Water Wettability Coupled with Film Growth on Realistic Cyclopentane Hydrate Surfaces

1973 ◽

Vol 31 ◽

pp. 122-123

Author(s):

J. S. Maa ◽

Thos. E. Hutchinson

Keyword(s):

Epitaxial Growth ◽

Film Growth ◽

Ion Beam ◽

Ion Beam Sputtering ◽

Microscopy Technique ◽

Direct Observations ◽

In Situ Electron Microscopy ◽

Beam Sputtering ◽

The Subject

The growth of Ag films deposited on various substrate materials such as MoS2, mica, graphite, and MgO has been investigated extensively using the in situ electron microscopy technique. The three stages of film growth, namely, the nucleation, growth of islands followed by liquid-like coalescence have been observed in both the vacuum vapor deposited and ion beam sputtered thin films. The mechanisms of nucleation and growth of silver films formed by ion beam sputtering on the (111) plane of silicon comprise the subject of this paper. A novel mode of epitaxial growth is observed to that seen previously.The experimental arrangement for the present study is the same as previous experiments, and the preparation procedure for obtaining thin silicon substrate is presented in a separate paper.

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Microstructural characterization of YBa2Cu3O7-x thin films formed by metalorganic CVD

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100089718 ◽

1991 ◽

Vol 49 ◽

pp. 1080-1081

Author(s):

P. Lu ◽

W. Huang ◽

C.S. Chern ◽

Y.Q. Li ◽

J. Zhao ◽

...

Keyword(s):

Thin Film ◽

Thin Films ◽

Critical Current Density ◽

Critical Current ◽

Current Density ◽

Film Growth ◽

Chemical Vapor ◽

Microstructural Characterization ◽

Ion Milling ◽

Conventional Grinding

The YBa2Cu3O7-x thin films formed by metalorganic chemical vapor deposition(MOCVD) have been reported to have excellent superconducting properties including a sharp zero resistance transition temperature (Tc) of 89 K and a high critical current density of 2.3x106 A/cm2 or higher. The origin of the high critical current in the thin film compared to bulk materials is attributed to its structural properties such as orientation, grain boundaries and defects on the scale of the coherent length. In this report, we present microstructural aspects of the thin films deposited on the (100) LaAlO3 substrate, which process the highest critical current density.Details of the thin film growth process have been reported elsewhere. The thin films were examined in both planar and cross-section view by electron microscopy. TEM sample preparation was carried out using conventional grinding, dimpling and ion milling techniques. Special care was taken to avoid exposure of the thin films to water during the preparation processes.

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The annealed (0001) α-alumina surface and its influence on thin-film growth

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100138051 ◽

1995 ◽

Vol 53 ◽

pp. 336-337

Author(s):

Michael W. Bench ◽

Paul G. Kotula ◽

C. Barry Carter

Keyword(s):

Electron Microscopy ◽

Surface Energy ◽

Film Growth ◽

Thin Film Growth ◽

Energy Calculations ◽

Transmission Electron ◽

Reflection Electron Microscopy ◽

Low Energy Electron ◽

Surface Nature

The growth of semiconductors, superconductors, metals, and other insulators has been investigated using alumina substrates in a variety of orientations. The surface state of the alumina (for example surface reconstruction and step nature) can be expected to affect the growth nature and quality of the epilayers. As such, the surface nature has been studied using a number of techniques including low energy electron diffraction (LEED), reflection electron microscopy (REM), transmission electron microscopy (TEM), molecular dynamics computer simulations, and also by theoretical surface energy calculations. In the (0001) orientation, the bulk alumina lattice can be thought of as a layered structure with A1-A1-O stacking. This gives three possible terminations of the bulk alumina lattice, with theoretical surface energy calculations suggesting that termination should occur between the Al layers. Thus, the lattice often has been described as being made up of layers of (Al-O-Al) unit stacking sequences. There is a 180° rotation in the surface symmetry of successive layers and a total of six layers are required to form the alumina unit cell.

