N2 - The miscibility of polymethylmethacrylate (PMMA) and polyethyleneglycol (PEG) blends in tetrahydrofuran. MeTHF is between THF and Ethylether in Lewis Base strength and polarity Property MeTHF THF Et 2O dielectric const 6.97 7.5 4.42 dipole moment, Debye 1.38 1.69 1.11 water solubility, g/100g 4 mis 1.2 Hildebrand, MPa ½ 16.9 18.7 15.5 solvation energy, kcal/mol 0.6 0 2.3 Donor Number 18 20.5 19.2 title = "Miscibility of polymethylmethacrylate and polyethyleneglycol blends in tetrahydrofuran". THF (Merck) was distilled before use. The bright and dark regions in Figure 2(a) are corresponding to PMMA and PUA, respectively. From academic labs to industrial applications users have been able to formulate … The column oven and refractive index temperature were maintained at 40 °C. The results indicated the existence of positive interactions in the blend polymer solutions and that they are miscible in THF in the entire composition range. The molecular weight was determined using the ... good solubility parameter for PMMA - 17.2 (J1/2 cm-3/2), which provides a difference greater than 1.5. The study also revealed that variation in the temperature does not affect the miscibility of PMMA and PEG blends in THF significantly. O * * n O O H H O Transmittance [%] Note that the UV curing process was performed in the argon purged glove box, because oxygen plays a role as an inhibitor to photoinitiators. For selective dissolution of PMMA, the spin-coated film was dipped into tetrahydrofuran (THF) for 1 min after being exposed to UV light at ~365 nm (with a power of 4 W) for 40 s, and the film was then rinsed with deionized water and dried by blowing with N2. The study also revealed that variation in the temperature does not affect the miscibility of PMMA and PEG blends in THF significantly. Padmanabhan P(1), Chavis M, Ober CK, Escobedo FA. Morphological control of immiscible polymer blends has been widely studied in regard to phase geometry and dimensions, which can lead to many practical applications [1–5]. We are committed to sharing findings related to COVID-19 as quickly as possible. In addition, morphology of the PMMA/PUA blends can be easily controlled by changing composition (i.e., total concentration and weight ratio) of the blends. You can find more detailed information (Health & Safety, Physical, Regulatory, Environmental) on … The presence of hydrogen bonding in the blends in the solid state has also been indicated by FTIR studies.". When the value of increased up to ~0.4, the island-like PMMA features were finally connected to each other and formed larger domains (Figure 4(b)). Averaged height differences between the cured PUA domains and the PMMA domains before the THF treatments were ~35 nm, ~72 nm, and ~157 nm for the 10 wt%, 15 wt%, and 20 wt% blended solutions, respectively (Figures 3(a)–3(c)). The substrate exposure after film deposition also can be achieved by the selective dissolution without additional etching process, which may lead to further applications such as antireflection layers. Spin casting the PMMA/PUA blends in propylene glycol monomethyl ether acetate (PGMEA) was accompanied with phase separation, and PUA was subsequently cross-linked under UV radiation. The PMMA/PUA blends with different weight ratios of PMMA : PUA (3 : 7, 4 : 6, and 5 : 5, resp.) M. Selvakumar, D. Krishna Bhat, N. G. Renganathan, Research output: Contribution to journal ⺠Article ⺠peer-review. Island-like features with the diameter of ~600 nm were clearly observed when the PMMA mass fraction () was 0.3 (i.e., PMMA/PUA = 30/70) as shown in Figure 4(a), and the size of island-like features became larger as the value of increased. Schematic illustration of phase separation of PMMA/PUA upon the spin-coating process and selective dissolution before and after UV curing. Selective dissolution of PMMA in the phase-separated films was feasible using tetrahydrofuran (THF) solvent after the UV curing process, because the cured PUA material is highly stable against THF. It is worth noting that only one phase was observed on the surface without any evidence of phase separation when the value of was below 0.2 or above 0.8, due to the excess amount of one component in the blends. Solubilities are in water and are reported as grams solvent/100 grams water. Olga A. Efremova * ab, Konstantin A. Brylev cde, Yuri A. Vorotnikov cdf, Lucie Vejsadová bg, Michael A. Shestopalov cdf, Gwen F. Chimonides b, Petr Mikes g, Paul D. Topham b, Sung-Jin Kim e, Noboru Kitamura h and Andrew J. Sutherland b a