Graphite exfoliation by supercritical carbon dioxide extraction

Supercritical carbon dioxide is used to exfoliate graphite, producing a small, several-layer graphitic flake. The supercritical conditions of 2000, 2500, and 3000 psi and temperatures of 40°, 50°, and 60°C, have been used to study the effect of critical density on the sizes and zeta potentials of the treated flakes. Photon Correlation Spectroscopy (PCS), Brunauer-Emmett-Teller (BET) surface area measurement, field emission scanning electron microscopy (FE-SEM), and atomic force microscopy (AFM) are used to observe the features of the flakes. N-methyl-2-pyrrolidinone (NMP), dimethylformamide (DMF), and isopropanol are used as co-solvents to enhance the supercritical carbon dioxide treatment. As a result, the PCS results show that the flakes obtained from high critical density treatment (low temperature and high pressure) are more stable due to more negative charges of zeta potential, but have smaller sizes than those from low critical density (high temperature and low pressure). However, when an additional 1-hour sonication is applied, the size of the flakes from low critical density treatment becomes smaller than those from high critical density treatment. This is probably due to more CO2 molecules stacked between the layers of the graphitic flakes. The zeta potentials of the sonicated samples were slightly more negative than nonsonicated samples. NMP and DMF co-solvents maintain stability and prevented reaggregation of the flakes better than isopropanol. The flakes tend to be larger and more stable as the treatment time increases since larger flat area of graphite is exfoliated. In these experiments, the temperature has more impact on the flakes than pressure. The BET surface area resultsshow that CO2 penetrates the graphite layers more than N2. Moreover, the negative surface area of the treated graphite indicates that the CO2 molecules may be adsorbed between the graphite layers during supercritical treatment. The FE-SEM and AFM images show that the flakes have various shapes and sizes. The effects of surfactants can be observed on the FE-SEM images of the samples in one percent by weight solution of SDBS in water since the sodium dodecylbenzene sulfonate (SDBS) residue covers all of the remaining flakes. The AFM images show that the vertical thickness of the graphitic flakes can ranges from several nanometers (less than ten layers thick), to more than a hundred nanometers. In conclusion, supercritical carbon dioxide treatment is a promising step compared to mechanical and chemical exfoliation techniques in the large scale production of thin graphitic flake, breaking down the graphite flakes into flakes only a fewer graphene layers thick.

Analysis of a Non-Traditional Micro Tube Hydroforming Process

As the demand for miniature products and components continues to increase, the need for manufacturing processes to provide these products and components has also increased. To meet this need, successful macroscale processes are being scaled down and applied at the microscale. Unfortunately, many challenges have been experienced when directly scaling down macro processes. Initially, frictional effects were believed to be the largest challenge encountered. However, in recent studies it has been found that the greatest challenge encountered has been with size effects. Size effect is a broad term that largely refers to the thickness of the material being formed and how this thickness directly affects the product dimensions and manufacturability. At the microscale, the thickness becomes critical due to the reduced number of grains. When surface contact between the forming tools and the material blanks occur at the macroscale, there is enough material (hundreds of layers of material grains) across the blank thickness to compensate for material flow and the effect of grain orientation. At the microscale, there may be under 10 grains across the blank thickness. With a decreased amount of grains across the thickness, the influence of the grain size, shape and orientation is significant. Any material defects (either natural occurring or ones that occur as a result of the material preparation) have a significant role in altering the forming potential. To date, various micro metal forming and micro materials testing equipment setups have been constructed at the Michigan Tech lab. Initially, the research focus was to create a micro deep drawing setup to potentially build micro sensor encapsulation housings. The research focus shifted to micro metal materials testing equipment setups. These include the construction and testing of the following setups: a micro mechanical bulge test, a micro sheet tension test (testing micro tensile bars), a micro strain analysis (with the use of optical lithography and chemical etching) and a micro sheet hydroforming bulge test. Recently, the focus has shifted to study a micro tube hydroforming process. The intent is to target fuel cells, medical, and sensor encapsulation applications. While the tube hydroforming process is widely understood at the macroscale, the microscale process also offers some significant challenges in terms of size effects. Current work is being conducted in applying direct current to enhance micro tube hydroforming formability. Initially, adding direct current to various metal forming operations has shown some phenomenal results. The focus of current research is to determine the validity of this process.