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. Preparação da amostra para a Focused Ion Beam (FIB) Emagrecimento (Figura 1) <ol><li> Clivar o wafer completo em pequenos chips (~ 10 milímetros por 10 milímetros) com um escriba diamante. </li><li> Marque a posição da estrutura de &quot;ponta-a-ponta&quot; sobre os chips. </li><li> Viu o chip com uma máquina de corte em cubos para obter barras de 60 mm por 2 mm de tamanho. O bar inclui a estrutura &quot;ponta-a-ponta&quot; no centro. </li><li> Cole o bar alvo em um meio anel Cu usando o super-cola. Em seguida, cole o bar em um estágio da amostra Cu também usando o super-cola. Então, o uso de prata colar para definir a condução entre a metade e o anel de fase de amostra de cobre. Nota: Ao manusear a amostra, certifique-se de usar sempre uma pulseira antiestática para evitar descargas eletrostáticas, que podem danificar a estrutura sensível na amostra. </li></ol> 2. FIB Emagrecimento no Microscópio Eletrônico de Varredura (Figura 2) <ol><li> Colocar a amostra obtida no passo 1 numan SEM estágio da amostra e colocar o palco com cuidado no SEM. </li><li> Escolheu o modo de deposição, e configurar as dimensões (área e espessura) da camada precisava de proteção Pt. Sempre use um feixe de íons de 30 kV para manter a mais alta precisão. Ajustar a corrente para obter a eficiência satisfeito, dependente das dimensões da camada de Pt necessário. <ol><li> Depositar uma linha Pt entrar em contato com um bloco para a fase de Cu (potencial de terra). Subsequentemente, depositar uma camada de Pt de espessura na parte superior da estrutura de &quot;ponta-a-ponta&quot;, o que é muito importante para minimizar os danos iónica durante o processo de desbaste FIB e para reforçar a lamela fina. Este é um procedimento padrão utilizado na preparação de FIB. </li><li> Tome cuidado para não introduzir quaisquer caminhos condutores entre os dois blocos no topo da estrutura de &quot;ponta-a-ponta&quot; através da camada de Pt ao realizar a deposição de Pt. Qualquer caminho condutor será curto circuito elétrico (Figura 2 A e B). </li></ol></li><li> FIB moagem <ol><li> Use uma tensão de 30 kV e corrente de 10 pA para o corte final. Diluir o alvo em um bar TEM lamela H-bar com uma espessura entre 150 e 180 nm. </li><li> Corte um entalhe perto da almofada (V + pad) que será tocado por um transdutor na ponta TEM. Utilizar o entalhe como um marcador para identificar a almofada correcta no MET. </li></ol></li></ol> 3. Amostra de transferência do SEM ao TEM <ol><li> Coloque a pulseira anti-estática antes de tocar na amostra. </li><li> Desmontar a amostra H-bar preparado a partir da fase de SEM. Manter a amostra no palco Cu quando removê-lo do SEM. </li><li> Fixe a fase Cu no suporte do TEM. Mover a ponta do transdutor do suporte de MET perto da estrutura de teste (algumas centenas de micrómetros de distância a partir da estrutura de teste) sob o microscópio óptico. <ol><li> Insira o suporte da TEM na TEM cuidadosamente. Não utilizar qualquer tratamento de limpeza (por exemplo, limpeza de plasma) durante o transfer processo, caso contrário, a lamela pode ser influenciado. </li></ol></li><li> Mantenha o tempo para a transferência da amostra em 15 minutos ou