High Temperature X-ray Diffraction - J. P. Cline

The x-ray diffraction facility at NIST consists of a high-temperature machine of theta-two theta geometry equipped with an incident beam monochrometer and a position sensitive proportional counter. The incident beam monochrometer removes the K2 radiation and results in diffraction profiles that are more sensitive to effects of sample character. The position sensitive detector allows for data collection at a rate two orders of magnitude faster than conventional detectors. The furnace is an enclosed high vacuum chamber capable of reaching 3000 K, and is equipped with a mass flow controller for atmospheric control. This equipment is used for the study of high-temperature phase equilibria, high-temperature reaction kinetics, sintering of monolithic ceramics, and strain development during sintering of ceramic composites. Additional equipment consists of four automated and updated Philips diffractometers which are used for certification of standard reference materials (SRMs), studies on the effects of microabsorption and extinction, and the development of the Rietveld method for a conventional, sealed tube, x-ray diffraction equipment.

Electrokinetic Measurements - V. A. Hackley and S. G. Malghan

The Matec ESA-8000 system has the unique capability for measuring colloidal properties in dense slurries. The analytical capabilities of the ESA system include performance in the following modes: potentiometric titration, conductometric titration, time-series titration, and concentration series titration. In the selected mode, the equipment can monitor: electrokinetic sonic amplitude, zeta-potential, electrophoretic mobility, electrical conductivity, isoelectric point, surface charge density, and phase angle of the material with the specified experimental conditions. The latest addition to this laboratory is a Acousto-Sizer by Matec Applied Sciences.

Slurry Rheology - S. G. Malghan and V. A. Hackley

The RTI rheometer allows for viscosity as well as rheology characterization of ceramic slurries. Rheological measurements are more informative and flexible with respect to the various slurry properties: Newtonian, pseudoplastic, plastic, dilatant, and thixotropic. The modeling of these rheological properties as a function of sample treatment and surface chemical properties is paramount in developing and improving the slurry processing technology.

Physical Properties Characterization Laboratory - L. Lum, D. B. Minor, P. T. Pei and S. G. Malghan

The physical properties characterization laboratory is equipped with state-of-the-art techniques for the measurement of particle size distribution, specific surface area, specific gravity, tap density, and porosity. The particle size distribution is measured by three techniques -- gravity sedimentation by Sedigraph, centrifugal sedimentation by Joyce-Loeble, and laser diffraction by Horiba LA-900. The range of particle size distribution covered by these techniques is (0.01 to 200) µm. The specific surface area determination is carried out by nitrogen adsorption and the BET method. The porosity of powders and ceramics is measured by mercury intrusion.

Colloidal Processing of Powders - S. G. Malghan, D. B. Minor and P. T. Pei

The focus of this laboratory is to develop data and understanding of non-oxide powders processing in aqueous environment. The laboratory is equipped with instruments and equipment for studying deagglomeration, dispersion, suspension stability, slurry casting, and green body microstructure evaluation.

Agitation Milling of Powders - D. B. Minor and S. G. Malghan

High energy agitation milling of silicon nitride powders is carried out with a minimum contamination by the use of a specially designed milling system. This milling device allows for the size reduction of silicon nitride powder by milling at high slurry densities in approximately 1/6th to 1/10th of the time required by the conventional tumbling ball mill. The mill is lined with silicon nitride and the media are made of silicon nitride materials; hence, external sources of contamination can be minimized.

Nuclear Magnetic Resonance (NMR) - P. S. Wang

The solid state NMR facility includes a Bruker MSL-400 NMR system capable of studying almost all NMR-active nuclei in the periodic table in both solid and liquid states as well as performing NMR imaging in proton and carbon-13 frequencies. Currently, the operation parameters for both states at proton, deuterium, carbon-13, and aluminum-27 have been defined and proved by documented NMR spectra of organic and inorganic molecules. The equipment has been tuned to Si-29, Cu-63, and Y-89.

