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.

Numune Hazırlama 1. Odaklı İyon Işın (FIB) İnceltme (Şekil 1) <ol><li> (~ 10 mm 10 mm) bir elmas çizici küçük cips içine tam gofret parçalamak. </li><li> Yongaları üzerinde &quot;uç-to-ucu&quot; yapı konumlarını işaretleyin. </li><li> 2 mm boyutuna göre 60 mikron bar elde etmek için bir dicing makinesi ile çip gördüm. bar merkezinde &quot;uç-to-ucu&quot; yapı içerir. </li><li> Süper yapıştırıcı kullanılarak Cu yarım halka hedef çubuğunu Tutkal. Sonra, aynı zamanda süper yapıştırıcı kullanılarak bir Cu örnek sahnede bar tutkal. Ardından, kullanım gümüş yüzük yarım ve bakır örnek aşaması arasındaki iletimi ayarlamak için yapıştırın. Not: örnek ele aldığınızda her zaman numune hassas yapısına zarar verebilir elektrostatik boşalmayı önlemek için bir antistatik bileklik giymek emin olun. </li></ol> Taramalı Elektron Mikroskobu 2. FIB İnceltme (Şekil 2) <ol><li> Bir adım 1&#39;de elde edilen örnek koyn SEM örnek sahne ve SEM dikkatlice sahne yerleştirin. </li><li> Biriktirme modunu seçti ve gerekli Pt koruma tabakasının boyutları (bölge ve kalınlık) kurdu. Daima yüksek hassasiyet sağlamak için 30 kV iyon ışını kullanın. Dinle akımı gerekli Pt tabakasının boyutlarına bağlıdır memnun verim almak için. <ol><li> Cu aşamada (toprak potansiyel) bir ped irtibata Pt hattını yatırın. Daha sonra, FIB inceltme işlemi sırasında iyon hasarı en aza indirmek için ince lamel pekiştirmek için çok önemli &quot;uç-to-ucu&quot; yapısı, üstünde kalın bir tabaka Pt mevduat. Bu FIB hazırlanmasında kullanılan standart bir prosedürdür. </li><li> Pt birikimi yaparken Pt katmanı üzerinden &quot;uç-to-ucu&quot; yapının üstünde iki ped arasındaki herhangi bir iletken yolları tanıtmak için değil dikkatli olun. Herhangi bir iletken yol olacak kısa elektrik devresi (Şekil 2A ve B). </li></ol></li><li> FIB freze <ol><li> Final Cut 10 pA bir 30 kV voltaj ve akım kullanın. 150 ve 180 nm arasında bir kalınlığa sahip bir H-çubuğu TEM lamel içine ince bir hedef bar. </li><li> TEM bir dönüştürücü ucu ile dokundu edilecek ped (V + pad) yakın bir çentik kesin. TEM doğru pedi tanımlamak için bir işaretleyici olarak çentik kullanın. </li></ol></li></ol> TEM SEM 3. Numune Transferi <ol><li> Örnek dokunmadan önce antistatik bileklik takın. </li><li> SEM sahneye hazırlanan H-bar örneği ayırın. SEM çıkarırken Cu sahnede örnek tutun. </li><li> TEM tutucu üzerine Cu sahne sabitleyin. Test yapısına yakın TEM tutucu optik mikroskop altında (uzak deney yapısından mikrometre birkaç yüz) ve dönüştürücü ucunu hareket ettirin. <ol><li> Dikkatle TEM içine TEM yuvasını yerleştirin. Tr sırasında herhangi bir temizlik tedavisi (örn plazma temizleme) kullanmak etmeyinansfer işlem olup, aksi takdirde lamel etkilenebilir. </li></ol></li><li> Ortam nem ve oksijene çok fazla maruz kalmaktan kaçınmak için 15 dakika veya daha kısa