CARBON NANOTUBE CHARACTERIZATION

Photon etc has designed two narrowband tunable filters for resonance Raman spectroscopy (RRS). These matched tunable passband and notch filters, based on thick volume Bragg gratings, exhibit a bandwidth less than 10cm-1 and cover a wavelength range of several hundred nanometers.

Raman spectroscopy (RS) is a powerful tool to study the vibrational, optical, and electronic properties of materials in a nondestructive manner. Raman signals are typically orders of magnitude lower than the intensity of the excitation laser line. However, it is possible to significantly increase Raman signals by choosing an excitation wavelength that corresponds to an optical transition of the material under investigation.

Resonant Raman Spectroscopy provides a unique tool to characterize the diameter and chirality distribution of a mixed population of carbon nanotubes (CNT). RRS is also a powerful method to monitor in-situ the CNT properties during growth. Thus, it can serve as a diagnosis tool in order to achieve better control of the CNT production.

Experimental Conditions

Using volume Bragg grating (VBG) technology, Photon etc has developed, specifically for RRS, two types of ultra narrow band tunable filters: a laser line filter and a notch filter. The Laser Line Tunable Filter (LLTF) is installed on the Tunable Ti:Saph laser (Figure 2) and blocks the unwanted fluorescence produced by the laser, leaving the excitation laser line untouched. Two steering mirrors (M1 and BS) send the laser line into a standard microscope where the laser beam is focused on the sample of interest. The second filter, a Tunable Top Notch Filter (TTNF), is installed on the microscope. The TTNF blocks the Rayleigh scattering coming from the material, leaving the Raman signal untouched down to 50 cm-1 (20cm-1 has been achieved) with a throughput of up to 80%. The tunable filters are controlled by a computer via USB links, allowing fast wavelength selection.

Results

Stokes and anti-Stokes Raman spectra of single-walled carbon nanotube (SWNT) powder (Figure 1) were measured within less than one hour using a standard spectrometer. Each peak corresponds to a radial breathing mode (RBM), and the center frequency of a given peak is inversely proportional to the nanotube diameter of a given population. Several populations of nanotubes with different diameters can therefore be readily observed and effectively characterized.

 

MAIN TECHNICAL SPECIFICATIONS

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Excitation Wavelength Range   700-1000 nm  or  800-1100 nm
Average Power at the Sample
5 mW
Microscope Objective and Spatial Resolution
50x (< 1 µm)  and  100x (< 0,8 µm)
Detection Range
from 50 cm-1 and up to CCD detection limit (1100nm)
Detection Resolution @ 715 nm
0.6 cm-1
Detection Resolution @ 1100 nm
0.2 cm-1

 

DETAILED TECHNICAL SPECIFICATIONS

LASER LINE TUNABLE FILTER


Bandwidth @ 715 nm 0.4 nm (8 cm-1
  @ 1100 nm 0.4 nm (3 cm-1)
Spectral Range   715 - 1000 nm or 800 -1100 nm
                 Peak Transmission
Up to 60%                                                                                

TUNABLE TOP NOTCH FILTER


Bandwidth @ 715 nm 0.4 nm (8cm-1)

@ 1100 nm 0.4 nm (3 cm-1)                 
Spectral Range
715 - 1000 nm or 800 - 1100 nm                                           
Optical Density
4.0
Signal Out-of-Band Throughput   Up to 80%


SPECTROMETER


Raman Resolution @ 715 nm 0.6 cm-1
  @ 1100 nm 0.2 cm-1
Raman Range   from 50 cm-1 and up to CCD detection limit (1100 nm)        
Monochromator Focal Length   500 nm

DETECTOR


CCD type   "Back-illuminated" CCD                          
Cooling System optional   Liquid nitrogen cooled EMCCD                                   
     Active Pixels    1340 x 100
    Cooled   1340 x 400
Pixel Size   20 x 20 µm

EXCITATION SOURCE Ti : Saphire CW Laser


Excitation Wavelength   700-1000 nm or 800-1100nm                                                   
Spacial Mode                       TEM00
Polarization   > 100:1 Horizontal
Average Power at the Sample
5 mW
Laser linewidth
< 40 GHz

MICROSCOPE SYSTEM


Objective               50x  , 100x
Spatial Resolution
< 2 µm
Manual Translation of sample                     76 x 52 mm and 250° rotatable                                                

   Sample surface imaging with white light and CCD camera

 

 

Photon etc's turn-key Raman Resonant Spectroscopy System

 

F.1. Raman spectra of carbon nanotubes using TI:SAPH Laser & Tunable Top Notch Filter
(Courtesy of Prof. R. Martel, U of Montreal)

Raman spectra of carbon nanotubes using TI:SAPH Laser & Tunable Top Notch Filter (Courtesy of Prof. R. Martel, U of Montreal)

 

F.2. Resonant Raman System Configuration

Raman Resonant Spectroscopy System