Software suite for Rigaku X-ray diffractometers
Integrates user privileges, measurements, analyses, data visualization and reporting
SmartLab Studio II is a new Windows®-based software suite developed for the flagship Rigaku SmartLab X-ray diffractometer that integrates user privileges, measurements, analyses, data visualization and reporting. Newly available for the MiniFlex, the modular (plugin) architecture of this software delivers state-of-the-art interoperability between the functional components. Just one click switches from measurement to analysis. Watch real-time scans from one experiment while simultaneously analyzing other data on the same desktop by selecting an appropriate layout. The software provides various analysis tools such as automatic phase identification, quantitative analysis, crystallite-size analysis, lattice constants refinement, Rietveld analysis, ab initio structure determination, etc.
- Seamless operations from measurement to reporting by single software platform
- Covers basic XRPD applications, e.g. qualitative, quantitative, crystallite size, Rietveld analysis, as well as advanced analysis, e.g. X-ray reflectivity, HRXRD, pole figure and PDF.
- Clustering analysis and Data Visualization supports various data treatments
- Supports FDA 21 CFR Part 11 data integrity
- Network dongle provides software licenses maximum 10 PCs
Explore these plugins
A measurement package built by experts in XRD
- User Guidance guides instrument operation for beginners and experts
- Wizard recommends measurement conditions to users depending on sample types
- One click operation from measurement to analysis if defined
- Measurement and analysis on 0-, 1- and 2-D data
- In-situ and operando measurements support synchronizing with external device
The state-of-the-art consolidated powder X-ray analysis package
- Unified interface from qualitative analysis to structure determination
- Direct Derivation (DD) method for quantification from crystalline to amorphous samples
- Whole powder patten fitting (WPPF) based on Fundamental Parameters (FP) approach
- Supporting norms defined by ASTM, JIS and NIOSH/OSHA for respirable silica and retained austenite analysis
- Direct phase identification from 2-D data utilizing crystallite size information
Hybrid Search/Match enhancing qualification analysis
Hybrid Search/Match is crystalline phase identification based on two types of measured data: peak position and profile shape. Using this method, the accuracy of phase identification has drastically improved. It can also be used to identify crystal phases with preferred-orientation or heavily distorted lattices.
User-friendly operations for Rietveld analysis
SmartLab Studio II provides a user-friendly interface for Rietveld analysis, which enables users of any experience level to load crystal structure parameters from a database, set analysis conditions, display graphical images of crystal structures and quantify results without difficulty.
High-speed search with fully automated profile fitting
Simply by loading measurement data, SmartLab Studio II executes fully automated profile fitting to calculate peak position, FWHM, integrated intensity, and crystallite size (using the Scherrer method).
Crystallite size distribution analysis
Using the fundamental parameter method (FP method), theoretical peak shapes are calculated based on optical information to obtain more detailed analysis results, such as crystallite size distribution.
DD method package (optional)
Quantification with DD method is available
Quantification can be performed using the chemical composition and total peak intensity of each crystalline phase based on the DD method. The quantification can be used to estimate the amount of unknown impurity or amorphous phase. In addition, the profile of each phase, if measured, can be used to quantify the phases in a mixture.
Quantification package (optional)
Simplified procedure for creating calibration curves
This optional quantification package supports various calibration methods: Internal standard method, External standard method, Standard addition method. Peak intensity can be extracted and plotted with the software to create and use calibration curves. Quantification using the calibration method is suitable for quantification and management of specific crystal phases.
Qualitative analysis package (optional)
Flexible search using Hybrid Search/Match
Rigaku’s unique “Hybrid Search/Match” uses peak-base qualification, which detects heavily distorted lattices, to identify solid solution phases that are generally hard to identify. In addition, it determines whether preferred orientation exists based on separated peak intensities, which cannot be determined by the profile-base qualification.
Comprehensive analysis package (optional)
A variety of analyses
This package is capable of providing analysis results such as crystallite size, lattice strain, lattice parameters refinement and %crystallinity based on fully automated profile fitting executed when loading measured data. The obtained information helps understand the relationship between structure and physical properties, and allows users to compare the results of different samples.
