure of the V TCNE (x) (TCNE = tetracyanoethylene) room-temperature, organic-based magnet - A personal perspective.</a> Polyhedron. 28, 1596-1605 (2009).</li><li>Haskel, D., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Local+structural+order+in+the+disordered+vanadium+tetracyanoethylene+room-temperature+molecule-based+magnet.">Local structural order in the disordered vanadium tetracyanoethylene room-temperature molecule-based magnet.</a> Phys. Rev. B. 70, 054422 (2004).</li><li>Prigodin, V. N., Raju, N. P., Pokhodnya, K. I., Miller, J. S., Epstein, A. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Spin-Driven+Resistance+in+Organic-Based+Magnetic+Semiconductor+V[TCNE]x.">Spin-Driven Resistance in Organic-Based Magnetic Semiconductor V[TCNE]x.</a> Adv. Mater. 14, 1230-1233 (2002).</li><li>Yoo, J. W., Edelstein, R. S., Lincoln, D. M., Raju, N. P., Epstein, A. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Photoinduced+magnetism+and+random+magnetic+anisotropy+in+organic-based+magnetic+semiconductor+V(TCNE)(x)+films,+for+x+similar+to+2.">Photoinduced magnetism and random magnetic anisotropy in organic-based magnetic semiconductor V(TCNE)(x) films, for x similar to 2.</a> Phys. Rev. Lett. 99 (15), 157205 (2007).</li><li>Cimpoesu, F., Frecus, B., Oprea, C. I., Panait, P., G&#238;r&#355;u, M. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Disorder,+exchange+and+magnetic+anisotropy+in+the+room-temperature+molecular+magnet+V[TCNE]x+&#8211;+A+theoretical+study.">Disorder, exchange and magnetic anisotropy in the room-temperature molecular magnet V[TCNE]x &#8211; A theoretical study.</a> Computational Materials Science. 91, 320-328 (2014).</li><li>Raju, N. P., Prigodin, V. N., Pokhodnya, K. I., Miller, J. S., Epstein, A. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=High+field+linear+magnetoresistance+in+fully+spin-polarized+high-temperature+organic-based+ferrimagnetic+semiconductor+V(TCNE)(x)+films,+x+similar+to+2.">High field linear magnetoresistance in fully spin-polarized high-temperature organic-based ferrimagnetic semiconductor V(TCNE)(x) films, x similar to 2.</a> Synth. Met. 160, 307-310 (2010).</li><li>Raju, N. P., 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=Anomalous+magnetoresistance+in+high-temperature+organic-based+magnetic+semiconducting+V(TCNE)(x)+films.">Anomalous magnetoresistance in high-temperature organic-based magnetic semiconducting V(TCNE)(x) films.</a> J. Appl. Phys. 93, 6799-6801 (2003).</li><li>Yoo, J. W., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Multiple+photonic+responses+in+films+of+organic-based+magnetic+semiconductor+V(TCNE)(x),+x+similar+to+2.">Multiple photonic responses in films of organic-based magnetic semiconductor V(TCNE)(x), x similar to 2.</a> Phys. Rev. Lett. 97, 247205 (2006).</li><li>Yoo, J. W., Edelstein, R. S., Raju, N. P., Lincoln, D. M., Epstein, A. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Novel+mechanism+of+photoinduced+magnetism+in+organic-based+magnetic+semiconductor+V(TCNE)(x),+x+similar+to+2.">Novel mechanism of photoinduced magnetism in organic-based magnetic semiconductor V(TCNE)(x), x similar to 2.</a> J. Appl. Phys. 103, 07B912 (2008).</li><li>Caro, D., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=CVD-grown+thin+films+of+molecule-based+magnets.">CVD-grown thin films of molecule-based magnets.</a> Chem. Mat. 12, 587-589 (2000).</li><li>Erickson, P. K., Miller, J. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thin+film+Co+TCNE+(2)+and+VyCo1-y+TCNE+(2)+magnetic+materials.">Thin film Co TCNE (2) and VyCo1-y TCNE (2) magnetic materials.</a> J. Magn. Magn. Mater. 324 (2), 2218-2223 (2012).</li><li>Valade, L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thin+films+of+molecular+materials+grown+on+silicon+substrates+by+chemical+vapor+deposition+and+electrodeposition.">Thin films of molecular materials grown on silicon substrates by chemical vapor deposition and electrodeposition.</a> J. Low Temp. Phys. 142, 393-396 (2006).</li><li>Casellas, H., de Caro, D., Valade, L., Cassoux, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+new+chromium-based+molecular+magnet+grown+as+a+thin+film+by+CVD.">A new chromium-based molecular magnet grown as a thin film by CVD.</a> Chem. Vapor Depos. 8, 145-147 (2002).</li><li>Barybin, M. V., Pomije, M. K., Ellis, J. E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Highly+reduced+organometallics+-+42.+A+new+method+for+the+syntheses+of+V(CO)(6)+(-)+and+V(PF3)(6)+(-)+involving+anthracenide+mediated+reductions+of+VCl3(THF)(3).">Highly reduced organometallics - 42. A new method for the syntheses of V(CO)(6) (-) and V(PF3)(6) (-) involving anthracenide mediated reductions of VCl3(THF)(3).</a> Inorg. Chim. Acta. 269, 58-62 (1998).</li><li>Froning, I. H. M., Lu, Y., Epstein, A. J., Johnston-Halperin, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thin-film+Encapsulation+of+the+Air-Sensitive+Organic+Ferrimagnet+Vanadium+Tetracyanoethylene.">Thin-film Encapsulation of the Air-Sensitive Organic Ferrimagnet Vanadium Tetracyanoethylene.</a> Appl. Phys. Lett. 106, 122403 (2015).</li><li>Pokhodnya, K. I., Bonner, M., Miller, J. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Parylene+protection+coatings+for+thin+film+V+TCNE+(x)+room+temperature+magnets.">Parylene protection coatings for thin film V TCNE (x) room temperature magnets.</a> Chem. Mat. 16, 5114-5119 (2004).</li><li>Shima Edelstein, R., Yoo, J. -. W., Raju, N. P., Bergeson, J. D., Pokhodnya, K. I., Miller, J. S., Epstein, A. J., Tessler, N., Arias, A. C., Burgi, L., Emerson, J. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Materials Research Society. , (2005).</li><li>Katz, H. E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Recent+advances+in+semiconductor+performance+and+printing+processes+for+organic+transistor-based+electronics).">Recent advances in semiconductor performance and printing processes for organic transistor-based electronics).</a> Chem. Mat. 16, 4748-4756 (2004).</li><li>Subbarao, S. P., Bahlke, M. E., Kymissis, I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Laboratory+Thin-Film+Encapsulation+of+Air-Sensitive+Organic+Semiconductor+Devices.">Laboratory Thin-Film Encapsulation of Air-Sensitive Organic Semiconductor Devices.</a> IEEE Trans. Electron Devices. 57, 153-156 (2010).</li><li>Lungenschmied, C., 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=Flexible,+long-lived,+large-area,+organic+solar+cells.">Flexible, long-lived, large-area, organic solar cells.</a> Solar Energy Materials and Solar Cells. 91, 379-384 (2007).</li><li>Lu, Y., 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=Thin-Film+Deposition+of+an+Organic+Magnet+Based+on+Vanadium+Methyl+Tricyanoethylenecarboxylate.">Thin-Film Deposition of an Organic Magnet Based on Vanadium Methyl Tricyanoethylenecarboxylate.</a> Adv. Mater. 26, 7632-7636 (2014).</li></ol>

