Instruments

We have 7 powder XRD systems of which four are generally used for thin-film analysis and three are used for Bragg-Brentano bulk powder analysis. We have a range of X-ray sources (rotating anode, Cu, Co, Ag) and special samples stages for analysis at variable temperatures and under different atmospheres. We have two Bruker single-crystal XRD systems (Mo sources) for chemical crystallography.

PANalytical MPD

The PANalytical Xpert Multipurpose X-ray Diffraction System (MPD) is a theta to theta goniometer system with programmable slits, curved monochromator, automatic sample changer, used for powder diffraction. The sample stays at the leveled position during the measurement. Thus it is possible to test gel or liquid samples. 

It is equipped with the following components: 

  • Incident beam path - Programmable divergence slit, which can be configured as a fixed slit or a variable slit, with masks.
  • Diffracted beam path - Programmable anti-scattering slit and receiving slit, curved monochromator and proportional detector.
  • Automatic multi-sample changer (15 samples) can increase productivity and a sample spinner is to eliminate the preferred orientation.

The X-ray operating conditions are 45 kV and 40 mA. The MPD is suitable for routine measurement of powder samples, either phase identification or quantitative analysis. Sample should be enough to fill the holder of 25 mm diameter and 5 mm depth. 

  • Incident beam path - Programmable divergence slit, which can be configured as a fixed slit or an variable slit, masks.
  • Diffracted beam path - Programmable anti-scattering slit and receiving slit, curved monochromator and proportional detector.
  • Automatic multi-sample changer (15 samples) can increase productivity and a sample spinner is to eliminate the preferred orientation.

PANalytical MRD

The PANalytical Xpert Materials Research diffractomter (MRD) system is a flexible X-ray diffraction system for analysis of thin films, nano-structures, semiconductor materials, stresses and textures. It is equipped with several active components including  an X-ray mirror, Ge 220 monochromator, X-ray lens and mono-capillary for incident beam conditioning, and parallel plate collimator or triple-axis for diffracted beam conditioning. 

It can be configured to suit quite wide range of applications, such as phase identification for thin film, analysis of stresses and textures, rocking curve analysis, reciprocal space mapping and X-ray reflectivity. 

The MRD has been heavily used for research on thin films and nanomaterials. The polycrystalline phases within a film of 20 nanometer thick can be precisely identified using grazing angle diffraction. 

The MRD is also equipped with a Vacuum Stage and can safely test 8 inch wafer samples. The sample must be a bulk solid, no thicker than 9 mm (for the standard sample stage) or 4 mm (for the vacuum stage). 

The MRD runs in the following modes: 

  • MRD Setting 1 - high resolution module with the X-ray mirror + Ge (220) monochromator, used for rocking curve, reciprocal space mapping.
  • MRD Setting 2 - medium resolution module with the X-ray mirror and collimator, used for thin film analysis and phase identification.
  • MRD Setting 3 - low resolution module with the Cu tube, X-ray lens and collimator, used for analysis of textures and stresses and phase identification.
  • MRD Setting 5 - medium resolution transmission module with X-ray mirror and collimator; used for phase identification of tiny powder sample (less than 0.5 g) and specific XRD transmission measurement.

The MRD is normally configured at Setting 2 and requests for use in other modes must be sent to the lab manager before the booking and at least 30 minutes allowance for configuration of the hardware and software. Operation on Setting 5 can only be performed by a qualified member of staff.

PANalytical Empyrean 1 Thin-Film XRD

The Empyrean Thin-Film XRD is a copper tube system mainly used for thin-film analysis. the instrument has a cryostage and heating stages for dynamic monitoring of phase changes ranging from 10-1800 Kelvin. Heating experiments can be performed using a controlled atmosphere or vacuum. Contact the laboratory manager for measurements using one of the specialised stages.

PANalytical Empyrean 2 Co Source XRD

This Empyrean XRD is a cobalt source instrument using Bragg-Brentano geometry for loose powders. The cobalt source is useful for samples with high iron, as a copper generates X-ray fluorescence and poor background in this type of sample. The system is fitted with a sample changer and an optics for the incident beam to minimise background interference.

PANalytical Empyrean 3 Ag Source XRD

This Empyrean XRD is a silver source instrument fitted with a position-sensitive detector designed to capture a wide 2theta range for in situ experiments and capillary measurements.

Bruker D8 Thin-Film XRD with Rotating Anode

This is a flexible instrument with a rotating copper anode X-ray source (5-6 kW) that enables a higher X-ray flux at your sample than is possible with the sealed X-ray sources on the other instruments. It uses a centric Eulerian cradle that integrates Chi and Phi rotations, and X-Y-Z translations. The instrument can be set up with a 1-dimensional compound silicon strip detector (the "Lynx-Eye") for ultra fast X-ray diffraction measurements, as well as a large area detector (the "VÅNTEC-500" with 13.5 cm diameter) for 2D XRD experiments including RSM and diffraction mapping. The instrument can be operated with an Anton Paar DCS 350 Wide Range Chamber enabling measurements under vacuum between -100°C up to +350°C. Contact Dr Yu Wang to discuss access on this instrument.

Rigaku Smartlab Thin-Film XRD with Rotating Anode

This is a powerful thin-film analysis instrument with a rotating copper anode X-ray source (9 kW) that enables a higher X-ray flux at your sample than is possible with the sealed X-ray sources on the other instruments. Contact Dr Yu Wang to discuss access to this instrument.

Bruker Kappa Apex and Bruker Advance Single Crystal Diffractometers

The Bruker Kappa Apex and Bruker Advance are each fitted with micro-focus molybdenum sealed X-ray sources to determine the molecular and crystal structure of small molecules from a single crystal.

Currently the instruments can be operated by experienced staff only, although specialised user training is possible. Contact Dr Mohan Bhadbhade (Tel - 02 9385 9898, Office M67 - access via Lab G65). 

 

Thin Film Analyser - Mikropack NanoCalc 2000 UV-Vis-NIR

This instrument measures light reflected perpendicular to a sample surface which can provide information on the thickness of up to 4 layers in a sample, and is UV-light-NIR Thin film analyser which can provide a measurement of the thickness of multilayer films. Useful for an independent comparison with film-thickness measurements obtained on the MRD, for example. The wavelengths available range from 250nm to 850nm, which enable measurement of film thickness from 10nm up to 20micron. This instrument is located in lab G65, and it available at no charge to UNSW users.

Leica 165C and M205C Microscopes

These Leica optical microscope have a large working distance between the objective and sample and an incident cold light source to enable our crystallographers to mount single-crystals onto a capillary, prior to measuring the diffraction pattern. A digital Image and and dimensions of a crystal can be collected using a camera. When not in use by our crystallographers, the microscope may be used, at no cost, by UNSW researchers who require a low to medium magnification (max.90x) digital image of their sample.