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Direct STEM ADF imaging of gold on silicon (111)

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100154330 ◽

1989 ◽

Vol 47 ◽

pp. 472-473

Author(s):

P. Xu ◽

E. J. Kirkland ◽

J. Silcox

Keyword(s):

Film Growth ◽

Heavy Atom ◽

High Vacuum ◽

Dark Field ◽

Thin Metal Film ◽

Base Pressure ◽

Ultra High Vacuum ◽

Specimen Preparation ◽

Dark Field Imaging ◽

Wide Range

Many studies of thin metal film growth and the formation of metal-semiconductor contacts have been performed using a wide range of experimental methods. STEM annular dark field imaging could be an important complement since it may allow direct imaging of a single heavy atom on a thin silicon substrate. This would enable studies of the local atomic arrangements and defects in the initial stage of metal silicide formation.Preliminary experiments were performed in an ultra-high vacuum VG HB501A STEM with a base pressure of 1 × 10-10 mbar. An antechamber directly attached to the microscope for specimen preparation has a base pressure of 2×l0-10 mbar. A thin single crystal membrane was fabricated by anodic etching and subsequent reactive etching. The specimen was cleaned by the Shiraki method and had a very thin oxide layer left on the surface. 5 Å of gold was deposited on the specimen at room temperature from a tungsten filament coil monitored by a quartz crystal monitor.

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Microstructural characterization of YBaCuO Films on LaAlO3 substrates

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100152872 ◽

1989 ◽

Vol 47 ◽

pp. 180-181

Author(s):

E. L. Hall ◽

A. Mogro-Campero ◽

N. Lewis ◽

L. G. Turner

Keyword(s):

Dielectric Constant ◽

Single Crystal ◽

Film Growth ◽

Microstructural Characterization ◽

Lattice Parameter ◽

Film Plane ◽

Substrate Material ◽

High Loss ◽

Amorphous Substrates ◽

High Dielectric

There have been a large number of recent studies of the growth of Y-Ba-Cu-O thin films, and these studies have employed a variety of substrates and growth techniques. To date, the highest values of Tc and Jc have been found for films grown by sputtering or coevaporation on single-crystal SrTiO3 substrates, which produces a uniaxially-aligned film with the YBa2Cu3Ox c-axis normal to the film plane. Multilayer growth of films on the same substrate produces a triaxially-aligned film (regions of the film have their c-axis parallel to each of the three substrate <100> directions) with lower values of Jc. Growth of films on a variety of other polycrystalline or amorphous substrates produces randomly-oriented polycrystalline films with low Jc. Although single-crystal SrTiO3 thus produces the best results, this substrate material has a number of undesireable characteristics relative to electronic applications, including very high dielectric constant and a high loss tangent at microwave frequencies. Recently, Simon et al. have shown that LaAlO3 could be used as a substrate for YBaCuO film growth. This substrate is essentially a cubic perovskite with a lattice parameter of 0.3792nm (it has a slight rhombohedral distortion at room temperature) and this material exhibits much lower dielectric constant and microwave loss tangents than SrTiO3. It is also interesting from a film growth standpoint since it has a slightly smaller lattice parameter than YBa2Cu3Ox (a=0.382nm, b=c/3=0.389nm), while SrTiO3 is slightly larger (a=0.3905nm).

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Modifications of a JEOL 2000EX TEM for insSitu surface studies

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100149039 ◽

1993 ◽

Vol 51 ◽

pp. 640-641

Author(s):

Michael T. Marshall ◽

Xianghong Tong ◽

J. Murray Gibson

Keyword(s):

Electron Diffraction ◽

Surface Science ◽

Film Growth ◽

High Vacuum ◽

High Energy ◽

Energy Electron ◽

Ultra High Vacuum ◽

Transmission Electron ◽

Fundamental Insight

We have modified a JEOL 2000EX Transmission Electron Microscope (TEM) to allow in-situ ultra-high vacuum (UHV) surface science experiments as well as transmission electron diffraction and imaging. Our goal is to support research in the areas of in-situ film growth, oxidation, and etching on semiconducter surfaces and, hence, gain fundamental insight of the structural components involved with these processes. The large volume chamber needed for such experiments limits the resolution to about 30 Å, primarily due to electron optics. Figure 1 shows the standard JEOL 2000EX TEM. The UHV chamber in figure 2 replaces the specimen area of the TEM, as shown in figure 3. The chamber is outfitted with Low Energy Electron Diffraction (LEED), Auger Electron Spectroscopy (AES), Residual Gas Analyzer (RGA), gas dosing, and evaporation sources. Reflection Electron Microscopy (REM) is also possible. This instrument is referred to as SHEBA (Surface High-energy Electron Beam Apparatus).The UHV chamber measures 800 mm in diameter and 400 mm in height. JEOL provided adapter flanges for the column.

