Practice for Determining Vacuum Chamber Gaseous Environment Using a Cold Finger

2021 ◽  
Author(s):  
Author(s):  
George H. N. Riddle ◽  
Benjamin M. Siegel

A routine procedure for growing very thin graphite substrate films has been developed. The films are grown pyrolytically in an ultra-high vacuum chamber by exposing (111) epitaxial nickel films to carbon monoxide gas. The nickel serves as a catalyst for the disproportionation of CO through the reaction 2C0 → C + CO2. The nickel catalyst is prepared by evaporation onto artificial mica at 400°C and annealing for 1/2 hour at 600°C in vacuum. Exposure of the annealed nickel to 1 torr CO for 3 hours at 500°C results in the growth of very thin continuous graphite films. The graphite is stripped from its nickel substrate in acid and mounted on holey formvar support films for use as specimen substrates.The graphite films, self-supporting over formvar holes up to five microns in diameter, have been studied by bright and dark field electron microscopy, by electron diffraction, and have been shadowed to reveal their topography and thickness. The films consist of individual crystallites typically a micron across with their basal planes parallel to the surface but oriented in different, apparently random directions about the normal to the basal plane.


Author(s):  
A. Tanaka ◽  
M. Yamaguchi ◽  
T. Hirano

The plasma polymerization replica method and its apparatus have been devised by Tanaka (1-3). We have published several reports on its application: surface replicas of biological and inorganic specimens, replicas of freeze-fractured tissues and metal-extraction replicas with immunocytochemical markers.The apparatus for plasma polymerization consists of a high voltage power supply, a vacuum chamber containing a hydrocarbon gas (naphthalene, methane, ethylene), and electrodes of an anode disk and a cathode of the specimen base. The surface replication by plasma polymerization in negative glow phase on the cathode was carried out by gassing at 0.05-0.1 Torr and glow discharging at 1.5-3 kV D.C. Ionized hydrocarbon molecules diffused into complex surface configurations and deposited as a three-dimensionally polymerized film of 1050 nm in thickness.The resulting film on the complex surface had uniform thickness and showed no granular texture. Since the film was chemically inert, resistant to heat and mecanically strong, it could be treated with almost any organic or inorganic solvents.


Author(s):  
Klaus-Ruediger Peters

Only recently it became possible to expand scanning electron microscopy to low vacuum and atmospheric pressure through the introduction of several new technologies. In principle, only the specimen is provided with a controlled gaseous environment while the optical microscope column is kept at high vacuum. In the specimen chamber, the gas can generate new interactions with i) the probe electrons, ii) the specimen surface, and iii) the specimen-specific signal electrons. The results of these interactions yield new information about specimen surfaces not accessible to conventional high vacuum SEM. Several microscope types are available differing from each other by the maximum available gas pressure and the types of signals which can be used for investigation of specimen properties.Electrical non-conductors can be easily imaged despite charge accumulations at and beneath their surface. At high gas pressures between 10-2 and 2 torr, gas molecules are ionized in the electrical field between the specimen surface and the surrounding microscope parts through signal electrons and, to a certain extent, probe electrons. The gas provides a stable ion flux for a surface charge equalization if sufficient gas ions are provided.


Author(s):  
S.A. Wight

Measurements of electrons striking the sample in the Environmental Scanning Electron Microscope (ESEM) are needed to begin to understand the effect of the presence of the gas on analytical measurements. Accurate beam current is important to x-ray microanalysis and it is typically measured with a faraday cup. A faraday cup (Figure 1) was constructed from a carbon block embedded in non-conductive epoxy with a 45 micrometer bore platinum aperture over the hole. Currents were measured with an electrometer and recorded as instrument parameters were varied.Instrument parameters investigated included working distance, chamber pressure, condenser percentage, and accelerating voltage. The conditions studied were low vacuum with gaseous secondary electron detector (GSED) voltage on; low vacuum with GSED voltage off; and high vacuum (GSED off). The base conditions were 30 kV, 667 Pa (5 Torr) water vapor, 100,000x magnification with the beam centered inside aperture, GSED voltage at 370 VDC, condenser at 50%, and working distance at 19.5 mm. All modifications of instrument parameters were made from these conditions.


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