Nano Composite Membranes of Sulfonated Amine-Poly(ether sulfone)s and SiO2 for Fuel Cell Application

2010 ◽  
Vol 658 ◽  
pp. 392-395 ◽  
Author(s):  
Dong Wan Seo ◽  
Young Don Lim ◽  
Soon Ho Lee ◽  
Md. Monirul Islam ◽  
Hyun Mi Jin ◽  
...  
Keyword(s):  
Sol Gel ◽  
Thermo Gravimetric Analysis ◽  
Composite Membranes ◽  
Exchange Capacity ◽  
Gravimetric Analysis ◽  
Scanning Calorimetry ◽  
Nano Composite ◽  
Fuel Cell Application ◽  
Sol Gel Process ◽  
20 Nm

Organic-inorganic Nano composite membranes were prepared by Sulfonated amine-poly(ether sulfone)s (S-APES)s and SiO2. S-APESs were prepared by nitration, reduction and sulfonation of poly(ether sulfone) (ultrason®-S6010). Poly(ether sulfone) was reacted with ammonium nitrate and trifluoroacetic anhydride to produce the nitrated poly(ether sulfone), and was followed by reduction using tin(Ⅱ)chloride and sodium iodide as reducing agents to give the amino-poly(ether sulfone). The S-APES was obtained by reaction of 1,3-propanesultone and the amino-poly(ether sulfone) (NH2-PES) with sodium methoxide. The different degrees of nitration and reduction of poly(ether sulfone) were successfully synthesized by an optimized process. Organic-inorganic nano composite membranes were obtained by mixing S-APES (45 %) with hydrophilic SiO2 (20 nm, 4-10 %) obtained by sol-gel process. Different contents of SiO2 of the S-APES were studied by FT-IR, 1H-NMR spectroscopy, differential scanning calorimetry (DSC), and thermo gravimetric analysis (TGA). Sorption experiments were conducted to observe the interaction of sulfonated polymers with water and methanol. The ion exchange capacity (IEC), a measure of proton conductivity, was evaluated. The nano composite membranes exhibit conductivities (25 °C) from 3.51 x 10-3 to 4.10 x 10-3 S/cm, water swell from 57.25 to 60.50 %, IEC from 0.68 to 0.73 meq/g, and methanol diffusion coefficients from 2.81 x 10-7 to 3.33 x 10-7 cm2/S at 25 °C.

Nano Composite Membranes of Sulfonated Poly (Ether Ketone)/ Poly (Ether Sulfone) Copolymer and SiO2 for Fuel Cell Application

2007 ◽  
Vol 544-545 ◽  
pp. 1013-1016
Author(s):  
Hae Suck Park ◽  
Dong Hwan Suh ◽  
Dong Hun Lee ◽  
Whan Gi Kim
Keyword(s):  
Sol Gel ◽  
Chemical Properties ◽  
Composite Membranes ◽  
Scanning Calorimetry ◽  
Nano Composite ◽  
Force Microscopy ◽  
Atomic Force ◽  
Fuel Cell Application ◽  
Sol Gel Process ◽  
Ether Ketone

Novel bisphenol-based wholly aromatic poly(ether ketone)/poly(ether sulfone) copolymers containing pendant sulfonate groups were prepared by direct aromatic nucleophilic substitution polycondensation of 4,4-difluoro-3,3’-disodiumsulfonylbenzophenone (40mol% of bisphenol), difluorophenylsulfone and bisphenol A. Organic-inorganic composite membranes were obtained by mixing organic polymers with hydrophilic SiO2 (ca. 20nm) obtained by sol-gel process. The physic-chemical properties of these composite membranes were studied by thermogravimetry analysis(TGA), differential scanning calorimetry (DSC) and transform infrared(FTIR) spectroscopy. Scanning electron microscopy (SEM) and atomic Force microscopy (AFM) were used to observe the surface of membrances. The proton conductivity as a function of temperature decreased as SiO2 content increased, but water uptake increased. The membranes were shown all requisite properties; IEC (1.5meq./g), thermal stablity (Tg= 185°C), and low affinity towards methanol (1.5x10-7 - 4.3x10-7 cm2/S).