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Microstructural observations of the “Wustite-Spinel” coexistence following quenching of cation-excess spinels, Ni2(1+x)Ti1-xO4

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100178422 ◽

1990 ◽

Vol 48 (4) ◽

pp. 1058-1059

Author(s):

Ian M. Anderson ◽

Arnulf Muan ◽

C. Barry Carter

Keyword(s):

Film Growth ◽

Spinel Phase ◽

Model Systems ◽

Ion Milling ◽

Coexistence Of Phases ◽

Nonequilibrium Conditions ◽

Diffraction Patterns ◽

Spinel Structures ◽

Highly Porous ◽

Standard Techniques

Oxide mixtures which feature a coexistence of phases with the wüstite and spinel structures are considered model systems for the study of solid-state reaction kinetics, phase boundaries, and thin-film growth, and such systems are especially suited to TEM studies. (In this paper, the terms “wüstite” and “spinel” will refer to phases of those structure types.) The study of wüstite-spinel coexistence has been limited mostly to systems near their equilibrium condition, where the assumptions of local thermodynamic equilibrium are valid. The cation-excess spinels of the type Ni2(1+x)Ti1-xO4, which reportedly exist only above 1375°C4, provide an excellent system for the study of wüstite-spinel coexistence under highly nonequilibrium conditions. The nature of these compounds has been debated in the literature. X-ray and neutron powder diffraction patterns have been used to advocate the existence of a single-phase, non- stoichiometric spinel. TEM studies of the microstructure have been used to suggest equilibrium coexistence of a stoichiometric spinel, Ni2TiO4, and a wüstite phase; this latter study has shown a coexistence of wüstite and spinel phases in specimens thought to have been composed of a single, non- stoichiometric spinel phase. The microstructure and nature of this phase coexistence is the focus of this study. Specimens were prepared by ball-milling a mixture of NiO and TiO2 powders with 10 wt.% TiO2. The mixture was fired in air at 1483°C for 5 days, and then quenched to room temperature. The aggregate thus produced was highly porous, and needed to be infiltrated prior to TEM sample preparation, which was performed using the standard techniques of lapping, dimpling, and ion milling.

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Studies of Ge/Si(100) and Observation of Atomic Steps on Si(100) using Biassed Secondary Electron Imaging in a UHV STEM

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s042482010018029x ◽

1990 ◽

Vol 48 (1) ◽

pp. 308-309

Author(s):

Mohan Krishnamurthy ◽

Jeff S. Drucker ◽

John A. Venablest

Keyword(s):

Secondary Electron ◽

Critical Thickness ◽

Surface Defects ◽

Film Growth ◽

Growth Parameters ◽

High Vacuum ◽

Ultra High Vacuum ◽

Surface Steps ◽

Epitaxial Crystal Growth ◽

Electron Imaging

Secondary Electron Imaging (SEI) has become a useful mode of studying surfaces in SEM[1] and STEM[2,3] instruments. Samples have been biassed (b-SEI) to provide increased sensitivity to topographic and thin film deposits in ultra high vacuum (UHV)-SEM[1,4]; but this has not generally been done in previous STEM studies. The recently developed UHV-STEM ( codenamed MIDAS) at ASU has efficient collection of secondary electrons using a 'parallelizer' and full sample preparation system[5]. Here we report in-situ deposition and annealing studies on the Ge/Si(100) epitaxial system, and the observation of surface steps on vicinal Si(100) using b-SEI under UHV conditions in MIDAS.Epitaxial crystal growth has previously been studied using SEM and SAM based experiments [4]. The influence of surface defects such as steps on epitaxial growth requires study with high spatial resolution, which we report for the Ge/Si(100) system. Ge grows on Si(100) in the Stranski-Krastonov growth mode wherein it forms pseudomorphic layers for the first 3-4 ML (critical thickness) and beyond which it clusters into islands[6]. In the present experiment, Ge was deposited onto clean Si(100) substrates misoriented 1° and 5° toward <110>. This was done using a mini MBE Knudsen cell at base pressure ~ 5×10-11 mbar and at typical rates of 0.1ML/min (1ML =0.14nm). Depositions just above the critical thickness were done for substrates kept at room temperature, 375°C and 525°C. The R T deposits were annealed at 375°C and 525°C for various times. Detailed studies were done of the initial stages of clustering into very fine (∼1nm) Ge islands and their subsequent coarsening and facetting with longer anneals. From the particle size distributions as a function of time and temperature, useful film growth parameters have been obtained. Fig. 1 shows a b-SE image of Ge island size distribution for a R T deposit and anneal at 525°C. Fig.2(a) shows the distribution for a deposition at 375°C and Fig.2(b) shows at a higher magnification a large facetted island of Ge. Fig.3 shows a distribution of very fine islands from a 525°C deposition. A strong contrast is obtained from these islands which are at most a few ML thick and mottled structure can be seen in the background between the islands, especially in Fig.2(a) and Fig.3.

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