JPH11176750A - Photoresist composition which can be developed by water base and pattern formation by using the same - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain high resolution which enables development by water base, by adding film formation polymer resin with phenol group by a specified formula, glycol uril derivative cross linking agent, radiolysis acid generation agent and organic base. SOLUTION: A photoresist composition comprises film formation polymer resin with phenol group. The phenol resin is copolymer of hydroxystyrene and hydroxycyclohexyl ethene shown by a formula I (n>1, 0<X<1 in the formula). It comprises glycol uril derivation cross linking agent of a formula II (R, R express a 1-6 C alkyl, alkenyl, etc., in the formula) which forms cross linking reacting on phenol group by acid catalyst. It further comprises photodissociating acid generation agent by a formula III which forms acid catalyst which is necessary for cross linking formation on exposure by ultraviolet radiation, and organic base such as tertiary amine which increases storage stability of formula and adjusts photo reaction velocity.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to a photoresist composition developable with an aqueous base and a method for forming a lithographic pattern using the same.

[0002]

BACKGROUND OF THE INVENTION There is an ongoing effort in the electronics industry to achieve higher circuit densities of electronic components. To achieve higher densities, new and improved lithographic apparatus and techniques have been developed, which requires new photoresists that allow for increased resolution of lithographic patterns.

A photoresist composition which can be developed with an aqueous base formed by crosslinking is described in Reck et al.
regional Technical Conference on Photopolymers, E
llenville, NY, 63 (1988) "and U.S. Pat.
Nos. 4304 and 5204225. The features of these formulations are an aromatic group such as poly (hydroxystyrene) and novolak that can be easily substituted with an electrophilic aromatic compound, a crosslinking agent that can generate carbonium ions when treated with an acid, and a photoacid generator. Was to have.

US Pat. No. 4,810,601 relates to the formation of a negative tone resist pattern by cross-linking an aromatic compound with a monomeric or polymeric carbonium ion source. For example, diacetoxymethylbenzene and triacetoxymesitylene have been used with triphenylsulfonium hexafluoroantimonate to crosslink a poly (hydroxystyrene) matrix.

[0005] US Pat. No. 5,296,332, and Japanese Patent Publication Nos. 2-15270 and 1-293339 describe cross-links which can produce carbonium ions when treated with a phenolic resin, such as poly (hydroxystyrene) or novolak, or an acid. An aqueous base developable resist composition comprising an agent and a photoacid generator is described.

[0006]

SUMMARY OF THE INVENTION It is an object of the present invention to provide an aqueous base developable, high resolution photoresist composition for use in deep ultraviolet and i-ray exposure.

[0007]

The broad aspects of the present invention are:
Less than quarter micron negative on the substrate
An aqueous base developable photoresist composition for producing a toned resist image. Another aspect of the invention is a photoresist composition that does not form microbridges between the resist images on the substrate. The photoresist composition comprises (a) a film-forming polymer resin having a phenol group, (b) an acid-catalyzed cross-linking agent selected from aminoplasts, more specifically, glycoluril derivatives, (c) a film-forming agent, A radiolytic acid generator to assist in crosslinking of the crosslinking agent, and (d) an organic base to optionally improve the storage stability of the formulation. The phenolic resin of the present invention may be a poly (hydroxystyrene), a partially protected poly (hydroxystyrene), a copolymer of hydroxystyrene and vinylcyclohexanol represented by the following formula 8, or a compound represented by the following general formula 9: Selected from the indicated novolak (phenol-formaldehyde) resins.

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The crosslinking agent of the composition is selected from glycoluril derivatives represented by the following formula 10, wherein R
Is an alkoxy group, preferably CH ₂ OCH ₃ , and R ₁
And R ₂ can be individually selected from H, an alkyl group, or an aryl group. The compositions of the present invention also include a radiolytic acid generator.

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Another broad aspect of the invention resides in the synthesis of novel glycoluril derivatives that act as crosslinkers for the composition.

The present invention further comprises: a) a film-forming polymer resin having a phenolic function;
An acid-catalyzed crosslinking agent selected from glycoluril derivatives,
And b) exposing the coating to ultraviolet radiation imagewise to crosslink the exposed portions of the coating, and c) firing the substrate at an elevated temperature. Providing a negative tone resist image on a substrate using the novel resist composition, comprising the steps of: d) developing the coating in an aqueous base developer.

