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Dr. Kris Lipinska


Associate Research Professor

Department of Mechanical Engineering

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THE LABS
FAME-Tech labs include:
1. the Materials Synthesis cluster
2. the Optical Characterization cluster
3. the Materials at Extreme Environments cluster

The facilities in these Labs offer unique research opportunities for faculty and students interested in materials sciences.

Research at FAME-Tech Labs revolves around synthesis and characterization of glasses, ceramics and glass ceramic materials for optical and other applications, examining the role of structure/property relationships on resulting properties and performance.


OPTICAL SPECTROSCOPY SETUP

We use the Optical Spectroscopy Setup Jobin-Yvon Horiba T-64000 Raman Spectrometer is ideal to study liquids, gases and solids in 3 "regimes":
- Raman Scattering Spectroscopy
- Laser Spectroscopy
- Surface and Bulk Mapping/Imaging in XYZ


Equipment:
1. Jobin-Yvon Horiba T-64000 Raman Spectrometer is a state-of-the art, high-resolution, triple-grating system, equipped with a back-illuminated liquid nitrogen cooled CCD detector, and with multiple motorized switching mirrors.
2. Olympus BX-41 Microscope coupled with the Raman Spectrometer permits for detailed surface analysis in a process called Raman/Luminescence Mapping or Imaging. A motorized XYZ Translation Stage allows for very high spatial resolution (sub-micron scale) scanning over surfaces and bulks.
3. Argon/Krypton Stabilite 2018 Spectra Physics Gas Laser with a maximum output power of 2.5 W can generate laser light in a range of visible lines ranging from deep violet through green, blue and up to red: 454.5 nm, 457.9 nm, 476.5 nm, 488 nm, 514.5 nm, 520.8 nm, 530.9 nm, 568.2 nm, 647.1 nm, and 676.4 nm.
4. Newport SMART ST-UT2 HoneyComb, research grade Optical Table with an actively damped vibration-controlled system hosts the entire setup.

The Raman spectroscopy setup is ideal for the investigation of not only crystalline materials, but also glasses and glass-based materials. Raman is recognized as a very powerful, nondestructive tool to study both glass surface and bulk structures and chemistry. Raman spectra reflect changes in glass composition and the modifications of connectivity of glass forming units (ex. SiO4 tetrahedra) as well as the degree of polymerization of the glass network (ring structure).

In Luminescence Spectroscopy we use a laser to excite fluorescence of a sample of solid, liquid or gas and we can detect the light emitted by the sample. In this way we get information about the energy of the electronic levels. These measurements can also be done while subjecting a sample to tens of thousands of atmospheres of pressure (in a Diamond Anvil Cell)

In Surface XYZ Mapping we can investigate the surface (XY) or depth (Z) of a solid and create 3D surface maps with precision of 100nm. This technique combines the power of a confocal microscope with the probing capability of a spectometer. We use it in detecting uneven surfaces, chemical inclusions, layers in a sandwitch-type material.

All of the above measurements can also be done on samples loaded inside of a Diamond Anvil Cell (DAC) which allows to study materials in situ, at extreme pressures. Studies in the DAC include Raman or luminescence spectroscoy and phenomena that can be detected are: phase transitions, amorphization, bond contraction and expansion.

 

Raman SpectrometerRaman violet laser

Raman setup frontRaman back

Raman sideOlympus Microscope



SIMULTANEOUS DIFFERENTIAL SCANNING CALORIMETER AND THERMOGRAVIMETER (DSC-TG-Cp)

NETZSCH STA 449 F1 Jupiter allows us to measure Heat Flow and Mass Changes in a solid or liquid sample at the same time! Heating can be up to 1550 deg. C and mass changes are recorded with a nano-gram precision.

The NETZSCH STA 449 F1 Jupiter allows in situ quantitative determination of caloric effects (DSC-Differential Scanning Calorimetry) and mass change effects (Thermo-Gravimetry) in materials during a heating and cooling cycles.

This instrument is especially useful for out studies of glass characteristic temperatures, such as glass melting point, glass transformation temperature, crystallization point.

The possibilities of analysis are many:

- specific heat Cp,
- for glasses: characteristic temperatures Tg, Tm, Tc
- corrosion
- oxidative stability,
- material purity determination,
- melting/crystallization behavior,
- solid-solid phase transitions,
- polymorphism,
- degree of crystallinity,
- glass transitions,
- thermo kinetics,
- mass changes,
- decomposition, etc.

DSC openDSC in Lab



HIGH TEMPERATURE FURNACES FOR GLASS MELTING AND SOLID STATE SYNTHESIS

High Temperature Furnaces: Melting of Glasses and Solid State Synthesis.

The Materials Synthesis cluster is equipped with research grade electric laboratory furnaces. We use them for melting glasses, for solid state synthesis, as well as for programmed heating treatments for annealing glasses or for driving nanocrystallization processes in glasses.Complementary equipment includes a variety of crucibles: alumina, platinum and ceramic.

1. Carbolite Furnace 1700oC / 3100 F
Carbolite HTF-17/5 is a rapid heating, high-temperature furnacecapable of operating up to 1700oC (=3100 F) with excellent thermal insulation. The furnace has molybdenum disilicide heating elements and has programmable operation modes. Carbolite HTF-17/5 allows for controlled-atmosphere, very high temperature melting or sintering of diverse materials and high-temperature materials synthesis such asmelt-quench regimes (ex: for melting silica).

2. Carbolite Furnace 1400oC /2550 F
Carbolite RHF 14/8 furnace operating up to 1400oC (=2550 F) with silicon carbide heating elements and a programmable rapid heating. The furnace is excellent for solid state synthesis or annealing processes involving long heating regimes.

