Name: synthesis of graphene nanofluids with controllable flake size distributions
Uploaded: 2019-07-17T13:00:00
Description: Watch this Scientific Journal Video about Synthesis of Graphene Nanofluids with Controllable Flake Size Distributions at JoVE.com

这项工作得到了国家自然科学基金(授权号21776095)、广州市科技重点项目(授权号201804020048)和广东省清洁能源技术重点实验室(授权号2008A060301002)的支持。我们感谢LetPub(www.letpub.com)在编写本手稿期间提供的语言帮助。

1. 液相中石墨的去角化
<ol><li>试剂制备<ol>
<li>在干燥清洁的平底烧瓶中,加入20克聚乙烯醇(PVA),然后加入1000mL蒸馏水。 注:如果暂停处理未达到满意程度,可以重复执行该步骤以获得额外的暂停。</li>
		<li>轻轻旋转烧瓶,直到 PVA 完全溶解。 注意:PVA对人体有害;因此,应该使用防护手套和外科口罩。</li>
		<li>将 50 克石墨粉加入平底烧瓶,轻轻旋转烧瓶,直到石墨粉在悬架中完全分散。</li>
		<li>将产生?...

<ol>
	<li>Sadeghinezhad, E., 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=A+comprehensive+review+on+graphene+nanofluids:+Recent+research,+development+and+applications.">A comprehensive review on graphene nanofluids: Recent research, development and applications.</a> Energy Conversion and Management. 111, 466-487 (2016).</li><li>Wang, 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=Highly+Efficient+Production+of+Graphene+by+an+Ultrasound+Coupled+with+a+Shear+Mixer+in+Supercritical+CO2.">Highly Efficient Production of Graphene by an Ultrasound Coupled with a Shear Mixer in Supercritical CO2.</a> Industrial &amp; Engineering Chemistry Research. 57 (49), 16701-16708 (2018).</li><li>Cao, H. Y., Guo, Z. X., Xiang, H., Gong, X. 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H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Facile+and+size-controllable+preparation+of+graphene+oxide+nanosheets+using+high+shear+method+and+ultrasonic+method.">Facile and size-controllable preparation of graphene oxide nanosheets using high shear method and ultrasonic method.</a> Journal of Experimental Nanoscience. 12 (1), 247-262 (2017).</li><li>Chen, L. X., 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=Oriented+graphene+nanoribbons+embedded+in+hexagonal+boron+nitride+trenches.">Oriented graphene nanoribbons embedded in hexagonal boron nitride trenches.</a> Nature Communications. 8, (2017).</li><li>Fan, T. J., 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=Controllable+size-selective+method+to+prepare+graphene+quantum+dots+from+graphene+oxide.">Controllable size-selective method to prepare graphene quantum dots from graphene oxide.</a> Nanoscale Research Letters. 10, 1-8 (2015).</li><li>Oikonomou, 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=Scalable+bottom-up+assembly+of+suspended+carbon+nanotube+and+graphene+devices+by+dielectrophoresis.">Scalable bottom-up assembly of suspended carbon nanotube and graphene devices by dielectrophoresis.</a> Physica Status Solidi-Rapid Research Letters. 9 (9), 539-543 (2015).</li><li>Liu, Y., Zhang, D., Pang, S. W., Liu, Y. Y., Shang, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Size+separation+of+graphene+oxide+using+preparative+free-flow+electrophoresis.">Size separation of graphene oxide using preparative free-flow electrophoresis.</a> Journal of Separation Science. 38 (1), 157-163 (2015).</li><li>Cui, C. N., Huang, J. T., Huang, J. H., Chen, G. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Size+separation+of+mechanically+exfoliated+graphene+sheets+by+electrophoresis.">Size separation of mechanically exfoliated graphene sheets by electrophoresis.</a> Electrochimica Acta. 258, 793-799 (2017).</li><li>Sun, Z. 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=High-yield+exfoliation+of+graphite+in+acrylate+polymers:+A+stable+few-layer+graphene+nanofluid+with+enhanced+thermal+conductivity.">High-yield exfoliation of graphite in acrylate polymers: A stable few-layer graphene nanofluid with enhanced thermal conductivity.</a> Carbon. 64, 288-294 (2013).</li><li>Sun, Z. 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=Amine-based+solvents+for+exfoliating+graphite+to+graphene+outperform+the+dispersing+capacity+of+N-methyl-pyrrolidone+and+surfactants.">Amine-based solvents for exfoliating graphite to graphene outperform the dispersing capacity of N-methyl-pyrrolidone and surfactants.</a> Chemical Communications. 50 (72), 10382-10385 (2014).</li><li>Du, B. L., Jian, Q. F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Size+controllable+synthesis+of+graphene+water+nanofluid+with+enhanced+stability.">Size controllable synthesis of graphene water nanofluid with enhanced stability.</a> Fullerenes Nanotubes and Carbon Nanostructures. 27 (1), 87-96 (2019).</li><li>Tao, H. 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=Scalable+exfoliation+and+dispersion+of+two-dimensional+materials+-+an+update.">Scalable exfoliation and dispersion of two-dimensional materials - an update.</a> Physical Chemistry Chemical Physics. 19 (2), 921-960 (2017).</li><li>Phiri, J., Gane, P., Maloney, T. 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我们提出了一种将石墨烯纳米流体与可控的片状分布进行合成的方法。该方法结合了两个过程:去角质和离心。去角化控制纳米粒子的下尺寸限制,离心控制纳米粒子的上限。
尽管我们采用石墨的液相去角质来生产石墨烯纳米粒子,但应考虑对协议进行以下修改。应考虑其他去角质参数(例如转子速度、石墨浓度和其他表面活性剂的使用),以获得石墨烯纳米片的下尺寸限制。在离?...

