Institute of Molecular Physics of the Polish Academy of Sciences

FT-IR spectrometer Bruker Equinox 55 combined with FT-IR microscope Bruker Hyperion 2000 and accessories

The measuring system allows for recording spectra in polarized light from 30 to 18 000 cm^-1. The radiation sources in the spectrometer are a tungsten halogen lamp (1800-18000 cm^-1) and a silicon carbide ceramic rod (30-7000 cm^-1). The system is equipped with the following detectors: Si (operating in the range 10000-20000 cm^-1), InSb (3000-12500 cm^-1), MCT (400-7500 cm^-1), DLaTGS (180-12000 cm^-1) and DTGS (10-700 cm^-1). The instrument is equipped with the following beam splitters: quartz (3300-18000 cm^-1), KBr (370-7500 cm^-1), and Mylar (30-700 cm^-1). The spectrometer operates with a maximum spectral resolution of 0.5 cm^-1. FT-IR microscope Hyperion 2000 from Bruker attached to the spectrometer allows measuring reflection and transmission spectra in polarized light of micro samples with dimensions of fractions of a millimeter in the spectral range from 600 to 18000 cm^-1 as a function of temperature from 10 to 870 K. The microscope is equipped with an objective for recording reflection-absorption spectra from thin films applied to metallic substrates (600-6500 cm^-1). The microscope table (controlled by stepper motors) enables to study of the spatial distribution of substances in the material (spatial resolution of 1 mm). The diamond anvils allow for recording mid-infrared transmission spectra as a function of pressure (up to 20 GPa) at room temperature.

The spectrometer equipment includes the following components:

• Parker dry air purge system (the system is connected to the spectrometer and microscope)
• Bruker variable-angle reflectance accessory (enables recording of reflectance spectra in polarized light in the range from 400 to 7000 cm^-1 for angles of incidence and reflection from 10° to 80°)
• Gateway™ Attenuated Total Internal Reflection (ATR) accessory (six reflections horizontal ATR sampling system) to record ATR spectra as a function of temperature from room temperature to 200 °C in the spectral range from 600 to 7000 cm^-1)
• Beckman reflectance spectra accessory (enables the registration of reflectance spectra in a spectrometer chamber in the spectral range from 400 to 7000 cm^-1)
• Perkin-Elmer Diffuse Reflection (DRIFT) accessory (allows registration of reflectance-absorption spectra in the range of 400 to 7000 cm^-1)
• mirrors, cuvettes, and polarizers

Raman spectrometer LabRAM HR 800 Jobin Yvon and accessories

The spectrometer contains two diffraction gratings (600 and 1800 lines/mm), input and filter optics, and a multi-channel detector (CCD 1024´256) operating at liquid nitrogen temperature. It is equipped with a He–Ne laser (λ_ext = 632.8 nm), a tunable Stabilite 2017 argon laser with a power supply (λ_ext=454.5, 457.9, 465.8, 472.7, 476.5, 488.0, 496.5, 501.7, 514.5 nm) and a NIR laser with power supply (λ_ext=785 nm). The spectrometer is equipped with "Notch" type VLFIE filter sets: for 457 mm line (allowing approach to Rayleigh line at 150 cm^-1), for 488 mm line (allowing approach to Rayleigh line at 50 cm^-1), for 514 mm line (allowing approach to Rayleigh line at 50 cm^-1), for 633 mm line (allowing approach to Rayleigh line at 50 cm^-1), and for 785 mm line (allowing approach to Rayleigh line at 100 cm^-1). The spectrometer is equipped with an L-BXFM confocal microscope containing the following objectives: plan-achromatic objective ´10, NA=0.25, WD=10.6 mm, plan-achromatic objective ´50, NA=0.75, WD=0.37 mm, plan-achromatic lens ´100, NA=0.90, WD=0.21 mm, long-focus lens ´10, NA=0.25, WD=21 mm, long-focus lens ´20, NA=0.25, WD=12 mm, and macro-sample lens WD=40 mm. The LabRAM HR 800 Jobin Yvon Raman spectrometer is used to study Raman scattering spectra as a function of temperature and pressure.

Hitachi U-2900 NIR/Vis/UV Spectrometer

It enables the registration of absorption spectra in polarized light in the spectral range from 190 to 1100 nm of solid and liquid phase samples. Transmission and reflection spectra can be recorded at scan rates of: 10, 100, 200, 400, 800, 1200, 2400, and 3600 nm/min. The instrument has two radiation sources: a tungsten lamp (measurements in the visible light range) and a deuterium lamp (measurements in the ultraviolet light range). A silicon photodiode is used as a radiation detector. The spectrum measurement accuracy changes with the absorbance range change and is as follows: in the range from 0 to 0.5 ±0.002, from 0.5 to 1.0 ±0.004, and 1.0 to 2.0 ±0.008. The measurement error of transmittance value is equal to ±0.3%.