作者什么都没有透露。

关键参数中V [TCNE]×〜2沉积包括温度，载气流量，压力，和前体的比例。因为化学气相沉积设置不是市售这些参数将需要为每一个系统进行优化。先前的研究由麻等人透露，温度对TCNE前体26的升华速率的影响最大。温度可通过在温度控制器和还通过调整在加热线圈和作为这样的丝间距将需要校准每个系统中设置的值进行修改两者。温度的校准是通过测量反应器内之前?...

有机基铁氧体磁性半导体钒四氰（Ⅴ[TCNE]，则x〜2）表现出室温磁有序和承诺的磁电子应用，如柔软性，低成本的生产，和化学可调谐性的有机材料的优点。以前的研究已经证明，在自旋电子器件，包括杂化有机/无机1,2-和全有机自旋阀3的功能，和作为活性有机/无机半导体异质结构4自旋偏振器。此外，V [TCNE]×〜2展示了承诺列入高频电子产品，由于其极窄的铁磁共振行距5。 有已建立的合成V [TCNE]×〜2月 6日至九日四种不同的方法。 V [TCNE]×〜2首次合成powde经由TCNE和V的反应中的R二氯甲烷（C 6 H 6）6。这些粉末表现出在有机系材料中观察到的第一个室温磁有序。然而，这种材料的粉末形式是极其空气敏感，限制了其在薄膜器件的应用。在2000年，化学气相沉积（CVD）方法建立用于创建V [TCNE]×〜2薄膜7。更多最近的物理气相沉积（PVD）8和分子层沉积（MLD）9也已用于制造薄膜。 PVD法需要超高真空（UHV）系统和两者PVD和MLD方法需要极长的时间来生长膜厚度大于100纳米，而在CVD膜可以很容易地在厚度范围从30纳米到几微米沉积。除了各种可用与CVD法厚度，广泛的研究已经取得了优化的薄膜即一直显示高Quality磁特性包括：窄铁磁共振（FMR）线宽（1.5克），高的居里温度（600 K）和尖锐的磁开关5。 以V [TCNE]×〜2薄膜磁有序通过非常规途径进行。 SQUID磁力测量显示强大的本地磁有序，但由于没有X射线衍射峰和特征的透射型电子显微镜（TEM）10形态揭示缺乏长程结构秩序。然而，扩展X射线吸收精细结构（EXAFS）研究11表明每个钒离子八面体配位与六个不同TCNE分子，表明与2.084（5）埃的钒-氮键长度的稳定的局部结构秩序。磁性源于TCNE的未配对自旋之间的反铁磁性交换耦合-基阴离子，它们分布在整个TCNE -分子，并且在V 2+离子的自旋，导致本地铁磁有序与T C 〜600 K中优化膜5。除了 ​​表现出室温磁有序，V [TCNE]×〜2薄膜半导体为0.5 EV带隙12。值得注意的其他性能包括低于〜150开13,14，反常正磁阻12,15,16，和光诱导磁13,17,18的冷冻温度可能sperimagnetism。 CVD法合成V [TCNE]×〜2薄膜与各种基质的相容因低温（&lt;60℃）和保形沉积。以前的研究显示了V [TCNE]×〜2成功沉积在刚性和柔性基板7。此外，该沉积技术适合于调谐通过前体和改性克owth参数19-22虽然此处所示的协议产生最优化的膜迄今为止，显著进展已取得，因为这种方法的发现改善的一些膜的性质和进一步的增益是可能的。

