Surface Preparation of Cross Sections of Traditional and Modern Paint Using the Argon Ion Milling Polishing CP System

In the oxidation of metals and alloys, microstructural features at the atomic level play an important role in the nucleation and growth of the oxide, but little is known about the atomic mechanisms of high temperature oxidation. The present paper describes current progress on crystallographic aspects of aluminum oxidation. The 99.999% pure, polycrystalline aluminum was chemically polished and oxidized in 1 atm air at either 550°C or 600°C for times from 0.5 hr to 4 weeks. Cross-sectional specimens were prepared by forming a sandwich with epoxy, followed by mechanical polishing and then argon ion milling. High resolution images were recorded in a <110>oxide zone-axis orientation with a JE0L JEM 200CX microscope operated at 200 keV.

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A technique for preparing semiconductor cross sections for both TEM and SEM analysis

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100155530 ◽

1989 ◽

Vol 47 ◽

pp. 712-713

Author(s):

Stanley J. Klepeis ◽

J.P. Benedict ◽

R.M Anderson

Keyword(s):

Sample Preparation ◽

Cross Section ◽

Cross Sections ◽

Sem Analysis ◽

Preparation Technique ◽

Ion Milling ◽

Tem Analysis ◽

Polished Cross Section ◽

Area Of Interest ◽

Polished Side

The ability to prepare a cross-section of a specific semiconductor structure for both SEM and TEM analysis is vital in characterizing the smaller, more complex devices that are now being designed and manufactured. In the past, a unique sample was prepared for either SEM or TEM analysis of a structure. In choosing to do SEM, valuable and unique information was lost to TEM analysis. An alternative, the SEM examination of thinned TEM samples, was frequently made difficult by topographical artifacts introduced by mechanical polishing and lengthy ion-milling. Thus, the need to produce a TEM sample from a unique,cross-sectioned SEM sample has produced this sample preparation technique.The technique is divided into an SEM and a TEM sample preparation phase. The first four steps in the SEM phase: bulk reduction, cleaning, gluing and trimming produces a reinforced sample with the area of interest in the center of the sample. This sample is then mounted on a special SEM stud. The stud is inserted into an L-shaped holder and this holder is attached to the Klepeis polisher (see figs. 1 and 2). An SEM cross-section of the sample is then prepared by mechanically polishing the sample to the area of interest using the Klepeis polisher. The polished cross-section is cleaned and the SEM stud with the attached sample, is removed from the L-shaped holder. The stud is then inserted into the ion-miller and the sample is briefly milled (less than 2 minutes) on the polished side. The sample on the stud may then be carbon coated and placed in the SEM for analysis.

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Comparison of ultra high resolution immersion lens CFESEM and TEM for imaging of semiconductor devices

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100176241 ◽

1990 ◽

Vol 48 (4) ◽

pp. 622-623

Author(s):

Terrence Reilly ◽

Al Pelillo ◽

Barbara Miner

Keyword(s):

High Resolution ◽

Sample Preparation ◽

Cross Sections ◽

Semiconductor Devices ◽

Ion Milling ◽

Observation Area ◽

Transmission Electron ◽

Milling Machines ◽

Resolution Imaging ◽

Electron Microscopes

The use of transmission electron microscopes (TEM) has proven to be very valuable in the observation of semiconductor devices. The need for high resolution imaging becomes more important as the devices become smaller and more complex. However, the sample preparation for TEM observation of semiconductor devices have generally proven to be complex and time consuming. The use of ion milling machines usually require a certain degree of expertise and allow a very limited viewing area. Recently, the use of an ultra high resolution "immersion lens" cold cathode field emission scanning electron microscope (CFESEM) has proven to be very useful in the observation of semiconductor devices. Particularly at low accelerating voltages where compositional contrast is increased. The Hitachi S-900 has provided comparable resolution to a 300kV TEM on semiconductor cross sections. Using the CFESEM to supplement work currently being done with high voltage TEMs provides many advantages: sample preparation time is greatly reduced and the observation area has also been increased to 7mm. The larger viewing area provides the operator a much greater area to search for a particular feature of interest. More samples can be imaged on the CFESEM, leaving the TEM for analyses requiring diffraction work and/or detecting the nature of the crystallinity.

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Low Energy Ar Ion Milling of FIB TEM Specimens from 14 nm and Future FinFET Technologies

10.31399/asm.cp.istfa2018p0241 ◽

2018 ◽

Author(s):

C.S. Bonifacio ◽

P. Nowakowski ◽

M.J. Campin ◽

M.L. Ray ◽

P.E. Fischione

Keyword(s):

Field Effect Transistor ◽

Focused Ion Beam ◽

Ion Beam ◽

Specimen Preparation ◽

Ion Milling ◽

Transmission Electron ◽

High Resolution Tem ◽

Effect Transistor ◽

20 Nm ◽

Argon Ion

Abstract Transmission electron microscopy (TEM) specimens are typically prepared using the focused ion beam (FIB) due to its site specificity, and fast and accurate thinning capabilities. However, TEM and high-resolution TEM (HRTEM) analysis may be limited due to the resulting FIB-induced artifacts. This work identifies FIB artifacts and presents the use of argon ion milling for the removal of FIB-induced damage for reproducible TEM specimen preparation of current and future fin field effect transistor (FinFET) technologies. Subsequently, high-quality and electron-transparent TEM specimens of less than 20 nm are obtained.

