The Department of Materials Science and Engineering occupies more than 100,000 square feet of laboratory and office space in Watts Hall, MacQuigg Laboratory, Fontana Laboratories, Koffolt Laboratories and the Edison Joining Technology Center.
In collaboration with other engineering departments and research units at Ohio State, high-tech equipment and facilities support the educational and research programs of the department. Examples of the facilities and equipment available--valued at nearly $30 million--are described below.
Ceramic Processing | Chemical Sensor Materials Characterization | Computing | Electrical and Electrochemical Measurement | Electron Optics and X-Ray Characterization | Inorganic Materials | Mechanical Testing and Forming | Microstructural Characterization | Sensors and Measurements | Solidification and Metal Casting | Superconducting Materials Characterization | Thermal Analysis | Thin Film Preparation and Characterization
Ohio State’s Department of Materials Science and Engineering (MSE) has comprehensive powder processing facilities, including particle size reduction mills, an attrition mill, a re-circulating sonicator, an Hg-Porosimeter, a glove box for processing water-sensitive materials, and an array of thermoanalytical tools. A wide range of furnaces (air-fired, vacuum and controlled-atmosphere) are available for calcining and sintering studies as well as a precision dilatometer to measure compact shrinkage. In addition, a vacuum hot press capable of temperatures in excess of 2000°C and loads up to 15,000 pounds is available.
Also included in the facilities are a hot isostatic press, capable of temperatures up to 1200°C and pressures up to 30,000 psi, and a cold isotatic press for dry pressing that’s capable of pressures up to 30,000 psi. An instrumented laboratory scale extruder and a laboratory scale tape caster are among the other available forming equipment. Additional capabilities in the ceramic processing facilities include:
- Electrochemical deposition of nanomaterials
- Electrospinning capabilities
- Controlled atmosphere reaction chambers for fabricating 1D oxide nano-structures
- High-temperature, low-pressure CVD chambers
- Colloidal processing
- A range of high-temperature furnaces with controlled atmosphere capabilities
- A sputtering facility with both dc and rf capabilities for thin-films of metals and ceramics
- A PLD system for oxide thin-films
- Brittle failure in layered systems
- High-temperature TGA and DSC facilities
Research conducted in this laboratory focuses on chemical sensor arrays, which are based on the concept that, for an array of sensor materials, its individual, differentially selective responses to changes in gas compositions can be modeled and then used to identify unknown gas compositions. The more selective the individual responses, the fewer responses needed for the model and, hence, fewer materials for the array. That, in turn, means the actual device will be simpler and more affordable.
The materials challenge is to synthesize then characterize the responses of large numbers of candidate materials in order to find a small array set of materials with enough differentiation to predict the concentrations of the gases of interest. Listed below are descriptions of the equipment available at Ohio State to perform this type of research.
Infrared Thermographic Screening
A novel IR thermographic technique has been developed to rapidly screen compositional libraries of semiconducting oxides for chemical sensing applications. The system was designed to monitor and measure the changes in the electrical properties of an array of materials when they interact with a variety of gases and gas mixtures of interest. The responses are derived by subtracting the responses in a reference gas from those in the test gas of interest. The novel aspect of this technique centers on the application of a voltage bias across the multiple sample array. This provides a more effective determination of a semiconducting oxide material's sensitivity because the resistance change that occurs with gas adsorption is amplified by directly monitoring the associated I, V thermal response. More than 2,000 materials have been characterized by this technique. Materials determined to be "hits" (i.e., showing activity and selectivity to a gas of interest) are then more rigorously characterized through additional techniques.
AC Impedance Measurements
AC impedance measurements are taken in a controlled atmosphere tube furnace. Typically, the resistance of a metal oxide semiconductor is measured as a function of gas concentration and temperature. When compared to a standard state condition, the resistivity changes associated with changes in the concentration of various gas components yield a measure of both a material's sensitivity and its selectivity to those components. Unfortunately, the design of the apparatus does not permit the measurement of dynamic properties, such as response time. However, the AC impedance-derived sensitivity and selectivity data facilitate the selection of candidate array sets of materials through the Principal Components Analysis (PCA) of the materials' responses. The AC impedance measurements made as a function of frequency (1 Hz-1 MHz) and temperature (400-800°C) in various gas environments also allows for the study of a material's conduction mechanisms.
Ohio State’s Device Sensitivity, Chemistry and Response Time Experimental System (Descartes) was designed to measure a material's sensitivity and selectivity as well as its dynamic response to changes in gas composition. High-gas velocity and a small sample chamber, coupled with a computer-controlled gas manifold, give the Descartes system a dynamic gas switching time constant of approximately 0.65 seconds, which is faster than the 1 Hz data acquisition rate.
