The authors would like to thank R&#252;diger Rosenkranz and Sven Niese (Fraunhofer IKTS-MD) for their assistance in sample preparation, and Ude Hangen, Douglas Stauffer, Ryan Major and Oden Warren (Hysitron Inc.) for their technical support on the PI95 TEM holder. The support of the Center for Advancing Electronics Dresden (cfaed) and the Dresden Center for Nanoanalysis (DCN) at Technische Universit&#228;t Dresden is acknowledged as well.

1.集束イオンビーム（FIB）間伐（図1）のためのサンプルの準備<ol><li> （〜10ミリメートルで10 mm）のダイヤモンドスクライブとを小さなチップに完全なウェハを切断します。 </li><li>チップ上の「チップ·ツー·チップ」構造の位置をマークします。 </li><li> 2mmの大きさで60μmのバーを得るために、ダイシング装置でチップを見ました。バーでは、中心部にある「先端間」構造を含みます。 </li><li>スーパー接着剤を使用して銅の半分リング上のターゲットバーを接着。次に、スーパー接着剤を使用しても銅試料ステージ上のバーを接着。そして、銀はハーフリングと銅試料ステージとの導通を設定するために貼り付けて使用します。 注：サンプルを取り扱う際は、常にサンプルに敏感な構造に損傷を与える可能性が静電放電を防ぐために、静電気防止用リストストラップを着用してください。 </li></ol>走査型電子顕微鏡で2 FIB間伐（図2） <ol><li>上のステップ1で得られた試​​料を入れてnは、SEM試料台とSEMに慎重に段階を置きます。 </li><li>堆積モードを選び、必要な白金保護層の寸法（面積や厚さ）を設定。常に最高の精度を維持するために、30 kVのイオンビームを使用しています。必要なPt層の寸法に依存チューン満足効率を得るために、現在、。 <ol><li>銅ステージ（接地電位）に一つのパッドに接触するように白金線を堆積。次に、FIBの間引き処理中のイオンダメージを最小限に抑えるために、薄型ラメラを強化することが非常に重要である「チップ·ツー·チップ」構造の上に厚さのPt層を堆積させます。これは、FIBの調製に使用される標準的な手順です。 </li><li> Ptの堆積を行う際にPt層を介して「先端間」構造の上部にある2つのパッド間の任意の導電性パスを導入しない注意してください。任意の導電性パスが短い電気回路（ 図2AおよびB）になります。 </li></ol></li><li> FIBミリング<ol><li>最終的なカットのための10のPA 30キロボルトの電圧と電流を使用してください。 150と180 nmの厚さのHバーTEMラメラに薄いターゲットバー。 </li><li> TEMでトランスデューサ先端が触れるますパッド（V +パッド）の近くにノッチをカット。 TEMで正しいパッドを識別するためのマーカーとしてのノッチを使用してください。 </li></ol></li></ol> TEMのSEMから3.サンプルトランスファー<ol><li>サンプルに触れる前に、静電気防止用リストストラップを着ました。 </li><li> SEM段階から準備されたH-バーサンプルのマウントを解除します。 SEMからそれを除去する際のCuステージ上にサンプルを保管してください。 </li><li> TEMホルダーにCuの段階を修正しました。光学顕微鏡で試験構造に近いTEMホルダー（離れたテスト構造からマイクロメートルの数百）の変換器先端を移動します。 <ol><li>慎重にTEMにTEMホルダーを挿入します。 TR中の任意の洗浄処理（ 例えば 、プラズマ洗浄）を利用しないでくださいansferプロセス、そうでない場合はラメラが影響を受ける可能性があります。 </li></ol></li><li>周囲の水分や酸素にあまりにも多くの露出を避けるために、15分またはより短い内にサンプル移送のための時間をおいてください。 </li></ol> 4.電気的に接続する（図3） <ol><li>その制御システムおよびソースメータにTEMホルダーを接続します。そして、制御システムとソースメータをオンにします。 </li><li> TEMホルダにノブを調整することによって、テスト構造にトランスデューサ先端の粗いアプローチをしているときに、TEMトランスデューサチップを監視します。 <ol><li> （500nmの≤）のV +パッドに近いTEMホルダーのトランスデューサ先端を移動します。パッドとして：同じレベル（高さZ）への変換器チップを持参してください。曲先端の位置と先端がV +パッドの中心に直面します。 </li></ol></li><li> V +パッドにトランスデューサチップにお問い合わせください。パッドに近づいている間（約1 Vまで0.5 V）先端に非常に低い電圧を設定します。現在simultaneoを監視usly接触が確立されることを確認します。 </li></ol> その場 TDDB実験5. <ol><li> TEMで200キロボルトの加速電圧を使用してください。関心のある領域に電子ビームを移動します。適切な倍率を選択し、画像の焦点を合わせます。 </li><li>低照度の手順を実行します（≤8）試験構造上のビームダメージを低減します。のみH-バーサンプルの薄い部分内の照明領域をローカライズするためにコンデンサー絞りを使用してください。 </li><li> その場での TEM画像（2-3フレーム/秒）を記録しながら、ソースメータを使用して「先端間」構造に一定の電圧（≤40 V）を適用します。 DigitalMicrographソフトウェアを使用して、例えば 、自己のスクリプトコードを使用して自動的に画像を記録します。 </li><li> ULK誘電体への金属の見かけの拡散を見ると、実験を一時停止し、電子分光イメージング（ESI）、化学分析を行います。 <ol><li> OMEGにフィルタスリット開口を挿入TEMでのエネルギーフィルタ。 </li><li>チューニングフィルタシルト開口の幅は、電子エネルギー損失スペクトル（EELS）で適切なエネルギー幅（10~20 eVの）を取得します。 </li><li> EELSにおける銅M-エッジ吸着ピークにエネルギーをシフトします。 </li><li>銅M-エッジ吸収ピークのエネルギーフィルタ処理TEM画像を取得するために戻って撮影モードに戻ります。 </li><li>銅Mエッジの前縁部にエネルギーをシフトし、別のエネルギーフィルタ処理TEM像を得ます。 </li><li>二つの画像間の試料のドリフトを修正してください。 </li><li>銅のジャンプ比画像を取得するために、第2のいずれかで最初の画像を分割します。 </li></ol></li><li> TDDB実験を続行：ソースメータを使用して「先端間」構造に一定の電圧（≤40 V）を再適用し、TEM像を記録します。 </li></ol> 6.コンピュータ断層撮影<ol><li> TDDB実験が終了したTEMコンピュータ断層撮影を行い、ディ約3次元分布情報を取得しますffused粒子。 </li><li>サンプルを傾けて、138°のチルトシリーズを記録します。 1°の傾斜ステップを使用し、明視野（BF）STEMモードでのすべてのステップの間に画像を記録。 </li><li> （画像を整列させる傾斜軸を決定し、3次元断層ボリュームを形成するために、ボリュームとセグメンテーションを再構成含む）のシリーズを再構築します。 </li></ol>

