Agilent uFTIR Microscope and Bench
| Agilent uFTIR Microscope and Bench | |
|---|---|
 Agilent uFTIR Microscope and Bench | |
| Equipment Details | |
| Technology | Metrology |
| Materials Restriction | General |
| Sample Size | maximum height 2 cm |
| Equipment Manual | |
| Overview | System Overview |
| Operating Procedure | SOP |
| Supported Processes | Supported Processes |
| Maintenance | Maintenance |
The Agilent uFTIR Microscope and Bench combines both the microscope (Cary 620) and the analytical bench (Cary 670) capabilities for the Fourier Transform Infrared Spectroscopy (FTIR) analysis of samples. FTIR can be used to measure and identify the vibrational modes of any substance or molecules whose lattice vibrations have the symmetry necessary to be detected in the IR to mid-IR wavelength range. FTIR is also commonly used to measure absorption in the IR region, and is commonly used to analyze organic films (such as Parylene C, PDMS, photoresist) liquids, powders and patterned materials such as gratings or nanostructures.
In addition to the conventional capabilities of the analytical bench, this microscope offers both transmission and reflection measurements on samples as small as 5 microns, and chemical mapping. The microscope is equipped with an MCT detector, while the bench has both a DTGS and an MCT detector and exchangeable beam splitters (KBr and Quartz) allowing an spectral range from 9000 to 700 cm-1 . The collection resolution can be changed from 2 to 16 cm-1. The scan speed is 150kHz. All these capabilities allow the instrument to acquire high resolution spectra of very small samples and thin films in a short time. The microscope accessories include an ATR and GAO objective as well as an IR polarizer.
Contents
Announcements
Acquisition program files are in C:\Program files\Varian\Resolution\ .
There has been an update to the beam splitter change instructions in the SOP
Capabilities
- Transmission and Reflection in microscope
- Transmission and Reflection in the bench
- Near IR and Mid-IR range
- Fast acquisition - high throughput
- Small (5 μm) samples and very thin films
- Chemical mapping
- Bench Specular reflection attachment - incidence angle 10o
System overview
Hardware details
- This instrument is both a traditional FTIR bench and an FTIR microscope
- The microscope is an Olympus frame modified to allow room for the necessary controls
- Cary 620 microscope
- Cary 670 Analytical Bench
- 15X Cassegrain with removable ATR attachment
- Separate GAO (15X)
- 10X optical objective
- Extra sample compartment in the bench for emission studies
- KBr and Quartz beam splitters, exchangeable
- MCT detector in microscope
- MCT and DTGS detector in the bench
- IR polarizer (must ask staff)
- The stage travel is 5x5 cm in the x-y plane and 2 cm in the z axis
Substrate requirements
This is an analytical instrument, as such should be accessible to all class of materials: solid, liquids and gases. The material characteristics will determine the technique to be utilized.
- Sample for microscope can be irregular and as small as 5x5 μm. Max sample height = 2 cm.
- Sample to be analyzed should be active in the IR or near IR regions
- Sample to be analyzed should not be buried underneath another layer
- In both cases, transmission and reflectance must have access to sample background
- Ideal substrate for reflectance sample is a glass slide with a non-transparent film such as gold
- Ideal sample for a transmission sample is a sample on a glass slide
- Bench samples must be prepared as pellets if sample is a powder, supported if sample is a film or in a liquid-cell if it is a liquid
- Gases can also be analyzed in the bench sample compartment as long as a suitable cell is used
Material restrictions
The Agilent uFTIR Microscope and Bench is designated as a General class tool. Below is a list of approved materials for the tool. Approved means the material is allowed in the tool under normal circumstances. If a material is not listed, please create a helpdesk ticket or email info@lnf.umich.edu for any material requests or questions.
Standard operating procedure
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Checkout procedure
- Read through this page and the Standard Operating Procedure above.
- Complete the SOP quiz until you get all answers correct. You may retake the quiz as many times as necessary.
- Contact the tool engineer via Helpdesk to discuss sample preparation and other information needed (energy ranges, detectors, etc.)
- Create a Helpdesk Ticket requesting training.
- A tool engineer will schedule a time for initial training.
- Practice with your mentor or another authorized user until you are comfortable with tool operation.
- Schedule a checkout session with a tool engineer via the Helpdesk ticket system. If this checkout is successful, the engineer will authorize you on the tool.
Maintenance
Users are not allowed to carry out maintenance on the micro FTIR. For issues with the tool, please contact the tool engineer or create a helpdesk ticket. Users are prohibited from trying to troubleshoot without authorization from the tool engineers.
- Tool must be maintained under dry nitrogen permanently to protect the beam splitter crystals.
- Keep the work area clean
- Cool down the detector with liquid N2 at least 10 min before using it
- Turn sample stage N2 off.
Further Reading
FTIR is one of the most popular analytical chemistry techniques, there are countless books, articles, guides, handbooks available. The articles in this list assembled by Mettler TOLEDO, an FTIR equipment manufacturer, is a good beginning:
[1]
For complex films, you may get unexpected results. This article discusses using Kramers-Kronig Relations for multilayered films to correct for Fabry-Perot-interferences in reflection mode.
