Adhesive composition for photocurable interface and surface modification method of substrate using the same
10557066 ยท 2020-02-11
Assignee
Inventors
- Hyung-Jong Lee (Sejong, KR)
- Nam Seob Baek (Daejeon, KR)
- Jonghwi Lee (Daejeon, KR)
- Yun Jung Seo (Daejeon, KR)
- Jin-Kwon Jeong (Daejeon, KR)
Cpc classification
C08F283/124
CHEMISTRY; METALLURGY
C08G77/20
CHEMISTRY; METALLURGY
C08F220/325
CHEMISTRY; METALLURGY
C08F220/325
CHEMISTRY; METALLURGY
C09D183/14
CHEMISTRY; METALLURGY
C08F283/124
CHEMISTRY; METALLURGY
C09J183/06
CHEMISTRY; METALLURGY
C09J183/08
CHEMISTRY; METALLURGY
International classification
C09J183/06
CHEMISTRY; METALLURGY
C09J151/08
CHEMISTRY; METALLURGY
C09J183/08
CHEMISTRY; METALLURGY
Abstract
The present invention relates to an adhesive composition capable of improving adhesion force between two interfaces through thermal crosslinking and photo-crosslinking of a substrate and a resin, or a resin and a resin, in processes for optical devices and electronic devices, and a preparation method thereof. Specifically, the present invention relates to an adhesive composition capable of adhering an interface between a substrate and a photocurable resin, and a method of adhering an interface using the same.
Claims
1. An adhesive composition for photocurable interface comprising: an organic functional silane compound represented by Chemical Formula 1 below, a silane compound represented by Chemical Formula 2 below, and methoxypropanol: ##STR00009## in Chemical Formula 1, R.sub.1 is C.sub.3-C.sub.20 alkyl substituted with an organic functional group selected from the group consisting of mercapto, epoxy, methacryloxy, acryloxy, chloro, cyano, ketone, aldehyde, carboxylate, amine, C.sub.1-C.sub.10 alkylamine, amide, isocyanurate, glycidyloxy and C.sub.1-C.sub.10 alkylamino, and R.sub.2, R.sub.3 and R.sub.4 are the same as each other or different from each other, and each independently selected from the group consisting of C.sub.1-C.sub.10 alkyl, C.sub.1-C.sub.10 alkyl substituted with C.sub.1-C.sub.10 alkoxy, and C.sub.6-C.sub.20 aryl, and ##STR00010## in Chemical Formula 2, R.sub.5, R.sub.6, R.sub.7, R.sub.8, R.sub.9 and R.sub.10 are each independently selected from the group consisting of C.sub.1-C.sub.10 alkyl, C.sub.1-C.sub.10 alkyl substituted with C.sub.1-C.sub.10 alkoxy, and C.sub.6-C.sub.20 aryl, and A is selected from the group consisting of C.sub.1-C.sub.10 alkylene, and C.sub.6-C.sub.20 arylene; and wherein the organic functional silane compound represented by Chemical Formula 1 has 0.01 to 2 wt % of the total composition, and the silane compound represented by Chemical Formula 2 has 0.001 to 0.5 wt % of the total composition.
2. The adhesive composition of claim 1, wherein in Chemical Formula 1, R.sub.1 is C.sub.3-C.sub.20 alkyl substituted with an organic functional group selected from the group consisting of mercapto, methacryloxy, acryloxy, amine, amide, glycidyloxy and C.sub.1-C.sub.10 alkylamino, and R.sub.2, R.sub.3, and R.sub.4 are each independently C.sub.1-C.sub.5 alkyl.
3. The adhesive composition of claim 1, wherein in Chemical Formula 2, R.sub.5, R.sub.6, R.sub.7, R.sub.8, R.sub.9 and R.sub.10 are each independently selected from the group consisting of C.sub.1-C.sub.10 alkyl, and A is selected from C.sub.1-C.sub.10 alkylene, and C.sub.6-C.sub.20 arylene.
