Table of Contents

Optical Spectrometers

Located in David McIntyre's lab Weniger 118.

Scanning Monochromator (Grating Spectrometer or GS)

The Scanning Monochromator can make transmission, specular reflection, and diffuse reflection measurements on thin film, single crystal, and powder samples. Here is the grating spectrometer manual, written in 2002, parts of which may be obsolete, but the basic structure is OK.

Sources

There are two broadband sources for the Scanning Monochromator. The W-halogen lamp is used in the visible and NIR (note spectrum depends on filters and grating used):

and the Xe lamp in the UV-and visible.

Detectors

There are two detectors for the Scanning Monochromator. The Silicon detector is 13 mm^2 and works in the UV-Vis range 350-1100 nm (down to ~1.1 eV).

The InGaAs detector is used for NIR measurements and is 3.1 mm^2 and thus it's is much more difficult, compared to the Si detector, to capture all the light. This detector can work in the range of 800-1800 nm.

Gratings

There are five sets of gratings for the monochromators - 0.25 µm, 0.5 µm, 1.0 µm, 2.0 µm, and 4.0 µm. The number indicates the wavelength at which the gratings perform the best. Typically, for UV-Vis measurements, you want to use the 0.5µm gratings, because the lamp is fairly weak at this wavelength, yet very intense at 1.0 µm. Thus, you're unlikely to get a usable signal at 500 nm with the 1.0 µm gratings, but you will still get a strong a signal at 1 µm when using the 0.5 µm gratings.

:opticalspectrometers:w_spectrum.png

A word of caution about the gratings: Reported problem, “I found that the monochrometer seems to be having trouble. I tried to reset it to 518 nm and found that thanks to what seems to be a belt problem, it is stuck at 926 nm”, David Mc responded on (9/12/21), “I (kind of) fixed the spectrometer. I know what the problem was, but I do not know what caused it. BUT, YOU should figure out what caused the problem, as it has damaged the instrument already and if it happens again it may further damage the instrument. The indicators on the 2 spectrometers read the wavelength in the range 0-999. But what they are really doing is indicating the angle of the grating, which is turned with the sets of gears and pulleys. The indicator that was at 926 nm had arrived at that point not by going from 518 nm up to 926 nm, but rather by going from 518 nm, down to 0 and thorough 0 (to the negative side) and stopping at 926. Thus the grating was at an angle where no light goes through the spectrometer. The spectrometer is not designed to go past 0, so the gears and belts locked up. By removing some belts and applying gentle but firm force, I was able to independently get the 2 spectrometers back into the “positive” region. With the coupling belt removed, I set one spectrometer to 518 and then adjusted the other by monitoring the spectrometer output. The output was maximized with the second spectrometer (closer to the lamp) set to 545 nm. This indicates that the gears and belts slipped quite a bit. Unfortunately, now we do not know which dial, if either, is correct. The system needs to be recalibrated. Moreover, the gears appear to slip during a manual scan and this may cause problems for a computer controlled scan.”

Sampling Accessories

The Scanning Monochromator has an Oriel 70491 integrating sphere to make diffuse reflection measurements.

Ocean Optics Spectrometer (OO; also "Fiber Optic Spectrometer")

The Ocean Optics Spectrometer can make transmission, specular reflection, and diffuse reflection measurements on thin film, single crystal, and powder samples. Diffuse reflection measurements can only be made on strongly diffusely reflecting materials.

Detectors

The Ocean Optics spectrometer has two detectors: Ocean Optics HR 4000 and Ocean Optics NIR256-2.5.

The Ocean Optics HR 4000 spectrometer is used to take ultraviolet-visible spectra. The HR 4000 has a 3648-element CCD-array detector with an optical resolution of 0.27 nm. The ultraviolet-visible measurements span a wavelength range from 200 nm to 1150 nm.

Ocean Optics NIR256-2.5 spectrometer is used to take the visible-near infer red spectra. The NIR256-2.5 has an InGaAs detector array with an optical resolution of 6.85 nm. The visible-near infer red measurements span a wavelength range of 850 nm to 2600 nm.

Light Sources

An Ocean Optics Mikropack DH-2000-BAL Deuterium Tungsten Halogen Light Source is used for the ultraviolet-visible measurements and an Ocean Optics Mikropack HL-2000 Tungsten Halogen Light Source is used for the visible-near infer red measurements. The spot size and incidence angle for both instruments are approximately 1.5 mm and 0 º.

Software & Data Analysis

Filmetrix Spectrometer (Not used much in 2020)

Documentation

There is a manual for the OO spectrometer located permanently in Wngr 118. Never remove it from that room. The manual is based on some of the following documentation:

Optical data

DateAuthorTitleNotes
--Optical constants from Sopra labsOptical constants of many different materials. Widely quoted site.
Journal of Physical and Chemical Reference Data 9, 561 (1980)H. H. LiRefractive Index of Silicon and Germanium and Its Wavelength and Temperature DerivativesExhaustive compilation of refractive index of Si, Ge, temp dep etc. Available at NIST reprint site.
Journal of Physical and Chemical Reference Data 31, 931 (2002)R.D. Shannon et al.Refractive Index and Dispersion of Fluorides and OxidesExhaustive compilation of refractive index of fits to refractive indices of common fluoride and oxides using Sellmeier formalism.
Journal of Physical and Chemical Reference Data 13, 103 (1984)H. H. LiRefractive Index of ZnS, ZnSe, and ZnTe and its wavelength and temperature derivativesExhaustive compilation of refractive index of ZnCh temp dep etc. Available at NIST reprint site.
Melles Griot Technical Manual, Materials Properties Melles GriotMaterials PropertiesGood compilation of refractive index, transmission of different kinds of glasses - BK7, suprasil, CaF, crystal quartz, etc. Also silicon and germanium.
Melles Griot Technical Manual, Optical Coatings Melles GriotOptical CoatingsGood discussion of coatings and materials, reflection, angles of incidence, phase changes, fringes etc.