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td>Equipment</td>
		</tr>
		<tr>
			<td>Nitrogen Glovebox</td>
			<td>Vacuum Atmospheres</td>
			<td>Omni</td>
			<td>steps done in nitrogen glovebox can also be done in an argon glovebox</td>
		</tr>
		<tr>
			<td>1 L three-neck round bottom flask</td>
			<td>Corning</td>
			<td>4965A-1L</td>
			<td></td>
		</tr>
		<tr>
			<td>500 mL round bottom flask</td>
			<td>Sigma Aldrich</td>
			<td>64678</td>
			<td></td>
		</tr>
		<tr>
			<td>Turbo vacuum pumping station</td>
			<td>Agilent Varian</td>
			<td>G8701A-011-037</td>
			<td></td>
		</tr>
		<tr>
			<td>Glass Stopcock</td>
			<td>Kontes</td>
			<td>185000-2440</td>
			<td></td>
		</tr>
		<tr>
			<td>Glass two way connecting tube</td>
			<td>Corning</td>
			<td>8940-24</td>
			<td>Corning Pyrex(R) 105 degree Angled Tube Adapter with Two-Way 24/40 Standard Taper Joint</td>
		</tr>
		<tr>
			<td>Coldfinger</td>
			<td></td>
			<td></td>
			<td>Custom part made by OSU chemistry glass shop</td>
		</tr>
		<tr>
			<td>Argon Glovebox</td>
			<td>Vacuum Atmospheres</td>
			<td>Nexus I</td>
			<td></td>
		</tr>
		<tr>
			<td>Hot plate stirrer</td>
			<td>Corning</td>
			<td>6795</td>
			<td></td>
		</tr>
		<tr>
			<td>Thermoeletric cooler</td>
			<td>Advanced Thermoelectric</td>
			<td>TCP-50</td>
			<td></td>
		</tr>
		<tr>
			<td>Temperature controller</td>
			<td>Advanced Thermoelectric</td>
			<td>TLZ10</td>
			<td>for TE cooler</td>
		</tr>
		<tr>
			<td>Power supply</td>
			<td>Advanced Thermoelectric</td>
			<td>PS-145W-12V&#160;</td>
			<td>for TE cooler and temperature controller</td>
		</tr>
		<tr>
			<td>Temperature controller</td>
			<td>J-Kem&#160; Scientific</td>
			<td>Model 150</td>
			<td>For heating coil</td>
		</tr>
		<tr>
			<td>Heating wire</td>
			<td>Pelican Wire Company</td>
			<td>Nichrome 60</td>
			<td></td>
		</tr>
		<tr>
			<td>Custom glassware pieces</td>
			<td></td>
			<td></td>
			<td>Made by OSU Chemistry glass shop</td>
		</tr>
		<tr>
			<td>Vacuum pump</td>
			<td>BOC Edwards</td>
			<td>XDS-5</td>
			<td>Connected to the CVD set-up</td>
		</tr>
		<tr>
			<td>Flow meter</td>
			<td>Gilmont</td>
			<td>GF-2260</td>
			<td></td>
		</tr>
		<tr>
			<td>Micrometer valve</td>
			<td>Gilmont</td>
			<td>7300</td>
			<td>Controls flow of argon over TCNE</td>
		</tr>
		<tr>
			<td>Micrometer valve</td>
			<td>Gilmont</td>
			<td>7100</td>
			<td>Controls flow of argon over&#160; V(CO)6</td>
		</tr>
		<tr>
			<td>Tubing</td>
			<td>Tygon</td>
			<td>R3603</td>
			<td>1/8 in walls, connected between valves and meter</td>
		</tr>
		<tr>
			<td>3-way Stopcock</td>
