Name: liquid-cell transmission electron microscopy for tracking self-assembly of nanoparticles
Uploaded: 2017-10-16T13:00:00
Description: Watch this Scientific Journal Video about Liquid-cell Transmission Electron Microscopy for Tracking Self-assembly of Nanoparticles at JoVE.com

役に立つ議論のためカリフォルニア大学の教授 a. ポール Alivisatos、バークレーとソウル国立大学教授 Taeghwan ヒョンに感謝しますこの作品は、IBS R006 D1 によって支えられました。W.C.L. は感謝、漢陽大学 (HY-2015-N) の研究基金から支援を認めています。

1 ナノ粒子合成 <ol><li>白金ナノ粒子の合成 <ol><li>アンモニウム hexachloroplatinate(IV) の結合 17.75 mg ((NH 4) 2 Pt (IV) Cl 6)、3.72 mg。tetrachloroplatinate(II) アンモニウム ((NH 4) 2 Pt (II) Cl 4)、テトラメチル アンモニウム ブロマイド、ポリビニルピロリドンの 109 mg 115.5 mg (MW: 29,000)、エチレング リコール 100 mL 3 首丸底フラスコに攪拌棒の 10 mlゴム...

<ol>
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白金ナノ粒子サイズは 7 nm アンモニウム ヘキサクロロ白金 (IV) 酸およびアンモニウム テトラクロロ白金 (II) 酸27 還元剤および溶媒として配位子とエチレング リコールとしてポリ (ビニルピロリドン) (PVP) を用いた還元による合成.オレイルアミンと配位子交換反応は、疎水性溶媒中の粒子を分散させるために行った。セレン ソース28 (29カ?...

自己集合コロイドナノ粒子系の興味の個々 のナノ粒子の11集団の物理的なプロパティにアクセスする機会を提供するため。揮発性溶剤6,7,8,の蒸着基板上のナノ粒子の自己組織化は、最も効果的な方法の 1 つ自己実用的なデバイス規模のアプリケーションで使用9,10,11. この溶媒蒸発法は蒸発速度などナノ粒子基板相互作用の変化速度論因子による大きな影響は、非平衡プロセス。ただし、推定し、動力学的要因を制御することは困難なので溶剤の蒸発による自己組織化ナノ粒子の機械的な理解は完全に成熟しません。その場x 線散乱法による研究はアンサンブル平均の情報を提供しているが、非平衡のナノ粒子の自己集合処理12,13,14、このテクニックのことはできません。個々 のナノ粒子の運動が決まります、全体的な軌道との関連付けを簡単にアクセスすることはできません。
液体セル TEM は個々 のナノ粒子の軌道を追跡するための新興ツール ナノ粒子運動の不均一性やアンサンブル動作15,16への貢献を理解する私たちを有効にします。 17,18,19,20,21,22,23,24,25、 26。溶媒の境界の動きが18基板上自己組織化ナノ粒子を誘導するための主要な原動力であることを示す溶媒蒸発中に個々 のナノ粒子の運動を追跡する液体セル電子顕微鏡を用いて以前,19します。 ここで、ナノ粒子の自己集合液体セル TEM を使用してのプロセスを観察することができます我々 の実験を紹介します。まず、プラチナの合成のためのプロトコルを提供し、TEM とナノ粒子を液体セルに読み込む方法の液体セルの作製手順を導入する前にセレン化ナノ粒子を導きます。代表的な結果として溶媒乾燥による自己組織化ナノ粒子の TEM 映画からのスナップショット ・ イメージを示します。これらの映画の中の個々 の粒子を追跡するシングルナノ粒子レベルで自己溶媒乾燥媒介の詳細な機構を理解できます。中に組み立て式、シリコン窒化ウィンドウで白金ナノ粒子は主に蒸発の溶媒フロントの動き溶剤の薄層に強い毛管力のため。同様の現象は他のナノ粒子 (セレン化鉛) の基板 (シリコン)、溶媒フロントの毛管力が、基板近傍粒子移行の重要な要因であることを示すも観察されました。

