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Electrospinning Technique Final Report
Electrospinning Technique Final Report
Electrospinning Technique Final Report
Electrospinning Technique Final Report
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Electrospinning Technique Final Report

  1. Translational and Rotational Target Effect on Electrospun Nanofibers José A. Cruz-Arzón1 , Edwin J. Alvarado2 Department of Biology, University of Puerto Rico at Cayey, PR1 Department of Mathematics-Physics, University of Puerto Rico at Cayey, PR1 A B S T R A C T Using PEO stock solution, non-aligned nanofibers can be formed. The electrospinning technique makes the formation of these fibers more bearable by using electrical conductivity. Independently if the fibers are aligned or not, the metallization by Sputtering can be helpful because it adds less oxidation to the fibers, allowing them to be seen under the electronic microscope. The shells formed by this process of Sputtering are what researchers are looking for, because they have the ability of performing a specific function such as gas sensing. The electronic microscope also helps in the characterization and analysis of the Nanofibers and more important the shells. If one wants to study the shells in details, the calcination process can be a way of evaporating the fibers to characterize only the shells previously metalized. This abstract seems incomplete to me because I do not see the objective of the researchor the hypothesis, the methodology, the results, the conclusions, and the future directionnecessary in any abstract of primary research. Introduction Nanofibers are fibers that one of their dimensions has a diameter of 100nm or less. These Nanofibers are used because of their high surface-to-volume ratio thatallows certain substances and particles to attach to its surface in order to perform a specific function. Their physicochemical properties and high porosity allow the fibers to have a high chemical reactivity with the particles attached to it, and any other substance or chemical. These fibers have to first be prepared using a solution-based method in order to produce a fiber. PEO Nanofibers are a good example; they are made based on a solution of 95% water and ethanol and 5% weight/ weight of the solute PEO. The solution has to be spun in order to create a fiber. In this case, electrospinning is used to produce the PEO nanofibers (Deitzel et al. 2001). The electrospinning technique was reinforced on 1930 as a simple and versatile method for making fibers of polymer solutions with the specified diameter (Katta et al. 2004). Other types of spinning involve melt spinning, solution spinning, and gel state spinning. The electrospinning technique uses a power supply to provide electricity so the solution, placed inside a syringe, runs using electrical charges. A negatively charged electrode would be attached to the syringe, and a positively charged electrode to a collector which has a substrate that is going to catch the fibers when they deposit. The size of a syringe’s tip is going to create a slow acceleration at the beginning, and then when it comes out from the tip, a fast acceleration creates a fiber deposited on the substrate. In this case, the substrate used is Silicon, because it can be used to study conductivity and oxidation of the fibers.
  2. Yet, there are two methods in which the fibers can be formed by electrospinning, the aligned electrospinning method and the non-aligned electrospinning. Basically, they both work the same way, but the aligned electrospinning posses a moving collector which has rotational and translational movement so it can create more organized and aligned fibers for future characterization. The objective was to determine the effect of that aligned electrospinning on the fibers. The non-aligned electrospinning just has a static collector. So the hypothesis states that having rotational and x-translational target will produce uniform fibers. Certain other processes are involved in making a good fiber for their usage. In case that the fibers cannot be seen under an electronic microscope because of their high oxidation thanks to electron bombing of the microscope, the fibers have to go through a metallization process. A metal, palladium, is deposited on the fiber inside a Vacuum Chamber to avoid oxidation. Also, this metal forms a shell which can be used for further studies in the field. Nanofibers in this case are used as templates for the formation of palladium shells which can be used for studies on the sensing of certain gases such as Hydrogen. Electrospinning also provides a variety of possibilities for the formation of fibers. Collagen fibers are also synthesized using electrospinning, but the collagen fiber is the material used for Biomedical Applications, like the regeneration of the hydroxyapatite in bones (Mathews et al. 2002). DNA nanofibers can also be created using electrospinning, to study their sequences in details. Materials and Methods The original solution planned to be used in this experiment was PVA and Zn (Ac) 2 