The ease of visually comparing a material's response characteristics using the Descartes system makes it the instrument of choice for investigation and optimization of materials microstructures. The Descartes system can be run either as a hot wall reactor (isothermal operation) or cold wall with heated chips. The standard configuration allows for 48 materials to be tested at one time (six on each side of four chips) or, in the case of heated chips, 24 materials per run (six on one side of four chips). AC impedance measurements can also be taken on sensor devices in the Descartes system to examine the electrical characteristics of the materials in the frequency domain.
While instabilities over the short term (a few hours) can be detected with Descartes data, a measure of each material's long-term response stability and durability is critical to the eventual success of sensor materials for applications. This need is addressed through Ohio State’s Device Stability and Durability Experiment (DeSade), a derivative of the Descartes system. In DeSade, the sensor materials can be subjected to both dynamic synthetic exhaust gas cycling and to thermal cycling by computer-controlled chip heating. A typical DeSade run will be between 500 and 1,500 hours. Over that time, a material's standard state resistance and sensitivities are expected to have changed by less than 10 percent, making it a candidate array material.
and Faculty Computing Resources
All students and faculty in the Department of Materials Science and Engineering have access to extensive computing and information resources located in the materials science and chemical and biological engineering complex on Ohio State’s campus. More than 100 computers with the latest technology are available to support innovative teaching and cutting-edge research. A large array of software enables 3D imaging of atomic structures, diffraction analysis, mathematical modeling, casting simulations, stress analysis, and a variety of other engineering capabilities. Gigabit Ethernet switches provide quick access to a wide variety of resources, including internet-based materials databases as well as e-books, journals and search engines offered by The Ohio State University and Ohio-link Information Network. DVD recording, color laser printing, large format plotting, digital video recording and editing, and high-resolution scanning provide students and faculty with the tools needed to prepare professional presentations and manuscripts.
In 2011, three of the computing rooms in the facility were renovated to support classroom instruction in computational material science. The novel design includes TouchSmart computers, custom tables, wall-mounted flat panel displays and digital white boards to help convey technical information. Clustered seating and interactive switching enable student teams to display their information to other team members or the entire class. Both on-campus and distance students benefit from on-the-fly recording of lectures that can be streamed live or archived for reference.
Students enrolled in Materials Science and Engineering or Chemical and Biomolecular Engineering programs at Ohio State can pay a quarterly computer fee to use the ECR6 facility, one of several computer laboratories available to students in the College of Engineering.
Staff and faculty have access to the 512-CPU (2.4 GHz Intel Xeon) Beowulf cluster at the Ohio Supercomputer Center located on Ohio State’s West Campus. The Center holds frequent training sessions on parallel programming and performance optimization, and also offers Cray supercomputers for demanding computational projects.
The laboratories in Ohio State’s Fontana Corrosion Center are equipped with a wide range of instrumentation, including:
- Computer-controlled stations for electrochemical measurements
- Two scanning probe microscopes
- A Scanning Kelvin Probe
- An electrochemical microcell
- Slow strain rate frames for testing stress corrosion cracking susceptibility
- A salt spray chamber and ultraviolet exposure chamber
- Quartz crystal microbalance
- A multichannel microelectrode analyzer
- Facilities for fabricating bulk and thin film samples
- Interferometric optical profilometer
The Ohio State Department of Materials Science and Engineering, through its Center for Industrial Sensors and Measurements (CISM), supports the development of solid-state electrochemical devices such as sensors and fuel cells. Capabilities include:
- Thick film fabrication by screen printing, ink jet printing and spin coating
- A wide range of electrical (dc and ac) measurement equipment, including a probe station
- A set-up suitable for photo-catalytic studies
- A complete sensor measurement and testing facility with capability for controlled gas flow and mixing systems
- Computer-controlled data acquisition and analyses with specially written software
- A ferroelectric test system
The MSE Department houses and administers Ohio State’s Campus Electron Optics Facility (CEOF), which was recently expanded to accommodate additional equipment, personnel and capabilities. The equipment, valued at more than $10 million, is used for both graduate and undergraduate instruction, as well as by researchers at Ohio State and elsewhere. CEOF also offers for use four transmission electron microscopes, three scanning electron microscopes and a variety of x-ray diffractometers.