Nano Composite Membranes of Sulfonated Poly(ether sulfone) Containing 4,4-Bis(4-hydroxylphenyl)valeric Acid and SiO2 for PEMFC

2011 ◽  
Vol 695 ◽  
pp. 37-40
Author(s):  
Young Don Lim ◽  
Dong Wan Seo ◽  
Soon Ho Lee ◽  
Md. Monirul Islam ◽  
Hyun Mi Jin ◽  
...  
Keyword(s):  
Thermo Gravimetric Analysis ◽  
Composite Membranes ◽  
Valeric Acid ◽  
Gravimetric Analysis ◽  
Scanning Calorimetry ◽  
Nano Composite ◽  
Co Catalyst ◽  
H Nmr ◽  
20 Nm ◽  
Sulfonated Poly

Poly(ether sulfone)s (PES) containing 25-75 mol % valeric acid were prepared with bisphenol A, bis(4-chlorophenyl)sulfone and 4,4-Bis(4-hydroxylphenyl)valeric acid using potassium carbonate in DMAc (dimethylacetamide) at 160 °C. Copolymers containing carboxylacid group were reduced to hydroxy group by BH3solution 1M in THF and NaBH4 co-catalyst. Sulfonated poly(ether sulfone)s (S-PES) were obtained by reaction of 1,3-propanesultone and the reduced copolymer (PES-OH) with potassium t-butoxide. Composite membranes were prepared with copolymers and SiO2nanoparticles(20 nm, 4-10 wt%). The composite membranes were cast from DMSO.A series of composite membranes were studied by1H-NMR spectroscopy, differential scanning calorimetry (DSC), and thermo gravimetric analysis (TGA). Sorption experiments were conducted to observe the interaction of sulfonated polymers with water and methanol.

Study of Pseudoboehmite Synthesis by Sol-Gel Process

2006 ◽  
Vol 45 ◽  
pp. 260-265 ◽  
Author(s):  
Antônio Hortêncio Munhoz Jr. ◽  
Leila Figueiredo de Miranda ◽  
G.N. Uehara
Keyword(s):  
Sol Gel ◽  
Thermo Gravimetric Analysis ◽  
Ammonium Hydroxide ◽  
Gravimetric Analysis ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Sol Gel Process ◽  
Different Temperatures ◽  
Sol Gel Synthesis

A pseudoboehmite was obtained by sol-gel synthesis using aluminum nitrate as precursor. It was used a 2n full factorial design for studying the effect of the temperature of synthesis, the concentration of ammonium hydroxide, and the radiation dose in the product of sol-gel synthesis. The product of the synthesis was analyzed by scanning electron microscopy, x-ray diffraction of the product (after firing the pseudoboehmite at different temperatures), and it was also analyzed the temperature of endothermic and exothermic transformations using the thermo gravimetric analysis (TG) and differential scanning calorimetry (DSC). The X-ray diffraction data show that α-alumina was obtained at 1100o C.

Organic-Inorganic Nano Composite Membranes of Sulfonated Poly(ether Sulfone-Ketone) Copolymer and SiO2 for Fuel Cell Application

2007 ◽  
Vol 534-536 ◽  
pp. 97-100
Author(s):  
Dong Hoon Lee ◽  
Hye Suk Park ◽  
Dong Wan Seo ◽  
Whan Gi Kim
Keyword(s):  
Fuel Cell ◽  
Bisphenol A ◽  
Sol Gel ◽  
Composite Membranes ◽  
Exchange Capacity ◽  
Methanol Permeability ◽  
Scanning Calorimetry ◽  
Nano Composite ◽  
Inorganic Composite ◽  
Sulfonated Poly

