Spectroscopy
Tuned for absorption measurements, this system utilizes a balanced deuterium-tungsten halogen light source (DH-2000-BAL) with a typical output of 194 μW (deuterium bulb) and 615 μW (tungsten bulb) through an SMA 905 connector, covering a range from 230 nm – 2.5 μm. Multimode fiber-optic cables with SMA connectors on both ends and a 600 μm core diameter (QP600-025-SR) connect the light source to the sample holder. For dilute solution measurements a qpod cuvette holder (QNW qpod 2eTM) capable of magnetic stirring and peltier-driven temperature control from -30 °C to 105 °C is used. For thin-film absorption measurements a reflection-transmission sample stage from Ocean Insight (STAGE-RTL-T) is used. The sample holder is coupled through another multimode fiber to the spectrometer (QEPRO-ABS) having an entrance slit of 5 μm (INTSMA-005 Interchangeable Slit). The spectrometer measures in the range from 200-950 nm, at an optical resolution of 1.7 nm, using a back-thinned, TE cooled, 1024 x 58 element CCD array. Note – irradiation perpendicular to the probe beam can be accomplished on the qpod holder using a light source, such as the light emitting diode (LED) from Mightex imaged here (high-power LED collimator source, 530nm, 15W, 22mm aperture, Type-B (LCS-0530-15-22)), coupled through a multimode fiber patchcord, such as the one shown here having a 0.22 numerical aperture (NA), 1000 µm core diameter, and SMA connectors on each end (QP1000-2-SR).
Ocean Optics (now Insight) QE PRO-ABS Fiber Optic Spectrophotometer
Tuned for absorption measurements, this system utilizes a balanced deuterium-tungsten halogen light source (DH-MINI) with a typical output of 19 μW (deuterium bulb) and 14 μW (tungsten bulb) through an SMA 905 connector, covering a range from 200 nm – 2.5 μm. Multimode fiber-optic cables with SMA connectors on both ends and a 600 μm core diameter (QP600-025-SR) connect the light source to the sample holder. For dilute solution measurements a cuvette holder (CUV-UV) is used. For thin-film absorption measurements a reflection-transmission sample stage from Ocean Insight (STAGE-RTL-T) is used. The sample holder is coupled through another multimode fiber to the spectrometer (FLAME-S-UV-VIS) having an entrance slit of 25 μm. The spectrometer measures in the range from 200-850 nm, at an optical resolution of 1.33 nm, using linear silicon CCD array.
Ocean Optics DH-MINI Fiber Optic Spectrometer
Utilizing prealigned deuterium and tungsten halogen lamps with a wavelength range of 190-1100 nm the model 35 features a variable selectable bandwidth at 0.5, 1, 2, 4 nm. An integrating sphere accessory (C6951014) is used to measure cloth, powders, and other diffuse or light-scattered samples.
Perkin Elmer Lambda 35 UV-Visible Spectrometer
Fourier-transform infrared (IR) spectroscopy is performed on a Bruker INVENIO-R, which contains a rapid scan option (S129/IR) and liquid nitrogen cooled MCT detector (D316/B), enabling more than 70 spectra/sec at a resolution of 16 cm-1 and with a spectral range of 12,000 to 600 cm-1. Spectra are analyzed using an OPUS/3D software package (O/3D-N). Additional accessories available for this FTIR include attenuated total reflectance (ATR), without and with bottom-up illumination, a transmission unit, and a hollow waveguide.
Bruker INVENIO-R
Surface FTIR characterization of solids and liquids is accomplished using a platinum-ATR-accessory (A225/Q), which contains a single reflection diamond crystal with a spectral range of 10,000 to 10 cm-1.
Attenuated Total Reflectance (ATR) Accessory
Surface FTIR characterization of solids and liquids under illumination is accomplished using a GladiATR Illuminate accessory (SKU 026-XXXX) from PIKE Technologies that couples to the Bruker INVENIO through Quick-Lock recognition. Illumination occurs from under a diamond ATR element, which sits in a heated plate with a maximum temperature of 210 °C. The angle of incidence of the IR probe beam is 45°, the diamond crystal surface is 3 mm, and the spectral range is 4000 to 30 cm-1. The sampling depth is calculated using an on-line calculator from PIKE Technologies (https://www.piketech.com/pikecalc/).
GladiATR Illuminate Accessory
Bulk FTIR characterization of samples with and without illumination is accomplished using a transmission accessory (A043-N/Q) from Bruker. Samples sit horizontally in housing that can be purged with an inert gas and that contains an opening and holder for sample illumination via a fiber optic cable or liquid light guide.
Transmission Accessory
Hollow Waveguide Accessory. Remote infrared sampling is accomplished using a high-temperature/high-pressure FlexIR diamond probe (part #045-4300) with a FlexIR mid-band MCT detector (part #045-3200) from PIKE Technologies. The accessory is coupled to the Bruker INVENIO FTIR through an external detector assembly (part #660-1000) and FlexIR Mid-IR base-Bruker QL (045-3051). The accessory provides a spectral range of 5,000 to 700 cm-1 and has a maximum operating temperature of 150 °C and maximum pressure of 6.9 MPa (1000 psi).