menos para evitar o excesso de exposição à humidade ambiente e oxigênio. </li></ol> 4. Estabelecer a ligação eléctrica (Figura 3) <ol><li> Conecte o suporte do TEM para seu sistema de controle eo SourceMeter. Em seguida, ligar o sistema de controle eo SourceMeter. </li><li> Monitorar a ponta do transdutor na TEM ao fazer a abordagem grosseira da ponta do transdutor para a estrutura de teste por meio do ajuste dos botões no suporte do TEM. <ol><li> Mova a ponta do transdutor do titular do TEM perto do bloco V + (≤ 500 nm). Coloque a extremidade do transdutor para o mesmo nível (Z: altura) como o pad. Ajustar a posição da ponta e fazer a ponta voltado para o centro da almofada de V +. </li></ol></li><li> Contacte a ponta do transdutor para o bloco V +. Definir uma tensão muito baixa na ponta (0,5 V a cerca de 1 V) quando se aproxima o pad. Monitorar o simultáneo atualusly para garantir que o contato é estabelecido. </li></ol> 5. Experimento In Situ TDDB <ol><li> Utilize uma tensão de aceleração de 200 kV no MET. Mova o feixe de elétrons para a área de interesse; escolher uma ampliação adequada e focar a imagem. </li><li> Use passos de iluminação baixos (≤ 8) para reduzir os danos na estrutura de feixe de teste. Use uma abertura do condensador para localizar a área de iluminação apenas dentro da parte fina da amostra H-bar. </li><li> Aplicar uma tensão constante (≤ 40 V) sobre a estrutura &quot;ponta-a-ponta&quot; usando o SourceMeter enquanto grava as imagens em MET in situ (2-3 frames / seg). Grave as imagens automaticamente, utilizando um código de auto-scripted, por exemplo, utilizando o software DigitalMicrograph. </li><li> Pause o experimento ao ver uma difusão aparente de metal em os dielétricos ULK e fazer a análise química Electron espectroscópica Imagem (ESI). <ol><li> Insira a abertura de fenda filtro no Omegum filtro de energia no MET. </li><li> Ajustar a largura da abertura de lama do filtro para obter uma largura adequada da energia (20/10 eV) no espectro de perda de energia dos electrões (EELS). </li><li> Deslocar a energia para o pico de adsorção de cobre M-borda nas EELS. </li><li> Volte para o modo de imagem para adquirir uma imagem TEM energia filtrada no Cu M-borda de absorção de pico. </li><li> Deslocar a energia para o pré-borda do M-borda de cobre e obter uma outra imagem TEM energia filtrada. </li><li> Corrigir a deriva da amostra entre as duas imagens. </li><li> Divida a primeira imagem por um segundo para obter a imagem relação salto de Cu. </li></ol></li><li> Continuar o experimento TDDB: reaplicar uma tensão constante (≤ 40 V) sobre a estrutura &quot;ponta-a-ponta&quot; usando o SourceMeter e gravar as imagens em MET. </li></ol> 6. Tomografia Computadorizada <ol><li> Execute TEM tomografia computadorizada quando o experimento TDDB for concluída, para obter informações sobre a distribuição 3D diffused partículas. </li><li> Incline a amostra e gravar uma série de inclinação de 138 °. Use um passo de inclinação de 1 °, e gravar a imagem em cada passo no modo STEM campo claro (BF). </li><li> Reconstruir a série (inclui o alinhamento de imagens, determinando eixo de inclinação, reconstruindo volume e segmentação para formar o volume tomografia 3D). </li></ol>

