Name: surface properties of synthesized nanoporous carbon and silica matrices
Uploaded: 2019-03-27T14:00:00
Description: Watch this Scientific Journal Video about Surface Properties of Synthesized Nanoporous Carbon and Silica Matrices at JoVE.com

作者要感谢国家科学中心提供财政支持, 并提供了赠款。DEC-2019/BB越来越/379/11 和 UMO2-2016/STM/00092。提交人还感谢波兰人力资本计划人力资本PO kl 4.1.1 以及国家研究和发展中心在研究赠款下提供的部分支持。PBSNAJN13<UNK> 2012。提交人特别感谢波兰卢布林 Maria Curie-skvodowska 大学化学系国际现象司 l. Hovysz 教授的善良和能够测量 SBA-15 纳米粒子的润湿性。

1. OMC 材料的制备
<ol><li>
作为 OMC 前体的二氧化硅基体的合成
	<ol>
<li>加入50毫升 HCl (36%-38%), 制备 1.6 m HCl 的360毫升在500毫升的圆底瓶中, 然后加入310毫升的超纯水 (电阻率为 18.2 mmy·cm)。</li>
		<li>除此之外, 还加入10克 PE 10500 聚合物 (6.500 g/mol)。</li>
		<li>将烧瓶放在超声波浴缸中。将溶液加热至 35°c, 搅拌至固体聚合物完全溶解, 形成均匀的混合物。</li>
		<li>在烧瓶中加入10克的 1, 3, 5-三...

