Preparation of TEM plan-view and cross-sectional specimens of ZnSe/GaAs epilayers by chemical thinning and argon ion milling

ABSTRACTTechniques for the preparation of specimens for Transmission Electron Microscopy analysis are described. Cross-sectional specimens of insulator/semiconductor heterostructures have been successfully prepared. The problem of differential thinning rates and interface amorphization during argon ion-milling have been overcome using low argon ion accelerating voltages and shallow angles of incidence. Techniques for preparation of plan view specimens include the preparation of silicon substrates for in-situ crystal growth in an ultrahigh vacuum Transmission Electron Microscope.

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Transmission Electron Microscopy Studies of Aluminum Oxidation

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100118254 ◽

1985 ◽

Vol 43 ◽

pp. 268-269

Author(s):

J.Y. Lee

Keyword(s):

Nucleation And Growth ◽

Ion Milling ◽

Cross Sectional ◽

Polycrystalline Aluminum ◽

Axis Orientation ◽

Temperature Oxidation ◽

Aluminum Oxidation ◽

Transmission Electron ◽

High Resolution Images ◽

Argon Ion

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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Tem Specimen Preparation for Display Materials of Vacuum Fluorescent Displays

Microscopy and Microanalysis ◽

10.1017/s1431927600024478 ◽

1998 ◽

Vol 4 (S2) ◽

pp. 870-871

Author(s):

T. Dolukhanyan ◽

C. Sung ◽

S. Ahn ◽

J. Lee

Keyword(s):

Bulk Material ◽

Low Cost ◽

High Yield ◽

Specimen Preparation ◽

List Type ◽

Ion Milling ◽

Cross Sectional ◽

Preparation Methods ◽

Plan View ◽

Submicron Scale

Further development of Vacuum Fluorescent Displays (Fig.l) for low cost production and high yield requires investigation of all the components on a submicron scale at various processing stages.A variety of specimen preparation methods have been used for making different types of high quality cross-sectional and plan-view TEM specimens from:1.Initial phosphor materials - ZnCdS powders admixed with conducting powder of ln2O3;2.In2O3 mixed ZnCdS phosphor layers of ready-made working VFD;3.W - filament cathodes coated with (Ba,Sr,Ca) oxides.Rapid sharing of results.Group 1 specimens were made both by direct dispersion of phosphor powder particles on the carbon coated copper grid from acetone diluted powder suspension, and by preparation of cured bulk material from the powder using Gatan G-l epoxy, followed by cutting, grinding-dimpling and final ion milling in Gatan DuoMill 600 (Fig.2).

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Cross-Sectional Tem Sample Preparation of Phase-Change Optical Disk by Ion Milling

MRS Proceedings ◽

10.1557/proc-480-251 ◽

1997 ◽

Vol 480 ◽

Author(s):

T. Kouzaki ◽

K. Yoshioka ◽

E. Ohno

Keyword(s):

Sample Preparation ◽

Phase Change ◽

Polymer Substrate ◽

Ion Milling ◽

Cross Sectional ◽

Milling Method ◽

Optical Disks ◽

The Difference ◽

Argon Ion ◽

Sectional Structure

AbstractIt is very difficult to prepare cross-sectional TEM samples for phase-change optical disks by conventional argon ion milling because of the difference of ion milling rates between multilayers and the polymer substrate. We have been successful in preparing samples of those optical disks by ion milling method with dissolution of the polymer substrate in advance. The cross-sectional structure was observed more clearly in this method rather than in ultramicrotome method.