4. The adhesive composition of claim 1, wherein the compound represented by Chemical Formula 1 is selected from the group consisting of 3-methacryloxypropyltrimethoxysilane, 3-methacryloxypropyltriethoxysilane, 3-acryloxypropyltrimethoxysilane, 3-acryloxypropyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropyltriethoxysilane, 3-mercaptopropyltriethoxysilane, 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, and N-methylaminopropyltrimethoxysilane.
5. The adhesive composition of claim 1, wherein the compound represented by Chemical Formula 2 is selected from the group consisting of bistrimethoxysilylethane, bistriethoxysilylethane, bistrimethoxysilylmethane, bistriethoxysilylmethane, bistriethoxysilyloctane, bistriethoxysilylethylene, 1,4-bistriethoxysilylbenzene, bistriethoxysilylpropane, and bistrimethoxysilylhexane.
6. The adhesive composition of claim 1, wherein the adhesive composition includes the organic functional silane compound represented by Chemical Formula 1, has the silane compound represented by Chemical Formula 2, a pH adjuster, and the methoxypropanol.
7. A surface modification method of a substrate comprising: applying the adhesive composition for photocurable interface of claim 1 to any one substrate selected from the group consisting of a silicon wafer or a glass substrate; and drying the composition to form a coating layer.
8. The surface modification method of claim 7, wherein the applying is performed by a method selected from the group consisting of spin coating, bar coating, and spray coating.
9. The surface modification method of claim 7, wherein the coating layer has a dry application thickness of 1 to 10 nm.
10. The surface modification method of claim 7, wherein the drying is heat drying at 100 to 150 C. for 1 to 60 minutes.
Description
DESCRIPTION OF DRAWINGS
(1)
(2)
DETAILED DESCRIPTION OF MAIN ELEMENTS
(3) 10: Substrate 20: Adhesive composition for interface 30: Resin
BEST MODE
(4) Hereinafter, an adhesive composition for interface according to the present invention, and a surface modification method of a substrate using the same will be described in more detail according to specific exemplary embodiments or Examples including the accompanying drawings. Meanwhile, the following exemplary embodiments or Examples are provided as a reference for explaining the present invention in detail, and therefore, the present invention is not limited thereto, but may be implemented in various ways.
(5) Unless defined otherwise, all technical and scientific terms used herein have the same meanings generally understood by those skilled in the art to which the present invention pertains. Terms used in the specification of the present invention are to effectively describe specific exemplary embodiments, but are not intended to limit the present invention.
(6) It is intended that singular forms used in the appended specification and claims include plural forms unless otherwise indicated in the context.
(7) The adhesive composition for photocurable interface of the present invention is applied to an interface between a photocurable resin thin layer and a substrate to express adhesion, and the adhesive composition for photocurable interface of the present invention is possible to be subjected to thermal curing.
(8) Terms: alkyl, and substituents including alkyl part used herein include all linear or branched types, and alkenyl includes all of linear types or branched types, containing 2 to 8 carbon atoms and at least one double bond.
(9) An embodiment of the present invention is the adhesive composition for photocurable interface includes an organic functional silane compound represented by Chemical Formula 1 below, and a silane compound represented by Chemical Formula 2 below:
(10) ##STR00005##
(11) in Chemical Formula 1,
(12) R.sub.1 is C.sub.3-C.sub.20alkyl or C.sub.3-C.sub.20alkenyl substituted with an organic functional group selected from mercapto, epoxy, methacryloxy, acryloxy, chloro, cyano, ketone, aldehyde, carboxylate, amine, C.sub.1-C.sub.10alkylamine, amide, isocyanurate, glycidyloxy and C.sub.1-C.sub.10alkylamino, and
(13) R.sub.2, R.sub.3 and R.sub.4 are the same as each other or different from each other, and each independently selected from C.sub.1-C.sub.10alkyl, C.sub.1-C.sub.10alkyl substituted with C.sub.1-C.sub.10alkoxy, and C.sub.6-C.sub.20aryl, and
(14) ##STR00006##
(15) in Chemical Formula 2,
(16) R.sub.5, R.sub.6, R.sub.7, R.sub.8, R.sub.9 and R.sub.10 are each independently selected from C.sub.1-C.sub.10alkyl, C.sub.1-C.sub.10alkyl substituted with C.sub.1-C.sub.10alkoxy, and C.sub.6-C.sub.20aryl, and
(17) A is selected from C.sub.1-C.sub.10alkylene, C.sub.2-C.sub.4alkenylene, C.sub.6-C.sub.20arylene,
(18) ##STR00007##
wherein R.sub.11 is C.sub.1-C.sub.10alkyl, and m and 1 are each independently an integer selected from 1 to 5.
