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NRS-7000 Series Raman

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The performance and functions expected on a micro-Raman spectrometer are all provided with the NRS-7000 series Raman systems, assuring consistent performance for rapid acquisition of high quality data with automated system control and minimal optical adjustments.

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System Description

The innovative instrument design ensures freedom from daily adjustments and alignment. A specially designed honeycomb optical base plate is the foundation for the entire instrument guaranteeing alignment and stability. The laser(s), enclosed microscope, software-switched optics and a unique aberration-corrected polychromator with CCD detector provide an integrated package that is compact enough to fit on a laboratory bench.

With superb stability and effortless software controlled optics, the NRS Series Raman systems offer performance second to none, and with no time-consuming realignment. Simply insert the sample, focus, and collect the spectrum. The integrated, automated x-y-z mapping stage with auto-focusing option allows full PC control. Complete operator safety is maintained by the fully enclosed automated sample chamber door which provides a 120 degree opening to allow full microscope access.

All NRS Series Raman instruments include a color CCD sample viewing system with image capture capability. For additional flexibility, a trinocular microscope attachment can be added for direct binocular viewing. Utilizing the same basic optical system, we’ve designed a family of micro-Raman spectrometers that offer a range of capabilities from simple, single laser, single grating instruments to advanced research grade systems with low wave number measurement, wavelength extension from the deep UV to NIR, and the ability to use or add up to six lasers.

For application expansion, an automated multi-grating turret, 2 internally mounted detectors and a maximum of 8 lasers ranging from the UV through the NIR are capable of integration with the instrument system, all optical components are PC controlled for maximum flexibility with minimum user interaction.

NRS-7100

Maximum Resolution 0.7 cm -1/ 0.3 cm -1 (optional)
Measurement Range 50 to 8000 cm -1

 

NRS-7200

Maximum Resolution 0.7 cm -1/ 0.3 cm -1 (optional)
Measurement Range 5 to 8000 cm -1

System Features

  • Research-grade model assuring high spectral quality
  • Exceptional wavenumber accuracy with a high-precision rotary-encoder direct drive mechanism
  • Low wavenumber measurement (NRS-5200/7200)
  • Auto-alignment of microscope laser introduction optics and Raman scattering light path
  • Wavenumber calibration using an integrated Ne lamp
  • Unique Dual Spatial Filter (DSF) for higher spatial resolution than conventional confocal optics
  • Patented Spatial Resolution Image (SRI) function for simultaneous observation of sample image, laser spot and aperture image
  • Full range of options including macro-Raman measurement unit and fiber optic probes
 

Specifications

 

NRS-7100

NRS-7200

Spectrograph

Spectrograph (Focal length)
Aberration-corrected Czerny-Turner monochrometer (f = 500 mm)
Scanning Mechanism
High-precision direct drive
Low Wavenumber Attachment None Standard
(Excitation WL: 400 ~ 800 nm)
Wavenumber Range
(Raman shift)
50 ~ 8000 cm-1 *1 10 ~ 8000 cm-1 *2
Maximum Resolution
0.7 cm -1 (532 nm excitation, 1800 gr/mm, 1024 pixel CCD)
0.3 cm-1 optional (532 nm excitation, 2400 gr/mm, 2048 pixel CCD)
Grating
1800 gr/mm (Option: 3600, 2400, 1200, 600, 300, 150 gr/mm)
Max. No. of Mountable Grating

4
UV Upgrade
Factory option for UV laser excitation
(including UV optical elements and UV light observation camera) *3
Rejection Filter
532 nm notch filter
(Option: Notch filters and edge filters for other excitation wavelengths)
Rejection Filter Switching
Manual exchange (Option: automated 8-position switching mechanism)
Beam Splitter
Beam splitter with automated switching mechanism
(Option: Dichroic Mirrors, Max. 2 dichroic mirrors can be mounted) *4

Detector

Standard Detector
4-stage Peltier cooled CCD detector (UV-NIR range, 1024 × 255 pixel)
Optional Detectors
4-stage Peltier cooled CCD detector (high-resolution, 2048 × 512 pixel)
Liquid-nitrogen-cooled InGaAs detector (for 1064 nm excitation laser, 1024 pixel)
Dual Detector Switching
Factory option (required when using 2 detectors)