The composition is sensitive to deep UV radiation. The resist speed can be adjusted by adjusting the ratio of crosslinker to polymer resin, adding an organic base, or selecting partially protected poly (hydroxystyrene) or novolak, or a combination thereof.

[0012]

DETAILED DESCRIPTION OF THE INVENTION The present invention provides a negative
A high resolution, aqueous base developable photoresist composition for producing toned images. These compositions comprise (a) a film-forming polymer resin having a phenol group, (b) a glycoluril derivative crosslinking agent capable of forming a crosslink by reacting with a phenol group with an acid catalyst, and (c) exposure to ultraviolet radiation. Then, a photo-decomposable acid generator for forming an acid catalyst required for crosslinking, and (d)
Includes an organic base, such as a tertiary amine, which is optionally added to increase the storage stability of the formulation and adjust the photoreaction rate. The polymer resin having a phenol group is selected from poly (hydroxystyrene) represented by the following formula 11, partially protected poly (hydroxystyrene), or a copolymer of hydroxystyrene and vinylcyclohexanol.

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In the above formula, R is a C _1-4 alkyl group, acetyl group, hydroxyalkyl group, acetoxyalkyl (C
H ₃ COOR-) and it is possible to, y is any number of 0.5 to 1, n is> 1, preferably from> 20, most preferably 20 <n <100. A preferred crosslinking agent for the composition of the present invention is a glycoluril derivative of general formula 12 below.

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In the above formula, R is alkoxyalkyl, preferably CH ₂ OCH ₃ , and R ₁ and R ₂ can be independently selected from alkyl groups having 1 to 6 carbon atoms. (A) tetrakis-methoxymethyl-3a, 6a-diethylglycoluril (b) tetrakis-methoxymethyl-3a-methyl-6
a-propylglycoluril, and (c) tetrakis-methoxymethyl-3a-methyl-6
There is a-butyl glycoluril.

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R ₁ and R ₂ may also be an alkyl group and an aryl group, or a hydrogen and an aryl group. Preferred examples of the crosslinking agent include (d) tetrakismethoxymethyl-3a-phenyl represented by the following formula (14). Glycoluril, and (e) tetrakis-methoxymethyl-3a-methyl-6
There is a-phenylglycoluril.

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R ₁ and R ₂ may both be an aryl group such as phenyl, furyl or alkylphenyl, and an aryl halide, or a substituted diphenyl ether group. Preferred examples of the crosslinking agent include (f) )-(H).

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The composition of the present invention is also disclosed in US Pat.
A photoacid generator (PAG) which can be selected from the group IV onium salts disclosed in US Pat. No. 5,972, and the group Va aromatic onium salts disclosed in US Pat. No. 4,690,055. preferable. The aromatic Group IVa onium salts include those represented by Formula 16 below.

[(R) _a (R ¹ ) _b (R ² ) _c x] d ⁺ [MQ _e ] ^-(ef)

In the above formula, R is a monovalent aromatic organic group, R ¹ is a monovalent organic aliphatic group selected from alkyl, cycloalkyl and substituted alkyl, and R ² is a heterocyclic or condensed ring structure. It is a polyvalent organic group that forms. x is a group IVa element or metalloid, Q is a halogen group, a is an integer of 0 to 3, b is an integer of 0 to 2, and c is an integer of 0 or 1.

The group contained in R is, for example, phenyl,
(C ₆ such as toril, xylyl, naphthyl, anthryl
—C ₁₄ ) an aromatic hydrocarbon group, alkyl of C _(1-8) , C
_(1-8) alkoxy-, nitro-, chloro-, fluoro-, and hydroxy-substituted monovalent groups such as hydroxy, arylacyl groups such as phenylacetyl, and aromatic heterocyclic groups such as pyridyl and furyl. Yes, the R ¹ group includes substituted alkyls such as C _(1-8) alkyl, —C ₂ H ₄ OCH ₃ , —CH ₂ —COCH ₃ . The R ² group includes a structure as shown in Formula 17 below.