Hitachi F-7000 Spectrofluorimeter

Enables measurements of fluorescence, luminescence, and phosphorescence of solutions and solid samples as a function of temperature (Optistat CF cryostat by Oxford Inst). It is possible to perform measurements of fluorescence lifetime up to 1 ms. It is equipped with two monochromators allowing continuous selection of excitation and fluorescence emission wavelengths. The spectrofluorimeter is fitted with a set of edge filters and polarizers, allowing emission and excitation spectra to be measured in the range from 900 to 200 nm.

Conductivity measuring station

Specific electrical conductivity measurements are made using the four-electrode method. A Keithley 220 programmable current source allows current variations in the range of 1 nA - 100 mA, and a Keithley 182 digital voltmeter will enable measurements in the range of 3 mV - 30 V with a resolution of 1 nV - 10 μV. Temperature measurements are made in the range of 1.8 - 370 K. A 40 μm silver wire is used to attach the sample to the copper paths using a silver paste, which is also used for the electrodes. We can use gold or carbon paste (and other wire than silver) depending on our needs. The system allows the measurement of samples smaller than 1 mm (maximum about 1 cm).

Thermo-optical Analysis (TOA) Workstation

The thermo-optical analysis is a visual aid to observe physical effects during thermal analysis measurements. It allows for the determination of the temperature of the phase transition in the condensed phase under the occurrence of apparent texture changes in the tested material. This method is complementary to DSC, TG, or infrared measurements as a function of temperature. The measurement system consists of the following elements: stereo microscope Delta Optical IPOS 810 WS (objective plan achromat ´2 - maximum magnification ´400 together with coaxial illuminator, dark field module, photographic adapter with microscope camera), cryostat Linkam TC92 with accessories, multimeter - HP 34401a (ranges: 10 mA, 100 mA, 1A, 3A; maximum resolution: 10 nA), diode - OSRAM BPW 21 (dark current: 2 nA; wavelength 350-820 nm) and computer.

Temperature testing systems

• System for testing as a function of temperature from 1.8 to 370 K
  (Optistat CF optical cryostat by Oxford Inst. (sets of windows - KBr, KRS-5, quartz), Oxford Inst. ITC 503 thermoregulator, transfer line GFS 650, flowmeter PKR 251/26001, helium dewar 50 l, pump system: turbomolecular pump TSH 071E, membrane pump MVP 015, circulating pump, pressure gauge PKR 251 / 26001)
  Enables recording of fluorescence spectra as a function of temperature and is used in conductivity measurements.

• System for testing as a function of temperature from 4.2 to 300 K
  (Optical cryostat CF 2102 by Oxford Inst., thermoregulator Oxford Inst. ITC 503, transfer line GFS 650, flowmeter PKR 251/26001, helium dewar 50 l, pump system: turbomolecular pump TSH 071E, membrane pump MVP 015, circulation pump, pressure gauge PKR 251 / 26001).
  Enables absorption and reflection spectra recording in polarized light (600 -18000 cm^-1) and Raman scattering spectra.

• System for testing as a function of temperature from 77 K to 870 K
  (cryostat from Linkam Corp. TC92, Linkam Inst. thermoregulator, nitrogen dewar with desiccants for blowing the cryostat, heating line for cryostat housing)
  It enables the recording of absorption and reflection spectra in polarized light (600 -18000 cm^-1) and Raman scattering spectra and is used in the thermo-optical analysis (TOA).
• System for testing optical properties simultaneously as a function of temperature (4.2-300 K) and pressure (from atmospheric pressure to 20 GPa)
  (Optical cryostat CF 2102 by Oxford Inst. with equipment, diamond anvil Diacell D-07 placed on a cold finger of the cryostat - max. pressure 100 GPa)
  It allows the recording of Raman scattering spectra as a function of temperature and pressure.

Equipment for sample preparation

• chemistry lab
• Laurell W5-650MZ-23NPPB Rotary thin-film coater
• mechanosynthesis ball mill
• laboratory dryer
• KBr Pellet Making Die Set
• hydraulic press,
• laboratory balance
• cuvettes for gases (l=10 cm) and liquids (l = 0.1 mm - 50 mm) made of glass, quartz, NaCl, KRS-5, BaF2, KBr, CsJ
• diamond anvils,
• ED wire cutting machine for making holes in gaskets,
• device for assembling gaskets,
• ultrasonic cleaner,
• stereo microscope (max. 20),
• soldering station
• stereo microscope Delta Optical IPOS 810 WS (objective plan achromat 2 - maximum magnification 400 with coaxial illuminator, dark field module, and camera adapter

Computing stations

The software we use (Gaussian and Crystal programs) enables us to perform lattice vibration (phonon), vibrational, and electron transition calculations.