Laser

Laser
532 nm, 50 mW (Option: 244*5, 266*5, 325*5, 355*5,
442, 488, 514.5, 633, 660, 785, 1064 nm)
Maximum Number of Laser
Mounted at a Time
Internal: Max. 2 *6, External: Max. 6
(VIS-NIR laser: Max. 3, UV laser: Max. 3),
Total: Max. 8 lasers, 9 wavelengths
Microscope
Microscopic Observation
Standard:High-resolution built-in CMOS camera
(Option:binocular, trinocular, polarization observation,
differential interference, transmission illumination)
Confocal Optics
Standard
DSF (Dual Spatial Filter)
Standard *Not available for UV upgraded model
SRl (Spatial Resolution Image)
Standard *Not available for UV upgraded model
Objectives
5×, 20×, 100× objectives (Option: Long working
distance type, UV type, NIR type)
Standard Sample Stage
Manual XYZ stage (operable distance X: 75, Y: 50, Z: 30 mm)
Optional Sample Stages
XY autostage with joystick accessory
(travel range X:100, Y:70 mm, 0.04 µm step),
Z autostage (travel range Z:30 mm, 0.1 µm step)
SPRIntS imaging
Factory option (including VertiScan, high-speed data import,
3D imaging measurement, Z autostage, autofocus function)
Autostage Imaging
Factory option (including imaging measurement,
3D imaging measurement, XYZ autostage, autofocus function)
Macro Measurement Unit
Factory option (SPRIntS imaging system and the
Macro measurement unit cannot be provided simultaneously)
Auto-alignment Feature
Laser beam auto-alignment, Raman scattering auto-alignment
SGI (Slit Guide Image)
Standard
Neon Lamp
Standard (for wavenumber correction)
Safety Feature
Integrated sample chamber laser interlock, laser light-path protection (Class 1 compliance)

Software

Standard Function
Point measurement, wide spectral-band measurement, basic spectral data processing functions,
search/functional group analysis (Sadtler KnowItAll), cosmic-ray removal,
auto-fluorescence-correction, wavenumber correction, sensitivity correction,
JASCO canvas (printing function), validation, user help function
Functions included in
SPRIntS imaging and
autostage imaging
Omnifocal image, Real-time display of spectrum, chemical image and current measurement point, multi-image map, auto-focus (supporting both sample image contrast and laser focus algorithms), imaging analysis (including Peak height (ratio), Peak area (ratio), Peak shift, PWHH), PCA mapping, 3-D imaging (including 3-D Raman image display, 3-D image slice display)
Optional Programs
High-throughput screening measurement *7, interval measurement analysis, stress analysis *8, carbon analysis, polysilicon crystallinity evaluation, 2D correlation
Anti-Vibration Table *9
Option (air source for anti-vibration table: nitrogen gas or air source, secondary pressure 0.25 - 0.3 MPa)
Dimensions
(Main Unit Only)
1060(W) × 1220(D) × 670(H) mm 1540(W) × 122 (D) × 670(H) mm
Weight
(Main Unit Only)
About 230 kg About 270 kg
Power Requirement
AC100 V ±10 V, 200 V ±20 V, 200 VA

*1 At 532 nm excitation wavelength with the standard rejection filter.
*2 At 532 nm excitation wavelength with the low wavenumber attachment.
*3 UV laser, edge filter for UV laser, and UV objectives are additionally required.
*4 One dichroic mirror can be mounted when either the UV upgrade or the SPRIntS imaging option is configured.
No dichroic mirror can be utilized when both the UV upgrade and the SPRIntS imaging options are fitted.
*5 The specifications are partially different from the standard model when UV laser is used.
*6 The laser may not be internally mounted due to the specification of the laser.
*7 Autostage imaging option is required.
*8 SPRIntS imaging option or autostage imaging option is required.
*9 Raman system must be placed on anti-vibration or equivalent table.

Details

High performance Raman microscopy systems

1064 nm laser and InGaAs detector options for fluorescence free measurements

detector-options

All models can integrate Near-IR excitation lasers, especially useful for samples which generate fluorescence, even when excited using 785 nm.

Unique DFS function for high spatial resolution

dfs-function

Unique DFS function provides higher spatial resolution than normal confocal optics to irradiate only the target sample.

Applications

Raman Spectral Imaging - Expanding Capabilities to Fulfill Application Requirements

Richard A. Larsena, Yoshiko Kubob, Ken-ichi Akaob, Yusei Ohkubob, Masaki Yumotob, and Toshiyuki Nagoshib

 a Jasco, Inc., 28600 Mary's Court, Easton, MD 21601
b Jasco Corporation, 2967-5 Ishikawa-cho, Hachioji-shi, Tokyo, Japan 192-8537

Introduction

Raman spectroscopic imaging has increasingly gathered momentum as a method of interest for a wide range of users1, including those involved in materials analysis and bio-analysis applications. The relative simplicity and the reliability of modern Raman instrumentation, the higher spatial resolution capabilities and a gradual decline in purchase pricing have continued to attract new and varied users to Raman spectroscopy. Raman spectroscopy can provide the same component identification capability as infrared spectroscopy but without the extensive sample preparation often required for infrared analysis. Raman spectroscopy also offers a 'confocal' capability enabling data collection of subsurface sample spectra for laser transparent samples. The use of Raman for spectral imaging has encountered some restrictions, however, due to the length of time required when obtaining Raman image data for larger sample areas.

Infrared imaging still enjoys an advantage due to lower instrument purchase costs and a longer history as a result of earlier development of the necessary technology. The major obstacles to infrared imaging though, are the restrictions on the spatial resolution for infrared spectroscopy (approximately 2-10 microns) and the requirement to properly prepare the sample to obtain optimal infrared absorption intensities. Ideally, one would use both infrared and Raman imaging techniques for sample analysis, combining the strengths of both analytical methods to exploit the advantages of each method.