3. Thermolyne Furnace 1150oC / 2000 F
Thermolyne 1200 electric furnace with resistive heating is capable of operating up to 1150oC (=2000 F). This furnace has a small chamber that assure fast heating/cooling and it can be used for materials sintering, annealing and solid state synthesis.

   Big FurnacesHot furnace

small furnaceFurnaces



HIGH-PRESSURE EQUIPMENT: DIAMOND ANVIL CELLS

The Materials at Extreme Environments (High-Pressure) Laboratory is equipped with Diamond Anvil Cells (DACs) as well as anvils and various matching high-pressure related tools.

The DACs allow to subject various samples to pressures of up to 1,000,000 atmospheres (>100 GPa). The samples studied are compressed between culets of two diamonds.

The DACs enable for in situ study of pressure-induced structural changes (phase transformations) in diverse materials such as crystals, polycrystals, amorphous materials (glasses), ceramics, nanocrystals and composites as well as in liquids and in gases compressed up to very high pressures (on the order of pressures at the center of the earth).

Diamond Anvil Cells can be combined with the T-64000 Raman System (see above) - by using a long-working distance objective - to collect in situ Raman scattering or Luminescence spectra in function of elevated pressure.

DACs can be combined with x-ray diffraction at a synchrotron light source to study modification of diffraction patterns in function of elevated pressure.


DAC and Raman

 DACsHP Station



MICROSCOPE WITH X300 MAGNIFICATION AND HD CAMERA

The Leica MZ-16A Motorized Stereo-Microscope allows for examining and for real time video-recording of materials at magnifications up to 300x.

The microscope also allows for fast switching between a stereo view and a perfectly vertical object viewing (vital for example when aligning diamonds in a Diamond Anvil Cell).

The integrated HD Video-Camera allows for capturing of pictures and videos, as well as for real time display of images on a 24 inch LCD monitor.

   Leica



MICRO ELECTRIC DISCHARGE MACHINING SYSTEM - EDM

We use the Micro Electric Discharge Machining System from Hylozoic Products to drill axially symmetric holes of the order of ~100 m in rhenium or steel gasket. The act of drilling (or electric discharge machinig) is done with inexpensive copper or tungsten wires.

It is equipped with a 20X magnification microscope for easy operation.

The Micro EDM System is also well suited for many other specialized micro-machining operations in a laboratory setting, such as machining of slits and apertures to collimate light, and cutting small disks or slabs from metal foils, wires, or crystals.

Hole in Gasket

   edm



DIAMOND WHEEL SAW

The Model 650 Low-Speed Diamond Wheel Saw (SB Tech) is a compact, multipurpose precision saw.

It is designed for a low-speed cutting of a wide variety of materials with minimal subsurface damage. Its low speed makes it possible to cut fragile materials that would otherwise fracture.

We use it to cut glasses for optical studies and ceramics into rectangles or plates with parallel and smooth surfaces and precise thickness.

   Diamond Saw



HANDS-FREE GRINDING AND POLISHING SETUP

The Model 900 Hands-Free Grinding/Polishing set-up (SB Tech) allows for convenient surface preparation (polishing) of small specimens (ceramics, glasses, crystals, bone fragment) including high speed rough grinding and low speed final polishing..

We use it to polish glasses and ceramic samples to obtain mirror-like smooth surfaces which are necessary for optical spectroscopy measurements. The hands-free feature is really neat and allows to "save" your fingers!

This setup is also perfect to grinding down a solid to an exact thickness with micron precision!

   Polisher



15 TON HYDRAULIC PRESS WITH GAUGE

The 15-ton Hydraulic Press, SPECAC ATLAS, with a gauge and with an evacuable Pellet Die set-up has an adjustable pressure control.

The Hydraulic Press is particularly well-suited for preparing variable thickness pellets out of powdered samples for the use in solid state synthesis as well as for FTIR KBr pellets, XRF pellets as well as for preparing samples for certain optical spectroscopy studies.

We use it make pellets (discs) from all sorts of powders. It is really effortless (!) to use and the calibrated gauge allows to control the amount of force applied.

   PressPellet Die




OTHER GENERAL PURPOSE EQUIPMENT

Ultrasonic Bath (VWR B1500AMTH) for direct and indirect cleaning
Hot plate with magnetic stirring function (Corning)
High Precision Analytical Balance, Mettler Toledo AB104-S/ FACT, has readability down to 0.0001 g and max capacity of 220g.

   Mitutoyo


 
 
EXPERIMENTS THAT WE DO AT NATIONAL USER FACILITIES
SYNCHOTRON LIGHT SOURCES: X-RAY DIFFRACTION AT HIGH PRESSURES

APS SketchA Large portion of our experiments is carried out at national sycnhrotron light sources: Sector 16 (HPCAT), Sector 9 (MRCAT) at the Advanced Photon Source, Argonne National Laboratory, APS-ANL (Chicago, IL) and the Advanced Light Source of Lawrence Berkeley National Laboratory, CALYPSO beamline(Berkeley, CA)

   National Labs

 
EXAFS AT ARGONNE NATIONAL LAB - MRCAT & CMC
X-ray Absorption Fine Structure, XAFS setup at Beamline 9-BM of Advanced Photon Source of Argonne National Laboratory. When coupled with a cryostat (see picture) this setup allows measurements at temperatures of the order of a few kelvin. We use this setup for studying local atomic environment of various nanomaterials.

   9bm

 
 
    © 2015, Kris Lipinska
University of Nevada Las Vegas. All rights reserved.