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No competing financial interests.

O pré-requisito para o sucesso da experiência TDDB é boa preparação de amostras, especialmente no processo de moagem FIB no SEM. Em primeiro lugar, uma camada de Pt de espessura na parte superior da estrutura de &quot;ponta-a-ponta&quot; tem de ser depositada. A espessura e o tamanho da camada de Pt pode ser ajustada pelo operador de SEM, mas tem que seguir três princípios: (1) A espessura e o tamanho é suficiente para proteger a área alvo de possíveis danos do feixe de iões ao longo de todo o processo de moa...

Desde interconexões Cu foram primeiramente introduzido na tecnologia de integração ultra-large-scale (ULSI) em 1997 1, low-k e ultra-low-k (ULK) dielétricos foram adotadas no back-end-of-line (BEOL) como os materiais isolantes entre interconexões on-chip. A combinação de novos materiais, por exemplo, Cu para redução da resistência e de baixo k / ULK dielétricos de baixa capacitância, supera os efeitos do aumento da resistência-capacitância (RC) atraso causado por interconectam dimensional encolhimento 2, 3. No entanto, esse benefício foi invadido pela escala agressiva contínua de dispositivos microeletrônicos nos últimos anos. O uso de low-k / ULK materiais resulta em vários desafios no processo de fabricação e para a confiabilidade do produto, especialmente se o campo de interconexão atinge cerca de 100 nm ou menos 4-6. TDDB refere-se ao mecanismo de um material dieléctrico falha física como uma função de temposob um campo eléctrico. O teste de fiabilidade TDDB é normalmente levada a cabo sob condições aceleradas (campo eléctrico elevada e / ou temperatura elevada). O TDDB em on-chip stacks interconexão é um dos mecanismos de falha mais críticos para os dispositivos microeletrônicos, que já suscitou preocupações intensas na comunidade confiabilidade. Ele continuará a ser o centro das atenções de engenheiros de confiabilidade desde dielétricos ULK com propriedades elétricas e mecânicas mesmo mais fracos estão sendo integrados nos dispositivos nos nós de tecnologia avançada. Dedicado experiências foram realizadas para investigar o mecanismo de falha TDDB 7-9, e uma quantidade significativa de esforço tem sido investido para desenvolver modelos que descrevem a relação entre o campo eléctrico e tempo de vida dos dispositivos 10-13. Os estudos existentes beneficiar a comunidade de engenheiros de confiabilidade em microeletrônica; no entanto, muitos challenges ainda existem e muitas questões ainda precisam ser respondidas em detalhes. Por exemplo, os modelos comprovados para descrever o mecanismo de falha e degradação física cinética no processo TDDB ea respectiva verificação experimental ainda estão faltando. Como uma necessidade particular, um modelo mais apropriado é necessário para substituir o modelo conservador √E-14. Como uma parte muito importante da investigação TDDB, análise de falhas típico está enfrentando um desafio sem precedentes, ou seja, fornecendo evidências abrangente e difícil de explicar a física dos mecanismos de falha e cinética de degradação. Aparentemente, inspeccionando milhões de metros vias e de linhas de Cu nanoescala um por um e ex situ imagiologia do site de falha não é a escolha apropriada de obstáculo a este desafio, porque é muito demorado, e informação limitada sobre a cinética do mecanismo de dano pode ser fornecida. Por isso, uma tarefa urgente surgiu para desenvolver umnd para otimizar experiências e para obter uma melhor procedimento para estudar os mecanismos de falha TDDB e cinética de degradação. Neste artigo, vamos demonstrar uma metodologia experimental em situ para investigar o mecanismo de falha TDDB em Cu / ULK pilhas de interconexão. Um TEM com a capacidade de imagem de alta qualidade e análise química é usado para estudar o processo de cinética em estruturas de teste dedicados. O teste em eléctrica situ é integrado no experimento MET para proporcionar um campo eléctrico elevado para os dieléctricos. A estrutura personalizado &quot;ponta-a-ponta&quot;, consistindo de interconexões Cu totalmente encapsulados e isolados por um material ULK, é projetado no nó de 32 nm CMOS tecnologia. O procedimento experimental descrito aqui pode também ser estendido a outras estruturas em dispositivos activos.

<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.

A Figura 4 mostra brilhante campo (BF) imagens de TEM de um teste em situ. Não são parcialmente violado TaN / barreiras Ta e átomos Cu pré-existentes nos dielétricos ULK antes do teste elétrico (Figura 4A), devido a armazenamento prolongado no ambiente. Depois de apenas 376 segundos a 40 V, a ruptura dielétrica começou e foi acompanhada de duas grandes vias migratórias de cobre de metal M1, com um potencial positivo com referência a lado no chão 15-16. As ...

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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.

Em ruptura dielétrica Situ dependentes do tempo no Microscópio Eletrônico de Transmissão: A possibilidade de compreender o mecanismo de falha em dispositivos microeletrônicos

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

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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 visualizações.  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. 

Vídeo: 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.

Revelando processos dinâmicos de Materiais em Líquidos Usando líquido celular Microscopia Eletrônica de Transmissão

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

Engenharia

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.

Detecção e recuperação de paládio, do ouro e cobalto Metais da Mina Urbana Usando novos sensores / adsorventes Designados com poros em nanoescala em forma de roda de carroça

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.

Usando Synchrotron Radiation microtomografia para investigar Multi-escala Pacotes de microeletrônicos tridimensionais

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.

Caracterização abrangente de Defeitos estendidos em Materiais Semicondutores por um Microscópio Eletrônico de Varredura

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.

Armadilha óptica carregamento de dielétrico micropartículas no ar

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.

Um método para a obtenção de seções ultra-finas Serial de microorganismos em microscopia eletrônica de transmissão

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.

Métodos de Ex Situ e In Situ investigações de transformações estruturais: O caso de cristalização de vidros metálicos

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.

Litografia de feixe de elétrons do nanômetro do dígito com uma aberração corrigida digitalização microscópio eletrônico de transmissão

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.

Aplicação de um agente de acoplamento para melhorar as propriedades dielétricas de nanocompactos baseados em polímeros

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.