Amorphous perfluorinated polymers

A perfluorinated, polymer technology, which is applied in the direction of originals for photomechanical processing, photographic process for patterned surfaces, photosensitive materials for photomechanical equipment, etc., and can solve the problem of unrecorded polymer transmittance values question

Inactive Publication Date: 2007-11-21
SOLVAY SOLEXIS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A polymer with a transmittance value higher than 95% at a wavelength of 200nm is described in the examples, but the transmittance value of this polymer at a wavelength of 157nm is not described
And there is no hint that you can choose a fluoropolymer with high transmission at 157nm wavelength

Method used

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  • Amorphous perfluorinated polymers
  • Amorphous perfluorinated polymers
  • Amorphous perfluorinated polymers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0084] Embodiment 1 (comparative example)

[0085] A copolymer of TFE / TTD=20 / 80 was prepared using an AISI 316 reactor and at a temperature of 75°C.

[0086] After evacuating with an oil pump, 2,790 ml of demineralized water was added to a 5 liter AISI 316 autoclave equipped with a stirrer at 650 rpm, followed by mixing the following materials to obtain a 6.67 g / l water microemulsion:

[0087] 7.5ml of perfluoropolyoxyalkylene with acid end groups, the general formula of this perfluoropolyoxyalkylene is:

[0088] CF 2 ClO(CF 2 -CF(CF 3 )O) n (CF 2 O) m CF 2 COOH

[0089] Wherein n / m=10, the average molecular weight is 600;

[0090] -30% volume NH 3 7.5ml of aqueous solution;

[0091] -15ml demineralized water;

[0092] - 4.5ml of Galden with the following general structure  D02:

[0093] CF 3 O(CF 2 -CF(CF 3 )O) n (CF 2 O) m CF 3

[0094] Where n / m=20, the average molecular weight is 450.

[0095] The autoclave was heated to 75° C. and 33.3 (g / l water)...

Embodiment 1A

[0097] Embodiment 1A (comparative example)

[0098] The ionic labile groups of the copolymer obtained from Example 1 were fluorinated (comparative).

[0099] Dissolving the perfluorinated solvent Galden obtained by embodiment 1 (comparative example)  The 420g 5%wt copolymer solution of D100 (perfluoropolyether having a boiling point of 100°C) was added to a 300ml photochemical glass reactor equipped with a mechanical stirrer and a mercury vapor-immersed ultraviolet lamp (Hanau TQ150 ). Inject nitrogen gas into the solution for 1 hour until oxygen is completely eliminated, and then input a nitrogen / fluorine mixture with a volume ratio of 1:1 at a temperature of 25°C under ultraviolet irradiation for 30 hours. After the reaction is completed, remove it by reducing pressure. Residual fluorine and solvents.

[0100] After 13 hours of fluorination, 1 mmol / kg of residual COOH end groups and 1.4 mmol / kg of COF end groups formed by the reaction were still found by infrared spectr...

Embodiment 2

[0105] Preparation of Copolymer of TFE / TTD=3 / 97(mol)

[0106] After evacuating with an oil pump, in a 1-liter autoclave equipped with magnetic stirring, add 350 ml of demineralized water and 15 ml of microemulsion obtained by mixing the following materials:

[0107] - 1.486 ml of perfluoropolyoxyalkylenes having acid end groups of the general formula:

[0108] CF 2 ClO(CF 2 -CF(CF 3 )O) n (CF 2 O) m CF 2 COOH

[0109] Wherein n / m=l0, average molecular weight is 600;

[0110] - 1.486ml of 30% volume NH 3 aqueous solution

[0111] - 2.973ml of demineralized water;

[0112] -9.054ml of Galden with the following general structure  D02:

[0113] CF 3 O(CF 2 -CF(CF 3 )O) n (CF 2 O) m CF 3

[0114] Where n / m=20, the average molecular weight is 450;

[0115] 174g of TTD was added. 0.72 g of gaseous tetrafluoroethylene (TFE) at 0.03 MPa was charged to the reactor. Then 0.1 g of ammonium persulfate was added. The autoclave was heated to 50°C. After 12 hours t...

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Abstract

Use of amorphous perfluorinated polymers for preparing transparent films at 157 nm, said perfluorinated polymers being free from unstable ionic end groups COF, COOH or their amidic derivatives, esters or salts, said polymers formed by cyclic units deriving from perfluorodioxoles of formula: wherein R'F is equal to RF or ORF wherein RF is a perfluoroalkyl radical having 1-5 carbon atoms; X1 and X2, equal to or different from each other, are F, CF3; said polymers optionally containing units deriving from perfluorinated comonomers optionally containing oxygen atoms; in said polymers the cyclic units deriving from the perfluorodioxoles of formula (IA) being >= 95% by moles.

Description

technical field [0001] The present invention relates to an amorphous perfluorinated polymer having a transmittance greater than 50%, preferably greater than 55%, at a wavelength of 157 nm. The polymer does not contain labile ionic end groups, particularly COF, COOH or their corresponding esters, salts or amic acid derivatives, as determined by the method reported below. [0002] More specifically, the present invention relates to amorphous perfluorinated polymers containing specific cyclic perfluorinated structures. As said, this polymer is characterized by a high transmittance at a wavelength of 157nm, at which it can be used as a protective film in semiconductor production by microlithography. [0003] It is well known that for an amorphous perfluorinated polymer to be useful for microlithographic applications, the polymer must have the smallest possible absorption for incident light of a certain wavelength, especially at 248 nm and 193 nm. Transparent films are also requi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F34/02C08J5/18G03F7/11C08F214/18C08J5/22G03F1/14H01L21/027
CPCC08F34/02A47G19/2227
Inventor V·阿尔切拉M·阿波斯托洛F·特留尔兹
Owner SOLVAY SOLEXIS
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