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Microstructural And Microchemical Analysis of Chalcopyrite Cu(In,Ga)Se2 Films

MRS Proceedings ◽

10.1557/proc-763-b4.2 ◽

2003 ◽

Vol 763 ◽

Cited By ~ 3

Author(s):

Chun-Ming Li ◽

Chang-Hui Lei ◽

Ian M. Robertson ◽

Angus Rockett

Keyword(s):

Grain Boundaries ◽

High Performance ◽

Structural Defects ◽

Ion Milling ◽

Mechanical Grinding ◽

Cross Sectional ◽

Plan View ◽

Microchemical Analysis ◽

Transmission Electron ◽

Means Of Transmission

AbstractThe microstructure and microchemistry of Cu(In, Ga)Se2 (CIGS) films have been analyzed by means of transmission electron microscopy (TEM). Specimens were obtained from a number of groups producing high-performance solar cells from these materials. Both plan-view and cross-sectional TEM samples were prepared by mechanical grinding and ion milling. Twins can be found easily within the films while dislocations are present only in a few grains and with low density. No extended structural defects such as stacking faults were discovered. X-ray energy dispersive spectroscopy was used to study the chemical composition of grains and grain boundaries. Experimental results showed no difference between the composition in the grain interiors and the grain boundary. In addition, there is no obvious enhancement of oxygen and sodium at grain boundaries. Structural depth dependences were also not found.

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Preparation of Cross Sectional and Plan View TEM Samples of Thin Films on Mgo Substrates with an Additional Chemical Thinning Step

MRS Proceedings ◽

10.1557/proc-199-225 ◽

1990 ◽

Vol 199 ◽

Cited By ~ 2

Author(s):

Shang. H. Rou ◽

Philip. D. Hren ◽

Angus. I. Kingon

Keyword(s):

Thin Films ◽

Orthophosphoric Acid ◽

Ion Beam ◽

Ion Milling ◽

Cross Sectional ◽

Plan View ◽

Transmission Electron ◽

Sample Preparation Procedure ◽

Common Substrate ◽

Beam Damage

ABSTRACTSingle crystal MgO is a common substrate for the deposition of oxide thin films. The conventional cross sectional transmission electron microscopy sample preparation procedure suffers the drawbacks of: 1)- extensive ion milling time; 2) a higher milling rate for the thin films than for the substrate; 3) introduction of artifacts and contamination during ion milling; and 4) generation of excess defects into the substrate during mechanical thinning. An additional chemical thinning step using hot orthophosphoric acid can reduce or eliminate these adverse effects.This technique can be applied generally to thin film samples deposited on substrates with a low ion milling rate. Furthermore, substrates which are sensitive to mechanical stress and ion beam damage are also suitable for this technique, provided an appropriate chemical polishing solution and compatible epoxy can be found. The unique features of this technique are briefly presented.

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Reduction of the Damage Induced in an Fib-Fabricated X-Tem Specimen

MRS Proceedings ◽

10.1557/proc-523-39 ◽

1998 ◽

Vol 523 ◽

Cited By ~ 1

Author(s):

N. I. Kato ◽

K. Tsujimoto ◽

N. Miura

Keyword(s):

Focused Ion Beam ◽

Crystalline Silicon ◽

Ion Beam ◽

Side Wall ◽

Beam Current ◽

Wet Etching ◽

Ion Milling ◽

Cross Sectional ◽

20 Nm ◽

Argon Ion

AbstractIn focused ion beam (FIB) fabrication of cross-sectional transmission electron microscopy (X-TEM) specimens, highly accelerated ion beams sometimes cause serious damage. The damage can be induced in both the specimen surface and in the side walls. We used X-TEM observations to investigate the side-wall damage induced by FIB fabrication in crystalline silicon. The damaged layer was found to be about 20 nm thick in the case of 30-keV FIB etching. We tried to reduce the damage by several methods, such as gas-assisted etching (GAE) with iodine, broad argon ion milling and wet etching. The damaged layer was 19 nm for GAE and 12 nm for argon ion milling with a beam current of 70 mA and the tilt angle between the beam and the specimen of 15 degrees. Wet etching using a mixture of nitric and hydrofluoric acid removes most of the damaged layer.

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Investigation of III–V Nanowires by Plan-View Transmission Electron Microscopy: InN Case Study

Microscopy and Microanalysis ◽

10.1017/s1431927614013038 ◽

2014 ◽

Vol 20 (5) ◽

pp. 1471-1478 ◽

Cited By ~ 4

Author(s):

Esperanza Luna ◽

Javier Grandal ◽

Eva Gallardo ◽

José M. Calleja ◽

Miguel Á. Sánchez-García ◽

...

