WO2012108072A1 - Composition pour former un film de revêtement contenant de la silice pour des applications de jet d'encre, procédé pour former un film de revêtement contenant de la silice, dispositif à semi-conducteur, et système de cellule solaire - Google Patents

Composition pour former un film de revêtement contenant de la silice pour des applications de jet d'encre, procédé pour former un film de revêtement contenant de la silice, dispositif à semi-conducteur, et système de cellule solaire Download PDF

Info

Publication number
WO2012108072A1
WO2012108072A1 PCT/JP2011/069198 JP2011069198W WO2012108072A1 WO 2012108072 A1 WO2012108072 A1 WO 2012108072A1 JP 2011069198 W JP2011069198 W JP 2011069198W WO 2012108072 A1 WO2012108072 A1 WO 2012108072A1
Authority
WO
WIPO (PCT)
Prior art keywords
boiling point
solvent
silica
mass ratio
content
Prior art date
Application number
PCT/JP2011/069198
Other languages
English (en)
Japanese (ja)
Inventor
貴浩 吉川
悠平 岡田
治彰 桜井
恭 神代
格 山浦
Original Assignee
日立化成工業株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 日立化成工業株式会社 filed Critical 日立化成工業株式会社
Priority to JP2012556748A priority Critical patent/JPWO2012108072A1/ja
Publication of WO2012108072A1 publication Critical patent/WO2012108072A1/fr

Links

Classifications

    • 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
    • C09D183/04—Polysiloxanes
    • 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
    • C09D11/00—Inks
    • C09D11/30—Inkjet printing inks
    • C09D11/36—Inkjet printing inks based on non-aqueous solvents
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/20—Diluents or solvents

