Name: microbubble fabrication of concave-porosity pdms beads
Uploaded: 2015-12-15T14:00:00
Description: Watch this Scientific Journal Video about Microbubble Fabrication of Concave-porosity PDMS Beads at JoVE.com

이 작품은 화학의 부서 및 연구의 사무실 (RCAP 13-8032)에서 내부 지원을 포함하여 과학 및 공학, 웨스턴 켄터키 대학의 오그 덴 대학에서 지원하고있다. WKU 현미경 시설에서 닥터 존 Andersland (SEM 이미지) 및 연소 공학 (BET 분석)에 대한 WKU 연구소의 부교수 연의 카오의 지원은이 작업을 수행의 중심이되고있다.

에멀젼 1. 준비 <ol><li> 에멀젼 내용 <ol><li> 질량 소금 적당량 0.03 M 용액 10 ㎖를 제조한다. 백금 (IV) 클로라이드 측정 0.101 g, 아연 (II) 클로라이드 (ZnCl 2) 측정 값 0.032 g 및 염화나트륨 0.018 g위한 계수. </li><li> 각각의 시험관에, DI 물 10 ㎖로 각각의 염을 용해. 나중에 사용하기 위해 따로 설정합니다. </li><li> 이 절차를 통해 내용에 대한 20 ml의 밀봉 유리 병을 사용합니다. 유리 병에 균형을 용?...

<ol>
	<li>Pedraza, E., Brady, A. C., Fraker, C. A., Stabler, C. L. <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+macroporous+poly(dimethylsiloxane)+scaffolds+for+tissue+engineering+applications.">Synthesis of macroporous poly(dimethylsiloxane) scaffolds for tissue engineering applications.</a> J. Biomater. Sci., Polym. Ed. 24 (9), 1041-1056 (2013).</li><li>Ratner, B. D., Bryant, S. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Biomaterials:+Where+we+have+been+and+where+we+are+going.">Biomaterials: Where we have been and where we are going.</a> Annu. Rev. Biomed. Eng. 6, 41-75 (2004).</li><li>B&#233;langer, M. C., Marois, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Hemocompatibility,+biocompatibility,+inflammatory+and+in+vivo+studies+of+primary+reference+materials+low-density+polyethylene+and+polydimethylsiloxane:+A+review.">Hemocompatibility, biocompatibility, inflammatory and in vivo studies of primary reference materials low-density polyethylene and polydimethylsiloxane: A review.</a> J. Biomed. Mater. 58 (5), 467-477 (2001).</li><li>Kobayashi, T., Saitoh, H., Fujii, N., Hoshino, Y., Takanashi, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Porous+membrane+of+polydimethylsiloxane+by+hydrosilylation+cure:+characteristics+of+membranes+having+pores+formed+by+hydrogen+foams.">Porous membrane of polydimethylsiloxane by hydrosilylation cure: characteristics of membranes having pores formed by hydrogen foams.</a> J. Appl. Polym. Sci. 50 (6), 971-979 (1993).</li><li>Yager, 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=Microfluidic+diagnostic+technologies+for+global+public+health.">Microfluidic diagnostic technologies for global public health.</a> Nature. 442 (7101), 412-418 (2006).</li><li>Yu, P., Lu, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=PDMS+used+in+microfluidic+devices:+principles,+devices+and+technologies.">PDMS used in microfluidic devices: principles, devices and technologies.</a> Adv. Mater. Sci. Res. 11, 443-450 (2011).</li><li>Zhou, J., Khodakov, D. A., Ellis, A. V., Voelcker, N. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Surface+modification+for+PDMS-based+microfluidic+devices.">Surface modification for PDMS-based microfluidic devices.</a> Electrophoresis. 33 (1), 89-104 (2012).</li><li>Spietelun, A., Pilarczyk, M., Kloskowski, A., Namie&#347;nik, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Polyethylene+glycol-coated+solid-phase+microextraction+fibres+for+the+extraction+of+polar+analytes&#8212;A+review.">Polyethylene glycol-coated solid-phase microextraction fibres for the extraction of polar analytes&#8212;A review.</a> Talanta. 87, 1-7 (2011).</li><li>Vas, G., V&#233;key, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Solid-phase+microextraction:+a+powerful+sample+preparation+tool+prior+to+mass+spectrometric+analysis.">Solid-phase microextraction: a powerful sample preparation tool prior to mass spectrometric analysis.</a> J. Mass Spectrom. 39 (3), 233-254 (2004).</li><li>Odziemkowski, M., Koziel, J. A., Irish, D. E., Pawliszyn, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Sampling+and+Raman+confocal+microspectroscopic+analysis+of+airborne+particulate+matter+using+poly(dimethylsiloxane)+solid+phase+microextraction+fibers.">Sampling and Raman confocal microspectroscopic analysis of airborne particulate matter using poly(dimethylsiloxane) solid phase microextraction fibers.</a> Anal. Chem. 73 (13), 3131-3139 (2001).</li><li>Grosse, M. T., Lamotte, M., Birot, M., Deleuze, H. <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+microcellular+polysiloxane+monoliths.">Preparation of microcellular polysiloxane monoliths.</a> J. Polym. Sci., Part A: Polym. Chem. 46 (1), 21-32 (2007).</li><li>Sun, W., Yan, X., Zhu, X. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis,+porous+structure,+and+underwater+acoustic+properties+of+macroporous+cross-linked+copolymer+beads.">Synthesis, porous structure, and underwater acoustic properties of macroporous cross-linked copolymer beads.</a> Colloid Polym. Sci. 290 (1), 73-80 (2012).</li><li>Dufaud, O., Favre, E., Sadtler, V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Porous+elastomeric+beads+from+crosslinked+emulsions.">Porous elastomeric beads from crosslinked emulsions.</a> J. Appl. Polym. Sci. 83 (5), 967-971 (2002).</li><li>Farmer, B. C., Mason, M., Nee, M. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Concave+porosity+non-polar+beads+by+a+modified+microbubble+fabrication.">Concave porosity non-polar beads by a modified microbubble fabrication.</a> Mater. Lett. 98, 105-107 (2013).</li><li>Flegler, S. L., Heckman, J. W., Klomparens, K. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Scanning and Transmission Electron Microscopy: An Introduction. , 151-155 (1995).</li><li>Brunauer, S., Emmett, P. H., Teller, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Adsorption+of+Gases+in+Multimolecular+Layers.">Adsorption of Gases in Multimolecular Layers.</a> J. Am. Chem. Soc. 60 (2), 309-319 (1938).</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=Characterization+of+porous+materials:+past,+present+and+future.">Characterization of porous materials: past, present and future.</a> Colloids Surf. A. 241 (1), 3-7 (2004).</li></ol>

