Equipment

GC-MS

A gas chromatograph (Agilent 7890B) equipped with thermal conductivity detector (TCD) and mass spectrometer detector (GC-MS) is used to analyze the real time composition of the synthesis gases in the floating catalyst chemical vapor deposition (FCCVD) furnaces, where the carbon nanotubes growth occurs. The GC-MS allows to get insights on the process chemical kinetics and to identify the most relevant species that dominate the CNTs growth.

Contact person: Eldar Khabushev

 

FTIR Absorption Spectrometer

A custom-made Fourier Transform InfraRed (FTIR,) gas flow cell (Interspec 301-X) is used to analyze the real time composition of the synthesis gases in the FCCVD furnaces. Also in this case, the gas detector is used to get insights on the process chemical kinetics and to identify the most relevant species that dominate the CNTs growth, particularly IR-active gases as methane and olefins.

Contact person: Eldar Khabushev

 

UV-Vis Absorption Spectrophotometer

A UV-Vis spectrophotometer (Shimadzu UV-1800) is used to analyze the concentration of of chemical species in liquid solutions or the thickness of CNT/BNNT films, utilizing the Beer-Lambert’s law.

Contact person: Lily Gong

 

Scanning Mobility Particle Sizer

The Scanning Mobility Particle Sizer (SMPS, TSI) is used to analyze the characteristics (size distribution, mass distribution, concentration) of aerosols as the iron nanoparticles aerosol obtained inside the FCCVD furnaces. The SMPS combines a condensation particle counter (CPC), with a nano-enhancer and differential mobility analyzer (DMA) to study aerosols with particles in the range between 1 nm and 50 nm. That is very small!

Contact person: Jui Junnarkar

 

High Temperature FCCVD Furnaces

At the heart of CNT synthesis research are the FCCVD tube furnaces. Available in both vertical and horizontal configurations, these furnaces can reach temperatures of 1250–1300 °C, creating the ideal reaction environment for growing CNTs from natural gas.

Contact person: Eldar Khabushev, AnaVi Benavides Figueroa, Lily Gong, Jui Junnarkar, Davide Cavuto

 

High Temperature Tube Furnaces and Box Furnaces

The high temperature furnaces are used for conducting high temperature processing (annealing, purification, doping) of carbon and boron nitride based nanomaterials under controlled atmosphere conditions. Temperatures up to 1200°C are achievable with both oxidant and inert environments. A water bubbler is also available for providing a steam-rich environment.

Contact person: Davide Cavuto

 

Microscopes

Nikon Eclipse E600 is a high-end upright research-grade microscope for brightfield, polarization and epi-fluorescence imaging. The microscope is equipped with a mercury lamp, filter cubes (XF-100-2 and XF 37 Omega Filters), 10X, 20X, 60X (oil) and 100X (oil) objectives and a Prior Proscan motorized stage.

Contact person: Joe Khoury & Michelle Duran-Chaves

The Axiplan 2 polarized optical microscope has been designed as a universal microscope and can be used for many areas of light microscopy. The microscope is equipped with a heating and cooling stage, a polarizer and an analyzer, and 10X, 20X, and 50X objectives. The optovar attachment allows for 2.5X false magnification. The Axioplan 2 microscope can be used in transmission (brightfield), reflection (darkfield or brightfield or fluorescence) with or without polarized light. Please see the manual for more information. Please go to FOM to request training for the microscope.

Contact person: Joe Khoury & Michelle Duran-Chaves

The Zeiss Axioplan 2 is a high-end upright research-grade microscope for transmitted and reflected (brightfield, darkfield, and fluorescence) applications. It has a high resolution digital camera and a medium resolution color camera, a rotational stage with controlled capabilities to provide Z-stack analysis, and image processing software. It has a polarizer for both the transmitted and reflected light sources with a rotatable analyzer. It is capable of differential interference contrast (DIC) imaging. It is equipped with 4 objectives: 10X, 20X, 50X and an oil immersion (1.4 NA) 63X, with capabilities of up to 2.5X false magnification.

Contact person: Michelle Duran-Chaves

 

Cameras

Hamamatsu

Hamamatsu EB-CCD camera (type C7190-21) is a high-end video-rate camera for high gain, high resolution image acquisition in very low light. The camera is connected to a camera controller with sensitivity control and contrast enhancement capabilities and is controlled by Metamorph imaging software.

Contact person: Michelle Duran-Chaves

Kodak Ektapro model 1000HRC Motion Analyzer

This is a high speed camera that can be used either with an attached lens or by being mounted on a microscope. The camera can capture videos with frame exposure times as short as 50 microseconds, allowing observation of processes on very short time scales.

Contact person: Michelle Duran Chaves

 

Rheometers

ARES (Advanced Rheometric Expansion System) This rheometer was manufactured by Rheometric Scientific Inc., which is currently owned by TA Instruments. A direct-drive motor places a strain on the sample and an air bearing precision transducer then measures the stress. The rheometer has two transducers with a minimum torque of 2×10-7 N·m. It is a strain-controlled rheometer. It is equipped with a Neslab RTE-130 temperature control system. We have a special acid shield and fume system to create a dry, isolated environment for the rheometer to make measurements on SWNT/superacid mixtures.

