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

1990 ◽  
Vol 199 ◽  
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.

TEM Characterization of As-Deposited and Annealed Ni/Al Multilayer Thin Film

2010 ◽  
Vol 16 (6) ◽  
pp. 662-669 ◽  
Author(s):  
S. Simões ◽  
F. Viana ◽  
A.S. Ramos ◽  
M.T. Vieira ◽  
M.F. Vieira
Keyword(s):  
Electron Microscopy ◽  
Thin Films ◽  
Transmission Electron Microscopy ◽  
Cross Section ◽  
Ion Beam ◽  
Microstructural Characterization ◽  
Multilayer Thin Films ◽  
Tem Analysis ◽  
Plan View ◽  
Transmission Electron

AbstractReactive multilayer thin films that undergo highly exothermic reactions are attractive choices for applications in ignition, propulsion, and joining systems. Ni/Al reactive multilayer thin films were deposited by dc magnetron sputtering with a period of 14 nm. The microstructure of the as-deposited and heat-treated Ni/Al multilayers was studied by transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) in plan view and in cross section. The cross-section samples for TEM and STEM were prepared by focused ion beam lift-out technique. TEM analysis indicates that the as-deposited samples were composed of Ni and Al. High-resolution TEM images reveal the presence of NiAl in small localized regions. Microstructural characterization shows that heat treating at 450 and 700°C transforms the Ni/Al multilayered structure into equiaxed NiAl fine grains.

Orientational and Microstructural Evolution During Epitaxial Growth of Cu on Si(001) by Sputter Deposition

1992 ◽  
Vol 280 ◽  
Author(s):  
I. Hashim ◽  
B. Park ◽  
H. A. Atwater
Keyword(s):  
Epitaxial Growth ◽  
Ion Beam ◽  
High Energy ◽  
Sputter Deposition ◽  
X Ray Diffraction ◽  
Cross Sectional ◽  
Plan View ◽  
Transmission Electron

ABSTRACTEpitaxial Cu thin films have been grown on H-terminated Si(OOl) substrates at room temperature by D.C. ion-beam sputter deposition in ultrahigh vacuum. The development of orientation and microstructure during epitaxial growth from the initial stages of Cu growth up to Cu thicknesses of few hundred nm has been investigated. Analysis by in-situ reflection high energy electron diffraction, thin film x-ray diffraction, and plan-view and cross-sectional transmission electron microscopy indicates that the films are well textured with Cu(001)∥ Si(001) and Cu[100]∥ Si[110]. Interestingly, it is found that a distribution of orientations occurs at the early stages of Cu epitaxy on Si(001) surface, and that a (001) texture emerges gradually with increasing Cu thickness. The effect of silicide formation and deposition conditions on the crystalline quality of Cu epitaxy is also discussed.

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

2003 ◽  
Vol 763 ◽  
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.

Influence of Rapid Thermal Annealing on Shallow BF2 Implantation into Pre-Amorphized Silicon

1983 ◽  
Vol 23 ◽  
Author(s):  
W. Maszara ◽  
C. Carter ◽  
D. K. Sadana ◽  
J. Liu ◽  
V. Ozguz ◽  
...  
Keyword(s):  
Thermal Annealing ◽  
Rapid Thermal Annealing ◽  
Ion Beam ◽  
Liquid Nitrogen Temperature ◽  
Structural Defects ◽  
Structural Quality ◽  
Halogen Lamp ◽  
Cross Sectional ◽  
Plan View ◽  
Transmission Electron

ABSTRACTLow energy, shallow BF2+ implants were carried out at room or liquid nitrogen temperature into deep pre-amorphized (100) Si for better control of the dopant profile and post-annealing structural defects. Cross sectional and angle polished plan view transmission electron microscopy were used to study the structural quality of the implanted layer, while SIMS provided a chemical profile. Four types of structural defects were observed in BF2+ implanted, pre-amorphized samples following rapid thermal annealing with a halogen lamp. An in-situ ion beam annealing and the presence of F in the Si lattice were related to the creation of the defects. Good correlations between F gettering and TEM observed defects were found to exist. Implantation of B+ into a pre-amorphized Si surface and subsequent rapid thermal annealing was found to produce a wide defect-free surface layer.

Rocking-Angle Ion-Milling of Cross-Sectional Samples for Transmission Electron Microscopy of Multi-Layer Systems

1997 ◽  
Vol 480 ◽  
Author(s):  
Jeong Soo Lee ◽  
Hyun Ha Kim ◽  
Young Woo Jeong
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Incidence Angle ◽  
Ion Beam ◽  
Quantitative Information ◽  
Ion Milling ◽  
Angle Variation ◽  
Cross Sectional ◽  
Transmission Electron ◽  
The Cross

