KR101991696B1 - Composition for forming silica layer, method for manufacturing silica layer, and silica layer - Google Patents
Composition for forming silica layer, method for manufacturing silica layer, and silica layer Download PDFInfo
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- KR101991696B1 KR101991696B1 KR1020160004196A KR20160004196A KR101991696B1 KR 101991696 B1 KR101991696 B1 KR 101991696B1 KR 1020160004196 A KR1020160004196 A KR 1020160004196A KR 20160004196 A KR20160004196 A KR 20160004196A KR 101991696 B1 KR101991696 B1 KR 101991696B1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
- C08G77/26—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen nitrogen-containing groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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Abstract
It relates to a silicon-containing polymer formed by polymerizing a compound represented by the following formula (1), and a composition for forming a silica film comprising a solvent.
[Formula 1]
N [SiR 1 R 2 R 3 ] 3
In Chemical Formula 1,
R 1 , R 2 and R 3 are each independently hydrogen, a substituted or unsubstituted C1 to C10 alkyl group, a substituted or unsubstituted vinyl group, a substituted or unsubstituted phenyl group, or a combination thereof.
Description
The present invention relates to a composition for forming a silica film, a method for producing a silica film, and a silica film prepared accordingly.
In a flat panel display device, a thin film transistor (TFT) including a gate electrode, a source electrode, a drain electrode, and a semiconductor is used as a switching element, and a gate line transferring a scan signal for controlling the thin film transistor is used. ) And a data line for transmitting a signal to be applied to the pixel electrode are provided in the flat panel display. In addition, an insulating film is formed between the semiconductor and the various electrodes to separate them. The insulating film may be a silica film including a silicon component.
As the material of the silica film, for example, a silicon-containing polymer such as polysilazane or polysiloxazane may be used, and the physical properties of the silicon-containing polymer may affect the shrinkage of the silica film.
One embodiment provides a composition for forming a silica film capable of forming a silica film having good shrinkage.
Another embodiment provides a method of preparing a silica film using the composition for forming a silica film.
Another embodiment provides a silica film prepared from the composition for forming a silica film.
According to one embodiment, a silicon-containing polymer formed by polymerizing a compound represented by the following Chemical Formula 1, and a composition for forming a silica film comprising a solvent.
[Formula 1]
N [SiR 1 R 2 R 3 ] 3
In Chemical Formula 1,
R 1 , R 2 and R 3 are each independently hydrogen, a substituted or unsubstituted C1 to C10 alkyl group, a substituted or unsubstituted vinyl group, a substituted or unsubstituted phenyl group, or a combination thereof.
The silicon-containing polymer may have a nitrogen content of 20% to 28% by weight of the entire silicon-containing polymer.
The silicon-containing polymer may be formed by polymerizing a compound represented by Chemical Formula 1 and a compound represented by Chemical Formula 2.
[Formula 2]
NR 4 R 5 R 6
In Chemical Formula 2,
R 4 to R 6 are each independently hydrogen, a substituted or unsubstituted C1 to C10 alkyl group, a substituted or unsubstituted vinyl group, a substituted or unsubstituted phenyl group, or a combination thereof.
The silicon polymer may have a weight average molecular weight of 1,000 to 100,000.
The solvent is benzene, toluene, xylene, ethylbenzene, diethylbenzene, trimethylbenzene, triethylbenzene, cyclohexane, cyclohexene, decahydrnaphthalene, dipentene, pentane, hexane, heptane, octane, nonane, decane, Group consisting of ethylcyclohexane, methylcyclohexane, cyclohexane, cyclohexene, p-mentane, dipropyl ether, dibutyl ether diisoamyl ether, anisole, butyl acetate, amyl acetate, methyl isobutyl ketone and combinations thereof It may include at least one selected from.
According to another embodiment, applying the above-described composition for forming a silica film on a substrate, drying the substrate coated with the composition for forming a silica film, and the composition for forming a silica film at 250 ° C. to 1,000 ° C. It provides a method for producing a silica film comprising the step of curing.
