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

Author(s):  
Mohan Krishnamurthy ◽  
Jeff S. Drucker ◽  
John A. Venablest

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.

1990 ◽  
Vol 198 ◽  
Author(s):  
Mohan Krishnamurthy ◽  
Jeff S. Drucker ◽  
J.A. Venables

ABSTRACTThe initial stages of germanium heteroepitaxy on vicinal Si(100) have been studied using in-situ deposition in a UHV STEM. Germanium was deposited using molecular beam techniques onto substrates misoriented 1° and 5* toward <110> held at room temperature, 375°C and 525°C. Film thicknesses were in the range 4-6 ML, just greater than the stable intermediate layer of 3-4ML (1ML = 0.14nm). The Ge clusters were observed using biassed secondary electron (b-SE) imaging with nanometer resolution. Comparisons were made between deposition at the elevated temperatures, and room temperature deposition followed by anneals at the same temperatures.Annealing the low temperature deposits produces coarsening of the islands which is similar on the 1° and 5° samples. Island size distributions and other film growth parameters obtained from the 375°C and 525°C anneals indicate that the coarsening is different at these temperatures and is possibly affected by instabilities in the intermediate layer. Results of the high temperature depositions indicate that neither surface steps nor the edges of islands act as perfect sinks, and that diffusion distances are of the order of several microns. The nucleation density and size distributions are markedly different for deposition at 375°C and 525°C possibly due to competitive capture at strong sinks.In a parallel set of experiments in a standard UHV chamber, macroscopic wafer samples were analyzed with RHEED, Auger and secondary electron spectroscopy. These correlate well with the intermediate layer thicknesses previously reported in the literature, and the large contrast observed in the b-SE images. Ex situ TEM studies of samples grown in this chamber show islands with various contrast features including those of coherent strain.


Author(s):  
A. J. Bleeker ◽  
P. Kruit

Combining of the high spatial resolution of a Scanning Transmission Electron Microscope and the wealth of information from the secondary electrons and Auger spectra opens up new possibilities for materials research. In a prototype instrument at the Delft University of Technology we have shown that it is possible from the optical point of view to combine STEM and Auger spectroscopy [1]. With an Electron Energy Loss Spectrometer attached to the microscope it also became possible to perform coincidence measurements between the secondary electron signal and the EELS signal. We measured Auger spectra of carbon aluminium and Argon gas showing energy resolutions better than 1eV [2]. The coincidence measurements on carbon with a time resolution of 5 ns yielded basic insight in secondary electron emission processes [3]. However, for serious Auger spectroscopy, the specimen needs to be in Ultra High Vacuum. ( 10−10 Torr ). At this moment a new setup is in its last phase of construction.


Author(s):  
P. Xu ◽  
E. J. Kirkland ◽  
J. Silcox

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.


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.


2017 ◽  
Vol 608 ◽  
pp. A50 ◽  
Author(s):  
M. Bertin ◽  
M. Doronin ◽  
X. Michaut ◽  
L. Philippe ◽  
A. Markovits ◽  
...  

Context. Almost 20% of the ~200 different species detected in the interstellar and circumstellar media present a carbon atom linked to nitrogen by a triple bond. Of these 37 molecules, 30 are nitrile R-CN compounds, the remaining 7 belonging to the isonitrile R-NC family. How these species behave in their interactions with the grain surfaces is still an open question. Aims. In a previous work, we have investigated whether the difference between nitrile and isonitrile functional groups may induce differences in the adsorption energies of the related isomers at the surfaces of interstellar grains of various nature and morphologies. This study is a follow up of this work, where we focus on the adsorption on carbonaceous aromatic surfaces. Methods. The question is addressed by means of a concerted experimental and theoretical approach of the adsorption energies of CH3CN and CH3NC on the surface of graphite (with and without surface defects). The experimental determination of the molecule and surface interaction energies is carried out using temperature-programmed desorption in an ultra-high vacuum between 70 and 160 K. Theoretically, the question is addressed using first-principle periodic density functional theory to represent the organised solid support. Results. The adsorption energy of each compound is found to be very sensitive to the structural defects of the aromatic carbonaceous surface: these defects, expected to be present in a large numbers and great diversity on a realistic surface, significantly increase the average adsorption energies to more than 50% as compared to adsorption on perfect graphene planes. The most stable isomer (CH3CN) interacts more efficiently with the carbonaceous solid support than the higher energy isomer (CH3NC), however.


2000 ◽  
Vol 6 (S2) ◽  
pp. 750-751
Author(s):  
David C Joy ◽  
David Braski

It has been estimated that more than 90% of all scanning electron microscope (SEM) images ever published have been obtained using secondary electrons (SE) which are defined as being those electrons emitted with energies between 0 and 50eV. The properties of these secondary electron are therefore of considerable interest and importance. However, although secondary electrons have been intensively studied since their discovery by Starke in 1901 the majority of the work has been aimed at determining the SE yield coefficient and its variation with energy for elements and compounds. The energy spectrum of secondary electrons has received far less attention although it is evident that the form of the spectrum must have an effect on the image contrast observed in the SEM because SE detectors are energy selective devices. The few studies that have been made have mostly concentrated on spectra obtained from clean samples observed under ultra-high vacuum conditions. This is understandable, because it is certain that the presence of a surface layer of contamination will change the SE spectrum to some degree or other, but it is unfortunate because all specimens in real SEMs are dirty and it is information about this situation that is required.


1992 ◽  
Vol 295 ◽  
Author(s):  
M. R. Scheinfein ◽  
J. S. Drucker ◽  
J. Liu ◽  
J. K. Weiss ◽  
G. G. Hembree ◽  
...  

AbstractThe secondary electron generation process is studied in an ultra-high vacuum scanning transmission electron microscope using electron coincidence spectroscopy. Production pathways for secondary electrons are determined by analyzing coincidences between secondary electrons and individual excitation events. The ultimate spatial resolution available in scanning electron microscopy is limited by the delocalization of the secondary electron generation process. This delocalization is studied using momentum resolved coincidence electron spectroscopy. The fraction of secondary electrons resulting from localized excitations can explain the high spatial resolution observed in secondary electron microscopy images.


1989 ◽  
Vol 159 ◽  
Author(s):  
J. Osaka ◽  
N. Inoue

ABSTRACTAn ultra high vacuum scanning electron microscope equipped to an MBE system is utilized to study a transient of a surface atomic structure during MBE growth of GaAs and AlGaAs by the alternate supply method. Lateral growth of a Ga-monolayer over microns is realized utilizing Ga droplets. This is confirmed by discriminating the Ga and As top layer by using the secondary electron intensity difference between the Ga and As top layer. The growth mechanism of the Ga monolayer is discussed based on the results.


2012 ◽  
Vol 571 ◽  
pp. 564-568
Author(s):  
Zhi Dan Yan ◽  
Li Dong Sun ◽  
Chun Guang Hu ◽  
Xiao Tang Hu ◽  
Peter Zeppenfeld

Deposition temperature is a key factor influencing the growth morphology of thin-films, aiming at this phenomenon, a precise control system of deposition temperature in ultra-high vacuum is developed in the paper. It can realize accurate temperature control in a range of 150K to 450K during experiment by combination of resistance heating up and liquid helium cooling down strategies, which is benefit to further understand the temperature-depended mechanism of organic molecule thin-film growth. Besides, it is experimentally studied that the growth morphology of p-6p molecules on a mica substrate is closely related to the substrate deposition temperature, indicating that the length of p-6p nano-fibers is proportional to the deposition temperature, while their distribution density is inversely proportional to the temperature.


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