Specimen heating stage with in-situ evaporator in UHV-STEM for the observation and characterization of monolayered superstructures

Author(s):  
M. Ohtsuki ◽  
J.J. Schuler ◽  
A.V. Crewe ◽  
T. Ichinokawa

In-situ evaporating experiments on solid surfaces become meaningful only when the evaporation takes place after the surface of the object is fully cleaned in ultra high vacuum (UHV). A specimen heating stage is usually used for the cleaning process.For the observation of single heavy atom superstructures at atomic resolution in UHV, we have constructed a new specimen heating stage equipped with an insitu evaporator. The device is built into the specimen ante-chamber of the high-resolution UHV-STEM as shown in Figures 1 and 2. The vacuum of the chamber has been tested at 4 × 10-10 torr. with two 20 ℓ/ sec ion pumps attached close to the chamber. The vacuum of the STEM column is better than 1 × 10-10 torr. The heating stage is built into the specimen holder so that direct heating of the specimen is possible. In the detail shown in Figure 2, a thin specimen is mounted between two supporting grids which are then fastened together by two semi-circular tantalum clips. These clips are also used as contacts which carry the current to heat the specimen directly.

1997 ◽  
Vol 477 ◽  
Author(s):  
C. L. Petersen ◽  
F. Grey

ABSTRACTWe have investigated the oxidation of clean reconstructed silicon surfaces in-situ using a fourpoint probe technique. The measured conductance variations, on Si(111) and Si(100) surfaces as a function of oxygen exposure are markedly different. On Si(100) surfaces, the conductance displays a rapid fall during the first 100 L exposure to O2, followed by a slower steady decrease at higher oxygen exposures. This behavior is similar for both n-type arid p-type silicon. The conductance of Si(111) surfaces increases significantly at the onset of the oxidation. This conductance increase is found on both n-type and p-type Si(111) samples. We interpret this as being due to the molecular precursor which is known to form in the peroxy bridge position.


2020 ◽  
Vol 91 (8) ◽  
pp. 085109 ◽  
Author(s):  
G. Vinai ◽  
F. Motti ◽  
A. Yu. Petrov ◽  
V. Polewczyk ◽  
V. Bonanni ◽  
...  

Author(s):  
L. E. Murr ◽  
G. Wong

Palladium single-crystal films have been prepared by Matthews in ultra-high vacuum by evaporation onto (001) NaCl substrates cleaved in-situ, and maintained at ∼ 350° C. Murr has also produced large-grained and single-crystal Pd films by high-rate evaporation onto (001) NaCl air-cleaved substrates at 350°C. In the present work, very large (∼ 3cm2), continuous single-crystal films of Pd have been prepared by flash evaporation onto air-cleaved (001) NaCl substrates at temperatures at or below 250°C. Evaporation rates estimated to be ≧ 2000 Å/sec, were obtained by effectively short-circuiting 1 mil tungsten evaporation boats in a self-regulating system which maintained an optimum load current of approximately 90 amperes; corresponding to a current density through the boat of ∼ 4 × 104 amperes/cm2.


Author(s):  
J. E. O'Neal ◽  
J. J. Bellina ◽  
B. B. Rath

Thin films of the bcc metals vanadium, niobium and tantalum were epitaxially grown on (0001) and sapphire substrates. Prior to deposition, the mechanical polishing damage on the substrates was removed by an in-situ etch. The metal films were deposited by electron-beam evaporation in ultra-high vacuum. The substrates were heated by thermal contact with an electron-bombarded backing plate. The deposition parameters are summarized in Table 1.The films were replicated and examined by electron microscopy and their crystallographic orientation and texture were determined by reflection electron diffraction. Verneuil-grown and Czochralskigrown sapphire substrates of both orientations were employed for each evaporation. The orientation of the metal deposit was not affected by either increasing the density of sub-grain boundaries by about a factor of ten or decreasing the deposition rate by a factor of two. The results on growth epitaxy are summarized in Tables 2 and 3.


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

The cobalt disilicide/silicon system has potential applications as a metal-base and as a permeable-base transistor. Although thin, low defect density, films of CoSi2 on Si(111) have been successfully grown, there are reasons to believe that Si(100)/CoSi2 may be better suited to the transmission of electrons at the silicon/silicide interface than Si(111)/CoSi2. A TEM study of the formation of CoSi2 on Si(100) is therefore being conducted. We have previously reported TEM observations on Si(111)/CoSi2 grown both in situ, in an ultra high vacuum (UHV) TEM and ex situ, in a conventional Molecular Beam Epitaxy system.The procedures used for the MBE growth have been described elsewhere. In situ experiments were performed in a JEOL 200CX electron microscope, extensively modified to give a vacuum of better than 10-9 T in the specimen region and the capacity to do in situ sample heating and deposition. Cobalt was deposited onto clean Si(100) samples by thermal evaporation from cobalt-coated Ta filaments.


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):  
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):  
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.


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