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NTEGRA Spectra II


NTEGRA Spectra II, Versatile automated AFM-Raman, SNOM and TERS system

Versatile automated AFM-Raman, SNOM and TERS system

Brochure

  • Physical and chemical characterization at the nanoscale
  • Atomic Force Microscopy
  • Confocal Raman / Fluorescence Microscopy
  • Tip Enhanced Raman Scattering
  • Scanning Near-field Optical Microscopy
  • Open architecture system
  • Automated AFM alignment
  • User-friendly software
  • Ergonomic design

Key features

Integration

NTEGRA Spectra II is the first system on the market that seamlessly integrates the best of two worlds: AFM and Raman microscopy.

From topography to spectrum analysis, from electrical and mechanical properties to optical spatial resolution below the diffraction limit.

At the fingertips of scientists now is the capability to run a full surface analysis of a sample along with chemical study of the same area of interest.

Researches now receive unlimited possibilities to extend their laboratory capacity.

 

TERS by means of HybriD ModeTM

Tip Enhanced Raman Scattering allows carrying out spectroscopy/microscopy with nanometer scale resolution.

TERS imaging requires prolonged tip-sample contact at each scanning point, but Contact AFM is destructive for both the tip and the sample.

Thereby, HybriD ModeTM is a superior technique for cantilever-type TERS since it dramatically increases the tip lifetime, allows non-destructive studies, and besides enables Quantitative Nanomechanics.

The presented results using the example of graphene oxide flakes, show that HybriD ModeTM allows one to effectively enhance the Raman scattering and, at the same time, significantly reduces the mechanical effect on the sample and on the probe during scanning.

 

Intelligent ScanT™

Program has been developed with the help of neural networks to provide auto-tuning of scanning parameters for imaging in AM-AFM.

Automatic maintenance of attractive (non-contact) & repulsive (intermittent-contact) regimes.

Artefact-free scanning without parachuting. Perfect performance at samples with any kind of morphology.

To learn more


Al2O3 with ScanTTM

Working principle

Resolution and capabilities of different techniques

- Optical techniques (color imaging, physical & chemical analysis)
- Scanning probe microscopy (topography, mechanical, electrical, magnetic and other properties of the surface)
- AFM (STM) + Optical techniques = Dramatic increase of resolution and sensitivity

 

Solution for all possible excitation/detection, TERS and SNOM geometries


Solution for all possible excitation/detection and TERS geometries

Aperture Scanning Near-Field Optical Microscopy

Principal optical scheme NTEGRA Spectra II

  • Novel optical scheme consists of three independent channels of sample excitation: from top, side and bottom directions. Each channel is developed as independent module
  • Sample excitation directions are easy to exchange between each other. Light collection could be done by excitation optical channel or by different one
  • Open design provides great opportunities in system customization. Every particular channel allows to observe the sample by the objective with magnification factor up to 200x, excite the sample by laser beam and scan by focused laser spot
  • Excitation wavelength range is from 325 nm up to 1064 nm*

* Compatibility with other wavelength upon request

  • AFM registration laser system independent on Raman objective and this allows fast and easy exchange of objectives which are centered onto the same point on the surface
  • Automated AFM laser, probe and photodiode alignment minimize customer routine operations
  • User-friendly change of AFM registration system wavelength provides compatibility with any excitation or collection wavelength
  • Stand-alone optical periscope allows to combine AFM-Raman system with virtually all Raman spectrometers available on the market upon customer request
  • Spectrometer could be equipped with number of etectors: PMT, APD, CCD. Both Rayleigh optical image and Raman map could be obtained simultaneously

 

PS-PVAC blend



Raman spectra of PVAC & PS

Height

PVAC (2839 cm‑1 - 2980 cm‑1)

PS (3000 cm‑1 - 3140 cm‑1)
PS-PVAC blend: (а)-(d) Raman spectra of PVAC & PS, AFM topography, Intensity maps of Raman scattering bands specific to PVAC (orange) and PS (pink) overlayed on the topography

 

Applications

  • 0D materials: Quantum dots
  • 1D materials: Nanotubes, Nanowires
  • 2D materials: Graphene, Graphene Oxide, MoSe2, WS2 etc.
  • Piezoelectrics & Ferroelectrics
  • Photonic crystals
  • Surface plasmon polaritons
  • Biological objects: cells, DNA, viruses
  • Amyloid fibrils, peptide nanotapes, lipid monolayers
  • Polymers & Thin organic layers
  • Chemical reaction control
  • Optical device characterization:
    semiconductor lasers, optical fibers,
    waveguides, plasmonic devices

Graphene flakes
30x30 um

Ni foil
20x20 um

PC-PVAC film
30x30 um

MoO3
30x30 um

Webinars

AFM-Raman, SNOM and TERS: Recent Advances and Applications”. pdf (14.5 Mb)
Scanning Near-Field Optical Microscopy: Relevant Insights and Trends pdf (15 Mb)

 

CdS nanowire

CdS nanowire was connected with metal electrode by conductive polymer nanowires. AFM probe is positioned on the structure with the help of viewing microscope. Thanks to the shape of the AFM probe laser can be positioned directly onto the tip apex.

