N2 - The miscibility of polymethylmethacrylate (PMMA) and polyethyleneglycol (PEG) blends in tetrahydrofuran. The study also revealed that variation in the temperature does not affect the miscibility of PMMA and PEG blends in THF significantly. The column oven and refractive index temperature were maintained at 40 °C. (THF) has been investigated by viscosity, density, refractive index, and ultrasonic velocity studies. The study also revealed that variation in the temperature does not affect the miscibility of PMMA and PEG blends in THF significantly. The study also revealed that variation in the temperature does not affect the miscibility of PMMA and PEG blends in THF significantly. Spin-coated immiscible PMMA and UV curable PUA blends are phase-separated owing to the differences of solvent evaporation rate for each polymer and polymer solubility in the common solvent. Morphology of the PMMA/PUA blend, including domain size and height, can be varied with the total concentration of solution. 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 … The main by-products formed are CO 2, CO, CH 4, CH 3OH, light Hydro-carbons and char. Solubility of polymethyl methacrylate in 12 organic solvents at 30–70°C was studied. The hole diameter decreased to ~100 nm as the value of increased up to ~0.6. journal = "Journal of Applied Polymer Science", Department of Chemistry, Manipal Institute of Technology, Manipal. Although the solubility of PUA in THF is relatively low, the noncured PUA can be dissolved in THF due to the polymer interactions between PUA and PMMA [12]. 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 study also revealed that variation in the temperature does not affect the miscibility of PMMA and PEG blends in THF significantly. In addition, the PMMA/PUA blends with different weight ratios of PMMA : PUA were also examined for further evaluation of the mixing effects (see Section 2). The height of the cured PUA domains was almost the same as the total thickness of the blended film, implying that PUA and PMMA are phase-separated on the substrate as illustrated in Figure 1(b). The Si substrate was exposed to the air after the selective dissolution as shown in Figure 2(d), and averaged height of the cured PUA domains was ~170 nm. 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. O 10 wt-% H. 2. The bright region in Figure 2(b) corresponds to the PUA domains dispersed on the substrate after spin-coating. 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. 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. 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. 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. Author information: (1)School of Chemical and Biomolecular Engineering, Cornell University, Ithaca, NY 14853, USA. 2 Departamento de Ciencias de los Materiales, Facultad de Ciencias … The PMMA/PUA blends with different weight ratios of PMMA : PUA (3 : 7, 4 : 6, and 5 : 5, resp.) Solubilities are in water and are reported as grams solvent/100 grams water. Under this link you find the solubility of PMMA in 12 different organic solvents. The presence of hydrogen bonding in the blends in the solid state has also been indicated by FTIR studies.". 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 *. 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. 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). PVDF can be dissolved in THF. The bright and dark regions in Figure 2(a) are corresponding to PMMA and PUA, respectively. Solubility of polymers in organic solvents has important applications in the field of paints and coatings. 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. The PMMA was soluble in THF in all composition ranges and was immiscible in water. It is worth noting that the noncured PUA domains are also well-dissolved in THF. Phase separation and selective dissolution in the PMMA/PUA blend are schematically illustrated in Figure 1. 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. Price includes VAT for USA. Also, pure PMMA is soluble in acetone, THF, MEK, ethyl acetate, acetonitrile and insoluble in alcohols and ether. The weight ratios of PMMA : PUA are (a) 3 : 7 (, Nanotextured Morphology of Poly(methyl methacrylate) and Ultraviolet Curable Poly(urethane acrylate) Blends via Phase Separation, Department of Chemical Engineering, Pukyong National University, Busan 608-739, Republic of Korea, School of Chemical and Biological Engineering, Seoul National University, Seoul 151-742, Republic of Korea, College of BioNano Technology, Gachon University, Gyeonggi 461-701, Republic of Korea, M. Boltau, S. Walheim, J. Mlynek, G. Krausch, and U. Steiner, “Surface-induced structure formation of polymer blends on patterned substrates,”, S. Walheim, E. Schäffer, J. Mlynek, and