Department of Chemistry, University of … These results imply that morphology of phase-separated structure with varied features can be easily controlled by changing composition of the blends. Although the blends with the varied concentrations showed similar tendencies according to the weight ratios, the 12 wt% solution most specifically revealed morphological changes in the blended films. Photoluminescent materials based on PMMA and a highly-emissive octahedral molybdenum metal cluster complex†. The densities of the polymer solutions in THF … However, no apparent domains were left on the noncured film after dissolving in THF as shown in Figure 2(c), which implies that the noncured PUA domains are removed with PMMA together during the THF treatment. The presence of hydrogen bonding in the blends in the solid state has also been indicated by FTIR studies. These results indicate that both PMMA and PUA heights increase as the total concentration of the blend increases. Solubility of PMMA inAlcohol-Water Solvent Mixtures 1175 0 10 20 30 40 50 60 70 80 90 100 Ethanol 5 wt-% H. 2. The UV curable PUA mixture consists of functionalized prepolymer with acrylate group, photoinitiator, and releasing agent for the surface activity, and the UV curing process induces cross-linking in the PUA mixture [17, 18]. The cross-linked PUA in the polymer-blended films provides strong chemical stability in the solvents such as THF, and thus target materials for dissolution can be selectively available via a simple curing process. Thus the cured PUA mixture is chemically stable against the THF treatment compared to noncured PUA and also shows high durability at high temperature (~300°C). Three different total concentrations with the same weight ratio of PMMA : PUA (35 : 65) were used to evaluate the effects of total concentration (see Section 2). Morphological changes in the PMMA/PUA blended film according to total concentration and weight ratio of the blended solution were investigated using atomic force microscopy (AFM). Instant access to the full article PDF. The polymer-blended solutions were then individually spin-coated at 3000 rpm for 30 s onto the prepared Si substrates. Solvent parameters, including Lewis basicity, solubility parameters, and a hydrophobicity parameter, were used to discuss the change in the PMMA solubility … Suh, “Modulus- and surface energy-tunable ultraviolet-curable polyurethane acrylate: properties and applications,”, J.-H. Kim, S. H. Hong, K.-D. Seong, and S. Seo, “Fabrication of organic thin-film transistors on three-dimensional substrates using free-standing polymeric masks based on soft lithography,”, A. Bernasik, J. Włodarczyk-Miśkiewicz, W. Łuzny et al., “Lamellar structures formed in spin-cast blends of insulating and conducting polymers,”, J. Jaczewska, A. Budkowski, A. Bernasik et al., “Humidity and solvent effects in spin-coated polythiophene-polystyrene blends,”. AFM images of (a) the PMMA/PUA (30 : 70) blended film after spin-coating of the 15 wt% blended solution, (b) the cured PUA domains remaining after selective dissolution of PMMA in THF, and (c) the noncured film after dissolving in THF. However, THF is a poor solvent of PVDF, so that it can't be used to dissolve PVDF at high concentration. Various interaction parameters such as polymer-solvent and blend-solvent interaction parameters and heat of mixing have been calculated using the viscosity, density, and ultrasonic velocity data. ... You can dissolve 3g of PMMA in 10ml of THF with stirring at room temp in less than 10hrs . The morphological controls include domain size, height, and nanoscale features such as island-like and hole-like structures. Island-like features completely disappeared at , and hole-like features with the diameter of ~500 nm were rather found as shown in Figure 4(c). In this chapter additional studies on operational variables, particularly dead volume, is … Morphology of the PMMA/PUA blend, including domain size and height, can be varied with the total concentration of solution. The PMMA was soluble in THF in all composition ranges and was immiscible in water. Solubility exists on a spectrum. The film thickness of each sample was measured using reflectometer, as indicated in the insets of Figure 2. Solubility of Potassium Acetate in Water, 2,2,2-Trifluoroethanol, Ethanol and Their Binary Mixtures at 288.15–333.15 K. Chemical Research in Chinese Universities 2019, 550 DOI: 10.1007/s40242-019-9193-3. Shop a large selection of products and learn more about Ammonia , 0.5M solution in THF, AcroSeal , ACROS Organics. PMMA (Mn = 11,500 g/mol, Mw/Mn = 1.08, Polymer Source Inc.) was used as received, and the UV curable PUA mixture was synthesized in accordance with the previous reports [17]. Previous study also showed that surface structures of the blended films of polystyrene (PS) and poly(methyl methacrylate) (PMMA) are remarkably changed by varying the film thickness [7]. Conclusions • Solvent-selective solubility of PLGA with different LA:GA ratio holds promise to separate PLGAs with varying LA:GA ratios. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. Lhoest, P. Bertrand, L. T. Weng, and J.-L. Dewez, “Combined time-of-flight secondary ion mass spectrometry and X-ray photoelectron spectroscopy study of the surface segregation of poly(methyl methacrylate) (PMMA) in bisphenol A polycarbonate/PMMA blends,”, M. C. Davies, K. M. Shakesheff, A. G. Shard et al., “Surface analysis of biodegradable polymer blends of poly(sebacic anhydride) and poly(dl-lactic acid),”, P. Wang and J. T. Koberstein, “Morphology of immiscible polymer blend thin films prepared by spin-coating,”, T. Kikuchi, M. Kudo, C. Jing, T. Tsukada, and M. Hozawa, “Electrohydrodynamic effect on phase separation morphology in polymer blend films,”, M. Ibn-Elhaj and M. Schadt, “Optical polymer thin films with isotropic and anisotropic nano-corrugated surface topologies,”, J. Kim, M. Inoue, L. Zhao et al., “Tunable and flexible solvent-free liquid organic distributed feedback lasers,”, S.-J. (THF) has been investigated by viscosity, density, refractive index, and ultrasonic velocity studies. Fig. The solvents that dissolve PMMA are dimethylformamide (DMF) and Diethyl carbonate (DEC). Cyanoacrylate and acrylic [PMMA, MMA, etc] based polymers can get good bonding at the molecular level. Price includes VAT for USA. Various interaction parameters such as polymer-solvent and blend-solvent interaction parameters and heat of mixing have been calculated using the viscosity, density, and ultrasonic velocity data. Hall, P. Underhill, and J. M. Torkelson, “Spin coating of thin and ultrathin polymer films,”, D. W. Schubert and T. Dunkel, “Spin coating from a molecular point of view: its concentration regimes, influence of molar mass and distribution,”, J. S. Chiou, J. W. Barlow, and D. R. Paul, “Miscibility of bisphenol-a polycarbonate with poly(methyl methacrylate),”, J.-B. [ABS, PVC, HIPS] => Acetone and M ethyl E thyl K etone [MEK aka 2-Butanone] will dissolve both ABS and PVC and chemically rebuild the joint in a less ordered manner as the solvents dries. Several other solvents like toluene give cloudy solutions. Ju-Hyung Kim, Joon H. Kim, Soonmin Seo, "Nanotextured Morphology of Poly(methyl methacrylate) and Ultraviolet Curable Poly(urethane acrylate) Blends via Phase Separation", Journal of Nanomaterials, vol. In consideration of thermodynamic behaviors, PUA material would move to the air-polymer interface to minimize interfacial free energy, because PUA has a lower surface tension than PMMA (i.e., 26 mN/m for PUA and 42 mN/m for PMMA). @article{ee4718f3e9094d13a3e4b41dc08c1b6a. PMMA samples were solubilized at 0.1% (w/w) in THF and injected into the chromatograph (100 μL). The results indicated the existence of positive interactions in the blend polymer solutions and that they are miscible in THF in the entire composition range. The nuances of particle solubility in a given solvent should ultimately be investigated by the experimenter during assay optimization and this guide is not a substitute for bench top evaluation.Adapted from: Brandrup, J., and The effect of various solvents on the morphology of polymethyl methacrylate (PMMA) particles synthesized by spray drying is examined. SYNTHESIS, THERMAL BEHAVIOR, AND AGGREGATION IN AQUEOUS SOLUTION OF POLY(METHYL METHACRYLATE)-B-POLY(2-HYDROXYETHYL METHACRYLATE) B. ACEVEDO 1, F. MARTINEZ 2, A. F. OLEA 1 *. Together they form a unique fingerprint. Miscibility of polymethylmethacrylate and polyethyleneglycol blends in tetrahydrofuran. were also prepared by mixing 12 wt% of PMMA and PUA for further evaluation of the mixing effects. These results indicate that target materials for dissolution can be selectively available via a simple UV curing process. Solutions of lower concentrations were then prepared by appropriately diluting these stock solutions with THF. Also, pure PMMA is soluble in acetone, THF, MEK, ethyl acetate, acetonitrile and insoluble in alcohols and ether. However, in this work, PUA mostly remains at the polymer-substrate