Application and Optimization of Automated ECCI Mapping to the Analysis of Lowly Defective Epitaxial Films on Blanket or Patterned Wafers

The physical limits of CMOS scaling, as predicted by Moore's Law, should have already been reached several years ago. However, the scaling of transistors is still ongoing due to continuous improvements in material quality enabling the fabrication of complex device structures with nm-size dimensions. More than ever, the structural properties and the eventual presence of crystalline defects in the various semiconductor materials (SiGe, III/V) play a critical role. Electron channeling contrast imaging (ECCI) is a powerful defect analysis technique developed in recent years. The technique allows for fast and non-destructive characterizations with the potential for extremely low detection limits. The analysis of lowly defective materials requires measurements over large areas to obtain statistically relevant data. Automated ECCI mapping routines enable the quantification of crystalline defect densities as low as ~1e5 cm-2, e.g., Si0.75Ge0.25 strain relaxed buffers (SRB) epitaxially grown on a Si substrate. Methods to reduce the total measurement time without compromising its sensitivity will be discussed. The measurement routine has also been optimized to detect extended crystalline defects in III/V layers, selectively grown on shallow trench isolation patterned Si wafers. Throughout these examples, this study demonstrates the great potential of ECCI as a versatile and industry-relevant technique for defect analysis.

Dynamic-range extension of MAES multichannel analyzers based on BLPP-2000 and BLPP 4000 photodetector arrays

One trend in the development of integral atomic emission spectral analysis with low spectral background excitation sources, such as inductively coupled or microwave plasma, is to increase the dynamic range of spectrum recording systems based on photodetector arrays. To achieve low detection limits, it is necessary to use photodetector arrays with low reading noise. The dynamic range of a single readout of such photodetector arrays usually does not exceed four orders of magnitude. The dynamic range increase due to the accumulation of spectra from multiple acquisition leads to a quadratic increase in the measurement time. This method does not allow one to cover the entire dynamic range of spectral line intensities of inductively coupled or microwave plasma (which can reach seven orders of magnitude) while maintaining an acceptable total measurement time of a sample spectrum. As an alternative, it is proposed to increase the dynamic range toward higher line intensities by using two different alternating accumulation times during measurement. The objective of this study is to implement the proposed recording mode in MAES analyzers based on BLPP-2000 and BLPP-4000 photodetector arrays in order to increase the dynamic range of recorded spectral lines. Dependences of the signal-to-noise ratio and the dynamic range of spectral lines recorded in integral atomic emission spectrometry on the accumulation time, the total measurement time, the spectral background level, and the photodetector array parameters are obtained. It is shown theoretically that the use of the recording mode with alternating different accumulation times should increase the dynamic range of BLPP-2000 and BLPP-4000 photodetector arrays by two orders of magnitude. The dynamic range of spectral line intensities of a hollow-cathode lamp is shown experimentally to increase by two orders of magnitude (to five orders of magnitude).

Broadband Time-Resolved Absorption and Dispersion Spectroscopy of Methane and Ethane in a Plasma Using a Mid-Infrared Dual-Comb Spectrometer

Conventional mechanical Fourier Transform Spectrometers (FTS) can simultaneously measure absorption and dispersion spectra of gas-phase samples. However, they usually need very long measurement times to achieve time-resolved spectra with a good spectral and temporal resolution. Here, we present a mid-infrared dual-comb-based FTS in an asymmetric configuration, providing broadband absorption and dispersion spectra with a spectral resolution of 5 GHz (0.18 nm at a wavelength of 3333 nm), a temporal resolution of 20 μs, a total wavelength coverage over 300 cm−1 and a total measurement time of ~70 s. We used the dual-comb spectrometer to monitor the reaction dynamics of methane and ethane in an electrical plasma discharge. We observed ethane/methane formation as a recombination reaction of hydrocarbon radicals in the discharge in various static and dynamic conditions. The results demonstrate a new analytical approach for measuring fast molecular absorption and dispersion changes and monitoring the fast dynamics of chemical reactions over a broad wavelength range, which can be interesting for chemical kinetic research, particularly for the combustion and plasma analysis community.

Toward a cyber-physical manufacturing metrology model for industry 4.0

Industry 4.0 represents high-level methodologies for the development of new generation manufacturing metrology systems, which are more intelligent (smart), autonomous, flexible, high-productive, and self-adaptable. One of the systems capable of responding to these challenges is a cyber-physical manufacturing metrology system (CP2MS) with techniques of artificial intelligence (AI). In general, CP2MS systems generate Big data, horizontally by integration [coordinate measuring machines (CMMs)] and vertically by control. This paper presents a cyber-physical manufacturing metrology model (CP3M) for Industry 4.0 developed by applying AI techniques such as engineering ontology (EO), ant-colony optimization (ACO), and genetic algorithms (GAs). Particularly, the CP3M presents an intelligent approach of probe configuration and setup planning for inspection of prismatic measurement parts (PMPs) on a CMM. A set of possible PMP setups and probe configurations is reduced to optimal number using developed GA-based methodology. The major novelty is the development of a new CP3M capable of responding to the requirements of an Industry 4.0 concept such as intelligent, autonomous, and productive measuring systems. As such, they respond to one smart metrology requirement within the framework of Industry 4.0, referring to the optimal number of PMPs setups and for each setup defines the configurations of probes. The main contribution of the model is productivity increase of the measuring process through the reduction of the total measurement time, as well as the elimination of errors due to the human factor through intelligent planning of probe configuration and part setup. The experiment was successfully performed using a PMP specially designed and manufactured for the purpose.