传统的合成石墨烯纳米流体的方法通常使用声波来分散流体中的石墨烯粉末1,并且声波已被证明会改变石墨烯纳米粒子2的大小分布。 由于石墨烯的导热性取决于片状长度3,4,因此合成具有可控片状分布的石墨烯纳米流体对传热应用至关重要。受控离心已成功应用于液体去角质石墨烯分散体,将悬浮液分离成不同平均片数5、6的馏分。离心中使用的不同终端速度导致不同的临界沉降颗粒尺寸7。终端速度可用于消除大石墨烯纳米粒子8。
最近,通过液相去角质合成石墨烯的可控制尺寸的方法被引入,以克服传统方法9、10、11、9、10、11、9、10、11、9、10、11、9、10、11、9、10、11、9、10、11、9、1、9、11、9、11、9、1、1、1、9、1、9、9、1、9、1、1、9、1、9、1、1、 12,13.石墨的液相去角质已被证明是产生石墨烯悬浮液14、15、16的有效方法,其基础机制表明,工艺参数与石墨烯纳米颗粒尺寸分布的较低限制。石墨烯纳米流体是石墨的液体去角质在表面活性剂17的帮助下合成的。虽然石墨烯纳米颗粒尺寸分布的下限可以通过在去角质过程中调整参数来控制,但较少注意石墨烯纳米颗粒尺寸分布的上限。
这项工作的目的是开发一种可用于合成可控制片状分布的石墨烯纳米流体的协议。由于去角质只负责产生的石墨烯的下尺寸限制,因此引入了额外的离心,以控制生成的石墨烯的上限。然而,该方法并不特定于石墨烯,可能适用于不能使用传统方法合成的任何其他分层化合物。