The curing may include a first curing in a steam atmosphere of 250 ℃ to 1,000 ℃, the second curing in a nitrogen atmosphere of 600 ℃ to 1,000 ℃.
According to another embodiment, a silica film formed according to the above-described method is provided.
Silica films having good shrinkage rates can be realized even under various curing conditions.
Embodiments of the present invention will be described in detail so that those skilled in the art to which the present invention pertains can easily practice. As those skilled in the art would realize, the described embodiments may be modified in various different ways, all without departing from the spirit or scope of the present invention.
In the drawings, the thickness of layers, films, panels, regions, etc., are exaggerated for clarity. Like parts are designated by like reference numerals throughout the specification. When a portion of a layer, film, region, plate, etc. is said to be "on top" of another part, this includes not only when the other part is "right over" but also when there is another part in between. On the contrary, when a part is "just above" another part, there is no other part in the middle.
Unless otherwise defined herein, "substituted" means that a hydrogen atom in the compound is a halogen atom, a hydroxy group, an alkoxy group, a nitro group, a cyano group, an amino group, an azido group, an amidino group, a hydrazino group, a hydrazono group , Carbonyl group, carbamyl group, thiol group, ester group, carboxyl group or salt thereof, sulfonic acid group or salt thereof, phosphoric acid or salt thereof, C1 to C20 alkyl group, C2 to C20 alkenyl group, C2 to C20 alkynyl group, C6 to C30 aryl group , C7 to C30 arylalkyl group, C1 to C30 alkoxy group, C1 to C20 heteroalkyl group, C2 to C20 heteroaryl group, C3 to C20 heteroarylalkyl group, C3 to C30 cycloalkyl group, C3 to C15 cycloalkenyl group, C6 to C15 It means substituted with a substituent selected from a cycloalkynyl group, a C2 to C30 heterocycloalkyl group, and a combination thereof.
In addition, unless otherwise defined herein, "hetero" means containing 1 to 3 heteroatoms selected from N, O, S and P.
In addition, in this specification, "*" means the part connected with the same or different atom or formula.
Hereinafter, a composition for forming a silica film according to one embodiment of the present invention will be described.
The composition for forming a silica film according to one embodiment includes a silicon-containing polymer (a) and a solvent (b) formed by polymerizing a compound represented by Formula 1 below.
[Formula 1]
N [SiR 1 R 2 R 3 ] 3
In Chemical Formula 1,
R 1 , R 2 and R 3 are each independently hydrogen, a substituted or unsubstituted C1 to C10 alkyl group, a substituted or unsubstituted vinyl group, a substituted or unsubstituted phenyl group, or a combination thereof.
The compound represented by Chemical Formula 1 includes a nitrogen atom (N) and three silicon (Si) atoms. By using the compound having such a basic structure as a monomer in the polymerization reaction, the Si content contained in the silicon-containing polymer can be relatively increased. Accordingly, the silica film formed from the silicon-containing polymer as a material can have excellent film shrinkage.
In addition, a low temperature curing process is required in order to reduce film stress, and the silicon-containing polymer includes nitrogen in a specific content range, so that the silica film formed using the same may ensure a good film shrinkage rate even at low temperature curing. In this regard, the silicon-containing polymer may include, for example, 20 wt% to 28 wt% of nitrogen in the silicon-containing polymer as a whole, and specifically, may be 22 wt% to 28 wt%.
For example, the silicon-containing polymer may be prepared by using the compound represented by Chemical Formula 1 alone, or from the compound represented by Chemical Formula 1 (first reactant) and the compound represented by Chemical Formula 2 (second reactant) Can be prepared. In this case, the first reactant and the second reactant may be reacted in a molar ratio of 1: 0.3 to 1: 1.
[Formula 2]
NR 4 R 5 R 6
In Chemical Formula 2,
R 4 to R 6 are each independently hydrogen, a substituted or unsubstituted C1 to C10 alkyl group, a substituted or unsubstituted vinyl group, a substituted or unsubstituted phenyl group, or a combination thereof.
For example, the weight average molecular weight of the silicon-containing polymer may be 1,000 to 100,000.