U. Steiner, “Nanophase-separated polymer films as high-performance antireflection coatings,”, S. Nilsson, A. Bernasik, A. Budkowski, and E. Moons, “Morphology and phase segregation of spin-casted films of polyfluorene/PCBM blends,”, C. Huang, J. Gao, W. Yu, and C. Zhou, “Phase separation of poly(methyl methacrylate)/poly(styrene-, S. Kato and A. Sato, “Micro/nanotextured polymer coatings fabricated by UV curing-induced phase separation: creation of superhydrophobic surfaces,”, S. Walheim, M. Böltau, J. Mlynek, G. Krausch, and U. Steiner, “Structure formation via polymer demixing in spin-cast films,”, K. Tanaka, A. Takahara, and T. Kajiyama, “Film thickness dependence of the surface structure of immiscible polystyrene/poly(methyl methacrylate) blends,”, D. B. Total thickness of the blended film just after spin-coating was approximately 180 nm and averaged height difference between PUA and PMMA was 64 nm (Figure 2(a)). Propylene glycol monomethyl ether acetate (PGMEA) was selected for a common solvent for the immiscible polymer blend of PMMA and PUA. Extensive efforts have been devoted to study immiscible polymer blends to unveil the detailed mechanism of phase separation involved in spin-coating [10–14]. 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,”. The column oven and refractive index temperature were maintained at 40 °C. author = "M. Selvakumar and Bhat, {D. Krishna} and Renganathan, {N. G.}". Schematic illustration of phase separation of PMMA/PUA upon the spin-coating process and selective dissolution before and after UV curing. Spin-coating is a simple method for fabricating thin polymer films, which facilitates precise and easy control of film thickness by rotational velocity and concentration of polymer solution [8, 9]. Tetrahydrofuran (THF), or oxolane, is an organic compound with the formula (CH 2) 4 O. The miscibility of polymethylmethacrylate (PMMA) and polyethyleneglycol (PEG) blends in tetrahydrofuran. Dive into the research topics of 'Miscibility of polymethylmethacrylate and polyethyleneglycol blends in tetrahydrofuran'. THF (Merck) was distilled before use. Note that various total concentrations of the blended solutions were examined with the three different weight ratios. The presence of hydrogen bonding in the blends in the solid state has also been indicated by FTIR studies. The effect of various solvents on the morphology of polymethyl methacrylate (PMMA) particles synthesized by spray drying is examined. Product literature and technical reports present a bewilderingassortment of such systems: Kaouri-Butanol number, solubility grade,aromatic character, analine cloud point, wax number, heptane number,and Hildebrand solubility parameter, among others. The polymer-blended solutions were then individually spin-coated at 3000 rpm for 30 s onto the prepared Si substrates. Zinc chloride solution 0.5 M in THF; CAS Number: 7646-85-7; Linear Formula: Cl2Zn; find Sigma-Aldrich-366374 MSDS, related peer-reviewed papers, technical documents, similar products & … Dilute solutions of 2% (w/v) PMMA and PEG in THF were prepared separately in different stoppered conical flasks. (d) SEM image of (b). These results strongly suggest great potential for various applications in the field of soft lithography, such as antireflection layers, polymer membranes, artificial superhydrophobic surfaces, and nanopatterned structures. Figure 3 shows the morphological change as the total PMMA/PUA concentration increases. (THF) has been investigated by viscosity, density, refractive index, and ultrasonic velocity studies. 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]. Solubility and miscibility describe similar phenomena, but they are not the same. 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]. 6 ... /Length 7903 Remarkable is the extreme solubility of PMMA in trichloroethylene. The study also revealed that variation in the temperature does not affect the miscibility of PMMA and PEG blends in THF significantly. If the blended solution of two different immiscible polymers dissolved in a common solvent is spin-coated, phase separation normally occurs during the evaporation of solvent. Shop a large selection of products and learn more about Ammonia , 0.5M solution in THF, AcroSeal , ACROS Organics. (THF) has been investigated by viscosity, density, refractive index, and ultrasonic velocity studies. Rent this article via DeepDyve. However, various interactions, such as polymer-polymer and polymer-surface interactions, cause complexity and difficulty in control of the selective dissolution and fabrication of desired structures. Nomenclature M N number average molecular weight M W weight average molecular weight x AB Flory–Huggins interaction parameter V ref reference volume d i solubility parameter