			<td>Nalgene</td>
			<td>6470</td>
			<td>used to adjust the flow rates</td>
		</tr>
		<tr>
			<td>Pressure gauge</td>
			<td>Matheson</td>
			<td>63-4105</td>
			<td>connects to the top of Figure 1 part A</td>
		</tr>
		<tr>
			<td>SQUID magnetometer</td>
			<td>Quantum Design</td>
			<td>MPMS-XL</td>
			<td></td>
		</tr>
		<tr>
			<td>EPR</td>
			<td>Bruker</td>
			<td>Elexsys</td>
			<td></td>
		</tr>
		<tr>
			<td>PPMS</td>
			<td>Quantum Design</td>
			<td>14T PPMS</td>
			<td></td>
		</tr>
		<tr>
			<td>Sourcemeter</td>
			<td>Keithely&#160;</td>
			<td>2400</td>
			<td></td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td>Materials</td>
		</tr>
		<tr>
			<td>Sodium metal</td>
			<td>Sigma Aldrich</td>
			<td>262714</td>
			<td></td>
		</tr>
		<tr>
			<td>Anthracene</td>
			<td>Sigma Aldrich</td>
			<td>141062</td>
			<td></td>
		</tr>
		<tr>
			<td>Anhydrous tetrahydrofuran</td>
			<td>Sigma Aldrich</td>
			<td>186562</td>
			<td></td>
		</tr>
		<tr>
			<td>Vanadium(III) chloride tetrahydrofuran complex</td>
			<td>Sigma Aldrich</td>
			<td>395382</td>
			<td></td>
		</tr>
		<tr>
			<td>Carbon monoxide gas</td>
			<td>OSU stores</td>
			<td>98610</td>
			<td></td>
		</tr>
		<tr>
			<td>Tetraethylammonium bromide</td>
			<td>Sigma Aldrich</td>
			<td>241059</td>
			<td></td>
		</tr>
		<tr>
			<td>Phosphoric acid</td>
			<td>Sigma Aldrich</td>
			<td>79622</td>
			<td></td>
		</tr>
		<tr>
			<td>Methanol</td>
			<td>Sigma Aldrich</td>
			<td>14262</td>
			<td></td>
		</tr>
		<tr>
			<td>Silcone oil</td>
			<td>Sigma Aldrich</td>
			<td>146153</td>
			<td></td>
		</tr>
		<tr>
			<td>Copper pellets</td>
			<td></td>
			<td></td>
			<td>Cut from spare copper wire</td>
		</tr>
		<tr>
			<td>Tetracyanoethylene</td>
			<td>Sigma Aldrich</td>
			<td>T8809</td>
			<td></td>
		</tr>
		<tr>
			<td>Glass slides</td>
			<td>Gold Seal</td>
			<td>3010</td>
			<td></td>
		</tr>
		<tr>
			<td>Activated Charcoal</td>
			<td>Sigma Aldrich</td>
			<td>242276</td>
			<td></td>
		</tr>
	</tbody>
</table>

chemical vapor deposition of an organic magnet, vanadium tetracyanoethylene

在有机材料领域中的最新进展已经产生了器件如有机发光二极管（OLED），其具有传统的材料，包括低成本和机械柔韧性没有发现的优点。与此类似，这将是有利的，以扩大利用有机物成高频电子器件和基于自旋的电子器件。这项工作提出的合成方法，薄膜的室温有机亚铁磁的生长，钒四氰（Ⅴ[TCNE]，则x〜2）通过低温化学气相沉积（CVD）。薄膜生长在&lt;60℃下，可容纳各种基材，包括但不限于，硅，玻璃，聚四氟乙烯和柔性基板。的保形沉积，有利于预图案化和三维结构为好。另外，该技术可以得到具有厚度范围从30纳米到几微米的薄膜。最新进展在膜生长的优化产生的膜的品质，如更高的居里温度（600 K），改进的磁性均匀性和窄铁磁谐振线路宽度为各种在自旋电子学和微波电子应用（1.5 g）示出的承诺。

第一和最容易的方法，用于确定一个沉积是成功的是做膜的目视检查。这部电影应该会出现暗紫色采用了镜面设计是整个基板均匀。如果在衬底的表面上的斑点，其中有否v [TCNE]×〜2，或者它是在颜色较浅，则这可能是由于溶剂或其它杂质的衬底表面上的存在。此外，该电影应该是不透明的。除非薄膜沉积在只有几分钟的短时间内，半透明膜往往意味着有可能已被与前体的沉积期间...