FTIR Liquid Sampling Accessory
Real-time temperature-controlled measurements on FTIR can be accomplished with PIKE Heated Demounted Liquid Cell and PIKE Universal Temperature Controller. The heated demounted liquid cell allows variable pathlength liquid transmission cell with spacers from 15 micron to 1 mm. The PIKE Universal Temperature Controller offers precise temperature control within ± 0.5% of the set point and fast responsive heating/cooling ramping. The working temperature of cell ranges from ambient to 150 °C.
Transmission FTIR-Heated cell and controller
The POM is customized to enable experiments for anisotropic materials, such as liquid crystals. The POM setup includes a Nikon upright microscope, multiple light sources including a halogen lamp and a mercury lamp, a heating and cooling stage, a rotating stage, and a Mightex Polygon pattern illuminator. Additional LED light sources can be introduced with liquid lightguides and adaptors. UV-VIS measurements can be conducted with a Nikon LT-TV Tube Adaptor.
The Nikon Industrial ECLIPSE LV 100 ND upright microscope model has multiple observation methods (brightfield, darkfield, DIC, and epifluorescence) and five nosepieces with magnifications ranging from 2X to 50X. The microscope has a 10X eyepiece and a DS-RI2 color CMOS camera. A variety of experiments and analyses can be performed with the Nikon NIS-ELEMENTS platform. Four polarizers are installed in the microscope: a polarizer for the universal illuminator, a rotatable polarizer below the eyepiece, a polarizer below the Mightex polygon pattern illuminator, and a polarizer attached to the bottom light source. A Nikon LV-LH50PC-CH Precentered Lamphouse provides a high-intensity 12V-50W halogen light source for illumination. The C-LHGF I HG Precentered Fiber Illuminator provides even higher-intensity light source suitable for fluorescence microscopy. Additional LED light sources can be connected to the POM with ThorLabs 3 mm-core liquid lightguide, compatible with wavelength ranges from 340 nm to 800 nm, collimated with Mightex 3 mm light guide collimator.
Instec TS102 Thermo-electric Heating and Cooling Stage is configured with mK2000 temperature controller. The stage has a sample area of 38mm x 52mm, and a temperature range from -30°C to 120°C. The system includes a stage, temperature controller, Instec host software, and water circulator for base cooling. The PI rotating stage, Model U-651, allows fast and precise control over 360° rotation. With the rotating stage, the microscope is enabled with a four-axis control system (X, Y, Z, and rotation). The motorized stage control can be accomplished by the analog joysticks or the NIS-ELEMENTS motorized stage control module.
In addition to general experiments with the microscope, the POM setup also allows for patterning and UV-Vis measurements. The Mightex Polygon digital micromirror device pattern illuminator, model Polygon 1000-G, serves as a patterning tool of the POM. The model is cable of providing precise spatio-temporal control of light with subcellular resolution, real-time projection, and fast pattern switching speed. It is compatible with lightguide as the light source. The beam splitter provides 90% reflection and 10% transmission with a wavelength range of 350 nm to 700 nm. UV-VIS measurements can be conducted by replacing the camera with Nikon LT-TV Tube Adaptor and an additional UV-VIS light source.
Polarized Optical Microscope (POM)
SuperK Fianium (model FIU-15) provides a supercontinuum white light laser from 400 nm to 2400 nm with variable repetition rate from 0.15 to 78 MHz. It has a total laser power of ~5.5 W across the whole spectral range with a power of ~1.5 W in the visible range and spectral power density ranging from 2.0-4.0 mW/nm. The three different SuperK filters (described below) allow for tunable wavelength and bandwidth with free-space laser delivery or fiber coupled through a SuperK Connect module (FD10).
NKT SuperK Fianium Laser
SuperK Varia provides a tunable wavelength selection from 400-800 nm with variable bandwidth from 10-100 nm and > 50 dB out-of-band suppression. Coupling with the SuperK Fianium, the Varia filter has a transmission efficiency of ~80% with an integrated laser safety interlock and mechanical shutters.
NKT SuperK Varia Accessory
SuperK Laser Line Tunable Filter (LLTF) is equipped with a continuously tunable high-resolution bandpass filter that allows precise wavelength selection from 400-1000 nm with 1-2 nm bandwidth. Coupling with the SuperK Fianium, the LLTF filter has a transmission efficiency of ~65%.
Laser Line Tunable Filter (LLTF) Accessory
SuperK SELECT is equipped with a tunable wavelength filter based on Acousto-Optic Tunable Filters (AOTF). The SELECT filter integrates two AOTF crystals for multiple tunable lines (1-8 per AOTF) for single or multiple wavelength selections in the visible (400-850 nm) and NIR (900-2000 nm) range between the 16 channels. The filter bandwidth is dependent on the wavelength and varies from 1.8 – 9.6 nm per channel. The AOTF deflection efficiency is > 90% with an integrated laser safety interlock and mechanical shutters.