The silicon-containing polymer described above may include, for example, a moiety represented by the following formula (A).
[Formula A]
In Formula A, R 1 to R 3 are each independently hydrogen, a substituted or unsubstituted C1 to C30 alkyl group, a substituted or unsubstituted C3 to C30 cycloalkyl group , a substituted or unsubstituted C6 to C30 aryl Groups, substituted or unsubstituted C7 to C30 arylalkyl group, substituted or unsubstituted C1 to C30 heteroalkyl group, substituted or unsubstituted C2 to C30 heterocycloalkyl group, substituted or unsubstituted C2 to C30 alkenyl group , A substituted or unsubstituted alkoxy group, carboxyl group, aldehyde group, hydroxy group, or a combination thereof,
"*" Means a connection point.
For example, the silicon-containing polymer may be polysilazane produced by the reaction of halosilane and ammonia.
For example, the silicon-containing polymer included in the composition for forming a silica film may further include a moiety represented by the following Chemical Formula B in addition to the moiety represented by the Chemical Formula A above.
[Formula B]
R 4 to R 7 in Formula B are each independently hydrogen, substituted or unsubstituted C1 to C30 alkyl group, substituted or unsubstituted C3 to C30 cycloalkyl group, substituted or unsubstituted C6 to C30 aryl group , Substituted or unsubstituted C7 to C30 arylalkyl group, substituted or unsubstituted C1 to C30 heteroalkyl group, substituted or unsubstituted C2 to C30 heterocycloalkyl group, substituted or unsubstituted C2 to C30 alkenyl group, A substituted or unsubstituted alkoxy group, carboxyl group, aldehyde group, hydroxy group, or a combination thereof,
"*" Means a connection point.
In this case, the silicon-containing polymer includes a silicon-oxygen-silicon (Si-O-Si) bonding portion in addition to the silicon-nitrogen (Si-N) bonding portion in its structure, such a silicon-oxygen-silicon (Si-O) -Si) bonded part can reduce the shrinkage by curing stress during heat treatment by heat treatment.
For example, the silicon-containing polymer may include a moiety represented by Chemical Formula A, a moiety represented by Chemical Formula B, and further include a moiety represented by Chemical Formula C below.
[Formula C]
The moiety represented by Chemical Formula C is a structure in which the terminal is capped with hydrogen, which may be included in an amount of 15 to 35 wt% based on the total content of Si—H bond in the polysilazane or polysiloxazane structure. When the part of the formula (3) is included in the polysilazane or polysiloxazane structure in the above range, while the oxidation reaction occurs during the heat treatment to prevent the shrinkage by preventing the SiH 3 portion is scattered to SiH 4 during heat treatment, thereby Cracks can be prevented from occurring.
The solvent included in the composition for forming a silica film is not particularly limited as long as it is a solvent capable of dissolving the silicon-containing polymer, and specifically, benzene, toluene, xylene, ethylbenzene, diethylbenzene, trimethylbenzene, triethylbenzene, Cyclohexane, cyclohexene, decahydro naphthalene, dipentene, pentane, hexane, heptane, octane, nonane, decane, ethylcyclohexane, methylcyclohexane, cyclohexane, cyclohexene, p-mentane, dipropylether, dibutyl It may include at least one selected from the group consisting of ether, diisoamyl ether, anisole, butyl acetate, amyl acetate, methyl isobutyl ketone and combinations thereof.
The silica film forming composition may further include a thermal acid generator (TAG).
The thermal acid generator is an additive for improving the developability of the composition for forming a silica film, so that the polymer included in the composition may be developed at a relatively low temperature.
The thermal acid generator is not particularly limited as long as it is a compound capable of generating an acid (H + ) by heat, but may be selected to be activated at 90 ° C. or higher to generate sufficient acid and have low volatility.
The thermal acid generator may for example be selected from nitrobenzyltosylate, nitrobenzylbenzenesulfonate, phenol sulfonate and combinations thereof.