<table>
	<tbody>
		<tr>
			<td>Beaker</td>
			<td>China Jiangsu Mingtai Education Equipments Co., Ltd.</td>
			<td>500 mL</td>
			<td></td>
		</tr>
		<tr>
			<td>Beaker</td>
			<td>China Jiangsu Mingtai Education Equipments Co., Ltd.</td>
			<td>5000 mL</td>
			<td></td>
		</tr>
		<tr>
			<td>Deionized water</td>
			<td>Guangzhou Yafei Water Treatment Equipment Co., Ltd.</td>
			<td></td>
			<td>analytical grade</td>
		</tr>
		<tr>
			<td>Electronic balance</td>
			<td>Shanghai Puchun Co., Ltd.</td>
			<td>JEa10001</td>
			<td></td>
		</tr>
		<tr>
			<td>Filter membrane</td>
			<td>China Tianjin Jinteng Experiment Equipments Co., Ltd.</td>
			<td>0.2 micron</td>
			<td></td>
		</tr>
		<tr>
			<td>Graphite powder</td>
			<td>Tianjin Dengke chemical reagent Co., Ltd.</td>
			<td></td>
			<td>analytical grade</td>
		</tr>
		<tr>
			<td>Hand gloves</td>
			<td>China Jiangsu Mingtai Education Equipments Co., Ltd.</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Laboratory shear mixer</td>
			<td>Shanghai Specimen and Model Factory</td>
			<td>jrj-300</td>
			<td></td>
		</tr>
		<tr>
			<td>Long neck flat bottom flask</td>
			<td>China Jiangsu Mingtai Education Equipments Co., Ltd.</td>
			<td>1000 ml</td>
			<td></td>
		</tr>
		<tr>
			<td>Nanoparticle analyzer</td>
			<td>HORIBA, Ltd.</td>
			<td>SZ-100Z</td>
			<td></td>
		</tr>
		<tr>
			<td>PVA</td>
			<td>Shanghai Yingjia Industrial Development Co., Ltd.</td>
			<td>1788</td>
			<td>analytical grade</td>
		</tr>
		<tr>
			<td>Raman spectrophotometer</td>
			<td>HORIBA, Ltd.</td>
			<td>Horiba LabRam 2</td>
			<td></td>
		</tr>
		<tr>
			<td>Scanning electron microscope</td>
			<td>Zeiss Co., Ltd.</td>
			<td>LEO1530VP</td>
			<td>SEM</td>
		</tr>
		<tr>
			<td>Surgical mask</td>
			<td>China Jiangsu Mingtai Education Equipments Co., Ltd.</td>
			<td>for one-time use</td>
			<td></td>
		</tr>
		<tr>
			<td>Thermal Gravimetric Analyzer</td>
			<td>German NETZSCH Co., Ltd.</td>
			<td>NETZSCH TG 209 F1 Libra</td>
			<td>TGA analysis</td>
		</tr>
		<tr>
			<td>Transmission electron microscope</td>
			<td>Japan Electron Optics Laboratory Co., Ltd.</td>
			<td>JEM-1400plus</td>
			<td>TEM</td>
		</tr>
		<tr>
			<td>UV-Vis spectrophotometer</td>
			<td>Agilent Technologies, Inc.+BB2:B18</td>
			<td>Varian Cary 60</td>
			<td></td>
		</tr>
	</tbody>
</table>
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synthesis of graphene nanofluids with controllable flake size distributions

提出了一种将石墨烯纳米流体与可控片状分布进行合成的方法。石墨烯纳米洛湖可以通过石墨在液相中的去角质获得,并且利用去角质时间来控制石墨烯南越湖尺寸分布的下限。离心成功地用于控制纳米颗粒大小分布的上限。这项工作的目的是结合去角质和离心,以控制石墨烯南越湖大小分布在由此产生的悬浮液。

石墨烯纳米片的存在可以通过各种特性技术进行验证。图 1显示了上述协议产生的各种片状分布的 UV-Vis 测量结果。波长为 270 nm 获得的光谱吸收峰是石墨烯片的证据。不同的吸收度对应于不同的浓度。观察到的最低吸收度对应于最高的离心速度。光谱强烈确认石墨烯的存在。
拉曼光谱的D波段和2D波段可用于确定石墨烯纳米的薄片厚度。?...

