根据合同DE-AC52-07NA27344美国能源署的主持下进行的由劳伦斯·利弗莫尔国家实验室的这项工作。

1.溶液的制备<ol><li>滤波器60乳酸乙酯的使用注射器和一个0.20微米的注射器过滤器。添加0.3克聚乙烯醇缩甲醛的乳酸乙酯。放置在50℃下将溶液放入烘箱4小时。摇动小瓶轻轻以查看是否在聚合物完全溶解。 <ol><li>如果溶液混浊或仍显示光的不均匀性，返回小瓶烘箱另外2小时。此配方是为0.5重量％的聚合物溶液，其典型地用于膜厚大约30毫微米。与较高的聚合物的重量含量的解决方案可以用于较厚的膜。 </li></ol></li><li>通过称量1.0克PDAC试剂在20ml的容量瓶中，并填充所述烧瓶用去离子（DI）水的测量线准备一个PDAC溶液。将其转移到贮藏容器之前轻轻摇动溶液中。 </li></ol> 2.基板制备<ol><li>小心。倒入60毫升浓硫酸的酸到一个干净的250毫升烧杯中。慢慢加入20毫升30％的过氧化氢。等到发烟补贴，然后摇动轻轻的解决方案。溶液中，将烧杯会变得非常热，该混合物是具有腐蚀性。 </li><li>将150毫米的培养皿上的热点板块，倒入酸入菜。设置加热板为100℃。 <ol><li>放置4&#39;的硅晶片与该抛光面朝上的酸。轻轻晶片向下推，中间有一对镊子的，以确保整个表面都被浸湿。留在酸晶片30分钟。 </li></ol></li><li>除去从酸晶片有一对镊子和冲洗的正面和背面的晶片的彻底用DI水从喷瓶。水应该片断以规则图案。干洁净工作台的晶片。 </li><li>冲洗一次性3毫升注射器和一个0.2微米的过滤器首先用DI水，然后用PDAC溶液由液体抽入注射器，在安装过滤器，并且Ñ​​推动液体通过过滤器。 </li><li>安装在旋涂机在清洁的晶片。制定1.0-1.2毫升PDAC溶液到注射器和分配它虽然过滤到晶片的中间。旋在4,000rpm下15秒，然后将晶片传送到一个​​热板（预热至50℃）并让它坐30秒。 </li><li>用去离子水冲洗干PDAC层关闭，让晶圆干燥洁净工作台。 </li></ol> 3.电影制作<ol><li>放置干燥PDAC处理晶片上旋涂机。 </li><li>冲洗一次性3毫升注射器和0.45微米的过滤器，使用下2.4的程序的乳酸乙酯溶液）。 </li><li>存款2.5毫升以200rpm通过过滤器的乳酸乙酯溶液用注射器在晶片和自旋的中间为10秒，然后，持续3秒在1700转（取决于所需的膜厚度）。应在晶片上均匀的液体膜。 </li><li>让该膜干燥，在旋涂机直到它明显地干燥（通常10-15分钟），然后将其放置在热板上（预热至50℃）10分钟。 </li><li>切块的薄膜成更小的最小二乘剥离，一般为2厘米×2厘米，但可以更大，这取决于所用片夹（3.5.1-3.5.2）的大小。另外，做两个文士的分层晶圆尺寸薄膜（3.5.3）。 注:标准片夹是19×19毫米，在中间的圆形开口的直径为13毫米。对于晶片尺寸薄膜，使用钢丝箍（形成为圆例如 ，不锈钢丝），其直径为1"比晶片小。圆形开口被选中，是因为离地升空和膨胀在影片通常会吸收水分。作为薄膜干燥支架上时，水被除去，薄膜将收缩。圆形开口允许均匀分布的压力。 <ol><li>放置在一切割模板的晶片。使用方形模板上的所有边缘比晶片更高防止直êDGE用于从接触晶圆刻划期间指导刀片。标记2厘米的间距的边缘，以引导放置在直刃的切割时。推动晶圆对两名边对齐。 </li><li>放置一个直边沿两个对准标记，并轻轻划刀片沿直刃刻划膜。施加足够的压力，以纪念这部电影，但不要太多，以纪念该晶片本身并产生颗粒。上较厚的膜，切割线将清晰可见。 </li><li>到剥离的膜在从晶片一片，隶用刀片晶片边缘。在晶片上的两个单位之间，隶带足够宽到晶片夹紧在齿条和小齿轮。 </li></ol></li><li>填写一个190×100毫米的培养皿用去离子水。晶片由大平板夹紧到齿条和小齿轮安装到倾斜阶段和缓慢向下放入DI水。这部电影应该分开晶圆在水位线。 <ol><li>继续降低WAF尔的速率，使该膜足够的时间来从晶片中分离出来，而不是推水线下的剥离界面。当方块的第一行已经与晶片分离并漂浮在表面上，暂停晶片的降低。对于一个晶片大小的膜，继续浸渍晶片直到薄膜分离完全。 </li><li>浸入片夹的头部入水和移动它的膜之下。排队的薄膜边缘之一箍的手柄的边缘，并与薄膜触摸箍。如果成功的话，这部电影会坚持到篮下。 <ol><li>对于一个晶片大小的膜，放置在刻划部下方的电线圈，只是一厘米远离边缘。确保箍是围绕膜之下开始捕捉，保持膜边缘与箍边缘之间有一定距离，使得薄膜缠绕箍和向后翻转折迭之前。 </li></ol></li><li>从水中拉回圈缓慢的的35°角。提起电影出来的水非常缓慢。 注意:对于薄膜小于20nm厚，增加角度后大约一半的膜一直拉到从水到几乎90°（ 即 ，垂直于水面），以避免通过支架拉膜。当改变电梯出角度，这样做的慢，以避免通过箍揪片子。 </li><li>当箍完全缩回，将其放置到一边干燥。确保箍的底部是免费滴把箍下来之前，并使用曲面（如晶圆托盘），以避免造成箍和表面之间的液体密封。 </li><li>如果更多的划线正方形留在晶片上，继续降低晶片放入水中，并重复步骤3.6.1-3.6.4上述剩余正方形。 </li><li>让薄膜干燥O / N。 </li></ol></li></ol>

