Pharmaceutical Research

, Volume 24, Issue 11, pp 2048–2054 | Cite as

Nanoscale Characterisation and Imaging of Partially Amorphous Materials using Local Thermomechanical Analysis and Heated Tip AFM

  • Ljiljana Harding
  • William P. King
  • Xuan Dai
  • Duncan Q. M. Craig
  • Mike Reading
Research Paper



The purpose is to investigate the use of thermal nanoprobes in thermomechanical and heated tip pulsed force modes as novel means of discriminating between amorphous and crystalline material on a sub-micron scale.

Materials and methods

Indometacin powder was compressed and partially converted into amorphous material. Thermal nanoprobes were used to perform localised thermomechanical analysis (L-TMA) and heated tip pulsed force mode imaging as a function of temperature.


L-TMA with submicron lateral spatial resolution and sub-100 nm depth penetration was achieved, allowing us to thermomechanically discriminate between amorphous and crystalline material at a nanoscale for the first time. The amorphous and crystalline regions were imaged as a function of temperature using heated tip pulsed force AFM and a resolution of circa 50 nm was achieved. We are also able to observe tip-induced recrystallisation of the amorphous material.


The study demonstrates that we are able to discriminate and characterise amorphous and crystalline regions at a submicron scale of scrutiny. We have demonstrated the utility of two methods, L-TMA and heated tip pulsed force mode AFM, that allow us to respectively characterise and image adjacent amorphous and crystalline regions at a nanoscale.


The study has demonstrated that thermal nanoprobes represent a novel method of characterising and imaging partially amorphous materials.

Key words

amorphous atomic force microscopy glass transition indometacin microthermal analysis 



atomic force microscopy


localised thermomechanical analysis


microthermal analysis


pulsed force mode



We would like to thank the EPSRC for financial support for L Harding.

We wish to declare that Mike Reading is a director of Anasys Instruments who are marketing the probes designed by Bill King.


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Copyright information

© Springer Science+Business Media, LLC 2007

Authors and Affiliations

  1. 1.School of Chemical Sciences and PharmacyUniversity of East AngliaNorwichUK
  2. 2.Department of Mechanical Science and EngineeringUniversity of Illinois Urbana-ChampaignUrbanaUSA

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