Definitions

  • the present invention relates to a silica-based film forming composition for inkjet, a method for forming a silica film, a semiconductor device, and a solar cell system.
  • Silica-based coatings are applied in various fields because they are excellent in insulation, heat resistance, transparency, wear resistance, and the like.
  • it is used as an insulation film between wires, element isolation films and mask materials from the viewpoint of insulation, heat resistance, and barrier properties.
  • insulation, heat resistance, and transparency are used in liquid crystal devices. From the viewpoint of performance, it is applied as a protective film of the element.
  • a gas phase growth method and a coating method are known as general methods for obtaining a silica-based film.
  • the gas layer growth method is widely applied and has a feature that a dense silica film can be obtained.
  • the coating method has features such that film formation can be performed with a relatively simple apparatus and film formation on a large-sized substrate is relatively easy. Examples of the coating method include spin coating, spraying, dipping, roll coating, and screen printing.
  • Patent Document 1 An inkjet method has been studied as a method for easily and inexpensively forming a pattern. Since the inkjet method can form a desired pattern at a desired position, it is not necessary to form a silica film on the entire surface of the substrate unlike the photolithography method, and the amount of material to be used can be greatly reduced. There is a big merit in terms of environment.
  • Patent Documents 2 and 3 As a method for obtaining an ink jet-compatible silica-based film forming composition, a sol-gel method using alkoxysilane as a raw material is known (Patent Documents 2 and 3).
  • Patent Document 2 when ethanol or water is used as a solvent, or as described in Patent Document 3, a solvent at 100 ° C. or less may occupy 70 to 90% by weight of the entire composition. In such a case, if the non-ejection and ejection operations are repeated in ink jet drawing, nozzle clogging is likely to occur. In mass production, since such discharge and non-discharge are repeated, the conventional silica-based film-forming composition is not yet sufficient for practical use.
  • the silica-based film forming composition for ink jet is required to have a characteristic that the pattern at the time of drawing is difficult to bleed when the pattern is drawn using the composition.
  • the nozzle tip of the silica-based film forming composition for ink jet It is necessary to satisfy both the non-drying property and the quick drying property at the time of pattern drawing. However, it is very difficult to satisfy these conflicting characteristics.
  • the present invention provides a silica-based film-forming composition for inkjet that can be ejected without causing clogging of inkjet nozzles even when the operations of non-ejection and ejection are repeated, and the pattern at the time of drawing is difficult to bleed, and the composition
  • An object of the present invention is to provide a method for forming a silica-based film using a product, a semiconductor device, and a solar cell system.
  • the present invention provides a silica-based film-forming composition for inkjet as described in the following (1) and (2), a method for forming a silica-based film as described in (3) below, (4) And the solar cell system described in the following (5).
  • the silica-type film formation composition for inkjets which satisfies the relationship represented by the following conditions A, B, or C.
  • Condition A When the boiling point of the first solvent is 80 to 100 ° C., the mass ratio is 0.3 to 0.5.
  • Condition B When the boiling point of the first solvent is 100 to 130 ° C., the mass ratio is 0.4 to 0.6.
  • Condition C When the boiling point of the first solvent is 130 to 160 ° C., the mass ratio is 0.5 to 0.7.
  • R 1 n SiX 4-n (I) [Wherein R 1 represents an organic group having 1 to 20 carbon atoms, X represents a hydrolyzable group, and n represents an integer of 0 to 2.
  • n 2
  • a plurality of R 1 may be the same or different
  • n 0 to 2
  • a plurality of X 1 may be the same or different.
  • a semiconductor device comprising a substrate and a silica-based coating film having a pattern formed on the substrate by the method described in (3).
  • (5) A solar cell system comprising the semiconductor device according to (4).
  • a silica-based film-forming composition for inkjet that can be ejected without causing clogging of inkjet nozzles even when the operations of non-ejection and ejection are repeated, and the pattern at the time of drawing is difficult to bleed, and A method for forming a silica-based film using the composition, a semiconductor device, and a solar cell system are provided.
  • a mixed solvent containing a first solvent that is a low-boiling component and a second solvent that is a high-boiling component is used as the solvent for the silica-based film-forming composition for inkjet. This is very important.
  • the non-drying property at the nozzle tip is achieved at a high level mainly by the action of the second solvent, and the quick drying property at the time of drawing is mainly achieved by the action of the first solvent.
  • the solvent contained in the ink-jet silica-based film forming composition of the present invention is such that the mass ratio of the content of the first solvent to the total content of the first solvent and the second solvent is the above-mentioned conditions A to C. One of the above is satisfied. This is based on the knowledge of the present inventors that these conditions are suitable from the viewpoint of compatibility between non-drying at the nozzle tip of the silica-based film-forming composition for inkjet and quick drying at the time of pattern drawing. It is.
  • the effect that the pattern at the time of drawing hardly bleeds is also due to the fact that the silica-based film-forming composition for inkjet contains a surface conditioner. Accordingly, it is considered that bleeding of the drawing pattern is suppressed by controlling the wettability to the substrate and the fluidity of the silica-based resin. More specifically, the bleeding of the drawing pattern is caused by a local increase in ink viscosity or surface due to non-uniform wetting (repelling, etc.) of the ink on the coated object or non-uniform evaporation of the solvent of the ink during ejection. It is thought to be caused by a change in tension.
  • the surface conditioner in the present invention is (1) a compound having the action of uniformizing the surface tension of the coating film in the drying process and improving the wettability to the coating object, and (2) evaporation of the solvent from the coating film surface.
  • the silica-based film-forming composition for inkjet contains the following components (a) to (c).
  • condition A When the boiling point of the first solvent is 80 to 100 ° C., the mass ratio is 0.3 to 0.5.
  • Condition B When the boiling point of the first solvent is 100 to 130 ° C., the mass ratio is 0.4 to 0.6.
  • Condition C When the boiling point of the first solvent is 130 to 160 ° C., the mass ratio is 0.5 to 0.7. (C) Surface conditioner.
  • (A) Component Silicon compound
  • the silica-based film-forming composition for ink jet according to this embodiment has a silicon compound obtained by hydrolysis and polycondensation of the compound represented by the general formula (I) as an essential component. .
  • hydrolysis / polycondensation means that the compound represented by the general formula (I) is hydrolyzed, condensed while dehydrating (H 2 O), and polymerized. To do.
  • Examples of X in the general formula (I) include an alkoxy group, a halogen atom, an acetoxy group, an isocyanate group, and a hydroxyl group, and among these, an alkoxy group is preferable.
  • alkoxysilane examples include tetraalkoxysilane represented by the following general formula (I-1), trialkoxysilane represented by the following general formula (I-2), and the following general formula (I Dialkoxysilane represented by -3).
  • An alkoxysilane may be used individually by 1 type, and may be used in combination of 2 or more type.
  • Si (OR 2 ) 4 (I-1) Wherein R 2 may be the same or different and each independently represents an alkyl group.
  • R 3 Si (OR 4 ) 3 (I-2) [Wherein R 3 represents an alkyl group or a phenyl group, the phenyl group may have a substituent, and R 4 may be the same or different, and each independently represents an alkyl group. ]
  • R 5 2 Si (OR 6 ) 2 (I-3) [In the formula, R 5 may be the same or different, each independently represents an alkyl group or a phenyl group, the phenyl group may have a substituent, and R 6 may be the same or different, Each independently represents an alkyl group. ]
  • the number of carbon atoms of the alkoxy group R (R 2 , R 4 and R 6 ) is not particularly limited, Usually, it has 1 to 10 carbon atoms, preferably 1 to 5 carbon atoms, more preferably 1 to 3 carbon atoms from the viewpoint of availability. Further, R (R 2 , R 4, and R 6 ) of the alkoxy group may be one in which a part of hydrogen atoms is substituted with fluorine.
  • Examples of the tetraalkoxysilane represented by the general formula (I-1) include tetramethoxysilane, tetraethoxysilane, tetra-n-propoxysilane, tetra-iso-propoxysilane, and tetrabutoxysilane. Of these, tetraethoxysilane is preferably used in terms of reactivity and reaction by-products.
  • trialkoxysilanes represented by the general formula (I-2) include methyltrimethoxysilane, methyltriethoxysilane, methyltri-n-propoxysilane, methyltri-iso-propoxysilane, ethyltrimethoxysilane, and ethyltriethoxysilane.
  • methyltriethoxysilane, ethyltriethoxysilane, propyltriethoxysilane, and phenyltriethoxysilane are preferably used in terms of reactivity and reaction by-products.
  • dialkoxysilanes represented by the general formula (I-3) include dimethyldimethoxysilane, dimethyldiethoxysilane, dimethyldi-n-propoxysilane, dimethyldi-iso-propoxysilane, diethyldimethoxysilane, diethyldiethoxysilane, and diethyldiethoxysilane.
  • the alkoxysilanes represented by the general formula (I-1), general formula (I-2) and general formula (I-3) may be used alone or in combination of two or more. Also good.
  • the alkoxysilanes represented by the general formula (I-1), general formula (I-2) and general formula (I-3) are used in combination of two or more, the mixing ratio is not particularly limited.
