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Synthesis and Analysis of Metal Oxide-Graphene Composites

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Synthesis and Analysis of Metal Oxide-Graphene Composites 1 Synthesis and Analysis of Metal Oxide-Graphene Composites A project completed in partial fulfillment of the requirements for the Honors Program by McKenna Carey May 8th, 2021 Chemistry Ohio Dominican University Approved by Honors Project Review Committee: Dan Little, Ph.D., Project Advisor Blake Mathys, Ph.D., Reviewer Kristall Day, Ph.D., Reviewer, Honors Committee Accepted by Director, ODU Honors Program 2 Abstract There is not much research done regarding metal oxide and graphene composites. However, there have been some studies done regarding zinc oxide and graphene, and this paper delves into research done regarding tin (IV) oxide, magnesium oxide, and iron (III) oxide to add to the ever-growing body of scientific research. These metal oxides were synthesized from precursors in situ directly onto graphene. Each metal oxide and graphene composite was then analyzed using XPS, while tin (IV) oxide was analyzed using XRD as well. Due to the presence of metal to oxygen to carbon bridges, it has been shown that these composites were successfully synthesized. 3 Equipment Needed Chemicals Needed: Graphene platelets, Tin (II) Chloride, Oxalic Acid, Magnesium Carbonate, Ferrocene, Ammonium Iron (II) Sulfate, Sulfuric Acid, Magnesium Nitrate Lab Equipment Needed: Equipment Quantity Beakers (250mL) 10 Crucibles 10 Petri Dish 3 Weigh Paper Box of 100 Balance 1 Scoopula 2 Centrifuge Tubes 5 Mortar and Pestle 1 Hot Plate 1 Stir Bar 2 Instruments/Machines Needed: Instrument/Machine Name Location X-Ray Photoelectron Spectrometer (XPS) Wisconsin Powder X-Ray Diffractometer (XRD) Wisconsin Ultrasonicator Ohio Dominican University Drying Oven Ohio Dominican University Muffle Furnace Ohio Dominican University 4 Introduction Metal oxides are widely studied in the field of chemistry. More specifically the properties of these metal oxides are studied and analyzed to see if they can be applied to other fields of science. These studies often have to combine the metal oxides with another compound. The area of research that is lacking however, is when metal oxides are combined with graphene and analyzing the characteristics of this composite. There are a wide range of studies that metal oxides have been used in. There is evidence that the use of metal oxides, in the nano form, can be used to remove heavy metals from wastewater (1). Some of the metal oxides included iron (III) oxide (Fe2O3) and magnesium oxide (MgO), and these metal oxides, among others, were able to remove other metals from the water due to their high surface area and high affinity for other metals (1). Research like this could be a breakthrough in the field of renewable energy and may lead to a way to purify wastewater without causing harm to the environment, as well as other areas of science that could lead to a cleaner way to perform things necessary for our survival. Fe2O3 and MgO will be used in this research due to the research that has already shown that the physical characteristics of each have high surface areas, which could prove to be important when analyzing the data taken from this research. Fe2O3 is also a common photocatalyst due to it having a relatively narrow bandgap. In a study where tin (IV) oxide (SnO2) was combined with graphene, it was found that the composite could be used to detect gas in a room at normal temperature (2). The study also led researchers to believe that this ability to detect gas in a room was due to high graphene conductivity, a great amount of surface area, and observed interactions between the graphene and SnO2 (2). This is another example of an application of how metal oxides can impact other fields of science. SnO2 is the other metal oxide that is going to be analyzed in this study. Knowing that there are specific characteristics between graphene and SnO2 could be helpful when analyzing data of other metal oxides and graphene. There are two main chemical components in this research: metal oxides and graphene. Both compounds have chemical and physical characteristics that contribute and alter how they interact with one another: conductivity, band gap, and the physical structure. There are many types of semiconductors including metal oxides. Semiconductors are materials that have a low resistance to the flow of an electrical current so only some of the current can be conducted (3). When discussing semiconductors, there are bands that are energy 5 states where electrons can occur. The valence band would be considered the populated band with the highest energy level and the conduction band is the unpopulated band with the lowest energy level (4). However only electrons in the conduction band can move through the material. The difference in energy between the valence band and conduction band in known as the band