Atomic Engineering Laboratory

Better Materials through Better Chemistry

Facilities

Laboratory Space.   The Atomic Engineering Laboratories located in Oliver and Temple Halls.   There are tow 600 sq ft wet laboratories, one located in Oliver Hall and the other in Temple Hall.  These laboratories are designed for the synthesis of nanoparticles using mostly wet chemical methods in three separate workstations.   Each workstation is equipped with a lattice framework and custom designed inert air manifold.  One of the three workstations is equipped with 8 foot by 6 foot lattice framework for larger experimental set-up.  The laboratory also has bench top centrifuge, vacuum oven, drying oven and a Heidolph Laborota 4003 automatic rotary evaporator with continuous feed capabilities.

 

Additionally, there are 2 dry laboratories equipped with 7’ fume hood housing a 1.5” Lindberg tube furnace and small pumping station for solid state reactions.  For inert atmosphere reactions, the room houses a vacuum atmosphere glove-box which maintains a <0.5 ppm oxygen as monitored by an Illinois Instruments oxygen sensor. 

 

Major Equipment.  Magnetic Characterization: There are two instruments capable of magnetic characterization: a Lakeshore Vibrating Sample Magnetometer (VSM) and a SQUID magnetometer.   The VSM is capable of 1.2T DC magnetic fields allowing for magnetization as a function of magnetic field strength at room temperature.  For further magnetic characterization, the laboratory is equipped with a Quantum Design MPMS-5S magnetometer.  The magnetometer utilizes a newly upgraded thin-film SQUID detector and allows for measurement of magnetization as low as 10^-8 emu range as a function of temperature and magnetic field.  Temperature can be controlled from 1.7K-400K while field strength from 0 to ±5 tesla.

 

Particle Size:  Particle size is determined using a Malvern Nano-SW particle size analyzer.  This instrument utilizes dynamic light scattering principles to measure diffusion coefficients of nanoparticles moving via Brownian motion.  With viscosity and refractive index (which can be accurately measured in the laboratory) this diffusion coefficient can be converted to hydrodynamic radii.  The instrument configuration is optimized for measurement of particle size from ~2 nm to 2000 nm.

 

Parallel Synthesizer:   The Surveyor is an automated processor capable of running 10 reactions independently with complete computer control and fully automated liquid handling.  Solvents and reagents are introduced with microliter precision via the internal plumbing from 9 bottles as needed or via an autosampler needle.  Additionally the needle can introduce expensive reagents or place aliquots using 4 Gilson autosampler trays.  The instrument is fitted with a HPLC injection port allowing direct injection into coupled instruments like HPLC, DLS, or even sipper cells for XAS analysis.  The reactions vessels contain roughly 23ml volume and are kept under dynamic nitrogen atmosphere.  Temperature is controlled from -80^oC to 150^oC via attached liquid nitrogen dewers.

Major Equipment.  Available in the department of Chemistry for AEL projects:

The Department of Chemistry features a user instrumentation facility as well as several well equipped teaching laboratories.  The instrumental facility houses a Varian – Vista ICP-OES for elemental analysis and is outfitted with an autosampler.  There is a Nicolet – Nexus FT-IR with a FT-Raman Module.  This instrument has the capabilities to measure from the near to far IR.   There are additional Attenuated Total Reflectance and Diffuse Reflectance attachments which dramatically reduce sample preparation times.   The User facility features several different types of chromatography stations, including GC-MS, LC, IEC, and Sec stations.  The department also features a JEOL JSM-T300 scanning electron microscopes equipped with EDAX options allowing for elemental analysis.

 

Dr. Carpenter is the custodian of four departmental instruments; 1) A PANalytical X'Pert Pro X-ray powder diffractometer installed in Oliver Hall room 3055 which features a Cu anode source, a Scintillation detector, variable receiving and diffracting slits, 2) TAInstruments Q5000IR thermogravimetric analysizer featuring a Curie point feature and autosampler tray, and 3) TA Instruments Q200 differential Scanning Calorimeter and 4) a Varian 820-MS ICP-MS featuring a coupled LC for speciation as well as collision reaction interface for suppressionof interferants.  The  instrument is capable of ppt concentrations or ppb detection on as little as 2ml of sample.

 

Major Equipment.  Available at Virginia Commonwealth University User Facilities:

The most recent user center is the Nanomaterials Characterization Center (NCC) and the cornerstone of that center is a new ThermoFisher ESCAlab 250 X-ray photoelectron spectrometer.  The instrument utilizes multiple characterization techniques such as Ultraviolet photoelectron spectroscopy (UPS), Auger Spectroscopy, Ion Scattering Spectroscopy, depth profiling and angle resolved XPS, Scanning Auger Spectroscopy, and Scanning Electron Imaging.  The instrument is also fitted with a high pressure reaction chamber which allows for the reaction of materials and gases without exposure to atmospheric conditions.  The chemical changes on the surface as a function of temperature can be studied using the temperature controlled stage from 77K to 800K.

 

The NCC is outfitted with two Scanning electron microscopes; a Hitachi SU-70 and a JEOL 5610-LV.  The Hitachi unit is a high resolution field emission microscope capable of ultra-high resolution.  This instrument is fitted with a 6” sample introduction chamber and is fitted for scanning tunneling electron microscopy, energy-dispersive x-ray spectroscopy, and a Nabity lithography system.  The JEOL instrument is capable of variable vacuum sample chambers for use in environmental specimens.  It is also fitted with a energy-dispersive x-ray spectroscopy.  The digital camera on both microscopes allow for x-ray mapping of samples.

 

The NCC houses the first commercial VEECO IKON atomic force microscope sold in the United States.  The IKON is can operate in many different modes including magnetic force microscopy, lateral force microscopy, electrical force microscopy, and scanning tunneling microscopy.  Our instrument includes a heating and cooling stage for operation from -35oC to 250oC and a wet cell for biologically relevant samples.  The IKON has a z noise level of 35 pm and an X-Y noise level of less than 0.10 nm.