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Authors: Qualitative and Quantitative Analysis of Co-authors: PS/PMMA Spin-coated Graduates: Thin Films through Optical Microscopy and

Atomic Force Microscopy to Explore Immiscible Film Behavior

Abstract: Our group of two learned essential lab skills and determined the ratio of polystyrene to poly(methyl methacrylate) at which the least phase separation was evident. We prepared a solution of approximately 5 mg/mL of polystyrene and approximately 15 mg/mL of poly(methyl methacrylate) in toluene, such that the ratio of polystyrene to poly(methyl methacrylate) was 1 to 3. We then spin-casted this solution onto cleaved [1,0,0] silicon wafers. We examined these wafers under an optical microscope and found that spun-cast polymer molecules were not in their lowest energy positions. We also examined these wafers under an atomic force microscope and found that the surface of the spun-cast film exhibited both holes and bumps. Comparing data across groups, we concluded that the ratio of polystyrene to poly(methyl methacrylate) at which the least phase separation was evident was 1:1.

Undergraduates: High Schoolers:

I. Introduction

Recycling has become a major green trend in past years. The success of recycling depends on ease of use and cost-effectiveness. It is easiest, on the consumer end, and most costeffective to recycle similar materials mixed together rather than separated by polymer and the structure of PMMA is as follows: composition. Thus, an important question to answer is whether certain polymers, such as polystyrene (PS) and poly(methyl methacrylate) (PMMA), may be melted down and recycled together without consequence. To answer this question, we first spincoated silicon wafers with toluene solutions of various ratios of PS/PMMA. Though both PS and PMMA are soluble in toluene, they are immiscible with each other. We then examined these samples through light microscopy and atomic force microscopy to determine how the immiscibility and solute ratios affected the films' topography. In short, the purpose of this experiment We were also given a stock [1,0,0] silicon wafer, was to analyze the topography of PS/PMMA tweezers, a diamond-tipped cutter, two Petri thin films in varying PS:PMMA ratios to dishes, two graduated Fischer Scientific determine if a mixture of these polymers could pipettes, one ungraduated Fisher Scientific be successfully recycled. pipette, one glass vial, Parafilm, and numerous pairs of Kimberly-Clark Purple Nitrile Gloves.

A. Goals

The goals of this experiment are 1. Machines Used twofold: first, to gain necessary skills to prepare The machines used in this experiment us for our upcoming research projects; and were a Headway second, to determine if it is possible to recycle a Research Inc. PWM32 Spin-Caster mixture of PS and PMMA. In this experiment, , an Asylum Atomic Force Microscope, an we learned how to use a pipette, make solutions Olympus BH2-UMA Optical Microscope in a fume hood, cleave silicon wafers, and spin- , and a Fred S. Carver Inc. Model C Hot coat solutions onto silicon wafers. Importantly, Press we learned the proper safety procedures to . employ during lab work.

B. Methods

II. Materials and Methods

1. Preparing PS/PMMA Solution We started with a pre-prepared vial A. Materials Stony Brook University provided us withcontaining 26.45 mg of PS and 76.36 mg of PS and PMMA, along with toluene to make a PMMA. Under a fume hood, we used the graduated pipette to add exactly 5.00 mL of solution. The structure of PS is as follows: toluene to the vial, thus making a solution.

2. Cleaving the Silicon Wafers In the next phase of the experiment, we first observed the cleaving of a [1,1,1] silicon wafer. We were then given a circular stock wafer of [1,0,0] silicon with one shiny side and one dull side. (the shiny side was face-up). Placing the tweezers in the middle of the wafer to hold it in place, we cleaved the wafer by applying pressure on the edge of the wafer with the diamond-tipped cutter. We repeated this process until we had four 1 cm x 1 cm silicon wafers.

In creating our PS/PMMA solution, we learned how to properly use a pipette to prepare a solution under a fume hood. We also determined that both PS and PMMA are soluble in toluene.