<ol>
	<li>Tao, Y., Kanoh, H., Abrams, L., Kaneko, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mesopore-Modified+Zeolites:+Preparation,+Characterization,+and+Applications.">Mesopore-Modified Zeolites: Preparation, Characterization, and Applications.</a> Chemical Reviews. , 896-910 (2006).</li><li>Wan, Y., Zhao, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=On+the+Controllable+Soft-Templating+Approach+to+Mesoporous+Silicates.">On the Controllable Soft-Templating Approach to Mesoporous Silicates.</a> Chemical Reviews. 107, 2821-2860 (2007).</li><li>Khder, A. E. S., Hassan, H. M. A., El-Shall, M. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Acid+catalyzed+organic+transformations+by+heteropolytungstophosphoric+acid+supported+on+MCM-41.">Acid catalyzed organic transformations by heteropolytungstophosphoric acid supported on MCM-41.</a> Applied Catalysis A. 411, 77-86 (2012).</li><li>Zhao, D. 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=Triblock+Copolymer+Syntheses+of+Mesoporous+Silica+with+Periodic+50+to+300+Angstrom+Pores.">Triblock Copolymer Syntheses of Mesoporous Silica with Periodic 50 to 300 Angstrom Pores.</a> Science. 279, 548-552 (1998).</li><li>Linssen, T., Cassiers, K., Cool, P., Vansant, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mesoporous+templated+silicates:+an+overview+of+their+synthesis,+catalytic+activation+and+evaluation+of+the+stability.">Mesoporous templated silicates: an overview of their synthesis, catalytic activation and evaluation of the stability.</a> Advances in Colloid and Interface Science. 103, 121-147 (2003).</li><li>Eftekhari, A., Fan, Z. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ordered+mesoporous+carbon+and+its+applications+for+electrochemical+energy+storage+and+conversion.">Ordered mesoporous carbon and its applications for electrochemical energy storage and conversion.</a> Materials Chemistry Frontiers. 1, 1001-1027 (2017).</li><li>Sing, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Characterization+of+porous+materials:+past,+present+and+future.">Characterization of porous materials: past, present and future.</a> Colloids and Surfaces A. 241, 3-7 (2004).</li><li>Huo, Q., Margolese, D. I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Generalized+synthesis+of+periodic+surfactant/inorganic+composite+materials.">Generalized synthesis of periodic surfactant/inorganic composite materials.</a> Nature. 368, 317-321 (1994).</li><li>Selvaraj, M., Kawi, S., Park, D. W., Ha, C. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+and+characterization+of+GaSBA-15:+Effect+of+synthesis+parameters+and+hydrothermal+stability.">Synthesis and characterization of GaSBA-15: Effect of synthesis parameters and hydrothermal stability.</a> Microporous and Mesoporous Materials. , 586-595 (2009).</li><li>Leonard, A., 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=Toward+a+better+control+of+internal+structure+and+external+morphology+of+mesoporous+silicas+synthesized+using+a+nonionic+surfactant.">Toward a better control of internal structure and external morphology of mesoporous silicas synthesized using a nonionic surfactant.</a> Langmuir. 19, 5484-5490 (2003).</li><li>Liang, C., Li, Z., Dai, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mesoporous+Carbon+Materials:+Synthesis+and+Modification.">Mesoporous Carbon Materials: Synthesis and Modification.</a> Angewandte Chemie International Edition. 47, 3696-3717 (2008).</li><li>Babi&#263;, 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=New+mesoporous+carbon+materials+synthesized+by+a+templating+procedure.">New mesoporous carbon materials synthesized by a templating procedure.</a> Ceramics International. 39 (4), 4035-4043 (2013).</li><li>Allen, S. J., Whitten, L., Mckay, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+Production+and+Characterization+of+Activated+Carbons:+A+Review.">The Production and Characterization of Activated Carbons: A Review.</a> Developments in Chemical Engineering and Mineral Processing. 6, 231-261 (1998).</li><li>Kwak, G., 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=Preparation+Method+of+Co3O4+Nanoparticles+Using+Ordered+Mesoporous+Carbons+as+a+Template+and+Their+Application+for+Fischer-Tropsch+Synthesis.">Preparation Method of Co3O4 Nanoparticles Using Ordered Mesoporous Carbons as a Template and Their Application for Fischer-Tropsch Synthesis.</a> The Journal of Physical Chemistry C. 117 (4), 1773-1779 (2013).</li><li>Koo, H. M., 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=Effect+of+the+ordered+meso-macroporous+structure+of+Co/SiO2+on+the+enhanced+activity+of+hydrogenation+of+CO+to+hydrocarbons.">Effect of the ordered meso-macroporous structure of Co/SiO2 on the enhanced activity of hydrogenation of CO to hydrocarbons.</a> Catalysis Science and Technology. 6, 4221-4231 (2016).</li><li>Jun, S., Joo, S. H., Ryoo, R., Kruk, M., Jaroniec, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+of+New,+Nanoporous+Carbon+with+Hexagonally+Ordered+Mesostructure.">Synthesis of New, Nanoporous Carbon with Hexagonally Ordered Mesostructure.</a> Journal of the American Chemical Society. 122 (43), 10712-10713 (2000).</li><li>Washburn, E. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+dynamics+of+capillary+flow.">The dynamics of capillary flow.</a> Physical Review Series2. 17, 273 (1921).</li><li>&#346;liwi&#324;ska-Bartkowiak, M., Sterczy&#324;ska, A., Long, Y., Gubbins, K. E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Influence+of+Microroughness+on+the+Wetting+Properties+of+Nano-Porous+Silica+Matrices.">Influence of Microroughness on the Wetting Properties of Nano-Porous Silica Matrices.</a> Molecular Physics. 112, 2365-2371 (2014).</li><li>&#346;liwi&#324;ska-Bartkowiak, M., 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=Melting/freezing+behavior+of+a+fluid+confined+in+porous+glasses+and+MCM-41:+dielectric+spectroscopy+and+molecular+simulation.">Melting/freezing behavior of a fluid confined in porous glasses and MCM-41: dielectric spectroscopy and molecular simulation.</a> Journal of Chemical Physics. 114, 950-962 (2001).</li><li>Coasne, B., Czwartos, J., &#346;liwi&#324;ska-Bartkowiak, M., Gubbins, K. E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Freezing+of+mixtures+confined+in+silica+nanopores:+experiment+and+molecular+simulation.">Freezing of mixtures confined in silica nanopores: experiment and molecular simulation.</a> Journal of Chemical Physics. 133, 084701-084709 (2010).