High purity phenyl silicone ladder polymer and method for producing the same
First Claim
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1. High purity phenyl silicone ladder polymer, which contains therein 1 ppm or below of each of sodium, potassium, iron, copper, lead and chlorine, and 1 ppb or below of each of uranium and thorium, and which is represented by the following formula (I):
- ##STR15## where R1 and R4 denote respectively hydrogen or a lower alkyl group; and
n is an integer of from 8 to 1,600.
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Abstract
High purity phenyl silicone ladder polymer, and a method for producing such polymer, suitable for use as the protective film, the interlayer insulating film, etc. in the fabrication of semiconductor elements, which polymer contains therein 1 ppm or below of each of sodium, potassium, iron, copper, lead and chlorine, and 1 ppb or below of each of uranium and thorium, and which is represented by the following general formula (I): ##STR1## (where: R1 to R4 denote respectively hydrogen or a lower alkyl group; n is an integer of from 8 to 1,000); or the following general formula (II): ##STR2## (where: n is an integer of from 8 to 1,600).
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Citations
11 Claims
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1. High purity phenyl silicone ladder polymer, which contains therein 1 ppm or below of each of sodium, potassium, iron, copper, lead and chlorine, and 1 ppb or below of each of uranium and thorium, and which is represented by the following formula (I):
- ##STR15## where R1 and R4 denote respectively hydrogen or a lower alkyl group; and
n is an integer of from 8 to 1,600. - View Dependent Claims (2, 3, 4, 5, 6, 7)
- ##STR15## where R1 and R4 denote respectively hydrogen or a lower alkyl group; and
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8. A method for producing high purity phenyl silicone ladder polymer, which contains therein 1 ppm or below of sodium, potassium, iron, copper, lead and chlorine, and 1 ppb or below of each of uranium and thorium, and which is represented by the following formula (I):
- ##STR16## where R1 to R4 are respectively a lower alkyl group; and
n is an integer of from 8 to 12,said method being characterized by dissolving phenyl tri(lower)alkoxy silane in an organic solvent;
dripping super-demineralized water containing 0.02-0.23 mol hydrogen chloride based on 1 mol phenyl tri(lower)alkoxy silane into said phenyl tri(lower)alkoxy silane, under cooling, thereby hydrolyzing said compound; and
thereafter washing said hydrolyzed substance with super-demineralized water.
- ##STR16## where R1 to R4 are respectively a lower alkyl group; and
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9. A method for producing high purity phenyl silicone ladder polymer, which contains therein 1 ppm or below of sodium, potassium, iron, copper, lead and chlorine, and 1 ppb or below of each of uranium and thorium, and which is represented by the following formula (I):
- ##STR17## where R1 to R4 are respectively a lower alkyl group; and
n is an integer of from 13 to 1,000,said method being characterized by the steps of;
dissolving phenyl tri(lower)alkoxy silane in an organic solvent;
dripping super-demineralized water containing 0.02-0.23 mol hydrogen chloride based on 1 mol phenyl tri(lower)alkoxy silane into said solvent solution of phenyl tri(lower)alkoxy silane, under cooling, thereby hydrolyzing said compound;
then washing the resulting hydrolyzed substance with super-demineralized water;
thereafter subjecting said solution containing therein said hydrolyzed substance to dehydration-condensation reaction by addition of a nucleophilic reagent; and
finally refining the thus obtained high molecular weight substance by a dissolution-and-reprecipitation method.
- ##STR17## where R1 to R4 are respectively a lower alkyl group; and
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10. A method for producing high purity phenyl silicone ladder polymer, which contains therein 1 ppm or below of sodium, potassium, iron, copper, lead and chlorine, and 1 ppb or below of each of uranium and thorium, and which is represented by the following formula (II):
- ##STR18## where n is an integer of from 8 to 16, said method being characterized by the steps of;
dissolving phenyl trichlorosilane in an organic solvent;
dripping super-demineralized water into said solvent solution of phenyl trichlorosilane, under cooling, to hydrolyze said compound; and
thereafter washing the resulting hydrolyzed substance with super-demineralized water.
- ##STR18## where n is an integer of from 8 to 16, said method being characterized by the steps of;
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11. A method for producing high purity phenyl silicone ladder polymer, which contains therein 1 ppm or below of sodium, potassium, iron, copper, lead and chlorine, and 1 ppb or below of each of uranium and thorium, and which is represented by the following formula (II):
- ##STR19## where n is an integer of from 17 to 1,600, said method being characterized by the steps of;
dissolving phenyl trichlorosilane in an organic solvent;
dripping super-demineralized water into said solvent solution of phenyl trichlorosilane, under cooling, thereby hydrolyzing said compound;
then washing the resulting hydrolyzed substance with super-demineralized water;
subsequently adding a nucleophilic reagent to said organic solvent phase to subject said hydrolyzed substance to dehydration-condensation reaction under heat; and
refining the resulting high molecular weight substance by a dissolution-and-recipitation method.
- ##STR19## where n is an integer of from 17 to 1,600, said method being characterized by the steps of;
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Current AssigneeMitsubishi Denki Kabushiki Kaisha (Mitsubishi Electric Corporation)
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Original AssigneeMitsubishi Denki Kabushiki Kaisha (Mitsubishi Electric Corporation)
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InventorsAdachi, Etsushi, Okahashi, Kazuo, Adachi, Hiroshi, Hayashi, Osamu
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Primary Examiner(s)Marquis, Melvyn I.
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Application NumberUS07/437,826Time in Patent Office788 DaysField of Search528/12, 528/43, 556/489US Class Current528/43CPC Class CodesC08G 77/16 to hydroxyl groupsC08G 77/18 to alkoxy or aryloxy groupsC08G 77/34 Purification