<table>
	<tbody>
		<tr>
			<td>ammonium hexachloroplatinate (IV)</td>
			<td>Sigma-Aldrich</td>
			<td>204021</td>
			<td></td>
		</tr>
		<tr>
			<td>ammonium tetrachloroplatinate (II)</td>
			<td>Sigma-Aldrich</td>
			<td>206105</td>
			<td></td>
		</tr>
		<tr>
			<td>tetramethylammonium bromide, 98%</td>
			<td>Sigma-Aldrich</td>
			<td>195758</td>
			<td></td>
		</tr>
		<tr>
			<td>poly(vinylpyrrolidone) powder</td>
			<td>Sigma-Aldrich</td>
			<td>234257</td>
			<td>Mw ~29,000</td>
		</tr>
		<tr>
			<td>ethylene glycol, anhydrous, 99.8%</td>
			<td>Sigma-Aldrich</td>
			<td>324558</td>
			<td></td>
		</tr>
		<tr>
			<td>n-hexane, anhydrous, 95%</td>
			<td>Samchun Chem.</td>
			<td>H0114</td>
			<td></td>
		</tr>
		<tr>
			<td>ethanol, anhydrous, 99.5%</td>
			<td>Sigma-Aldrich</td>
			<td>459836</td>
			<td></td>
		</tr>
		<tr>
			<td>oleylamine, 70%</td>
			<td>Sigma-Aldrich</td>
			<td>O7805</td>
			<td>Technical grade</td>
		</tr>
		<tr>
			<td>lead(II) acetate trihydrate, 99.99%</td>
			<td>Sigma-Aldrich</td>
			<td>467863</td>
			<td></td>
		</tr>
		<tr>
			<td>oleic acid, 90%</td>
			<td>Sigma-Aldrich</td>
			<td>364525</td>
			<td>Technical grade</td>
		</tr>
		<tr>
			<td>diphenyl ether, 99%</td>
			<td>Sigma-Aldrich</td>
			<td>P24101</td>
			<td>ReagentPlus</td>
		</tr>
		<tr>
			<td>selenium powder, 99.99%</td>
			<td>Sigma-Aldrich</td>
			<td>229865</td>
			<td></td>
		</tr>
		<tr>
			<td>tri-n-octylphosphine, 97%</td>
			<td>Strem</td>
			<td>15-6655</td>
			<td>Air sensistive</td>
		</tr>
		<tr>
			<td>Toluene, anhydrous, 99.9%</td>
			<td>Samchun Chem.</td>
			<td>T2419</td>
			<td></td>
		</tr>
		<tr>
			<td>acetone 99.8%</td>
			<td>Daejung Chem.</td>
			<td>1009-2304</td>
			<td></td>
		</tr>
		<tr>
			<td>potassium hydroxide, 95%</td>
			<td>Samchun Chem.</td>
			<td>P0925</td>
			<td></td>
		</tr>
		<tr>
			<td>p-type silicon-on-insulator wafers</td>
			<td>Soitec</td>
			<td>Power-SOI</td>
			<td>for liquid cells with silicon windows</td>
		</tr>
		<tr>
			<td>tetramethylammonium hydroxide, 25% in H2O</td>
			<td>J.T.Baker</td>
			<td>02-002-109</td>
			<td></td>
		</tr>
		<tr>
			<td>AZ 5214 E</td>
			<td>AZ Electronic Materials</td>
			<td>AZ 5214 E</td>
			<td>Positive photorest</td>
		</tr>
		<tr>
			<td>AZ-327</td>
			<td>AZ Electronic Materials</td>
			<td>AZ-327</td>
			<td>AZ 5214 develper</td>
		</tr>
		<tr>
			<td>indium pellets 99.98-99.99%</td>
			<td>Kurt J. Lesker Company</td>
			<td>EVMIN40EXEB</td>
			<td>thermal evaporator target</td>
		</tr>
		<tr>
			<td>1,2-dichlorobenzene, &#62;99%</td>
			<td>TCI</td>
			<td>D1116</td>
			<td></td>
		</tr>
		<tr>
			<td>pentadecane, &#62;99%</td>
			<td>Sigma-Aldrich</td>
			<td>P3406</td>
			<td></td>
		</tr>
		<tr>
			<td>buffered oxide etch 7:1</td>
			<td>microchemicals</td>
			<td>BOE 7-1 VLSI</td>
			<td></td>
		</tr>
		<tr>
			<td>phosphoric acid, 85%</td>
			<td>Samchun Chem.</td>
			<td>P0449</td>
			<td></td>
		</tr>
	</tbody>
</table>