(19) The adhesive composition for photocurable interface of the present invention may have more improved adhesion force by including the silane compound having the organic functional groups and being represented by Chemical Formula 1. In particular, the silane compound has two different kinds of organic functional groups, wherein one functional group may be bonded to a substrate and the other functional group may be bonded to a photocurable resin.
(20) More preferably, in Chemical Formula 1,
(21) R.sub.1 is C.sub.3-C.sub.10alkyl substituted with an organic functional group selected from mercapto, methacryloxy, acryloxy, amine, amide, glycidyloxy and C.sub.1-C.sub.10alkylamino, and
(22) R.sub.2, R.sub.3, and R.sub.4 are each independently C.sub.1-C.sub.5alkyl.
(23) More specifically, the compound represented by Chemical Formula 1 may be selected from 3-methacryloxypropyltrimethoxysilane, 3-methacryloxypropyltriethoxysilane, 3-acryloxypropyltrimethoxysilane, 3-acryloxypropyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropyltriethoxysilane, 3-mercaptopropyltriethoxysilane, 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, and n-methylaminopropyltrimethoxysilane, but is not limited thereto.
(24) The organic functional silane compound represented by Chemical Formula 1 preferably has 0.01 to 2 wt %, still preferably, 0.05 to 1 wt %, and more preferably, 0.1 to 0.5 wt % of the total composition. Within a range at which the organic functional silane compound represented by Chemical Formula 1 has 0.01 to 2 wt %, it is preferred since sufficient modification of a substrate surface is performed, storage stability of a mixed solution is excellent, and foreign materials do not occur on a surface at the time of coating.
(25) In an exemplary embodiment of the present invention, the silane compound represented by Chemical Formula 2 is used to form a chemical bond together with the organic functional silane compound represented by Chemical Formula 1 and to further maximize effects of the organic functional silane compound represented by Chemical Formula 1. The silane compound represented by Chemical Formula 2 and the organic functional silane compound represented by Chemical Formula 1 may be simultaneously mixed to achieve physical properties to be desired.
(26) In an exemplary embodiment of the present invention, in the silane compound represented by Chemical Formula 2, more specifically, R.sub.5, R.sub.6, R.sub.7, R.sub.8, R.sub.9 and R.sub.10 are each independently selected from C.sub.1-C.sub.10alkyl, and
(27) A is selected from C.sub.1-C.sub.10alkylene, C.sub.2-C.sub.4alkenylene, C.sub.6-C.sub.20arylene,
(28) ##STR00008##
wherein R.sub.11 is C.sub.1-C.sub.10alkyl, and m and 1 are each independently an integer selected from 1 to 5.
(29) More specifically, the compound represented by Chemical Formula 2 may be selected from bistrimethoxysilylethane, bistriethoxysilylethane, bistrimethoxysilylmethane, bistriethoxysilylmethane, bistriethoxysilyloctane, bistriethoxysilylethylene, 1,4-bistriethoxysilylbenzene, bistriethoxysilylpropylamine, bis-3-triethoxysilylpropylbisulfite, bistriethoxysilylpropane, and bistrimethoxysilylhexane, but is not limited thereto.
(30) The silane compound represented by Chemical Formula 2 preferably has 0.001 to 0.5 wt %, still preferably, 0.01 to 0.1 wt %, and more preferably, 0.01 to 0.05 wt % of the total composition. Within the above-described content range, it is preferred since sufficient modification of a substrate surface is performed, storage stability of a mixed solution is excellent, and foreign materials do not occur on a surface at the time of coating.
