Benchtop X-ray diffraction (XRD) instrument

Qualitative and quantitative analysis of polycrystalline materials

MiniFlex

New sixth generation MiniFlex X-ray diffractometer (XRD) is a multipurpose analytical instrument that can determine: phase identification and quantification, percent (%) crystallinity, crystallite size and strain, lattice parameter refinement, Rietveld refinement, and molecular structure. It is widely used in research, especially in material science and chemistry, as well as in industry for research and quality control. It is the newest addition to MiniFlex series of benchtop X-ray diffraction analyzers from Rigaku, which began with the introduction of the original MiniFlex system decades ago.

Advanced HPAD detector: 0D, 1D, and 2D modes

MiniFlex XRD system delivers speed and sensitivity through innovative technology advances, including the HyPix-400 MF 2D hybrid pixel array detector (HPAD) together with an available 600 W X-ray source and new 8-position automatic sample changer. This new direct photon counting detector enables high-speed, low-noise data collection and may be operated in 0D and 1D modes for conventional XRD analysis and 2D mode for samples with coarse grain size and/or preferred orientation. A variety of X-ray tube anodes – along with a range of sample rotation and positioning accessories, together with a variety of temperature attachments – are offered to ensure that the MiniFlex X-ray diffraction (XRD) system is versatile enough to perform challenging qualitative and quantitative analyses of a broad range of samples, whether performing research or routine quality control. The new (Gen 6) MiniFlex X-ray diffractometer system embodies the Rigaku philosophy of “Leading with Innovation” by offering the world’s most advanced benchtop XRD.
Powerful PDXL software is easy-to-use
Each MiniFlex comes standard with the latest version of PDXL, Rigaku's full-function powder diffraction analysis package. The latest version of PDXL offers important new functionality; including a fundamental parameter method (FP) for more accurate peak calculation, phase identification using the Crystallography Open Database (COD), and a wizard for ab inito crystal structure analysis.
MiniFlex X-ray diffractometer history
The Rigaku MiniFlex X-ray diffractometer (XRD) is historically significant in that it was the first commercial benchtop (tabletop) X-ray diffraction instrument. When introduced in 1973, the original Miniflex™ XRD was about one-tenth the size, and dramatically less expensive, than conventional X-ray diffraction (XRD) equipment of the period. The original instrument (Gen 1), and its successor that was introduced in 1976 (Gen 2), employed a horizontal goniometer with data output provided by an internal strip chart recorder. The third generation (Gen 3) instrument, introduced in 1995, was called Miniflex+. It provided a dramatic advance in X-ray power to 450 watts (by operating at 30kV and 15mA) and Windows® PC computer control. Both the Miniflex+ and the succeeding generation products employ a vertical goniometer and allow the use of an automatic sample changer. The fourth generation (Gen 4) Miniflex II instrument was introduced in 2006 and offered the advance of a monochromatic X-ray source and a D/teX Ultra 1D silicon strip detector. The fifth generation (Gen 5) MiniFlex600 system, introduced in 2012, built upon this legacy with 600W of available power and new PDXL powder diffraction software.
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Data example from HyPix-400 MF detector

Overview:

  • New 6th generation design
  • Compact, fail-safe radiation enclosure
  • Incident beam variable slit
  • Simple installation and user training
  • Factory aligned goniometer system
  • Laptop computer operation
Measurements:
  • Phase identification
  • Phase quantification
  • Percent (%) crystallinity
  • Crystallite size and strain
  • Lattice parameter refinement
  • Rietveld refinement
  • Molecular structure
Options:
  • 8-position autosampler
  • Graphite monochromator
  • D/teX Ultra: silicon strip detector
  • HyPix-400 MF: 2D HPAD detector
  • Air sensitive sample holder
  • Travel case

MiniFlex accessories

ASC-8 : automatic 8 position sample changer with spinner
Automatic 8-position sample changer is compact and rugged. Integrated spinning improves particle statistics in polycrystalline sample measurements. Fully automatic alignment. Programmable.
 
Sample holders
Various sample holder are available to meet the specific needs of particular applications.
 
Specimen rotation attachment
The sample rotation stage allows continuous rotation at variable
speed of the sample holder to improve particle statistics during
powder diffraction measurements.
 
Graphite monochromator for D/teX Ultra
The graphite monochromator optimizes sensitivity by lowering the background level. It improves signal-to-noise by eliminating fluorescence from Mn, Fe, Co, and Ni containing materials.
 
Air-sensitive sample holder
An enclosed sample holder is available for users studying materials that might degrade in the presence of oxygen.
 
D/teX Ultra high speed detector
This 1D silicon strip detector is optionally available for fast, high-resolution scanning.
 
BTS 500 high temperature attachment
The high temperature attachment can heat a sample to do in-situ powder diffraction measurements under high temperature conditions from ambient to 500°C.
 
HyPix-400 MF: 2D HPAD detector
Advanced hybrid array pixel detector (HPAD) with zero background noise, an active area of ​​400 mm2, spatial resolution of 100 μm, and maximum count rate of 106 cps/pixel or more. HyPix-400 can operate in 0D, 1D or 2D modes.

PDXL is a one-stop full-function powder diffraction analysis software suite. The modular design, advanced engine and user-friendly GUI have been satisfying both experienced and novice users since PDXL was released in 2007.

PDXL provides various analysis tools such as automatic phase identification, quantitative analysis, crystallite-size analysis, lattice constants refinement, Rietveld analysis, ab initio structure determination, etc.

Fundamental parameter method

The peak shape in a powder diffraction pattern would appear to be a delta function if measured under ideal conditions. In reality, the peak shape changes depending on a number of measurement conditions: wavelength distribution of the source, optical systems, slit conditions, crystallite size and strain, and so on. The peak shapes obtained from measurements made under real-world conditions are described using an empirical function such as a split pseudo-Voigt function, or a split Pearson VII function which has a good agreement with the obtained peak shapes. The fundamental parameter method (FP method) is a method to calculate peak shape by convolution of the shapes caused by all the instrumental and sample conditions.

Phase identification using COD

The Crystallography Open Database (COD) is a free, public-domain database of the crystal structures published in International Union of Crystallography, Mineralogical Society of America and so on. PDXL can incorporate both ICDD/PDF-2 and COD to perform automatic phase identification, adding the COD library of over 150,000 crystal structures to PDXL 2’s already substantial capabilities.
Wizard for ab initio crystal structure analysis
Recently, there have been many published examples of ab initio crystal structure analysis performed on powder diffraction data. This development is attributed primarily to significant improvements in PC processing speed and in the efficiency of the algorithms used for structure determination.

PDXL has so far provided all of the functions required for ab initio crystal structure analysis, such as indexing, structure determination and structure refinement by the Rietveld method. Now the “Structure Analysis Wizard” is available in PDXL to provide support and guidance for users undertaking the complicated procedure of structure analysis, particularly of organic compounds. This wizard system will make it possible for even the beginner to achieve analytical success

Clustering function
The PDXL clustering feature can group multiple scan data based on the similarity of powder diffraction patterns and peak positions, and displays the grouped data in an easy-to-read tree. This is particularly effective when it comes to classifying and screening the data from a large number of scans.

  • Search/Match analysis with PDF-2 and Crystallography Open Database
  • Quantitative analysis
  • Percent crystallinity
  • Crystallite size and strain
  • Cell refinement
  • Residual stress
  • Indexing
  • Whole pattern profile fitting
  • Ab initio structure solving with wizard
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