liquid-cell transmission electron microscopy for tracking self-assembly of nanoparticles

ナノ粒子の自己組織化構造を作成する汎用性の高い方法は、ナノ粒子の分散を乾燥が、このプロセスのメカニズムが十分に理解されていません。我々 は、液晶セルの透過型電子顕微鏡 (TEM) を使用してアセンブリ プロセスのメカニズムを調査する個々 のナノ粒子の軌跡を追跡しています。ここで、液体セル TEM 研究で使用するプロトコルを提案する、自己組織化。まず、セレン化ナノ粒子になり、均一に大きさで分類されたプラチナを生成に使用される詳細な合成プロトコルを紹介します。次に、窒化ケイ素やシリコン windows 液体セルを生成し、読み込みと画像検査液細胞の電子顕微鏡技術の手順を説明するために使用する微細加工プロセスを提案します。いくつかのノートは壊れやすい細胞ウィンドウを管理する方法など、全体のプロセスのための有用なヒントを提供するために含まれます。液体セル TEM によって追跡されるナノ粒子の個々 の運動では、蒸発による溶剤の境界の変更は、ナノ粒子の自己組織化プロセスの影響を受けることを明らかにしました。溶媒の境界は、主に非晶質集合体を形成、2 次元 (2 D) 自己組織化構造を生成する集計の平坦化の順にナノ粒子を運転しました。これらの動作は、種類の異なるナノ粒子と液体細胞組成の異なるも観察されます。

液体セルは 25 の厚さによる電子ビームに透明シリコン窒化 windows に装備されている上チップと下チップから成る nm。上部のチップ試料溶液及び蒸発の溶媒を格納するための貯留しています。チップは、従来の微細加工処理25を介して行われます。上部と下部のチップ用マスクが図 1 aに示されていると1 b</strong...

Watch this Scientific Journal Video about Liquid-cell Transmission Electron Microscopy for Tracking Self-assembly of Nanoparticles at JoVE.com

Liquid-cell Transmission Electron Microscopy for Tracking Self-assembly of Nanoparticles

ナノ粒子の自己集合の追跡のため液晶セルの透過電子顕微鏡観察

ここで紹介する自己組織化プロセスのリアルタイム観測のための実験プロトコル液晶セルの透過型電子顕微鏡を用いたします。

Drying a nanoparticle dispersion is a versatile way to create self-assembled structures of nanoparticles, but the mechanism of this process is not fully ...