  • the general formula (I -1) The molar amount M 2 of the trialkoxysilane represented by the general formula (I-2) and the dialkoxy represented by the general formula (I-3) relative to the molar amount M 1 of the tetraalkoxysilane represented by -1)
  • the ratio (M 2 + M 3 ) / M 1 of the total amount of the silane molar amount M 3 is preferably 0.1 or more, more preferably 0.5 or more, and 0.8 or more. Highly preferred. From the viewpoint of good wettability with the base substrate, (M 2 + M 3 ) / M 1 is preferably 4.0 or less, more preferably 2.5 or less, and 1.5 or less. It is very preferable that
  • the component (b) may be used as a solvent, or a solvent other than the component (b) may be used.
  • Solvents used for hydrolysis and polycondensation of alkoxysilane include acetone, methyl ethyl ketone, methyl-n-propyl ketone, methyl-iso-propyl ketone, methyl-n-butyl ketone, methyl-iso-butyl ketone, methyl-n- Pentyl ketone, methyl-n-hexyl ketone, diethyl ketone, dipropyl ketone, di-iso-butyl ketone, trimethylnonanone, cyclohexanone, cyclopentanone, methylcyclohexanone, 2,4-pentanedione, acetonylacetone, ⁇ -butyrolactone Ketone solvents such as ⁇ -val
  • the solvent when a solvent other than the component (b) is used when hydrolyzing and polycondensing the alkoxysilane, the solvent is removed by distillation after the reaction, and the resulting siloxane resin is used as a silica-based film-forming composition for inkjet. It can be used for the preparation of products.
  • the amount of the solvent when the general formula (I-1), the general formula (I-2), and the general formulas to (I-3) are hydrolyzed and polycondensed using the above-mentioned solvent is determined depending on the uniformity of the reaction. Therefore, it is preferable that the SiO 2 equivalent concentration be in the range of 5% by mass to 35% by mass, the lower limit being 10% by mass or more, and the upper limit being 30% by mass or less. .
  • a catalyst when hydrolyzing and polycondensing alkoxysilane, a catalyst can be added to shorten the reaction time and make the reaction uniform.
  • the catalyst include an acid catalyst, an alkali catalyst, a metal chelate compound, and the like, but it is preferable to use an acid catalyst from the viewpoint of ensuring the stability of the resulting silica-based film-forming composition for inkjet.
  • Examples of the acid catalyst include organic acids and inorganic acids.
  • organic acids include formic acid, maleic acid, fumaric acid, phthalic acid, malonic acid, succinic acid, tartaric acid, malic acid, lactic acid, citric acid, acetic acid, propionic acid, butanoic acid, pentanoic acid, hexanoic acid, heptanoic acid , Octanoic acid, nonanoic acid, decanoic acid, oxalic acid, adipic acid, sebacic acid, butyric acid, oleic acid, stearic acid, linoleic acid, linolenic acid, salicylic acid, benzenesulfonic acid, benzoic acid, p-aminobenzoic acid, p- Examples include toluenesulfonic acid, methanesulfonic acid, trifluoromethanesulfonic acid and trifluoroethanesulfonic acid.
  • inorganic acids examples include hydrochloric acid, phosphoric acid, nitric acid, boric acid, sulfuric acid, and hydrofluoric acid.
  • maleic acid as the organic acid and nitric acid as the inorganic acid.
  • the amount of catalyst used can be appropriately selected according to the type and amount of alkoxysilane, the type of catalyst, and the like.
  • a tetraalkoxysilane represented by the general formula (I-1), a trialkoxysilane represented by the general formula (I-2), and a dialkoxysilane represented by the general formula (I-3) are used in combination.
  • an acid catalyst is used as the catalyst, the molar ratio of the tetraalkoxysilane represented by the general formula (I-1) to the total number of moles of the alkoxysilane is represented by A and the trioxide represented by the general formula (I-2).
  • the amount (molar ratio) of the acid catalyst used is [(4A + 3B + 2C) / 3000] to [
  • the range of (4A + 3B + 2C) / 10] is preferable, and the range of [(4A + 3B + 2C) / 3000] to [(4A + 3B + 2C) / 100] is more preferable.
  • the amount of water to be used can be appropriately selected according to the type and amount of the alkoxysilane used.
  • a tetraalkoxysilane represented by general formula (I-1), a trialkoxysilane represented by general formula (I-2), and a dialkoxysilane represented by general formula (I-3) are used in combination.
  • the molar ratio of the tetraalkoxysilane represented by the general formula (I-1) to the total number of moles of alkoxysilane is A
  • the molar ratio of the trialkoxysilane represented by the general formula (I-2) is B
  • the amount of water (molar ratio) is preferably in the range of [(4A + 3B + 2C) / 2] to [(4A + 3B + 2C) ⁇ 2]
  • the range of [(4A + 3B + 2C) / 2] to [4A + 3B + 2C) ⁇ 1] is more preferable.
  • the weight average molecular weight (Mw) of the silicon compound as component (a) is preferably from 500 to 20000, more preferably from 500 to 10,000, from the viewpoints of solubility in a solvent and inkjet discharge properties.
  • Mw weight average molecular weight
  • the weight average molecular weight is measured by gel permeation chromatography (hereinafter referred to as “GPC”) and converted using a standard polystyrene calibration curve.
  • the weight average molecular weight (Mw) can be measured, for example, by GPC under the following conditions.
  • Sample 10 ⁇ L of silica-based film forming composition for inkjet Standard polystyrene: Standard polystyrene manufactured by Tosoh Corporation (molecular weight: 190000, 17900, 9100, 2980, 578, 474, 370, 266)
  • Detector manufactured by Hitachi, Ltd., RI-monitor, trade name “L-3000” Integrator: Hitachi, Ltd., GPC integrator, product name “D-2200”
  • Pump Hitachi, Ltd., trade name “L-6000”
  • Degassing device Showa Denko Co., Ltd., trade name "Shodex DEGAS” Column: manufactured by Hitachi Chemical Co., Ltd., trade names “GL-R440”, “GL-R430”, “GL-R420” are used in this order and are used Eluent: Tetrahydrofur
  • the content of the component (a) in the silica-based film-forming composition for inkjet is preferably 5 to 35% by mass, and more preferably 5 to 30% by mass. If the content of the component (a) is 5% by mass or more, the film thickness of the silica-based film to be formed is not too thin and has an appropriate thickness. The possibility of being necessary can be reduced. Thereby, it becomes easy to suppress the increase in process time and the occurrence of bleeding of the drawing pattern due to the overlapping drawing. On the other hand, if content of (a) component is 35 mass% or less, there exists a tendency which can make the storage stability of the silica-type film forming composition for inkjets favorable.
  • (B) Component Solvent
  • the component (b) according to the present embodiment contains a first solvent having a boiling point of 80 to 160 ° C. and a second solvent having a boiling point of 180 to 230 ° C. content (hereinafter, “C 1" hereinafter.) and the content of the second solvent (hereinafter, “C 2" hereinafter.) the total amount of (C 1 + C 2) of the C 1 to the weight ratio C 1 / (C 1 + C 2 ) is a mixed solvent that satisfies the relationship represented by the following conditions A, B, or C.
  • “boiling point” means a boiling point at normal pressure.
  • Condition A When the boiling point of the first solvent is 80 to 100 ° C., 0.3 ⁇ C 1 / (C 1 + C 2 ) ⁇ 0.5.
  • Condition B When the boiling point of the first solvent is 100 to 130 ° C., 0.4 ⁇ C 1 / (C 1 + C 2 ) ⁇ 0.6.
  • Condition C 0.5 ⁇ C 1 / (C 1 + C 2 ⁇ 0.7 when the boiling point of the first solvent is 130 to 160 ° C.
  • the first solvent is not particularly limited as long as the boiling point is in the range of 80 to 160 ° C.
  • the 1st solvent contained in a composition may be 1 type, or 2 or more types.
  • Examples of the first solvent having a boiling point of 80 to 100 ° C. satisfying the condition (A) include 1-propanol, 2-propanol, 2-butanol and the like. Among these solvents, 2-propanol is preferably used because of compatibility with the resulting siloxane resin and the second solvent.
  • Examples of the first solvent having a boiling point of 100 to 130 ° C. satisfying the condition (B) include butyl acetate, isobutyl acetate, propylene glycol monomethyl ether and the like.
  • the boiling point of the first solvent in the condition (B) is preferably 110 to 130 ° C.
  • isobutyl acetate is preferably used because of compatibility with the resulting siloxane resin and the second solvent.
  • Examples of the first solvent having a boiling point of 130 to 160 ° C. satisfying the condition (C) include propylene glycol monopropyl ether, ethyl lactate and cyclohexanone.
  • the boiling point of the first solvent in the condition (C) is preferably 140 to 160 ° C.
  • the second solvent has a boiling point of 180 ° C. to 230 ° C., preferably 180 ° C. to 200 ° C. There is no particular limitation as long as the boiling point is within such a range.
  • the second solvent ⁇ -butyrolactone, ethers and glycols can be used, and examples thereof include dipropylene glycol monomethyl ether and propylene glycol.
  • the second solvent contained in the composition may be one type or two or more types.
  • the mass ratio C 1 / (C 1 + C 2 ) satisfies the relationship represented by the above condition A, condition B, or condition C according to the boiling point of the first solvent. Therefore, it is possible to achieve both non-drying at the nozzle tip when discharging the composition and quick drying at the time of pattern drawing, and the ink jet nozzles will not be clogged even when non-discharge and discharge operations are repeated, and at the time of drawing The pattern can be hard to spread.
  • Component (c) is a surface conditioner.
  • a surface conditioner When the composition contains a surface conditioner, it is possible to control the wettability of the ink to the substrate surface and the cross-sectional shape of the pattern, which is effective in preventing the pattern from bleeding.
  • a commercially available compound as a surface conditioner can be used without particular limitation. Specifically, a fluorine-based surface conditioner, a silicone-based surface conditioner, a nonionic surface conditioner, and the like can be used. Can be used. Of these, the use of a silicone-based surface conditioner is particularly effective in suppressing pattern bleeding.