Watch this Scientific Journal Video about Chemical Vapor Deposition of an Organic Magnet, Vanadium Tetracyanoethylene at JoVE.com

Chemical Vapor Deposition of an Organic Magnet, Vanadium Tetracyanoethylene

我们提出的基于有机物的亚铁磁钒四氰的合成（Ⅴ[TCNE]，则x〜2）通过低温化学气相沉积（CVD）。这种优化配方产生增加居里温度从400 K至600 K和磁共振性能的显着改善。

化学气相沉积的有机磁体，钒四氰

Recent progress in the field of organic materials has yielded devices such as organic light emitting diodes (OLEDs) which have advantages not found in ...

chemical-vapor-deposition-an-organic-magnet-vanadium

Research

JoVE Journal

Chemistry

11.4K 次观看.  The Ohio State University. 我们提出的基于有机物的亚铁磁钒四氰的合成（Ⅴ[TCNE]，则x〜2）通过低温化学气相沉积（CVD）。这种优化配方产生增加居里温度从400 K至600 K和磁共振性能的显着改善。 

视频: Chemical Vapor Deposition of an Organic Magnet, Vanadium Tetracyanoethylene

Preparation of Hydrophobic Metal-Organic Frameworks via Plasma Enhanced Chemical Vapor Deposition of Perfluoroalkanes for the Removal of Ammonia

Plasma enhanced chemical vapor deposition (PECVD) of perfluoroalkanes has long been studied for tuning the wetting properties of surfaces. For high surface area microporous materials, such as metal-organic frameworks (MOFs), unique challenges present themselves for PECVD treatments. Herein the protocol for development of a MOF that was previously unstable to humid conditions is presented. The protocol describes the synthesis of Cu-BTC (also known as HKUST-1), the treatment of Cu-BTC with PECVD of perfluoroalkanes, the aging of materials under humid conditions, and the subsequent ammonia microbreakthrough experiments on milligram quantities of microporous materials. Cu-BTC has an extremely high surface area (~1,800 m2/g) when compared to most materials or surfaces that have been previously treated by PECVD methods. Parameters such as chamber pressure and treatment time are extremely important to ensure the perfluoroalkane plasma penetrates to and reacts with the inner MOF surfaces. Furthermore, the protocol for ammonia microbreakthrough experiments set forth here can be utilized for a variety of test gases and microporous materials.

Herein the procedures for plasma enhanced chemical vapor deposition of perfluoroalkanes on microporous materials such as metal-organic frameworks to enhance their stability and hydrophobicity are described. Furthermore, breakthrough testing of milligram quantities of samples is described in detail.

增强型氟烷烃的化学气相沉积等离子通过疏水金属 - 有机骨架的制备氨的去除

Plasma enhanced chemical vapor deposition (PECVD) of perfluoroalkanes has long been studied for tuning the wetting properties of surfaces. For high ...

科研

化学

High-pressure Sapphire Cell for Phase Equilibria Measurements of CO2/Organic/Water Systems

The high pressure sapphire cell apparatus was constructed to visually determine the composition of multiphase systems without physical sampling. Specifically, the sapphire cell enables visual data collection from multiple loadings to solve a set of material balances to precisely determine phase composition. Ternary phase diagrams can then be established to determine the proportion of each component in each phase at a given condition. In principle, any ternary system can be studied although ternary systems (gas-liquid-liquid) are the specific examples discussed herein. For instance, the ternary THF-Water-CO2 system was studied at 25 and 40&#160;&#176;C and is described herein. Of key importance, this technique does not require sampling. Circumventing the possible disturbance of the system equilibrium upon sampling, inherent measurement errors, and technical difficulties of physically sampling under pressure is a significant benefit of this technique. Perhaps as important, the sapphire cell also enables the direct visual observation of the phase behavior. In fact, as the CO2 pressure is increased, the homogeneous THF-Water solution phase splits at about 2 MPa. With this technique, it was possible to easily and clearly observe the cloud point and determine the composition of the newly formed phases as a function of pressure.
The data acquired with the sapphire cell technique can be used for many applications. In our case, we measured swelling and composition for tunable solvents, like gas-expanded liquids, gas-expanded ionic liquids and Organic Aqueous Tunable Systems (OATS)1-4. For the latest system, OATS, the high-pressure sapphire cell enabled the study of (1) phase behavior as a function of pressure and temperature, (2) composition of each phase (gas-liquid-liquid) as a function of pressure and temperature and (3) catalyst partitioning in the two liquid phases as a function of pressure and composition. Finally, the sapphire cell is an especially effective tool to gather accurate and reproducible measurements in a timely fashion.