Novel bisphenol-based wholly aromatic sulfonated poly(ether sulfone-ketone) copolymer and organic-inorganic composite membranes were prepared for operation 80°C in polymer electrolyte membrane fuel cell (PEMFCs). The copolymer were synthesized by direct aromatic nucleophilic substitution polycondensation of 4,4-difluorobenzophenone, 2,2’-disodiumsulfonyl- 4,4’-fluorophenylsulfone (40mole% of bisphenol A) and bisphenol A. Polymerization proceeded quantitatively to high molecular weight in N-methyl-2-pyrrolidinone at 180°C. Organic-inorganic composite membranes were obtained by mixing organic polymers with hydrophilic SiO2 obtained by sol-gel process. The polymer and a series of composite membranes were studied by FT-IR, 1HNMR, differential scanning calorimetry (DSC) and thermal stability. The proton conductivity as a function of temperature decreased as SiO2 content increased, but methanol permeability decreased. The nano composite membranes were found to poses all requisite properties; Ion exchange capacity (1.2meq./g), glass transition temperatures (164-183), and low affinity towards methanol (4.63-1.08x10-7 cm2/S).

scholarly journals Irradiation of a Nanocomposite of Pseudoboehmite-Nylon 6,12

2010 ◽  
Vol 71 ◽  
pp. 28-33 ◽  
Author(s):  
Antônio Hortêncio Munhoz Jr. ◽  
Renato Meneghetti Peres ◽  
L.H. Silveira ◽  
Leonardo Gondim Andrade e Silva ◽  
L.F. de Miranda
Keyword(s):  
Sol Gel ◽  
Thermo Gravimetric Analysis ◽  
Mechanical Tests ◽  
Polymeric Matrix ◽  
Nano Particles ◽  
Gravimetric Analysis ◽  
Polymeric Nanocomposites ◽  
X Ray Diffraction ◽  
Inorganic Substances ◽  
Sol Gel Process

Nanocomposites are nanometrical material particles embedded in a specific matrix. The degree of organization of the nanostructures and their properties depend on the nature of the organic and inorganic components of the structure that can generate synergic interactions. Polymeric nanocomposites are related to a class of hybrid materials where inorganic substances of nanometric dimensions are dispersed in a polymeric matrix. In the present work, nanocomposites of nylon 6,12 with different concentrations of pseudoboehmite obtained by sol-gel process were prepared with and without the presence of octadecylamine. After preparation, the samples were irradiated with a 200 kGy radiation dose in an electron accelerator. The pseudoboehmite nano particles were characterized by X-ray diffraction, scanning electron microscopy, differential thermal analysis and thermo gravimetric analysis. The nanocomposites were characterized by thermal and mechanical tests. The addition of pseudoboehmite promoted a reduction of the melting flow during the production of the composites evidencing the interaction of pseudoboehmite with the polymeric matrix, probably modifying its crystalline structure.

Fabrication of Iron Carbide and Nitride Ceramics with Controlled Magnetic Properties by the Non-Oxide Sol-Gel Process

2012 ◽  
Vol 512-515 ◽  
pp. 1429-1433
Author(s):  
Xun Lao ◽  
Xiao Yan ◽  
Jiao Xie ◽  
Ya Li Li
Keyword(s):  
Magnetic Properties ◽  
Sol Gel ◽  
Iron Carbide ◽  
Iron Nitride ◽  
Gravimetric Analysis ◽  
Scanning Calorimetry ◽  
Ferromagnetic Properties ◽  
Sol Gel Process ◽  
Nitride Ceramics ◽  
Carbide Ceramics

