These three instruments run off the same TA60WS controller and can be operated simultaneously. There is also a FC-60A gas flow controller for experiments to be done under N₂, Argon or O₂ atmosphere. These three complimentary techniques allow us to study melting points, decompositions, phase transitions, glass transitions and weight losses as a function of temperature under various atmospheres. This information helps us design our synthetic experiments to best prepare the new materials in pure form and to design crystal growth experiments.

A new MBraun LabMaster 130 double glove box with a single filter column gas purification system shown below is used for the manipulation of air-sensitive and moisture-sensitive products and starting materials. The glovebox is equipped with a CCD camera, Optem 1:10 zoom, with a color video monitor. With the use of a switch box the image can be transferred from the video monitor over to a PC where it can be saved for future reference or printed out for pasting into laboratory notebooks.

Our Cary5000 UV/Vis/NIR spectrometer from Varian (shown below) is used to study the optical properties of our new materials. From diffuse reflectance measurements we estimate the band gap energies of our new semiconductor compounds.

For diffuse reflectance we use the Praying Mantis attachment from Harrick Scientific (shown below).

It incorporates two 6:1, 90° off-axis ellipsoids, which form a highly efficient, diffuse reflection illumination and collection system. This unique configuration deflects the specular reflectance away from the collecting ellipsoid, minimizing the associated spectral distortions. This attachment is also used with a rear beam attenuator. We also have an ambient sample chamber to go inside the praying mantis. This chamber allow us to prepare our air-sensitive materials for measurement inside our glovebox, seal them up in the chamber, and bring them out of the box to take measurements. The praying mantis is better than an integrating sphere for our work. One reason is because you can use much less sample and you can recover the sample after the measurement. Another reason is that it is not wavelength limiting. The Praying Mantis allows us access to the entire UV/Vis/NIR range. We can also pop the attachment out of the Cary 5000 and insert it into almost any FT-IR instrument. For measurements in the mid-IR range we are using the new Nexus 470 FT-IR by Thermo in the lab of Dr. Ellen Gawalt down the hall.

Most of our reactions are carried out in sealed tubes under vacuum. The tubes are made of either Pyrex or Fused-Silica depending on the reaction temperature used. We use a Natural gas/O₂ flame to make the reactions tubes. The tubes are loaded with the solid reactants in the inert atmosphere glovebox under Argon. The tubes are then removed from the box and attached to this high vacuum line, shown below. The line is evacuated by an Edwards pumping system, which consists of an RV5 backing pump and an E050/60 air-cooled diffusion pump. An Edwards wide range gauge reads from atmospheric pressures all the way down to 5 x 10^-9 mbar. In most cases we can usually get the line to pump down into the 10^-5 range.

We have a Precision Thelco mechanical convection oven (below) with a maximum temperature of 250° C. It is controlled by a microprocessor temperature control so that no one needs to be in the lab to shut it off when a reaction is finished.

We also have a Venticell oven by Grieve (left below) for the same purpose. These ovens are used for the heating of our solvothermal reactions. Each reaction is contained in PTFE cup, which is inserted into a Parr 23 ml acid digestion bomb. A Scientific Products vacuum oven (right below) with a maximum temperature of 225° C is used to dry samples under vacuum. Samples that are dried under vacuum are usually those obtained via solution chemistry. The oven is evacuated by an Edwards RV3 vacuum pump and is capable of holding a vacuum of 30 inches of Hg.

What is a solid-state inorganic lab without high-temperature furnaces? We currently have four hinged tube furnaces in our laboratory. The three minimites by Lindberg have a maximum temperature of 1100 °C and can fit about 4 reactions tubes per run (shown on the right below). A large Thermolyne furnace has a maximum temperature of 1200 °C and can fit up to 20 reactions at once (left below). We also have the use of a furnace capable of reaching 1700 °C over in the lab of our collaborator, Monica Sorescu, in the Physics Department at Duquesne.

We are currently in the process of designing our own furnaces, which we will assemble next year with the help of our competent instrument shop personnel who are specialists in the area of electronics.
Our supply of Pyrex and Fused-Silica used to make reaction tubes is stored in this professional glassblowers supply cabinet. The cabinet is nearly full with several different sizes of tubing including 8mm, 9mm, 11mm and 12 mm OD. We have several different sized Swagelock adapters to attach these sizes of tubing to the high-vacuum line.

The larger of our two laboratories has been completely renovated (see photo below) with new casework and a new fume hood. The smaller laboratory is equipped with two more fume hoods.

Powder X-ray diffraction measurements are performed on our Rigaku DmaxB powder X-ray diffractometer using Cu Ka radiation. An automatic sample changer allows us to do up to 25 samples in sequence. The instrument is located in the Bayer Learning Center and is available free of charge to all researchers at Duquesne University.

Currently single crystal X-ray diffraction experiments are performed on our Rigaku AFC7R rotating anode X-ray diffractometer that is equipped a Mo Ka radiation.

Recently our department has been awarded an NSF-CRIF grant to obtain a new diffractometer with a CCD area detector. The instrument will be used first and foremost for elucidation of new crystal structures involved in Duquesne University research projects; however, it will be also used as tool for teaching X-ray crystallography. Several area colleges have expressed interest in becoming involved with our "teaching and learning center for X-ray diffraction". We hope to provide remote access to the instrumentation so that students from other universities can collect data on their samples without actually traveling to Duquesne University. In addition, we hope to get more Duquesne students interested in X-ray diffraction by developing a skills course in X-ray diffraction techniques.

Magnetic measurements are performed in the laboratory of our collaborator, Monica Sorescu, using a susceptometer-magnetometer system with a 3 Tesla superconducting magnet and liquid helium cryostat for dc hysteresis loops and ac susceptibility measurements (shown below). We are using this measurement system to study our diluted magnetic semiconductors based on diamond-like semiconductors.