<ol>
	<li>Cheng, W., Campolongo, M. J., Tan, S. J., Luo, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Freestanding+ultrathin+nano-membranes+via+self-assembly.">Freestanding ultrathin nano-membranes via self-assembly.</a> Nano Today. 4, 482-493 (2009).</li><li>Greco, F., 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-thin+conductive+free-standing+PEDOT/PSS+nanofilms.">Ultra-thin conductive free-standing PEDOT/PSS nanofilms.</a> Soft Matter. 7, 10642-10650 (2011).</li><li>Matsui, J., Mitsuishi, M., Aoki, A., Miyashita, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Molecular+Optical+Gating+Devices+Based+on+Polymer+Nanosheets+Assemblies.">Molecular Optical Gating Devices Based on Polymer Nanosheets Assemblies.</a> J. Am. Chem. Soc. 126, 3708-3709 (2004).</li><li>Ulbricht, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Advanced+functional+polymer+membranes.">Advanced functional polymer membranes.</a> Polymer. 47, 2217-2262 (2006).</li><li>Fujie, T., 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=Robust+Polysaccharide+Nanosheets+Integrated+for+Tissue-Defect+Repair.">Robust Polysaccharide Nanosheets Integrated for Tissue-Defect Repair.</a> Adv. Funct. Mater. 19, 2560-2568 (2009).</li><li>Okamura, Y., Kabata, K., Kinoshita, M., Saitoh, D., Takeoka, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Free-Standing+Biodegradable+Poly(lactic+acid)+Nanosheet+for+Sealing+Operations+in+Surgery.">Free-Standing Biodegradable Poly(lactic acid) Nanosheet for Sealing Operations in Surgery.</a> Adv. Mater. 21, 4388-4392 (2009).</li><li>Sreenivasan, R., Bassett, E. K., Hoganson, D. M., Vacanti, J. P., Gleason, K. K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ultra-thin+gas+permeable+free-standing+and+composite+membranes+for+microfluidic+lung+assist+devices.">Ultra-thin gas permeable free-standing and composite membranes for microfluidic lung assist devices.</a> Biomaterials. 32, 3883-3889 (2011).</li><li>Wan, L. -. S., Liu, Z. -. M., Xu, Z. -. K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Surface+engineering+of+macroporous+polypropylene+membranes.">Surface engineering of macroporous polypropylene membranes.</a> Soft Matter. 5, 1775-1785 (2009).</li><li>Alcoutlabi, M., McKenna, G. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effects+of+confinement+on+material+behaviour+at+the+nanometre+size+scale.">Effects of confinement on material behaviour at the nanometre size scale.</a> Journal of Physics-Condensed Matter. 17, R461-R524 (2005).</li><li>Ellison, C. J., Torkelson, J. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+distribution+of+glass-transition+temperatures+in+nanoscopically+confined+glass+formers.">The distribution of glass-transition temperatures in nanoscopically confined glass formers.</a> Nature Materials. 2, 695-700 (2003).</li><li>Priestley, R. D., Ellison, C. J., Broadbelt, L. J., Torkelson, J. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Structural+relaxation+of+polymer+glasses+at+surfaces,+interfaces+and+in+between.">Structural relaxation of polymer glasses at surfaces, interfaces and in between.</a> Science. 309, 456-459 (2005).</li><li>Si, L., Massa, M. V., Dalnoki-Veress, K., Brown, H. R., Jones, R. A. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Chain+entanglement+in+thin+freestanding+polymer+films.">Chain entanglement in thin freestanding polymer films.</a> Phys. Rev. Lett. 94, (2005).</li><li>Torres, J. M., Stafford, C. M., Vogt, B. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Elastic+Modulus+of+Amorphous+Polymer+Thin+Films:+Relationship+to+the+Glass+Transition+Temperature.">Elastic Modulus of Amorphous Polymer Thin Films: Relationship to the Glass Transition Temperature.