</li><li>Che&#322;kowski, 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> Dielectric Physics. , (1990).</li><li>Radhakrishnan, R., Gubbins, K. E., &#346;liwi&#324;ska-Bartkowiak, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Global+phase+diagrams+for+freezing+in+porous+media.">Global phase diagrams for freezing in porous media.</a> Journal of Chemical Physics. 116, 1147-1155 (2002).</li><li>Gubbins, K. E., Long, Y., &#346;liwi&#324;ska-Bartkowiak, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thermodynamics+of+confined+nano-phases.">Thermodynamics of confined nano-phases.</a> Journal of Chemical Thermodynamics. 74, 169-183 (2014).</li><li>Radhakrishnan, R., Gubbins, K. E., &#346;liwi&#324;ska-Bartkowiak, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effect+of+the+fluid-wall+interaction+on+freezing+of+confined+fluids:+Toward+the+development+of+a+global+phase+diagram.">Effect of the fluid-wall interaction on freezing of confined fluids: Toward the development of a global phase diagram.</a> Journal of Chemical Physics. 112, 11048 (2000).</li><li>Cassie, A. B. D., Baxter, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Wettability+of+porous+surfaces.">Wettability of porous surfaces.</a> Transactions of the Faraday Society. 40, 546 (1944).</li><li>Sing, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Adsorption+methods+for+the+characterization+of+porous+materials.">Adsorption methods for the characterization of porous materials.</a> Advances in Colloid and Interface Science. 76, 3-11 (1998).</li><li>Sing, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+use+of+nitrogen+adsorption+for+the+characterisation+of+porous+materials.">The use of nitrogen adsorption for the characterisation of porous materials.</a> Colloids and Surfaces A. 187, 3-9 (2001).</li><li>Yu, C., Fan, J., Tian, B., Zhao, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Morphology+Development+of+Mesoporous+Materials:+a+Colloidal+Phase+Separation+Mechanism.">Morphology Development of Mesoporous Materials: a Colloidal Phase Separation Mechanism.</a> Chemistry of Materials. 16 (5), 889-898 (2004).</li><li>Liu, 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=Enhancement+of+Electrochemical+Hydrogen+Insertion+in+N-Doped+Highly+Ordered+Mesoporous+Carbon.">Enhancement of Electrochemical Hydrogen Insertion in N-Doped Highly Ordered Mesoporous Carbon.</a> The Journal of Physical Chemistry C. 118 (5), 2370-2374 (2014).</li><li>Choi, W. 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=Platinum+Nanoclusters+Studded+in+the+Microporous+Nanowalls+of+Ordered+Mesoporous+Carbon.">Platinum Nanoclusters Studded in the Microporous Nanowalls of Ordered Mesoporous Carbon.</a> Advanced Materials. 17, 446-451 (2005).</li><li>Rouquerol, F., Rouquerol, J., Sing, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Adsorption by Powders and Porous Solids: Principles, Methodology and Application. , (1999).</li><li>Gregg, S. J., Sing, K. S. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Adsorption, Surface Area and Porosity. , (1982).</li><li>Llewellyn, P. L., Rouquerol, F., Rouquerol, J., Sing, K. S. W., Unger, K. K., Kreysa, G., Baselt, J. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Critical+appraisal+of+the+use+of+nitrogen+adsorption+for+the+characterization+of+porous+carbons.">Critical appraisal of the use of nitrogen adsorption for the characterization of porous carbons.</a> Characterization of Porous Solids V. , 421-427 (2000).</li><li>Sing, K. S. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+use+of+gas+adsorption+for+the+characterization+of+porous+solids.">The use of gas adsorption for the characterization of porous solids.</a> Colloids and Surfaces. 38, 113-124 (1989).</li><li>Rouquerol, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Recommendations+for+the+characterization+of+porous+solids.">Recommendations for the characterization of porous solids.</a> Pure &amp; Applied Chemistry. 66, 1739-1758 (1994).</li><li>Marega, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+direct+SAXS+approach+for+the+determination+of+specific+surface+area+of+clay+in+polymer-layered+silicate+nanocomposites.">A direct SAXS approach for the determination of specific surface area of clay in polymer-layered silicate nanocomposites.</a> The Journal of Physical Chemistry B. 116, 7596-7602 (2012).</li><li>Tsao, C. S., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Neutron+Scattering+Methodology+for+Absolute+Measurement+of+Room-Temperature+Hydrogen+Storage+Capacity+and+Evidence+for+Spillover+Effect+in+a+Pt-Doped+Activated+Carbon.">Neutron Scattering Methodology for Absolute Measurement of Room-Temperature Hydrogen Storage Capacity and Evidence for Spillover Effect in a Pt-Doped Activated Carbon.</a> The Journal of Physical Chemistry Letters. 1, 1569-1573 (2010).</li><li>Mattson, J. S., Mark, H. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Activated Carbon: Surface Chemistry and Adsorption from Solution. , (1971).</li><li>L&#225;szl&#243;, K., Szucs, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Surface+characterization+of+polyethyleneterephthalate+(PET)+based+activated+carbon+and+the+effect+of+pH+on+its+adsorption+capacity+from+aqueous+phenol+and+2,3,4-trichlorophenol+solutions.">Surface characterization of polyethyleneterephthalate (PET) based activated carbon and the effect of pH on its adsorption capacity from aqueous phenol and 2,3,4-trichlorophenol solutions.</a> Carbon. 39, 1945-1953 (2001).</li><li>Garten, V. A., Weiss, D. E., Willis, 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=A+new+interpretation+of+the+acidic+and+basic+structures+in+carbons.">A new interpretation of the acidic and basic structures in carbons.</a> Australian Journal of Chemistry. 10, 309-328 (1957).</li><li>Boehm, H. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Surface+oxides+on+carbon+and+their+analysis:+A+critical+assessment.">Surface oxides on carbon and their analysis: A critical assessment.</a> Carbon. 40, 145-149 (2002).</li><li>Menendez, J. A., Phillips, J., Xia, B., Radovic, L. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=On+the+modification+and+characterization+of+chemical+surface+properties+of+activated+carbon:+In+the+search+of+carbons+with+stable+basic+properties.">On the modification and characterization of chemical surface properties of activated carbon: In the search of carbons with stable basic properties.</a> Langmuir. 12, 4404-4410 (1996).</li></ol>

