FLUORINE-CONTAINING RESIN COMPOSITION AND PREPARATION METHOD THEREOF, AND PREPARATION METHOD OF CURED FILM CONTAINING SAME

Abstract

The present disclosure discloses a fluorine-containing resin composition, including the following as raw materials, in parts by weight: a alkali-soluble resin (A) containing a compound (I), a photoinitiator, a sensitizer, a reactive diluent, a solvent and an assistant; the structural formula of the monomer of the compound (I) is shown as follows:

##STR00001##

wherein R is selected from the group consisting of —CH═CH.sub.2, —C(CH.sub.3)═CH.sub.2, acryloyl and methacryloyl; R.sub.1, R.sub.1′, R.sub.2, and R.sub.2′ are each independently selected from the group consisting of hydrogen, hydroxyl, C.sub.1-C.sub.4 alkyl and C.sub.1-C.sub.4 alkoxy; R.sub.3 is selected from the group consisting of hydrogen and C1-C6 alkyl; the A ring is selected from the group consisting of cyclohexyl and phenyl; and the B ring is selected from the group consisting of phenyl, naphthyl and anthryl.

Claims

1: A fluorine-containing resin composition, comprising the following as raw materials, in parts by weight: 18 to 42 parts of a alkali-soluble resin (A) containing a compound (I), 2 to 8 parts of a photoinitiator, 0.3 to 1.2 parts of a sensitizer, 0 to 15 parts of a reactive diluent, 60 to 90 parts of a solvent, and 1 to 8 parts of an assistant; the structural formula of the monomer of the compound (I) is shown as: ##STR00015## wherein R is selected from the group consisting of —CH═CH.sub.2, —C(CH.sub.3)═CH.sub.2, acryloyl and methacryloyl; R.sub.1, R.sub.1′, R.sub.2, and R.sub.2′ are each independently selected from the group consisting of hydrogen, hydroxyl, C.sub.1-C.sub.4 alkyl and C.sub.1-C.sub.4 alkoxy; R.sub.3 is selected from the group consisting of hydrogen and C.sub.1-C.sub.6 alkyl; the ring A is selected from the group consisting of cyclohexyl and phenyl; and, the ring B is selected from the group consisting of phenyl, naphthyl and anthryl.

2: The fluorine-containing resin composition of claim 1, wherein a method for preparing the alkali-soluble resin (A) is performed as follows: adding 2 to 5 parts of the monomer of the compound (I), 1 to 5 parts of an acrylic monomer, 10 to 30 parts of a acrylate monomer, 2 to 5 parts of a maleimide monomer, 1 to 5 parts of an initiator, 0.2 to 1.0 parts of a molecular weight regulator and 50 to 84 parts of an organic solvent into a three-necked flask for mixing under stirring, and heating to 75-80° C., holding the temperature to react for 3-6 h, and cooling to room temperature to terminate the reaction, to obtain the alkali-soluble resin (A).

3: The fluorine-containing resin composition of claim 1, wherein the photoinitiator is prepared by a condensation reaction of a phenolic compound and 215-nitrine naphthoquinone sulfonyl chloride according to a molar ratio of (1:0.5)-(1:4).

4: The fluorine-containing resin composition of claim 3, wherein the phenolic compound is one at least selected from the group consisting of 4-hydroxybenzophenone, 4,4′-dihydroxybenzophenone, 2,4-dihydroxybenzophenone, 2,4,6-trihydroxybenzophenone, 2,3,4-trihydroxybenzophenone, 2,2′,4,4′-tetrahydroxybenzophenone, 2,3,4,4′-tetrahydroxybenzophenone, 2,3,4,2′,6′-pentahydroxybenzophenone, 2,3,4,3′,4′,5′-hexahydroxybenzophenone, 3,4,5,3′,4′,5′-hexahydroxybenzophenone, bisphenol A, spirobiindane, cresol trimer, tris(4-hydroxyphenyl)methane, 1,1,1-tris(tetrahydrohydroxyphenyl)ethane, 1,1,1-tris(4-hydroxyphenyl)propane, 1,1,1-tris(4-hydroxyphenyl)butane, 1,1-bis(4-hydroxyphenyl)cyclohexane, and α,α,α′ -tris(4-hydroxyphenyl)-1-ethyl-4-cumene.