</a> Acs Nano. 3, 2677-2685 (2009).</li><li>Baxamusa, S. 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=Enhanced+Delamination+of+Ultrathin+Free-Standing+Polymer+Films+via+Self-Limiting+Surface+Modification.">Enhanced Delamination of Ultrathin Free-Standing Polymer Films via Self-Limiting Surface Modification.</a> Langmuir. 30, 5126-5132 (2014).</li><li>Buck, M. E., Lynn, D. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Free-Standing+and+Reactive+Thin+Films+Fabricated+by+Covalent+Layer-by-Layer+Assembly+and+Subsequent+Lift-Off+of+Azlactone-Containing+Polymer+Multilayers.">Free-Standing and Reactive Thin Films Fabricated by Covalent Layer-by-Layer Assembly and Subsequent Lift-Off of Azlactone-Containing Polymer Multilayers.</a> Langmuir. 26, 16134-16140 (2010).</li><li>Freund, L. B., Suresh, 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 Materials: Stress, Defect Formation and Surface Evolution. , (2003).</li><li>Dubas, S. T., Farhat, T. R., Schlenoff, J. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Multiple+Membranes+from+&#8220;True&#8221;+Polyelectrolyte+Multilayers.">Multiple Membranes from &#8220;True&#8221; Polyelectrolyte Multilayers.</a> J. Am. Chem. Soc. 123, 5368-5369 (2001).</li><li>Linder, V., Gates, B. D., Ryan, D., Parviz, B. A., Whitesides, G. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Water-soluble+sacrificial+layers+for+surface+micromachining.">Water-soluble sacrificial layers for surface micromachining.</a> Small. 1, 730-736 (2005).</li><li>Mamedov, A. A., Kotov, N. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Free-Standing+Layer-by-Layer+Assembled+Films+of+Magnetite+Nanoparticles.">Free-Standing Layer-by-Layer Assembled Films of Magnetite Nanoparticles.</a> Langmuir. 16, 5530-5533 (2000).</li><li>Ono, S. S., Decher, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Preparation+of+Ultrathin+Self-Standing+Polyelectrolyte+Multilayer+Membranes+at+Physiological+Conditions+Using+pH-Responsive+Film+Segments+as+Sacrificial+Layers.">Preparation of Ultrathin Self-Standing Polyelectrolyte Multilayer Membranes at Physiological Conditions Using pH-Responsive Film Segments as Sacrificial Layers.</a> Nano Lett. 6, 592-598 (2006).</li><li>Stroock, A. D., Kane, R. S., Weck, M., Metallo, S. J., Whitesides, G. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Synthesis of Free-Standing Quasi-Two-Dimensional Polymers. Langmuir. 19, 2466-2472 (2002).</li><li>Kriz, J., Dybal, J., Kurkova, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Cooperativity+in+macromolecular+interactions+as+a+proximity+effect:+NMR+and+theoretical+study+of+electrostatic+coupling+of+weakly+charged+complementary+polyions.">Cooperativity in macromolecular interactions as a proximity effect: NMR and theoretical study of electrostatic coupling of weakly charged complementary polyions.</a> J. Phys. Chem. B. 107, 12165-12174 (2003).</li><li>Krogman, K. C., Zacharia, N. S., Schroeder, S., Hammond, P. T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Automated+Process+for+Improved+Uniformity+and+Versatility+of+Layer-by-Layer+Deposition.">Automated Process for Improved Uniformity and Versatility of Layer-by-Layer Deposition.</a> Langmuir. 23, 3137-3141 (2007).</li><li>Hall, D. B., Underhill, P., Torkelson, J. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Spin+coating+of+thin+and+ultrathin+polymer+films.">Spin coating of thin and ultrathin polymer films.</a> Polymer Engineering &amp; Science. 38, 2039-2045 (1998).</li></ol>