High resolution AFM images provide information about sample topography. Raman and luminescence maps taken from the same area show difference in nanowires chemical composition.


Optical viewing system image with approached AFM probe

Topography

Raman map (conductive polymer nanowires)

Photoluminescence (CdS)

Raman and PL spectrum of CdS nanowire
Sample courtesy: prof. R. Carpick, Penn State University. Scan size 20x20 µm

Graphene flake on Si/SiO2


Topography

G band intensity

2D band intensity

Raman spectra

 

Ultrafast Raman mapping

Fast Raman mapping is a crucial option for high-speed processes detection. Thanks to galvanic scanning mirror technology it is possible to acquire Raman map of selected band with acquisition time down to <50 us/point, which is about 1 sec/image.

Build-in capacitance sensors make possible laser spot positioning with precision less than 20 nm. This is especially important when one need to select a particular point on the acquired Raman map and position spot there for a long time. For example for "hot spot" finding in TERS or aperture finding in SNOM.

HybriD Mode™

NTEGRA Spectra II 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.

In HybriD mode the tip-sample distance is modulated according to the quasi-harmonic law. Thus tip enters a force interaction with the sample thousands times per second. Force-distance curve analysis enables maps of topographical, nanomechanical, electrical, thermal and piezoelectric properties of the sample to be extracted with high spatial resolution and minimized lateral forces.

High-performance electronic components and unique algorithms implemented in the state-of-the-art HybriD 2.0 Control Electronics provide superb level of real-time signal processing and analysis. Combining mode with cutting-edge optical microscopy and spectroscopy techniques opens-up novel opportunities of cantilever-based tip-enhanced Raman scattering (TERS) and scattering scanning near-field optical microscopy (s-SNOM).

To learn more

 


Stiffness of HDPE/LDPE polymer sandwich cut by microtomewe

Overlap of Raman maps: HDPE (red), LDPE (blue)

AFM topography

TERS

  • Cantilever-type, Excellent and Reliable
  • Enhancement factors: 100x and more
  • Lateral resolution in TERS: down to 10 nm
  • High speed TERS mapping
  • Top-down illumination configuration (opaque samples)
  • Based on commercial AFM cantilevers (contact, non-contact): multiple AFM modes, excellent imaging performance

Principle of Tip Enhanced Raman Scattering and other tip- assisted optical techniques (left). Localized surface plasmon (electron density oscillations) at the end of a metal TERS probe (nano-antenna), resulting in light localization and enhancement at the probe apex (right).

 

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. The light enhancement is typically reached when excitation laser light is in resonance with localized surface plasmon at the end of the TERS probe. 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 More information.


 

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. 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

SEM image of “Top Visual” AFM probe. Protruding probe geometry allows optical access to the apex from the top (left). Experimental TERS configuration (right).

 

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

 


Typical Raman signal enhancement (>100x) of NT-MDT TERS AFM probe

High resolution TERS map.
Resolution: ~20 nm. Sample: BCB thin molecular layer on Au substrate

High resolution TERS map of carbon nanotubes on Au substrate.
Resolution: ~10 nm

Specifications

Top-Grade Atomic Force Microscope

  • High-performance AFM: Z noise down to 15 pm
  • Spatial resolution: down to 1 nm
  • XYZ sample scanner: 100x100x10 μm
  • Automated AFM laser, probe and photodiode positioning and alignment
  • Simple exchange OBD registration system operational wavelength (670, 830, 1300 nm)
  • Different techniques and TERS probes can be used: STM, AFM cantilever, quartz tuning fork in tapping and shear force modes
  • HybriD ModeTM is a superior technique for cantilever-type TERS since it noticeably increases the tip lifetime and makes possible TERS imaging of soft, loose and fragile samples

 

