Suib Lab has three Powder X-Ray Diffractometers in-house: A Scintag model XDS 1000, a Thermo-ARL X’TRA, and a Rigaku Ultima IV system, all running Cu K-alpha x-ray emitter tubes. The Thermo-ARL is equipped with an Anton-Parr XRK-900 In-Situ reactor chamber capable of vacuum operation at 10E-5 Torr, Pressurization at 10 Bar, and thermal control to 900°C.
Above from Top Left: Scintag XDS 1000, Rigaku Ultima IV, Thermo ARL X’TRA, ARL X’TRA showing Anton-Parr XRK-900, XRK-900 Sample Mount of Copper Thin Film on Quartz
Cyclic Voltammetry (CV)
Electrochemical properties of materials are analyzed with a BAS Model 100B/W instrument. This instrument is capable of measuring current as a function of applied potential for cyclic voltammetry (CV) studies. The software is equipped with pulse, square wave, and stripping techniques.
The Micromeritics ASAP 2010 system is equipped with an optional molecular diffusion pump, a chemisortion system, and a density functional theory (DFT) software package. It can be used to measure surface area, pore volume, mesopore and micropore size distribution, adsorbate-adsorbent interaction energy (physisorption ), and dispersion and partricle size of supported metals (chemisorption).
The Quantochrome Autosorb iQ2 is a highly sophisticated gas sorption analyzer available with two physisorption analysis ports and provides an easy upgrade path to high vacuum, low pressure and chemisorption capabilities.
Above Left: Micromeritics ASAP 2010, Above: Quantochrome autosorb iQ2 is a highly sophisticated gas sorption analyzer available with two physisorption analysis ports and provides an easy upgrade path to high vacuum, low pressure and chemisorption capabilities.
Auger spectra are acquired using a Physical Electronics PHI 610 Scanning Auger Microprobe. Auger depth profile spectra can be acquired while sputtering the specimen with Ar+ ions.
The laboratory uses XPS to study various materials and coatings. Photoemission (XPS) data are aquired using a Leybold-Heraeus LHS modified with a SPECS EA 10MCD energy analyzer. The instrument is equipped with a dual X-ray anode for exciting photoemmision with either Mg K a or Al K a radiation.
The lab uses a Shimadzu UV 2450 is equipped with a single monochromatic system. The low stray light, wide dynamic range, small beam size combination makes this instrument well suited to handle a variety of practical situations. The UV-Vis is capable of transmittance and reflectance studies.
FT/IR, ATR, Raman, Spectroscopy
The Nicolet 8700 offers a full range of step-scan operation modes, dual-channel internal digitizers, extended spectral range, and flexible inputs and status signals for interfacing the Nicolet 8700, as we have done with the Nicolet NXR FT-Raman spectrometer attachment, which combines exceptionally high performance with a wide range of sample accessories to create a system that is capable of running everything from bulk samples to microscopic samples. A Ventacon Catalysis Evaluation Cell is also available for in-situ gas phase measurements up to 300 Celsius. The Lab also has an iD3 ATR accessory, ideal for many samples including solids, liquids, pastes, and gels. Two crystal types are available including zinc selenide (ZnSe) and germanium (Ge).
The Mass Spectrometer System is a mobile vacuum pumping station designed to be used in conjunction with MKS Residual Gas Analyzer. Quadrupole Mass Spectrometry is an efficient method of process gas analysis. The quadrupole sensor allows detection of distinct constituents in the gas environment. This system is connected to a resistively heated tube furnace controlled by a Watlow F4 Programmable PID controller for analysis in the range of 25-815°C. Familiar techniques for utilization of this system include
Temperature Programmed Reduction/Oxidation
Thermally Programmed Desorption
Ammonia Adsorption (Pulse Dosing)
Gas Phase Reaction Evaluation
The laboratory uses a series of gas-phase fixed bed reactors to evaluate materials for catalytic activities, adsorption capacities, material stabilities and a host of other properties.
System 1 consists of a pair of Alicat MFC’s (50 sscm N2) for pulse dosing a reactor held in a Thermo-Fisher single-step controlled clamshell furnace with 1” Tube capability. The effluent gas is analyzed by an SRI 8610c Gas Chromatograph with a TCD detector (Carrier gas He or N2).
System 2 consists of a trio of Brooks MFC’s (200 sscm) connected to a reactor in a 6” furnace with 1” Tube capability controlled by a Watlow F4 Programmable controller. The effluent gas is analyzed by an SRI 8610c Gas Chromatograph with a TCD detector and Helium Ionization Detector (HID) for analysis of hydrogen using a helium carrier gas.
System 3 consists of a series of Alicat MFC’s (50sscm N2) connected to a quartz U-tube held in an oven. The effluent gas is analyzed with an SRI 8610c Gas Chromatograph with a Flame-Photometric Detector (FPD) optimized for H2S analysis. Systems 1 & 2 are routinely adapted for analyses including carriers through bubblers, plate reactors for photo-catalysis, adsorption experiments, etc.
Liquid Phase Reaction Evaluation
The lab maintains an HP 6890 GC-MSD Gas chromatrograph system with an autosampler tray, running Chemstation control software. A direct 10 uL injection port is also configured on the instrument. The lab also has two 5890 GC-TCD insturuments with flow-over injection ports, though these are not in service.
Thin Film Fabrication Facilities
The Savannah 100 Atomic Layer Deposition allows growth of thin films, atomic layer by layer either in continuous or pulse deposition modes. The reactor is a 304 Stainless bed reactor optimized for 4” silicon wafers with a max T of 450C and fed with five heated precursor delivery lines and one unheated (water vapor delivery). A vacuum pump allows for pressure control down to 10E-4 Torr. The laboratory also maintains two glove boxes for sensitive precursor filling (Trimethylaluminum, Titanium Tri-isopropoxide).