Rietveld analysis package (optional)
Using the results of phase identification analysis
When a phase included in a sample is unknown, this package performs phase identification and then Rietveld analysis. Initial parameters required for Rietveld analysis are automatically estimated based on the measurement data after phase identification. This makes Rietveld analysis easy even for inexperienced users.
Using the Rietveld method for quantitative analysis
The Rietveld method obtains quantitative results directly from the measurement results of the sample in question, unlike the calibration curve method, which requires adding a standard reference substance to the sample and creating a calibration curve.
Using the WPPF method for lattice parameter refinement
Lattice parameter refinement performed by the Rietveld method or the whole powder pattern decomposition method (Pawley method) is based not only on the measured peak positions, but also on the peak shapes (WPPF method). More accurate values are obtained with the angle correction, performed using an internal standard phase or external standard sample.
Using FP method for theoretical peak profile calculation
The fundamental parameter method (FP method), which is used to calculate theoretical peak profiles taking into account the used optics and crystallite size distribution, shows great results for analysis of samples including several crystal phases, such as cement samples.
Structure determination package (optional)
Packaging the necessary functions for unknown crystal structure analysis To determine an initial structure in unknown crystal structure analysis, one method may not be enough. This structural analysis option offers a variety of analysis methods: Direct method and Direct space method with simulated annealing method using the popular EXPO2014, Direct space method with parallel tempering algorithm and Charge flipping.
Use of OChemDb information for constraint conditions
· Calculated interatomic distance or bond angle using the Rietveld refinement method in Powder structure analysis may deviate from a reasonable value.
· In the structure determination package, OChemDb is available to set constraint settings for Rietveld refinement. This makes it possible to perform the Rietveld refinement even with an unknown crystal structure, maintaining a reasonable structure.
X-ray reflectivity analysis software for a wide range of applications, from simple film thickness analysis to detailed multilayer structure analysis
- Flow bar guides user and provides necessary analysis steps to complete
- Oscillation analysis helps modeling the sample structure
- Density profile is graphically displayed across sample thickness
- Segmented measurement ranges maximize dynamic range of the data
- Simultaneous fittings on more than two data sets measured by different resolutions to extract one sample structure that includes largely different thicknesses
In reflectivity analysis using conventional nonlinear least-squares methods, a local minimum can be obtained as a solution. In this case, the final solution changes depending on the initial analysis model or on the operator’s skill. The reflectivity plugin performs analysis independent of initial models or operators by using the latest fitting algorithm that automatically searches many solutions.
Latest fitting algorithmUse of a genetic algorithm customized for reflectivity analysis to find a true solution (a global minimum) minimizes operator dependence. In addition, use of the algorithm helps determine a solution even when the initial model greatly deviates from the final solution.
Dual-fitting algorithmFor more precise analysis, the plugin incorporates a dual-fitting algorithm (genetic algorithm and least-squares method). After finding a global minimum by the genetic algorithm, the least-squares method is used for further precise fitting analysis. In the analysis, the precision can be improved by setting upper and lower limits on the film structure parameters and applying various constraints on the parameters.
Extended Fourier film thickness analysisExtended Fourier film thickness analysis provides rough information about the film thickness without performing a fitting analysis. Moreover, applying the obtained rough data of the film thickness to a fitting model, one can create an initial model in a form close to a final solution, which can shorten the analysis time.
A variety of modeling functionsThe software allows setting both the density gradient in a single layer and the density and film thickness gradients for a superlattice structure. These can be applied to the analysis of a complicated structure such as interface diffusion or non-uniform multilayer films.
More accurate analysis can be performed by setting a model of the X-ray optical system used for the measurement to account for the resolution of the system in the fitting analysis. Sample parameters obtained from the analysis can be saved for use in subsequent analyses. By doing so, the analysis of a complicated film structure can be started smoothly.
An integrated reciprocal lattice map and high-resolution rocking curve plugin for epitaxial films analysis
- Dynamical simulation fitting on high-resolution XRD (HRXRD) data and analysis of high-resolution reciprocal space mapping (RSM)
- Support all 230 space groups of crystal structures
- Stress-relaxation and composition analysis from asymmetric RSM
- Indexing on measured RSM
- Lattice parameters and strain calculation from RSM
Designed for advanced materialsThis plugin supports analysis of epitaxial growth with anisotropy within the surface plane of the substrate. Employing “anchor parameters,” which specify orientation in two directions of the sample surface plane, allows users to analyze anisotropic elastic deformation of epitaxial films in in-plane anisotropic tensions. The method can be applied to cutting-edge materials such as epitaxial films deposited on silicon (110 ) substrate or a-plane and m-plane sapphire substrate.