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No competing financial interests.

TDDB実験の成功の前提条件は、特にSEMでFIBミリングプロセスにおいて、良好なサンプル調製です。まず、「チップ·ツー·チップ」構造の上に厚さのPt層を堆積する必要があります。厚さ及びPt層のサイズは、SEMオペレータによって調整が、3つの原則に従わなければならないことができる：（1）厚さや大きさは、全体の微粉砕処理中に可能なイオンビームダメージから対象領域を保護するのに?...

Cu配線は、まず1997年1において、超大規模集積回路（ULSI）技術を導入したので、低誘電率及び超低k（ULK）誘電体は、バックエンド·オブ·ライン（BEOL）に採用されていますオンチップ配線間の絶縁材料として。新しい材料の組み合わせ、 例えば、より低い静電容量のための低抵抗化と低k / ULK誘電体のためのCuは、増加した抵抗-容量（RC）の効果は、配線寸法収縮2,3による遅延克服する。しかし、この利点は、侵食されました近年のマイクロ電子デバイスの継続的な積極的なスケーリングによる。製造プロセス及び製品の信頼性のために様々な課題で低k / ULK材料の結果を使用することは、配線ピッチが約100nm 4-6以下になる場合は特に。 TDDBは、時間の関数としての誘電体材料の物理的な故障メカニズムを指し電界下。 TDDB信頼性試験は、通常、加速条件（昇電界および/または高温）下で行われます。 オンチップの相互接続スタックにおけるTDDBは既に信頼性のコミュニティに強い懸念を表明したマイクロ電子デバイスのための最も重要な故障メカニズムの一つです。でも、弱い電気的および機械的特性を有するULK誘電体は、高度な技術ノードにあるデバイスに統合されているので、それは信頼性技術者のスポットライトであり続けるでしょう。 専用の実験は、TDDBの故障メカニズム7-9を調査するために行われており、労力のかなりの量は、デバイス10〜13の電界と寿命との関係を説明するモデルを開発するために投資されています。既存の研究では、マイクロエレクト​​ロニクスにおける信頼性技術者のコミュニティに利益をもたらします。しかし、多くのチャレンジVol。GESは依然として存在し、多くの疑問がまだ詳細に回答する必要があります。たとえば、実績のあるモデルは、TDDB法で物理的な障害のメカニズムと劣化速度を説明し、それぞれの実験的な検証がまだ不足しています。特に必要として、より適切なモデルが保守的√Eモデル14を代入するために必要とされます。 TDDB調査の非常に重要な部分として、典型的な故障解析は故障メカニズムと分解速度の物理学を説明するための包括的かつ確かな証拠を提供する、 すなわち 、前例のない課題に直面しています。それは非常に時間がかかるので、明らかに、一つ一つのナノスケールのCu配線のビア及びメートルの何百万人を検査し、 元が障害部位を画像インサイチュするには 、この課題のハードルに適切な選択ではなく、損傷機構の動力学についての限られた情報しか提供することができます。このため、緊急の課題は開発に浮上していますND実験を最適化し、TDDBの故障メカニズムと分解速度を研究するために、より良い手順を取得します。 本稿では、 その場実験方法における Cu / ULK配線スタック内のTDDBの故障メカニズムを調査するためにデモンストレーションを行います。高品質イメージングおよび化学分析の能力を持つTEMは、専用のテスト構造における動プロセスを研究するために使用されます。 その場で電気試験における誘電体に高められた電界を提供するために、TEM実験に統合されています。カスタマイズされた「先端間」構造、完全にカプセル化されたCu配線からなり、ULK材料で絶縁、32 nmのCMOS技術ノードに設計されています。ここに記載の実験手順は、能動素子の他の構造体に拡張することができます。

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>Automatic Dicing Saw</td>
			<td>DISCO Kiru-Kezuru-Migaku Technologies</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Scanning Electron Microscope</td>
			<td>Zeiss</td>
			<td>Zeiss Nvision 40</td>
			<td></td>
		</tr>
		<tr>
			<td>Picoindentor</td>
			<td>Hysitron</td>
			<td>Hysitron Pi95</td>
			<td></td>
		</tr>
		<tr>
			<td>Keithley SourceMeter</td>
			<td>Keithley</td>
			<td>Keithley 2602/237</td>
			<td></td>
		</tr>
		<tr>
			<td>Transmission Electron Microscope</td>
			<td>FEI</td>
			<td>FEI Tecnai F20</td>
			<td></td>
		</tr>
		<tr>
			<td>Transmission Electron Microscope</td>
			<td>Zeiss</td>
			<td>Zeiss Libra 200</td>
			<td></td>
		</tr>
	</tbody>
</table>

in situ time-dependent dielectric breakdown in the transmission electron microscope: a possibility to understand the failure mechanism in microelectronic devices