B. Cleaving the Silicon Wafers

We learned the correct way to cleave a silicon wafer using tweezers and a diamondtipped cutter. We also observed the difference between [1,0,0] and [1,1,1] silicon wafers. The [1,0,0] wafers cleaved into quadrangles with 90 degree interior angles, while the [1,1,1] wafers 3. Spin-Coating cleaved into triangles with 60 degree interior The next step in the experiment involved angles. This discrepancy occurs because the spin-coating our PS/PMMA solution onto two [1,0,0] wafer was manufactured such that it runs of our silicon wafers. First, we used the parallel to one plane of the silicon crystals, tweezers to gently place one of the silicon whereas the [1,1,1] wafer runs diagonal to all wafers onto the spin caster, making sure to three planes of the crystals, as seen in the below cover the entire area. Next, we used an image (blue is [1,0,0] and red is [1,1,1]). ungraduated pipette to set two drops of our solution onto the wafer, enough solution to cover the entire surface. We then turned on the vacuum to keep the wafer in place during the spin-coating process. After that, we spun the wafer for approximately 30 seconds. We repeated this process until all four wafers were spin-coated. 4. Optical Microscopy C. Spin-coating Once we created our spin-coated wafers, We learned how to use the spin-caster to we examined one of them under an optical cover a silicon wafer with a polymer thin film. microscope. We then annealed a sample and reWe also observed that spinning a silicon wafer examined it under optical microscope. with polymer solution on top created an extremely thin film of polymer on the wafer. 5. Atomic Force Microscopy This phenomenon is caused by the confluence The AFM ran a cantilevered needle over of centripetal force, evaporation rate of solvent, the surface of the coating while tracking the viscosity of solution, and molar mass of solutes amount of deflection of a laser trained on the (see Fig. 1). cantilever. Thus, the AFM was able to map the topography and friction of the surface of the coating.

III. Results and Discussion


A. Preparing PS/PMMA Solution

change in topography between these pictures suggests that the polymer molecules had not settled into the lowest possible energy level after spin-casting. Instead, they were frozen in place once the solvent evaporated. Annealing the wafer melted the film, allowing the polymer molecules to move about and settle into a lower energy configuration, thus changing the appearance of the film.

D. Optical Microscopy Results

The results from the optical microscope E. Atomic Force Microscopy Results showed that the spin-coated polymer thin film The AFM results showed us how PS and was not at the lowest possible energy level. PMMA, which are immiscible with each other, interact when in a 1:3 ratio.

Interestingly, when the ratio of PS to PMMA is 1:3, the surface of the polymer thin film exhibited both bumps (dark spots) and holes (bright spots). The depth of one hole was determined to be 9.567 nm, and the height of one bump was approximately the same value. The holes and bumps arise because PS and The upper picture is an optical PMMA phase separate during spin-coating, microscope image of the un-annealed silicon despite both being soluble in toluene. wafer, and the lower picture is of the same Even more interestingly, the presence of wafer at the same magnification, annealed. The holes and bumps varied depending on the ratio

of PS to PMMA.

essential to learn. The recyclability of a PS/PMMA blend is impeded by the immiscibility of the two polymers with each other. However, there seems to be an optimum ratio of PS to PMMA at which the two show the least phase separation, visible as a lack of bumps and holes in the polymer film. We concluded that the blend of PS and PMMA that demonstrated the smoothest film, and thus most recyclability, was the 1:1 blend.

V. References
Cho, Chun-Hyung. "Characterization of Youngs Modulus of Silicon versus Temperature Using a beam Deflection Method with a Four-point Bending Fixture." ScienceDirect.com. Elsevier B.V., 15 May 2008. Web. 11 July 2012. Holmes, Michael J., and Carl E. Mungan. "Photobleaching of Cresyl Violet in Poly(methyl Methacrylate)." Journal of Young Investigators. The National Science Foundation, May 2004. Web. 11 July 2012. "Polystyrene." Kids' Macrogalleria. Polymer Science Learning Center, 2003. Web. 11 The ratios of PS to PMMA, from left to July 2012. right and from top to bottom, were 1:9, 1:3 Schubert, Dirk W., and Thomas Dunkel. "Spin (shown previously), 1:1, 3:1, and 9:1. The 1:9 Coating from a Molecular Point of View: and 3:1 wafers both exhibited bumps of Its Concentration Regimes, Influence of whichever polymer was in the minority. The 9:1 Molar Mass and Distribution." Materials wafer contained a remarkable amount of holes, Research Innovations 7.5 (2003): 314possibly containing PMMA, of apparently 21. Print. uniform depth. The 1:1 wafer was the only one to exhibit a blanketing effect, in which underlying holes and bumps were covered by a filling layer of either PS or PMMA.

IV. Conclusion
Through preforming this lab, we acquired numerous skills that will serve us well in the near future. The machines and procedures we learned to use are involved in many different areas of researchwe will likely be involved in at least some of themso these skills are

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