olan numune transferi için zaman tutun. </li></ol> 4. Elektrik Bağlantısı Kurulması (Şekil 3) <ol><li> Kendi kontrol sistemi ve SourceMeter TEM tutucu bağlayın. Sonra kontrol sistemi ve SourceMeter açın. </li><li> TEM tutucu üzerindeki düğmeleri ayarlama test yapısına dönüştürücü ucunun kaba yaklaşım yaparken TEM dönüştürücü ucu izleyin. <ol><li> (500 nm ≤) V + pad yakın TEM sahibinin dönüştürücü ucunu hareket ettirin. Ped olarak: (yükseklik Z) aynı seviyeye dönüştürücü ucunu getirin. Dinle ucunun pozisyonu ve ucu V + ped merkezini yüz yapmak. </li></ol></li><li> V + pad dönüştürücü ucunu başvurun. Ped yaklaşırken (yaklaşık 1 V 0.5 V) ucunda çok düşük voltaj ayarlayın. Geçerli simultaneo Monitörusly temas kurulmuş olduğundan emin olun. </li></ol> Yerinde TDDB deney 5. <ol><li> TEM 200 kV hızlandırılmış voltajını kullanın. Ilgi alanına elektron ışını taşı; Uygun bir büyütme seçin ve görüntüyü odaklanın. </li><li> Test yapısına ışın zararı azaltmak için düşük aydınlatma adımlarını (≤ 8) kullanın. Sadece H-bar numunenin ince bir parçası olan aydınlatma alanını lokalize bir kondansatör diyafram kullanın. </li><li> In situ TEM görüntüleri (2-3 kare / sn) kaydederken SourceMeter kullanarak &quot;uç-to-ucu&quot; yapısı üzerinde sabit gerilim (≤ 40 V) uygulayın. DigitalMicrograph yazılımını kullanarak, örneğin, bir öz-senaryosunu kodu kullanarak otomatik olarak görüntüleri kaydedebilirsiniz. </li><li> Ulk Dielektriklerin içine metal belirgin bir difüzyon görünce deney Pause ve Elektron Spektroskopisi Görüntüleme (ESI) kimyasal analiz yapmak. <ol><li> OMEG içine filtre yarık açıklığı takınTEM bir enerji filtresi. </li><li> Dinle filtre silt diyafram genişliği elektron enerji kaybı spektrumunun (EELS) uygun bir enerji genişliği (10-20 eV) alır. </li><li> EELS bakır M-kenar adsorpsiyon zirve enerji Shift. </li><li> Cu M-kenar absorpsiyon zirvesindeki bir enerji filtrelenmiş TEM görüntü elde etmek için geri görüntüleme modu gidin. </li><li> Bakır M-kenar ön kenarına enerji Shift ve başka enerji filtrelenmiş TEM görüntü almak. </li><li> Iki resim arasındaki örnek sürüklenme düzeltin. </li><li> Cu atlama oranı görüntü almak için ikinci bir ilk görüntüyü bölün. </li></ol></li><li> TDDB deneyi devam: SourceMeter kullanarak &quot;uç-to-ucu&quot; yapısı üzerinde sabit gerilim (≤ 40 V) yeniden ve TEM görüntüleri kaydedebilirsiniz. </li></ol> 6. Bilgisayarlı Tomografi <ol><li> TDDB deneme bittiğinde TEM bilgisayarlı tomografi gerçekleştirin, di hakkında 3D dağıtım bilgi almak içinffused parçacıklar. </li><li> Örnek eğin ve 138 ° &#39;lik bir eğim dizi kaydedin. 1 ° &#39;lik bir eğim adımı kullanın ve parlak saha (BF) KÖK modunda her aşamasında görüntü kaydetmek. </li><li> (Görüntüleri hizalayarak eğim ekseni belirleyen, 3D tomografik hacmi oluşturmak için ses ve segmentasyon yeniden dahil) serisi yeniden yapılandırma. </li></ol>