作者什么都没有透露。

在PDAC基板处理是基于自限静电相互作用，这意味着任何尺寸的基板可以容易地处理过的，只要它们是带负电荷的（ 例如 ，硅或玻璃）。 图1-2显示了非常大的薄膜（13厘米在直径）制造使用此协议，唯一的变化是所用的试剂的体积。最终达到的尺寸出现仅由沉积和剥离设备或用于制造自支撑结构的聚合物的最终强度的限制。而前者显然是一个实际的问题，后者不是的聚合物的?...

自由站立薄聚合物膜被用在各种应用，包括传感器，1-3的MEMs，催化或过滤，4和组织工程。5-8它们还用于基础研究探索聚合物在封闭条件下的行为。9- 13所述的自立式膜是一个支撑在非连续基底例如环形环或环箍相对于在硅晶片或玻璃载玻片。这项工作描述了一个简单的，可重复的制造过程为超薄的自立聚合物膜，是适合于大面积膜或高通量的生产。它是一种具有多种不同的聚合物，包括聚（乙烯醇缩甲醛），聚苯乙烯，和聚（甲基丙烯酸甲酯）的兼容。它可被用于制造自支撑膜是一样大的13厘米直径或薄10纳米。 的自由站立的聚合物的制造包括三个基本步骤:1）D聚合物膜的eposition到传统衬底诸如晶片或幻灯片，2） 释放或从基材膜的剥离 ，和3） 捕获得到的膜的到载体上。本文详细介绍了我们在报道的各种版本方法的早期研究的过程。14 沉积可通过任何数目的基本聚合物薄膜的技术，如旋涂，蒸镀，或浸涂来实现。在这项工作中，我们采用标准的旋涂技术。 的"剥离浮于"技术是最常用的方法，用于从它的基底释放超薄膜15在这种技术中，薄膜和基板浸在适当的溶剂浴中。溶剂溶胀的膜和诱导自发分层，释放膜并使其漂浮到浴的顶部。最小膜厚度可使用提起被释放断开浮筒上通过与膨胀引起的应变能平衡界面剥离能量确定:16 <img alt="式（1）" src="/files/ftp_upload/52832/52832eq1.jpg" width="200" /> （1） 其中，L是膜厚度，νf是薄膜的泊松比，E是杨氏模量的膜，ξ为膜的溶胀比，和γ是剥离的界面能。的典型方式绕过由公式所施加的限制（1）是沉积膜和淀积衬底之间的牺牲层间17-20当此夹层溶解在溶剂浴，膜被释放，并且可以在支撑被捕获。一个相关的方法是牺牲覆盖层的方法，它利用膜的机械剥离到牺牲层PRIOR溶解。21 使用牺牲材料的有几个主要缺点。首先，增加了一个额外的处理材料和步骤，可能需要最佳膜制造条件和牺牲材料的加工条件之间的折衷。第二，牺牲材料可能难以存在不影响机械性能的最终自立式膜的或纯度。第三，该方法用于沉积牺牲材料必须优化并监测质量在整体自立式膜制造的操作。14 在这项工作中，我们描述了一种表面改性技术，降低了界面剥离能量，使剥离浮于技术用于超薄膜。淀积衬底通过组装一个自限，自优化近单层的聚阳离子polydiallyldiammonium氯（PDAC）改性。由于聚阳离子和基片之间的结合强度，该表面改性是稳健的后续工艺步骤。近单层形成的自我限制和自我优化性质要求几乎为零优化是容易扩展到大面积。 以下的去除，该膜浮到溶剂浴的顶部，其中它被捕获在环箍状支撑。尽管不十分重视在现存文献，在这项工作中，我们将描述用于捕获大面积薄膜在载体上，以减少撕裂或以其他方式损坏膜的概率技术。

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>Vinylec E</td>
			<td>SPI</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>ethyl lactate, &#62;98%, FCC, FG,</td>
			<td>Sigma-Aldrich</td>
			<td>W244007-1KG-K</td>
			<td></td>
		</tr>
		<tr>
			<td>4&#34; silicon wafers &#60;100&#62;, Single side polished</td>
			<td>International Wafer Service</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>sulfuric acid, 98%, ACS reagent grade</td>
			<td>Sigma-Aldrich</td>
			<td>320501-6X500ML</td>
			<td></td>
		</tr>
		<tr>
			<td>hydrogen peroxide, 30%, semiconductor grade</td>
			<td>Sigma-Aldrich</td>
			<td>316989-3.7L</td>
			<td></td>
		</tr>
		<tr>
			<td>isopropanol, ACS grade, 4 L</td>
			<td>Fisher Scientific</td>
			<td>A464-4</td>
			<td></td>
		</tr>
		<tr>
			<td>dichloromethane, ACS grade</td>
			<td>Alfa-Aesar</td>
			<td>22917</td>
			<td></td>
		</tr>
		<tr>
			<td>deionized water , distilled</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>PDAC reagent (Sigma-Aldrich 409014)</td>
			<td>Sigma-Aldrich</td>
			<td>409014</td>
			<td></td>
		</tr>
		<tr>
			<td>Spin Coater</td>
			<td>Laurell Technologies&#160;</td>
			<td>WS-650-23</td>
			<td></td>
		</tr>
		<tr>
			<td>Barnstead/Thermolyne Super Nuova explosion-proof hot plate&#160;</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>explosion-proof forced air oven</td>
			<td>VWR&#160;</td>
			<td>1330 FMS&#160;</td>
			<td></td>
		</tr>
		<tr>
			<td>balance with a range of 1 mg to 1020 g</td>
			<td>Mettler Toledo</td>
			<td>MS1003S</td>
			<td></td>
		</tr>
		<tr>
			<td>reflectance spectrometer</td>
			<td>Filmetrics</td>
			<td>F20-UV</td>
			<td></td>
		</tr>
		<tr>
			<td>manipulator consisting of a Klinger tilt stage, a Brinkman rack-and-pinion and a lab jack&#160;</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Cutting tool/template, LLNL-built, no drawings</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>straight edge, LLNL, no drawings</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Tent hoop, LLNL</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>culture dish 190 mm x 100 mm, Pyrex</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>20 ml beaker, Pyrex</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>250 ml beaker, Pyrex</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>1000 ml beaker, Pyrex</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>60 ml glass vial with plastic stopper&#160;</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>petri dish, 150 mm diameter x2, Pyrex</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>600 ml beaker x2, Pyrex</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>tweezers, stainless steel</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>cutting blade</td>
			<td>Exacto</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>clean room wipes</td>
			<td>Contec&#160;</td>
			<td>PNHS-99</td>
			<td></td>
		</tr>
		<tr>
			<td>polyester knit 9/91 IPA/DI water wipes</td>
			<td>Contec&#160;</td>
			<td>Prosat&#160;</td>
			<td></td>
		</tr>
		<tr>
			<td>Fluoroware wafer trays</td>
			<td>Ted Pella</td>
			<td>1395-40</td>
			<td></td>
		</tr>
		<tr>
			<td>Nylon Micro fiber (camel hair)</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Disposable BD 3-mL plastic syringe</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>0.2 um&#160; Luer-lock PTFE filters</td>
			<td>Acrodisc&#160;</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>0.45 um&#160; Luer-lock PTFE filters</td>
			<td>Acrodisc&#160;</td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