在制备有序介孔碳材料过程中的关键步骤包括制备有序介孔二氧化硅材料, 作为模板, 其结构性能明确, 影响最终材料的性能,在氮气气氛下的回火碳化步骤。对具有圆柱形孔28的介孔有序硅酸盐的典型制备方法进行了改进,涉及到 pe10500 聚合物在结构改进中的应用。材料的性能。模板的三维、互联和稳定的多孔结构是制备介孔碳材料所必需的。此外, 制备的一个关键缺点是模板去除?...

1992年, 首次采用有机模板获得了有序的纳米多孔二氧化硅材料;此后, 大量与这些结构的不同方面、合成方法、其性质的调查、修改和不同应用有关的出版物出现在文献1、2 中 ,3。对 SBA-15 纳米多孔二氧化硅基体 4的兴趣在于其独特的质量: 表面积大、毛孔宽、孔径分布均匀、化学和机械性能好。具有圆柱形孔隙的纳米多孔二氧化硅材料, 如 sba-155,通常被用作催化剂的多孔基质, 因为它们是有机反应6,7中的高效催化剂。该材料可以用多种方法合成, 这些方法可以影响其特性8、9、10.因此, 优化这些方法对于许多领域的潜在应用至关重要: 电化学设备、纳米技术、生物和医学、药物输送系统, 或粘附和摩擦学。在本研究中, 提出了两种不同类型的纳米多孔结构, 即二氧化硅和碳多孔基体。为了比较其性能, 采用溶胶-凝胶法合成了 SBA-15 基体, 并利用得到的二氧化硅基体与碳前体的浸渍法制备了有序的纳米多孔碳材料。
多孔碳材料在许多电器中都很重要, 因为它们的表面积很大, 具有独特和明确的物理化学特性, 6、11、12.典型的制备结果是材料具有随机分布的孔隙率和无序结构;一般孔隙参数变化的可能性也有限, 因此, 得到了孔隙尺寸分布相对较大的结构。对于具有高表面积和有序的纳米孔系统的纳米多孔碳材料, 这种可能性得到了扩大。在许多应用中, 更多的预测几何形状和对孔隙空间内物理化学过程的更多控制都很重要: 作为催化剂、分离介质系统、先进的电子材料和许多科学领域的纳米反应器14,15岁
为了获得多孔碳副本, 有序硅酸盐可以作为一个固体基质, 直接引入碳前体。该方法可分为几个阶段: 有序二氧化硅材料的选择;碳前驱体沉积在二氧化硅基体中;碳化;然后, 去除二氧化硅基体。这种方法可以获得许多不同类型的碳质材料, 但并非所有的无孔材料都有有序的结构。这一过程的一个重要因素是选择合适的基质, 其纳米孔必须形成稳定的三维结构16。
本文研究了孔壁类型对合成纳米多孔基体表面性能的影响。OMC 材料的表面性能反映在 OMC 二氧化硅模拟 (SBA-15) 的表面性能上。这两类材料 (OMC 和 SBA-15) 的结构和结构特性的特点是低温 N2吸附吸附-解吸测量 (在 77 k)、透射电子显微镜 (tem) 和能量色散 x 射线分析 (编辑)。
低温气体吸附-解吸测量是多孔材料表征中最重要的技术之一。氮气由于其纯度高, 并且有可能与固体吸附剂产生强烈的相互作用, 因此被用作吸附剂。这种技术的重要优点是方便用户使用的商业设备和相对容易的数据处理程序。氮吸附剂/解吸等温线的测定是基于吸附剂分子在广泛的压力范围内在 77 K 的位置上的积累.采用巴雷特、乔伊纳和哈伦达 (BJH) 的方法, 从实验吸附或解吸等温线计算孔径分布。BJH 方法最重要的假设包括平面和吸附物在被调查表面上的均匀分布。然而, 这一理论是基于开尔文方程, 它仍然是最广泛使用的方法, 计算孔径分布在介孔范围内。
为了评价样品的电化学特性, 采用了电位滴定法。材料的表面化学取决于与表面异质原子或官能团的存在有关的表面电荷。通过接触角分析, 研究了表面性能。毛孔内的润湿性提供了有关吸附吸附剂相互作用的信息。利用介电松弛光谱 (DRS) 技术研究了壁面粗糙度对两种样品中封闭水熔融温度的影响。介电常数的测量允许对熔融现象的研究, 因为液体和固相的极化性是不同的。电容温度依赖性斜率的变化表明, 系统中发生了熔融现象。