The time-dependent dielectric breakdown (TDDB) in on-chip interconnect stacks is one of the most critical failure mechanisms for microelectronic devices. The aggressive scaling of feature sizes, both on devices and interconnects, leads to serious challenges to ensure the required product reliability. Standard reliability tests and post-mortem failure analysis provide only limited information about the physics of failure mechanisms and degradation kinetics. Therefore it is necessary to develop new experimental approaches and procedures to study the TDDB failure mechanisms and degradation kinetics in particular. In this paper, an in situ experimental methodology in the transmission electron microscope (TEM) is demonstrated to investigate the TDDB degradation and failure mechanisms in Cu/ULK interconnect stacks. High quality imaging and chemical analysis are used to study the kinetic process. The in situ electrical test is integrated into the TEM to provide an elevated electrical field to the dielectrics. Electron tomography is utilized to characterize the directed Cu diffusion in the insulating dielectrics. This experimental procedure opens a possibility to study the failure mechanism in interconnect stacks of microelectronic products, and it could also be extended to other structures in active devices.

図4は、 その場での試験での明視野（BF）のTEM像を示します。部分的に起因する雰囲気で、拡張ストレージに電気試験（ 図4A）の前にULK誘電体中でのTaN / Taの障壁と、既存のCu原子に違反があります。 40 Vでの唯一の376秒後に、絶縁破壊が開始され、M1金属からの銅の二つの主要な移行経路を伴った、グランド側15-16を参照して、正の電位を有しま?...

Watch this Scientific Journal Video about In Situ Time-dependent Dielectric Breakdown in the Transmission Electron Microscope: A Possibility to Understand the Failure Mechanism in Microelectronic Devi

In Situ Time-dependent Dielectric Breakdown in the Transmission Electron Microscope: A Possibility to Understand the Failure Mechanism in Microelectronic Devices

The time-dependent dielectric breakdown (TDDB) in on-chip interconnect stacks is one of the most critical failure mechanisms for microelectronic devices. This paper demonstrates the procedure of an in situ TDDB experiment in the transmission electron microscope, which opens a possibility to study the failure mechanism in microelectronic products.

その場での透過型電子顕微鏡での時間依存絶縁破壊：マイクロエレクトロニクスデバイスの故障メカニズムを理解することが可能

The time-dependent dielectric breakdown (TDDB) in on-chip interconnect stacks is one of the most critical failure mechanisms for microelectronic devices. ...

in-situ-time-dependent-dielectric-breakdown-transmission-electron

Research

JoVE Journal

Engineering

In Situ Time-dependent Dielectric Breakdown in the Transmission Electron Microscope: A Possibility to Understand the Failure Mechanism in Microelectronic Devices

8.6K ビュー.  Fraunhofer Institute for Ceramic Technologies and Systems. The time-dependent dielectric breakdown (TDDB) in on-chip interconnect stacks is one of the most critical failure mechanisms for microelectronic devices. This paper demonstrates the procedure of an in situ TDDB experiment in the transmission electron microscope, which opens a possibility to study the failure mechanism in microelectronic products. 

ビデオ: In Situ Time-dependent Dielectric Breakdown in the Transmission Electron Microscope: A Possibility to Understand the Failure Mechanism in Microelectronic Devices

Revealing Dynamic Processes of Materials in Liquids Using Liquid Cell Transmission Electron Microscopy

The recent development for in situ transmission electron microscopy, which allows imaging through liquids with high spatial resolution, has attracted significant interests across the research fields of materials science, physics, chemistry and biology. The key enabling technology is a liquid cell. We fabricate liquid cells with thin viewing windows through a sequential microfabrication process, including silicon nitride membrane deposition, photolithographic patterning, wafer etching, cell bonding, etc. A liquid cell with the dimensions of a regular TEM grid can fit in any standard TEM sample holder. About 100 nanoliters reaction solution is loaded into the reservoirs and about 30 picoliters liquid is drawn into the viewing windows by capillary force. Subsequently, the cell is sealed and loaded into a microscope for in situ imaging. Inside the TEM, the electron beam goes through the thin liquid layer sandwiched between two silicon nitride membranes. Dynamic processes of nanoparticles in liquids, such as nucleation and growth of nanocrystals, diffusion and assembly of nanoparticles, etc., have been imaged in real time with sub-nanometer resolution. We have also applied this method to other research areas, e.g., imaging proteins in water. Liquid cell TEM is poised to play a major role in revealing dynamic processes of materials in their working environments. It may also bring high impact in the study of biological processes in their native environment.