gap (4). Band gap is considered to be the most important characteristic of a semiconductor because it has a strong influence over all of the semiconductor’s electrical properties (4). It is also important to note that the range for band gap in a semiconductor is between 0.3-3.5 eV (4). These band gaps vary between different metal oxides, as well as different semiconductors in general. When discussing band gap, semiconductors typically have a wider band gap than the band gaps of compounds that would be considered insulators, and their electrical properties can be analyzed and then applied to the field of electronics (5). Figure 1: An explanation of band gap and the energy differences (4). Ecb represents the voltage of the conduction bad, while Evb represents the voltage of the valence band. Eg represents the energy difference, or the band gap. The hv represents a photon that can be absorbed by the semiconductor. Graphene is a known conductor that is widely studied due to it having many interesting properties in regard to electricity (6). Graphene has the ability to conduct electricity because it has a lattice structure that is perfectly flat made up of carbon atoms. The electron charge is able to delocalize throughout the lattice due to the pi system which is the presence of alternating pi bonds, or double bonds, that can delocalize through the entire contiguous material (6). Graphene’s physical structure is two dimensional and has carbon rings in the form of hexagons, 6 as seen in figure 2 (7). Graphene also has a band gap with which is essentially zero, which is outside the range for a typical semiconductor (6). Figure 2: This is the structure of what graphene looks like. When discussing metal oxides there has been very little, if any, research of their properties when combined with graphene. In the research that has been done, ZnO has been the most commonly studied metal oxide and graphene combination. In many of these studies with ZnO, it has been found that there are useful electrical characteristics due to the high surface area and high conductivity when combined with graphene (8). The graphene increases the electrical activity or photocatalytic activity on the surface of the ZnO, so the electrical characteristics are even more present with the addition of graphene (8). Since the majority of the research revolves around ZnO, there is a need for information regarding the electrical characteristics of SnO2, MgO, and Fe2O3 when combined with graphene. Studies about electrical characteristics involving these metal oxides can be recorded and then used for future use in studies involving these metal oxides. This research regarding ZnO has shown that it is an effective photocatalyst that can be used in the field of environmental conservation (8). In another study where ZnO was composited with graphene, it was shown that this composition can be an effective catalyst and can be then used in photo electronics (9). This is because ZnO, like many metal oxides, is an efficient electron donor, where graphene is a perfect match for metal oxides because it is a great electron acceptor (9). This study also showed that ZnO composited with graphene has a greater electrical conductivity when compared to just the conductivity of the graphene (9). Aside from ZnO, SnO2 would be the most widely studied metal oxide that is combined with graphene. However, there is a great disparity between the research done regarding SnO2 with graphene when compared to ZnO. In studies that have a focus on SnO2, it has been shown that SnO2 by itself has efficient photocatalytic activity that can be useful in the field of photo 7 electronics (10). SnO2 has been shown to have a band gap of 0.1-0.8 eV, which is also known as a band gap that has been narrowing (11). SnO2 has also been used in various studies that look for a more environmentally friendly way to store energy, and has been shown to have highly efficient electrochemical properties (12). Fe2O3 is found abundantly in nature and is a very stable compound. This makes it slightly more difficult to work with since the graphene is combined with a precursor so, an appropriate Fe2O3 precursor needed to be found (13). Fe2O3 has electrical characteristics that can be utilized in the oxidation of water, which could cause great progress in the field of environmental protection and is being studied as an application of clean energy (14). There have also been studies that have shown that Fe2O3 can be used to oxidize organic products which can be useful in the purification of wastewater, and this oxidation can be amplified when composited with graphene (15). MgO can be synthesized in various ways using various precursors. MgO is much different than the other two metal oxides that will be studied within this research due to it having a very different band gap. The band gap of MgO is around 6 eV which is much greater than the band gap of SnO2 and Fe2O3 (16).
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