Advanced peak search and display functionsFunctions used frequently for the analysis of reciprocal lattice map data have been simplified. A single click can switch the display of goniometer coordinates or reciprocal lattice space coordinates in reciprocal space mapping data and activate an advanced peak search function that can also be applied to 2D diffraction data in order to obtain precise coordinates of reciprocal lattice points in a simple way. Measurement results can be easily interpreted using a function that overlaps a simulation result obtained for a sample model onto measurement data.
Applicable to various film structure modelsStructure models of samples having complicated multilayer film structures can be created smoothly using the inter-layer parameter link function or superlattice modeling function. Parameters to describe a state of strain can be chosen from relaxation, strain, and lattice mismatch in two directions within the plane. Functions to set orientation deviation (tilt and twist)of multilayer films and evaluate mosaicity have been added. Parameters can be fine-tuned using a slider bar. A sample profile chart shows a complicated sample structure in an easy-to-understand visual way by specifying a display color for each crystal phase.
Function of simultaneous fitting of multiple dataA function to fit multiple measurement data with different reflection indices to a film structure model was installed. Management of the conditions and results of analysis are easy because the measurement data and film structure model used for the analysis are saved as one project.
Accurate and quick fitting analysisA genetic algorithm and least-squares method are employed as fitting algorithms. Appropriate setting of constraints and upper and lower limits can prevent value divergence in the simultaneous fitting of many parameters to obtain stable analysis results.
By incorporating four-wave approximation and recursive matrix theories in theoretical profile analysis, a measurement with small incident angle and a deformed state of an epitaxial thin film such as complete relaxation, partial deformation, and overall deformation can be reproduced more accurately.
Step-by-step instructions on the flow bar allow smooth calculation of the crystal orientation distribution map
- Pole figure representation and Orientation Distribution Function (ODF) analysis
- Representation and analysis on complete pole figures obtained from transmission and reflection measurements
- Analysis of preferred orientation direction (hkl)[uvw] and its volume fraction
- Inverse pole figure calculation
- Kearns and Herman’s orientation functions for quantitative analysis
Creating and displaying pole figures
Texture plugin is designed to analyze the ODF (Orientation Distribution Function) from pole figure data measured with 0D or 2D detectors. The plugin supports defocusing correction and absorption correction of pole figures. In addition, the plugin includes functions such as smoothing, rotation and regrid of the pole figures. Measured 2D data, 2D diffraction data polarization correction and absorption correction are also available. Pole figures can be displayed in different formats.
ODF calculation (optional) Two methods of ODF calculation are available: WIMV and the component approximation analysis method. Both methods are suitable for the calculation of a crystal orientation distribution map and recalculation of whole pole figure corresponding to an arbitrary index. One of the optimization algorithms for component approximation is the genetic algorithm. When using this algorithm, there is no need to match parameters with a measured pole figure beforehand.
Also, the inverse pole figure can be created using the obtained crystal orientation distribution map.
Calculation of orientation function
An orientation function can be calculated by connecting transmission and reflection pole figures, or overall pole figures recalculated by ODF analysis. “Information” contained in the pole figure can be compared and managed as “values” presenting a degree of orientation. Differences in physical properties and performance due to differences in production methods can be evaluated through the connection to an orientation function obtained from the pole figures.
Stress plugin for a variety of purposes from QC to R&D
- Sin2ψ, 2D-stress and Multiple HKL methods are supported
- Residual stress analysis from bulk to thin film samples
- Principal and tri-axial residual stress analysis using 2-D method
- Stiffness tensor or Young’s modulus & Poisson’s ratio for calculation
Residual stress analysis.