interface, which possibly originates from spinodal decomposition due to the differences of solvent evaporation rate for each polymer and polymer solubility in the common solvent. See: Pubchem; T = 20 °C unless specified otherwise. As the solvent evaporates during spin-coating, PGMEA in PMMA drains away prior to the PUA domains which are still swollen with PGMEA. The height profiles are shown in insets. Sign up here as a reviewer to help fast-track new submissions. O 15 wt-% H. 2. The results indicated the existence of positive interactions in the blend polymer solutions and that they are miscible in THF in the entire composition range. Under this link you find the solubility of PMMA in 12 different organic solvents. For more than 50 years Hansen Solubility Parameters, HSP, have proven to be a powerful, practical way to understand issues of solubility, dispersion, diffusion, chromatography and more. After selective PMMA dissolution, the remaining film thickness was ~106 nm (Figure 2(b)). Particularly, it is well known that domain structures and surface topography strongly depend on various polymer interactions (i.e., polymer-polymer and polymer-surface interactions) in the blended films, and the relative solubility of polymers in a common solvent can play a crucial role in determination of surface morphology [6]. Cite. PVDF can be dissolved in THF. Being polar and having a wide liquid range, THF is a versatile solvent The results indicated the existence of positive interactions in the blend polymer solutions and that they are miscible in THF in the entire composition range. Tetrahydrofuran (THF), or oxolane, is an organic compound with the formula (CH 2) 4 O. Selective dissolution of PMMA in the phase-separated films was feasible using tetrahydrofuran (THF) solvent after the UV curing process, because the cured PUA material is highly stable against THF. Choi, P. J. Yoo, S. J. Baek, T. W. Kim, and H. H. Lee, “An ultraviolet-curable mold for Sub-100-nm lithography,”, S.-J. Figure 3 shows the morphological change as the total PMMA/PUA concentration increases. Consequently, the solvent in PMMA is quickly depleted in the spin-coating process, which leads to elevation of the PMMA domains onto the PUA-rich domains. It is concluded that the product PMMA particles, derived from the PMMA-acetone dilute solution, have a smaller particle size than those from the PMMA-THF dilute solution. The PMMA is degraded almost exclusively under action of the heat in MMA with yield up to 97%. UR - http://www.scopus.com/inward/record.url?scp=58149229111&partnerID=8YFLogxK, UR - http://www.scopus.com/inward/citedby.url?scp=58149229111&partnerID=8YFLogxK. 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By FTIR studies. `` immiscible polymer-blended System with high stability which complete... More than one phase and as a result experience a gap in miscibility at room temp in less 10hrs! Lower concentrations were prepared separately in different stoppered conical flasks equally to this work after THF... Of Applied polymer Science '', Department of Chemistry, Manipal Institute of Technology, Manipal, India form! High stability which enables complete selective dissolution of PMMA in trichloroethylene to ~100 nm as total... Concentrations of the PMMA/PUA blend was well-driven via solvent evaporation during spin-coating, in... Engineering, Cornell University, Ithaca, NY 14853, USA, Wei Li, Zhou. Stirring at room temp in less than 10hrs blend are schematically illustrated Figure! Features can be varied with the total concentration of the PMMA/PUA blended films with different total concentrations of PMMA/PUA!, N. G. Renganathan, N. G. T1 - miscibility of PMMA in 10ml of THF stirring... Was used to dissolve PVDF at high concentration at 3000 rpm for 30 s onto the prepared substrates. Used to demonstrate the complete selective dissolution of one component interests regarding the of. Solutions of lower pmma solubility in thf were then individually spin-coated at 3000 rpm for 30 s onto the prepared Si.. Dispersed on the morphology of the PMMA/PUA blend, including domain size, height and... Various total concentrations of the PMMA/PUA blend are schematically illustrated in Figure 1 ( a ) are corresponding PMMA! The immiscible polymer blends to unveil the detailed mechanism of phase separation will be Applied to Engineering... To evaluate the effects polymethylmethacrylate and polyethyleneglycol blends in tetrahydrofuran PVDF, that! The prepared Si substrates one component ; T = 20 °C unless specified....