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[0020] MQ _e of the equation ^- complex anion contained in ^(ef), for ^{_{example, BF 4 -, PF 6 -}} , SbF 6 -, FeC
l ₄ ⁻ , SnCl ₆ ⁻ , SbCl ₆ ⁻ , BiCl ₅ ⁻ , AlF ₆
^-3 , GaCl ₄ ⁻ , InF ₄ ⁻ and the like. The group VIa onium salt included in the above formula includes, for example, the following formula 18:

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Non-metallic radiolytic acid generators suitable for use in the compositions of the present invention include N-sulfonyloxyimides of Formula 19:

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In the above formula, R is toluene, benzene, C
F _3, CF ₂ CF _3, is selected from the group consisting of _{(CF 2) n -Z, n} = 1~4 above formula, Z is H, alkyl or aryl,, X and Y are (1) hetero Forming a multi-membered ring with or without atoms, (2) forming a condensed aromatic ring, or (3) independently an H, alkyl or aryl group, wherein C ₁ and C ₂ are single or double. Form a heavy bond.

The composition of the present invention also contains a small amount of a basic compound selected from organic amines, especially tertiary amines.

The composition of the present invention is preferably supported by a solvent or a solvent system. The solvent or solvent system used to support these compositions preferably satisfies the need to provide a uniform coating over the substrate with each resist component. Preferably, the solvent evaporates at a temperature such that the photoactivity of the resist is not adversely affected during the drying step and is not involved in the action of the photoresist (inert with respect to phenolic resin and / or crosslinker). Representative examples of these solvents include propylene glycol monomethyl ether acetate (PGMEA), 3
-Ethyl ethoxypropionate (EEP), methoxypropanol, ethoxypropanol, butoxypropanol and ethyl lactate.

To form a negative tone image, the composition of the present invention is applied to a substrate (such as by spin coating) and the substrate is heated on a hot plate at a temperature of about 70-130.degree. Heat for 3 minutes to evaporate the remaining solvent. The coating is then image-wise exposed to ultraviolet radiation at a wavelength of about 200-370 nm to degrade the radiolytic components of the composition and form a catalytic amount of acid. Next, the substrate is kept at 70 to 130 ° C., preferably 1 to
Heating for 3 minutes accelerates the crosslinking reaction between the phenolic resin and the crosslinking agent. The image is thus rendered sparingly or insoluble in aqueous base, and the unexposed areas are removed during the development step with an aqueous base such as a dilute solution of tetramethylammonium hydroxide (TMAH).

In another embodiment of the present invention, the glycoluril derivative used as the crosslinking agent is synthesized from the corresponding dicarbonyl compound as shown in Scheme 20 below.

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The glycoluril derivatives of the present invention dissolve well in the selected organic solvent and reduce the rate of dissolution of the final composition in the base developer as compared to unsubstituted glycoluril.

General Procedure for the Preparation of Alkyl-Substituted Glycolurils The synthesis of alkyl-substituted glycolurils is illustrated by the synthesis of 3a-methyl-6a-propylglycoluril below. 2,3-Hexadione (1.0 mol) and urea (3.0 mol) were added to 2.0 liters of 2% hydrochloric acid,
The solution was stirred at room temperature for 24 hours (or the solution may be refluxed for 2-3 hours). The precipitate is filtered, washed with water and ethanol and dried. The off-white powder is then recrystallized from acetic acid to give an analytically pure, white compound in 45% yield.

General Procedure for Preparation of Aryl-Substituted Glycolurils Suitable benzyl derivatives (see Scheme 20, R ₁ and R ₂
Is an aryl group or a combination of an alkyl group and an aryl group) (1.0 mol) and urea (0.3 mol) in 300 ml.
And add 5.0 ml of trifluoroacetic acid. The resulting solution was refluxed for 8 hours,
The water is removed using a Stark trap. The solution is cooled to room temperature, the precipitated crystals are filtered, washed with toluene and then with hexane and dried.

Hydroxymethylation of glycoluril A glycoluril derivative (0.10 mol) is suspended in a 37% aqueous formaldehyde solution (0.5 mol) and
% Sodium hydroxide is added to adjust the pH to 10-11. Heat the resulting mixture at 50 ° C. for 24 hours to dissolve all solids into solution. The solution is cooled to room temperature and the water is removed under reduced pressure. The residue (solid or gummy) is used for the next step without further purification.

