|TITANIUM||AFM - Raman - SNOM||Modular AFM||Automated AFM||Practical AFM|
at the nanometer scale:
AFM + Confocal Raman + SNOM + TERS
NTEGRA Spectra Brochure (8 Mb)
|Working principle||TERS Probes||Applications||Specifications||Downloads||Contact Us|
Integration of SPM and confocal microscopy/Raman scattering spectroscopy. Owing to Tip Enhances Raman Scattering it allows carrying out spectroscopy/microscopy with up to 10 nm resolution.
NTEGRA Spectra - AFM / CONFOCAL RAMAN & FLUORESCENCE / SNOM / TERS
Integration: The key to the new sciences
Change happens at interfaces and today’s most exciting changes in microscopy are happening where multiple technologies are interfaced together. NTEGRA Spectra is a prime example, uniting the full power of atomic force microscopy (AFM), confocal Raman and fluorescence microscopy and scanning near-field optical microscopy (SNOM) in one platform. more info
Different configuration of AFM with confocal Raman/Fluorescence microscope
- Atomic Force Microscopy ( > 30 modes )
- Confocal Raman / Fluorescence / Rayleigh Microscopy
- Scanning Near-Field Optical Microscopy ( SNOM / NSOM )
- Optimized for Tip Enhanced Raman and Fluorescence (TERS, TEFS, TERFS) and scattering SNOM (s-SNOM)
Ntegra Spectra equipped with new electronics and software allows to combine a recently developed innovative HybriD Mode™ (HD-AFM™ Mode) for nanomechanical proprieties and Raman for chemical imaging of exactly the same area within single measurement session.
- Cantilever-type, Excellent and Reliable
- Enhancement factors: 100x and more
- Lateral resolution in TERS: down to 10nm
- High speed TERS mapping
- Top-down illumination configuration (opaque samples)
- Based on commercial AFM cantilevers (contact, non-contact): multiple AFM modes, excellent imaging performance
Introduction to TERS (nano-Raman)
Tip Enhanced Raman Scattering (TERS, nano-Raman) is the technique for enhancement of weak Raman signals and for super-resolution Raman imaging with spatial resolution ~10 nm. Nano-Raman imaging provides unique insights into sample structure and chemical composition on the nanometer scale.
In TERS, a sharp metal probe (nano-antenna) is used to localize and enhance optical field at the tip apex (fig. 1a). The light enhancement is typically reached when excitation laser light is in resonance with localized surface plasmon at the end of the TERS probe (fig. 1b). Enhancement of electromagnetic field (light) intensity on the TERS probe apex can reach many orders of magnitudes. In TERS mapping the sample is scanned with respect to the nano-antenna; the enhanced Raman signal localized near the probe apex is measured resulting in Raman maps of the sample surface with nanometer scale resolution.
TERS (nano-Raman) imaging by NT-MDT AFM-Raman instrument
NT-MDT develops and supplies unique instrumentation for AFM integration with various optical microscopy and spectroscopy techniques. NT-MDT was the first to introduce integrated AFM-Raman instrument in 1998 and is now the leading developer and supplier of such instruments worldwide.
NT-MDT AFM-Raman instrument has been successfully used for TERS (nano-Raman) mapping of various objects with spatial resolution reaching 10 nm: graphene and other carbon nanomaterials, polymers, thin molecular layers (including monolayers), semiconductor nanostructures, lipid membranes, various protein structures, DNA molecules etc. References to corresponding publications can be found at download page.
TERS probe challenge
While the AFM-Raman instrumentation has been developing relatively fast, TERS probes have always remained main limiting factor for nano-Raman to become routine characterization technique. The main challenges are: (i) manufacturing reproducible probes with high enhancement factors and high resolution imaging capabilities; (ii) probe lifetime; (iii) probe ease of use; (iv) probe mass production not involving complicated and poorly reproducible manual procedures.
TERS probes originally used in scientific publications were usually etched metal wires - attached to tuning fork or working in STM (tunneling) regime. Preparation of such probes requires elaborated manual operations; probes are typically not very reproducible. Another approach to TERS probe preparation utilizes focused ion beam to manufacture special structure on the tip end. This approach is very resource consuming and also lacks reproducibility. Different metal coatings of AFM cantilevers have been reported recently – with different degrees of enhancements and reproducibility.
Reproducible TERS probes from NT-MDT
As a result of comprehensive research performed together with NT-MDT customers and partners, NT-MDT is now able to offer to its AFM-Raman customers mass produced reproducible cantilever-type TERS probes. The probes are prepared based on so-called “Top Visual” AFM Si cantilevers (Fig. 2). Special proprietary probe preparation and TERS metal coating are applied.