The Need for Speed: Methods to Increase Raman Imaging Efficiency 

Various methods have been proposed to increase the imaging speed of Raman spectrometer systems while still maintaining the data quality, confocal capability and spatial resolution that can be obtained for 'standard' sample spectra. While no single technology appears to enjoy a superior advantage for increasing the speed of Raman imaging, there are attractive features for each method2, 3 (and a corresponding buzzword to describe the instrument system).;

Jasco NRS 5000/7000 series

Jasco NRS 5000/7000 Series Raman

The Jasco NRS-5000/7000 series of Raman microscopy instruments employs the SPRIntS high-speed imaging system to increase the data collection speed for an imaging sample. The Verti-Scan sample illumination capability of this system provides optimal, reproducible control of the laser illumination spot on the sample, allowing a data collection step-size of less than 50 nanometers while maintaining the confocal capabilities of the instrument. This system provides the ability to obtain high resolution, high speed imaging of standard surface analysis samples, but also provides a 3-D imaging capability that allows confocal imaging of a laser transparent sample in the XYZ format. When combined with the Interval Measurement control software, dynamic imaging experiments for a sample can also be realized, obtaining data in an intensity vs. time format.

This paper will outline the rapid Raman mapping of samples utilizing a sample excitation technology that improves spatial resolution while maintaining the confocal capability of the Raman technique. This mechanism also enables the 3-D mapping of a sample to provide a three dimensional image of component 'inclusions' within a sample matrix. Data will be presented from several samples demonstrating the increased speed and efficiency of this Raman mapping method. We will also discuss the benefits and advantages of this mapping method and outline the capabilities of this instrument system for selected samples.

Introduction

To increase the speed and efficiency of Raman mapping or 'imaging' applications one could:

  • Use 'macro' illumination of sample, micro Raman signal collection
  • Obtain 'bare minimum' signal for strongest peaks of the sample
  • Reduce spectral/spatial resolution requirements
  • Use a fast response CCD detector with electron-multiplying to enhance Raman signals
  • Reduce need to move sample stage for every measurement point

'VertiScan' Sample Excitation

  • The laser always irradiates the sample vertically to obtain a Raman image without distortion
  • Accurate image information also obtained when using 3-D imaging
  • A wide area sample measurement using only laser scanning (50 µm x 50 µm using a 100X objective lens)

SPRIntS High Speed Imaging

The SPRIntS and VertiScan functions can provide an imaging measurement with a minimum 30 nm spatial resolution, without the use of an auto-stage.

 Raman imaging of small area at sub-micron scale

 

The instrument system can acquire depth imaging data from a sample using the confocal capability of the Raman spectrometer and create a 3-D image from the Raman intensity data. Multilayer sample analysis is also possible using this feature.


A polymer laminate of multiple layers is comprised of 3 primary polymer components - data can be collected using a 'cross-section' of the laminate

 

Polymer Laminate - Cross Section Spectral images Based on Integrated Peak Height

 

Polymer Laminate - Image Overlay of Individual Laminate Spectral images

 

Polymer Laminate - 3-D Image Representations (1639 cm-1)

 

Polymer Laminate - 3-D Composite Image

 

Cyanoacrylate Adhesive Reaction Kinetics

  • A cyanoacrylate adhesive was analyzed during the 'drying' process to examine the changes in spectra.
  • Raman spectra were collected of a single drop of adhesive as it dried, then analyzed to determine what spectral changes occurred.
  • The intensity changes for a peak in the C-H stretching region were analyzed to obtain the rate constants for the reaction process.
  • Spectra were collected for a single-point of the glue surface; then a mapping of the glue surface was attempted to obtain data for the reaction time course.

CyanoAcrylate Adhesive - Raman Spectra at Different Reaction Times

 

Cyanoacrylate Adhesive - Single-point, 3-D Spectra, C-H Stretching Region 

 

CyanoAcrylate Adhesive - Single-Point Kinetics Analysis

 

Rate Equation    Y(t) = 67.7083 * exp(-t / 378.689)
Time constant    378.689 [1/sec] 
Rate constant    0.00264069 [sec] 
Half-life             262.487 [sec]

 CyanoAcrylate Adhesive - 3-D Mapping Data

 

CyanoAcrylate Adhesive - Mapping Data Analysis  Figures

 

CyanoAcrylate Adhesive - Mapping Data Kinetics Analysis 

 

 Rate Equation     Y(t) = 10254.2 * exp(-t / 419.303)
Time constant      419.303 [1/sec]
Rate constant      0.00238491 [sec]
Half-life               290.639 [sec]

Conclusions

  •  The NRS-5000/7000 series instruments offer the SPRIntS and VertiScan features to provide a rapid imaging capability, even when using a manual stage, without:
    • Confocal distortion
    • Loss of spectral or spatial resolution
    • Losses in sensitivity
  • 3-D confocal imaging can be obtained using the VertiScan feature, ensuring XYZ imaging without spectral or optical distortion.
  • Rapid data collection provides '3-D' spectral mapping of sample surface versus time to obtain reaction rate data of a cyanoacrylate adhesive drying process.
  • Further experiments needed to quantify the reaction-rate data for various cyanoacrylate adhesives.