(31) In an exemplary embodiment of the present invention, the adhesive composition for photocurable interface may include a pH adjuster, and a solvent, in addition to the organic functional silane compound represented by Chemical Formula 1 and the silane compound represented by Chemical Formula 2.
(32) The pH of the organic functional silane compound represented by Chemical Formula 1 and the silane compound represented by Chemical Formula 2 may affect stability of a hydroxyl group. High acidity of the composition accelerates hydrolysis and condensation reaction of an alkoxysilyl group of the silane. Accordingly, as pH of the composition is close to be neutral, storage stability of the solution may be more excellent. However, since the hydrolysis of the alkoxysilyl group is not completely performed in the neutral pH, it is not possible to achieve sufficient increase in adhesion force.
(33) In an exemplary embodiment of the present invention, the composition may include the pH adjuster for performing appropriate hydrolysis, and may include both organic and inorganic acids. As examples thereof, nitric acid, sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid, carbonic acid, boric acid, etc., may be used together with water.
(34) In an exemplary embodiment of the present invention, the pH of the adhesive composition for photocurable interface is preferably 3 to 7, and more preferably 3.5 to 5. When the pH of the composition is less than 3, the hydrolysis and the condensation reaction of the mixed solution may be promoted to inhibit the storage stability, and when the pH of the composition is more than 7, the hydrolysis may not be appropriately performed, and thus, it is difficult to expect improvement in adhesion force.
(35) Further, the composition may include the solvent to improve miscibility of each component of the adhesive composition for photocurable interface according to the present invention. The solvent is preferably alcohols such as methanol, ethanol, propanol, isopropanol, butanol, methoxypropanol, etc., and the most preferably, methoxypropanol, which is because the adhesion force is more improved even though the reason of improvement in adhesion force has not been figured out yet. A content of the solvent may have a range so that total content is satisfied to be 100 wt % except for the content of the organic functional silane compound represented by Chemical Formula 1 and the content of the silane compound represented by Chemical Formula 2.
(36) In an exemplary embodiment of the present invention, a viscosity of the adhesive composition for photocurable interface may be 2.5 to 3.5 cps measured at 25 C., and the viscosity thereof is not limited thereto. Within the above-described viscosity range, a uniform layer having a monolayer form may be formed, and the storage stability may be excellent.
(37) In still another exemplary embodiment of the present invention, the present invention provides a surface modification method of any one substrate selected from a silicon wafer or a glass substrate using the adhesive composition for photocurable interface as described above.
(38) Specifically, the surface modification method of a substrate includes: applying the adhesive composition for photocurable interface as described above to any one substrate selected from a silicon wafer or a glass substrate; and drying the composition to form a coating layer.
(39) Further, after the drying of the composition to form the coating layer, the surface modification method may further include forming a thin layer by applying a photocurable resin, followed by photocuring. Here, the photocurable resin may be a fluorine-based polymer.
(40) In an exemplary embodiment of the present invention, the applying may be performed by a method selected from spin coating, bar coating, and spray coating.
(41) More preferably, the spin coating is performed. Specifically, when a 4-inch wafer substrate is used, 0.5 to 2 mL of the resin may be applied and spin-coated by using a spin coater at 1,000 to 4,000 rpm/30 seconds. When the number of spin coating rotations is 1,000 or less per minute, liquid foreign materials may remain on the substrate surface, and a temperature for drying after the spin coating is preferably 80 to 150 C.
(42) In addition, in an exemplary embodiment of the present invention, the drying may be performed by heating. A temperature for heating is preferably 100 to 150 C., and more preferably, 120 to 130 C., and time for heating may be 1 to 60 minutes, and more preferably, 5 to 30 minutes, which is preferred since it is possible to form a coating layer having excellent adhesion force.
(43) The coating layer formed by the method may have a dry application thickness of 10 nm or less, and more specifically, 1 to 10 nm. When the coating layer has the above-described thickness range, it does not affect subsequent processes, and adhesion may be excellent.
(44) Hereinafter, the present invention is described in detail on the basis of Examples and Comparative Examples. Meanwhile, the following Examples and Comparative Examples are provided by way of example for explaining the present invention in more detail, and therefore, the present invention is not limited thereto.