of species i R gas constant T absolute temperature DG m Gibbs free energy change on mixing DH m enthalpy change on mixing DS m entropy change on mixing V mix volume of the mixture DEV i energy of vaporization of … ... You can dissolve 3g of PMMA in 10ml of THF with stirring at room temp in less than 10hrs . In a simpler approach valid for slightly polar solvents, the capacity of a solvent to dissolve a polymer can be estimated by means of the Hildebrand solubility parameter (see regular solution theory in Section 6.3.3) defined as the square root of the cohesive energy: 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 Here we present a binary immiscible polymer-blended system with high stability which enables complete selective dissolution of one component. The solvents that dissolve PMMA are dimethylformamide (DMF) and Diethyl carbonate (DEC). 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 densities of the polymer solutions in THF … 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. 1 Departamento de Ciencias Químicas, Facultad de Ciencias Exactas, Universidad Andrés Bello, Quillota 980, Viña del Mar, Chile. Instant access to the full article PDF. 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. 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)). ... (THF) and water are miscible. Several other solvents like toluene give cloudy solutions. In addition, theHildebrand solubility parameter, perhaps the most widely applicableof all the systems, includes such variations as the Hildebrandnumber, hydrogen bonding value, Hansen parameter, and fractionalparameter, to name a few… You can find more detailed information (Health & Safety, Physical, Regulatory, Environmental) on … We anticipate that these controllable structures originating from the phase separation will be applied to various engineering fields such as soft lithography. 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. Access options Buy single article. Solutions of lower concentrations were then prepared by appropriately diluting these stock solutions with THF. [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. As illustrated in Figure 1, the cross-linked PUA domains remain even after dissolving the blended film in THF, whereas the PMMA domains are completely dissolved in THF. PMMA samples were solubilized at 0.1% (w/w) in THF and injected into the chromatograph (100 μL). For this work, PMMA and ultraviolet (UV) curable poly(urethane acrylate) (PUA) were used [17–19], and the phase separation of PMMA/PUA blend was well-driven via solvent evaporation. AFM images of the PMMA/PUA blended films with different total concentrations. checked visually for a qualitative determination of solubility and scored “0” – “2” to indicate no dissolution (0), partial dissolution (1), and full dissolution (2). M. Selvakumar, D. Krishna Bhat, N. G. Renganathan, Research output: Contribution to journal › Article › peer-review. (THF) has been investigated by viscosity, density, refractive index, and ultrasonic velocity studies. 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). 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. The blend with 15 wt% PUA and 15 wt% PMMA was used to demonstrate the complete selective dissolution of PMMA. In this chapter additional studies on operational variables, particularly dead volume, is … 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)). 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. Solvent parameters, including Lewis basicity, solubility parameters, and a hydrophobicity parameter, were used to discuss the change in the PMMA solubility … Click to download pdf version.This solubility list is based on the Hansen Solubility Parameters and should be used as a guide in methods development. Contact angles and surface tension data were measured to obtain the surface tension components of polyacrylamide (PAM). / Selvakumar, M.; Bhat, D. Krishna; Renganathan, N. G. T1 - Miscibility of polymethylmethacrylate and polyethyleneglycol blends in tetrahydrofuran. 3 shows the phase diagram for the ternary system PMMA/THF/H 2 O at 25°C, with very large immiscibility gaps, meaning that the area of homogeneity was very small. Figure 4 shows morphology of the PMMA/PUA blended films with different weight ratios of PMMA : PUA (3 : 7, 4 : 6, and 5 : 5 in the 12 wt% solutions). The cured PUA domains and the PMMA domains before the THF treatments for (a) 10 wt%, (b) 15 wt%, and (c) 20 wt% blended solutions, and the cured PUA domains remaining after the THF treatments for (d) 10 wt%, (e) 15 wt%, and (f) 20 wt% blended solutions. 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. In Table 1 are presented the 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. These results indicate that target materials for dissolution can be selectively available via a simple UV curing process. 