skip to main content
OSTI.GOV title logo U.S. Department of Energy
Office of Scientific and Technical Information

Title: Co-registered Topographical, Band Excitation Nanomechanical, and Mass Spectral Imaging Using a Combined Atomic Force Microscopy/Mass Spectrometry Platform

Journal Article · · ACS Nano

The advancement of a hybrid atomic force microscopy/mass spectrometry imaging platform demonstrating for the first time co-registered topographical, band excitation nanomechanical, and mass spectral imaging of a surface using a single instrument is reported. The mass spectrometry-based chemical imaging component of the system utilized nanothermal analysis probes for pyrolytic surface sampling followed by atmospheric pressure chemical ionization of the gas phase species produced with subsequent mass analysis. We discuss the basic instrumental setup and operation and the multimodal imaging capability and utility are demonstrated using a phase separated polystyrene/poly(2-vinylpyridine) polymer blend thin film. The topography and band excitation images showed that the valley and plateau regions of the thin film surface were comprised primarily of one of the two polymers in the blend with the mass spectral chemical image used to definitively identify the polymers at the different locations. Data point pixel size for the topography (390 nm x 390 nm), band excitation (781 nm x 781 nm), mass spectrometry (690 nm x 500 nm) images was comparable and submicrometer in all three cases, but the data voxel size for each of the three images was dramatically different. The topography image was uniquely a surface measurement, whereas the band excitation image included information from an estimated 10 nm deep into the sample and the mass spectral image from 110-140 nm in depth. Moreover, because of this dramatic sampling depth variance, some differences in the band excitation and mass spectrometry chemical images were observed and were interpreted to indicate the presence of a buried interface in the sample. The spatial resolution of the mass spectral image was estimated to be between 1.5 m 2.6 m, based on the ability to distinguish surface features in that image that were also observed in the other images.

Research Organization:
Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
Grant/Contract Number:
AC05-00OR22725
OSTI ID:
1185909
Journal Information:
ACS Nano, Vol. 9, Issue 4; ISSN 1936-0851
Publisher:
American Chemical Society (ACS)Copyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 28 works
Citation information provided by
Web of Science

References (46)