fabrication of large-area free-standing ultrathin polymer films

This procedure describes a method for the fabrication of large-area and ultrathin free-standing polymer films. Typically, ultrathin films are prepared using either sacrificial layers, which may damage the film or affect its mechanical properties, or they are made on freshly cleaved mica, a substrate that is difficult to scale. Further, the size of ultrathin film is typically limited to a few square millimeters. In this method, we modify a surface with a polyelectrolyte that alters the strength of adhesion between polymer and deposition substrate. The polyelectrolyte can be shown to remain on the wafer using spectroscopy, and a treated wafer can be used to produce multiple films, indicating that at best minimal amounts of the polyelectrolyte are added to the film. The process has thus far been shown to be limited in scalability only by the size of the coating equipment, and is expected to be readily scalable to industrial processes. In this study, the protocol for making the solutions, preparing the deposition surface, and producing the films is described.

图1示出了在大面积上一个独立的聚合物薄膜的一个例子。使用此处介绍的过程，并安装在一个13厘米直径的钢箍此为55nm厚的聚乙烯醇缩甲醛膜制成。发生脱层大面积不引入，导致撕开薄膜的缺陷。因此，聚乙烯醇缩甲醛的内在强度甚至可以为非常薄的膜利用。 图2示出了一个22纳米厚的自支撑膜是足够强以装载用表玻璃和铜珠称量的质量&gt; 3×10 5次电影本身。椭?...

Watch this Scientific Journal Video about Fabrication of Large-area Free-standing Ultrathin Polymer Films at JoVE.com

Fabrication of Large-area Free-standing Ultrathin Polymer Films

We describe a method for the fabrication of large-area (up to 13 cm diameter) and ultrathin (as thin as 8 nm) polymer films. Instead of using a sacrificial interlayer to delaminate the film from its substrate, we use a self-limiting surface treatment suitable for arbitrarily large areas.

大面积的制造自立性的超薄聚合物薄膜

This procedure describes a method for the fabrication of large-area and ultrathin free-standing polymer films.  Typically, ultrathin films are prepared ...

fabrication-of-large-area-free-standing-ultrathin-polymer-films

Research

JoVE Journal

Chemistry

15.2K 次观看.  Lawrence Livermore National Laboratory. We describe a method for the fabrication of large-area (up to 13 cm diameter) and ultrathin (as thin as 8 nm) polymer films. Instead of using a sacrificial interlayer to delaminate the film from its substrate, we use a self-limiting surface treatment suitable for arbitrarily large areas.

视频: Fabrication of Large-area Free-standing Ultrathin Polymer Films

Towards Biomimicking Wood: Fabricated Free-standing Films of Nanocellulose, Lignin, and a Synthetic Polycation

Woody materials are comprised of plant cell walls that contain a layered secondary cell wall composed of structural polymers of polysaccharides and lignin. Layer-by-layer (LbL) assembly process which relies on the assembly of oppositely charged molecules from aqueous solutions was used to build a freestanding composite film of isolated wood polymers of lignin and oxidized nanofibril cellulose (NFC). To facilitate the assembly of these negatively charged polymers, a positively charged polyelectrolyte, poly(diallyldimethylammomium chloride) (PDDA), was used as a linking layer to create this simplified model cell wall. The layered adsorption process was studied quantitatively using quartz crystal microbalance with dissipation monitoring (QCM-D) and ellipsometry. The results showed that layer mass/thickness per adsorbed layer increased as a function of total number of layers. The surface coverage of the adsorbed layers was studied with atomic force microscopy (AFM). Complete coverage of the surface with lignin in all the deposition cycles was found for the system, however, surface coverage by NFC increased with the number of layers. The adsorption process was carried out for 250 cycles (500 bilayers) on a cellulose acetate (CA) substrate. Transparent free-standing LBL assembled nanocomposite films were obtained when the CA substrate was later dissolved in acetone. Scanning electron microscopy (SEM) of the fractured cross-sections showed a lamellar structure, and the thickness per adsorption cycle (PDDA-Lignin-PDDA-NC) was estimated to be 17 nm for two different lignin types used in the study. The data indicates a film with highly controlled architecture where nanocellulose and lignin are spatially deposited on the nanoscale (a polymer-polymer nanocomposites), similar to what is observed in the native cell wall.