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The Use of Ion Milling for Surface Preparation for EBSD Analysis

Materials ◽

10.3390/ma14143970 ◽

2021 ◽

Vol 14 (14) ◽

pp. 3970

Author(s):

Wojciech J. Nowak

Keyword(s):

Plasma Etching ◽

Ion Beam ◽

Metallic Matrix ◽

Surface Preparation ◽

Optical Emission ◽

Alternative Methods ◽

Ebsd Analysis ◽

Crystallographic Structure ◽

Ion Milling ◽

Electron Backscattered Diffraction

An electron backscattered diffraction (EBSD) method provides information about the crystallographic structure of materials. However, a surface subjected to analysis needs to be well-prepared. This usually requires following a time-consuming procedure of mechanical polishing. The alternative methods of surface preparation for EBSD are performed via electropolishing or focus ion beam (FIB). In the present study, plasma etching using a glow discharge optical emission spectrometer (GD-OES) was applied for surface preparation for EBSD analysis. The obtained results revealed that plasma etching through GD-OES can be successfully used for surface preparation for EBSD analysis. However, it was also found that the plasma etching is sensitive for the alloy microstructure, i.e., the presence of intermetallic phases and precipitates such as carbides possess a different sputtering rate, resulting in non-uniform plasma etching. Preparation of the cross-section of oxidized CM247 revealed a similar problem with non-uniformity of plasma etching. The carbides and oxide scale possess a lower sputtering rate than the metallic matrix, which caused formation of relief. Based on obtained results, possible resolutions to suppress the effect of different sputtering rates are proposed.

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The Preparation of Submicron Precision Cross Sections by Dimpling With A ‘Flatting Tool’

MRS Proceedings ◽

10.1557/proc-480-117 ◽

1997 ◽

Vol 480 ◽

Author(s):

Helen L. Humiston

Keyword(s):

Cross Section ◽

Cross Sections ◽

Microstructural Analysis ◽

Complex Materials ◽

Ion Milling ◽

Step Procedure ◽

Simple Step ◽

Primary Advantage ◽

Preparation Techniques ◽

Support Grid

AbstractThe complex materials systems in VLSI devices require specialized preparation techniques for TEM microstructural analysis. For this purpose, it is desirable to obtain electron transparency in all material layers from the oxides used in dielectrics to refractory metals such as tungsten. The primary advantage of dimpling these materials is that ideal specimens are obtained for low angle ion milling. By dimpling both sides of the cross section with a padded flatting tool, a thicker specimen of 130μm at the outer rim of the 3mm disc is produced that narrows to the 125nm thickness fringes in the center. These samples do not require a copper support grid, thereby allowing for a lower milling angle of 2.5 degrees on both sides of the specimen. This technique provides a cross section that is electron transparent in all layers without the loss of oxides due to differential thinning rates of various materials at higher milling angles.It is generally thought that precision thinning through a submicron feature is not possible on the dimpler. However, a simple step-by-step procedure for this technique will be demonstrated and discussed.

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Sensing properties of infrared nanostructured plasmonic crystals fabricated by electron beam lithography and argon ion milling

Journal of Vacuum Science & Technology B Nanotechnology and Microelectronics Materials Processing Measurement and Phenomena ◽

10.1116/1.4767274 ◽

2012 ◽

Vol 30 (6) ◽

pp. 06FE02 ◽

Cited By ~ 1

Author(s):

Baogang Quan ◽

Zhe Liu ◽

Lin Li ◽

Weijie Sun ◽

Xinlong Xu ◽

...

Keyword(s):

Electron Beam ◽

Electron Beam Lithography ◽

Ion Milling ◽

Sensing Properties ◽

Plasmonic Crystals ◽

Argon Ion

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Focused Ion Beam Study of Ni5Al Single Splat Microstructure

MRS Proceedings ◽

10.1557/proc-983-0983-ll04-04-kk04-04 ◽

2006 ◽

Vol 983 ◽

Cited By ~ 1

Author(s):

Yuhong Wu ◽

Meng Qu ◽

Lucille A Giannuzzi ◽

Sanjay Sampath ◽

Andrew Gouldstone

Keyword(s):

Cross Sections ◽

Focused Ion Beam ◽

Surface Engineering ◽

Ion Beam ◽

Deposition Process ◽

Rapid Quenching ◽

Specimen Preparation ◽

Ion Milling ◽

Columnar Grains ◽

Lift Off

AbstractThermally sprayed (TS) coatings are widely used for surface engineering across a range of industries, including aerospace, infrastructure and biomedical. TS materials are formed via the successive impingement, rapid quenching and build-up of molten powder particles on a substrate. The impacted ‘splats’ are thus the fundamental microstructural constituents of the coatings, and their intrinsic properties, as well as intersplat bonding and morphology, dictate coating behavior. Beyond the obvious practical considerations, from a scientific standpoint, splats represent a fascinating template for study, due to the highly non-equilibrium processing conditions (rapid deceleration from sub-sonic velocities, million-degree/sec cooling rates). In the literature, many studies of isolated splats on substrates have been carried out, but these have focused on overall morphology (disc-shape vs fragmented). Direct observations of microstructure, in particular cross-section, are limited in the specimen preparation stage due to splat size (tens of microns in diameter, 1-2 microns in thickness). However, Focused Ion Beam (FIB) techniques have allowed this problem to be addressed in a robust manner; in this paper we will discuss such approaches to observe Ni5Al splats on stainless steel substrates. Cross-sections through the splat and the substrate were created by recourse to ion milling and the ion beam itself provided good channeling contrast for grain imaging. The typical splat microstructure with sub-micron Ni(Al) columnar grains, a chill zone at the bottom and a lift off area is observed in high detail. In addition, an amorphous aluminum oxide top layer of 100-200 nm is partially present on top of the Ni(Al) columnar grains. At the splat/substrate interface, defects such as micro- and nano-scale pores were characterized for the first time and will be discussed. These observations provide insights into splat and interface formation during the deposition process and may drastically improve our current understanding of Ni5Al splat properties.

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