High-pressure Sapphire Cell for Phase Equilibria Measurements of CO2/Organic/Water Systems

The high pressure sapphire cell apparatus is a unique tool to study, without sampling, phase behavior under a wide range of pressures. Using a cathetometer, very precise volume measurements can be recorded to measure liquid expansion and phase composition. Thus, this synthetic method enables the study of (1) phase equilibria of multi-component mixtures and (2) the partition behavior of catalyst or model compounds as a function of pressure.

高压蓝宝石细胞对CO的相平衡测量<sub&gt; 2</sub&gt; /有机/水系统

The high pressure sapphire cell apparatus was constructed to visually determine the composition of multiphase systems without physical sampling. ...

Analysis of Volatile and Oxidation Sensitive Compounds Using a Cold Inlet System and Electron Impact Mass Spectrometry

This video presents a protocol for the mass spectrometrical analysis of volatile and oxidation sensitive compounds using electron impact ionization. The analysis of volatile and oxidation sensitive compounds by mass spectrometry is not easily achieved, as all state-of-the-art mass spectrometric methods require at least one sample preparation step, e.g., dissolution and dilution of the analyte (electrospray ionization), co-crystallization of the analyte with a matrix compound (matrix-assisted laser desorption/ionization), or transfer of the prepared samples into the ionization source of the mass spectrometer, to be conducted under atmospheric conditions. Here, the use of a sample inlet system is described which enables the analysis of volatile metal organyls, silanes, and phosphanes using a sector field mass spectrometer equipped with an electron impact ionization source. All sample preparation steps and the sample introduction into the ion source of the mass spectrometer take place either under air-free conditions or under vacuum, enabling the analysis of compounds highly susceptible to oxidation. The presented technique is especially of interest for inorganic chemists, working with metal organyls, silanes, or phosphanes, which have to be handled using inert conditions, such as the Schlenk technique. The principle of operation is presented in this video.

This video presents a protocol for the mass spectrometrical analysis of volatile and oxidation sensitive compounds using electron impact ionization. The presented technique is especially of interest for inorganic chemists, working with metal organyls, silanes, or phosphanes which have to be handled using inert conditions, such as the Schlenk technique.

挥发和氧化敏感的化合物使用冷进气系统和电子轰击质谱分析

This video presents a protocol for the mass spectrometrical analysis of volatile and oxidation sensitive compounds using electron impact ionization. The ...

Preparation of Macroporous Epitaxial Quartz Films on Silicon by Chemical Solution Deposition

This work describes the detailed protocol for preparing piezoelectric macroporous epitaxial quartz films on silicon(100) substrates. This is a three-step process based on the preparation of a sol in a one-pot synthesis which is followed by the deposition of a gel film on Si(100) substrates by evaporation induced self-assembly using the dip-coating technique and ends with a thermal treatment of the material to induce the gel crystallization and the growth of the quartz film. The formation of a silica gel is based on the reaction of a tetraethyl orthosilicate and water, catalyzed by HCl, in ethanol. However, the solution contains two additional components that are essential for preparing mesoporous epitaxial quartz films from these silica gels dip-coated on Si. Alkaline earth ions, like Sr2+ act as glass melting agents that facilitate the crystallization of silica and in combination with cetyl trimethylammonium bromide (CTAB) amphiphilic template form a phase separation responsible of the macroporosity of the films. The good matching between the quartz and silicon cell parameters is also essential in the stabilization of quartz over other SiO2 polymorphs and is at the origin of the epitaxial growth.

A protocol is presented for the preparation of piezoelectric macroporous epitaxial films of quartz on silicon by solution chemistry using dip-coating and thermal treatments in air.

化学溶液沉积在硅外延大孔石英薄膜的制备

This work describes the detailed protocol for preparing piezoelectric macroporous epitaxial quartz films on silicon(100) substrates. This is a three-step ...

Synthesis and Characterization of Supramolecular Colloids

Control over colloidal assembly is of utmost importance for the development of functional colloidal materials with tailored structural and mechanical properties for applications in photonics, drug delivery and coating technology. Here we present a new family of colloidal building blocks, coined supramolecular colloids, whose self-assembly is controlled through surface-functionalization with a benzene-1,3,5-tricarboxamide (BTA) derived supramolecular moiety. Such BTAs interact via directional, strong, yet reversible hydrogen-bonds with other identical BTAs. Herein, a protocol is presented that describes how to couple these BTAs to colloids and how to quantify the number of coupling sites, which determines the multivalency of the supramolecular colloids. Light scattering measurements show that the refractive index of the colloids is almost matched with that of the solvent, which strongly reduces the van der Waals forces between the colloids. Before photo-activation, the colloids remain well dispersed, as the BTAs are equipped with a photo-labile group that blocks the formation of hydrogen-bonds. Controlled deprotection with UV-light activates the short-range hydrogen-bonds between the BTAs, which triggers the colloidal self-assembly. The evolution from the dispersed state to the clustered state is monitored by confocal microscopy. These results are further quantified by image analysis with simple routines using ImageJ and Matlab. This merger of supramolecular chemistry and colloidal science offers a direct route towards light- and thermo-responsive colloidal assembly encoded in the surface-grafted monolayer.