Watch this Scientific Journal Video about Synthesis of Graphene Nanofluids with Controllable Flake Size Distributions at JoVE.com

Synthesis of Graphene Nanofluids with Controllable Flake Size Distributions

提出了一种将石墨烯纳米流体与可控片状分布进行合成的方法。

具有可控片状分布的石墨烯纳米流体合成

A method for synthesizing graphene nanofluids with controllable flake size distributions is presented. Graphene nanoflakes can be obtained by the ...

该方法采用去角质工艺和离心工艺，分别控制所画悬浮液尺寸分布的下限和上限。该方法的主要优点是，通过调整去角质步和离心步法的工艺参数，可以控制最终尺寸分布。在干燥、清洁、平底的烧瓶中，加入20克PVA，然后加入1000毫升蒸馏水。轻轻旋转烧瓶，直到 PVA 完全溶解。然后将 50 克石墨粉末添加到平底烧瓶中，轻轻旋转烧瓶，直到石墨粉末完全分散在悬浮液中。将产生的悬浮液的 500 毫升转移到 500 毫升烧杯中。将烧杯放在剪切搅拌机下，将烧杯放在搅拌容器中心附近，以防止形成涡流。将混合头降至最低位置，从基平面降至 30 毫米。接下来，准备一个水浴，将5000毫升的烧杯装满室温水，并在浴缸中放置500毫升烧杯。启动搅拌机，并逐渐将转速提高至 4，500 rpm。以此速度混合 120 分钟。每30分钟换一次水。在不同持续时间内执行此去角质步骤五次。混合时间决定了石墨烯纳米片的横向尺寸限制。收集每个去角质步骤后产生的 500 毫升悬浮液。将每个悬浮液与分离时间标记，并在 140 次 g 下将收集的悬架离心机 45 分钟。要去除未离去的石墨，请使用移液器从每个离心管中收集上经剂的80%，以进一步离心。将上经式悬浮液从最后一个离心步骤中离以 8，951 次 g 离心 45 分钟。在离心管中收集上半占 50% 的上一代，并给样品贴上编号标签。然后，回收离心管底部的沉积物，将先前准备的PVA水试剂的50毫升加入沉淀物中，用手大力摇动管，直到沉淀物在悬浮液中充分分散。将悬架在 8，951 次 g 下离心 45 分钟。收集上部 80%以进行进一步测量。以四种不同的离心速度对颗粒重复四次离心步骤。离心速度决定了石墨烯纳米片的上部横向尺寸限制。现在，准备紫外线可见光谱。使用以前制备的干燥、清洁的样品单元中的 PVA 水溶液，校准紫外可见光谱仪，将 PVA 水浓度设置为 0%，然后将 PVA 水在离心后重新吸收添加到干燥、清洁的样品单元中，路径长度为 10 毫米，并使用制造商的软件获得读出。单击"获取"按钮获取测量结果图，并保存结果。接下来，为了确定石墨烯的重量，使用孔径为0.2微米的尼龙膜对样品悬浮液进行真空过滤。获得膜膜，用约200毫升的水洗入烧杯。重复洗涤三次，直到所有的固体被洗离膜。使用高精度微平衡确定洗涤水量，以获得固体的重量。同样，使用孔径为 0.2 微米的尼龙膜进行真空过滤水悬浮液。获得膜，并在室温下干燥超过12小时。随后，用200毫升的去维化水将薄膜冲洗到烧杯中。如果所需浓度低于每毫升一毫克的生产速率，则加入准备好的PVA水溶液以获得所需的浓度。如果所需浓度高于1%，在烘干机的真空下干燥脱化水24小时，以获得石墨烯纳米板。在此协议中，各种薄片尺寸分布的紫外可见度测量显示波长为270纳米的光谱吸收峰值，表明石墨烯片的证据。不同浓度的悬架具有不同的660纳米吸收。拉曼光谱的D波段和2D波段决定了石墨烯纳米片的薄片厚度。拉曼光谱的D波段与石墨烯sp3碳原子有关，区分初始石墨和石墨烯纳米片。低 D 波段强度表示无缺陷石墨烯纳米板。使用不同的离心速度准备的悬架观察到了独特的尺寸分布。透射电子显微镜和扫描电子显微镜均表明石墨烯的产生，去角质是成功的。然而，离心步骤只对平均直径大于1000纳米的纳米粒子起作用。应预先确定大小分布与离心速度的上限之间的关系。由于尺寸与建议的方法不一样，因此在中心某些连接、对流和传输应用等条件下，可以操纵传热效率。PVA聚合物对人体有害。应使用面罩和手套来保护操作员。