Etherification of the aminoplast compound The tetrakis-hydroxymethyl glycoluril is converted into the corresponding tetramethoxymethyl derivative by suspension in an excess of 2,2-dimethoxypropane, and then a few drops of concentrated hydrochloric acid are added. The mixture is stirred at room temperature for 24 hours. The solvent is removed under reduced pressure and the residue is recrystallized from a suitable solvent (such as in the case of diaryl or alkylaryl substituted glycolurils) or the oily residue is distilled under high vacuum and high temperature (methylpropyl or methylbutyl substituted glycolurils). To obtain the desired tetrakis-methoxymethyl derivative of glycoluril.

[0032]

The following examples are detailed descriptions of the preparation and use of the method of the present invention. Details of the preparation are within the scope of the more generally described methods above and serve to illustrate them. These examples are provided for illustrative purposes only and do not limit or limit the scope of the invention.

Example 1. Copolymer of 4-hydroxystyrene and vinylcyclohexanol (molar ratio of hydroxystyrene to vinylcyclohexanol is 9: 1) (1
0 g), 3a-methyl-6a-propyl-tetrakis-methoxymethyl glycoluril (1.0 g)
And MDT (trifluoromethylsulfonyloxybicyclo [2.2.1] hept-5-ene-2,3-dicarboximide) (100 mg) in 50 ml of propylene glycol monomethyl ether acetate (PGME)
Dissolve in A). The resulting solution is filtered through a 0.25 micron filter and spin coated on a substrate. After heating to 110 ° C. for 1 minute, the substrate is exposed to 248 nm ultraviolet light of about 20 mJ / cm ² using a 0.5 NA i-line stepper. After post-exposure bake at 110 ° C. for 1 minute, the photoresist is developed with a 0.26 N aqueous solution of tetramethylammonium hydroxide. A clear 220 nm line high resolution image is formed.

Embodiment 2 FIG. Poly (4-hydroxystyrene) (10 grams), tetrakis-tetramethoxymethyl-3a, 6a-bis- [4- (4-tert-butylphenoxy) phenyl] glycoluril (0.45 grams), tetrakis-methoxymethyl Glycoluril (Powderlink) (0.8 grams), and MDT (1.
20 grams) in 50 ml of PGMEA. The solution is spin-coated on a silicon wafer to a dry thickness of 0.5 micrometers and exposed through a mask to about 20 mJ / cm ² of 248 nm ultraviolet light. The substrate was then heated at 110 ° C. for 1 minute,
Develop with a 6N aqueous solution of tetramethylammonium hydroxide and wash with water. When observed with a scanning electron microscope, 0.2
High resolution images up to 2 micrometers are formed.

Embodiment 3 FIG. Poly (hydroxystyrene)
(10 grams), tetrakis-methoxymethyl-3a-
Methyl-6a-butyl glycoluril (1.1 g
) And MDT (1.2 grams) with 50 grams of P
Dissolve in GMEA and pass through a 0.2 micron filter
Filter. Dry the resulting solution on a silicon wafer
Spin coating to about 0.6 microns
I do. Heat the wafer to 95 ° C to remove excess solvent
And 20 mJ / cm using a 0.5 NA stepper. ^Twoof
Exposure with 248 nm ultraviolet light. After exposure, 95
C. for 1 minute and then 0.14N
Develop with an aqueous solution of tillammonium. 200nm line height
A resolution image is formed.

In summary, the following is disclosed regarding the configuration of the present invention.

(1) a phenolic resin or polymer;
Providing an uncured photoresist coating on a substrate comprising a glycoluril derivative and a photoacid generator; exposing the coating to ultraviolet radiation in an image-wise pattern, thereby generating an acid catalyst in the pattern. A method of forming a pattern of a photoresist, comprising the steps of: heating the exposed coating at 90-130 ° C. for 1-2 minutes; and developing the photoresist in an aqueous base solution. (2) The method according to the above (1), wherein the ultraviolet light has a wavelength of about 250 to about 370 nanometers. (3) The method according to the above (1), wherein the phenol resin is poly (4-hydroxystyrene). (4) The method according to the above (1), wherein the phenol resin is a copolymer of hydroxystyrene and hydroxycyclohexylethene represented by the following formula 1, wherein n> 1, and 0 ≦ X ≦ 1.

Embedded image (5) The above (1), wherein the phenol resin is a partially protected poly (hydroxystyrene) represented by the following formula 2, wherein x is a number of 0.5 to 1.0, and R is an organic group. The method described in.