5: The fluorine-containing resin composition of claim 1, wherein the photoinitiator is one at least selected from the group consisting of a phosphorus salt, an iodonium salt, an o-nitrobenzyl salt, an oxime ketone ester and a triazine compound.

6: The fluorine-containing resin composition of claim 1, wherein: the sensitizer is 4-hydroxybenzophenone and/or 4,4′-dihydroxybenzophenone; the reactive diluent is a methacrylate monomer or a alicyclic monomer having a heterocyclic structure.

7: The fluorine-containing resin composition of claim 1, wherein: the solvent is one at least selected from the group consisting of a diethylene glycol alkyl ether compound, a dipropylene glycol alkyl ether compound, a propylene glycol monoalkyl ether compound, a propylene glycol monoalkyl ether acetate compound, a N,N-dimethylamide compound, a lactate compound, ketone and a 3-alkoxypropionate compound; and, the assistant is one at least selected from the group consisting of a surfactant, a defoaming agent, an antioxidant and a coupling agent.

8: A method for preparing a fluorine-containing resin composition, comprising: weighing respective raw materials in parts by weight according to the fluorine-containing resin composition of claim 1, and stirring uniformly, and filtering the obtained mixture with a filter membrane with a thickness of 0.1-0.5 μm to obtain the fluorine-containing resin composition.

9: A method for preparing a cured film, comprising: coating the fluorine-containing resin composition of claim 1 on a surface of a substrate, and subjecting to a soft baking, a light exposure, a development, a UV irradiation and a hardening to obtain the cured film.

10: The method of claim 9, wherein the soft baking is conducted at a temperature of 90-130° C. for 120 s-200 s; the value of the exposure is in a range of 80 mJ-200 mJ; the development is performed by: cleaning with a cleaning solvent; the light intensity of the UV irradiation is in a range of 100-2000 mj/cm.sup.2; and, the hardening is performed by: baking the developed thin film at a temperature of 150-250° C.

11: The method of claim 9, wherein the fluorine-containing resin composition is prepared by the following method, comprising: weighing respective raw materials in parts by weight according to the fluorine-containing resin composition of claim 1, and stirring uniformly, and filtering the obtained mixture with a filter membrane with a thickness of 0.1-0.5 μm to obtain the fluorine-containing resin composition.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0044] In order to describe the technical schemes in the embodiments of the present disclosure or in the prior more clearly, the following will briefly introduce the drawings required to be used in the description of the examples or the prior art. It is evident that the drawings in the following description are merely examples of the present disclosure, and those ordinary skilled in the art may still obtain other drawings based on the provided drawings without creative work.

[0045] FIG. 1 shows a schematic structural diagram of film uniformity evaluation of the cured film in the present disclosure.

[0046] FIG. 2 shows a test box schematic diagram of the insulation evaluating of the cured film in the present disclosure.

[0047] FIG. 3 is a TGA diagram showing the evaluation of heat resistance of the film in the present disclosure.

[0048] FIG. 4-1 is an SEM image showing the evaluation of graphic morphology in the present disclosure.

[0049] FIG. 4-2 is a micrograph showing the evaluation of graphic morphology in the present disclosure.

DETAILED DESCRIPTION

[0050] The technical schemes in the examples of the present disclosure will be clearly and completely described below with reference with drawings in the examples. It is evident that the described examples are only a part of examples and not all of them. Based on the examples of the present disclosure, all other examples obtained by those ordinary skilled in the art without creative work shall fall within the protection scope of the present disclosure.

EXAMPLE 1

[0051] The synthesis of a alkali-soluble resin A-1 was performed by the following steps: Under the protection of nitrogen, 22.0 kg of diethylene glycol diethyl ether, 1.0 kg of methacrylic acid, 1.0 kg of methyl methacrylate, 6 kg of tetrahydrofurfuryl methacrylate, 1.0 kg of a compound 1-2, 1.0 kg of N-cyclohexylmaleimide, 0.5 kg of azobisisobutyronitrile and 0.5 kg of an α-methylstyrene dimer were added into a three-necked flask, heated to 78° C. under stirring, held at the temperature for 4 h to react, and cooled to room temperature to terminate the reaction.