solution.However, due to a possible contamination through humidity, the solution was changed to a PEO stock solution (Deitzel et al. 2001). Before beginning to use any other equipment, the use of gloves is compulsory to avoid further contamination of the fibers or any other samples. The electrospinning chamber used was the non-aligned electrospinning chamber, because the aligned fibers were already synthesized. A Vacuum Chamber was used to metalize the fibers with palladium for the future creation of shells. The Scanning Electron Microscope was used to characterize the aligned and non-aligned fibers and analyze the formation of shells on the fibers. Last of all, an oven was used to calcinate the fibers and leave only the shells for research of their capability as hydrogen sensors. Electrospinning Approximately 1.5ml of the PEO stock solution was placed inside a syringe. The syringe was then placed inside the electrospinning chamber with the negative electrode attached to it, and the positive electrode attached to the substrate on the target. The power supply was turned on at 20.0 KV at a rate of 0.5 ml/hr. It took two hours for the solution to deposit itself on the substrate creating the Nanofibers. Sputtering or Metallization The sample including the Silicon substrate and the fibers, were placed inside the Vacuum Chamber to start the metallization process by sputtering. The chamber was set to a Base Pressure of 1.6 x 10-5 torr, a Deposition Pressure of 13mtorr and a power of 25 W. A magnet and a power source together formed an electromagnetic field, which hadfree electrons in constant motion within it. The electrons began to collide with highenergy ions of argon, which was chemically inert, creating plasma surrounding the target which contained the metal, palladium. The collisions of electrons and ions made the material of palladiumeject and start depositingitself all over the inner surface of the chamber. Since the substrate, containedsilicon and PEO fibers, facing the target, more palladiumwasdeposited on the fiber sample. This process occurred in a span of 2 minutes. After the deposition process finished, it was important to remember to create a vacuum, and fill the chamber with nitrogen to balance the pressure from the outside, just before opening the chamber.
  3. Characterization of the fibers The characterization of the fibers wasdone under an electronic microscope. The fibers were analyzed using a magnification of 600×, 900×, 1,500×, 2,000×, 8,000×, 12,000×, and 22,000×. Calcination The fibers were calcinatedfor 2 hours at 325 ºC, causing the fibers to evaporateand isolating the palladium shells. After the calcinations, the shells were analyzed again under the microscope. Fig.2 Palladium shells after calcination (SEM micrograph at 2,000×) Results The electrospinning process was done successfully, and with the PEO fibers no contamination occurred. The non-aligned fibers were done using the established parameters (20.0V and 0.50 mL/h). Using the pressures established in the Sputtering process, the palladium material was deposited on the fibers inside the Vacuum Chamber. Using the electronic microscope, the objective was accomplished.Rotational and translational movement of the collector produced uniform and more organized fibers. With the calcinations step completed, the fibers used as a template were evaporated, leaving the palladium shells for future characterization. These shells were seen under a microscope. concluding that shells were formed by the calcinations process letting further research on the shells (This last part is not clear. Yet, since you are concluding it should appear in thediscussion section.). Discussion Non-aligned PEO fibers were produced to be used as a template for further sensing of gases such as hydrogen. One of the characteristics of palladium is that it has a great affinity for gases, especially hydrogen, so the palladium shells formed by the metallization of PEO fibers can be a great material for gas sensing. As a conclusion, the aligned PEO fibers could work better for the formation of shells than the non-aligned fibers, because they are more organized and uniform, allowing the deposition of palladium to be more successful. Further research of the characteristics of the aligned and non-aligned fibers could open doors for improvements to the electrospinning technique for better fiber production, and therefore forthe better formation of shells that may be used for different kinds of functions that include not only gas sensing, but also certain biomedical applications. References Katta P, Alessandro M, Ramsier R D, Chase GG. 2004. Continuous electrospinning of aligned polymer nanofibers onto a wire drum collector. Nano Lett [Internet]. 4(11):2215-8. Matthews JA, Wnek GE, Simpson DG, Bowlin GL. 2002. Electrospinning of Collagen Nanofibers. Biomacromolecules [Internet]. 3(2):232–8 Deitzel JM, Kleinmeyer JD, Hirvonen JK, Beck Tan NC. 2001. Controlled Deposition and Collection of Electro-spun Poly (ethylene oxide) Fibers. ARL [Internet]. 2415: 9-27
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