  • the content of the component (c) is preferably 0.1% by mass or more and more preferably 0.2% by mass or more with respect to the component (a). Moreover, 1.0 mass% or less is preferable with respect to (a) component, and, as for content of (c) component, 0.8 mass% or less is more preferable.
  • (c) component may be used individually by 1 type or in combination of 2 or more types.
  • the method for forming a silica-based film according to the present embodiment includes a step of forming a drawing pattern film by discharging the composition onto a substrate by an inkjet method to form a drawing pattern film, and a step of precuring the drawing pattern film. And a step of curing the drawing pattern film to obtain a silica-based film having a pattern.
  • Pattern drawing by the inkjet method can be performed using an inkjet apparatus.
  • Ink jet devices are generally roughly classified into two types, a continuous type (continuous discharge type) and an on-demand type.
  • the continuous type is a system in which ink is always ejected continuously even when a pattern is not drawn on a substrate.
  • On-demand type is a method of drawing a pattern on a substrate by ejecting ink in a necessary amount when necessary.
  • the on-demand type includes an inkjet apparatus using a piezoelectric element that deforms when a voltage is applied, and a thermal inkjet apparatus that discharges using bubbles generated by heating.
  • the silica-based film-forming composition for inkjet according to the present embodiment may basically use either method, but it is preferable to use an inkjet device using a piezo element from the viewpoint of suppressing ink composition change. .
  • the substrate on which the pattern is drawn may be drawn while being heated in the range of 50 to 100 ° C.
  • the quick drying property of the ink on the substrate can be further improved, and the disorder of the drawing pattern can be prevented.
  • a step of precuring the drawing pattern film may be provided before the step of curing the drawing pattern film.
  • the polycondensation reaction of the siloxane resin in the drawing pattern film is accelerated and the organic solvent is heated with a hot plate or the like at the first stage baking: 80 to 140 ° C. and the second stage baking: 180 to 250 ° C. You may perform drying in steps.
  • the first stage and the second stage bake may be further multistaged. By the multi-stage baking, the siloxane resin is uniformly cured, and it is possible to prevent the drawing pattern from being disturbed due to the thermal convection when the solvent is removed.
  • Step of curing drawing pattern film> the final curing is performed, for example, by baking the drawing pattern film (which may not be precured) at a heating temperature of 350 to 1000 ° C. If the heating temperature for final curing is 350 ° C. or higher, sufficient curing is easily achieved, and if it is 1000 ° C. or lower, the substrate is unlikely to be adversely affected.
  • the heating time for the final curing is preferably 2 to 60 minutes, more preferably 2 to 30 minutes. If this heating time is 60 minutes or less, the amount of heat input will not increase excessively, and thus the deterioration of the substrate will be suppressed gradually.
  • a heat treatment device such as a quartz tube furnace, other furnaces, a hot plate, rapid thermal annealing (RTA), UV irradiation annealing, EB irradiation annealing, or the like can be used.
  • the atmosphere of the gas at the time of final curing may be either an inert gas atmosphere such as nitrogen, argon or helium, or an active gas atmosphere such as oxygen or ozone, as long as the substrate is not adversely affected.
  • the use of the silica-based film forming composition for inkjet according to the present embodiment and the method for forming the silica-based film is not particularly limited, but for example, it can be used for a device including an insulating film such as a semiconductor device (element) or a multilayer wiring board. Can be mentioned. More specifically, in a semiconductor device, it can be used as a surface protective film (passivation film), a buffer coat film, an interlayer insulating film, a diffusion prevention film, and the like. On the other hand, in a multilayer wiring board, it can be suitably used as an interlayer insulating film.
  • the semiconductor device of this embodiment includes a substrate and a silica-based film having a predetermined pattern formed on the substrate by the method for forming a silica-based film.
  • Such semiconductor devices include, for example, individual semiconductors such as diodes, transistors, compound semiconductors, thermistors, varistors, thyristors, DRAMs (Dynamic Random Access Memory), SRAMs (Static Random Access Memory), EPROMs.
  • Theoretical circuit elements such as ASIC, integrated circuit elements such as compound semiconductors represented by MMIC (monolithic microwave integrated circuit), hybrid integrated circuits (hybrid IC) , Light emitting diodes, and a photoelectric conversion element such as a charge coupled device.
  • MMIC monolithic microwave integrated circuit
  • hybrid integrated circuits hybrid integrated circuits
  • Light emitting diodes and a photoelectric conversion element such as a charge coupled device.
  • examples of the multilayer wiring board include a high-density wiring board such as MCM.
  • the solar cell system of this embodiment includes the semiconductor device.
  • the photoelectric conversion element is a semiconductor device used in a solar cell system, and has been actively developed due to the influence of recent environmental problems.
  • a typical photoelectric conversion element includes a semiconductor Si wafer in which an impurity called a dopant is diffused to form a pn junction.
  • an element in which a non-diffusion region and a diffusion region of a dopant are mixed on one Si wafer is sometimes produced in order to increase the efficiency of the solar cell. In such a case, it is necessary to form a diffusion prevention mask in the non-diffusion region.
  • a diffusion prevention mask has been obtained by patterning a silica-based film formed by CVD or the like by a photolithography method.
  • the silica-based film forming composition for inkjet according to the present embodiment is used, a silica-based film patterned by inkjet can be obtained, which is useful because the number of steps and the necessary materials can be reduced.
  • the silica-based coating according to this embodiment can be used for applications such as liquid crystal parts, optical waveguides, and photoresists, but the usage is not limited to this.
  • the siloxane resin solid content concentration of the silicon compound A at this time was 60% by mass.
  • the siloxane resin solid content concentration of the silicon compound B at this time was 60% by mass.
  • silicon compound C was obtained by adding tetraethylene glycol dimethyl ether until the total amount of the silicon compound solution reached 100 g. At this time, the siloxane resin solid content concentration of the silicon compound C was 60% by mass.
  • Example 1 To the silicon compound A, 0.3 g of Dispalon 1711 (trade name, manufactured by Enomoto Kasei Co., Ltd., registered trade name) is added and stirred to the silicon compound A, and 2-propanol (boiling point 82 ° C.) is added to 17. 2g was added. At this time, the mass ratio of the 2-propanol content to the total content of 2-propanol (boiling point 82 ° C.) and dipropylene glycol monomethyl ether (boiling point 188 ° C.) was 0.3. Moreover, the siloxane resin solid content concentration at this time was 51%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.3 is added until the solid content concentration of the siloxane resin is 20%.
  • Silica-based film-forming composition A-1 was produced.
  • Example 2 To the silicon compound A, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 26.7 g of 2-propanol (boiling point 82 ° C.) was added. At this time, the mass ratio of the content of 2-propanol to the total content of 2-propanol (boiling point 82 ° C.) and dipropylene glycol monomethyl ether (boiling point 188 ° C.) was 0.4. At this time, the siloxane resin solid content concentration was 47%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.4 is added until the solid content concentration of the siloxane resin reaches 20%.
  • Silica-based film forming composition A-2 was prepared.
  • Example 3 To the silicon compound A, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 40.0 g of 2-propanol (boiling point 82 ° C.) was added. At this point, the mass ratio of the 2-propanol content to the total content of 2-propanol (boiling point 82 ° C.) and dipropylene glycol monomethyl ether (boiling point 188 ° C.) was 0.5. Moreover, the siloxane resin solid content concentration at this time was 43%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.5 is added until the solid content concentration of the siloxane resin reaches 20%.
  • Silica-based film forming composition A-3 was produced.
  • Example 4 To the silicon compound A, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 17.2 g of 1-propanol (boiling point 97 ° C.) was added. At this time, the mass ratio of the content of 1-propanol to the total content of 1-propanol (boiling point 97 ° C.) and dipropylene glycol monomethyl ether (boiling point 188 ° C.) was 0.3. Moreover, the siloxane resin solid content concentration at this time was 51%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.3 is added until the solid content concentration of the siloxane resin is 20%.
  • Silica-based film forming composition A-4 was prepared.
  • Example 5 To the silicon compound B, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 17.2 g of 2-propanol (boiling point 82 ° C.) was added. At this point, the mass ratio of the 2-propanol content to the total content of 2-propanol (boiling point 82 ° C.) and dimethyltriglycol (boiling point 216 ° C.) was 0.3. Moreover, the siloxane resin solid content concentration at this time was 51%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.3 is added until the solid content concentration of the siloxane resin is 20%.
  • Silica-based film forming composition A-5 was produced.
