Growth of Niobium Films at High Temperatures on Sapphire

1996 ◽  
Vol 440 ◽  
Author(s):  
T. Wagner

AbstractThe growth and microstructural evolution of Nb thin films on the basal plane of α-Al2O3 were studied at different growth temperatures. The influence of island orientation, density, and misfit strain energy on the growth behavior of Nb films on (0001)α-Al2O3 at high temperatures has been investigated. The films were grown by MBE at 900°C and 1100°C. At these temperatures the Nb grows in the Volmer-Weber growth mode on the basal plane. In-situ reflection high energy electron diffraction (RHEED), Auger electron spectroscopy (AES) and transmission electron microscopy (TEM) investigations revealed that in the initial growth stage, Nb nuclei with different epitaxial orientations were formed. This leads to different orientations of thicker Nb films at different growth temperatures. At a growth temperature of 900°C the Nb{111} planes are parallel to the sapphire basal plane whereas at 1100°C Nb grows with the {110) planes parallel to the basal plane of sapphire. The formation of two different epitaxial orientations of thick Nb films can only be explained by considering both the change in the total density of Nb islands with temperature and the influence of island size on their total energy.

1998 ◽  
Vol 13 (3) ◽  
pp. 693-702 ◽  
Author(s):  
Thomas Wagner

Epitaxial Nb thin films were grown via molecular beam epitaxy (MBE) at different substrate temperatures on α–Al2O3(0001) substrates. For temperatures of 900 °C to 1100 °C, it was found that Nb grows in the Volmer–Weber growth mode (formation of three-dimensional crystallites). Depending on the growth temperature, different epitaxial orientations of Nb films can be found. At a growth temperature of 900 °C, the Nb{111} planes are parallel to the sapphire basal plane whereas at 1100 °C the Nb grows with the {110} planes on the basal plane of sapphire. These orientations are present even in the initial stages of growth at both temperatures. The formation of two different epitaxial orientations of thick Nb films can be conclusively explained only by considering both the change in the total density of Nb islands with temperature and the influence of island size on the total energy of the islands. The Nb island growth process has been investigated in situ using reflection high energy electron diffraction (RHEED) and Auger electron spectroscopy (AES). Scanning electron microscopy (SEM), x-ray diffraction (XRD), and transmission electron microscopy (TEM) were employed to determine the morphology and structure of Nb islands, Nb films, and Nb/α–Al2O3 interfaces.


1996 ◽  
Vol 449 ◽  
Author(s):  
N. Grandjean ◽  
J. Massies ◽  
P. Vennègues ◽  
M. Laugt ◽  
M. Leroux

ABSTRACTThe analysis of the sapphire surface nitridation by in situ reflection high-energy electron diffraction evidences the formation of a relaxed AIN layer. Its role on the early stage of the GaN growth is investigated by transmission electron microscopy (TEM). GaN crystallites of high structural quality, with the c axis perpendicular to the sapphire basal plane, are observed when the starting surface is nitridated. On the other hand, the growth of GaN on a bare substrate involves the formation of larger islands with numerous defects. TEM study reveals that the c axis of these latter crystallites is systematically tilted by about 19° with respect to the sapphire basal plane. Actually, this orientation corresponds to a particular epitaxial relationship between GaN and sapphire (0001) substrates. Finally, the optical properties of GaN thin layers are shown to be strongly dependent on the nitridation state of the sapphire surface.


Author(s):  
Z. L. Wang ◽  
J. Bentley

Studying the behavior of surfaces at high temperatures is of great importance for understanding the properties of ceramics and associated surface-gas reactions. Atomic processes occurring on bulk crystal surfaces at high temperatures can be recorded by reflection electron microscopy (REM) in a conventional transmission electron microscope (TEM) with relatively high resolution, because REM is especially sensitive to atomic-height steps.Improved REM image resolution with a FEG: Cleaved surfaces of a-alumina (012) exhibit atomic flatness with steps of height about 5 Å, determined by reference to a screw (or near screw) dislocation with a presumed Burgers vector of b = (1/3)<012> (see Fig. 1). Steps of heights less than about 0.8 Å can be clearly resolved only with a field emission gun (FEG) (Fig. 2). The small steps are formed by the surface oscillating between the closely packed O and Al stacking layers. The bands of dark contrast (Fig. 2b) are the result of beam radiation damage to surface areas initially terminated with O ions.


Author(s):  
Tai D. Nguyen ◽  
Ronald Gronsky ◽  
Jeffrey B. Kortright

Nanometer period Ru/C multilayers are one of the prime candidates for normal incident reflecting mirrors at wavelengths < 10 nm. Superior performance, which requires uniform layers and smooth interfaces, and high stability of the layered structure under thermal loadings are some of the demands in practical applications. Previous studies however show that the Ru layers in the 2 nm period Ru/C multilayer agglomerate upon moderate annealing, and the layered structure is no longer retained. This agglomeration and crystallization of the Ru layers upon annealing to form almost spherical crystallites is a result of the reduction of surface or interfacial energy from die amorphous high energy non-equilibrium state of the as-prepared sample dirough diffusive arrangements of the atoms. Proposed models for mechanism of thin film agglomeration include one analogous to Rayleigh instability, and grain boundary grooving in polycrystalline films. These models however are not necessarily appropriate to explain for the agglomeration in the sub-nanometer amorphous Ru layers in Ru/C multilayers. The Ru-C phase diagram shows a wide miscible gap, which indicates the preference of phase separation between these two materials and provides an additional driving force for agglomeration. In this paper, we study the evolution of the microstructures and layered structure via in-situ Transmission Electron Microscopy (TEM), and attempt to determine the order of occurence of agglomeration and crystallization in the Ru layers by observing the diffraction patterns.