Scanning Electron Microscope/Image Analysis (SEM) Facility - J. F. Kelly

This laboratory is equipped with an Amray 1830 digital scanning electron microscope with LaB6 source and a Leitz optical microscope. The SEM is equipped with a solid-state backscatter detector and an ultrathin-window x-ray detector. A Kevex Delta V EDS x-ray analysis and image analysis system is interfaced to both the SEM and optical microscopes. Automated imaging capabilities enable rapid size and shape analysis of a variety of imaged features, including ceramic powder particles and second phase regions in composite structures. Fracture stages have been developed for real time observation and measurement of in-situ crack propagation in ceramic specimens. The addition of an interior mounted phosphor screen with video camera imaging provides the capability of imaging single-grain electron backscatter diffraction patterns from bulk specimens. This permits the measurement of crystallographic orientation in ceramic specimens.

Thermal Analysis Facility - J. S. Wallace and J. E. Blendell

This facility includes equipment for measurement of behavior of ceramic materials in a wide range of atmospheres and temperatures. The equipment is comprised of a computer-controlled differential pushrod dilatometer capable of measuring thermal expansion or sintering shrinkage in vacuum, inert, oxidizing or reducing conditions from room temperature to 1600øC. The atmosphere can be monitored using either a zirconia oxygen cell or an external mass spectrometer using its own associated computerized data acquisition system.

The second major piece of equipment is a simultaneous thermal analysis (STA) system which is capable of performing simultaneous thermogravimetric and differential thermal analysis from room temperature to 1700^oC. Atmospheres can be varied from vacuum to single and mixtures of gases using a four-channel mass flow controller. The STA is also connected to the mass spectrometer system and it's associated data acquisition system. The quadrapole mass spectrometer system has a capability of analyzing to 512 AMU.

Chemical Laboratory Facilities - J. J. Ritter

Chemical synthesis of powders is carried out in a well equipped laboratory, which consists of controlled atmosphere glove boxes, preparative chemical vacuum systems, and a chemical flow reactor. A range of powders can be synthesized for exploratory purposes.

Ceramics Powders Processing Laboratory - J. S. Wallace and J. E. Blendell

A processing laboratory for processing and sintering well controlled ceramic powders has been assembled. This facility consists of: equipment for chemical powder synthesis routes, attrition mills, ball mill, jet mill, pressure slip caster, uniaxial presses, cold isostatic press, spray dryers, drying ovens, hot presses, air furnaces to 1700^oC, controlled atmosphere furnaces with associated gas flow systems and oxygen sensors for temperatures to 1600^oC, graphite furnace for temperatures to 2300^oC, and a hot-isostatic-press/gas-pressure sintering furnace capable of 2300^oC and 200 MPa using graphite elements and insulation.

Nano-Size Powders Processing - E. Gonzalez, G. J. Piermarini and S. G. Malghan

This is a new facility which consists of equipment for powder handling in inert environment, compaction of nano-size powders, and sintering under environment control. The compaction equipment was designed to facilitate the application of wide range of pressures (up to 5 GPa), temperatures (cryogenic to 1000^oC), and environments. The size of green ceramic produced in this system is 3.0 mm diameter.

SURFACE PROPERTIES

Wear Tests - S. M. Hsu

A state-of-the-art friction and wear testing laboratory is available for the evaluation of materials under different applications and conditions. Contact geometries include pin-on-disk, cross cylinders, ball-on-flat, ball-on-balls, flat-on-flat, and ring-on-block. Various motions and operating conditions are available to simulate many industrial applications. Environmental control includes temperature (room temperature to 1200^oC), vacuum, and humidity.

Surface Analysis - S. M. Hsu and R. S. Gates

Many modern specialized instrumentation are available for the analysis of surface properties of materials. Mechanical property measurement include hot hardness tester, Vicker's indenter, nano- indentor, scratch test, and controlled-depth micro-scratch test. Chemical property measurement include time-resolved micro-Raman spectroscopy, FTIR microscopic spectroscopy, GC-MS, SEM with EDX analysis, IR and UV spectroscopies with API compound identification files. A specially designed, organo-metallic specification facility is also available to detect surface reaction products at ppm level. Access to conventional surface analysis such as XPS, ESCA, Auger, etc are also available through external contracts.

STM/AFM - S. M. Hsu

A digital commercial scanning tunnelling microscope (STM) and atomic force microscope (AFM) is available to measure surface properties at atomic level.