도 1의 다른 SEM 이미지로도 1a의 비교에 의해 볼 수 있듯이,이 프로토콜을 이용하여 (전해질 농도 및 아이덴티티를 조정함으로써) 생성 된 비드., 낮은 이온 강도 에멀젼 제조 것과는 근본적으로 다르다 당초 보고서 사용 상기 수성 지방족 인터페이스 14 중합 가교 결합 반응을 촉매 의도 PTCL 4. 이 보고서에서, 큰 오목 들여 쓰기는 볼 수 있었다. 해당 보고서...

Polydimethylsiloxane (PDMS) is one of the most widely used silicone compounds. Its biocompatibility has led to widespread use in implant and other biomedical engineering structures1,2. It is trivially cross-linked into elastic structures using an organosilyl compound (such as triethoxysilane), a simple and reliable procedure which has made it useful for cast polymer applications where some flexibility is required3. Once cross-linked, PDMS is largely inert, particularly in biological conditions, and is therefore useful for a variety of food and medical applications4,5. Ease of casting, chemical inertness, and hydrophobicity have made it a natural choice for microfluidic devices6,7. Its affinity for non-halogenated, non-polar organic compounds has made it a popular stationary phase in separations chemistry8-10. 
Recently, microbubble fabrications have been used to generate porous beads for use as catalyst structural substrates or in chemical separations11,12. In both applications, ideal materials will have a maximized surface-area-to-volume (SAV) ratio for best efficiency. In a microbubble fabrication process, microstructuring of materials is typically accomplished by isolating the polymer in aliphatic &#8220;microbubbles&#8221; by emulsification in an aqueous continuous phase. The initial report of microporous PDMS beads produced them by mechanical emulsification of two phases (aliphatic and aqueous)13. The stock PDMS liquid (and its cross-linking agent) is dissolved into the aliphatic phase, which is structured into microscopic beads by being forced to cavitate within the (continuous) aqueous phase. The emulsification is stabilized by the addition of a non-ionic surfactant. When the emulsion is added dropwise to a heated bath, solid beads form by agglomeration of the microbubbles into clusters of tiny spheres of cross-linked PDMS. Our goal in this protocol is to modify this procedure to develop beads with an inverted porosity to improve the SAV ratio of the material.
As reported previously, control of the beads can be directed to some extent by the aliphatic:aqueous ratios in the emulsion. However, we have reported recently that addition of platinum(IV) chloride (PtCl4) inverts the porosity: materials are formed in which the PDMS is riddled with concave pores14. This indicates that the aqueous layer cavitates inside the aliphatic one, despite having similar aliphatic:aqueous ratios to those published in the original work13. The primary advantage of our method is that this concave porosity should naturally result in an increased SAV ratio, and thus, improved efficiency for analytical chemistry applications. While we are continuing to explore the specific effects of the addition of the platinum compound, we show here that the same effect can be accomplished using any aqueously soluble ionic compound, though perhaps to a reduced extent. Because our techniques also differ in some key aspects from what has been previously reported, we present our protocols here as a video to encourage others to extend our methods. Most notably, we use a common bath sonicator of the type used to clean glassware or other equipment, rather than the (considerably more expensive) probe sonicator often used in microbubble fabrication. This adjusted approach to the microbubble fabrication procedure could potentially be extended for the production of large quantities of bulk materials as well, creating porous sheets or slabs which could have applications for biomedical devices, aerospace and automotive industry, or substrates for chemical catalysis. Users seeking to generate high-SAV-ratio, microstructured materials using other similar polymers for such analyses may find that our protocols can be extended to any polymer for which the microbubble emulsion technique can be applied.