  • Example 6 To the silicon compound B, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 40.0 g of 2-propanol (boiling point 82 ° C.) was added. At this time, the mass ratio of the content of 2-propanol to the total content of 2-propanol (boiling point 82 ° C.) and dimethyltriglycol (boiling point 216 ° C.) was 0.5. Moreover, the siloxane resin solid content concentration at this time was 43%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.5 is added until the solid content concentration of the siloxane resin reaches 20%.
  • Silica-based film forming composition A-6 was produced.
  • Example 7 To the silicon compound B, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 17.2 g of 1-propanol (boiling point 97 ° C.) was added. At this time, the mass ratio of the content of 1-propanol to the total content of 1-propanol (boiling point 97 ° C.) and dimethyltriglycol (boiling point 216 ° C.) was 0.3. Moreover, the siloxane resin solid content concentration at this time was 51%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.3 is added until the solid content concentration of the siloxane resin is 20%.
  • Silica-based film forming composition A-7 was produced.
  • Example 8 To the silicon compound A, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 10.0 g of 2-propanol (boiling point 82 ° C.) was added. At this point, the mass ratio of the 2-propanol content to the total content of 2-propanol (boiling point 82 ° C.) and dipropylene glycol monomethyl ether (boiling point 188 ° C.) was 0.2. Moreover, the siloxane resin solid content concentration at this time was 55%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.2 until the siloxane resin solid content concentration becomes 20% is added to the inkjet.
  • a silica-based film-forming composition a-1 was produced.
  • Example 9 To the silicon compound A, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 60.0 g of 2-propanol (boiling point 82 ° C.) was added. At this time, the mass ratio of the content of 2-propanol to the total content of 2-propanol (boiling point 82 ° C.) and dipropylene glycol monomethyl ether (boiling point 188 ° C.) was 0.6. At this time, the siloxane resin solid content concentration was 38%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.6 is added until the solid content concentration of the siloxane resin reaches 20%.
  • Silica-based film forming composition a-2 was prepared.
  • Example 11 To the silicon compound A, 0.3 g of Dispalon 1711 which is a silicone surface conditioner was added and stirred, and 17.2 g of isobutyl acetate (boiling point 118 ° C.) was added. At this time, the mass ratio of the content of isobutyl acetate to the total content of isobutyl acetate (boiling point 118 ° C.) and dipropylene glycol monomethyl ether (boiling point 188 ° C.) was 0.3. Moreover, the siloxane resin solid content concentration at this time was 51%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.3 is added until the solid content concentration of the siloxane resin is 20%.
  • Silica-based film forming composition a-4 was prepared.
  • Example 12 To the silicon compound C, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 40.0 g of 2-propanol (boiling point 82 ° C.) was added. At this time, the mass ratio of the content of 2-propanol to the total content of 2-propanol (boiling point 82 ° C.) and tetraethylene glycol dimethyl ether (boiling point 273 ° C.) was 0.5. Moreover, the siloxane resin solid content concentration at this time was 43%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.5 is added until the solid content concentration of the siloxane resin reaches 20%.
  • Silica-based film forming composition a-5 was produced.
  • Example 13 To the silicon compound A, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 26.7 g of isobutyl acetate (boiling point 118 ° C.) was added. At this time, the mass ratio of the content of isobutyl acetate to the total content of the content of isobutyl acetate (boiling point 118 ° C.) and the content of dipropylene glycol monomethyl ether (boiling point 188 ° C.) was 0.4. At this time, the siloxane resin solid content concentration was 47%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling point solvent to the total content of the high-boiling point component and the low-boiling point component is 0.4 is added until the solid content concentration of the siloxane resin reaches 20%.
  • Silica-based film forming composition B-1 was produced.
  • Example 14 To the silicon compound A, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 40.0 g of isobutyl acetate (boiling point 118 ° C.) was added. At this time, the mass ratio of the content of isobutyl acetate to the total content of the content of isobutyl acetate (boiling point 118 ° C.) and the content of dipropylene glycol monomethyl ether (boiling point 188 ° C.) was 0.5. Moreover, the siloxane resin solid content concentration at this time was 43%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.5 is added until the solid content concentration of the siloxane resin reaches 20%.
  • Silica-based film forming composition B-2 was prepared.
  • Example 15 To the silicon compound A, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 60.0 g of isobutyl acetate (boiling point 118 ° C.) was added. At this point, the mass ratio of the content of isobutyl acetate to the total content of isobutyl acetate (boiling point 118 ° C.) and dipropylene glycol monomethyl ether (boiling point 188 ° C.) was 0.6. At this time, the siloxane resin solid content concentration was 38%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.6 is added until the solid content concentration of the siloxane resin reaches 20%.
  • Silica-based film forming composition B-3 was prepared.
  • Example 16 To the silicon compound A, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 26.7 g of butyl acetate (boiling point 126 ° C.) was added. At this time, the mass ratio of the content of butyl acetate to the total content of butyl acetate (boiling point 126 ° C.) and dipropylene glycol monomethyl ether (boiling point 188 ° C.) was 0.4. At this time, the siloxane resin solid content concentration was 47%.
  • siloxane resin solid content concentration reaches 20%
  • a mixed solvent in which the mass ratio of the content of the low boiling point component to the total content of the high boiling point component and the low boiling point component is 0.4 is added, and the silica for inkjet A system film-forming composition B-4 was prepared.
  • Example 17 To the silicon compound B, 0.3 g of Dispalon 1711 (Tsubakimoto Kasei), a silicone-based surface conditioner, was added and stirred, and 26.7 g of isobutyl acetate (boiling point 118 ° C.) was added. At this point, the mass ratio of the isobutyl acetate content to the total content of isobutyl acetate (boiling point 118 ° C.) and dimethyltriglycol (boiling point 216 ° C.) was 0.4. At this time, the siloxane resin solid content concentration was 47%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.4 is added until the solid content concentration of the siloxane resin reaches 20%.
  • Silica-based film forming composition B-5 was produced.
  • Example 18 To the silicon compound B, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 60.0 g of isobutyl acetate (boiling point 118 ° C.) was added. At this time, the mass ratio of the content of isobutyl acetate to the total content of isobutyl acetate (boiling point 118 ° C.) and dimethyltriglycol (boiling point 216 ° C.) was 0.6. At this time, the siloxane resin solid content concentration was 38%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.6 is added until the solid content concentration of the siloxane resin reaches 20%.
  • Silica-based film forming composition B-6 was produced.
  • Example 19 To the silicon compound B, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 26.7 g of butyl acetate (boiling point 126 ° C.) was added. At this time, the mass ratio of the content of butyl acetate to the total content of butyl acetate (boiling point 126 ° C.) and dimethyltriglycol (boiling point 216 ° C.) was 0.4. At this time, the siloxane resin solid content concentration was 47%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.4 is added until the solid content concentration of the siloxane resin reaches 20%.
  • Silica-based film forming composition B-7 was produced.
  • Example 20 To the silicon compound A, 0.3 g of Dispalon 1711 which is a silicone surface conditioner was added and stirred, and 17.2 g of isobutyl acetate (boiling point 118 ° C.) was added. At this time, the mass ratio of the content of isobutyl acetate to the total content of isobutyl acetate (boiling point 118 ° C.) and dipropylene glycol monomethyl ether (boiling point 188 ° C.) was 0.3. Moreover, the siloxane resin solid content concentration at this time was 51%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.3 is added until the solid content concentration of the siloxane resin is 20%.
  • a silica-based film-forming composition b-1 was produced.
  • Example 21 To the silicon compound A, 0.3 g of Dispalon 1711 which is a silicone surface conditioner was added and stirred, and 93.5 g of isobutyl acetate (boiling point 118 ° C.) was added. At this time, the mass ratio of the content of isobutyl acetate to the total content of the content of isobutyl acetate (boiling point 118 ° C.) and the content of dipropylene glycol monomethyl ether (boiling point 188 ° C.) was 0.7. Moreover, the siloxane resin solid content concentration at this time was 31%.
  • this mixed solvent in which the mass ratio of the content of the low boiling point component to the total content of the high boiling point component and the low boiling point component is 0.7 is added until the solid content concentration of the siloxane resin reaches 20%.
  • a silica-based film forming composition b-2 was produced.
  • Example 22 40.0 g of isobutyl acetate (boiling point 118 ° C.) was added to the silicon compound A. At this time, the mass ratio of the content of isobutyl acetate to the total content of the content of isobutyl acetate (boiling point 118 ° C.) and the content of dipropylene glycol monomethyl ether (boiling point 188 ° C.) was 0.5. Moreover, the siloxane resin solid content concentration at this time was 43%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.5 is added until the solid content concentration of the siloxane resin reaches 20%.
  • a silica-based film-forming composition b-3 was produced.