AFM probes can have different stiffness and can be optimized for contact and non-contact regimes.
Protruding “nose-type” shape of the probes allows Raman laser light to be focused on the probe apex from the top: for use with non-transparent samples.
The probes provide guarantied TERS performance on a test sample (organic molecules on Au substrate):
- Enhancement factor >50x (Tip IN vs. Tip. OUT) for ~70% of probes. Typical enhancement factor : > 100x. Some probes reach >500x enhancement.
- TERS (nano-Raman mapping). ~20-70 nm resolution. >50% of probes.
- Remarkable lifetime without considerable enhancement degradation
The AFM TERS probes also feature excellent AFM performance in contact and non-contact regimes since they are prepared based on standard Si AFM cantilevers produced by mass technology. All advanced AFM modes (electrical, magnetic, nanomechanical etc.) are available with NT-MDT TERS probes. High resonance quality factors (for non-contact probes) allow excellent force sensitivity and guarantee long tip lifetime during measurements.
STM TERS probes (electrochemically etched metal wires) and TERS probes attached to tuning fork are also available.
The NT-MDT TERS probes reach their highest characteristics with the unique AFM-Raman instrument from NT-MDT: specifically designed for TERS research.
Probes are only supplied to be used with NT-MDT instrumentation. Contact us for more information.
More technical information about TERS cantilevers: http://www.ntmdt-tips.com/products/group/ters-afm-probes-new
|Confocal Raman/Fluorescence microscopy|
|AFM/STM: Integration with spectroscopy|
|Scanning Near Field Optical Microscopy (SNOM)|
|Optimized for Tip Enhanced Raman Scattering (TERS) and other tip-related optical techniques
(S-SNOM, SNIM, TEFS, STM-LE etc.)
|Confocal Raman/Fluorescence microscopy
|Confocal Raman/Fluorescence/Rayleigh imaging runs simultaneously with AFM (during one sample scan)|
|Diffraction limited spatial resolution: <200 nm in XY, <500 nm in Z (with immersion objective)|
|True confocality; push button from software to control the motorized confocal pinhole for optimal signal and confocality|
|Motorized variable beam expander/collimator: adjusts diameter and collimation of the laser beam individually for each laser and each objective used|
|Full 3D (XYZ) confocal imaging with powerful image analysis|
|Hyperspectral imaging (recording complete Raman spectrum in every point of 1D, 2D or 3D confocal scan) with further software analysis|
|Optical lithography (vector, raster)|
AFM/STM: Integration with spectroscopy
|Upright and Inverted optical AFM configurations (optimized for opaque and transparent samples correspondingly);
side illumination option
|Highest possible resolution (numerical aperture) optics is used simultaneously with AFM: 0.7 NA for Upright, 1.3–1.4 NA for Inverted|
|AFM/STM and confocal Raman/Fluorescence images are obtained simultaneously (during one scan)|
|All standard SPM imaging modes are supported (>30 modes) — combined with confocal Raman/Fluorescence|
|Low noise AFM/STM (atomic resolution)|
|Vibrations and thermal drifts originating from optical microscope body are minimized due to special design of optical AFM heads|
|Focus track feature: sample always stays in focus due to AFM Z-feedback; high quality confocal images of very rough or inclined samples can be obtained|
|Seamless integration of AFM and Raman; all AFM/ Raman/SNOM experiment and further data analysis is performed in one and the same software|
|Powerful analysis of 1D, 2D and 3D hyperspectral images|
|Powerful export to other software (Excel, MatLab, Cytospec etc.)|
|Extremely high efficiency 520 mm length spectrometer with 4 motorized gratings|
|Visible, UV and IR spectral ranges available
|Echelle grating with ultrahigh dispersion; spectral resolution: 0.007 nm (< 0.1 1/cm)**|
|Up to 3 different detectors can be installed
|Flexible motorized polarization optics in excitation and detection channels, cross-polarized Raman measurements|
|Fully automated switch between different lasers — with a few mouse clicks|
Scanning Near Field Optical Microscopy (SNOM)
|Two major SNOM techniques supported: (i) based on quartz fiber probes, (ii) based on silicon cantilever probes|
|All modes supported: Transmission, Collection, Reflection|
|All SNOM signals detected: laser intensity, fluorescence intensity, spectroscopy|
|SNOM lithography (vector, raster)|
Optimized for Tip Enhanced Raman Scattering (TERS) and other tip-related optical techniques
(S-SNOM, SNIM, TEFS, STM-LE etc.)