(45) 1) Evaluation of Adhesion Force
(46) In order to confirm adhesion force, a photocurable resin (CO-150 manufactured by CHEMOPTICS, including epoxy acrylate and an acrylate monomer as main components, and having a viscosity of 50 cps measured at 25 C.) was cured to form a film, and then, 100 grid patterned scratches were caused on the film surface using a cross cut test (ASTM D3359), and peeling was tested using an adhesive tape. The adhesion force was calculated by counting the number of scratches and the number of films adhered to the adhesive tape according to the following Equation.
Adhesion force=(the number of scratchesthe number of films adhered to the adhesive tape)100
(47) 2) Evaluation of Storage Stability
(48) The storage stability was evaluated by spin coating on a weekly basis, confirming whether liquid foreign materials remained on the substrate by a microscope, and checking the adhesion force by the same method as above to confirm whether there was any change.
(49) 3) Surface Layer Quality State
(50) The coating was performed using a spin coater, and immediately after the coating, and after thermal crosslinking, whether the liquid foreign materials remained was confirmed by the microscope. When the liquid foreign materials remained, round shaped droplets were shown, and on the contrary, the clear layers were observed without such traces.
EXAMPLE 1
(51) 1) Preparation of Adhesive Composition for Photocurable Interface
(52) Methoxypropanol 95 g, distilled water 4.89 g, 3-methacryloxypropyltrimethoxysilane 0.1 g, and bistrimethoxysilylethane 0.01 g were put into a Nalgene 100 ml PE container, and stirred for 24 hours.
(53) 2) Surface Modification Method of Substrate
(54) The adhesive composition for photocurable interface prepared in 1) above was applied on a silicon wafer substrate, and was subjected to spin coating at 3,000 rpm/30 seconds. Heat drying was performed in a hot plate at 120 C. for 5 minutes to perform surface modification of the substrate.
(55) In order to confirm the adhesion force, the above-explained photocurable resin (CO-150 manufactured by CHEMOPTICS, including epoxy acrylate and an acrylate monomer as main components, and having a viscosity of 50 cps measured at 25 C.) was applied, and photocured by irradiating UV of 15 mW/cm.sup.2 for 3 minutes under nitrogen atmosphere, thereby manufacturing specimen.
(56) Physical properties of the manufactured specimen were measured and shown in Table 2 below.
EXAMPLE 2
(57) Example 2 was performed by the same method as Example 1 except that methanol was used as the solvent rather than using methoxypropanol in Example 1.
(58) Physical properties of the manufactured specimen were measured and shown in Table 2 below.
EXAMPLE 3
(59) Example 3 was performed by the same method as Example 1 except that isopropanol was used as the solvent rather than using methoxypropanol in Example 1.
(60) Physical properties of the manufactured specimen were measured and shown in Table 2 below.
EXAMPLE 4
(61) Example 4 was performed by the same method as Example 1 except that a drying temperature for the heat drying in step 2) of Example 1 above was 100 C.
(62) Physical properties of the manufactured specimen were measured and shown in Table 2 below.
EXAMPLE 5
(63) Example 5 was performed by the same method as Example 1 except that a drying temperature for the heat drying in step 2) of Example 1 above was 80 C.
(64) Physical properties of the manufactured specimen were measured and shown in Table 2 below.
EXAMPLE 6
(65) Example 6 was performed by the same method as Example 1 except that 3-methacryloxypropyltrimethoxysilane 0.05 g and distilled water 4.94 g were used.
(66) Physical properties of the manufactured specimen were measured and shown in Table 2 below.
EXAMPLE 7
(67) Example 7 was performed by the same method as Example 1 except that 3-methacryloxypropyltrimethoxysilane 0.01 g and distilled water 4.98 g were used.
(68) Physical properties of the manufactured specimen were measured and shown in Table 2 below.
EXAMPLE 8
(69) Example 8 was performed by the same method as Example 1 except that bistrimethoxysilylethane 0.1 g and distilled water 4.98 g were used.
