Dry etching gases and method of dry etching
A dry etching and gas technology, used in electrical components, semiconductor/solid-state device manufacturing, circuits, etc., can solve the problem of high industrial cost, achieve the effect of small impact, safe use and short life
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[0097] The following examples are given to illustrate the present invention in more detail, but the present invention is not limited to the following examples. It should be noted that, unless otherwise specified, "parts" means "parts by weight".
[0098] In addition, the purity and yield of a compound were determined by the following GC (gas chromatography) analysis.
[0099] Measuring machine: G-5000 manufactured by Hitachi, Ltd.
[0100] Column: Neutrabond-1 (length 60m, inner diameter 0.25mm, film thickness 1.5μm)
[0101] Column temperature: fixed at 40°C for 10 minutes, then raised to 240°C within 10 minutes
[0102] Injection temperature: 200°C
[0103] Carrier gas: nitrogen (flow 1mL / min)
[0104] Detector: FID, sample volume: 1 μl
[0105] Internal standard: n-butane
preparation example 1
[0106] [Preparation Example 1] Preparation of a sample for dry etching of bis(trifluorovinyl)ether
[0107] (1-a) FOCCF 2 CF 2 OCF (CF 3 ) Synthesis of COF
[0108] This compound was synthesized according to the description in Dutch Patent No. 6605656 (Chemical Abstracts, Vol. 66, 65088s).
[0109] The autoclave made of SUS316 was fully dried and placed in an argon atmosphere. 5 parts of cesium fluoride, 50 parts of dry diethylene glycol dimethyl ether, and 90 parts of difluoromalonyl difluoride (manufactured by SynQuest) were charged into the autoclave, and the reactor was immersed in a dry ice / acetone bath and cooled. to -78°C.
[0110] 98 parts of hexafluoropropylene oxide (manufactured by SynQuest) were slowly supplied into the autoclave through a cylinder. The reaction mixture was stirred at -78°C for 3 hours. The reaction mixture was separated into two layers, and only the lower layer was taken out from the bottom valve of the autoclave. The separated lower layer...
manufacture example 2
[0116] [Production Example 2] Preparation of a sample for dry etching of hexafluoro-3-pentyn-2-one
[0117] (2-a) Synthesis of Trifluoroacetylmethylenetriphenylphosphorane
[0118] This compound was synthesized according to the method described in literature (Synthesis, 1984, Vol. 11, 924).
[0119] The glass reactor equipped with a three-way stopcock was fully dried and placed in an argon atmosphere. 250 parts of methyl triphenyl bromide (manufactured by Tokyo Chemical Industry Co., Ltd.) and 2500 parts of dry diethyl ether were placed in this reactor, and the reactor was cooled to -78°C. 392 parts of a 1.9 M cyclohexane-diethyl ether solution of phenyllithium (manufactured by Kanto Chemical Co., Ltd.) was slowly dropped there, and stirred for 1 hour. Further, a solution obtained by dissolving 66 parts of ethyl trifluoroacetate (manufactured by Tokyo Chemical Industry Co., Ltd.) in dry diethyl ether was slowly added dropwise at -78°C, followed by stirring for 1.5 hours. Th...
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