  • Example 23 To the silicon compound A, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 60.0 g of 2-propanol (boiling point 82 ° C.) was added. At this time, the mass ratio of the content of 2-propanol to the total content of 2-propanol (boiling point 82 ° C.) and dipropylene glycol monomethyl ether (boiling point 188 ° C.) was 0.6. At this time, the siloxane resin solid content concentration was 38%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.6 is added until the solid content concentration of the siloxane resin reaches 20%.
  • a silica-based film-forming composition b-4 was produced.
  • Example 24 To the silicon compound A, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 26.7 g of propylene glycol monopropyl ether (boiling point 150 ° C.) was added. At this point, the mass ratio of the content of propylene glycol monopropyl ether to the total content of propylene glycol monopropyl ether (boiling point 150 ° C.) and dipropylene glycol monomethyl ether (boiling point 188 ° C.) is 0.4. Met. At this time, the siloxane resin solid content concentration was 47%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.4 is added until the solid content concentration of the siloxane resin reaches 20%.
  • a silica-based film-forming composition b-5 was produced.
  • Example 25 To the silicon compound C, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 60.0 g of isobutyl acetate (boiling point 118 ° C.) was added. At this point, the mass ratio of the isobutyl acetate content to the total content of isobutyl acetate (boiling point 118 ° C.) content and tetraethylene glycol dimethyl ether (boiling point 273 ° C.) content was 0.6. At this time, the siloxane resin solid content concentration was 38%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.6 is added until the solid content concentration of the siloxane resin reaches 20%.
  • a silica-based film-forming composition b-6 was produced.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.5 until the siloxane resin solid content concentration becomes 20% is added, and the silica for inkjet A system film-forming composition C-1 was produced.
  • Example 27 To the silicon compound A, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 60.0 g of propylene glycol monopropyl ether (boiling point 150 ° C.) was added. At this time, the mass ratio of the content of propylene glycol monopropyl ether to the total content of propylene glycol monopropyl ether (boiling point 150 ° C.) and dipropylene glycol monomethyl ether (boiling point 188 ° C.) is 0.6. Met. At this time, the siloxane resin solid content concentration was 38%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.6 is added until the solid content concentration of the siloxane resin reaches 20%.
  • a silica-based film-forming composition C-2 was produced.
  • Example 28 To the silicon compound A, 0.3 g of Dispalon 1711 which is a silicone surface conditioner was added and stirred, and 93.5 g of propylene glycol monopropyl ether (boiling point 150 ° C.) was added. At this point, the mass ratio of the content of propylene glycol monopropyl ether to the total content of propylene glycol monopropyl ether (boiling point 150 ° C.) and dipropylene glycol monomethyl ether (boiling point 188 ° C.) is 0.7. Met. Moreover, the siloxane resin solid content concentration at this time was 31%.
  • this mixed solvent in which the mass ratio of the content of the low boiling point component to the total content of the high boiling point component and the low boiling point component is 0.7 is added until the solid content concentration of the siloxane resin reaches 20%.
  • Silica-based film forming composition C-3 was prepared.
  • Example 29 To the silicon compound A, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 40.0 g of cyclohexanone (boiling point 156 ° C.) was added. At this time, the mass ratio of the content of cyclohexanone to the total content of cyclohexanone (boiling point 156 ° C.) and dipropylene glycol monomethyl ether (boiling point 188 ° C.) was 0.5. Moreover, the siloxane resin solid content concentration at this time was 43%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.5 is added until the solid content concentration of the siloxane resin reaches 20%.
  • Silica-based film forming composition C-4 was produced.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.5 is added until the solid content concentration of the siloxane resin reaches 20%.
  • Silica-based film forming composition C-5 was produced.
  • Example 31 To the silicon compound B, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 93.5 g of propylene glycol monopropyl ether (boiling point 150 ° C.) was added. At this time, the mass ratio of the content of propylene glycol monopropyl ether to the total content of propylene glycol monopropyl ether (boiling point 150 ° C.) and dimethyltriglycol (boiling point 216 ° C.) was 0.7. . Moreover, the siloxane resin solid content concentration at this time was 31%.
  • this mixed solvent in which the mass ratio of the content of the low boiling point component to the total content of the high boiling point component and the low boiling point component is 0.7 is added until the solid content concentration of the siloxane resin reaches 20%.
  • Silica-based film forming composition C-6 was produced.
  • Example 32 To the silicon compound B, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 40.0 g of cyclohexanone (boiling point 156 ° C.) was added. At this time, the mass ratio of the content of cyclohexanone to the total content of cyclohexanone (boiling point 156 ° C.) and dimethyltriglycol (boiling point 216 ° C.) was 0.5. Moreover, the siloxane resin solid content concentration at this time was 43%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.5 is added until the solid content concentration of the siloxane resin reaches 20%.
  • Silica-based film forming composition C-7 was produced.
  • Example 33 To the silicon compound A, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 26.7 g of propylene glycol monopropyl ether (boiling point 150 ° C.) was added. At this point, the mass ratio of the content of propylene glycol monopropyl ether to the total content of propylene glycol monopropyl ether (boiling point 150 ° C.) and dipropylene glycol monomethyl ether (boiling point 188 ° C.) is 0.4. Met. At this time, the siloxane resin solid content concentration was 47%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.4 is added until the solid content concentration of the siloxane resin reaches 20%.
  • a silica-based film forming composition c-1 was prepared.
  • Example 34 To the silicon compound A, 0.3 g of Dispalon 1711 which is a silicone-based surface conditioner was added and stirred, and 160.0 g of propylene glycol monopropyl ether (boiling point 150 ° C.) was added. At this time, the mass ratio of the content of propylene glycol monopropyl ether to the total content of propylene glycol monopropyl ether (boiling point 150 ° C.) and dipropylene glycol monomethyl ether (boiling point 188 ° C.) is 0.8. Met. Moreover, the siloxane resin solid content concentration at this time was 23%.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.8 is added until the solid content of the siloxane resin reaches 20%.
  • a silica-based film forming composition c-2 was prepared.
  • this mixed solvent in which the mass ratio of the content of the low-boiling component to the total content of the high-boiling component and the low-boiling component is 0.4 is added until the solid content concentration of the siloxane resin reaches 20%.
  • a silica-based film forming composition c-3 was produced.
  • Example 36 To the silicon compound A, 0.3 g of Dispalon 1711 which is a silicone surface conditioner was added and stirred, and 93.5 g of 2-propanol (boiling point 82 ° C.) was added. At this point, the mass ratio of the 2-propanol content to the total content of 2-propanol (boiling point 82 ° C.) and dipropylene glycol monomethyl ether (boiling point 188 ° C.) was 0.7. Moreover, the siloxane resin solid content concentration at this time was 31%.
  • this mixed solvent in which the mass ratio of the content of the low boiling point component to the total content of the high boiling point component and the low boiling point component is 0.7 is added until the solid content concentration of the siloxane resin reaches 20%.
  • a silica-based film forming composition c-4 was prepared.
  • Example 37 To the silicon compound A, 0.3 g of Dispalon 1711 which is a silicone surface conditioner was added and stirred, and 93.5 g of isobutyl acetate (boiling point 118 ° C.) was added. At this time, the mass ratio of the content of isobutyl acetate to the total content of the content of isobutyl acetate (boiling point 118 ° C.) and the content of dipropylene glycol monomethyl ether (boiling point 188 ° C.) was 0.7. Moreover, the siloxane resin solid content concentration at this time was 31%.
  • this mixed solvent in which the mass ratio of the content of the low boiling point component to the total content of the high boiling point component and the low boiling point component is 0.7 is added until the solid content concentration of the siloxane resin reaches 20%.
  • a silica-based film-forming composition c-5 was produced.
  • this mixed solvent in which the mass ratio of the content of the low boiling point component to the total content of the high boiling point component and the low boiling point component is 0.7 is added until the solid content concentration of the siloxane resin reaches 20%.
  • a silica-based film forming composition c-6 was prepared.
  • ⁇ Clogging evaluation B Ink (silica-based film formation for each inkjet) in the order of discharge (3 minutes), non-discharge (10 minutes), discharge (30 seconds), non-discharge (10 minutes), discharge (30 seconds) at room temperature (23 ° C.) It was determined whether or not the ink was discharged without clogging the nozzles when the discharge and non-discharge of the composition were repeated.
  • the bleeding of the drawing pattern was evaluated as follows. First, using a NanoPrinter-1100 Standard inkjet ejector, ink (each silica-based film-forming composition for inkjet) was ejected, and a predetermined pattern was drawn on a mirror-Si wafer heated to 70 ° C. At this time, the drawing conditions of the apparatus were set to “width 800 ⁇ m, length 20000 ⁇ m, film thickness 1.2 ⁇ m”.
  • Tables 1 to 6 show the compositions of the ink-jet silica-based film forming compositions of Experimental Examples 1 to 38 and the evaluation results.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)
  • Paints Or Removers (AREA)
  • Formation Of Insulating Films (AREA)