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的模板导演电浆黄金纳米管的合成与可调谐红外吸收

A nearly parallel array of pores can be produced by anodizing aluminum foils in acidic environments1, 2. Applications of anodic aluminum oxide (AAO) ...

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化学

A Simple Method for the Size Controlled Synthesis of Stable Oligomeric Clusters of Gold Nanoparticles under Ambient Conditions

根据环境条件的金纳米粒子的稳定低聚簇的大小控制合成的一种简便方法

Reducing dilute aqueous HAuCl4 with sodium thiocyanate (NaSCN) under alkaline conditions produces 2 to 3 nm diameter nanoparticles. Stable grape-like ...

Synthesis and Characterization of Fe-doped Aluminosilicate Nanotubes with Enhanced Electron Conductive Properties

以增强电子导电性能的合成与表征Fe掺杂碳纳米管硅铝的

The goal of the protocol is to synthesize Fe-doped aluminosilicate nanotubes of the imogolite type with the formula (OH)3Al2-xFexO3SiOH. Doping with Fe ...

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

化学沉淀法合成铌2O5改性高比表面积镍催化剂

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of ...

Preparation and Characterization of C60/Graphene Hybrid Nanostructures

Preparation and Characterization of C60/Graphene Hybrid Nanostructures

C 型60/石墨烯混合纳米结构的制备与表征

Physical thermal deposition in a high vacuum environment is a clean and controllable method for fabricating novel molecular nanostructures on graphene. We ...

Synthesis of Substrate-Bound Au Nanowires Via an Active Surface Growth Mechanism

通过活性表面生长机制合成基片束缚金纳米线

Advancing synthetic capabilities is important for the development of nanoscience and nanotechnology. The synthesis of nanowires has always been a ...

Synthesis and Structure Determination of &#181;-Conotoxin PIIIA Isomers with Different Disulfide Connectivities

不同二硫 Connectivities µ-芋螺毒素 PIIIA 异构体的合成与结构测定

Peptides with a high number of cysteines are usually influenced regarding the three-dimensional structure by their disulfide connectivity. It is thus ...

Preparation of Graphene-Supported Microwell Liquid Cells for In Situ Transmission Electron Microscopy

Preparation of Graphene-Supported Microwell Liquid Cells for In Situ Transmission Electron Microscopy

石墨烯支持的微井液体细胞制备,用于原位透射电子显微镜

The fabrication and preparation of graphene-supported microwell liquid cells (GSMLCs) for in situ electron microscopy is presented in a stepwise protocol. ...

Application of Voltage in Dynamic Light Scattering Particle Size Analysis

电压在动态光散射粒子尺寸分析中的应用

Dynamic light scattering (DLS) is a common method for characterizing the size distribution of polymers, proteins, and other nano- and microparticles. ...

Synthesis of Aptamer-PEI-g-PEG Modified Gold Nanoparticles Loaded with Doxorubicin for Targeted Drug Delivery

合成阿普塔默-PEI-g-PEG改性金纳米粒子装载多索鲁比辛用于靶向药物输送

Due to drug resistance and toxicity in healthy cells, use of doxorubicin (DOX) has been limited in clinical cancer therapy. This protocol describes the ...