<table border="0">
	<tbody>
		<tr>
			<td>Poly(dimethylsiloxane), vinyl terminated</td>
			<td>Sigma-Aldrich</td>
			<td>68083-19-2</td>
			<td></td>
		</tr>
		<tr>
			<td>n-Heptane</td>
			<td>Sigma-Aldrich</td>
			<td>142-82-5</td>
			<td>Flammable</td>
		</tr>
		<tr>
			<td>Triethoxysilane</td>
			<td>Sigma-Aldrich</td>
			<td>998-30-1</td>
			<td>Flammable, Accutely Toxic</td>
		</tr>
		<tr>
			<td>Sorbitan Monoleate (Span-80)</td>
			<td>Fluker</td>
			<td>1338-43-8</td>
			<td></td>
		</tr>
		<tr>
			<td>Platinum (IV) Chloride</td>
			<td>Sigma-Aldrich</td>
			<td>13454-96-1</td>
			<td>Accutely Toxic</td>
		</tr>
		<tr>
			<td>Zinc (II) Chloride</td>
			<td>Sigma-Aldrich</td>
			<td>7646-85-7</td>
			<td></td>
		</tr>
		<tr>
			<td>Sodium Chloride</td>
			<td>Sigma-Aldrich</td>
			<td>7647-14-5</td>
			<td></td>
		</tr>
		<tr>
			<td>2.8L Water Bath Sonicator</td>
			<td>VWR</td>
			<td>97043-964</td>
			<td></td>
		</tr>
	</tbody>
</table>

microbubble fabrication of concave-porosity pdms beads

Microbubble fabrication (by use of a fine emulsion) provides a means of increasing the surface-area-to-volume (SAV) ratio of polymer materials, which is particularly useful for separations applications. Porous polydimethylsiloxane (PDMS) beads can be produced by heat-curing such an emulsion, allowing the interface between the aqueous and aliphatic phases to mold the morphology of the polymer. In the procedures described here, both polymer and crosslinker (triethoxysilane) are sonicated together in a cold-bath sonicator. Following a period of cross-linking, emulsions are added dropwise to a hot surfactant solution, allowing the aqueous phase of the emulsion to separate, and forming porous polymer beads. We demonstrate that this method can be tuned, and the SAV ratio optimized, by adjusting the electrolyte content of the aqueous phase in the emulsion. Beads produced in this way are imaged with scanning electron microscopy, and representative SAV ratios are determined using Brunauer&#8211;Emmett&#8211;Teller (BET) analysis. Considerable variability with the electrolyte identity is observed, but the general trend is consistent: there is a maximum in SAV obtained at a specific concentration, after which porosity decreases markedly.

다른 전해질 조건 에멀젼으로부터 발생 비드의 대표적인 SEM 이미지가도 1에 도시된다.도 1a는 DuFaud하여 얻은, 등. (13)과 유사한 비드를 도시 모든 전해질의 첨가없이, 우리의 방법을 사용하여 제조. 구슬은 각각의 금속 이온에 대해 서로 다른 형태 학적 결과, 그림 1B-D에 표시. 도시 된 모든 이미지에 대해, 0.03 - M 전해질 용액 300 μL 그 위상 0.012 M의 전해질 농...

Watch this Scientific Journal Video about Microbubble Fabrication of Concave-porosity PDMS Beads at JoVE.com

Microbubble Fabrication of Concave-porosity PDMS Beads

Procedures used to generate microstructured concave-porosity polydimethylsiloxane beads are presented. Effects of electrolyte concentration and identity within the aqueous phase are particularly emphasized.

오목 다공성 PDMS 비즈의 마이크로 버블 제작

Microbubble fabrication (by use of a fine emulsion) provides a means of increasing the surface-area-to-volume (SAV) ratio of polymer materials, which is ...

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