|All existing TERS geometries are available: illumination / collection from bottom, from top or from side|
|Different SPM techniques and TERS probes can be used: STM, AFM cantilever, quartz tuning fork in tapping and shear force modes|
|Dual scan (for Hot Point Mapping in TERS): scan by sample AND scan by tip / by laser spot|
|Motorized polarization optics to produce optimal polarization for TERS|
AFM-Raman measurements can run in air, in controlled atmosphere or in liquid — all with variable temperature (for Inverted configuration)
Some features listed are optional — not included into basic system configuration
* NT-MDT AFM can be integrated with Renishaw inVia or with NT-MDT spectrometer. Specifications are given for the latter. Renishaw specifications can be found at www.renishaw.com/AFM-Raman
** Exact value of spectral resolution highly depends on how “resolution” is defined
- NTEGRA Spectra Brochure (8.27 Mb)
- Scanning near-field optical microscopy (SNOM) (5.52 Mb)
- Tip Enhanced Raman Scattering (TERS) (8.89 Mb)
- Graphene (2.14 Mb)
- Characterization of Materials with a Combined AFM/Raman Microscope. Summary AN 089s (0,99 Mb)
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- Characterization of Materials with a Combined AFM/Raman Microscope AN 089 (1,18 Mb)
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- Solar Cell Diagnostics by Combination of Kelvin Probe Force Microscopy with Local Photoexitation
AN 091 (0,7 Mb)
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- AFM-Raman Characterization of Pharmaaceutical Tablets AN 092 (0,7 Mb)
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- AFM – Raman Characterization of Li-ion Batteries AN 093 (1,19 Mb)
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- Interplay between Raman Scattering and Atomic Force Microscopy in Characterization of Polymer
Blends AN 094 (0,9 Mb)
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- Zhang, M. & Wang, J. Plasmonic lens focused longitudinal field excitation for tip-enhanced Raman spectroscopy. Nanoscale Res. Lett. 10, 189 (2015).
- Baitimbetova, B. & Vermenichev, B. New Method for Producing Graphene by Magnetron Discharge in an Atmosphere of Aromatic Hydrocarbons. Graphene 04, 3844 (2015).
- Horimoto, N. N., Tomizawa, S., Fujita, Y., Kajimoto, S. & Fukumura, H. Nano-scale characterization of binary self-assembled monolayers under an ambient condition with STM and TERS. Chem. Commun. (Camb). 13 (2014)
- Lipiec, E., Sekine, R., Bielecki, J., Kwiatek, W. M. & Wood, B. R. Molecular characterization of DNA double strand breaks with tip-enhanced Raman scattering. Angew. Chem. Int. Ed. Engl. 53, 16972 (2014).
- Liu, B.-T. & Kuo, H.-L. Graphene/silver nanowire sandwich structures for transparent conductive films. Carbon N. Y. 63, 390396 (2013).
- Pashaee, F., Hou, R., Gobbo, P., Workentin, M. S. & Lagugné-Labarthet, F. Tip-Enhanced Raman Spectroscopy of Self-Assembled Thiolated Monolayers on Flat Gold Nanoplates Using Gaussian-Transverse and Radially Polarized Excitations. J. Phys. Chem. C 117, 1563915646 (2013).
- Lee, Y.-H. et al. Synthesis of large-area MoS2 atomic layers with chemical vapor deposition. Adv. Mater. 24, 23205 (2012).
- Duong, D. L. et al. Probing graphene grain boundaries with optical microscopy. Nature 490, 2359 (2012).
- Hermann, P. et al. Imaging and strain analysis of nano-scale SiGe structures by tip-enhanced Raman spectroscopy. Ultramicroscopy 111, 16305 (2011).
- Stadler, J. et al. Tip-enhanced Raman spectroscopic imaging of patterned thiol monolayers. Beilstein J. Nanotechnol. 2, 50915 (2011).
- Kagan, V. E. et al. Carbon nanotubes degraded by neutrophil myeloperoxidase induce less pulmonary inflammation. Nat. Nanotechnol. 5, 3549 (2010).
- Stadler, J., Schmid, T. & Zenobi, R. Nanoscale chemical imaging using top-illumination tip-enhanced Raman spectroscopy. Nano Lett. 10, 451420 (2010).
- Bradac, C., Gaebel, T., Naidoo, N., Rabeau, J. R. & Barnard, A. S. Prediction and measurement of the size-dependent stability of fluorescence in diamond over the entire nanoscale. Nano Lett. 9, 355564 (2009).
- Kharintsev, S. S., Hoffmann, G. G., Dorozhkin, P. S., With, G. De & Loos, J. Atomic force and shear force based tip-enhanced Raman spectroscopy and imaging. Nanotechnology 18, 315502 (2007).
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