(70) Physical properties of the manufactured specimen were measured and shown in Table 2 below.
EXAMPLE 9
(71) Example 9 was performed by the same method as Example 1 except that 3-acryloxypropyltrimethoxysilane 0.1 g and bistriethoxysilylethane 0.01 g were used in the preparation of the adhesive composition for photocurable interface.
(72) Physical properties of the manufactured specimen were measured and shown in Table 2 below.
EXAMPLE 10
(73) Example 10 was performed by the same method as Example 1 except that 3-glycidoxypropyltrimethoxysilane 0.1 g and bistriethoxysilylethane 0.01 g were used in the preparation of the adhesive composition for photocurable interface.
(74) Physical properties of the manufactured specimen were measured and shown in Table 2 below.
EXAMPLE 11
(75) Example 11 was performed by the same method as Example 1 except that 3-mercaptopropyltriethoxysilane 0.1 g and bistriethoxysilylethane 0.01 g were used in the preparation of the adhesive composition for photocurable interface.
(76) Physical properties of the manufactured specimen were measured and shown in Table 2 below.
EXAMPLE 12
(77) Example 12 was performed by the same method as Example 1 except that 3-aminopropyltrimethoxysilane 0.1 g and bistriethoxysilylethane 0.01 g were used in the preparation of the adhesive composition for photocurable interface.
(78) Physical properties of the manufactured specimen were measured and shown in Table 2 below.
EXAMPLE 13
(79) Example 13 was performed by the same method as Example 1 except that n-methylaminopropyltrimethoxysilane 0.1 g and bistriethoxysilylethane 0.01 g were used in the preparation of the adhesive composition for photocurable interface.
(80) Physical properties of the manufactured specimen were measured and shown in Table 2 below.
EXAMPLE 14
(81) Example 14 was performed by the same method as Example 1 except that 3-methacryloxypropyltriethoxysilane 0.1 g and bistriethoxysilylbenzene 0.01 g were used in the preparation of the adhesive composition for photocurable interface.
(82) Physical properties of the manufactured specimen were measured and shown in Table 2 below.
EXAMPLE 15
(83) Example 15 was performed by the same method as Example 1 except that 3-methacryloxypropyltriethoxysilane 0.1 g and bistriethoxysilyloctane 0.01 g were used in the preparation of the adhesive composition for photocurable interface.
(84) Physical properties of the manufactured specimen were measured and shown in Table 2 below.
EXAMPLE 16
(85) Example 16 was performed by the same method as Example 1 except that 3-methacryloxypropyltriethoxysilane 0.1 g and bistriethoxysilylethylene 0.01 g were used in the preparation of the adhesive composition for photocurable interface.
(86) Physical properties of the manufactured specimen were measured and shown in Table 2 below.
COMPARATIVE EXAMPLE 1
(87) 1) Preparation of Adhesive Composition for Photocurable Interface
(88) Methoxypropanol 95 g, distilled water 4.5 g, and 3-methacryloxypropyltrimethoxysilane 0.5 g were put into a Nalgene 100 ml PE container, and stirred for 24 hours.
(89) 2) Surface Modification Method of Substrate
(90) The adhesive composition for photocurable interface prepared in 1) above was applied on a silicon wafer substrate, and was subjected to spin coating at 3,000 rpm/30 seconds. Thermal drying was performed in a hot plate at 120 C. for 5 minutes to perform surface modification of the substrate.
(91) In order to confirm the adhesion force, the above-explained photocurable resin (CO-150 manufactured by CHEMOPTICS, including epoxy acrylate and an acrylate monomer as main components, and having a viscosity of 50 cps measured at 25 C.) was applied, and photocured by irradiating UV of 15 mW/cm.sup.2 for 3 minutes under nitrogen atmosphere, thereby manufacturing specimen.
(92) Physical properties of the manufactured specimen were measured and shown in Table 2 below.
COMPARATIVE EXAMPLE 2
(93) Comparative Example 2 was performed by the same method as Comparative Example 1 except that the content of 3-methacryloxypropyltrimethoxysilane was changed to 0.3 g and the content of distilled water was changed to 4.7 g as shown in Table 1 below.