The Inorganic Materials Science group focuses its research on materials that are made through the controlled consolidation of precursor particles and thermal processing. These materials have potential uses in fuel cells for energy conversion, membranes for separation, and sensors for environmental applications. Extensive facilities include:
- More than 2,700 square feet of lab space for taking high-precision measurements
- Swagelok stainless steel network for high purity gases that is required for synthesis, characterization and operational tests
- Cat-6 wired Ethernet, >1 Gbs data exchange between various set-ups that allows for "hardware in the loop" studies for system integration purposes
- Monitored inorganic membrane reactors and SOFC.
- High-definition colloidal processing of inorganic materials
- High-definition thermal processing of inorganic materials
- Membrane, particle and porosity characterization
The MSE department houses and administers the Mechanical Testing Facility (MTF). This facility has undergone a major expansion in equipment, personnel, and capabilities. The equipment, valued at over $1.5 million, is used for both graduate and undergraduate instruction and by researchers in need of the specialized facilities available at MSE. The MTF includes equipment to perform routine and short-term tests of tensile and compressive properties, hardness, fatigue life, and impact toughness. The primary mechanical characterization laboratory includes several computer-controlled instruments with computerized data acquisition. All listed test frames are servo-hydraulic type:
- MTS 810 test frame, 100KN load capacity, 150mm actuator stroke, new (as of October 2005) MTS FlexTest Controller with latest generation of MTS control software for tensile, compression, fatique, and crack growth testing. Controller is equipped with two strain channel signal conditioners for use with a biaxial extensometer. Four different gage length mechanical extensometers, plus a non-contacting laser extensometer are also available on this machine. The crack growth software/hardware supports DC potential drop and mechanical clip gage measurement techniques. MTS 100KN hydraulic grips are installed with five available wedge assemblies that allow mounting of flat specimens (sheet metal) up to 0.75mm thickness, 50mm width and round specimens from 5mm to 30mm in diameter.
- Instron 1322 test frame, 250 KN capacity, 250mm stroke, new (as of 10/05) MTS FlexTest Controller installed with latest generation of MTS control software for tensile, compression, fatique, and crack growth testing. Single strain channel signal conditioner, will support same extensometers as listed above with the exception of the biaxial. Two furnaces installed for elevated temperature testing in air(1200C max).
- MTS 810 test frame, 100KN load capacity, 150mm stroke, new (as of 10/05) MTS FlexTest controller with the above mentioned software packages installed. Frame is equipped with an all metal vacuum/argon atmosphere furnace made by Oxy-Gon. Hot zone measures 60mm in diameter by 75mm length, temperature up to 1950C. This machine is used for elevated temperature tensile, compression, and fatique tests.
- MTS 804 test frame, 500KN capacity, 150mm actuator stroke, new (as of 10/05) MTS FlexTest controller installed. Software same as above, one strain channel available. This machine is used for mechanical testing requiring high force levels.
- MTS 831 test frame, 25KN load capacity, 100mm actuator stroke, new (as of 10/05) MTS FlexTest controller installed. This machine is used for high cycle fatique testing. Special servo valves allow precise control of load or stroke up to a frequency of 200hz. An air furnace capable of 1400C is installed on this frame for elevated temperature tests.
- Mechanical Behavior Lab equipment also includes: Two Interlaken forming simulators with Interlaken software controls, these presses have clamp capacities of 300 Kip, punch force of 200 Kip. One machine is currently used for magnetic pulse forming tests, the other for standard die forming tests. An Interlaken 60 Kip press is used for lubricant and 3/4 formability testing, and an Interlaken hydraulic draw/bend test machine for sheet metal studies.
This general-use equipment is supported by a complete machine shop to prepare specimens and fixtures for testing. Several machine-mountable furnaces are available with capabilities up to 1300C. Mechanical forming equipment includes a rolling mill. Other standard facilities include Rockwell and Brinnel hardness, Vickers and Knoop microhardness, Charpy and Izod impact test, table-top tensile, and cam fatigue testing machines. A variety of specialized research equipment is also available for use. Many of these instruments were designed at Ohio State for research work supported by industrial, state, and federal grants. These unique machines include:
- Thermal cycling testing
- 227,000 kg hydraulic forming simulator, with complete computer control
- 50,000 Joule electro-hydraulic capacitive discharge high-rate tester
- 68,000 kg prototype sheet formability test system
- 55,000 kg double-action press and forming machine
Ohio State's Department of Materials Science and Engineering has a fully-equipped laboratory for cutting, grinding and polishing materials for microstructural characterization, including both manual and semi-automatic machines. A variety of optical microscopes are available, as well as Nikon epiphot and Nikon optiphot microscopes fitted with fully automatic exposure systems and interfaced with a TV monitor, VCR and color projector. The facility also provides computer-based quantitative image analysis and houses instruments for taking normal, superficial and microhardness measurements.