The thermal acid generator may be included in an amount of 0.01 to 25% by weight relative to the total content of the silica film forming composition, and when included in the above range, the polymer may be developed at a relatively low temperature and may improve coating properties. .
The composition for forming a silica film may further include a surfactant.
Surfactant is not specifically limited, For example, polyoxyethylene alkyl ethers, such as polyoxyethylene lauryl ether, polyoxyethylene stearyl ether, polyoxyethylene cetyl ether, polyoxyethylene oleyl ether, polyoxyethylene nonyl phenol ether Polyoxyethylene alkyl allyl ethers, polyoxyethylene polyoxypropylene block copolymers, sorbitan monolaurate, sorbitan monopalmitate, sorbitan monostearate, sorbitan monooleate, polyoxyethylene sorbita Nonionic surfactants, such as polyoxyethylene sorbitan fatty acid ester, such as tanmonostearate, polyoxyethylene sorbitan trioleate, and polyoxyethylene sorbitan tristearate, F-top EF301, EF303, EF352 Products), Megapack F171, F173 (manufactured by Dainippon Ink Co., Ltd.), Prorad FC430, FC431 (Sumitomo ThreeM Co., Ltd.) Fluorine-based surfactants such as Asahi Guard AG710, Saffron S-382, SC101, SC102, SC103, SC104, SC105, and SC106 (manufactured by Asahi Glass Co., Ltd.), and organosiloxane polymer KP341 (Shin-Etsu Chemical Co., Ltd.) Note) manufactured) and other silicone surfactants.
The surfactant may be included in an amount of 0.001 to 10% by weight based on the total content of the composition for forming a silica film. When included in the above range, the surfactant may improve the dispersibility of the solution and at the same time increase the uniformity of the film thickness.
According to another embodiment, the method may include applying the silica film forming composition, drying the substrate coated with the silica film forming composition, and curing the silica film forming composition. .
The composition for forming a silica film may be applied by a solution process, for example, by a method such as spin-on coating, slit coating, inkjet printing, or the like.
The substrate may be, for example, a device substrate such as a semiconductor or a liquid crystal, but is not limited thereto.
When the application of the composition for forming a silica film is completed, the substrate is then dried and cured. The drying and curing may be performed at a temperature of, for example, about 100 ° C. or more, and may be performed by applying energy such as heat, ultraviolet light, microwaves, sound waves, or ultrasonic waves.
For example, the drying may be performed at about 100 ° C to about 200 ° C, and the solvent in the composition for forming a silica film may be removed by going through the drying step. In addition, the curing may be carried out at about 250 ℃ to 1,000 ℃, it is possible to convert the composition for forming a silica film into a thin film of the oxide film by going through the curing step. The curing step may be, for example, after the first curing in a steam atmosphere of 250 ℃ to 1,000 ℃, the secondary curing in a nitrogen atmosphere of 600 ℃ to 1,000 ℃.
According to yet another embodiment there is provided a silica membrane prepared according to the method described above. The silica film may be, for example, an insulating film, a separator, or a protective film such as a hard coating, but is not limited thereto.
According to another embodiment of the present invention provides an electronic device comprising a silica film prepared according to the above-described method. The electronic device may be, for example, a display device such as an LCD or an LED, or a semiconductor device.
Hereinafter, embodiments of the present invention described above will be described in more detail with reference to Examples. However, the following examples are merely for illustrative purposes and do not limit the scope of the present invention.
Preparation of Silicon-Containing Polymers
Comparative Polymerization Example One
Agitated with a capacity of 2 L and the inside of the reactor with a temperature controller was replaced with dry nitrogen. Then, 1,500 g of dry pyridine was injected and sufficiently mixed, and then put into a reactor and kept at 5 ° C. Then, 140 g of dichlorosilane was slowly injected and stirred over 2 hours, while 85 g of ammonia was slowly injected over 4 hours. Next, dry nitrogen was injected for 120 minutes and the ammonia remaining in the reactor was removed. The obtained white slurry product was filtered using a 1 micrometer filter made of Teflon in a dry nitrogen atmosphere to obtain 1,000 g of a filtrate. After adding 1,000 g of dried xylene to this, the operation of replacing the solvent from pyridine to xylene using a rotary evaporator was repeated three times, and the solid content concentration was adjusted to 20% by weight. It filtered with the filter made of Teflon. 250 g of dry pyridine was added to the obtained solution after filtration, and the polymerization was carried out so that the weight average molecular weight was 4,000 at 100 占 폚.