Light delivery system

  • All existing TERS geometries: illumination & collection from bottom, from top or from side
  • Highest possible resolution optics is used simultaneously with AFM: up to 1.45 NA for Inverted, up to 0.7 NA for Upright, up to 0.7 NA for Side configurations
  • Exchangeable objectives with kinematic mounts: precision <2 μm
  • Independent CL controlled scanning mirrors for precise laser spot positioning & hot-spot maintenance
  • Built-in optical periscope allows integration of Spectra II with any commercial or home-built confocal Raman spectrometer

 

Spectroscopy

  • High efficiency 520 mm length spectrometer with 4 motorized gratings
  • Up to 5 lasers: from UV to IR range
  • Wavelength changes in a single click
  • Excitation wavelength range: 405-1050 nm
  • Spectral resolution: down to 0.007 nm (0.1 cm‑1)
  • 4 different detectors can be installed: TE cooled CCD/EMCCD cameras, APD, PMT & FLIM detector
  • Low frequency Raman detection: less than 10 cm-1
  • Detection of all SNOM signals: laser intensity, fluorescence intensity, spectroscopy

 

Confocal Raman & Fluorescence microscopy

  • Confocal Raman / Fluorescence / Rayleigh imaging runs simultaneously with AFM
  • Diffraction limited spatial resolution: <200 nm in XY, <500 nm in Z
  • Motorized confocal pinhole for optimal signal and confocality
  • Continuously variable ND filter with the range 1-0.001 for precise change of laser power
  • Motorized 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

 

More information


Application notes

 

 

Key publications

  • C. Lee et al., “Tip-Enhanced Raman Scattering Imaging of Two-Dimensional Tungsten Disulfide with Optimized Tip Fabrication Process,” Sci. Rep., vol. 7, no. September 2016, p. 40810, Jan. 2017. https://doi.org/10.1038/srep40810
  • V. V. Kotlyar, S. S. Stafeev, A. G. Nalimov, M. V. Kotlyar, L. O’Faolain, and E. S. Kozlova, “Tight focusing of laser light using a chromium Fresnel zone plate,” Opt. Express, vol. 25, no. 17, p. 19662, 2017. https://doi.org/10.1364/OE.25.019662.
  • N. Slekiene, L. Ramanauskaite, and V. Snitka, “Surface enhanced Raman spectroscopy of self-assembled layers of lipid molecules on nanostructured Au and Ag substrates,” Chem. Phys. Lipids, vol. 203, pp. 12–18, 2017. https://doi.org/10.1016/j.chemphyslip.2017.01.001
  • J. Li et al., “Tuning the photo-response in monolayer MoS2 by plasmonic nanoantenna.,” Sci. Rep., vol. 6, p. 23626, Mar. 2016. https://doi.org/10.1038/srep23626
  • Y. S. Yun et al., “Crumpled graphene paper for high power sodium battery anode,” Carbon N. Y., vol. 99, pp. 658–664, 2016. https://doi.org/10.1016/j.carbon.2015.12.047
  • S. S. Kharintsev, A. I. Fishman, S. K. Saikin, and S. G. Kazarian, “Near-field Raman dichroism of azo-polymers exposed to nanoscale dc electrical and optical poling,” Nanoscale, vol. 8, no. 47, pp. 19867–19875, 2016. https://doi.org/10.1039/C6NR07508H
  • Zhang, M. & Wang, J. Plasmonic lens focused longitudinal field excitation for tip-enhanced Raman spectroscopy. Nanoscale Res. Lett. 10, 189 (2015).
    https://doi.org/10.1186/s11671-015-0897-0
  • Baitimbetova, B. & Vermenichev, B. New Method for Producing Graphene by Magnetron Discharge in an Atmosphere of Aromatic Hydrocarbons. Graphene 04, 3844 (2015). https://doi.org/10.4236/graphene.2015.42004
  • 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) https://doi.org/10.1039/C4CC02754J
  • 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). https://doi.org/10.1021/jp403157v
  • Duong, D. L. et al. Probing graphene grain boundaries with optical microscopy. Nature 490, 2359 (2012). https://doi.org/10.1038/nature11562
  • Stadler, J. et al. Tip-enhanced Raman spectroscopic imaging of patterned thiol monolayers. Beilstein J. Nanotechnol. 2, 50915 (2011). https://doi.org/10.3762/bjnano.2.55
  • Stadler, J., Schmid, T. & Zenobi, R. Nanoscale chemical imaging using top-illumination tip-enhanced Raman spectroscopy. Nano Lett. 10, 451420 (2010).
    https://doi.org/10.1021/nl102423m

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