<table>
	<tbody>
		<tr>
			<td>1,3,5-trimethylbenzene</td>
			<td>Sigma-Aldrich, Poland</td>
			<td>M7200 Sigma-Aldrich</td>
			<td>Mesitylene, also known as 1,3,5-trimethylbenzene, reagent grade, assay: 98%.</td>
		</tr>
		<tr>
			<td>anhydrous ethanol</td>
			<td>POCH, Avantor Performance Materials Poland S.A.</td>
			<td>396480111</td>
			<td>Assay, min. 99.8 %, analysis-pur (a.p.)</td>
		</tr>
		<tr>
			<td>ASAP 2020. Accelerated Surface Area and Porosimetry System</td>
			<td>Micromeritics Instrument Corporation, Norcross, GA, USA</td>
			<td></td>
			<td>Samples were outgassed before analysis at 120 oC for 24 hours in degas port of analyzer. The dead space volume was measured for calibration on experimental measurement using helium as a adsorbate.</td>
		</tr>
		<tr>
			<td>Automatic burette Dosimat 665</td>
			<td>Metrohm, Switzerland</td>
			<td></td>
			<td>The surface charge properties were experimentally determined by potentiometric titration of the suspension at constant temperature 20&#176;C maintained by the thermostatic device. Prior to potentiometric titration measurements, the solid samples were dried by 24 hours at 120 oC. The initial pH was established by addition of 0.3 cm3 of 0.2 mol/L HCl. T The 0.1 mol/L NaOH solution was used as a titrant, added gradually by using automatic burette.</td>
		</tr>
		<tr>
			<td>Digital pH-meter pHm-240</td>
			<td>Radiometer, Copenhagen</td>
			<td></td>
			<td>Device coupled with automatic burette</td>
		</tr>
		<tr>
			<td>ethyl alcohol</td>
			<td>POCH, Avantor Performance Materials Poland S.A.</td>
			<td>396420420</td>
			<td>Assay, min. 96 %.analysis-pur (a.p.)</td>
		</tr>
		<tr>
			<td>glucose</td>
			<td>POCH, Avantor Performance Materials Poland S.A.</td>
			<td>459560448</td>
			<td>assay 99.5%</td>
		</tr>
		<tr>
			<td>Hydrochloric acid</td>
			<td>POCH, Avantor Performance Materials Poland S.A.</td>
			<td>575283115</td>
			<td>Hydrochloric acid, 35 - 38% analysis-pur (a.p.)</td>
		</tr>
		<tr>
			<td>HOPG graphite substrate</td>
			<td>Spi Supplies</td>
			<td>LOT#1170906</td>
			<td>HOPG SPI-2 Grade, 20x20x1 mm</td>
		</tr>
		<tr>
			<td>Impedance analyzer Solartron 1260</td>
			<td>Solartron</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Pluronic PE 6400 polymer</td>
			<td>BASF (Polska)</td>
			<td></td>
			<td>(EO13PO70EO13)</td>
		</tr>
		<tr>
			<td>Pluronic PE10500</td>
			<td>BASF Canada Inc.</td>
			<td></td>
			<td>Molar mass 6500 g/mol</td>
		</tr>
		<tr>
			<td>potassium hydroxide</td>
			<td>Sigma-Aldrich, Poland</td>
			<td>P5958 Sigma-Aldrich</td>
			<td>BioXtra, &#8805;85% KOH basis</td>
		</tr>
		<tr>
			<td>SEM microscope</td>
			<td>JEOL JSM-7001F</td>
			<td></td>
			<td>Scanning Electron Microscope with EDS detector</td>
		</tr>
		<tr>
			<td>Sigma Force Tensiometer 701</td>
			<td>KSV, Sigma701, Biolin Scientific</td>
			<td></td>
			<td>force tensiometer</td>
		</tr>
		<tr>
			<td>Sulfuric acid (VI)</td>
			<td>POCH, Avantor Performance Materials Poland S.A.</td>
			<td>575000115</td>
			<td></td>
		</tr>
		<tr>
			<td>surface glass type KS 324 Kavalier</td>
			<td>Megan Poland</td>
			<td></td>
			<td>80 % of SiO2 , 11% of Na2O and 9% of CaO</td>
		</tr>
		<tr>
			<td>Tecnai G2 T20 X-TWIN</td>
			<td>FEI, USA</td>
			<td></td>
			<td>Transmission Electron Microscope with EDX detector.</td>
		</tr>
		<tr>
			<td>TEM microscope</td>
			<td>JEOL JEM-1400</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>temperature controller ITC503</td>
			<td>Oxford Instruments</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Tetraethylorthosilicate</td>
			<td>Sigma-Aldrich, Poland</td>
			<td>131903</td>
			<td>Tetraethyl silicate, TEOS, reagent grade, assay 98%</td>
		</tr>
		<tr>
			<td>Ultrapure water</td>
			<td>Millipore, Merck KGaA, Darmstadt, Germany</td>
			<td>SIMSV0001</td>
			<td>Simplicity Water Purification SystemUltrapure Water: 18.2 MegOhm&#183;cm, TOC: &#60;5 ppb</td>
		</tr>
	</tbody>
</table>

