An ultra-high vacuum gauge calibration system

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.

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A High Voltage Electron Microscopy Study of Sub-Oxide Formation in Vanadium

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100065110 ◽

1971 ◽

Vol 29 ◽

pp. 212-213

Author(s):

R. H. Geiss ◽

R. L. Ladd ◽

K. R. Lawless

Keyword(s):

High Vacuum ◽

Microscopy Study ◽

Electron Microscopy Study ◽

Ultra High Vacuum ◽

Pure Oxygen ◽

Pressure Oxidation ◽

High Voltage Electron Microscopy ◽

Oxidation Study ◽

Voltage Electron ◽

Good Agreement

Detailed electron microscope and diffraction studies of the sub-oxides of vanadium have been reported by Cambini and co-workers, and an oxidation study, possibly complicated by carbon and/or nitrogen, has been published by Edington and Smallman. The results reported by these different authors are not in good agreement. For this study, high purity polycrystalline vanadium samples were electrochemically thinned in a dual jet polisher using a solution of 20% H2SO4, 80% CH3OH, and then oxidized in an ion-pumped ultra-high vacuum reactor system using spectroscopically pure oxygen. Samples were oxidized at 350°C and 100μ oxygen pressure for periods of 30,60,90 and 160 minutes. Since our primary interest is in the mechanism of the low pressure oxidation process, the oxidized samples were cooled rapidly and not homogenized. The specimens were then examined in the HVEM at voltages up to 500 kV, the higher voltages being necessary to examine thick sections for which the oxidation behavior was more characteristic of the bulk.

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The High Resolution Scanning Transmission Electron Microscope

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100051591 ◽

1974 ◽

Vol 32 ◽

pp. 316-317

Author(s):

A. V. Crewe

Keyword(s):

Electron Microscope ◽

High Resolution ◽

High Vacuum ◽

Scanning Transmission Electron Microscope ◽

Ultra High Vacuum ◽

Resolving Power ◽

Imaging Characteristics ◽

Transmission Electron ◽

Scanning Transmission ◽

The Moment

The high resolution STEM is now a fact of life. I think that we have, in the last few years, demonstrated that this instrument is capable of the same resolving power as a CEM but is sufficiently different in its imaging characteristics to offer some real advantages.It seems possible to prove in a quite general way that only a field emission source can give adequate intensity for the highest resolution^ and at the moment this means operating at ultra high vacuum levels. Our experience, however, is that neither the source nor the vacuum are difficult to manage and indeed are simpler than many other systems and substantially trouble-free.

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