Free-standing composite proton conducting film and preparation method thereof
A proton-conducting membrane and proton-conducting technology, applied in cable/conductor manufacturing, conductive layers on insulating carriers, circuits, etc., can solve problems such as application limitations, increase the complexity of membrane electrode preparation, and achieve high dimensional stability and durability Thermal properties, low methanol permeability, and the effect of solving existing technical problems
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Embodiment 1
[0038] Step 1: Prepare a sacrificial layer. Poly(p-styrenesulfonic acid) (PSS, Aldrich) was dissolved in deionized water to prepare a 5 wt% aqueous solution of PSS. Place the substrate on a spin coater at 3000 rpm for 1 minute to spin coat the PSS sacrificial layer.
[0039] Step 2: Prepare the organic layer. A polymer of formaldehyde, (chloromethyl)oxirane and 2-methylphenol (PCGF, Aldrich) was mixed with polyethyleneimine (PEI, Aldrich) in chloroform at a mass ratio of 1:1 to prepare 1 wt% solution. Spin-coat the PEI / PCGF organic layer on the substrate obtained in step 1 at 3000 rpm for 1 minute.
[0040] Step 3: Prepare the inorganic layer. Ethyl orthosilicate: n-propanol: water: hydrochloric acid: C 16 h 33 (OC 2 h 4 ) 10 OH (CEO, Aldrich) = 1: 11.4: 5: 0.004: 0.1 ratio preparation (CEO) SiO 2 Sol. Spin coat surfactant-containing SiO at 3000 rpm for 1 min 2 layer on the substrate obtained in step 2.
[0041] Step 4: Submerge the substrate in water to dissolve th...
Embodiment 2
[0043] Step 1: Prepare a sacrificial layer. Dissolve PSS in deionized water to prepare a 50 wt% PSS aqueous solution. Place the substrate on a spin coater at 10,000 rpm for 1 minute to spin coat the PSS sacrificial layer.
[0044] Step 2: Prepare the organic layer. PCGF and PEI were mixed in chloroform at a mass ratio of 1:1 to prepare a 50 wt% solution. Start the spin coater, and coat the PEI / PCGF organic layer on the substrate obtained in step 1.
[0045] Step 3: Prepare the inorganic layer. First, tetraethyl orthosilicate, deionized water, and hydrochloric acid were mixed according to the ratio of 1:4:4×10 -3 The molar ratio was vigorously stirred at room temperature for 30 minutes. Then according to 5%P 2 o 5 -95% SiO2 2 The molar percentage of phosphoric acid was slowly added to the solution and stirred for 20 minutes. The prepared sol was dropped on the substrate in step 2, held at 1000 rpm for 1 minute, spin-coated to obtain a phosphosilicate layer.
[0046] S...
Embodiment 3
[0049] Step 1: Prepare a sacrificial layer. Dissolve PSS in deionized water to prepare a 0.1 wt% PSS aqueous solution. Put the substrate on the spin coater, keep it at 100 rpm for 5 minutes, start the spin coater with rotation, and coat the PSS sacrificial layer.
[0050] Step 2: Prepare the organic layer. PEI was dissolved in chloroform to prepare a 0.01 wt% solution. Start the spin coater at 100 rpm, hold for 1 minute, and spin coat the PEI organic layer on the substrate obtained in step 1.
[0051] Step 3: Prepare the inorganic layer. zirconium n-butoxide: acetylacetone: water: propanol: surfactant F127 (BASF Corporation) = 1:5:5:20:0.01 ratio to prepare the sol. Dilute zirconium n-butoxide in butanol in proportion, add acetylacetone and water, stir at room temperature for 1h; surfactant F127 was dissolved in 5 times the volume of butanol and stirred at room temperature for 1 h; the above two solutions were mixed and stirred continuously at room temperature for 2 h ...
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