On-line topographic analysis in the SEM

A novel method for on-line topographic analysis of rough surfaces in the SEM has been investigated. It utilises a digital minicomputer configured to act as a programmable scan generator and automatic focusing unit. The computer is coupled to the microscope through digital-to-analogue converters which enable it to generate ramp waveforms allowing the beam to be scanned over a small sub-region of the field under program control. A further digital-to-analogue converter regulates the current supply to the objective lens of the microscope. The video signal is sampled by means of an analogue-to-digital converter and the resultant binary code stored in the computer's memory as an array of numbers describing relative image intensity. Computations based on the intensity gradient of the image allow the objective lens current to be found for the in-focus condition, which may be related to the working distance through a previous calibration experiment. The sensitivity of the method for detecting small height changes is theoretically of the order of 1 μm. In practice the operator specifies features of interest by means of a mobile spot cursor injected into the SEM display screen, or he may scan the specimen at sub-regions corresponding to pre-determined points on a regular grid defined by him. The operation then proceeds under program control. | A novel method for on-line topographic analysis of rough surfaces in the SEM has been investigated. It utilizes a digital minicomputer configured to act as a programmable scan generator and automatic focusing unit. A further digital-to-analog converter regulates the current supply to the objective lens of the microscope. The video signal is sampled by means of an analog-to-digital converter and the resultant binary code stored in the computer's memory as an array of numbers describing relative image intensity. The sensitivity of the method for detecting small height changes is theroretically of the order of 1 mu m.

Study of crystallinity and thermomechanical analysis of annealed poly(ethylene terephthalate) films

The objective of this article was the determination of the degree of crystallinity of a series of heat-set poly(ethylene terephthalate) (PET) films and their study by thermomechanical analysis (TMA) in order to elucidate a peculiar behaviour that takes place around the glass transition region. For this purpose, amorphous cast Mylar films from DuPont were annealed at 115 °C for various periods of time. Four methods were used to study the crystallinity of the samples prepared: differential scanning calorimetry (DSC), density measurements (DM), wide-angle X-ray diffraction (WAXD), and Fourier transform infrared spectroscopy (FT-IR). From the results obtained, the following conclusions are drawn: amorphous PET Mylar films can be crystallized in a degree of about up to 30% after thermal treatment for 30 min (cold crystallization) above glass transition temperature. When these semicrystalline samples are subjected to TMA, they show a two step penetration of the probe into them, which decreases with the increase of the degree of crystallinity. The first step of penetration was attributed to the shrinkage of the amorphous or semicrystalline sample, which takes place on the glass transition temperature, while the second step was attributed to the continuous softening of the sample, and the reorganization of the matter which takes place on heating run due to cold crystallization. © 2008 Elsevier Ltd. All rights reserved.