EXAMPLE 2

[0052] The synthesis of a alkali-soluble resin A-2 was performed by the following steps: Under the protection of nitrogen, 22.0 kg of diethylene glycol dimethyl ether, 1.0 kg of methacrylic acid, 0.5 kg of lauryl methacrylate, 6 kg of glycidyl methacrylate, 0.5 kg of dicyclopentyl methacrylate, 1.0 kg of a compound 1-25, 1.0 kg of N-cyclohexylmaleimide, 0.5 kg of azodiisoheptononitrile and 0.5 kg of an α-methylstyrene dimer were added into a three-necked flask, heated to 78° C. under stirring, held at the temperature for 4 h to react, and cooled to room temperature to terminate the reaction.

EXAMPLE 3

[0053] The synthesis of a alkali-soluble resin A-3 was performed by the following steps: Under the protection of nitrogen, 22.0 kg of diethylene glycol methyl ethyl ether, 1.0 kg of methacrylic acid, 0.5 kg of lauryl methacrylate, 4 kg of glycidyl methacrylate, 2 kg of tetrahydrofurfuryl methacrylate, 0.5 kg of dicyclopentyl methacrylate, 1.0 kg of a compound 1-26, 1.0 kg of N-cyclohexylmaleimide, 0.5 kg of azodiisoheptonitrile and 0.5 kg of an α-methylstyrene dimer were added into a three-necked flask, heated to 78° C. under stirring, held at the temperature for 4 h to react, and cooled to room temperature to terminate the reaction.

COMPARATIVE EXAMPLE 1

[0054] The synthesis of a copolymer A-4 was performed by the following steps: Under the protection of nitrogen, 22.0 kg of diethylene glycol methyl ethyl ether, 1.0 kg of methacrylic acid, 0.5 kg of lauryl methacrylate, 4 kg of glycidyl methacrylate, 2 kg of tetrahydrofurfuryl methacrylate, 0.5 kg of dicyclopentyl methacrylate, 1.0 kg of 4-hydroxyphenyl methacrylate, 1.0 kg of N-cyclohexylmaleimide, 0.5 kg of azodiisoheptonitrile and 0.5 kg of an α-methylstyrene dimer were added into a three-necked flask, heated to 78° C. under stirring, held at the temperature for 4 h to react, and cooled to room temperature to terminate the reaction.

[0055] Wherein, CF.sub.2O monomer was replaced.

COMPARATIVE EXAMPLE 2

[0056] The synthesis of a copolymer A-5 was performed by the following steps: Under the protection of nitrogen, 22.0 kg of diethylene glycol methyl ethyl ether, 1.0 kg of methacrylic acid, 0.5 kg of lauryl methacrylate, 4 kg of glycidyl methacrylate, 2 kg of tetrahydrofurfuryl methacrylate, 0.5 kg of dicyclopentyl methacrylate, 1.0 kg of 4′-tert-butoxy-(1,1′-biphenyl)-methacrylate, 1.0 kg of N-cyclohexylmaleimide, 0.5 kg of azodiisoheptonitrile and 0.5 kg of an α-methylstyrene dimer were added into a three-necked flask, heated to 78° C. under stirring, held at the temperature for 4 h to react, and cooled to room temperature to terminate the reaction.

[0057] Wherein, CF.sub.2O monomer was replaced.

[0058] 1. Testing of polymer (A) alkali-soluble resin

[0059] (1) GPC

[0060] Instrument: waters (515-2414)

[0061] Gel column: Shimadzu KF801+KF802+KF803

[0062] Solvent: THF

[0063] Flow rate: 0.8 mL/min

[0064] (2) Transmittance

[0065] Instrument: Shimadzu UV-2600

[0066] Determination manner: transmissivity

[0067] Wavelength range: 200 nm-800 nm

[0068] (3) TGA

[0069] Instrument: TGA-Q50 manufactured by TA in US

[0070] Heating rate: 10° C./min, heating to 800° C.

[0071] (4) The solid content of the resin was tested by: 1.0000 g of a resin solution was taken, baked at 120° C. for 2 h, and weighed, and an average value of three parallel samples was taken.

[0072] Solid content=(baked weight/weight before baking)×100%.