Keyword(s):

Electron Microscopy ◽

Transmission Electron Microscopy ◽

Strain Relaxation ◽

Milling Process ◽

Specimen Preparation ◽

Shell Layer ◽

Ion Milling ◽

Cross Sectional ◽

Plan View ◽

Transmission Electron

AbstractWe discuss observations of InN nanowires (NWs) by plan-view high-resolution transmission electron microscopy (TEM). The main difficulties arise from suitable methods available for plan-view specimen preparation. We explore different approaches and find that the best results are obtained using a refined preparation method based on the conventional procedure for plan-view TEM of thin films, specifically modified for the NW morphology. The fundamental aspects of such a preparation are the initial mechanical stabilization of the NWs and the minimization of the ion-milling process after dimpling the samples until perforation. The combined analysis by plan-view and cross-sectional TEM of the NWs allows determination of the degree of strain relaxation and reveals the formation of an unintentional shell layer (2–3-nm thick) around the InN NWs. The shell layer is composed of bcc In2O3 nanocrystals with a preferred orientation with respect to the wurtzite InN: In2O3 [111] || InN [0001] and In2O3 <110> || InN< $$ 11\bar 20 $$ >.

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TEM characterization of silicon epitaxial layer grown on Si-TaS2, eutectic composites

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100088324 ◽

1991 ◽

Vol 49 ◽

pp. 802-803

Author(s):

C.M. Sung ◽

M. Levinson ◽

M. Tabasky ◽

K. Ostreicher ◽

B.M. Ditchek

Keyword(s):

Substrate Surface ◽

Bulk Sample ◽

Surface Cleaning ◽

Native Oxide ◽

Czochralski Growth ◽

Ion Milling ◽

Cross Sectional ◽

Cleaning Methods ◽

Field Emission Cathodes

Directionally solidified Si/TaSi2 eutectic composites for the development of electronic devices (e.g. photodiodes and field-emission cathodes) were made using a Czochralski growth technique. High quality epitaxial growth of silicon on the eutectic composite substrates requires a clean silicon substrate surface prior to the growth process. Hence a preepitaxial surface cleaning step is highly desirable. The purpose of this paper is to investigate the effect of surface cleaning methods on the epilayer/substrate interface and the characterization of silicon epilayers grown on Si/TaSi2 substrates by TEM.Wafers were cut normal to the <111> growth axis of the silicon matrix from an approximately 1 cm diameter Si/TaSi2 composite boule. Four pre-treatments were employed to remove native oxide and other contaminants: 1) No treatment, 2) HF only; 3) HC1 only; and 4) both HF and HCl. The cross-sectional specimens for TEM study were prepared by cutting the bulk sample into sheets perpendicular to the TaSi2 fiber axes. The material was then prepared in the usual manner to produce samples having a thickness of 10μm. The final step was ion milling in Ar+ until breakthrough occurred. The TEM samples were then analyzed at 120 keV using the Philips EM400T.

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Comparison of Ion-Milling Techniques For Cross-Sectional TEM of Semiconductors

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100117807 ◽

1985 ◽

Vol 43 ◽

pp. 166-167

Author(s):

Julia T. Luck ◽

C. W. Boggs ◽

S. J. Pennycook

Keyword(s):

Analytical Techniques ◽

Sample Surface ◽

Ion Milling ◽

Cross Sectional ◽

Reliable Technique ◽

Near Surface ◽

Transmission Electron ◽

Thin Region ◽

Transient Thermal

The use of cross-sectional Transmission Electron Microscopy (TEM) has become invaluable for the characterization of the near-surface regions of semiconductors following ion-implantation and/or transient thermal processing. A fast and reliable technique is required which produces a large thin region while preserving the original sample surface. New analytical techniques, particularly the direct imaging of dopant distributions, also require good thickness uniformity. Two methods of ion milling are commonly used, and are compared below. The older method involves milling with a single gun from each side in turn, whereas a newer method uses two guns to mill from both sides simultaneously.

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