We have developed a self-contained liquid cell, which allows imaging through liquids using a transmission electron microscope. Dynamic processes of nanoparticles in liquids can be revealed in real time with sub-nanometer resolution.

液晶セルの透過型電子顕微鏡を使用して液体の材料の動的過程を明らかにする

The recent development for in situ transmission electron microscopy, which allows imaging through liquids with high spatial resolution, has attracted ...

工学

Detection and Recovery of Palladium, Gold and Cobalt Metals from the Urban Mine Using Novel Sensors/Adsorbents Designated with Nanoscale Wagon-wheel-shaped Pores

Developing low-cost, efficient processes for recovering and recycling palladium, gold and cobalt metals from urban mine remains a significant challenge in industrialized countries. Here, the development of optical mesosensors/adsorbents (MSAs) for efficient recognition and selective recovery of Pd(II), Au(III), and Co(II) from urban mine was achieved. A simple, general method for preparing MSAs based on using high-order mesoporous monolithic scaffolds was described. Hierarchical cubic Ia3d wagon-wheel-shaped MSAs were fabricated by anchoring chelating agents (colorants) into three-dimensional pores and micrometric particle surfaces of the mesoporous monolithic scaffolds. Findings show, for the first time, evidence of controlled optical recognition of Pd(II), Au(III), and Co(II) ions and a highly selective system for recovery of Pd(II) ions (up to ~95%) in ores and industrial wastes. Furthermore, the controlled assessment processes described herein involve evaluation of intrinsic properties (e.g., visual signal change, long-term stability, adsorption efficiency, extraordinary sensitivity, selectivity, and reusability); thus, expensive, sophisticated instruments are not required. Results show evidence that MSAs will attract worldwide attention as a promising technological means of recovering and recycling palladium, gold and cobalt metals.

Because of the importance and extensive use of palladium, gold and cobalt metals in high-technology equipment, their recovery and recycling constitute an important industrial challenge. The metal recovery system described herein is a simple, low-cost means for the effective detection, removal, and recovery of these metals from the urban mine.

検出とパラジウムの回収は、都市鉱山からの金やコバルト金属は、ナノスケールワゴンホイール形の細孔を有する指定小説センサ/吸着剤を使用しました

Developing low-cost, efficient processes for recovering and recycling palladium, gold and cobalt metals from urban mine remains a significant challenge in ...

Using Synchrotron Radiation Microtomography to Investigate Multi-scale Three-dimensional Microelectronic Packages

Synchrotron radiation micro-tomography (SR&#181;T) is a non-destructive three-dimensional (3D) imaging technique that offers high flux for fast data acquisition times with high spatial resolution. In the electronics industry there is serious interest in performing failure analysis on 3D microelectronic packages, many which contain multiple levels of high-density interconnections. Often in tomography there is a trade-off between image resolution and the volume of a sample that can be imaged. This inverse relationship limits the usefulness of conventional computed tomography (CT) systems since a microelectronic package is often large in cross sectional area 100-3,600 mm2, but has important features on the micron scale. The micro-tomography beamline at the Advanced Light Source (ALS), in Berkeley, CA USA, has a setup which is adaptable and can be tailored to a sample&#39;s properties, i.e., density, thickness, etc., with a maximum allowable cross-section of 36 x 36 mm. This setup also has the option of being either monochromatic in the energy range ~7-43 keV or operating with maximum flux in white light mode using a polychromatic beam. Presented here are details of the experimental steps taken to image an entire 16 x 16 mm system within a package, in order to obtain 3D images of the system with a spatial resolution of 8.7 &#181;m all within a scan time of less than 3 min. Also shown are results from packages scanned in different orientations and a sectioned package for higher resolution imaging. In contrast a conventional CT system would take hours to record data with potentially poorer resolution. Indeed, the ratio of field-of-view to throughput time is much higher when using the synchrotron radiation tomography setup. The description below of the experimental setup can be implemented and adapted for use with many other multi-materials.