surface properties of synthesized nanoporous carbon and silica matrices

在这项工作中, 我们报告了合成和表征有序的纳米多孔碳材料 (也称为有序介孔碳材料 [OMC]) 与4.6 纳米的孔径, 并有序的二氧化硅多孔基质, SBA-15, 具有5.3 纳米的孔径。本文描述了纳米多孔分子筛的表面性质、润湿性以及d2o在具有相似孔径的不同有序多孔材料中的熔融行为。为此, 分别应用碳前体和溶胶-凝胶法,通过对二氧化硅基体进行浸渍, 合成了具有高阶纳米多孔结构的 omc 和 SBA-15。研究系统的多孔结构的特点是在 77 K的 n 2吸附-解吸分析。为确定合成材料表面的电化学特性, 进行了电位滴定测量;对 OMC 的结果表明, 相对于 SBA-15, phpzc 向较高的 ph 值有显著的转移。这表明, 所研究的 OMC 具有与含氧功能基团有关的表面特性。为了描述材料的表面特性, 还确定了液体穿透所研究的多孔层的接触角。毛细管上升法证实了硅墙相对于碳壁的润湿性增加, 孔隙粗糙度对流体壁相互作用的影响, 这对二氧化硅比碳硅粉要明显得多。应用介电法研究了在 OMC 和 SBA-15 中限制的d2o的熔融行为。结果表明, 与5纳米大小的 SBA-15孔隙熔融温度的抑制相比, omc 孔隙中 d2o 熔融温度的抑制度高出约 15 k。这是由所研究矩阵的吸附吸附剂相互作用的影响造成的。

为了表征 OMC 和 SBA-15 样品的多孔结构, 记录了 N2吸附-解吸等温线在 77 k。实验图1a-d给出了实验 n2 气体吸附-解吸等温线, 描述了所研究系统的特征, 以及从吸附和解吸数据中得到的孔径分布 (psd)。拐点在吸附等温线上的位置 (图 1a, c) 表示中间孔充填过程开始的压力。根据 Kelvin 方程, 计?...