When the polymerization was completed, the operation of substituting the solvent with dibutyl ether using a rotary evaporator was repeated three times at 30 ° C. to adjust the solid content concentration to 20% by weight, and filtered with a 0.1 μm pron filter to form a silicon-containing polymer. (I) was obtained. Analysis of the obtained solution by FT-IR showed that polysilazane was formed, and the GPC (PLC Pump 1515, RI Detector 2414, manufactured by Waters, Inc.) showed a weight average molecular weight of 4,500.
Polymerization example One
The inside of the reactor with a stirring and a temperature control device having a capacity of 2 L was replaced with dry nitrogen. Then, 1,200 g of dry pyridine was injected and sufficiently mixed, and then placed in a reactor and kept at room temperature. Subsequently, 120 g of TSA, manufactured by Air liquid, was slowly injected and stirred over 30 minutes. Next, the temperature of the reactor was set to 40 ° C., and dry nitrogen was injected to remove gases remaining in the reactor. After 100 hours, the operation of replacing the solution in which polymerization was completed with dibutyl ether was repeated four times at 40 ° C. to adjust the solid content concentration to 20 wt%. This was filtered through a 0.1 µm Teflon filter to obtain Silicon-containing polymer (II). The obtained solution was analyzed by GPC (Water Pump Co., Ltd. GPC (PLC Pump 1515, RI Detector 2414)) and the weight average molecular weight was 4,500.
Polymerization example 2
The inside of the reactor with a stirring and a temperature control device having a capacity of 2 L was replaced with dry nitrogen. Then, 1,300 g of dry pyridine was injected and sufficiently mixed, and then placed in a reactor and maintained at -10 ° C. Subsequently, 23 g of TSA, manufactured by Air liquid, was slowly injected and stirred over 5 minutes. The temperature of the reactor was set to -10 ° C and 2 g of ammonia was slowly injected over 80 minutes. The gas remaining in the reactor was then removed while injecting dry nitrogen for 12 hours. The operation of substituting the solution having completed polymerization with dibutyl ether was repeated four times at 40 ° C. to adjust the solid content concentration to 20% by weight. This was filtered through a filter made of 0.1 μm Teflon to obtain silicon-containing polymer (III). The obtained solution was analyzed by GPC (Water Pump Co., Ltd. GPC (PLC Pump 1515, RI Detector 2414)) and the weight average molecular weight was 4,500.
Preparation of Silica Membrane
Comparative example One
The silicon-containing polymer 1 obtained in Comparative Polymerization Example 1 was mixed with a dibutyl ether solvent to prepare a composition for forming a silica film having a solid content of 20% by weight.
Thereafter, the silica film forming composition was spin-coated on an 8-inch silicon wafer, followed by soft baking at 150 ° C. for 3 minutes, and then placed in a furnace (SJJ-1000 manufactured by Sungjinsemitec Co., Ltd.), and curing conditions as shown in Table 2 below. The silica thin films were formed by changing the amounts of silica.
Example One
A silica thin film was formed in the same manner as in Comparative Example 1 except that the silicon-containing polymer (II) obtained in Polymerization Example 1 was used instead of the silicon-containing polymer (I) obtained in Comparative Polymerization Example 1.
Example 2
A silica thin film was formed in the same manner as in Comparative Example 1 except that the silicon-containing polymer (III) obtained in Polymerization Example 2 was used instead of the silicon-containing polymer (I) obtained in Comparative Polymerization Example 1.
Evaluation 1: Nitrogen Content
Nitrogen content of each silicon-containing polymer obtained in Comparative Polymerization Example 1, Polymerization Examples 1 and 2 was measured using BUCHI KjelFled K-360 equipment, the results are shown in Table 1 below.