For this study synchrotron radiation micro-tomography, a non-destructive three-dimensional imaging technique, is employed to investigate an entire microelectronic package with a cross-sectional area of 16 x 16 mm. Due to the synchrotron&#39;s high flux and brightness the sample was imaged in just 3 min&#160;with an 8.7 &#181;m spatial resolution.

マルチスケール三次元マイクロエレクト​​ロニクスパッケージを調査するために放射光マイクロトモグラフィーを用いて、

Synchrotron radiation micro-tomography (SR&#181;T) is a non-destructive three-dimensional (3D) imaging technique that offers high flux for fast data ...

Comprehensive Characterization of Extended Defects in Semiconductor Materials by a Scanning Electron Microscope

Extended defects such as dislocations and grain boundaries have a strong influence on the performance of microelectronic devices and on other applications of semiconductor materials. However, it is still under debate how the defect structure determines the band structure, and therefore, the recombination behavior of electron-hole pairs responsible for the optical and electrical properties of the extended defects. The present paper is a survey of procedures for the spatially resolved investigation of structural and of physical properties of extended defects in semiconductor materials with a scanning electron microscope (SEM). Representative examples are given for crystalline silicon. The luminescence behavior of extended defects can be investigated by cathodoluminescence (CL) measurements. They are particularly valuable because spectrally and spatially resolved information can be obtained simultaneously. For silicon, with an indirect electronic band structure, CL measurements should be carried out at low temperatures down to 5 K due to the low fraction of radiative recombination processes in comparison to non-radiative transitions at room temperature. For the study of the electrical properties of extended defects, the electron beam induced current (EBIC) technique can be applied. The EBIC image reflects the local distribution of defects due to the increased charge-carrier recombination in their vicinity. The procedure for EBIC investigations is described for measurements at room temperature and at low temperatures. Internal strain fields arising from extended defects can be determined quantitatively by cross-correlation electron backscatter diffraction (ccEBSD). This method is challenging because of the necessary preparation of the sample surface and because of the quality of the diffraction patterns which are recorded during the mapping of the sample. The spatial resolution of the three experimental techniques is compared.

The optical, electrical, and structural properties of dislocations and of grain boundaries in semiconductor materials can be determined by experiments performed in a scanning electron microscope. Electron microscopy has been used to investigate cathodoluminescence, electron beam induced current, and diffraction of backscattered electrons.

走査型電子顕微鏡による半導体材料における拡張欠陥の総合的な特性評価

Extended defects such as dislocations and grain boundaries have a strong influence on the performance of microelectronic devices and on other applications ...

Optical Trap Loading of Dielectric Microparticles In Air

We demonstrate a method to trap a selected dielectric microparticle in air using radiation pressure from a single-beam gradient optical trap. Randomly scattered dielectric microparticles adhered to a glass substrate are momentarily detached using ultrasonic vibrations generated by a piezoelectric transducer (PZT). Then, the optical beam focused on a selected particle lifts it up to the optical trap while the vibrationally excited microparticles fall back to the substrate. A particle may be trapped at the nominal focus of the trapping beam or at a position above the focus (referred to here as the levitation position) where gravity provides the restoring force. After the measurement, the trapped particle can be placed at a desired position on the substrate in a controlled manner. 
In this protocol, an experimental procedure for selective optical trap loading in air is outlined. First, the experimental setup is briefly introduced. Second, the design and fabrication of a PZT holder and a sample enclosure are illustrated in detail. The optical trap loading of a selected microparticle is then demonstrated with step-by-step instructions including sample preparation, launching into the trap, and use of electrostatic force to excite particle motion in the trap and measure charge. Finally, we present recorded particle trajectories of Brownian and ballistic motions of a trapped microparticle in air. These trajectories can be used to measure stiffness or to verify optical alignment through time domain and frequency domain analysis. Selective trap loading enables optical tweezers to track a particle and its changes over repeated trap loadings in a reversible manner, thereby enabling studies of particle-surface interaction.