Contact person: Joe Khoury

RDA III

The RDA III (Rheometric Dynamic Analyzer) is a controlled strain rheometer dedicated to high viscosity fluids and solids testing instead rotational and dynamic shear. With it’s durable ball bearing torque transducer, the product allows analysis of materials such as polymers, baby foods, inks, pharmaceutical gels, liquid crystals, crude oils, nd more solid-like materials. With a controlled temperature range of 25-50C, it is ideal for analyzing polymer melts and thermotropic liquid crystalline phase transitions. Parallel plates (25 mm and 40 mm) and Cone and Plate (25 mm and 40 mm) fixtures are available.

Contact person: Joe Khoury

Capillary Thinning Equipment

Contact person: Joe Khoury & Lily Gong

 

Fluid Processing Equipment

Two Flactek Speedmixers provide high speed, efficient mixing and compounding for liquid solutions, dispersions, and emulsions over a wide range of viscosities. The large Speedmixer (model DAC 600.1 FVZ) is capable of mixing samples (including container) of up to 600g at 2500rpm or less for 100 minutes. It includes the ability to create custom mixing programs for multi-stage mixing. The small Speedixer (model DAC 150.1 FVZ-K) is capable of mixing samples (including container) of up to 150g at speeds reaching 3500rpm for up to 5 minutes. Both utilize Flacktek’s Dual Asymmetric Centrifugal Mixing technology, which is a bladeless mixing technique that produces repeatable, bubble-free mixtures with high precision, repeatability, and speed.

Contact person: Michelle Duran Chaves 

 

Fiber Spinning Equipment

After mixing high-concentration CNT/superacid solutions, or “dopes”, these solutions are extruded through an air gap into a “coagulant” bath. In the air gap, the dope undergoes tensions, which further aligns the liquid crystalline CNT solution. In the coagulation bath, the acid is removed, and the CNTs coagulate to form a solid, aligned, neat fiber. Our group has a unique experimental setup for carrying out this extrusion process; syringe pumps are used to extrude the dope from the mixing vessel, and we have a  two-level arrangement where the dope is extruded downward from the first level through the air gap into the coagulation bath on the adjustable second level.

Contact person: Michelle Duran-Chaves

 

DrawDown Rod Coating

The Gardco Automatic Drawdown Machine is a benchtop device for draw down sample coatings with a high degree of reproducibility. With the Gardco Automatic Drawdown Machine the operator can get consistent, precision coating drawdowns every time. It can be use all different types of applicators–Microm applicators, Bird type, Wire wound rods, etc. The instrument can do coating with a speed range of 1.0 to 18.0 inches per second (IpS), in 0.1 inch/sec increments. There are four preset stroke lengths of 6, 9, 12 and 16 inches. The standard working surface is a 12 X 18 inch glass plate. An optional 12 X 18 inch vacuum plate can be used in place of the glass plate to accommodate different size paint charts. Standard 16″ OA Lab rods of either 1/2 or 3/8″ diameter can be used. The high temperature process furnace is used for conduction high temperature anneals of carbon and boron nitride based nanomaterials under controlled atmosphere conditions. Temperatures up to 1200C are available with an oxygen or nitrogen rich environment. A water bubbler is available for providing a steam-rich environment.

Contact person: Michelle Duran Chaves 

 

Microbalances

The Citizen CM 21X microbalance is capable of microgram-resolution mass measurements. The sample is loaded onto a plate within a closed chamber to prevent disturbances from air currents. The microbalance features hands-free chamber door operation and automatic temperature monitoring. It is typically used to obtain precise mass measurements for small amounts of carbon nanotubes or macroscopic materials composed of carbon nanotubes.

Contact person:  Michelle Duran-Chaves

 

Gamry Reference 600 Potentiostat

The reference 600 is a potentiostate/galvanostat/ZRA. It is used for a variety of applications in physical electrochemistry, including fast cyclic voltammetry, impedance measurements, electrochemical corrosion, etc.

Contact person: Aosheen Anand

 

Sorvall Legend X1 Centrifuge

The Sorvall Legend X1 Centrifuge is capable of rotating up to 6 by 100ml samples at 15000rpm tp produce an acceleration of approximately 24630g. It is used for nanotube phase separation and removal of sediment from aqueous dispersions.

Contact person: Joe Khoury

 

Freeze Drying Equipment

Free drying allows removal of water from a material without compromising the structure. The material is first frozen with liquid nitrogen, ten the sample vial is connected to the dryer, which reduces the surrounding pressure to allow the frozen water in the material to sublimate directly from the solid phase to the gas phase. The Millrock benchtop freeze dryer lowers the temperature of the sample up to -45 degrees C and is equipped with a manifold to allow up to 6 samples to be dried at a time.

Contact person: Aosheen Anand & Yang Lu

 

TEM, SEM, TGA, Raman Microscope, XPS

TEM, SEM, TGA, Raman Microscope and XPS equipments are used on a daily basis to characterize CNT materials. Access to this equipment is provided by the Rice Shared Equipment Authority (SEA).

Access the Rice SEA: http://sea.rice.edu/