Polybenzoxazole and Its Utilization
A technology of polybenzoxazole and precursor, applied in the field of polybenzoxazole and its utilization, can solve problems such as unfavorable manufacturing cost, complicated manufacturing engineering, lack of gas barrier properties and the like
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[0097] The following examples are given to describe the present invention more specifically, but the present invention is not limited to the following examples. In addition, the apparatuses used are as follows.
[0098] (1)FT-IR
[0099] Device: Made by Thermo Fisher Scientific Inc., NEXUS 670FTIR
[0100] (2) Molecular weight measurement: Manufactured by Showa Denko Co., Ltd., normal temperature gel permeation chromatography (GPC) apparatus (GPC-101) and column (KD-803L) made by Shodex
[0101] (measurement conditions)
[0102] Column temperature: 40°C
[0103] Eluent: Dimethylformamide (DMF), 10mL / L
[0104] Flow rate: 1.0mL / min
[0105]Standard sample for calibration curve creation: Showa Denko Co., Ltd., SL-105, standard polystyrene (molecular weight: about 580, 2970, 7200, 19900, 52400)
[0106] (3) Film thickness measurement: Micro shape measuring machine Surfcorder ET-4000 manufactured by Kosaka Laboratories Co., Ltd.
[0107] (4) Water vapor transmission rate: s...
manufacture example 1
[0118] Dissolve PDA20.261g (0.1875mol) and DATP12.206g (0.0469mol) in NMP617.4g, after cooling to 15°C, add PMDA50.112g (0.2298mol), and make it react at 50°C under nitrogen atmosphere for 48 Hour. The weight average molecular weight Mw of the obtained polymer was 82100, and the molecular weight distribution was 2.7. This polyamic acid was apply|coated on the glass substrate with the bar coater. This substrate was baked on a hot plate at 80° C. for 30 minutes, and further baked in an oven at 450° C. for 1 hour after depressurizing to obtain a polyimide-attached glass substrate with a film thickness of 11 μm.
[0119] [2] Production of polybenzoxazole precursor (film-forming composition)
Embodiment 1-1
[0120] [Example 1-1] Production of precursor [3]
[0121] [chemical 10]
[0122]
[0123] AHPE[2]0.851g (3.66mmol) was dissolved in NMP18g, and CBOCCl[1]1.149g (3.59mmol) was added, and it stirred at room temperature for 24 hours. Then, the obtained solution was poured into 500 mL of pure water. The obtained precipitate was separated by filtration, and then dried under reduced pressure at 80° C. for 24 hours to obtain the target precursor [3] (95% yield). The obtained precursor [3] had a weight average molecular weight Mw of 142,000 and a molecular weight distribution of 8.8. In addition, by FTIR measurement, it was confirmed that the 3300 cm from the phenolic hydroxyl group -1 and the peak from the amido group at 1651 cm -1 peak.
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