A protocol for launching and stably trapping selected dielectric microparticles in air is presented.

空気中の誘電体微粒子の光学トラップのロード

We demonstrate a method to trap a selected dielectric microparticle in air using radiation pressure from a single-beam gradient optical trap. Randomly ...

A Method for Obtaining Serial Ultrathin Sections of Microorganisms in Transmission Electron Microscopy

Observing cells and cell components in three dimensions at high magnification in transmission electron microscopy requires preparing serial ultrathin sections of the specimen. Although preparing serial ultrathin sections is considered to be very difficult, it is rather easy if the proper method is used. In this paper, we show a step-by-step procedure for safely obtaining serial ultrathin sections of microorganisms. The key points of this method are: 1) to use the large part of the specimen and adjust the specimen surface and knife edge so that they are parallel to each other; 2) to cut serial sections in groups and avoid difficulty in separating sections using a pair of hair strands when retrieving a group of serial sections onto the slit grids; 3) to use a 'Section-holding loop' and avoid mixing up the order of the section groups; 4) to use a 'Water-surface-raising loop' and make sure the sections are positioned on the apex of the water and that they touch the grid first, in order to place them in the desired position on the grids; 5) to use the support film on an aluminum rack and make it easier to recover the sections on the grids and to avoid wrinkling of the support film; and 6) to use a staining tube and avoid accidentally breaking the support films with tweezers. This new method enables obtaining serial ultrathin sections without difficulty. The method makes it possible to analyze cell structures of microorganisms at high resolution in 3D, which cannot be achieved by using the automatic tape-collecting ultramicrotome method and serial block-face or focused ion beam scanning electron microscopy.

This study presents reliable and easy procedures for obtaining serial ultrathin sections of a microorganism without expensive equipment in transmission electron microscopy.

透過型電子顕微鏡における微生物の連続超薄切片を得る方法

Observing cells and cell components in three dimensions at high magnification in transmission electron microscopy requires preparing serial ultrathin ...

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

We demonstrate the use of two nuclear-based analytical methods that can follow the modifications of microstructural arrangement of iron-based metallic glasses (MGs). Despite their amorphous nature, the identification of hyperfine interactions unveils faint structural modifications. For this purpose, we have employed two techniques that utilize nuclear resonance among nuclear levels of a stable 57Fe isotope, namely M&#246;ssbauer spectrometry and nuclear forward scattering (NFS) of synchrotron radiation. The effects of heat treatment upon (Fe2.85Co1)77Mo8Cu1B14 MG are discussed using the results of ex situ and in situ experiments, respectively. As both methods are sensitive to hyperfine interactions, information on structural arrangement as well as on magnetic microstructure is readily available. M&#246;ssbauer spectrometry performed ex situ describes how the structural arrangement and magnetic microstructure appears at room temperature after the annealing under certain conditions (temperature, time), and thus this technique inspects steady states. On the other hand, NFS data are recorded in situ during dynamically changing temperature and NFS examines transient states. The use of both techniques provides complementary information. In general, they can be applied to any suitable system in which it is important to know its steady state but also transient states.

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

Here, we present a protocol to describe ex situ and in situ investigations of structural transformations in metallic glasses. We employed nuclear-based analytical methods which inspect hyperfine interactions. We demonstrate the applicability of M&#246;ssbauer spectrometry and nuclear forward scattering of synchrotron radiation during temperature-driven experiments.

Ex その場その場で調査構造変換の方法: 金属ガラスの結晶化の事例

We demonstrate the use of two nuclear-based analytical methods that can follow the modifications of microstructural arrangement of iron-based metallic ...