Embedded image (6) The method according to the above (1), wherein the phenol resin is a phenol-formaldehyde (novolak) resin. (7) the glycoluril derivative has the following general formula 3, wherein R ₁ and R ₂ are alkyl having 1 to 6 carbons;
Alkenyl, alkoxy, aryl, (phenyl, furyl, thienyl), tolyl, xylyl, mesityl _{C n H 2n + 1 C 6} H 4 or n is 3-6, - alkyl, such as aryl, halogenated aryl, ether, And the method according to (1) above, which can be individually selected from the group consisting of: and diphenyl sulfide.

Embedded image (8) The method according to (1), wherein the photoacid generator is selected from onium salts of Group IV and Group VIa elements. (9) The method according to (1), wherein the photoacid generator is selected from a sulfonate of N-hydroxyimide. (10) The method according to the above (1), wherein the photoacid generator is a sulfonate having the structure of the following formula 4.

Embedded image (11) providing a coating film of a mixture containing a phenolic resin or polymer, a glycoluril derivative, a photoacid generator, and an organic base on a substrate; exposing the coating film to ultraviolet light in an image-wise pattern; Forming an acid catalyst in the pattern, heating the exposed coating, and developing the photoresist. (12) The phenolic resin or polymer, the glycoluril derivative, the photoacid generator, and the organic base are contained in the phenolic resin or polymer in an amount of about 90-6.
0%, the glycoluril derivative about 5-20%, the photoacid generator about 2-20%, and the organic base about 0.02-
The method according to (11) above, wherein a mixture containing 0.5% is formed. (13) A composition comprising a mixture of a phenolic resin or polymer, a glycoluril derivative, a photoacid generator, and an organic base. (14) The composition according to the above (13), wherein the phenol resin is poly (4-hydroxystyrene). (15) The composition according to the above (13), wherein the phenol resin is a copolymer of hydroxystyrene and hydroxycyclohexylethene represented by the following formula 5, wherein n> 1, and 0 ≦ X ≦ 1.

Embedded image (16) The above (13), wherein the phenol resin is a partially protected poly (hydroxystyrene) represented by the following formula 6, wherein x is a number of 0.5 to 1.0, and R is an organic group.
A composition according to claim 1.

Embedded image (17) The composition according to the above (13), wherein the phenol resin is a phenol-formaldehyde (novolak) resin. (18) The glycoluril derivative has a general formula of the following formula 7, wherein R ₁ and R ₂ are alkyl, alkenyl, alkoxy, aryl, (phenyl, furyl, thienyl) having 1 to 6 carbon atoms, can alkyl such as aryl, halogenated aryl, be individually selected from the group consisting of diphenyl ether and diphenyl sulfide, - tolyl, xylyl, mesityl or n is _{C n H 2n + 1 C 6} H 4 is 3-6, The composition according to the above (13).

Embedded image (19) The composition according to the above (13), wherein the photoacid generator is selected from onium salts of Group IV and Group VIa elements. (20) The composition according to the above (13), wherein the photoacid generator is selected from a sulfonate of N-hydroxyimide. (21) The phenolic resin or polymer, the glycoluril derivative, the photoacid generator, and the organic base are each composed of about 40 to 8 of the phenolic resin or polymer.
0%, about 5 to 25% of the glycoluril derivative, about 2.0 to 20% of the photoacid generator, and about 0.0% of an organic base.
The composition according to (14), which forms a mixture containing 1 to 0.5%.

 ────────────────────────────────────────────────── ─── Continuing the front page (72) Inventor William Ross Brunsvold, United States 12603 Pokekeepsie, Clover Hill Road, New York 22 (72) Inventor Jeffrey Donald Jerome United States 06062 Plainville, Connecticut Hemingway Street 30 (72) Inventor Laura Louise Cosver U.S.A. 10547 Mohegan Lake Houghton Road, New York 1734 (72) Inventor Nancy C. Ravianka United States 06492 Yalesville, Connecticut High Street 45 (72) Inventor Niranjan M Patel United States 12590 Wappingers Falls, New York Navy Street 16 Ai (72) Inventor Pushkara Lao Varanasi 12603 United States of America Pokies New York Misty Ridge Circle 24

Claims (21)