1 Recommendation. Photoluminescent materials based on PMMA and a highly-emissive octahedral molybdenum metal cluster complex†. Sign up here as a reviewer to help fast-track new submissions. Copyright © 2015 Ju-Hyung Kim et al. The polymer-blended solutions with different concentrations were prepared to evaluate the effects. This work was supported by a research grant of Pukyong National University (Year 2014). The molecular weight was determined using the software program Millennium 2010. As the solvent evaporates during spin-coating, PGMEA in PMMA drains away prior to the PUA domains which are still swollen with PGMEA. 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. Review articles are excluded from this waiver policy. See: Pubchem; T = 20 °C unless specified otherwise. The authors declare that there is no conflict of interests regarding the publication of this paper. This is a preview of subscription content, log in to check access. Morphology of phase-separated structure, including domain size and height, could be controlled by varying total concentration of the blended solution, and various nanoscale features such as island-like and hole-like structures were achieved by changing weight ratio of the two immiscible polymers. The film thickness of each sample was measured using reflectometer, as indicated in the insets of Figure 2. These results indicate that both PMMA and PUA heights increase as the total concentration of the blend increases. 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. O * * n O O H H O Transmittance [%] 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 phase separation of PMMA/PUA blend was well-driven via solvent evaporation during spin-coating. @article{ee4718f3e9094d13a3e4b41dc08c1b6a. O 15 wt-% H. 2. Being polar and having a wide liquid range, THF is a versatile solvent We are committed to sharing findings related to COVID-19 as quickly as possible. In the case of using were also prepared by mixing 12 wt% of PMMA and PUA for further evaluation of the mixing effects. Prior to spin-coating of the solutions, silicon (Si) wafer substrates were cleaned by successive sonication in trichloroethylene, acetone, and isopropyl alcohol for 5 min each. 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). Conclusions • Solvent-selective solubility of PLGA with different LA:GA ratio holds promise to separate PLGAs with varying LA:GA ratios. UR - http://www.scopus.com/inward/record.url?scp=58149229111&partnerID=8YFLogxK, UR - http://www.scopus.com/inward/citedby.url?scp=58149229111&partnerID=8YFLogxK. 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. The ratio of these products depends on the temperature of depolymerization. Ju-Hyung Kim and Joon H. Kim contributed equally to this work. O * * n O O H H O Transmittance [%] I tried to dissolve it in THF but it didn't dissolve properly even after heating at 40. The PMMA is degraded almost exclusively under action of the heat in MMA with yield up to 97%. PMMA samples were solubilized at 0.1% (w/w) in THF and injected into the chromatograph (100 μL). The compound is classified as heterocyclic compound, specifically a cyclic ether.It is a colorless, water-miscible organic liquid with low viscosity.It is mainly used as a precursor to polymers. reported for tetrahydrofuran (THF), dimethylformamide (DMF) and dimethylacetamide (DMAC) mobile phases. Solvent/100 grams water wt- % H. 2 Kim contributed equally to this work was by! Mixing effects blend increases regions in Figure 2 ( b ) shows the cured PUA domains after... Ab - the miscibility of polymethylmethacrylate and polyethyleneglycol blends in THF significantly Contribution journal. Lower concentrations were prepared to evaluate the effects research output: Contribution to ›. Be used to dissolve PAA of 1250 kDa ( 2 wt % of PMMA in.! The temperature does not affect the miscibility of PMMA and PUA, respectively was soluble in significantly... Solubilities are in water and are reported as grams solvent/100 grams water GPC. 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Well as case reports and case series related to COVID-19 in to check access AcroSeal glass bottle packed in can! Exclusively under action of the mixing effects and Renganathan, { D. Krishna Bhat {. Mixtures 1175 0 10 20 30 40 50 60 70 80 90 Ethanol!, log in to check access ~106 nm ( Figure 2 ( a are. Concentration increases propylene glycol monomethyl ether acetate ( PGMEA ) was selected for a common solvent the. Under this link you find the solubility of PLGA with different LA: GA.... Preview of subscription content, log in to check access, Baotong Li content, in... Was soluble in THF and injected into the chromatograph ( 100 μL....