Watch this Scientific Journal Video about Surface Properties of Synthesized Nanoporous Carbon and Silica Matrices at JoVE.com

Surface Properties of Synthesized Nanoporous Carbon and Silica Matrices

在这里, 我们报告了有序纳米多孔碳 (具有4.6 纳米孔尺寸) 和 SBA-15 (具有5.3 纳米孔径) 的合成和表征。本文介绍了纳米多孔分子筛的表面和结构特性、润湿性以及材料中的d2o的熔融行为。

合成纳米碳和二氧化硅矩阵的表面性能

In this work, we report the synthesis and characterization of ordered nanoporous carbon material (also called ordered mesoporous carbon material [OMC]) ...

该协议意义重大，因为与多孔基质中液体的闭塞效应有关的多孔表面特性是能源、医学和环境应用中的一个关键问题。新材料、碳和二氧化硅纳米孔的合成和表征，以及湿润参数的测定，为结合纳米相的特性提供了新的信息。在纳米技术、生物学和医学领域，优化新材料的合成方法对于获得具有所需性能的产品至关重要。基本合成及其表征方法应具有明显性，并呈现，以便获得具有所需结构和表面特性的产品。此过程的可视化演示非常重要，因为它提供了应用过程的详细说明，并确保了可重复的性能。演示该程序将是马尔戈扎塔·齐恩凯维奇-斯特扎尔卡博士，玛丽亚·居里-斯克洛多斯卡大学化学系的博士后，以及我实验室的博士后安吉丽娜·斯特钦斯卡博士。首先，在500毫升的圆底烧瓶中准备360毫升1.6摩尔盐酸。在烧瓶上加入10克聚乙烯10500聚合物。然后将烧瓶放在超声波浴中，将溶液加热至35摄氏度。搅拌，直到固体聚合物完全溶解，形成同质的混合物。接下来在烧瓶中加入10克1、3、5-三甲苯，搅拌其含量，同时在水浴中将其保持在35摄氏度。搅拌30分钟后，在烧瓶中加入34克四乙基正硅酸盐。超过10分钟，缓慢添加四乙基矫形，并不断搅拌滴。然后在35摄氏度下再搅拌20小时。20 小时后，将烧瓶中的内容转移到 PTFE 墨盒中。将墨盒放在自动驱动器中，在 90 摄氏度下烘烤溶液 24 小时。第二天，使用布赫纳漏斗过滤产生的沉淀物。然后用蒸馏水清洗，至少用一升水。在室温下干燥获得的固体，并在空气中使用消声炉，在500摄氏度下对样品进行热处理6小时。首先制备两种水、三摩尔硫酸和葡萄糖比例合适的浸渍溶液，其中葡萄糖起到碳前体的作用，硫酸起到催化剂的作用。要准备浸渍溶液一，混合5克水，0.14克三摩尔硫酸，每克二氧化硅1.25克葡萄糖。然后准备浸渍溶液二。对于此溶液，混合五克水、0.8 克三摩尔硫酸和每克二氧化硅 0.75 克葡萄糖。将一克二氧化硅材料、一克浸渍溶液和催化剂放在500毫升的烧瓶中。在真空干燥器中加热混合物在100摄氏度下6小时。接下来在真空干燥机的混合物中加入一克浸渍溶液二，并在真空干燥器中再次加热混合物，温度为160摄氏度，12小时。将获得的复合材料转移到砂浆中，研磨颗粒以形成均匀的混合物。将所得产品放入氮气下的流动炉中，以每分钟2.5摄氏度的加热速率加热至700摄氏度。在此温度下，在氮气下保持材料六小时。六小时后，关闭炉子，让溶液冷却后才能打开炉子。首先准备100毫升的蚀刻溶液。混合 50 毫升 95%乙醇和 50 毫升水。为此，加入七克氢氧化钾，搅拌至溶解。将获得的所有碳化材料放在250毫升的圆底烧瓶中，并加入100毫升的蚀刻溶液。为系统提供回流冷凝器和磁力搅拌器。在不断搅拌时将混合物加热至沸腾，并允许其煮沸一小时。将获得的材料转移到布赫纳漏斗。用至少四升蒸馏水清洗，然后晾干。如果需要，使用低温氮吸收-脱吸测量、TEM 成像、能量分散 X 射线光谱、电位滴定测量和/或介电松弛光谱来描述材料，如随附的文本协议中所述。氮吸附和TEM方法显示了合成材料中孔结构高度有序。EDS和电位滴定方法表明，OMC的特点是减少酸位点和减少氧气含量。要确定所研究样本毛孔内的接触角，请首先应用修改后的 Washburn 方程（此处显示并在文本协议中描述）来估计所研究毛孔内前进的接触角的值。然后准备力 Tensiometer。对于粉末，准备一个直径为三毫米的小管子。对于液体，准备直径为 22 毫米、最大体积为 10 毫升的容器。接下来启动连接到 Tensiometer 的计算机程序。然后将带液体的容器放在电机驱动的舞台上，将玻璃管与样品悬挂在电平衡上。启动电机，以每分钟 10 毫米的恒定速率接近样品。将样品管的浸入深度设置为液体中，以便其等于一毫米。当 m 平方等于 t 的 f 开始显示特征高原时停止实验。毛孔内的可加工性在很大程度上取决于孔隙的粗糙度、壁的种类和孔隙。毛孔中液体的流动性与理想平坦表面的流动性显著不同。以下是有序中孔碳材料纳米孔内接触角测量的样本结果。还显示了光滑、高度定向的热解石墨的参考可维性。测量的接触角显示为微观润湿参数的函数。接触角越低，越强，透水性越高，即穿透性液体分子与研究表面的相互作用更强。测量的接触角度表明，与OMC壁，二氧化硅壁的可韧性更好，并表明孔隙粗糙度对流体-壁相互作用的影响对二氧化硅的影响比碳纳米孔更明显。除了这里显示的，吸附-吸附相互作用，通过四面转换红外光谱的介电或X射线的结构分析，可以进一步深入了解材料的分子动力学。用于纳米材料表面特性表征的技术也可以应用于材料表面与生物活性物质之间的相互作用。浸渍二氧化硅基质时请小心，因为此步骤由于有毒硫酸而具有危险性。