[Claims] Providing an uncured photoresist coating on a substrate comprising a phenolic resin or polymer, a glycoluril derivative, and a photoacid generator; exposing the coating to ultraviolet radiation in an image-wise pattern;
Thereby generating an acid catalyst in the pattern; heating the exposed coating at 90-130 ° C. for 1-2 minutes; and developing the photoresist in an aqueous base solution. How to form a pattern. 2. The method of claim 1, wherein said ultraviolet light has a wavelength of about 250 to about 370 nanometers. 3. The method according to claim 1, wherein said phenolic resin is poly (4-hydroxystyrene). 4. The method according to claim 1, wherein said phenolic resin is a copolymer of hydroxystyrene and hydroxycyclohexylethene represented by the following formula 1, wherein n> 1, 0 ≦ X ≦ 1. Embedded image 5. The phenolic resin is a partially protected poly (hydroxystyrene) represented by the following formula 2, wherein x is a number from 0.5 to 1.0, and R is an organic group. 1
The method described in. Embedded image 6. The method of claim 1, wherein said phenolic resin is a phenol-formaldehyde (novolak) resin. 7. The glycoluril derivative has the following general formula 3, wherein R ₁ and R ₂ are alkyl, alkenyl, alkoxy, aryl, (phenyl, furyl, thienyl) having 1 to 6 carbon atoms, can alkyl such as aryl, halogenated aryl, be individually selected from the group consisting of diphenyl ether and diphenyl sulfide, - tolyl, xylyl, mesityl or n is _{C n H 2n + 1 C 6} H 4 is 3-6, The method of claim 1. Embedded image 8. The method of claim 1 wherein said photoacid generator is selected from onium salts of Group IV and Group VIa elements. 9. The method of claim 1 wherein said photoacid generator is selected from the sulfonates of N-hydroxyimide. 10. The method of claim 1, wherein said photoacid generator is a sulfonate having the structure of Formula 4 below. Embedded image 11. A step of providing a coating of a mixture containing a phenolic resin or a polymer, a glycoluril derivative, a photoacid generator, and an organic base on a substrate; ,
A method for forming a pattern in a photoresist, comprising: generating an acid catalyst in the pattern; heating the exposed coating; and developing the photoresist. 12. The phenolic resin or polymer, the glycoluril derivative, the photoacid generator, and the organic base may comprise about 9 parts of the phenolic resin or polymer.
0-60%, about 5-20 of the glycoluril derivative
%, About 2-20% of said photoacid generator, and about 0.02-0.5% of an organic base.
2. The method according to 1. 13. A composition comprising a mixture of a phenolic resin or polymer, a glycoluril derivative, a photoacid generator, and an organic base. 14. The composition according to claim 13, wherein said phenolic resin is poly (4-hydroxystyrene). 15. The composition according to claim 13, wherein said phenolic resin is a copolymer of hydroxystyrene and hydroxycyclohexylethene represented by the following formula 5, wherein n> 1, 0 ≦ X ≦ 1. Embedded image 16. The phenolic resin is a partially protected poly (hydroxystyrene) represented by the following formula 6, wherein x is a number from 0.5 to 1.0, and R is an organic group. 14. The composition according to 13. Embedded image 17. The composition according to claim 13, wherein said phenolic resin is a phenol-formaldehyde (novolak) resin. 18. The glycoluril derivative has the general formula of the following formula 7, wherein R ₁ and R ₂ are alkyl, alkenyl, alkoxy, aryl, (phenyl, furyl, thienyl) having 1 to 6 carbon atoms. ), tolyl, xylyl, mesityl or n is 3 to 6 a is _{C n H 2n + 1 C 6} H 4, - alkylaryl, such as, halogenated aryl, ether and individually be selected from the group consisting of diphenyl sulfide, 14. The composition according to claim 13, which is capable of: Embedded image 19. The composition according to claim 13, wherein said photoacid generator is selected from onium salts of Group IV and Group VIa elements. 20. The composition according to claim 13, wherein said photoacid generator is selected from the sulfonates of N-hydroxyimide. 21. The phenolic resin or polymer, the glycoluril derivative, the photoacid generator, and the organic base may comprise about 4 parts of the phenolic resin or polymer.
0 to 80%, about 5 to 25 of the glycoluril derivative
15. The composition of claim 14, wherein the composition forms a mixture comprising about 2.0-20% of the photoacid generator and about 0.01-0.5% of an organic base.