The objective of this research was to form synthetic plant cell wall tissue using layer-by-layer assembly of nanocellulose fibrils and isolated lignin assembled from dilute aqueous suspensions.&#160; Surface measurement techniques of quartz crystal microbalance and atomic force microscopy were used to monitor the formation of the polymer-polymer nanocomposite material.

朝仿生学木:纳米纤维素，木质素的装配式自由站立电影和合成聚阳离子

Woody materials are comprised of plant cell walls that contain a layered secondary cell wall composed of structural polymers of polysaccharides and ...

科研

化学

Confocal Imaging of Confined Quiescent and Flowing Colloid-polymer Mixtures

The behavior of confined colloidal suspensions with attractive interparticle interactions is critical to the rational design of materials for directed assembly1-3, drug delivery4, improved hydrocarbon recovery5-7, and flowable electrodes for energy storage8. Suspensions containing fluorescent colloids and non-adsorbing polymers are appealing model systems, as the ratio of the polymer radius of gyration to the particle radius&#160;and concentration of polymer control the range and strength of the interparticle attraction, respectively. By tuning the polymer properties and the volume fraction of the colloids, colloid fluids, fluids of clusters, gels, crystals, and glasses can be obtained9.&#160;Confocal microscopy, a variant of fluorescence microscopy, allows an optically transparent and fluorescent sample to be imaged with high spatial and temporal resolution in three dimensions. In this technique, a small pinhole or slit blocks the emitted fluorescent light from regions of the sample that are outside the focal volume of the microscope optical system. As a result, only a thin section of the sample in the focal plane is imaged. This technique is particularly well suited to probe the structure and dynamics in dense colloidal suspensions at the single-particle scale: the particles are large enough to be resolved using visible light and diffuse slowly enough to be captured at typical scan speeds of commercial confocal systems10. Improvements in scan speeds and analysis algorithms have also enabled quantitative confocal imaging of flowing suspensions11-16,37.&#160;In this paper, we demonstrate confocal microscopy experiments to probe the confined phase behavior and flow properties of colloid-polymer mixtures. We first prepare colloid-polymer mixtures that are density- and refractive-index matched. Next, we report a standard protocol for imaging quiescent dense colloid-polymer mixtures under varying confinement in thin wedge-shaped cells. Finally, we demonstrate a protocol for imaging colloid-polymer mixtures during microchannel flow.

Confocal microscopy is used to image quiescent and flowing colloid-polymer mixtures, which are studied as model systems for attractive suspensions. Image analysis algorithms are used to calculate structural and dynamic metrics for the colloidal particles that measure changes due to geometric confinement.

密闭静态和流动胶体聚合物混合物的共聚焦成像

The behavior of confined colloidal suspensions with attractive interparticle interactions is critical to the rational design of materials for directed ...

Preparation of Highly Porous Coordination Polymer Coatings on Macroporous Polymer Monoliths for Enhanced Enrichment of Phosphopeptides

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous polymer monoliths. The developed approach is based on the preparation of a macroporous polymer containing carboxylic acid functional groups and the subsequent step-by-step solution-based controlled growth of a layer of a porous coordination polymer on the surface of the pores of the polymer monolith. The prepared metal-organic polymer hybrid has a high specific micropore surface area. The amount of iron(III) sites is enhanced through metal-organic coordination on the surface of the pores of the functional polymer support. The increase of metal sites is related to the number of iterations of the coating process.
The developed preparation scheme is easily adapted to a capillary column format. The functional porous polymer is prepared as a self-contained single-block porous monolith within the capillary, yielding a flow-through separation device with excellent flow permeability and modest back-pressure. The metal-organic polymer hybrid column showed excellent performance for the enrichment of phosphopeptides from digested proteins and their subsequent detection using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. The presented experimental protocol is highly versatile, and can be easily implemented to different organic polymer supports and coatings with a plethora of porous coordination polymers and metal-organic frameworks for multiple purification and/or separation applications.

A procedure for the preparation of porous hybrid separation media composed of a macroporous polymer monolith internally coated by a high surface area microporous coordination polymer is presented.

对磷酸增强富集制备高度多孔配位聚合物涂层的孔聚合物石柱的

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous ...

Photodynamic Therapy with Blended Conducting Polymer/Fullerene Nanoparticle Photosensitizers

In this article a method for the fabrication and reproducible in-vitro evaluation of conducting polymer nanoparticles blended with fullerene as the next generation photosensitizers for Photodynamic Therapy (PDT) is reported. The nanoparticles are formed by hydrophobic interaction of the semiconducting polymer MEH-PPV (poly[2-methoxy-5-(2-ethylhexyloxy)-1,4-phenylenevinylene]) with the fullerene PCBM (phenyl-C61-butyric acid methyl ester) in the presence of a non-compatible solvent. MEH-PPV has a high extinction coefficient that leads to high rates of triplet formation, and efficient charge and energy transfer to the fullerene PCBM. The latter processes enhance the efficiency of the PDT system through fullerene assisted triplet and radical formation, and ultrafast deactivation of MEH-PPV excited stated. The results reported here show that this nanoparticle PDT sensitizing system is highly effective and shows unexpected specificity to cancer cell lines.