Thin-layer chromatography and mass spectrometry coupled using proximal probe thermal desorption with electrospray or atmospheric pressure chemical ionization: TLC and MS coupled using proximal probe TD/I with ESI or APCI journal May 2010
Molecular Surface Sampling and Chemical Imaging using Proximal Probe Thermal Desorption/Secondary Ionization Mass Spectrometry journal January 2011
Combined Atomic Force Microscope-Based Topographical Imaging and Nanometer-Scale Resolved Proximal Probe Thermal Desorption/Electrospray Ionization–Mass Spectrometry journal June 2011
Atomic Force Microscope Controlled Topographical Imaging and Proximal Probe Thermal Desorption/Ionization Mass Spectrometry Imaging journal December 2013
Low-stiffness silicon cantilevers with integrated heaters and piezoresistive sensors for high-density AFM thermomechanical data storage journal March 1998
Micro-thermal analysis: scanning thermal microscopy and localised thermal analysis journal December 1999
Micro-thermal analysis and evolved gas analysis journal March 2001
Localised Evolved Gas Analysis by Micro-thermal Analysis journal April 2001
Micro-thermal analysis of polymers: current capabilities and future prospects journal March 2001
Sub-micron proximal probe thermal desorption and laser mass spectrometry on painting cross-sections journal January 2014
Measuring adhesion, attraction, and repulsion between surfaces in liquids with an atomic-force microscope journal May 1992
Quantitative Mapping of the Elastic Modulus of Soft Materials with HarmoniX and PeakForce QNM AFM Modes journal November 2012
An atomic force microscope tip designed to measure time-varying nanomechanical forces journal July 2007
The simultaneous measurement of elastic, electrostatic and adhesive properties by scanning force microscopy: pulsed-force mode operation journal November 1997
Mapping nanoscale elasticity and dissipation using dual frequency contact resonance AFM journal August 2011
Three dimensional imaging using secondary ion mass spectrometry and atomic force microscopy journal December 2011
The SFM/ToF-SIMS combination for advanced chemically-resolved analysis at the nanoscale journal November 2014
Plasma Ionization Source for Atmospheric Pressure Mass Spectrometry Imaging Using Near-Field Optical Laser Ablation journal December 2014
The new future of scanning probe microscopy: Combining atomic force microscopy with other surface-sensitive techniques, optical microscopy and fluorescence techniques journal January 2009
Imaging methods for elemental, chemical, molecular, and morphological analyses of single cells journal March 2010
Correlated imaging – a grand challenge in chemical analysis journal January 2013
Visualizing the Subsurface of Soft Matter: Simultaneous Topographical Imaging, Depth Modulation, and Compositional Mapping with Triple Frequency Atomic Force Microscopy journal October 2013
The band excitation method in scanning probe microscopy for rapid mapping of energy dissipation on the nanoscale journal September 2007
Band Excitation in Scanning Probe Microscopy: Recognition and Functional Imaging journal April 2014
Viscoelastic Properties of Poly(2-vinylpyridine) in Bulk and Solution journal December 1996
Surface induced self assembly in thin polymer films journal March 1995
Morphologies in Ternary Polymer Blends after Spin-Coating journal July 1999
Perspectives on Organic Photovoltaics journal October 2010
Are Clusters Important in Understanding the Mechanisms in Atmospheric Pressure Ionization? Part 1: Reagent Ion Generation and Chemical Control of Ion Populations journal May 2014
Ring Structure of Cyclic Poly(2-vinylpyridine) Proved by Pyrolysis−GC/MS journal October 1999
Field penetration and band bending near semiconductor surfaces in high electric fields journal February 1979
Modeling the effect of subsurface interface defects on contact stiffness for ultrasonic atomic force microscopy journal June 2004
Thin film characterization by atomic force microscopy at ultrasonic frequencies journal April 2000
The Shannon sampling theorem—Its various extensions and applications: A tutorial review journal January 1977
Atomic and Molecular Imaging at the Single-Cell Level with TOF-SIMS journal July 1997
Tissue Imaging Using Nanospray Desorption Electrospray Ionization Mass Spectrometry journal December 2011
Laser microdissection and atmospheric pressure chemical ionization mass spectrometry coupled for multimodal imaging: LA-APCI/MS imaging journal May 2013
Infrared Matrix-Assisted Laser Desorption Electrospray Ionization (IR-MALDESI) Imaging Source Coupled to a FT-ICR Mass Spectrometer journal December 2012
Transmission geometry laser ablation into a non-contact liquid vortex capture probe for mass spectrometry imaging
  • Ovchinnikova, Olga S.; Bhandari, Deepak; Lorenz, Matthias
  • Rapid Communications in Mass Spectrometry, Vol. 28, Issue 15, p. 1665-1673 https://doi.org/10.1002/rcm.6946
journal June 2014
Ambient imaging mass spectrometry by electrospray ionization using solid needle as sampling probe journal October 2009
Improving Secondary Ion Mass Spectrometry Image Quality with Image Fusion journal June 2014
Nanoscale chemical analysis by tip-enhanced Raman spectroscopy journal February 2000
AFM–IR: Combining Atomic Force Microscopy and Infrared Spectroscopy for Nanoscale Chemical Characterization journal December 2012
Analysis of Pigmented Inkjet Printer Inks and Printed Documents by Laser Desorption/Mass Spectrometry journal January 2010
Morphology Mapping of Phase-Separated Polymer Films Using Nanothermal Analysis journal August 2010
Dynamic atomic force microscopy methods journal September 2002

Cited By (2)

Application of pan-sharpening algorithm for correlative multimodal imaging using AFM-IR journal April 2019
Molecular profiling of single axons and dendrites in living neurons using electrosyringe-assisted electrospray mass spectrometry journal January 2019