Abstract

La présente invention concerne une composition pour former un film de revêtement contenant de la silice pour des applications de jet d'encre, qui comprend un composé de silicium produit par l'hydrolyse/condensation d'un composé représenté par la formule générale (I), un solvant et un agent de contrôle de surface, le solvant comprenant un premier solvant ayant un point d'ébullition de 80 à 160 °C et un deuxième solvant ayant un point d'ébullition de 180 à 230 °C et le rapport de la teneur du premier solvant à la teneur totale des premier et deuxième solvants est de 0,3 à 0,7 en masse. Dans la formule, R1 représente un groupe organique ayant de 1 à 20 atomes de carbone ; X représente un groupe hydrolysable ; et n représente un entier de 0 à 2. R1 nSiX4-n … (I)
PCT/JP2011/069198 2011-02-07 2011-08-25 Composition pour former un film de revêtement contenant de la silice pour des applications de jet d'encre, procédé pour former un film de revêtement contenant de la silice, dispositif à semi-conducteur, et système de cellule solaire WO2012108072A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2012556748A JPWO2012108072A1 (ja) 2011-02-07 2011-08-25 インクジェット用シリカ系被膜形成組成物、シリカ系被膜の形成方法、半導体デバイス及び太陽電池システム

Applications Claiming Priority (6)

Application Number Priority Date Filing Date Title
JP2011024319 2011-02-07
JP2011-024319 2011-02-07
JP2011-024323 2011-02-07
JP2011024328 2011-02-07
JP2011024323 2011-02-07
JP2011-024328 2011-02-07