[0073] The test results of performance of the polymer (A) were as follows (Table 1):

TABLE-US-00002 Molecular Transmit- Solid Viscos- Weight Polymer TGA tance Content ity (Mw) A-1 252.9° C. 95.4% 28.2% 68 cP 12800 A-2 255.3° C. 95.8% 27.8% 58 cP 10200 A-3 257.4° C. 96.5% 28.4% 65 cP 12400 A-4 242.0° C. 96.4% 27.5% 60 cP 10800 A-5 255.6° C. 90.1% 28.0% 65 cP 11600

[0074] The raw materials of resin compositions prepared in Examples 4-13 and Comparative Examples 3-4 were shown in Table 2, in which the copolymer (A) alkali-soluble resin was prepared in Examples 1-3 and Comparative Example 1-2, wherein the resin compositions prepared in Examples 3-9 could be used for interlayer insulating films, and the resin compositions prepared in Examples 7-8 could be used for chemically-amplified interlayer insulating films, and the resin compositions prepared in Examples 12-13 could be used for OC films.

TABLE-US-00003 TABLE 2-1 The raw materials of resin compositions prepared in Examples 4-13 and Comparative Examples 3-4 (unit kg) Compar- Compar- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- ative ative Components ple 4 ple 5 ple 6 ple 7 ple 8 ple 9 ple 10 ple 11 ple 12 ple 13 Example 1 Example 2 Resin A-1 42 42 42 42 36 36 20 30 A-2 28 18 A-3 40 40 A-4 42 A-5 42 Solvent Propylene glycol 18 18 18 18 18 18 16 16 18 18 18 18 monomethyl ether Diethylene 22 22 27 28.7 22 27 18 18 22 22 22 22 glycol diethyl ether Methyl 3- 5 5 5 5 5 5 5 ethoxypropionate Propylene glycol 3.7 3.7 3.7 3.7 9 3.7 9 methyl ether acetate Ethylene glycol 3.7 3.7 3 3 3.7 monobutyl ether acetate Photoini- 4NT-250 3.2 3.2 3.2 3.2 3.2 3.2 3.2 3.2 tiator NT-200 0.8 0.8 0.8 0.8 0.8 0.8 0.8 0.8 Diphenyl[(phen- 3.5 3.5 ylthio)phenyl]sul- fonium hexa- fluorophosphate Fluorenone 1.5 1.5 phenyl iodonium salt PAG201 2.4 3.6 PBG-304 0.5 0.5 0.2 0.2 Sensitizer 4-hydroxy- 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 benzophenone UV-184 1.2 Reactive N- 0.75 0.75 1.75 1.75 0.25 0.25 0.75 diluent acryloylmorpho- line Dipentaerythritol 0.75 1.5 0.75 1.5 1.75 1.75 0.25 0.25 0.5 0.75 1.5 0.5 hexaacrylate Glycidyl 2 2 2 2 5 5 1.2 1.2 1 2 2 1 methacrylate Benzyl 1 1 methacrylate Hexanediol 1.2 1.2 diacrylate Hydroxy ethyl 1.75 1.75 methacrylate Coupling KBM403 1.2 1.2 1.2 1.2 1.2 1.2 1.5 1.5 2.4 2.4 1.2 2.4 agent Antioxi- BHT 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0.25 0.3 0.3 0.25 0.25 dant Leveling KP340 0.05 0.05 0.05 0.05 0.05 0.05 0.05 0.05 0.05 0.05 0.05 0.05 Agent

[0075] The methods for preparing the above Examples 4-13 and Comparative Examples 3-4 were all performed by: the above raw materials were dissolved in a clean environment with yellow light, dissolved under stirring at a controlled temperature of 20° C. to 25° C. for 2 h, and filtered through a filter with a pore size of 0.2 μm, obtaining a resin composition.

[0076] The method for preparing the cured films of Examples 14-23 was performed by: the solutions of the resin compositions prepared in Examples 4-13 were coated on a TFT glass substrate (Corning® EAGLE XG) with a size of 100 mm×100 mm×0.7 mm by using a rotary spin coater, subjected to a soft baking on a hot plate at 110° C. for 120 s, and then conducted an exposure at an exposure amount of 1,000 mj/cm.sup.2 by using an MJB4 exposure machine manufactured by SUSS, and subsequently subjected to a hardening in a clean oven at 230° C. for 40 min to form a cured film with a thickness of 2 μm on the TFT glass substrate.

[0077] A method for preparing the cured films of Comparative Examples 5-6 was the same as that of Examples 14-23.