Time-Resolved Micro-Raman - S. M. Hsu

This versatile facility consists of a pulsed Nd-YAG laser, a CW Ar-ion laser, a triple monochromator, and a gated intensified diode array detector. This facility, therefore, provides a wide variety of Raman analysis techniques in both time-resolved and continuous operation modes, using either visible or ultra-violet excitation sources for either operation mode. In addition, either bulk macro-Raman or 5-µm-resolution micro-Raman analyses are available.

MECHANICAL PROPERTIES

Surface Forces Laboratory - D. T. Smith

The surface forces laboratory consists of a semi-clean-room preparation facility and a crossed- cylinders surface force apparatus. The crossed-cylinder apparatus permits measurements of atomic-scale forces between surfaces. It can be operated with a variety of liquid or gaseous environments, thus allowing investigations of the effects of chemical changes on the forces between two surfaces. The apparatus includes several unique features that were developed and built by the surface forces group. First, sensitive custom electrometer circuits were built into the apparatus to allow in-situ measurements of surface charges resulting from contact electrification. Second, the apparatus has been modified to permit the sliding of one surface over the other under constant applied load.

Instrumented Microindenter - D. Smith

This apparatus is designed to bridge the gap between conventional hardness testers and the nano- indentation facility. It measures continuous load-displacement curves for indentations in the load range 10 g to 2 kg, and is of particular use in studying the mechanical properties of thermal-spray and other ceramic coatings with relatively coarse microstructures.

Analytical Electron Microscopy - B. J. Hockey

Several transmission and scanning electron microscopes are available for analysis of the changes in microstructure as a result of creep.

Glass Melting - D. A. Kauffman

Extensive glass melting and annealing facilities for production of melts up to 1600øC are available. Batch sizes up to about (2.5 to 3) kg can be produced using this equipment. Special facilities for melts containing heavy metals such as thallium and lead are also available.

Creep Apparatus - R. F. Krause, Jr. and S. M. Wiederhorn

The creep measurements laboratory possesses nineteen controlled-temperature furnaces (800 ^oC to 1700^oC), seven laser extensometers, ten optical long-distance microscopic extensometers, and twenty loading frames (fourteen pneumatically driven, four screw driven, and two direct weight). Among these loading frames fourteen can be used in tension, three in tension or compression, one in flexure, and one as a sintering forge.

Hot-Pressing Apparatus - R. F. Krause, Jr.

A graphite heating-element furnace (2300^oC maximum) which be can operated in vacuum or an inert gas atmosphere is mounted in a hydraulic loading frame (0.5 MN maximum). Ceramic powders can be hot pressed in graphite dies, (50, 75, 100, and 125) mm diameter.

Nano-Indentation Facility - D.T. Smith

The Ceramics Division nano-indentation facility consists of a Nano Indenter II indentation machine, manufactured by Nano Instruments, Inc., and related computer and optical components. The indenter, under computer control, is capable of measuring loading-unloading curves with displacement resolution better than 0.1 nm and load resolution better than 200 nN. Nomarski interference contrast (NIC) optics and translation stages with placement precision better than 1 µm permit the measurement of material properties such as hardness and Young's modulus in selected volumes as small as 10^-17 m³.

Optical Microscopy Laboratory - G. D. Quinn

The optical microscopy laboratory is equipped with conventional reflected light microscan inspection of polished specimen as well as stero-binocular microscopes and camera stands for fracture surface analysis. A WILD M-10 stereo discussion microscope system with video monitoring and instant photography capability is very well suited for fractography.

ELECTRONIC MATERIALS

Level 10 Clean Room - J. E. Blendell

A Level 10 Clean Room has been constructed for the processing of ceramics in a controlled environment where the presence of air contaminants at low levels can seriously affect the final product's properties. The room is provided with separated work stations to allow simultaneous conduct of experiments.

Thermal Wave Analysis Facility - A. Feldman and G. S. White

This facility is used for characterizations based on variations of thermal diffusivities. Equipped with both an Ar-ion and CO² laser, the facility permits analyses by infrared and mirage methods. It is especially useful as a nondestructive method of detecting flaws in near-surface regions of ceramics.

