Facilities & Laboratories

Microscopy, Spectroscopy, & Diffraction

The RMTD group has a suite of microscopy capabilities ranging from optical to scanning electron microscopes. Through the years, the group has garnered several different awards for its work in this area.

The RMTD group has many resources for materials science characterization, development, and synthesis; for applications ranging from bench-scale to field work. Some of these methods are tested through microscopy, spectroscopy, and diffraction.

Microscopy

The RMTD group has a suite of microscopy capabilities ranging from optical to scanning electron microscopes. There are three optical stereo zoom microscopes with digital imaging capabilities, a Lietz OrthoPlan research grade optical microscope with transmitted, reflected, and cross-polarized capabilities, and an Olympus inverted light microscope. Our group also has a JEOL 5900 tungsten filament SEM equipped with the following accessories: EDAX silicon drift detector energy dispersive spectrometer, IXRF micro x-ray fluorescence source, 4Pi digital image acquisition system, Robinson backscattered electron detector, XEI plasma chamber cleaner, and an infrared chamber camera. In addition to the microscopes, our group also has a sputter coater, a high-vacuum carbon evaporator, and an assortment of other sample preparation equipment.

L to R: Leica Zoom, Leitz Orthoplan, Olympus PMG3 (inverted light), Olympus Zoom.

Spectroscopy

Several members of our staff are interested in various aspects of spectroscopy for studying glasses, ceramics, and other materials. This includes vibrational spectroscopy, mass spectrometry, ion spectroscopy We steward certain of the following capabilities ourselves and partner with other groups in PNNL and EMSL for other capabilities (indicated by * in the following list):

Absorption spectroscopy (UV-VIS-NIR, mid and long-wave infrared, Far-infrared*, THz)
Reflection spectroscopy (UV-VIS-NIR*, mid and long-wave infrared*, THz, prism coupling*, ellipsometry*)
Dielectric spectroscopy* (DC, low frequency (impedance), RF, microwave, millimeter wave)
Millimeter wave radiometry/ interferometry
Raman spectroscopy* (UV, visible, and infrared excitation)
Ion spectroscopy* (Rutherford backscattering spectroscopy (RBS), secondary ion mass spectroscopy (SIMS)
Magnetic spectroscopy* (AC and DC susceptibility, electron paramagnetic resonance, nuclear magnetic resonance)

Equipment

Absorption spectroscopy

Varian Cary 500 dispersive spectrophotometer (Varian Inc., Palo Alto, CA), 100 to 1000 THz (λ=3.0 micro, µm to 0.3 µm )

Thermo Nicolet 6700 Fourier transform infrared spectrometer (Thermo Fisher Scientific, Waltham, MA), 2.5 to 25 µm

THz quasi-optical spectrometer (Microtech Instruments, Eugene, Oregon, USA) in the frequency range of 172 to 506 GHz (λ=0.6-1.7 mm)

Raman*

SPEX 1877 spectrometer, liquid nitrogen cooled CCD detector (Princeton instruments), Ar⁺ ion laser (Omnichrome), Kr⁺ ion laser (Omnichrome); 514.5 nm (green, Ar ion), 647.1 nm (red, Kr ion)

Horiba JY (Edison, NJ) LabRAM HR (high resolution) Raman (confocal) microscope system. Deep-UV 244-nm line of a Lexel (Fremont, CA) Model 85-SHG frequency-doubled Ar⁺ ion laser equipped with a non-linear BBO (beta barium borate) crystal.

Refractive index*

Modified prism coupler setup (Metricon 2010, Pennington, NJ). Laser wavelengths included 0.6328 µm (HeNe), 1.5473 µm (Er-doped telecom), 3.391 µm (HeNe), 5.348 µm (quantum cascade laser), 9.536 µm (CO₂), and 10.591 µm (CO₂). A germanium detector is used for 0.6328 and 1.5473 µm, and a Hg-Cd-Zn-Te detector was used for 3.391, 5.348, 9.294, and 10.591 µm.

MMW radiometer/viscometer*

Deep Level Transient Spectroscopy

X-Ray Diffraction

Bruker D8 advanced diffractometer is equipped with a Cu target and is configured at a goniometer radius of 250 mm. The system is equipped to perform a variety of diffraction experiments to include: Brag-Brentano, parallel beam, grazing incidence, capillary, and SAXS. The system can also be configured with an Anton-Parr HTK16 hot stage to perform experiments from room temperature up to 1600°C under high vacuum or in the following atmospheres (air, oxygen, and inert). Sample holders/heaters available for the hot stage, depending upon atmosphere are: Pt (oxidizing, inert), Ta (vacuum), or graphite (inert, vacuum).

Software: TOPAS, version 4.2, RIQAS version 4.0, Jade version 6.0, and EVA version 14.

Measurements: Phase ID, qualitative or quantitative phase analysis, crystallite size, particle size (1 – 100 nm)

Hot stage measurements: thermal expansion, meta-stable phase transitions, reaction kinetics can all be measured in the hot stage. Figures 1 and 2 show the in growth of a cubic phase at high temperature from a starting material that has a hexagonal structure.

Figure 1. Contour plot of epsilon metal phase heated from RT - 1500ºC under high vacuum

Figure 2. 3-D plot of epsilon metal phase heated from RT - 1500ºC under high vacuum

Point of Contact

Jarrod Crum