Evaluation of the Physical Properties of the Cured Film

[0078] 1. Evaluation of the Surface of the Cured Film

[0079] The surfaces of the films of Examples 14-23 and Comparative Examples 5-6 were irradiated with a sodium lamp, and the flatness of the surfaces of the films was visually observed. The results were shown in Table 3.

[0080] 2. Evaluation of Film Uniformity

[0081] For the films of Examples 14-23 and Comparative Examples 5-6, regions of 1 cm×1 cm were selected on the substrate covered with the film surface, and nine points were taken (as shown in FIG. 1).

[0082] The film thicknesses at different points were respectively detected by using a VASE ellipsometer (VB-400 manufacture by J. A. Woollam in U.S.), and calculated the film uniformity according to the following equation:

[0083] Detection was conducted at three different parts on the surface of the specimen, and an average value was taken. It was recorded as A, when the film uniformity was less than or equal to 2.0%, and as B when the film uniformity was in a range of 2.0%-4.0%, and as C when the film uniformity was more than or equal to 4.0%. The results were shown in Table 3.

[0084] 3. Evaluation of Film Adhesion

[0085] For the films of Examples 14-23 and Comparative Examples 5-6, the above substrate coated with the film was placed on a hard and flat object surface with its film face up. A scribing tester (BYK 5123, with a cutter tooth number of 11 and a cutter tooth spacing of 1 mm) was used, and a cutting knife was held so that the knife was perpendicular to the surface of the sample plate, and a force was applied evenly to scribe 11 parallel cutting lines in a stable manner; and then 11 parallel cutting lines that were crossed vertically with the original cutting lines at an angle of 90° to form a grid pattern, and all the cuts needed to penetrate the surface of the substrate. A banister brush was used for gently sweeping backward for several times and then forward for several times along each diagonal line of the grid pattern. An adhesive tape (a 3M 610 adhesive tape) was applied onto the surface of the film, wherein the forefront section of the adhesive tape was removed, then the adhesive tape with a length of about 75 mm was cut off and applied onto the surface of the film with its center point being placed above the grid and flattened, the length of the adhesive tape should at least exceed the grid by 20 mm, and it was ensured that it is in complete contact with the surface of the film. Within 5 min of sticking the adhesive tape, the dangling end of the adhesive tape was held, and the adhesive tape was torn away smoothly within 0.5-1.0 s at an angle of 60° with the surface of the film as far as possible, and then the falling off condition of the surface of the film was observed with a microscope. The test was conducted on three different parts on the surface of the sample, and the grades of the grid scribing test were recorded.

[0086] It was recorded as A when the cutting edge was completely smooth and no grid fell off, and recorded as B when there was a little separation of the membrane layer at the intersection of cuts and the affected grid scribing region was no more than 5%, and recorded as C when the affected grid scribing region was more than 5%. The results were shown in Table 3.

[0087] 4. Evaluation of Film Hardness

[0088] For the films of Examples 14-23 and Comparative Examples 5-6; the above substrate coated with the film was placed on a hard and flat object surface with its film face up, and a set of advanced drawing pencils conforming to GB 149, i.e., the pencil grades, such as 6H, 5H, 4H, 3H, 2H, H, HB, B, 2B, 3B, 4B, 5B and 6B, was used so that the refill was exposed to 4-6 mm, and it was polished vertically with a sandpaper until the end face was flat and the edge was sharp. A portable pencil hardness tester (QHO-A) was used as being pushed forward vigorously starting from the 6H pencil, wherein scribing with each grade of pencil was for 5 times, if there were 2 times of film scratch in each grade, a pencil of another grade was replaced until there was a pencil that could not scratch the film for at least 4 times, and the corresponding hardness values were recorded. The results were shown in Table 3.

[0089] 5. Evaluation of Film Transmittance

[0090] For the films of Examples 14-23 and Comparative Examples 5-6, the light transmittance of the glass substrate with the cured film was measured by using a spectrophotometer [Shimadzu UV2600] at a wavelength in the range of 400-800 nm. When the value of the minimum light transmittance was above 95%, the transparency was considered to be good. The results were shown in Table 3.

[0091] 6. Evaluation of Film Heat Resistance

[0092] For the films of Examples 14-23 and Comparative Examples 5-6, the cured film was peeled off, and measured by TGA for a temperature at which its weight loss was 5%. The results were shown in Table 3, and the TGA diagram of the examples was shown in FIG. 3.