In the stress plugin, the residual stress of a polycrystalline material can be quantitatively evaluated with X-ray diffraction data. In addition to ordinary stress analysis by the sin²ψ method, the stress tensor and the principal stress can be also analyzed under an assumption of the plane stress state: σ₁₁, σ₂₂ and σ₁₂, or the triaxial stress state: σ₁₁, σ₂₂, σ₃₃, σ₁₂, σ₂₃ and σ₁₃. The multiple hkl method, effective for thin film stress analysis, is also available in this stress plugin. The residual stress of a thin film can be analyzed with multi-directional strains in different diffraction planes, assuming the plane stress state. In the data processing function, all data from 0D, 1D and 2D modes can be loaded, and data processing, such as 2D diffraction data segmentation, smoothing, background elimination, LPA correction, Ka₂ elimination, peak position searching and profile pattern fitting, is easily done.
Moreover, the diffraction angle in the strain-free state (2θ₀), and the X-ray elastic constants (E, ν, K, S1 and 1 /2 S₂) can be calculated utilizing an extensive material database. The grain interaction model used for the calculation of the X-ray elastic constant can be arbitrarily selected from four models: 1) Reuss model: the stress is constant among the grains, 2 ) Voigt model: the strain is constant among the grains, 3) Neerfeld-Hill model: an arithmetic average between Reuss and Voigt, and 4 ) Kröner model: a large number of spherical grains of single crystal having the elastic anisotropy exist in a polycrystalline matrix.
Finally, the highly flexible stress plugin enables various stress analyses according to a wide range of purposes, from quality control to research and development.
Determination of particle/pore size distribution ranging from nano- to submicron order
- Particle size and distribution analysis from 1-D or 2-D SAXS data
- Size distribution, average, percentile D10, D50, D90 are calculated
- Sample that does not transmit visible light can be analyzed
- Analyze on sample with multiple particle size distributions
Particle/pore size analysis
Particle/pore size analysis determines the size distribution of particles/pores in powder, bulk, film samples and liquid. Generally, particles/pores on the order of 1 to 100 nm are available for analysis. Using ultra-small angle X-ray scattering (U-SAXS) optics, users can analyze particles/pores 1000 nm in size. Particle/pore shapes such as sphere, core-shell, cylinder and spheroid can be analyzed. The plugin also features the Debye model, which performs analysis without the shape being specified. In the case of high-density particles, the structure factor is taken into account for a more accurate size distribution calculation.
More accurate analysis of particle/pore size distribution in thin filmsThe particle/pore-size distribution in a thin-film sample can be analyzed more accurately by considering scattering from the roughness of a surface or an interface of the thin film. This method is particularly useful when the number of particles/pores is small or their sizes are small. For the XRD measurement plugin, a “Part Activity” to collect the necessary data for this analysis is available. Using Part Activity, the plugin can easily collect data with an input of some information about the samples.
Lattice simulation and Guinier/Kratky plotIn addition to analysis of particle/pore size distributions using least-squares methods, simulations of diffraction line positions from 1D or 2D lattices using a simple method can be performed. Furthermore, the radius of inertia can be calculated in a simple procedure using a Guinier plot.
Slit correctionSmall-angle scattering data are significantly affected by the umbrella effect; therefore, the obtained scattering intensity pattern is greatly distorted. The “slit correction” accounts for this distortion. The MRSAXS plugin accurately reproduces the scattering intensity pattern using Rigaku’s original algorithm and performs more accurate size distribution analysis.
Contribution to analysis of amorphous material
- Calculation of structure function S(Q) and pair distribution function (PDF)
- Overlay calculated atomic distances from crystal structure on PDF data
- PDF calculation from multiple data measured by different energies of X-ray
- Reasonable S(Q) and PDF profiles by ripple correction
- Exporting PDF profile to PDFgui and RMCProfile software
Calculation of RDF and PDFThe PDF plugin can calculate RDF (radial distribution function) and PDF (pair distribution function) with Fourier transform of S(Q) (Structure factor).
In order to obtain S(Q), the scattering intensity of only a sample is extracted from a measured X-ray diffraction pattern, with consideration for the absorption of the sample and its container (cell), and then the Compton scattering correction is performed to the extracted intensity.