Evaluation 2: membrane shrinkage
The shrinkage ratios of the silica films obtained in Comparative Examples 1, 1 and 2 were measured. Membrane shrinkage was calculated according to the following equations (1) and (2). In the following Equations 1 and 2, the thickness of the thin film was measured using a K-MAC Reflect Spectrophotometer (ST-4000).
[Equation 1]
Membrane shrinkage (%) when curing was only performed first = (film thickness after curing-film thickness before curing) / (film thickness before curing) × 100
[Equation 2]
Membrane shrinkage (%) when curing proceeded through 2 times = (film thickness after secondary curing-film thickness after primary curing) / (film thickness after primary curing) × 100
The membrane shrinkage evaluation results are shown in Table 2 below.
* Curing condition 1: Heat treatment for 1 hour in a steam atmosphere at 250 ℃
Cure condition 2: Heat treatment for 1 hour in a steam atmosphere at 600 ℃
Curing condition 3: Heat treatment for 1 hour in a steam atmosphere at 1,000 ℃
Curing condition 4: Heat treatment for 1 hour (primary curing) in a steam atmosphere at 400 ℃, heat treatment for 1 hour in a nitrogen atmosphere at 600 ℃ (second curing)
Referring to Tables 1 and 2, it can be seen that the silica membranes of Examples 1 and 2 prepared using the silicon-containing polymers according to Synthesis Examples 1 and 2 had a nitrogen content in the range of 20% to 28% by weight. In addition, it was found that the silica membranes of Examples 1 and 2 prepared using the silicon-containing polymers according to Polymerization Examples 1 and 2 had a relatively small value of film shrinkage under the same curing conditions as compared to the silica membrane of Comparative Example 1. In addition, it can be seen that the silica membranes of Examples 1 and 2 have a relatively excellent film shrinkage rate even under low temperature curing conditions.
Although preferred embodiments of the present invention have been described in detail above, the scope of the present invention is not limited thereto, and various modifications and improvements of those skilled in the art using the basic concepts of the present invention defined in the following claims are also provided. It belongs to the scope of the present invention.
Claims (8)
[Formula 1]
N [SiR 1 R 2 R 3 ] 3
In Chemical Formula 1,
R 1 , R 2 and R 3 are each independently hydrogen, a substituted or unsubstituted C1 to C10 alkyl group, a substituted or unsubstituted vinyl group, a substituted or unsubstituted phenyl group, or a combination thereof,
[Formula 2]
NR 4 R 5 R 6
In Chemical Formula 2,
R 4 to R 6 are each independently a substituted or unsubstituted C1 to C10 alkyl group, a substituted or unsubstituted vinyl group, a substituted or unsubstituted phenyl group, or a combination thereof,
The compound represented by Formula 1 and the compound represented by Formula 2 are polymerized in a molar ratio of 1: 0.3 to 1: 1,
The silicon-containing polymer is a composition for forming a silica film having a nitrogen content of 20% to 28% by weight of the entire silicon-containing polymer.
The silicon-containing polymer has a weight average molecular weight of 1,000 to 100,000 composition for forming a silica film.
The solvent is benzene, toluene, xylene, ethylbenzene, diethylbenzene, trimethylbenzene, triethylbenzene, cyclohexane, cyclohexene, decahydrnaphthalene, dipentene, pentane, hexane, heptane, octane, nonane, decane, Group consisting of ethylcyclohexane, methylcyclohexane, cyclohexane, cyclohexene, p-mentane, dipropyl ether, dibutyl ether diisoamyl ether, anisole, butyl acetate, amyl acetate, methyl isobutyl ketone and combinations thereof Silica film forming composition comprising at least one selected from.
Drying the substrate coated with the composition for forming a silica film, and
Curing the silica film-forming composition at 250 ° C. to 1,000 ° C.
Silica film production method comprising a.
The curing step is a method of producing a silica membrane comprising the second step of curing in a nitrogen atmosphere of 600 ℃ to 1,000 ℃ after the first curing in a steam atmosphere of 250 ℃ to 1,000 ℃.
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