Curing resin composition and semiconductor device employing same
A technology of curable resin and composition, which can be used in semiconductor devices, semiconductor/solid-state device parts, electric solid-state devices, etc., and can solve problems such as lack of records
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[0204] Hereinafter, the present invention will be described in more detail with reference to examples, but the present invention is not limited to these examples.
[0205] reaction products and products 1 H-NMR analysis can be performed using JEOLECA500 (500MHz). In addition, the measurement of the number-average molecular weight and weight-average molecular weight of the reaction product and the product can use AllianceHPLC system 2695 (manufactured by Waters), RefractiveIndexDetector2414 (manufactured by Waters), chromatographic column: TskgelGMH HR -M×2 (manufactured by Tosoh Co., Ltd.), guard column: TskgelguardcolumnH HR L (manufactured by Tosoh Co., Ltd.), column oven: COLUMN HEATERU-620 (manufactured by Sugai), solvent: THF, and measurement conditions: 40°C.
[0206] [Polyorganosiloxane (A)]
[0207] As the polyorganosiloxane (A), the following products were used.
[0208] GD-1125A: manufactured by Changxing Chemical Industry Co., Ltd., vinyl content 1.13% by weight...
Synthetic example 1
[0214] 15.86 g of phenyltriethoxysilane (manufactured by Shin-Etsu Chemical Co., Ltd.) and 6.16 g of methyl isobutyl ketone (MIBK) were charged into the reaction vessel, and the mixture thereof was cooled to 10°C. To the above mixture were added dropwise 4.32 g of water and 0.16 g of 5N hydrochloric acid (2.4 mmol as hydrogen chloride) over 1 hour. After the dropwise addition, their mixture was kept at 10°C for 1 hour. Thereafter, 26.67 g of MIBK was added to dilute the reaction solvent.
[0215] Next, the temperature of the reaction container was raised to 70° C., and when the temperature reached 70° C., 0.16 g (25 mmoles as hydrogen chloride) of 5N hydrochloric acid was added, and polycondensation reaction was performed in a nitrogen atmosphere for 4 hours.
[0216] Then, 11.18 g of divinyltetramethyldisiloxane and 3.25 g of hexamethyldisiloxane were added to the reaction solution, and a silylation reaction was performed at 70° C. for 4 hours. Thereafter, the reaction solu...
Synthetic example 2
[0227] Feed 210.9g of 3-glycidoxypropyltrimethoxysilane, 20.8g of tetraethoxysilane, 210.9g of methanol, 20.8g of ethanol and 17.4g of potassium fluoride (1% ethanol solution) in the reaction vessel, And their mixture was warmed to 50°C.
[0228] Next, 16.2 g of water and 16.2 g of ethanol were dripped over 30 minutes, and after further heating up, polycondensation reaction was performed under reflux for 4 hours.
[0229] Thereafter, volatile components were distilled off while raising the temperature to 80° C. under normal pressure. Thereafter, the remaining volatile components were distilled off while heating up to 100° C. under reduced pressure (30 Torr), to obtain a colorless and transparent liquid reaction product (141.5 g).
[0230] [Zinc compound (E)]
[0231] As the zinc compound (E), the following products were used.
[0232] Zinc octanoate: manufactured by Nippon Chemical Industry Co., Ltd., trade name "NIKKAOcthix Zinc" (Zn: 15%)
[0233]
[0234] Examples 1-5...
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