The average diameter of the first micrometer particle size standard (Standard Reference Material 1690), an aqueous suspension of monosized polystyrene spheres with a nominal gum diameter, was accurately determined by three independent techniques. In one technique the intensity of light scattered by a diluted suspension of polystyrene spheres was measured as a function of scattering angle, using a He-Ne laser polarized in the vertical direction. The second technique consisted of measuring as a function of angle the intensity of light scattered from individual polystyrene spheres suspended in air, using a He-Cd laser with light polarized parallel and perpendicular to the scattering plane. The measurement of row length by optical microscopy for polystyrene spheres arranged in close-packed, two-dimensional hexagonal arrays was the basis of the third technique. The measurement errors for each technique were quantitatively assessed. For the light scattering experiments, this required simulation with numerical experiments. The average diameter determined by each technique agreed within 0.5% with the most accurate value being 0.895±0.007 gm based on light scattering by an aqueous suspension. Transmission electron microscopy, flow through electrical sensing zone counter measurements, and optical microscopy were also used to obtain more detailed information on the size distribution including the standard deviation (0.0095 gum), fraction of off-size particles, and the fraction of agglomerated doublets (1.5%).
LANGMUIR are 100-500 eV. For SiO2 etch rates vary essentially in proportion to ion densities with all the different plasmas. In addition, there is evidence for a dependence of the etch rate on the ion energy. For Si in CF4-O2 plasmas of different composition, the anisotropic part of the etch rate also parallels the ion density. From an estimate of the ion flux ~o the substrate we are able to determine etch rates per ion in reactive sputter etching. These turn out to be comparable to, possibly even larger than, those in reactive ion beam etching, although in reactive sputter etching ion energies are much smaller.
This report describes the certification of SRM 1962, a NIST Standard Reference Material for particle diameter. It consists of an aqueous suspension of monosize 3 (μm polystyrene spheres. Two calibration techniques were used: optical microscopy and electron microscopy. The first one gave a mean diameter of
D¯=2.977±0.011 μm and a standard deviation of the size distribution σD = 0.020 μm, based on measurement of 4600 spheres. The second technique gave
D¯=2.990±0.009 μm, based on measurement of 120 spheres. The reported value covering the two results is
D¯=2.983 μm with a maximum uncertainly of 0.016 μm, with σD=0.020 μm.
Experimental, theoretical, and calculational details are presented for the three independent micrometrology techniques used to certify the mean diameter of Standard Reference Materisd 1960, nominal 10 μm diameter polystyrene spheres (“space beads”). The mean diameters determined by the three techniques agreed remarkably well, with all measurements within 0.1% of each other, an unprecedented achievement in the dimensional metrology of microspheres. Center distance finding (CDF), a method based on optical microscopy, gave a value of 9.89 ± 0.04 μm, which was chosen to be the certified mean diameter. The supporting measurements were done using metrology electron microscopy (MEM) and resonance light scattering (RLS). The MEM technique, based on scanning electron microscopy, yielded 9.89±0.06 μm for the mean diameter of the microspheres in vacuum, while the RLS value was 9.90 ±0.03 μm for the microspheres in liquid suspension. The main peak of the diameter distribution for SRM 1960 is nearly Gaussian with a certified standard deviation of 0.09 μm, as determined by CDF. Off the main peak, there are about 1% oversized particles and a negligible amount of undersized particles. The report gives a detailed description of the apparatus, the experimental methods, the data-reduction techniques, and an error analysis for each of the micro-metrology techniques. A distinctive characteristic of this SRM is that it was manufactured in microgravity aboard the NASA space shuttle Challenger and is the first commercial product to be made in space.
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