Author(s):  
Yoshichika Bando ◽  
Takahito Terashima ◽  
Kenji Iijima ◽  
Kazunuki Yamamoto ◽  
Kazuto Hirata ◽  
...  

The high quality thin films of high-Tc superconducting oxide are necessary for elucidating the superconducting mechanism and for device application. The recent trend in the preparation of high-Tc films has been toward “in-situ” growth of the superconducting phase at relatively low temperatures. The purpose of “in-situ” growth is to attain surface smoothness suitable for fabricating film devices but also to obtain high quality film. We present the investigation on the initial growth manner of YBCO by in-situ reflective high energy electron diffraction (RHEED) technique and on the structural and superconducting properties of the resulting ultrathin films below 100Å. The epitaxial films have been grown on (100) plane of MgO and SrTiO, heated below 650°C by activated reactive evaporation. The in-situ RHEED observation and the intensity measurement was carried out during deposition of YBCO on the substrate at 650°C. The deposition rate was 0.8Å/s. Fig. 1 shows the RHEED patterns at every stage of deposition of YBCO on MgO(100). All the patterns exhibit the sharp streaks, indicating that the film surface is atomically smooth and the growth manner is layer-by-layer.


Author(s):  
Xianghong Tong ◽  
Oliver Pohland ◽  
J. Murray Gibson

The nucleation and initial stage of Pd2Si crystals on Si(111) surface is studied in situ using an Ultra-High Vacuum (UHV) Transmission Electron Microscope (TEM). A modified JEOL 200CX TEM is used for the study. The Si(111) sample is prepared by chemical thinning and is cleaned inside the UHV chamber with base pressure of 1x10−9 τ. A Pd film of 20 Å thick is deposited on to the Si(111) sample in situ using a built-in mini evaporator. This room temperature deposited Pd film is thermally annealed subsequently to form Pd2Si crystals. Surface sensitive dark field imaging is used for the study to reveal the effect of surface and interface steps.The initial growth of the Pd2Si has three stages: nucleation, growth of the nuclei and coalescence of the nuclei. Our experiments shows that the nucleation of the Pd2Si crystal occurs randomly and almost instantaneously on the terraces upon thermal annealing or electron irradiation.


Author(s):  
D. Loretto ◽  
J. M. Gibson ◽  
S. M. Yalisove

The silicides CoSi2 and NiSi2 are both metallic with the fee flourite structure and lattice constants which are close to silicon (1.2% and 0.6% smaller at room temperature respectively) Consequently epitaxial cobalt and nickel disilicide can be grown on silicon. If these layers are formed by ultra high vacuum (UHV) deposition (also known as molecular beam epitaxy or MBE) their thickness can be controlled to within a few monolayers. Such ultrathin metal/silicon systems have many potential applications: for example electronic devices based on ballistic transport. They also provide a model system to study the properties of heterointerfaces. In this work we will discuss results obtained using in situ and ex situ transmission electron microscopy (TEM).In situ TEM is suited to the study of MBE growth for several reasons. It offers high spatial resolution and the ability to penetrate many monolayers of material. This is in contrast to the techniques which are usually employed for in situ measurements in MBE, for example low energy electron diffraction (LEED) and reflection high energy electron diffraction (RHEED), which are both sensitive to only a few monolayers at the surface.


Author(s):  
Michael T. Marshall ◽  
Xianghong Tong ◽  
J. Murray Gibson

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.


2019 ◽  
Vol 10 (1) ◽  
Author(s):  
Wei Han ◽  
Pu Huang ◽  
Liang Li ◽  
Fakun Wang ◽  
Peng Luo ◽  
...  

Abstract Two-dimensional molecular crystals, consisting of zero-dimensional molecules, are very appealing due to their novel physical properties. However, they are mostly limited to organic molecules. The synthesis of inorganic version of two-dimensional molecular crystals is still a challenge due to the difficulties in controlling the crystal phase and growth plane. Here, we design a passivator-assisted vapor deposition method for the growth of two-dimensional Sb2O3 inorganic molecular crystals as thin as monolayer. The passivator can prevent the heterophase nucleation and suppress the growth of low-energy planes, and enable the molecule-by-molecule lateral growth along high-energy planes. Using Raman spectroscopy and in situ transmission electron microscopy, we show that the insulating α-phase of Sb2O3 flakes can be transformed into semiconducting β-phase under heat and electron-beam irradiation. Our findings can be extended to the controlled growth of other two-dimensional inorganic molecular crystals and open up opportunities for potential molecular electronic devices.


1996 ◽  
Vol 441 ◽  
Author(s):  
J. Marien ◽  
T. Wagner ◽  
M. Rühle

AbstractThin Nb films were grown by MBE in a UHV chamber at two different temperatures (50°C and 950°C) on the (110) surface of TiO2 (rutile).At a growth temperature of 50°C, reflection high energy electron diffraction (RHEED) revealed epitaxial growth of Nb on rutile: (110)[001] TiO2 ¦¦ (100)[001] Nb. In addition, investigations with Auger electron spectroscopy (AES) revealed that a chemical reaction took place between the Nb overlayer and the TiO2 substrate at the initial growth stage. A 2 nm thick reaction layer at the Nb/TiO2 interface has been identified by means of conventional transmission electron microscopy (CTEM) and high-resolution transmission electron microscopy (HRTEM).At a substrate temperature of 950°C, during growth, the Nb film was oxidized completely, and NbO2 grew epitaxially on TiO2. The structure and the chemical composition of the overlayers have been investigated by RHEED, AES, CTEM and HRTEM. Furthermore, it was determined that the reaction of Nb with TiO2 is governed by the defect structure of the TiO2 and the relative oxygen affinities of Nb and TiO2.


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