AbstractThe cross-sectional transmission electron microscopy (TEM) specimens of Pt/Ti/SiO2/Si, RuO2/SiO2/Si, W/TiN/SiO2/Si, (Pb,La)TiO3/Pt/MgO, Bi4Ti3O12/Lal-xCaxMnO3/MgO, and GaN/Al2O3 were successfully made by the rocking-angle ion-milling technique. The differential thinning problems could be effectively mitigated when the rocking-angle and the ion-beam incidence angle were optimized for each heterostructure. It was found that the sputtering yield ratio between the layer milled most quickly and the layer milled most slowly is one of the important factors which determine the optimum rocking-angle ion-milling condition. The atomic force microscopy study on the surface topography of the cross-sectional Pt/Ti/SiO2/Si TEM sample after ion-milling provided quantitative information about the effects of the rocking-angle variation. A parameter which is the ratio between the layer with a minimum electron transparency and the layer with a maximum electron transparency was suggested.

scholarly journals Having Your Cake and Eating It Too: A Procedure for Obtaining Plan View and Cross Section TEM Images from the Same Site

2005 ◽  
Vol 13 (1) ◽  
pp. 26-29 ◽  
Author(s):  
R.B. Irwin ◽  
A. Anciso ◽  
P.J. Jones ◽  
C. Patton
Keyword(s):  
Sample Preparation ◽  
Cross Section ◽  
Focused Ion Beam ◽  
Bulk Material ◽  
Ion Beam ◽  
Preparation Technique ◽  
Ion Milling ◽  
Plan View ◽  
Transmission Electron ◽  
Final Sample

Sample preparation for Transmission Electron Microscopy (TEM) is usually performed such that the final sample orientation is either a cross section or a plan view of the bulk material, as shown schematically in Figure 1. The object of any sample preparation technique, for either of these two orientations, is to thin a selected volume of the sample from its initial bulk state to electron transparency, ~ 100nm thick. In doing so, the final sample must be mechanically stable, vacuum compatible, and, most of all, unchanged from the initial bulk material. Many techniques have been used to achieve this goal: cleaving, sawing, mechanical polishing, chemical etching, ion milling, focused ion beam (FIB) milling, and many others.

The Morphology of YBa2Cu3O7−x Thin Films Grown on Ceramic Substrates

1987 ◽  
Vol 99 ◽  
Author(s):  
L. A. Tietz ◽  
B. C. De Cooman ◽  
C. B. Carter ◽  
D. K. Lathrop ◽  
S. E. Russek ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Thin Films ◽  
Transmission Electron Microscopy ◽  
Single Crystal ◽  
Ion Beam ◽  
Substrate Surface ◽  
The Other ◽  
Ceramic Substrates ◽  
Transmission Electron ◽  
Beam Damage

ABSTRACTThe microstructure of thin films of the high Tc superconductor YBa2Cu3O7−x deposited on SrTiO3 and Y-stabilized cubic-zirconia (YSZ) single-crystal substrates has been characterized by transmission electron microscopy. Films on both substrates were polycrystalline. On {001 }-oriented SrTiO3, the grains are oriented with <110> normal to the substrate surface. On the same orientation of YSZ, two microstructures are observed: one in which grains have their c-axes normal to the substrate surface, the other in which grains have the a- (or b-) axis normal to the substrate surface. Both of these microstructures contain special grain boundaries. Annealing of ion-milled TEM specimens is presented as a means of removing ion-beam damage.

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

2014 ◽  
Vol 20 (5) ◽  
pp. 1471-1478 ◽  
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< $$ 11\bar 20 $$ >.

Transmission electron microscopy study of the structure of radio frequency sputter-deposited yttria-stabilized zirconia thin films

2003 ◽  
Vol 18 (1) ◽  
pp. 195-200 ◽  
Author(s):  
David E. Ruddell ◽  
Brian R. Stoner ◽  
Jeffrey Y. Thompson
Keyword(s):  
Electron Microscopy ◽  
Thin Films ◽  
Transmission Electron Microscopy ◽  
Yttria Stabilized Zirconia ◽  
Stabilized Zirconia ◽  
Cross Sectional ◽  
Plan View ◽  
Oxygen Levels ◽  
Transmission Electron ◽  
Sputter Deposited

Transmission electron microscopy (TEM) was used to investigate the structural properties of sputter-deposited yttria-stabilized zirconia (YSZ) thin films. YSZ films were deposited over a range of temperatures and background oxygen levels. Additionally, a multilayered structure was produced by cyclic application of a substrate bias. Plan-view TEM showed that temperature and oxygen levels did not have a significant effect on grain size but did alter the phases present in the thin films. Cross-sectional TEM showed the development of texture in the multilayer film, both within the individual layers and in the entire film.

Techniques of Insulator/Semiconductor Heterostructure Specimen Preparation

1987 ◽  
Vol 115 ◽  
Author(s):  
D. Bahnck ◽  
J. L. Batstone ◽  
Julia M. Phillips
Keyword(s):  
Specimen Preparation ◽  
Silicon Substrates ◽  
Ion Milling ◽  
Transmission Electron Microscopy Analysis ◽  
Cross Sectional ◽  
Plan View ◽  
Transmission Electron ◽  
Electron Microscopy Analysis ◽  
Microscopy Analysis ◽  
Argon Ion

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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