This collaborative product brings together for the first time, in one commercial system, the chemical sensitivity of Raman spectroscopy and the ultra-high spatial resolution of scanning probe and near-field optical microscopy.

The spatial resolution of Raman systems employing normal optical microscopes is limited to approximately the wavelength of the light (about 0.5 µm), because both the illuminating laser light and the Raman scattered light are collected in the optical far-field (i.e. many wavelengths of light away from the scattering material).

This resolution is sufficient for many users, but some need the higher resolutions attainable with scanning probe microscopies (SPM), such as atomic force microscopy (AFM) and near-field scanning optical microscopy (NSOM). This need is fulfilled with the new combined Nanonics NSOM/AFM-100 Confocal™/Renishaw RM Series Raman microscope.

The Renishaw/Nanonics combined instrument can operate in two modes:

AFM/NSOM with far-field Raman - Offers users high spatial resolution scanning probe data, combined with far-field resolution Raman data (typically 0.5 µm spatial resolution). Now Raman data can be recorded and correlated with high spatial resolution topographic, electrical, thermal and near-field optical data.

AFM/NSOM with near-field Raman - Offers users high spatial resolution data for both scanning probe and Raman.

The hardware and the software of the Nanonics NSOM/AFM-100 Confocal™ system are integrated with the Renishaw RM Series microscope. Previously, investigating a sample with both scanning probe microscopy and Raman microscopy required moving the sample from instrument to instrument. The exact region being analysed by the Raman microscope could not generally be found again for imaging with the chosen scanning probe microscopic technique. The Nanonics/Renishaw microscope system makes simultaneous Raman spectroscopy and scanning probe microscopy possible.

The Nanonics system uses a patented optical fibre probe design. The cantilevered optical fibre is held between the objective lens and the sample without obstructing any aspect of the far-field conventional microscope. The tip of the fibre is exposed, allowing direct viewing of the scanned region in the microscope eyepieces or on the video viewer. This is not possible in a standard AFM that uses a silicon micromachined tip, which obscures the scanned region in the standard upright microscope. It is also not possible with straight near-field optical fibre probes.

When mounted on a Renishaw Raman microscope, the novel design of the Nanonics system means that the user can record a wide variety of scanning probe imaging modes in parallel with Raman spectroscopy. For example, while the silicon Raman peak of a microcircuit is being monitored to detect stress in the silicon, the Raman spectroscopist can simultaneously measure the micro topography with AFM, and the micro reflectivity with NSOM.   

Nanonics Press Release: August 2013

Nanonics is  proud to announce that our triple beam integrated AFM/SEM/FIB system, the Nanonics 3TB4000, was judged one of the ten best microscopy innovations in 2013 and is the recipient of the prestigious

2013 Microscopy Today Innovation Award. The 3TB4000 provides the ultimate 3D nanoscale characterization capability through a revolutionary innovation of open architecture that provides open access to the SEM/FIB beams without any obstruction or interference to the injectors, detectors, or beam lines.

With the 3TB4000, the SEM,FIB, and AFM can now be used to provide complimentary information in order to provide a complete characterization of material by taking advantage of the functional and high resolution 3D capabilities of AFM, the large field of view and rapid scanning of the SEM, and the fabrication / material removal capability of the FIB. Applications demonstrating this powerful new capability have been shown in diverse areas including side wall imaging in semiconductors, locating and measuring optical properties of individual metal oxide nanowires or mechanical properties of surface features, and assessing AFM probes in situ while imaging.

Nanonics founders Aaron and Chaya Lewis accept the  2013 Microscopy Today Innovation Award at the 2013  Microscopy and Microanalysis meeting in Indianapolis	The award winning Nanonics3TB4000, an integrated AFM/SEM/FIB system

Origin of enhanced signal from TERS measurements on functionalized nanoparticles.

Recent work by Nanonics Users Z.D. Schultz and H. Wang (Analyst, 2013, 138, 3150-3157) on understanding the origin of TERS signals from functionalized nanoparticles was featured on the front cover of Analyst and identified as a “hot article” by its editors.  In this work , the authors used a Nanonics MV4000 customized with a homebuilt Raman microscope to measure the TERS signal of gold nanoparticles functionalized with proteins and compare that with SERS measurements of clustered gold nanoparticles to understand the source of enhancement of the TERS signal and its relation to location of the enhanced molecule with respect to the gap.  The ability to understand the source of the enhancement of the TERS signal provides flexibility in preparing complicated biological samples such as receptors for TERS imaging beyond the traditional method of affixing the target to a metallic surface, which cannot be applied to many materials (e.g. biological receptors).