[0093] 7. Evaluation of Solvent Resistance of Film

[0094] For the films of Examples 14-23 and Comparative Examples 5-6, the transmittance T2 of the cured film was measured by a spectrophotometer [Shimadzu UV2600] at 400 nm. Then, the sample was cut into two pieces with the same size, and the two pieces were respectively soaked in N-methylpyrrolidone (NMP) and isopropanol (IPA) at 25° C. for 60 min. After the solvent was blown off with a N.sub.2 gun, the transmittances T.sub.NMP and T.sub.IPA of the cured film were respectively detected at 400 nm, and the solvent resistance change rate of the cured film was calculated according to the following equation:

[00001]$\mathrm{Solvent}\mathrm{resistance}\mathrm{change}\mathrm{rate}=\frac{T2-T_{\mathrm{NMP}}\left(T_{\mathrm{IPA}}\right)}{T2}\times 100\%$

[0095] The results of the solvent resistance change rate of the cured film were shown in Table 3. It was considered that the solvent resistance was good when the value was below 2%.

[0096] 8. Evaluation of Film Alkali Resistance

[0097] For the films of Examples 14-23 and Comparative Examples 5-6, the film thickness T3 of the cured film was measured, and then the sample was soaked in an aqueous solution of 5% by mass potassium hydroxide at 25° C. for 60 min, and then the film layer was cleaned with ultrapure water, and blown dry with a N.sub.2 gun. Then the film thickness T3′ of the cured film was measured, and the thickness change rate of the alkali-resistant film was calculated according to the following equation:

[00002]$\begin{array}{c}\mathrm{the}\mathrm{thickness}\mathrm{change}\mathrm{rate}\mathrm{of}\\ \mathrm{the}\mathrm{alkali}‐\mathrm{resistant}\mathrm{film}\end{array}=\frac{T3-T{3}^{\prime }}{T3}\times 100\%$

[0098] The results of the thickness change rate of the alkali-resistant film were shown in Table 3. It was considered that alkali resistance was good when the value was below 5%.

[0099] 9. Evaluation of Sensitivity

[0100] The solutions of the resin compositions of Examples 4-13 and Comparative Examples 3-4 were coated on a TFT glass substrate (Corning® EAGLE XG) of 100 mm×100 mm×0.7 mm by using a rotary spin coater, and subjected to a baking on a hot plate at 110° C. for 120 s, forming a film with a thickness of 2.2 μm. The film layer was exposed by inserting the graphic masks of different resolutions and patterns by using a MJB4 exposure machine manufactured by SUSS for varied exposure times. Then, a developing treatment was conducted with an aqueous solution of 2.38% by mass tetramethylammonium hydroxide (developing solution) at 25° C. by static method, and the development was conducted for 60 s. After development, the film layer was cleaned with ultrapure water, blown dry with an N.sub.2 gun, and hardened in a clean oven at 230° C. for 40 min, forming a pattern on the substrate. After the exposure-development-hardening treatment, the exposure amount required for the complete development of the pattern at 5 μm was detected, and this value was used as the sensitivity. The measurement results were shown in table 3, and it was considered that the sensitivity was good when this value was less than 100 mj/cm.sup.2.

[0101] 10. Evaluation of Graphic Morphology

[0102] The preparation method was the same as that used in the above sensitivity evaluation, in which a pattern with a film thickness of 2 μm was formed on the glass substrate with the exposure amount required in the sensitivity evaluation. The shape of the pattern formed in this way was observed with a scanning electron microscope (SEM).

[0103] The lines and dot matrix patterns at 5 μm had no residual film. The lines were clear and neat, and the shape was considered to be good when the slope gradient was in a range of 30-70 degrees. The SEM diagram and micrograph of the example were shown in FIGS. 4-1 to 4-2.

Evaluation of Insulativity

[0104] A test box was made according to FIG. 2:

[0105] I. The solution of the prepared resin composition was coated on a 50 mm×50 mm glass substrate coated with a ITO film by using a rotary spin coater, and subjected to a baking on a hot plate at 110° C. for 120 s, forming a film layer.