A protocol for the synthesis and characterization of colloids coated with supramolecular moieties is described. These supramolecular colloids undergo self-assembly upon the activation of the hydrogen-bonds between the surface-anchored molecules by UV-light.

超分子胶体的合成与表征

Control over colloidal assembly is of utmost importance for the development of functional colloidal materials with tailored structural and mechanical ...

Epitaxial Growth of Perovskite Strontium Titanate on Germanium via Atomic Layer Deposition

Atomic layer deposition (ALD) is a commercially utilized deposition method for electronic materials. ALD growth of thin films offers thickness control and conformality by taking advantage of self-limiting reactions between vapor-phase precursors and the growing film. Perovskite oxides present potential for next-generation electronic materials, but to-date have mostly been deposited by physical methods. This work outlines a method for depositing SrTiO3 (STO) on germanium using ALD. Germanium has higher carrier mobilities than silicon and therefore offers an alternative semiconductor material with faster device operation. This method takes advantage of the instability of germanium's native oxide by using thermal deoxidation to clean and reconstruct the Ge (001) surface to the 2&#215;1 structure. 2-nm thick, amorphous STO is then deposited by ALD. The STO film is annealed under ultra-high vacuum and crystallizes on the reconstructed Ge surface. Reflection high-energy electron diffraction (RHEED) is used during this annealing step to monitor the STO crystallization. The thin, crystalline layer of STO acts as a template for subsequent growth of STO that is crystalline as-grown, as confirmed by RHEED. In situ X-ray photoelectron spectroscopy is used to verify film stoichiometry before and after the annealing step, as well as after subsequent STO growth. This procedure provides framework for additional perovskite oxides to be deposited on semiconductors via chemical methods in addition to the integration of more sophisticated heterostructures already achievable by physical methods.

This work details the procedures for the growth and characterization of crystalline SrTiO3 directly on germanium substrates by atomic layer deposition. The procedure illustrates the ability of an all-chemical growth method to integrate oxides monolithically onto semiconductors for metal-oxide semiconductor devices.

锗通过原子层沉积钙钛矿型钛酸锶的外延生长

Atomic layer deposition (ALD) is a commercially utilized deposition method for electronic materials. ALD growth of thin films offers thickness control and ...

Fizzy Extraction of Volatile Organic Compounds Combined with Atmospheric Pressure Chemical Ionization Quadrupole Mass Spectrometry

Chemical analysis of volatile and semivolatile compounds dissolved in liquid samples can be challenging. The dissolved components need to be brought to the gas phase, and efficiently transferred to a detection system. Fizzy extraction takes advantage of the effervescence phenomenon. First, a carrier gas (here, carbon dioxide) is dissolved in the sample by applying overpressure and stirring the sample. Second, the sample chamber is decompressed abruptly. Decompression leads to the formation of numerous carrier gas bubbles in the sample liquid. These bubbles assist the release of the dissolved analyte species from the liquid to the gas phase. The released analytes are immediately transferred to the atmospheric pressure chemical ionization interface of a triple quadrupole mass spectrometer. The ionizable analyte species give rise to mass spectrometric signals in the time domain. Because the release of the analyte species occurs over short periods of time (a few seconds), the temporal signals have high amplitudes and high signal-to-noise ratios. The amplitudes and areas of the temporal peaks can then be correlated with concentrations of the analytes in the liquid samples subjected to fizzy extraction, which enables quantitative analysis. The advantages of fizzy extraction include: simplicity, speed, and limited use of chemicals (solvents).

Fizzy extraction is a new laboratory technique for analysis of volatile and semivolatile compounds. A carrier gas is dissolved in the liquid sample by applying overpressure and stirring the sample. The sample chamber is then decompressed. The analyte species are liberated to the gas phase due to effervescence.

挥发性有机化合物与大气压化学电离四极杆质谱联用

Chemical analysis of volatile and semivolatile compounds dissolved in liquid samples can be challenging. The dissolved components need to be brought to ...