Background:

Surface enhanced Raman spectroscopy (SERS) is a surface sensitive technique where Raman scattering is enhanced by molecules adsorbed on a rough or nanostructured metal surface and is used for ultrasensitive detection resulting in single molecule sensitivity in a variety of fields including materials and biology.  TERS, or tip enhance Raman spectroscopy, also results in enhancement of the Raman signal and employs scanning a very sharp metallic or metalized tip to create a “nano-antenna” resulting in high resolution and enhanced Raman signal, and has been used to investigate carbon nanotubes, semiconductors, and biologically relevant molecules.  In TERS, substantial enhancement has been observed from gap-modes that arise from image dipoles as the tip approaches a metal surface. However, a limitation of gap-mode TERS is the requirement of a metallic or conducting substrate.  To address this limitation, nanoparticles on dielectric substrates interacting with the TERS tip have been shown to generate enhancement comparable to gap-modes and thus broadens the applicability of TERS with a more flexible sample preparation.

Goal and findings

The goal of this study is elucidate the location of the enhanced molecule within the gap that leads to the TERS signal, and to understand whether nanoparticles bound to proteins can provide additional TERS enhancement without the analyte of interest residing directly in the gap junction.  The authors focus on the biotin-streptavidin system, a popular ligand-receptor binding system.

This work suggests that TERS can distinguish between a protein located within the gap junction and a protein bound to the nanoparticle outside the gap (see schematics enclosed in blue and green rectangles in figure below, respectively); these results are compared with the SERS signal from aggregated gold nanoparticles (schematic enclosed in red rectangle below).  Furthermore, they saw an effect of nanoparticle probe size on absolute signal indicating either larger enhancements with larger particles or increased number of sample molecules.  The ability to enhance Raman scattering from molecules outside the gap junction by using functionalized nanoparticles provides a way to increase sensitivity in TERS experiments from complicated biological samples by providing another platform for preparing complex biological molecules that can be probed by the ultrasensitive TERS method.

 Standard AFM technology is currently deficient when it comes to  nanoindentation. During indentation, a sample that is in contact with a tip  moves up against the tip for the indentation operation. The sample indents  a given distance as  a result of the force, butthe critical force is unknown,  since standard cantilever structures bend. Thus, the distance indented  includes both the sample indentation depth and the cantilever bending.  Nanonics has solved this problem with its Multiprobe AFM Systems. MultiProbes allow straight diamond or other indenters and frees AFM nanoindentation from cantilever bending constraints.

Straight indenters of any type can be bonded to tuning forks, allowing them to be brought in contact with the working surface, while a second AFM probe monitors the indenter’s Z-axis alteration at and only at the straight indenter as the sample is lifted in the Z direction against the indenter. As a result, only the Z-axis alteration of the straight indenter is monitored, independent of any possible tuning fork bending that may occur in spite of the >5000 N/m Force Constant. Up to four probes can be added for on-line monitoring of electrical and thermal parameters during indentation.

For the first time, a state of the art AFM measures true indentation depth versus load, allowing the user to learn:

• Young’s modulus
• Indentation Modulus
• Indentation Creep
• Indentation Creep
• Indentation Hardness
• Progressive Load
• Constant Load
• Multipass Scratch & Wear Tests with Variable Force
• Including Force-displacement curves and scratch and
  wear tests with variable force, rate, length  and direction
• Rate, Length and Direction
• Environmental & temperature control
• High force constant (100 to300 N/m) quartz conical
  indenters with customization

• Nanoheater nanoindenters
• NanoIndenters with on-line Raman spectroscopy of
   vibrational alterations

Different Indentation Protocols

On-line Load and Unload Curves Versus Distance

The Choice Is Yours From Various Indentation To Scratch Protocols

Variety Of Probes For Hard & Soft Indentation:  Shown Indentation of Gold A Soft Material With Nanonics Unique Connical Glass Probes

Ultrahigh Control Of Load Parameters and Indentation Depth

On-line Raman Chemical Analysis

Tip-enhanced Raman scattering of  70 nm strained silicon layer single gold nanoparticle probe

Line profile Raman intensity of sSi silicon mesa: Blue: Far-field Green: Near-field Red: Difference

Reversible Defect in Graphene Investigated by Tip-Enhanced Raman Spectroscopy

AFM/Raman Imaging of Graphene

Single and Double  Layers