[0106] II. The film layer was exposed by inserting the graphic mask as shown with an exposure amount of 100 mj/cm.sup.2 by using an exposure machine (MJB4, GHI mixed lines manufacture by SUSS in Germany). Then, a developing treatment was conducted with an aqueous solution of 2.38% by mass tetramethylammonium hydroxide (developing solution) at 25° C. by static method, and the development was conducted for 60 s. After development, the film layer was cleaned with ultrapure water, blown dry with an N.sub.2 gun, and hardened in a clean oven at 230° C. for 40 min, forming a 2 μm thick cured film of 40 mm×40 mm with an ITO-exposed edge on the substrate. The film thickness d (m) was detected by a VASE ellipsometer (VB-400 manufacture by J. A. Woollam in US).

[0107] III. At the position as shown in the figure, a 5 mm×5 mm Al electrode (S=7.85×10.sup.−5 m.sup.2) was formed on the cured film by a vacuum evaporation device (Shenyang Ultrahigh Vacuum Appliance Technology Research Institute). Then, the ITO-exposed part and the Al electrode were connected to an LCR instrument (Agilent 4284A), and detected for the capacitance C at 0.1 V, 100 KHz and 25° C., and the dielectric constant was calculated according to the following equation:

[00003]$\mathrm{Dielectric}\mathrm{constant}K=\frac{C}{{\epsilon }_0}\times \frac{d}{S}\mathrm{\epsilon 0}=8.854\times 10^{-12}F/m$

[0108] The results of dielectric constant were shown in Table 3. The insulating property was considered to be good when the dielectric constant was below 3.3.

TABLE-US-00004 TABLE 3 Test results of performances of the cured films prepared in Examples 14-23 and Comparative Examples 5-6 Compar- Compar- Exam- Exam- Exam- Exam- Exam- Exam- ative ative Exam- Exam- Exam- Exam- Components ple 14 ple 15 ple 16 ple 17 ple 18 ple 19 Example 5 Example 6 ple 20 ple 21 ple 22 ple 23 Test Viscosity/cP 6.5 6.8 6.3 6.9 6.4 6.5 6.6 6.4 7.5 7.6 4.8 4.8 Result Solid 21.50 21.50 21.50 21.50 21.50 21.50 21.50 21.50 21.50 21.50 21.50 21.50 Content/% Surface Clean Clean Clean Clean Clean Clean Slightly Slightly Clean Clean Clean Clean and and and and and and worse worse and and and and flat flat flat flat flat flat flatness flatness flat flat flat flat Adhesion A B A A B B C B A B A A Transmittance 95.6 94.5 95.1 95.2 94.5 94.1 93.2 91.9 98.5 96.2 98.2 98.4 (400 nm)/% Dielectric 3.21 3.29 3.11 3.27 3.19 3.15 3.22 3.17 3.24 3.19 3.21 3.22 constant Heat 304.8 281.3 293.7 292.3 293.1 300.1 259.5 251.9 277.4 275.1 281.6 266.3 resistance/ ° C. Solvent 1.11 1.19 1.09 1.25 1.12 1.21 1.19 1.23 1.08 1.12 1.22 1.18 resistance NMP Solvent 0.52 0.62 0.54 0.68 0.55 0.65 0.63 0.66 0.52 0.58 0.65 0.60 resistance IPA Alkali 4.02 4.26 4.38 4.05 4.67 4.28 6.31 7.32 4.55 4.06 3.98 4.25 resistance Film A A A A A A A B A A A A Uniformity/% Sensitivity/ 70 75 80 80 80 80 90 90 110 120 100 110 (mj/cm.sup.2) Graphic excel- good excel- excel- excel- excel- excel- good excel- excel- excel- excel- morphology lent lent lent lent lent lent lent lent lent lent Hardness >H >H >H >H >H >H >HB >HB >H >H >H >H

[0109] Each example of the specification is described in a progressive manner, and each example focuses on the differences from other examples, and the same and similar parts between the examples can be seen from each other. For the device disclosed in the examples, since it corresponds to the method disclosed in the examples, the description is relatively simple, and reference can be seen in the method description.

[0110] The above description of the disclosed embodiments enables those skilled in the art to achieve or use the present disclosure. Various modifications to these embodiments are obvious to those skilled in the art, and the generic principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present disclosure. Thus, the present disclosure will not limited to the embodiments shown herein, but should conform to the widest scope consistent with the principles and novel features disclosed herein.