Several laboratories have been established at Ohio State to support the development of solid-state sensors. These facilities and accompanying capabilities, along with those in the Center for Industrial Sensors and Measurements (CISM), include:
- Thick-film and thin-film fabrication devices
- Electronic nose along with artificial intelligence and neural-net software
- A wide range of electrical measuring equipment
- A complete sensor measurement and testing facility with the capability for controlled gas flow and mixing systems
- Computer-controlled data acquisition and analyses
Electrical and Electrochemical Measurement Facility in
There are several laboratories in CISM that support the development of solid-state electrochemical devices such as sensors and fuel cells. These facilities include thick film fabrication by screen printing and spin coating, a wide range of electrical (dc and ac) measurement equipment, a set-up suitable for photo-catalytic studies, several sensor measurement and testing set-ups with the capability for controlled gas flow and mixing systems, computer-controlled data acquisition and analyses with specially written software, and a GC-MS for the analysis of gas-solid reaction.
Particle Size, Pore Size and Sorption Analysis Facility
Under an NSF-IGERT grant, CISM has set up a facility for particle size (Brookhaven 90 Plus with a high sensitivity APD detector and zeta potential option), pore size (Autopore IV 9500, Micromeretics), and sorption analysis for surface area (ASAP 2020, Micromeretics).
Thin-Film and Metallization Facility
As part of CISM, there is a multi-cathode dc/rf magnetron sputtering unit (Discovery 18 by Denton Vacuum) for thin-film research, a benchtop sputtering unit for electrode preparation, a surface profilometer for roughness and morphology, and a benchtop tape casting unit for planar sensors, electrodes and substrates.
A recently added facility includes a Neocera Pioneer 180 pulsed laser deposition system with six targets, a turbo pump capable of achieving < 10-8 torr, and the capability of substrate heating of up to 850°C.
Chemical Sensors Design and Testing
The Wright Center for Sensor Systems Engineering--an initiative established through a technology-based economic development program called Ohio Third Frontier-- provided funding to renovate an MSE laboratory used to design and test the next generation of chemical sensors. The lab's new state-of-the art capabilities and equipment include:
Sensor Testing Facility
- Sierra Smart Track2 Mass Flow Controllers with Command Module
- National Instruments Data Acquisition Systems with 32 Channel Multiplex Capabilities
- Lindberg/Blue Mini-Mite Tube Furnaces with Computer Control Capabilities
- Solartron Impedance Analyzer with High Dielectric Test Cell
- Precision Ferroelectric Testing Facility with Thermal Chuck
- Fast Response Oxygen Sensor
- Humidity Detector
Sensor Fabrication Equipment
- High Energy Ball Mill
- 1700°C Box Furnace
- 1500°C Tube Furnace
- 1500°C Box Furnace
- Mass Balance with Density Measurement
- Press Dies
- Table-top screen-printer
DC/RF Magnetron Sputter Deposition System for Thin-Film
- Pressure Sensor
- Computer Upgrade
- Heated Stage
- Water Chiller
- Cold Water Manifold
- Cathodes and Targets
The MSE Solidification and Metal Casting Laboratories include a 2,500-square-foot high bay Metal Casting Laboratory and a Solidification Laboratory.
The Metal Casting Laboratory is served by a five-ton crane system. The melting facilities include a 60kW Inductotherm electric induction generator with a lift-swing 40lb aluminum furnace as well as a 25kW electric induction furnace with a vacuum/inert-gas melting chamber. A cooling curve analysis system and an Electronite oxygen probe for ferrous alloys are also available. The sand preparation equipment consists of a muller for green sand.
The Solidification Laboratory is situated on the first floor in the Fontana building. The main equipment includes a free flight melt spinning system for the continuous casting of wire, a transparent organic metal analog directional solidification system for in-situ observation of solidification, a Mellon zone melting furnace, and an SR2 Prometal rapid casting system (rapid prototyping machine for making molds). In addition, casting simulation software is available. It consists of Magmasoft mold filling / solidification software and Ironcad solid modeling software.
The Laboratories for Applied Superconductivity and Magnetism (LASM) in Ohio State’s Department of Materials Science and Engineering is well equipped to perform superconductor property measurement and superconductor materials characterization. Equipment for materials studies, such as XRD and electron microscopy, is housed in the Campus Electron Optics Facility. The electromagnetic test stands are located in the LASM laboratories.