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No competing financial interests.

TDDB deneyde başarı ön koşul özellikle SEM FIB öğütme işleminde, iyi örnek hazırlıktır. İlk olarak, &quot;uç-to-tip&quot; yapı üstünde bir kalın bir Pt tabakası yatırılır. kalınlık ve Pt tabakasının boyutu SEM operatör tarafından ayarlanabilir ancak üç ilkeleri takip etmek zorunda olabilir: (1) kalınlık ve boyut tüm öğütme işlemi sırasında mümkün iyon ışını zararlardan hedef alanını korumak için yeterlidir; (2) freze sonra kalan numunenin üstüne nispeten kalın Pt tabak...

Cu ara bağlantıları öncelikle 1997 1 ultra-büyük ölçekli entegrasyon (ULSI) teknolojisi girmiştir beri, düşük k ve ultra-düşük-k (Ulk) dielektrikler arka uç-of-line içine (BEoL) kabul edilmiştir on-chip bağlantılarının arasında yalıtım malzemesi olarak. örneğin, yeni malzemeler, kombinasyonu, Cu, indirgenmiş direnci ve daha düşük olan kapasitans düşük-k / Ulk dielektrikler, boyutsal ara bağlantı çekme 2, 3 kaynaklanan gecikme artan direnç kapasitör (RC) etkilerini ortadan kaldıran için. Bununla birlikte, bu yararı işgal edilmiştir Son yıllarda mikroelektronik cihazların devam agresif pullanma ile. imalat işleminde ve ürün güvenilirliği için çeşitli zorluklar düşük k / Ulk malzemelerinin kullanımı, ara-bağlantı sahası 100 nm ya da daha az 4-6 ulaştığında, özellikle. TDDB zamanın bir fonksiyonu olarak bir dielektrik malzemenin fiziki başarısızlık mekanizması değinmektedirbir elektrik alanı altında. TDDB güvenilirlik testi genellikle hızlandırılmış koşullar (yüksek elektrik alanı ve / veya yüksek bir sıcaklıkta) altında gerçekleştirilir. Bağlantı yığınlarının on-chip in TDDB zaten güvenilirlik toplumda yoğun endişelerini artırdı mikroelektronik cihazlar için en kritik arıza mekanizmalarından biridir. Hatta zayıf elektriksel ve mekanik özellikleri ileri teknoloji düğümlerinde cihazlara entegre ediliyor ile Ulk dielektriğin beri güvenilirlik mühendislerinin gündemde olmaya devam edecektir. Adanmış deneyler TDDB hatası mekanizmasını 7-9 araştırmak için yapılmıştır, ve çaba önemli miktarda cihazlarının 10-13 elektrik alan ve ömür boyu arasındaki ilişkiyi açıklayan modeller geliştirmek için yatırım yapılmıştır. Mevcut çalışmalar mikroelektronik güvenilirlik mühendislerinin toplum yararına; Bununla birlikte, bir çok Challenges hala var ve bir çok soru hala detaylı bir şekilde cevaplanması gereken. Örneğin, kanıtlanmış modeller TDDB sürecinde fiziksel arıza mekanizması ve bozulma kinetiği tanımlamak ve ilgili deneysel doğrulama hala eksiktir. Belirli bir ihtiyaç olarak, daha uygun bir modeli konservatif √E-modeli 14 yerine gereklidir. TDDB soruşturma çok önemli bir parçası olarak, tipik başarısızlık analizi arıza mekanizmaları ve bozulma kinetik fizik açıklamak kapsamlı ve sert kanıt sağlama, yani benzeri görülmemiş bir meydan okumayla karşı karşıya. Görünüşe göre, bu hasar mekanizmasının kinetik hakkında sadece sınırlı bilgi çok zaman alıcı olduğundan ve arıza sitesi, engel bu meydan uygun seçim değildir görüntüleme tek tek ve ex situ ile yolların ve nano ölçekli Cu hatları metre milyonlarca teftiş sağlanabilir. Bu nedenle, acil bir görev, bir geliştirmeye ortaya çıkmıştırnd deneyler optimize etmek ve TDDB başarısızlık mekanizmalarını ve bozulma kinetiğinin incelemek için daha iyi bir prosedür olsun. Bu yazıda, yerinde deney metodoloji bir Cu / Ulk bağlantı yığınlar TDDB başarısızlık mekanizmasını araştırmak için gösterecektir. Yüksek kaliteli görüntüleme ve kimyasal analiz yeteneği ile bir TEM özel deney yapılarda kinetik sürecini incelemek için kullanılır. in situ elektriksel test dielektrikler yükseltilmiş bir elektrik alanı temin etmek TEM deney entegre edilir. Bir Ulk malzemeden tamamen kapsüllü Cu bağlantılarının oluşan ve yalıtılmış bir özelleştirilmiş &quot;uç-to-ucu&quot; yapı, 32 nm CMOS teknolojisi düğümünde tasarlanmıştır. Burada tarif edilen deney prosedürü, aynı zamanda, aktif cihazlarda diğer yapılara genişletilebilir.

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		</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.

Şekil 4 in situ testinde bir parlak alan (BF) TEM görüntüleri gösterir. Kısmen Orada ihlal edildiği TaN / nedeniyle ortam genişletilmiş depolama elektrik testi (Şekil 4A) önce Ulk dielektriğin Ta engeller ve önceden var olan Cu atomları. Zemin tarafına 15-16 referansla pozitif potansiyele sahip, 40 V sadece 376 saniye sonra, dielektrik dökümü başladı ve M1 metal bakır iki önemli göç yollarının ile eşlik etti. Ulk Dielektriklerde yayılmış...

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.

Transmisyon Elektron Mikroskobu Situ Zamana bağlı Dielektrik Dağılımı In: Bir imkanı Mikroelektronik aygıtlar Başarısızlık Mekanizması Anlayın

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 Görüntüleme.  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. 

Video: 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.

Sıvı Hücre Transmisyon Elektron Mikroskobu kullanarak Sıvılarda Malzemelerin Dinamik Süreçler Revealing

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

Mühendislik

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.

Algılama ve Palladium Kurtarma Kentsel Madeninde Altın ve Kobalt Metal Nano Wagon tekerlekli şeklindeki Porların ile Belirlenmiş Yeni Sensörler / adsorbanlar kullanma

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.

Çok ölçekli Üç boyutlu Mikroelektronik paketleri Soruşturma Sinkrotron Radyasyon Microtomography kullanma

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.

Bir Tarama Elektron Mikroskobu tarafından Yarıiletken Malzemelerin Genişletilmiş Kusur Kapsamlı Karakterizasyonu

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.

Havada Dielektrik mikropartiküllerin Optik Tuzak Yükleme

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.

Transmisyon elektron mikroskobu mikroorganizmaların seri Ultrathin bölümler elde etmek için bir yöntem

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 Situ ve yapısal dönüşümleri in Situ soruşturma yöntemleri: Metalik gözlük kristalleşme olgusu

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.

Tek basamaklı nanometre elektron ışını litografi bir sapma düzeltilmiş tarama transmisyon elektron mikroskobu ile

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.

Polimer Bazlı Nanokompozitlerin Dielektrik Özelliklerini Geliştirmek İçin Kaplin Maddesi Uygulaması

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.