(94) Physical properties of the manufactured specimen were measured and shown in Table 2 below.
COMPARATIVE EXAMPLE 3
(95) Comparative Example 3 was performed by the same method as Comparative Example 1 except that the content of 3-methacryloxypropyltrimethoxysilane was changed to 0.1 g and the content of distilled water was changed to 4.9 g as shown in Table 1 below.
(96) Physical properties of the manufactured specimen were measured and shown in Table 2 below.
(97) TABLE-US-00001 TABLE 1 Chem- Chem- Distilled ical ical water Drying For- For- (containing tem- mula 1 mula 2 acid, perature (wt %) (wt %) wt %) Solvent ( C.) Comparative 0.5 0 4.5 Methoxypropanol 120 Example 1 Comparative 0.3 0 4.7 Methoxypropanol 120 Example 2 Comparative 0.1 0 4.9 Methoxypropanol 120 Example 3 Example 1 0.1 0.01 4.89 Methoxypropanol 120 Example 2 0.1 0.01 4.89 Methanol 120 Example 3 0.1 0.01 4.89 Isopropanol 120 Example 4 0.1 0.01 4.89 Methoxypropanol 100 Example 5 0.1 0.01 4.89 Methoxypropanol 80 Example 6 0.05 0.01 4.94 Methoxypropanol 120 Example 7 0.01 0.01 4.98 Methoxypropanol 120 Example 8 0.1 0.1 4.98 Methoxypropanol 120 Example 9 0.1 0.01 4.89 Methoxypropanol 120 Example 10 0.1 0.01 4.89 Methoxypropanol 120 Example 11 0.1 0.01 4.89 Methoxypropanol 120 Example 12 0.1 0.01 4.89 Methoxypropanol 120 Example 13 0.1 0.01 4.89 Methoxypropanol 120 Example 14 0.1 0.01 4.89 Methoxypropanol 120 Example 15 0.1 0.01 4.89 Methoxypropanol 120 Example 16 0.1 0.01 4.89 Methoxypropanol 120
(98) TABLE-US-00002 TABLE 2 Adhesion force Surface layer Storage (Cross quality state stability cut/Tape test) Comparative Liquid foreign 100% Example 1 material occurs Comparative Liquid foreign 100% Example 2 material occurs Comparative Clear 60 or more 85% Example 3 days Example 1 Clear 60 or more 100% days Example 2 Clear 60 or more 10% days Example 3 Clear 60 or more 10% days Example 4 Clear 60 or more 70% days Example 5 Clear 60 or more 50% days Example 6 Clear 60 or more 50% days Example 7 Clear 60 or more 10% days Example 8 Clear 30 or more 100% days Example 9 Clear 60 or more 100% days Example 10 Clear 60 or more 100% days Example 11 Clear 60 or more 90% days Example 12 Clear 60 or more 100% days Example 13 Clear 60 or more 90% days Example 14 Clear 30 or more 100% days Example 15 Clear 60 or more 100% days Example 16 Clear 60 or more 100% days
(99) As shown in Table 2 above, it could be appreciated that when the compounds represented by Chemical Formulas 1 and 2 were mixed to be used, the storage stability, the surface layer quality state, and the adhesion force were excellent as compared to those of using the compound represented by Chemical Formula 1 alone.
(100) In addition, as shown in Examples 1 to 3, it was confirmed that when the solvent was changed, the adhesion force was affected, and it could be appreciated that when the methoxypropanol was used, the adhesion force was the most excellent.
(101) Further, as shown in Example 1 and Examples 4 and 5, it was confirmed that when the drying temperature was changed, the adhesion force was affected, and it could be appreciated that as the drying temperature was higher, the adhesion force was increased, and the adhesion force was the most excellent when the drying temperature was 120 C.
(102) Further, as shown in Example 1 and Examples 6 and 7, it was confirmed that when the content of the compound represented by Chemical Formula 1 was changed, the adhesion force was affected, and it could be appreciated that as the content was increased, the adhesion force was improved.