The overall goal of this procedure is to use liquid-cell transmission electron microscropy to investigate the motion of nanoparticles in the solution phase in real time. This method can help answer key questions in the field of nanoscience, for example, about how nanoparticles form self-assembled structures during solvent drying. The main advantage of this technique is that it makes checking nanoparticle motion in real space and real time possible.The implications of this liquid cell technique is tends towards tracking individual motions of nanoparticles that are not shown by conventional methods. Though this method can provide insight into self-assembly of nanoparticles it can be also applied into other models such as oriented attachment of nanoparticles. To begin the procedure, place in a 100 milliliter three neck round bottom flask 17.75 milligrams of ammonium hexacholoroplatinate, 3.72 milligrams of ammonium tetrachloroplatinate and 115.5 milligrams of tetramethylammonium bromide.Add to the flask 109 milligrams of polyvinylpyrrolidone and 10 milliliters of anhydrous ethylene glycol. Equip the flask with a stir bar, a rubber septum and a reflux condenser. Start the stir motor and while stirring at 1000 rpm, degas the reaction flask under vacuum for one hour.Then, under a flow of argon, heat the reaction mixture to 180 degrees Celsius at 10 degrees per minute. Stir the mixture at 180 degrees Celsius for 20 minutes then allow the mixture to cool to room temperature. Transfer the cooled mixture to a 50 milliliter centrifuge tube.Add to the tube 30 milliliters of acetone to precipitate the platinum nanoparticles. Centrifuge the mixture at 2400 times G for 10 minutes. Discard the supernatant and disperse the precipitate in 10 milliliters of ethanol.Obtain a four inch 100 micron silicon wafer coated with about 25 nanometers of silicon nitride. Load photo resist using a spin coater. Then use photo resist to mount the ultra thin wafer on a 500 micron thick silicon wafer.Spin coat the wafer with 10 milliliters of positive photo resist at 3000 rpm for 30 seconds. Bake the wafer at 85 degrees Celsius for 60 seconds. Then cover the wafer with a chromium mask and expose the wafer to 365 nanometer light for 10 seconds.Immerse the wafer in 50 milliliters of the appropriate developer solution for 40 seconds and then in 50 milliliters of deionized water for one minute. Immerse the wafer in 50 milliliters of deionized water for one minute, then place the patterned wafer in a reactive ion etcher. Etch the exposed silicon nitride for one minute.Use a water bath to evenly heat a container of a 30 milligram per liter aqueous solution of potassium hydroxide to 85 degrees Celsius. Soak the ultra thin wafer in the hot potassium hydroxide for two hours to etch the exposed silicon. When the exposed silicon appears to have been completely etched away, carefully remove the wafer from the solution at an angle to avoid rupturing the silicon nitride window.Repeat this process with the second chromium mask to obtain the top and bottom chips. Use the third chromium mask to pattern indium spacers onto the bottom chip. Align the top and bottom chips and bond the chips together at 100 degrees Celsius.Transfer 20 microliters of the prepared nanoparticle dispersion to a five milliliter vial. Allow the solvent to evaporate under ambient conditions for 10 minutes. Inspect the liquid cell under an optical microscope to verify that the silicon nitride windows are intact.Then disperse the nanoparticles in a mixture of one milliliter of orthodichlorobenzene, 250 microliters of pentadecane and 10 microliters of oleylamine. With the liquid cell under the optical microscope use an injector with an ultra thin capillary to load 100 nanoliters of the dispersion into the liquid cell reservoirs. Use filter paper to absorb the excess dispersion outside the reservoirs.Allow the cell to sit in ambient air for 10 minutes to evaporate the orthodichlorobenzene. Then apply vacuum grease to one side of a two millimeter copper aperture grid with a 600 micron hole. Carefully cover the liquid cell with the grid, being careful to align the aperture with the liquid cell window.Mount the cell in a standard TEM holder and load the cell into the instrument. Acquire images in continuous image acquisition mode as the solvent dries. Use image processing software to calculate the radial distribution function for the particles in each acquired image.TEM images of a platinum nanoparticle suspension drying in a silicon nitride liquid cell showed the nanoparticles being pulled inward by the receding solvent front. This behavior was attributed to the strong capillary forces of the thin layer of solvent and the reduced free energy of the nanoparticles at the solvent interface. The nanoparticles initially formed amorphous multilayer agglomerates as they were drawn together.As the solvent dried, the agglomerates flattened into an ordered monolayer. This ordering is reflected in the radial distribution functions derived from the TEM images. The radial distribution function of the image taken after 90 seconds had a large peak at 8.3 nanometers.The oleylamine capped platinum nanoparticles are about 8.3 nanometers in diameter, suggesting that a significant number of particles were assembled as closely as possible. Once mastered, this technique can be done in two days if it is performed properly. Generally individuals who are new to this method may struggle because fabricating and working with the liquid cell require different levels of optimization for different nanoparticles or liquid cell compositions.While attempting this procedure, remember to protect the windows of the liquid cell from breaking. Following this procedure, other methods like applying voltages to the liquid cell can be performed to answer additional questions about the self-assembly of nanoparticles in the presence of external forces. After its development, this technique paved the way for researchers in the field of nanoscience to explore the assembly process of nanoparticles in the overall dry mechanism.After watching this video, you should have a good understanding of how to prepare liquid cells and measure the motions of nanoparticles in TEM experiment. Don't forget that working with KUH agent can be extremely hazardous. Precautions such as wearing safety glasses should always be taken while performing this experiment.