The carbodiimide-based non-oxide sol-gel process is a novel route to non-oxide nitride and carbide ceramics. This process has been applied to fabricate ternary or binary silicon based nitride and carbide ceramics. Based on this non-oxide sol-gel process, iron carbide and nitride have been fabricated by reaction of iron trichloride with bis(trimethylsilyl)carbodiimide to form FeCN gel followed by pyrolysis in argon flow at different temperatures. The iron carbide material obtained at 700 °C exhibits hard ferromagnetic properties whereas α-iron along with iron nitride formed at 1300 °C shows soft ferromagnetic properties. Therefore, iron carbide and nitride ceramics with controlled magnetic properties can be obtained along this novel non-oxygen sol-gel process by controlled pyrolysis. The pyrolysis behavior was investigated based on thermal gravimetric analysis coupled with differential scanning calorimetry. The phase structures of the iron carbide and nitride are identified by X-ray diffraction and the magnetic properties of the materials are measured by magnetometer.

Nanoparticles Prepared by Sol-Gel Method Used in Pseudoboehmite-Reinforced Nylon 6.12 Nanocomposites

2014 ◽  
Vol 798-799 ◽  
pp. 732-736
Author(s):  
Renato Meneghetti Peres ◽  
C.Y.U. Peres ◽  
Leila F. de Miranda ◽  
Cesar Denuzzo ◽  
Gabriel Cavalcante Gomes ◽  
...  
Keyword(s):  
Sol Gel ◽  
Thermo Gravimetric Analysis ◽  
Mechanical Tests ◽  
High Specific Surface Area ◽  
Polymeric Matrix ◽  
Inorganic Materials ◽  
Gravimetric Analysis ◽  
X Ray Diffraction ◽  
Thermo Gravimetric ◽  
Sol Gel Process

Polymers nanocomposites are composed by nanometrical particles embedded in a specific matrix. Additions of small amount of nanoparticles of inorganic material in specific matrixes can greatly improve mechanical properties. The high specific surface area of the inorganic materials nanoparticles promotes its dispersion in the polymeric matrix, and the obtained properties are strongly related to the homogeneity of the dispersion. In the present work, nylon 6.12 nanocomposites with different concentrations of pseudoboehmite obtained by sol-gel process were prepared with different concentrations of octadecylamine. The pseudoboehmite was characterized by X-ray diffraction, scanning electron microscopy, differential thermal analysis and thermo gravimetric analysis. The nanocomposites were characterized by thermal and mechanical tests. The addition of pseudoboehmite reduces the melting flow, evidencing the interaction of pseudoboehmite with the polymeric matrix probably modifying its crystalline structure.

Synthesis of Magnesium Oxide Nanoparticles by Sol-Gel Process

2007 ◽  
Vol 558-559 ◽  
pp. 983-986 ◽  
Author(s):  
Rizwan Wahab ◽  
S.G. Ansari ◽  
M.A. Dar ◽  
Young Soon Kim ◽  
Hyung Shik Shin
Keyword(s):  
Magnesium Oxide ◽  
Sol Gel ◽  
Thermo Gravimetric Analysis ◽  
Magnesium Nitrate ◽  
Oxide Nanoparticles ◽  
Gravimetric Analysis ◽  
Magnesium Oxide Nanoparticles ◽  
Good Crystallinity ◽  
Sol Gel Process ◽  
Diffraction Patterns

Cubic shaped Magnesium oxide nanoparticles were successfully synthesized by sol-gel method using magnesium nitrate and sodium hydroxide at room temperature. Hydrated Magnesium oxide nanoparticles were annealed in air at 300 and 500°C. X-ray diffraction patterns indicate that the obtain nanoparticles are in good crystallinity, pure magnesium oxide periclase phase with (200) orientation. Morphological investigation by FESEM reveals that the typical sizes of the grown nanoparticles are in the range of 50-70nm. Powder composition was analyzed by the FTIR spectroscopy and the results confirms that the conversion of brucite phase magnesium hydroxide in to magnesium oxide periclase phase was achieved at 300°C.The Thermo-gravimetric analysis showed the phase transition of the synthesized magnesium oxide nanoparticles occurs at 280-300°C.