This protocol describes a method for the fabrication of conducting polymer nanoparticles blended with fullerene. These nanoparticles were investigated for their potential use as a next generation photosensitizers for Photodynamic Therapy (PDT).

光动力疗法与混合导电高分子/富勒烯纳米颗粒光敏剂

In this article a method for the fabrication and reproducible in-vitro evaluation of conducting polymer nanoparticles blended with fullerene as the next ...

Cooling Rate Dependent Ellipsometry Measurements to Determine the Dynamics of Thin Glassy Films

This report aims to fully describe the experimental technique of using ellipsometry for cooling rate dependent Tg (CR-Tg) experiments. These measurements are simple high-throughput characterization experiments, which can determine the glass transition temperature (Tg), average dynamics, fragility and the expansion coefficient of the super-cooled liquid and glassy states for a variety of glassy materials. This technique allows for these parameters to be measured in a single experiment, while other methods must combine a variety of different techniques to investigate all of these properties. Measurements of dynamics close to Tg are particularly challenging. The advantage of cooling rate dependent Tg measurements over other methods which directly probe bulk and surface relaxation dynamics is that they are relatively quick and simple experiments, which do not utilize fluorophores or other complicated experimental techniques. Furthermore, this technique probes the average dynamics of technologically relevant thin films in temperature and relaxation time (&#964;&#945;) regimes relevant to the glass transition (&#964;&#945; &#62; 100 sec). The limitation to using ellipsometry for cooling rate dependent Tg experiments is that it cannot probe relaxation times relevant to measurements of viscosity (&#964;&#945; &#60;&#60; 1 sec). Other cooling rate dependent Tg measurement techniques, however, can extend the CR-Tg method to faster relaxation times. Furthermore, this technique can be used for any glassy system so long as the integrity of the film remains throughout the experiment.

Here, we present a protocol for cooling rate dependent ellipsometry experiments, which can determine the glass transition temperature (Tg), average dynamics, fragility and the expansion coefficient of the super-cooled liquid and glass for a variety of glassy materials.

冷却率相关的椭偏仪测量确定薄膜玻膜的动力学

This report aims to fully describe the experimental technique of using ellipsometry for cooling rate dependent Tg (CR-Tg) experiments. These measurements ...

The Preparation and Properties of Thermo-reversibly Cross-linked Rubber Via Diels-Alder Chemistry

A method for using Diels Alder thermo-reversible chemistry as cross-linking tool for rubber products is demonstrated. In this work, a commercial ethylene-propylene rubber, grafted with maleic anhydride, is thermo-reversibly cross-linked in two steps. The pending anhydride moieties are first modified with furfurylamine to graft furan groups to the rubber backbone. These pendant furan groups are then cross-linked with a bis-maleimide via a Diels-Alder coupling reaction. Both reactions can be performed under a broad range of experimental conditions and can easily be applied on a large scale. The material properties of the resulting Diels-Alder cross-linked rubbers are similar to a peroxide-cured ethylene/propylene/diene rubber (EPDM) reference. The cross-links break at elevated temperatures (&#62; 150 &#176;C) via the retro-Diels-Alder reaction and can be reformed by thermal annealing at lower temperatures (50-70 &#176;C). Reversibility of the system was proven with infrared spectroscopy, solubility tests and mechanical properties. Recyclability of the material was also shown in a practical way, i.e., by cutting a cross-linked sample into small parts and compression molding them into new samples displaying comparable mechanical properties, which is not possible for conventionally cross-linked rubbers.

A simple two-step approach involving rubber modification and cross-linking yields fully reworkable, elastic rubber products.

热可逆交联橡胶通过的Diels-Alder反应的化学制备与性能

A method for using Diels Alder thermo-reversible chemistry as cross-linking tool for rubber products is demonstrated. In this work, a commercial ...

Capillary Electrophoresis to Monitor Peptide Grafting onto Chitosan Films in Real Time

Free-solution capillary electrophoresis (CE) separates analytes, generally charged compounds in solution through the application of an electric field. Compared to other analytical separation techniques, such as chromatography, CE is cheap, robust and effectively requires no sample preparation (for a number of complex natural matrices or polymeric samples). CE is fast and can be used to follow the evolution of mixtures in real time (e.g., chemical reaction kinetics), as the signals observed for the separated compounds are directly proportional to their quantity in solution.
Here, the efficiency of CE is demonstrated for monitoring the covalent grafting of peptides onto chitosan films for subsequent biomedical applications. Chitosan&#39;s antimicrobial and biocompatible properties make it an attractive material for biomedical applications such as cell growth substrates. Covalently grafting the peptide RGDS (arginine - glycine - aspartic acid - serine) onto the surface of chitosan films aims at improving cell attachment. Historically, chromatography and amino acid analysis have been used to provide a direct measurement of the amount of grafted peptide. However, the fast separation and absence of sample preparation provided by CE enables equally accurate yet real-time monitoring of the peptide grafting process. CE is able to separate and quantify the different components of the reaction mixture: the (non-grafted) peptide and the chemical coupling agents. In this way the use of CE results in improved films for downstream applications.
The chitosan films were characterized through solid-state NMR (nuclear magnetic resonance) spectroscopy. This technique is more time-consuming and cannot be applied in real time, but yields a direct measurement of the peptide and thus validates the CE technique.