Research

JoVE Journal

Chemistry

Origami Inspired Self-assembly of Patterned and Reconfigurable Particles

折り紙インスパイアパターン化され、再構成可能な粒子の自己組織化

There are numerous techniques such as photolithography, electron-beam lithography and soft-lithography that can be used to precisely pattern two ...

化学

Formation of Ordered Biomolecular Structures by the Self-assembly of Short Peptides

短いペプチドの自己組織化によって順序付け生体分子構造の形成

In nature, complex functional structures are formed by the self-assembly of biomolecules under mild conditions. Understanding the forces that control ...

Self-assembly of Complex Two-dimensional Shapes from Single-stranded DNA Tiles

一本鎖DNAタイルから複雑な2次元形状の自己集合

Current methods in DNA nano-architecture have successfully engineered a variety of 2D and 3D structures using principles of self-assembly. In this ...

Obtaining 3D Chemical Maps by Energy Filtered Transmission Electron Microscopy Tomography

エネルギー化学 3 D マップの取得フィルター透過電子顕微鏡トモグラフィー

Energy filtered transmission electron microscopy tomography (EFTEM tomography) can provide three-dimensional (3D) chemical maps of materials at a ...

Analysis of Minerals Produced by hFOB 1.19 and Saos-2 Cells Using Transmission Electron Microscopy with Energy Dispersive X-ray Microanalysis

HFOB 1.19 によって生成される鉱物と Sao 2 セルを使用して透過型電子顕微鏡エネルギー分散型 x 線微小分析での分析

This video presents the use of transmission electron microscopy with energy dispersive X-ray microanalysis (TEM-EDX) to compare the state of minerals in ...

Using Graphene Liquid Cell Transmission Electron Microscopy to Study in Situ Nanocrystal Etching

Using Graphene Liquid Cell Transmission Electron Microscopy to Study in Situ Nanocrystal Etching

グラフェン液セル透過型電子顕微鏡を使用してナノ結晶エッチングその場を研究するには

Graphene liquid cell electron microscopy provides the ability to observe nanoscale chemical transformations and dynamics as the reactions are occurring in ...

Performing Spectroscopy on Plasmonic Nanoparticles with Transmission-Based Nomarski-Type Differential Interference Contrast Microscopy

トランスミッションベースのノマルスキー型差動干渉造影顕微鏡を用いたプラズモニックナノ粒子の分光法の実行

Differential interference contrast (DIC) microscopy is a powerful imaging tool that is most commonly employed for imaging microscale objects using ...

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

その中透過電子顕微鏡におけるグラフェン支持マイクロウェル液体細胞の調製

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

Synthesis of Monodisperse Cylindrical Nanoparticles via Crystallization-driven Self-assembly of Biodegradable Block Copolymers

生分解性ブロック共重合体の結晶化駆動自己組織化による単分散円筒ナノ粒子の合成

The production of monodisperse cylindrical micelles is a significant challenge in polymer chemistry. Most cylindrical constructs formed from diblock ...

Self-Assembly of Hybrid Lipid Membranes Doped with Hydrophobic Organic Molecules at the Water/Air Interface

水/空気界面で疎水性有機分子をドープしたハイブリッド脂質膜の自己集合

Because of their unique properties, including an ultrathin thickness (3-4 nm), ultrahigh resistivity, fluidity and self-assembly ability, lipid bilayers ...