Broadband Time-Resolved Absorption and Dispersion Spectroscopy of Methane and Ethane in A Plasma Using a Mid-Infrared Dual-Comb Spectrometer

Conventional mechanical Fourier Transform Spectrometers (FTS) are able to simultaneously measure absorption and dispersion spectra of gas-phase samples. However, they usually need very long measurement times to achieve time-resolved spectra with a good spectral and temporal resolution. Here, we present a mid-infrared dual-comb-based FTS in an asymmetric configuration, providing broadband absorption and dispersion spectra with a spectral resolution of 5 GHz, a temporal resolution of 20 μs, and a total measurement time of a few minutes. We used the dual-comb spectrometer to monitor the reaction dynamics of methane and ethane in an electrical plasma discharge. We observed ethane/methane formation as a recombination reaction of hydrocarbon radicals in the discharge in various static and dynamic conditions. The results demonstrate a new analytical approach for measuring fast molecular absorption and dispersion changes and monitoring fast dynamics of chemical reactions, which can be interesting for chemical kinetic research and particularly for the combustion and plasma analysis community.

Simultaneous Determination of Five Components of Chaihu-Shugan-San in Beagle Plasma by HPLC-MS/MS and Its Application to a Pharmacokinetic Study after a Single Dose of Chaihu-Shugan-San

Chaihu-shugan-san (CHSGS) has been widely used in China to treat depression and gastrointestinal diseases for thousands of years, but little is known about its pharmacokinetic properties. The purpose of our study is to develop a reliable and sensitive high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method to detect five components in beagle plasma and study their pharmacokinetic after oral administration of CHSGS in beagles. An Agilent C18 column (2.1 × 150 mm, 3.5 μm) was used to separate the analytes, and the column temperature was maintained at 40°C. A gradient elution procedure was used with solvent A (acetonitrile) and solvent B (0.1% formic acid, aqueous) as mobile phases. The elution procedure was 60% B—10% B (0–3 min) and 10% B—60% B (3.1–4 min). The flow rate was 0.3 mL/min, and the total measurement time was 4 min. Within the determined range, the standard calibration curves of the five analytes had a satisfactory linear relationship (r2 ≥ 0.9923). The recovery rate (n = 6) of the five analytes was between 85.42% and 90.85%, and the matrix effects (n = 6) were between 94.52% and 103.91%. These results show that the validated method could be successfully applied to study the pharmacokinetic in beagles after a single dose of CHSGS.

Improving Activity Estimation in Passive Gamma Scanning for Radioactive Waste Drums

A method to improve radioactive waste drum activity estimation in Segmented Gamma Scanning (SGS) systems was developed for homogenous content. We describe a method to quantify the activity of spatially distributed gamma-emitting isotopes (‘hot spots’) in homogenous content waste drums without the use of a collimator. Instead of averaging all the detector's readings we treat it as many different spatial samples as if we have multiple detectors surrounding the waste drum ("virtual detectors"). From these readings, we form a general linear model. Next, we derive the Maximum Likelihood Estimator (MLE) for the multiple sources position and activity. We solve this hyper-dimensional search problem using an Alternating Projections (AP) technique which transforms the problem into a simpler one-dimensional maximization problem. We tested this method using a mathematical simulation with a various number of sources, at random activities and positions for several energy bands. The preliminary results are consistent and show large improvement of the accuracy with comparison to industrial SGS systems and the same accuracy as new methods which exploits the spatial samples. Furthermore, since this method eliminates the need for heavy led collimator, none of the sources is blocked for the whole measurement period, which provides increased count rates and decreases the total measurement time.

Optimization of Airborne Antenna Geometry for Ocean Surface Scatterometric Measurements

We consider different antenna configurations, ranging from simple X-configuration to multi-beam star geometries, for airborne scatterometric measurements of the wind vector near the ocean surface. For all geometries, track-stabilized antenna configurations, as well as horizontal transmitter and receiver polarizations, are considered. The wind vector retrieval algorithm is generalized here for an arbitrary star geometry antenna configuration and tested using the Ku-Band geophysical model function. Using Monte Carlo simulations for the fixed total measurement time, we show explicitly that the relative wind speed estimation accuracy barely depends on the chosen antenna geometry, while the maximum wind direction retrieval error reduces moderately with increasing angular resolution, although at the cost of increased retrieval algorithm computational complexity, thus, limiting online analysis options with onboard equipment. Remarkably, the simplest X-configuration, while the simplest in terms of hardware implementation and computational time, appears an outlier, yielding considerably higher maximum retrieval errors when compared to all other configurations. We believe that our results are useful for the optimization of both hardware and software design for modern airborne scatterometric measurement systems based on tunable antenna arrays especially, those requiring online data processing.

Continuous-scan capability at SSRL and applications to X-ray diffraction

Typical X-ray diffraction measurements are made by moving a detector to discrete positions in space and then measuring the signal at each stationary position. This step-scanning method can be time-consuming, and may induce vibrations in the measurement system when the motors are accelerated and decelerated at each position. Furthermore, diffraction information between the data points may be missed unless a fine step-scanning is used, which further increases the total measurement time. To utilize beam time efficiently, the motor acceleration and deceleration time should be minimized, and the signal-to-noise ratio should be maximized. To accomplish this, an integrated continuous-scan system was developed at the Stanford Synchrotron Radiation Lightsource (SSRL). The continuous-scan system uses an in-house integrated motor controller system and counter/timer electronics.SPECsoftware is used to control both the hardware and data acquisition systems. The time efficiency and repeatability of the continuous-scan system were tested using X-ray diffraction from a ZnO powder and compared with the step-scan technique. Advantages and limitations of the continuous-scan system and a demonstration of variable-velocity continuous scan are discussed.