Publications (1)

Publication Number Publication Date
WO2012108072A1 true WO2012108072A1 (fr) 2012-08-16

Family

ID=46638306

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2011/069198 WO2012108072A1 (fr) 2011-02-07 2011-08-25 Composition pour former un film de revêtement contenant de la silice pour des applications de jet d'encre, procédé pour former un film de revêtement contenant de la silice, dispositif à semi-conducteur, et système de cellule solaire

Country Status (3)

Country Link
JP (1) JPWO2012108072A1 (fr)
TW (1) TW201233737A (fr)
WO (1) WO2012108072A1 (fr)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09329707A (ja) * 1996-06-12 1997-12-22 Toray Ind Inc カラーフィルターの製造方法およびカラーフィルター
JPH1048619A (ja) * 1996-08-06 1998-02-20 Toray Ind Inc 液晶表示装置の製造方法および液晶表示装置
JP2002361906A (ja) * 2001-06-13 2002-12-18 Matsushita Electric Ind Co Ltd インクジェット式記録装置
JP2003246948A (ja) * 2002-02-26 2003-09-05 Matsushita Electric Ind Co Ltd インクジェット記録用インク、インクカートリッジ及び記録装置
WO2009125787A1 (fr) * 2008-04-09 2009-10-15 東京応化工業株式会社 Composition d’agent diffusant pour jet d’encre, et procédé de fabrication d’une électrode ou d’une batterie solaire utilisant la composition
JP2011000766A (ja) * 2009-06-17 2011-01-06 Tokyo Ohka Kogyo Co Ltd ナノインプリント用組成物およびパターン形成方法
JP2011119341A (ja) * 2009-12-01 2011-06-16 Sharp Corp 拡散防止マスクの形成方法およびそれを用いた太陽電池の製造方法

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09329707A (ja) * 1996-06-12 1997-12-22 Toray Ind Inc カラーフィルターの製造方法およびカラーフィルター
JPH1048619A (ja) * 1996-08-06 1998-02-20 Toray Ind Inc 液晶表示装置の製造方法および液晶表示装置
JP2002361906A (ja) * 2001-06-13 2002-12-18 Matsushita Electric Ind Co Ltd インクジェット式記録装置
JP2003246948A (ja) * 2002-02-26 2003-09-05 Matsushita Electric Ind Co Ltd インクジェット記録用インク、インクカートリッジ及び記録装置
WO2009125787A1 (fr) * 2008-04-09 2009-10-15 東京応化工業株式会社 Composition d’agent diffusant pour jet d’encre, et procédé de fabrication d’une électrode ou d’une batterie solaire utilisant la composition
JP2011000766A (ja) * 2009-06-17 2011-01-06 Tokyo Ohka Kogyo Co Ltd ナノインプリント用組成物およびパターン形成方法
JP2011119341A (ja) * 2009-12-01 2011-06-16 Sharp Corp 拡散防止マスクの形成方法およびそれを用いた太陽電池の製造方法

Also Published As

Publication number Publication date
TW201233737A (en) 2012-08-16
JPWO2012108072A1 (ja) 2014-07-03

Similar Documents

Publication Publication Date Title
KR100709644B1 (ko) 실리카계 막 및 그의 형성 방법, 반도체 장치의 절연막형성용 조성물, 및 배선 구조체 및 반도체 장치
KR100912566B1 (ko) 피막, 실리카계 피막 및 그 형성방법, 실리카계 피막형성용 조성물, 및 전자부품
JP3674041B2 (ja) シリカ系被膜形成用組成物、シリカ系被膜及びその形成方法、並びにシリカ系被膜を備える電子部品
US20040188846A1 (en) Porous film, composition and manufacturing method, interlayer dielectric film, and semiconductor device
US6235101B1 (en) Composition for film formation and film
JP3966026B2 (ja) シリカ系被膜形成用組成物、シリカ系被膜及びその製造方法、並びに電子部品
WO2012144291A1 (fr) Composition de formation de film à base de silice pour jet d'encre, procédé de formation de film à base de silice, dispositif à semi-conducteurs, et système de cellules solaires
WO2012144292A1 (fr) Composition de formation de film à base de silice pour jet d'encre, procédé de formation de film à base de silice, dispositif à semi-conducteurs, et système de cellules solaires
JP2003253204A (ja) シリカ系被膜形成用組成物、シリカ系被膜の製造方法及び電子部品
JP2003171616A (ja) シリカ系被膜形成用組成物、シリカ系被膜の製造方法及び電子部品
JP2006183029A (ja) シリカ系被膜形成用組成物、シリカ系被膜の形成方法、シリカ系被膜、及び、電子部品
JP5143335B2 (ja) シリカ系被膜形成用組成物、シリカ系被膜及びその形成方法、並びにシリカ系被膜を備える電子部品
JP4110796B2 (ja) シリカ系被膜形成用組成物、シリカ系被膜の製造方法及び電子部品
JP2014132044A (ja) インクジェット用シリカ系被膜形成組成物、シリカ系被膜の形成方法、半導体デバイス及び太陽電池システム
JP5143334B2 (ja) シリカ系被膜形成用組成物、シリカ系被膜及びその形成方法、並びにシリカ系被膜を備える電子部品
JP2006183028A (ja) シリカ系被膜形成用組成物、シリカ系被膜の形成方法、シリカ系被膜、及び、電子部品
WO2012108072A1 (fr) Composition pour former un film de revêtement contenant de la silice pour des applications de jet d'encre, procédé pour former un film de revêtement contenant de la silice, dispositif à semi-conducteur, et système de cellule solaire
JP2005136429A (ja) シリカ系被膜形成用組成物、シリカ系被膜及びその形成方法、並びにシリカ系被膜を備える電子部品
JP2005105281A (ja) シリカ系被膜形成用組成物、シリカ系被膜及びその形成方法、並びにシリカ系被膜を備える電子部品
JP2005042118A (ja) シリカ系被膜形成用組成物、シリカ系被膜の製造方法及び電子部品
JP2005105283A (ja) シリカ系被膜形成用組成物、シリカ系被膜及びその形成方法、並びにシリカ系被膜を備える電子部品
JP2005105282A (ja) シリカ系被膜形成用組成物、シリカ系被膜及びその形成方法、並びにシリカ系被膜を備える電子部品
JP2007291167A (ja) シリカ系被膜形成用組成物、シリカ系被膜の製造方法及び電子部品
JP2011006539A (ja) 塗布型シリカ系被膜形成用組成物、この塗布型シリカ系被膜形成用組成物を用いたシリカ系被膜、及びそれを用いた半導体装置
JP2006055700A (ja) シリカ系硬化被膜の形成方法、シリカ系硬化被膜改善用液体、シリカ系硬化被膜及び電子部品

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 11858148

Country of ref document: EP

Kind code of ref document: A1

ENP Entry into the national phase

Ref document number: 2012556748

Country of ref document: JP

Kind code of ref document: A

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 11858148

Country of ref document: EP

Kind code of ref document: A1