UNSWSolid state and Elemental Analysis Unit

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Solid State and Elemental Analysis Unit

Summary of available instruments:

  • X’pert Pro MPD - programmable slits, curved monochromator, automatic sample changer, used for powder diffraction.
  • Philips PW1830 - fixed slits, graphite monochromator, B-B goniometer, use for qualitative and quantitative analysis of powder and bulk samples.
  • Philips PW1729 - fixed slits, graphite monochromator, high temperature (20 - 1400 dc) for powder samples (system is undergoing repairs).
  • X’pert Pro MRD - X-ray mirror, (220) Ge monochromator, X-ray lens, mono-capillary, trible-axis, used for analysis of thin films, nano-structure, semiconductor materials, stresses and textures.
  • Bruker Kappa Apex and Enraf Nonius - Single Crystal diffraction, operated by our qualified staff.
  • Leica 165C Microscope (90x) for mounting crystals for x-ray diffraction, and viewing other XRD samples. Fitted with a CCD camera for digital image collection.
  • Mikropack NanoCalc 2000 - 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.

Summary of data processing software and databases:

  • High Score plus with ICDD database; Epitaxy; Textures; ProFit (window); Reflectivity (v1.2); Stresses

Philips X’pert Multipurpose X-ray Diffraction System ("MPD")


The Philips X’pert Multipurpose X-ray Diffraction System (MPD) is a theta to theta goniometer system. 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 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.

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.


Philips PW1830 X-ray Diffraction System ("PW1830")


The Philips PW1830 is a conventional system of Bragg-Brentano diffractometer. It has fixed divergence slits at the incident beam path, and receiving slit, anti-scattering slit, graphite monochromator and one proportional detector at the diffracted beam path.

Normal setting conditions: the divergence slit = 1 degree, the anti-scarttering slit = 1 degree and the receive slit = 0.1 mm. X-ray operating conditions: tension = 40 kV and current = 30 mA.

The PW1830 is a reliable system, suitable for qualitative and quantitative analysis of powder or bulk samples. Its control software is the X’pert Data Collector. Users can use HighScore plus or SIROQUANT for quantitative analysis.


Philips X’pert Materials Research diffractometer ("MRD")


The Philips X’pert Materials Research diffractomter (MRD) system is the most flexible X-ray diffraction system. It is equipped with a few active components, such as an X-ray mirror, Ge 220 monochromator, X-ray lens and mono-capillary for incident beam conditioning, and parallel plate collimator or trible-axis for diffracted beam conditioning. A proportional detector is currently in use, although this will be upgraded shortly.

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” wafer samples. The sample must be a bulk solid, no thicker than 9 mm (for the 4” sample stage) or 4 mm (for the vacuum stage).

The MRD runs in five different 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 4 - low resolution module with the Co 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. The request for use of the other modes must be sent to the lab manager before the booking and around 30 minutes allowance for configuration of the hardware and software. Operation on Setting 5 can only be performed by a qualified member of staff.


Bruker Kappa Apex and Enraf Nonius Single Crystal Diffractometers


The Bruker Kappa Apex and Enraf Nonius diffractometers are used to determine the molecular and crystal structure of materials from a single crystal.


Currently the instruments can be operated by experienced staff only, although specialised user training is possible. Contact Mohan Bhadbhade (Tel - 02 9385 9898, Office M68 - access via Lab G65) or Don Craig (02 9385 4595, Office M65 - access via Lab G61) .


Click here to view the crystallography sample submission form.


Leica 165C Microscope


The Leica has 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. Images and dimensions of a crystal can be collected using the CCD 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.


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. 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.



SSEAU

Unit Administration
Room M64
Chemical Sciences Bldg F10
University of NSW
Kensington NSW 2052
T +61 (2) 9385 4693
F +61 (2) 9385 4663

Deliveries (before 4pm)
Chemistry Store
Lower Ground
Chemical Sciences Bldg F10
Via Gate 2 High Street
University of NSW
Kensington NSW 2052

c.marjo@unsw.edu.au

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SSEA Unit - UNSW - Chemical Sciences Building F10, Sydney, NSW 2052 Australia | Tel: +61 (2) 9385 4693 Fax: +61 (2) 9385 4663
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Page Last Updated: Friday, April 13, 2007 10:32 AM