Aerosol-assisted Chemical Vapor Deposition of Metal Oxide Structures: Zinc Oxide Rods

Whilst columnar zinc oxide (ZnO) structures in the form of rods or wires have been synthesized previously by different liquid- or vapor-phase routes, their high cost production and/or incompatibility with microfabrication technologies, due to the use of pre-deposited catalyst-seeds and/or high processing temperatures exceeding 900 &#176;C, represent a drawback for a widespread use of these methods. Here, however, we report the synthesis of ZnO rods via a non-catalyzed vapor-solid mechanism enabled by using an aerosol-assisted chemical vapor deposition (CVD) method at 400 &#176;C with zinc chloride (ZnCl2) as the precursor and ethanol as the carrier solvent. This method provides both single-step formation of ZnO rods and the possibility of their direct integration with various substrate types, including silicon, silicon-based micromachined platforms, quartz, or high heat resistant polymers. This potentially facilitates the use of this method at a large-scale, due to its compatibility with state-of-the-art microfabrication processes for device manufacture. This report also describes the properties of these structures (e.g., morphology, crystalline phase, optical band gap, chemical composition, electrical resistance) and validates its gas sensing functionality towards carbon monoxide.

Columnar zinc oxide structures in the form of rods are synthesized via aerosol-assisted chemical vapor deposition without the use of pre-deposited catalyst-seed particles. This method is scalable and compatible with various substrates based on either silicon, quartz or polymers.

金属氧化物结构的气溶胶辅助化学气相沉积: 氧化锌棒

Whilst columnar zinc oxide (ZnO) structures in the form of rods or wires have been synthesized previously by different liquid- or vapor-phase routes, ...

Controlled Photoredox Ring-Opening Polymerization of O-Carboxyanhydrides Mediated by Ni/Zn Complexes

Here, we describe an effective protocol that combines photoredox Ni/Ir catalysis with the use of a Zn-alkoxide for efficient ring-opening polymerization, allowing for the synthesis of isotactic poly(&#945;-hydroxy acids) with expected molecular weights (&#62;140 kDa) and narrow molecular weight distributions (Mw/Mn &#60; 1.1). This ring-opening polymerization is mediated by Ni and Zn complexes in the presence of an alcohol initiator and a photoredox Ir catalyst, irradiated by a blue LED (400 - 500 nm). The polymerization is performed at a low temperature (-15 &#176;C) to avoid undesired side reactions. The complete monomer consumption can be achieved within 4 - 8 hours, providing a polymer close to the expected molecular weight with narrow molecular weight distribution. The resulted number-average molecular weight shows a linear correlation with the degree of polymerization up to 1000. The homodecoupling 1H NMR study confirms that the obtained polymer is isotactic without epimerization. This polymerization reported herein offers a strategy for achieving rapid, controlled O-carboxyanhydrides polymerization to prepare stereoregular poly(&#945;-hydroxy acids) and its copolymers bearing various functional side-chain groups.

Controlled Photoredox Ring-Opening Polymerization of O-Carboxyanhydrides Mediated by Ni/Zn Complexes

A protocol for the controlled photoredox ring-opening polymerization of O-carboxyanhydrides mediated by Ni/Zn complexes is presented.

镍/锌配合物介导的O-Carboxyanhydrides 的控制 Photoredox 环开聚合

Here, we describe an effective protocol that combines photoredox Ni/Ir catalysis with the use of a Zn-alkoxide for efficient ring-opening polymerization, ...

Reactive Vapor Deposition of Conjugated Polymer Films on Arbitrary Substrates

We demonstrate a method of conformally coating conjugated polymers on arbitrary substrates using a custom-designed, low-pressure reaction chamber. Conductive polymers, poly(3,4-ethylenedioxythiophene) (PEDOT) and poly(3,4-propylenedioxythiophene) (PProDOT), and a semiconducting polymer, poly(thieno[3,2-b]thiophene) (PTT), were deposited on unconventional highly-disordered and textured substrates with high surface areas, such as paper, towels and fabrics. This reported deposition chamber is an improvement of previous vapor reactors because our system can accommodate both volatile and nonvolatile monomers, such as 3,4-propylenedioxythiophene and thieno[3,2-b]thiophene. Utilization of both solid and liquid oxidants are also demonstrated. One limitation of this method is that it lacks sophisticated in situ thickness monitors. Polymer coatings made by the commonly used solution-based coating methods, such as spin-coating and surface grafting, are often not uniform or susceptible to mechanical degradation. This reported vapor phase deposition method overcomes those drawbacks and is a strong alternative to common solution-based coating methods. Notably, polymer films coated by the reported method are uniform and conformal on rough surfaces, even at a micrometer scale. This feature allows for future application of vapor deposited polymers in electronics devices on flexible and highly textured substrates.

This paper presents a protocol for reactive vapor deposition of poly(3,4-ethylenedioxythiophene), poly(3,4-propylenedioxythiophene), and poly(thieno[3,2-b]thiophene) films on glass slides and rough substrates, such as textiles and paper.