Free solution capillary electrophoresis is a fast, cheap and robust analytical method that enables the quantitative monitoring of chemical reactions in real time. Its utility for rapid, convenient and precise analysis is demonstrated here through analysis of covalent peptide grafting onto chitosan films for improved cell adhesion.

毛细管电泳监视肽接枝壳聚糖膜实时

Free-solution capillary electrophoresis (CE) separates analytes, generally charged compounds in solution through the application of an electric field. ...

Fabrication and Testing of Photonic Thermometers

In recent years, a push for developing novel silicon photonic devices for telecommunications has generated a vast knowledge base that is now being leveraged for developing sophisticated photonic sensors. Silicon photonic sensors seek to exploit the strong confinement of light in nano-waveguides to transduce changes in physical state to changes in resonance frequency. In the case of thermometry, the thermo-optic coefficient, i.e., changes in refractive index due to temperature, causes the resonant frequency of the photonic device such as a Bragg grating to drift with temperature. We are developing a suite of photonic devices that leverage recent advances in telecom compatible light sources to fabricate cost-effective photonic temperature sensors, which can be deployed in a wide variety of settings ranging from controlled laboratory conditions, to the noisy environment of a factory floor or a residence. In this manuscript, we detail our protocol for the fabrication and testing of photonic thermometers.

We describe the process of fabrication and testing of photonic thermometers.

光子温度计的制作与测试

In recent years, a push for developing novel silicon photonic devices for telecommunications has generated a vast knowledge base that is now being ...

Microfluidic Dry-spinning and Characterization of Regenerated Silk Fibroin Fibers

The protocol demonstrates a method for mimicking the spinning process of silkworm. In the native spinning process, the contracting spinning duct enables the silk proteins to be compact and ordered by shearing and elongation forces. Here, a biomimetic microfluidic channel was designed to mimic the specific geometry of the spinning duct of the silkworm. Regenerated silk fibroin (RSF) spinning doped with high concentration, was extruded through the microchannel to dry-spin fibers at ambient temperature and pressure. In the post-treated process, the as-spun fibers were drawn and stored in ethanol aqueous solution. Synchrotron radiation wide-angle X-ray diffraction (SR-WAXD) technology was used to investigate the microstructure of single RSF fibers, which were fixed to a sample holder with the RSF fiber axis normal to the microbeam of the X-ray. The crystallinity, crystallite size, and crystalline orientation of the fiber were calculated from the WAXD data. The diffraction arcs near the equator of the two-dimensional WAXD pattern indicate that the post-treated RSF fiber has a high orientation degree.

A protocol for the microfluidic spinning and microstructure characterization of regenerated silk fibroin monofilament is presented.

微流控干纺及再生丝素纤维的表征

The protocol demonstrates a method for mimicking the spinning process of silkworm. In the native spinning process, the contracting spinning duct enables ...

Time-resolved Photophysical Characterization of Triplet-harvesting Organic Compounds at an Oxygen-free Environment Using an iCCD Camera

Here, we present a sensible method of the acquisition and analysis of time-resolved photoluminescence using an ultrafast iCCD camera. This system enables the acquisition of photoluminescence spectra covering the time regime from nanoseconds up to 0.1 s. This enables us to follow the changes in the intensity (decay) and emission of the spectra over time. Using this method, it is possible to study diverse photophysical phenomena, such as the emission of phosphorescence, and the contributions of prompt and delayed fluorescence in molecules showing thermally activated delayed fluorescence (TADF). Remarkably, all spectra and decays are obtained in a single experiment. This can be done for solids (thin film, powder, crystal) and liquid samples, where the only limitations are the spectral sensitivity of the camera and the excitation wavelength (532 nm, 355 nm, 337 nm, and 266 nm). This technique is, thus, very important when investigating the excited state dynamics in organic emitters for their application in organic light-emitting diodes and other areas where triplet harvesting is of paramount importance. Since triplet states are strongly quenched by oxygen, emitters with efficient TADF luminescence, or those showing room temperature phosphorescence (RTP), must be correctly prepared in order to remove any dissolved oxygen from solutions and films. Otherwise, no long-lived emission will be observed. The method of degassing solid samples as presented in this work is basic and simple, but the degassing of liquid samples creates additional difficulties and is particularly interesting. A method of minimizing solvent loss and changing the sample concentration, while still enabling to remove oxygen in a very efficient and a repeatable manner, is presented in this work.

Here, we present a method of the spectroscopic characterization of organic molecules by means of time-resolved photoluminescence spectroscopy on the nanosecond-to-millisecond timescale in oxygen-free conditions. Methods to efficiently remove oxygen from the samples and, thus, limit luminescence quenching are also described.

利用 iccd 摄像机对无氧环境下的三重收集有机化合物进行光物理表征

Here, we present a sensible method of the acquisition and analysis of time-resolved photoluminescence using an ultrafast iCCD camera. This system enables ...