Single-Digit Nanometer Electron-Beam Lithography with an Aberration-Corrected Scanning Transmission Electron Microscope

We demonstrate extension of electron-beam lithography using conventional resists and pattern transfer processes to single-digit nanometer dimensions by employing an aberration-corrected scanning transmission electron microscope as the exposure tool. Here, we present results of single-digit nanometer patterning of two widely used electron-beam resists: poly (methyl methacrylate) and hydrogen silsesquioxane. The method achieves sub-5 nanometer features in poly (methyl methacrylate) and sub-10 nanometer resolution in hydrogen silsesquioxane. High-fidelity transfer of these patterns into target materials of choice can be performed using metal lift-off, plasma etch, and resist infiltration with organometallics.

We use an aberration-corrected scanning transmission electron microscope to define single-digit nanometer patterns in two widely-used electron-beam resists: poly (methyl methacrylate) and hydrogen silsesquioxane. Resist patterns can be replicated in target materials of choice with single-digit nanometer fidelity using liftoff, plasma etching, and resist infiltration by organometallics.

収差補正走査透過電子顕微鏡と 1 桁台のナノメートルの電子ビーム露光

We demonstrate extension of electron-beam lithography using conventional resists and pattern transfer processes to single-digit nanometer dimensions by ...

Application of a Coupling Agent to Improve the Dielectric Properties of Polymer-Based Nanocomposites

In this work, an easy, low-cost, and widely applicable method was developed to improve the compatibility between the ceramic fillers and the polymer matrix by adding 3-aminopropyltriethoxysilane (KH550) as a coupling agent during the fabrication process of BaTiO3-P(VDF-CTFE) nanocomposites through solution casting. Results show that the use of KH550 can modify the surface of ceramic nanofillers; therefore, good wettability on the ceramic-polymer interface was achieved, and the enhanced energy storage performances were obtained by a suitable amount of the coupling agent. This method can be used to prepare flexible composites, which is highly desirable for the production of high-performance film capacitors. If an excessive amount of coupling agent is used in the process, the non-attached coupling agent can participate in complex reactions, which leads to a decrease in dielectric constant and an increase in dielectric loss.

Here, we demonstrate a simple and low-cost solution-casting process to improve the compatibility between the filler and the matrix of polymer-based nanocomposites using surface modified BaTiO3 fillers, which can effectively enhance the energy density of the composites.

ポリマー系ナノ複合材料の誘電特性向上のためのカップリング剤の応用

In this work, an easy, low-cost, and widely applicable method was developed to improve the compatibility between the ceramic fillers and the polymer ...

In Situ Transmission Electron Microscopy with Biasing and Fabrication of Asymmetric Crossbars Based on Mixed-Phased a-VOx

Resistive switching crossbar architecture is highly desired in the field of digital memories due to low cost and high-density benefits. Different materials show variability in resistive switching properties due to the intrinsic nature of the material used, leading to discrepancies in the field because of underlying operation mechanisms. This highlights a need for a reliable technique to understand mechanisms using nanostructural observations. This protocol explains a detailed process and methodology of in&#160;situ nanostructural analysis as a result of electrical biasing using transmission electron microscopy (TEM). It provides visual and reliable evidence of underlying nanostructural changes in real time memory operations. Also included is the methodology of fabrication and electrical characterizations for asymmetric crossbar structures incorporating amorphous vanadium oxide. The protocol explained here for vanadium oxide films can be easily extended to any other materials in a metal-dielectric-metal sandwiched structure. Resistive switching crossbars are predicted to serve the programmable logic and neuromorphic circuits for next-generation memory devices, given the understanding of the operation mechanisms. This protocol reveals the switching mechanism in a reliable, timely, and cost-effective way in any type of resistive switching materials, and thereby predicts the device&#39;s applicability.

In Situ Transmission Electron Microscopy with Biasing and Fabrication of Asymmetric Crossbars Based on Mixed-Phased a-VOx

Presented here is a protocol for analyzing nanostructural changes during in&#160;situ biasing with transmission electron microscopy (TEM) for a stacked metal-insulator-metal structure. It has significant applications in resistive switching crossbars for the next generation of programmable logic circuits and neuromimicking hardware, to reveal their underlying operation mechanisms and practical applicability.