Correction using the short-range area of PDF (Ripple correction)
In a PDF obtained by Fourier transform of S(Q), peaks may appear at a distance shorter than the closest interatomic distance. The PDF plugin features S(Q) correction which rationally removes unnatural peaks from a PDF, taking into account the closest interatomic distance and the shorter distance peaks. This allows users to examine atomic arrangement in amorphous materials by comparing the interatomic distance based on crystal structures with the PDF, without worrying about unnatural peaks.
Ultra-efficient mass data analysis
- Analyze and display of multiple data
- 1-D data waterfall plot
- 2-D & 1-D data slideshow
- in-situ and operando data treatment and representation
- Temperature vs. XRD, Differential Scanning Calorimetry (DSC) profile vs. XRD data representation
- Importing & linking data from an external device, e.g. potentiometer with XRD data
- Spatial mapping data analysis and representation overlayed with sample snap-shot image
- Extracting data from selected point or area on a spatial mapping data
- Synchronization with analysis software plugins, e.g. PowderXRD, Stress, XRR and HRXRD, to analyze multiple data
- Displaying analyzed results by analysis software plugin, e.g. phase, stress, thickness, together with spatial mapping data and snap-shot sample image
- Statistical calculation of analyzed results by analysis software plugin over an area mapped
High-speed detectors make it possible to collect large amounts of data in a short time. The Data Visualization plugin efficiently processes thousands of data sets collected by operando measurements such as temperature-controlled measurements and displays the results in an easy-to-understand manner.
Using the XY mapping measurement Part Activity in the XRD measurement plugin, you can perform an XY mapping measurement with simple settings. The measurement position (XY coordinates) is recorded with each datum, so the physical quantity obtained from the XRD measurement can be easily mapped and displayed on the sample image. Physical quantities that can be mapped include peak information (position, FWHM, height, integrated intensity, etc.), weight ratio of crystal phase (quantitative analysis results), crystallite size, and stress analysis results using the sin2ψ method.
Measurement start synchronization and text reading function
Even attachments not supported by this software can be synchronized with digital signals to perform X-ray measurements. The Data Visualization plugin can read a text file of time vs. physical quantity output by an external attachment and display it in the same way as an operando measurement.
An X-ray diffraction measurement can be performed while changing temperature and humidity, and you can easily see how the X-ray diffraction pattern changes at the same time. A graph of temperature and humidity is displayed on the left side of the window, and an X-ray diffraction pattern is displayed on the right side. When you choose (click) a certain temperature or humidity in the graph on the left, The X-ray diffraction pattern at that temperature or humidity is displayed on the right. It is also possible to display a slide show, which makes it easy to grasp changes in the X-ray diffraction pattern visually.
Categorization and extraction of large amounts of data
Dendrogram and principal component analysis
The cluster analysis module of SmartLab Studio II is designed to perform clustering regardless of data type and dimension (categorizing data based on the degree of similarity). Clustered data are displayed as a dendrogram. The number of clusters is freely varied by simply changing the threshold of the similarity degree. The correlations between similar data are clearly displayed in the PCA view.
Extracting data similar to reference data
SmartLab Studio II has a data extracting function. By setting reference data beforehand, data similar to the reference data will be extracted from a specified folder. This function is useful for searching previously collected data.
User-friendly tool for simultaneous XRD-DSC measurement
- Representing Differential Scanning Calorimetry (DSC) and XRD profiles against time and temperature
- Analysis of DSC profile, e.g. starting temperature of exo- and endothermic reactions, energies absorbed and released
- Visualize crystallographic phase change depending on time
XRD-DSC data display
The XRD Measurement plugin is capable of displaying XRD-DSC data, but the XRD-DSC plugin features more advanced functions, such as changing the temperature range or thinning data to display graphs.
Linking XRD data and DSC chart
This plugin can simultaneously visualize relationships between changes in an X-ray diffraction pattern and thermal changes in a DSC measurement. This plugin is designed to present a graph of diffraction pattern or X-ray intensity and the DSC chart at the same time, allowing users to determine the changes in the crystal structure of the material.
The XRD-DSC plugin incorporates an automatic DSC chart analyzing feature, which was not available in earlier versions of Rigaku’s software. This feature facilitates the estimation of melting point and phase transition point, as well as endothermic/exothermic calorimetry of dissolution, solidification, etc.