Nano Composite Membranes of Sulfonated Poly(2,6-Dimethyl-1,4-Phenylene Oxide)/Poly(2,6-Diphenyl-1,4-Phenylene Oxide) Copolymer and SiO2 for Fuel Cell Application

2007 ◽  
Vol 26-28 ◽  
pp. 835-838 ◽  
Author(s):  
Young Gi Jeong ◽  
Hye Seok Park ◽  
Dong Wan Seo ◽  
Seung Woo Choi ◽  
Whan Gi Kim
Keyword(s):  
Chlorosulfonic Acid ◽  
Composite Membranes ◽  
Sio2 Nanoparticles ◽  
Scanning Calorimetry ◽  
Nano Composite ◽  
Acid Copolymer ◽  
Phenylene Oxide ◽  
20 Nm ◽  
Sulfonated Poly ◽  
Dimethyl Phenol

The Sulfonated poly(2,6-dimethyl-1,4-phenylene oxide) / poly(2,6-diphenyl-1,4-phenylene oxide) (S-PPO) was prepared by oxidative coupling polymerization with 2,6-dimethyl phenol, 2,6-diphenyl phenol, CuCl(І) and pyridine, and followed sulfonation with chlorosulfonic acid. Copolymer was consisted of 2,6-diphenyl phenol 30 mol% and 2,6-dimethyl phenol 70 mol%. Organic-inorganic nano composite membranes were prepared with copolymer and a series of SiO2 nanoparticles (20 nm, 4, 7 and 10 wt%). The composite membranes were cast from dimethylsulfoxide solution. The membranes were studied by differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Sorption experiments were conducted to observe the interaction of sulfonated polymers with water and methanol. S-PPO copolymer and nano composite membranes exhibited proton conductivities from 0.79×10-3 to 0.98×10-3 S/cm, water uptake from 21.70 to 24.77 %, IEC from 0.720 to 0.955 meq/g and methanol diffusion coefficients from 2.97×10-7 to 3.70×10-7 cm2/S.

Preparation and Characterization of Sulfonated Poly(ether Sulfone) Using 4,4-Bis(4-Hydroxylphenyl)valeric Acid for Proton Exchange Membrane Fuel Cell Application

2009 ◽  
Vol 620-622 ◽  
pp. 73-76 ◽  
Author(s):  
Dong Wan Seo ◽  
Young Don Lim ◽  
M. S. Islam Mollah ◽  
Soon Ho Lee ◽  
Sang Ho Moon ◽  
...  
Keyword(s):  
Proton Exchange Membrane ◽  
Thermo Gravimetric Analysis ◽  
Proton Exchange ◽  
Valeric Acid ◽  
Gravimetric Analysis ◽  
Scanning Calorimetry ◽  
Fuel Cell Application ◽  
Exchange Membrane ◽  
Sulfonated Poly

Poly(ether sulfone)s (PES) containing 25-75 mol % valeric acid were prepared with bisphenol A, bis(4-chlorophenyl)sulfone and 4,4-Bis(4-hydroxylphenyl)valeric acid using potassium carbonate in DMAc (dimethylacetamide) at 160 °C. Copolymers containing carboxylacid group were reduced to hydroxy group by BH3 solution 1M in THF and NaBH4 co-catalyst. Sulfonated poly(ether sulfone)s (S-PES) were obtained by reaction of 1,3-propanesultone and the reduced copolymer (PES-OH) with potassium t-butoxide. A series of copolymers were studied by 1H-NMR spectroscopy, differential scanning calorimetry (DSC), and thermo gravimetric analysis (TGA). Sorption experiments were conducted to observe the interaction of sulfonated polymers with water and methanol. The S-PES membranes exhibited proton conductivities from 1.20  10-3 to 3.40  10-3 S/cm, water swell from 12.25 to 31.50 %, IEC from 0.43 to 0.72 meq/g and methanol diffusion coefficients from 3.60  10-7 to 4.90  10-7 cm2/S at 25 °C.

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