OPTICAL MATERIALS

Optical Characterization - L. H. Robins and A. Feldman

Facilities include a Cary spectrophotometer for measuring optical transmittance in the spectral range 0.2 µ m to 2.5 µ m, optical spectrometers for measuring photoluminescence and Raman spectra, and an argon ion laser.

Magneto-Optical Imaging of High Temperature Superconductors - D. L. Kaiser, F. W. Gayle (Metallurgy) and A. Shapiro (Metallurgy).

The facility consists of a magneto-optical imaging system with attached video equipment. It is used to measure real-time flux distributions in high-temperature superconductors as a function of temperature, (7 - 300) K, and applied magnetic field, (0 to ± 65) mT.

Electro-optic Thin-film Characterization - L. D. Rotter

The facility consists of a vibration-isolated optical table, argon-ion and helium-neon laser sources, polarizing components, lenses, optical stages, optical detectors, and electronic signal processing equipment for measuring the electro-optic coefficients and optical birefringence of thin ferro- electric films.

Metalorganic Chemical Vapor Deposition (MOCVD) System - D. L. Kaiser

A specialized system was constructed for the deposition of oxide thin films from metalorganic precursors. It has been used to deposit BaTiO₃ films on 1.5 cm x 1.5 cm substrates.

Diamond Film Deposition - E.N. Farabaugh and A. Feldman

Facilities consist of three hot-filament CVD reactors and a microwave-enhanced CVD reactor. The hot-filament reactors can accommodate substrates up to 2.5 cm X 2.5 cm square. The microwave reactor can accommodate substrates up to 10 cm in diameter. The reactant gases are hydrogen, methane, oxygen, argon, and ethyl alcohol which contains boron of doping. Growth rates typically range from (0.1 to 0.6) µ m/h.

MATERIALS MICROSTRUCTURE CHARACTERIZATION

Synchrotron Radiation Beamlines - G. G. Long

The Materials Microstructure Characterization Group operates two beamstations on the X23A port at the National Synchrotron Light Source at Brookhaven National Laboratory in New York. These two beamstations offer access to dedicated instrumentation for small-angle x-ray scattering, x-ray diffraction imaging (topography) and EXAFS.

Small-angle x-ray scattering can be carried out in the energy range from (5 to 11) keV. The minimum wavevector is 4 x 10^-3 nm^-1 and the wavelength resolution is / = 10^-4, allowing anomalous small-angle scattering with excellent resolution. Diffraction imaging of single crystals and powders is carried out with monochromatic photons between (5 and 30) keV. An energy- tunable, x-ray image magnifier enables imaging of microstructure down to less than 1 µm. EXAFS experiments are also performed over an energy range from (5 to 30) keV.

Small-angle scattering measurements on ceramic and metallurgical materials are being used to characterize the microstructure in the 2 nm to 1 µm size range as a function of starting chemistry and processing parameters. Diffraction imaging is being used to study imperfections and strains in single crystals and powder compacts. EXAFS is being used to study the structure of strained semiconductor interfaces and metal multilayers. A combination of EXAFS and diffraction will provide a capability for site-specific local structure determination in crystals.

SANS - Ceramics Furnace - G. Long

The SANS-Ceramic furnace is a unique facility that has been recently commissioned. This system allows simultaneous in-situ densification studies of ceramic powders and SANS measurements. The experimental system has been designed to carry out densification studies of oxide powders at temperatures up to 2000^oC. In addition, the furnace will be equipped with a dilatometer.

PHASE EQUILIBRIA

Single Crystal X-ray Diffraction Facility- W. Wong-Ng

Currently, this research facility is primarily used to characterize single crystals in terms of crystal symmetry, lattice parameters and detailed structure.

Phase Equilibrium Facilities for High-T_c Superconductor Systems Bi(Pb)-Sr-Ca-Cu-O and Ba-R- Cu-O - W. Wong-Ng and L.P. Cook.

This facility consists of two controlled-atmosphere, quenched furnaces and a Mettler thermal analyzer for performing DTA/TGA experiments. Both solid and melt can be quenched into liquid nitrogen cooled helium atmosphere so that the high temperature structure can be captured and analyzed. Liquid composition can also be estimated quantitatively with a wicking method during the quenching experiments.