Research

JoVE Journal

Chemistry

Preparation of Silica Nanoparticles Through Microwave-assisted Acid-catalysis

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle ...

科研

化学

Exploring the Radical Nature of a Carbon Surface by Electron Paramagnetic Resonance and a Calibrated Gas Flow

通过电子顺磁共振和校准气体流量探索碳表面的激进性质

While the first Electron Paramagnetic Resonance (EPR) studies regarding the effects of oxidation on the structure and stability of carbon radicals date ...

Synthesis and Catalytic Performance of Gold Intercalated in the Walls of Mesoporous Silica

合成和金插在介孔二氧化硅的墙壁催化性能

As a promising catalytically active nano reactor, gold nanoparticles intercalated in mesoporous silica (GMS) were successfully synthesized and properties ...

Transport of Surface-modified Carbon Nanotubes through a Soil Column

表面修饰碳纳米管通过土柱运输

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

Preparation of Carbon Nanosheets at Room Temperature

碳纳米片在室温下准备

Amphiphilic molecules equipped with a reactive, carbon-rich "oligoyne" segment consisting of conjugated carbon-carbon triple bonds self-assemble into ...

TiO2-coated Hollow Glass Microspheres with Superhydrophobic and High IR-reflective Properties Synthesized by a Soft-chemistry Method

TiO2-coated Hollow Glass Microspheres with Superhydrophobic and High IR-reflective Properties Synthesized by a Soft-chemistry Method

二氧化钛<sub&gt; 2</sub与由软化学法合成的超疏水性和高IR反射属性&gt;涂覆的空心玻璃微球

This manuscript proposes a soft-chemistry method to develop superhydrophobic and highly IR-reflective hollow glass microspheres (HGM). The anatase TiO2 ...

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

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 ...

Raman and IR Spectroelectrochemical Methods as Tools to Analyze Conjugated Organic Compounds

拉曼光谱和红外光谱电化学法作为分析共轭有机化合物的工具

In the presented work, two spectroelectrochemical techniques are discussed as tools for the analysis of the structural changes occurring in the molecule ...

Preparation of Functional Silica Using a Bioinspired Method

用 Bioinspired 法制备功能性二氧化硅

The goal of the protocols described herein is to synthesize bioinspired silica materials, perform enzyme encapsulation therein, and partially or totally ...

Imine Metathesis by Silica-Supported Catalysts Using the Methodology of Surface Organometallic Chemistry

利用表面有机金属化学方法，利用硅支持的催化剂进行Imine金属分析

With this protocol, a well-defined singlesite silica-supported heterogeneous catalyst [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is designed and prepared ...