Magnetization may be measured by vibrating sample magnetometry (VSM) in three test stands:
- Low Field VSM-I, a LDJ Model 9300 instrument with a 1 T iron-core electromagnet
- Low Field VSM-II consisting of a PAR EG&G Model 4500 VSM associated with Janis Varitemp dewars (both liquid helium and liquid nitrogen) and an iron-core electromagnet energized to ? 1.7 T by a Tidewater ? 65A power supply
- High Field VSM consisting of a PAR EG&G Model 4500 VSM associated with an Oxford cryostat that houses a 6.4 cm (cold bore) 9 T superconducting solenoid
Transport Measurement in Magnetic Fields
- High-Current High-Field Jc Measurement is conducted with currents of up to 1,700 A provided by a stack of three HP6681A (0-8V, 0-580A) power supplies in the field of an Oxford hybrid NbTi/Nb3Sn solenoid excited by an Oxford Model PS120-10 magnet power supply. The maximum field available is 15 T at 4.2 K and 17 T at 2.2 K. A high-current probe is being used with a soldered ITER barrel mounting procedure and monitored contact resistances.
- Temperature Dependent Jc is measured at currents of up to 220 A in an exchange-gas can that is inserted into the bore of the above Oxford solenoid.
- Resistive Critical Field (Hirr and Hc2) measurements are made at currents of about 10 mA in a dedicated exchange-gas can that also can be positioned in the bore of the Oxford solenoid.
All instruments are computer controlled with programs written in LabView. An extensive inventory of ancillary equipment is available and includes amplifiers, multimeters, gaussmeters, a metallographic microscope, and numerous computers and work stations.
Transport Measurements of the Self-Field Critical Current
of Large Devices
Available for the measurement of self-field critical current in a large coils can is a large open-mouth dewar from Cryofab Inc. This has an inside diameter of 25 inches (635 mm) and a working height (below an 18-inch, 460mm thick plug) of 35 inches (890 mm). Measurements are made as function of temperature above 4 K as the internal structures slowly warm up. Self-field is monitored with a Hall probe.
AC Loss Measurement
Two test stands are housed in a laboratory dedicated to AC loss measurement:
- Self-Field (Transport-Current) Loss due to AC currents of up to 150 A (peak) at frequencies of up to 500 Hz is measured at 77 K (liquid nitrogen). A lock-up amplifier measures the voltage of the sample in-phase with transport current.
- External-Field AC Loss is measured in the applied fields of copper wound solenoids and race-track coils of various sizes. A system of pick-up coils connected to a digital oscilloscope records the samples' M-H loops whose areas provide a measurement of the loss per cycle.
Additional Cryogenic Test Equipment
- Physical Property Measurement System. A Quantum Design PPMS allows measurements from 4 K to room temperature in fields up to 15 T of: (a) magnetization using vibrating sample magnetometry, (b) heat capacity (c) AC and DC susceptibility (d) AC transport, and (e) thermal conductivity.
- Large Coil Test Stand. This consists of an insulated vacuum vessel 48 inches (1200 mm) in diameter and 25 inches (630 mm) high from Cryomagnetics cooled by two Gifford-McMahon cryocoolers, each capable of extracting 5 W at 10 K (1.5 W, 4 K). The system accomplishes the rapid cooling of large objects into the He-temperature range.
- Room Temperature Bore Cryocooled Magnet. This cryocooled magnet with a field of 9 T in a 60 mm diameter room temperature bore is capable of accepting a furnace for magnetic field processing or a varitemp (presently on hand) for property measurement as function of field and temperature.
Instrumentation used to study materials at elevated temperatures is housed in the state-of-the-art Patrick K. Gallagher Thermal Analysis Center. The Center is equipped with the following computer-controlled analytical systems:
- Differential scanning calorimeters
- Thermogravimetric analyzer capable of temperatures reaching 1350°C
- Dilatometer capable of reaching 1200°C
Within Ohio State’s Department of Materials Science and Engineering (MSE) , thin film growth facilities are on-site for research on epitaxy, interfacial structure, and growth of novel materials. Ultra-high vacuum and high-vacuum vapor deposition systems and a magnetron sputtering system are among the tools available to researchers. Additional processing can be done in associated facilities for rapid and conventional thermal annealing. Thin films are characterized in MSE’s x-ray diffraction and electron optics facilities as well as in central Ohio State facilities for surface analysis.
Thin-Film and Metallization Facility
- A multi-cathode dc/rf magnetron sputtering unit (Discovery 18 by Denton Vacuum)
- A benchtop sputtering unit for electrode preparation
- A surface profilometer for roughness and morphology
- A benchtop tape casting unit for planar sensors, electrodes and substrates