Above from Left, Savannah S100 Control Screen, Denton Benchtop Turbo PVD
The Denton Bench-Top Turbo (BTT) allows Physical Vapor Deposition (PVD) via resistive heating of metallic precursors. The system is equipped with a turbopump for vacuum control down to 10E-6 Torr, Pneumatic Shutter for Deposition Control of two resistive heaters, a 2kVA power supply, horizontal rotation stage and an Inficon In-Situ QCM for film thickness monitoring.
Electrochemical and Battery Studies
The laboratory is equipped with three in-house Galvano/Potentiostats: a Basi 100W Electroanalytical Workstation, and two Gamry REF600 Electrochemical Analyzers/ Zero Resistance Ammeters. Each system is configures to +/- 10V, 1 A Current Maximum, and is capable of cyclic, step, and sweep voltammetry, chronoamperometry, and most DC techniques. The Gamry Ref600 systems are also equipped with Electrical Impedance Spectroscopy (EIS) for battery and corrosion studies. The lab also has a MTI BTS-8 Battery Testing Station with 8 channels (0.001-1 mA/channel) for coin cell evaluation of CR2032 cells which can be fabricated in house.
Above from left: Three-electrode setup for evaluation of Lithium intercalation materials for non-aqueous battery systems. MBraun Glove box containing MTI CR2032 Coin Cell press for fabrication of half-cells and spectroelectrochemical cells.
The ceramics laboratory is fully equipped with a large amount of hood space dedicated to sol-gel synthesis and CVD research. This facility utilizes both CVD and sol-gel methods for various coating applications. The furnaces used in the CVD applications range dramatically in size from the small 1 inch diameter furnaces used in test reactions to the large 12 inch diameter furnaces used in scale-up processes. Both oxide and non oxide interface and environmental barrier coatings coatings are applied in reactors with high temperature capabilities (up to 1000°C) and extensive work in pre-ceramic polymers for use in ceramic matrix composites is performed.
Non oxide coatings (including boron nitride, carbon, silicon carbide, and silicon nitride) and oxide coatings (including alumina, zinc oxide, titanium dioxide, and silicon dioxide) have been deposited on substrates including ceramic fibers, metal sheets, and silicon and ceramic powders.
Above: Left: 12” I.D. Low-Pressure Chemical Vapor Deposition Reactor. Right: An inert-atmosphere setup for synthesis of a Pre-ceramic polymer (PCP).
SEM / EDXS
An Amray model 1810 scanning electron microscope is located inside the facility. The microscope shows surface images up to several thousand times magnification. An additional feature is the ability to determine elemental composition with the attached EDAX apparatus.
AFM / STM
Our SPM is a MultiMode scanning probe microscope. The MM-SPM is designed around a stationary probe (i.e. samples are scanned back and forth beneath the probe). It uses Nanoscope version 4.x. Digital Instruments software that has divided its SPM software into a two-function architecture: Real Time and Off-line.
The MultiMode-SPM can scan up to 200 mm laterally and 10 mm vertically. The MM-SPM is a multi mode instrument that includes Atomic Force Microscopy (AFM): contact, tapping-mode, and non-contact; Phase-Imaging; Magnetic Force Microscope (MFM); Electric Force Microscope (EFM); Surface Potential Microscopy; LiftMode; Force Modulation; Lateral Force Microscopy (LFM); Scanning Tunneling Microscopy (STM); Electrochemical Microscopy (ECSTM and ECAFM); and Lithography.
The MultiMode utilizes a Nanoscope IIIa Controller having a digital signal processor (DSP) with a 20 MHz peak rate for arithmetic operations. The MM-SPM is equipped with four auxiliary digital-to-analog converters (DACs). Three DACs have +10V outputs, and one DAC has a +12V and +220V outputs; all four channels have 16-bit resolution. In addition, there are two +10V analog-to-digital converters (ADCs) having 14-bit resolution and software selectable filters. One ADC has four-way multiplexing.
TGA / DSC
Thermal analysis of solids, liquid and powder samples can be carried out using the Dupont 951 Thermogravimetric Analyzer (TGA) and Dupont 910 Differential Scanning Calorimeter (DSC). These instruments are equipped with a Temperature Programmer Interface (TPI) TA Controller System. TGA can be used to measure the weight chanege of a sample with temperature while DSC measures temperature and heat flow associated with material transition providing data on endothermic (heat absorption) and exothermic (heat evolution) processes.
Microwaves (MW) are very efficient at heating many materials and removing water or other liquids from products. This technique allows researchers to obtain materials with unique characteristics in very short times. Our group is equiped with different microwaves ovens.
Top left ,(a) Biotage Initiator (60-250 °C, 0-20 bar, 0-300 W, 0-900 rpm, 2.45 GHz, single mode); top right, (b) Astex power source Model GL139 (0-1250 W, 2 .45GHz); bottom left, (c) Wavemat Model CMPR TM250 (0-1250 W, 2.45 GHz); bottom middle, (d) Variable Frequency Microwave Furnace Model LT 502Xb (0-500 W, 2.4-7.0 GHz); bottom right, (e) CEM MARS 5 Microwave - Accelerated Reaction System (0-1200 W, 2.45 GHz)
Mass Spectrometer System is a mobile vacuum pumping station designed to be used in conjunction with a Type PPT Residual Gas Analyzer. The PPT (Partial Pressure Transducer) utilizes Quadrupole Mass Analyzer technology. Quadropole Mass Spectrometry is an efficient method of process gas analysis. PPT quadrupole sensor allows detection of distinct constituents in the gas environment. The Electronic Control Unit, interactive software, and quadrupole sensor combine to provide the speed, resolution, and sensitivity required for partial pressure sensing.