Planarization film manufacturing method, planarization film material, and planarization film

Abstract

Provided are a method for manufacturing a planarizing film, with which it is possible to form a planarizing film having exceptional production properties and exceptional flatness on an uneven surface of a base material having low heat resistance; a planarizing film material; and a planarizing film.　This method for manufacturing a planarizing film 2 includes forming, from a planarizing film material through a PECVD method, a planarizing film 2 on a base material 1 having an uneven surface 11, the planarizing film 2 planarizing the uneven surface 11. This planarizing film material contains an organic silane compound in which an unsaturated aliphatic hydrocarbon group is bonded to an Si atom, and an oxidizing agent. This planarizing film 2 is formed by sequential or simultaneous formation and solidification of an unsolidified film on the base material 1, the unsolidified film being derived from the planarizing film material, and the formation and solidification of the unsolidified film both being performed through a chemical reaction induced by plasma.

Description

[Technical Field]

[0001] The present disclosure relates to a method for manufacturing a planarization film, a material for a planarization film, and a planarization film. [Background technology]

[0002] The planarizing film is formed for the purpose of flattening the uneven surface of the substrate by filling in grooves present in the substrate or filling in the periphery of structures or particles protruding from the substrate.

[0003] In semiconductor devices such as DRAM (Dynamic Random Access Memory), an insulating film (element isolation insulating film) is provided between adjacent elements to ensure insulation between the elements. Here, the element isolation insulating film is formed by burying the insulating film in a trench (element isolation trench) provided in the semiconductor substrate.

[0004] As a method for planarizing the irregularities of a substrate, for example, Patent Document 1 discloses a flowable CVD (Flowable Chemical Vapor Deposition) method. The flowable CVD method uses organosilane or organosiloxane as a raw material to form a film of a flowable silicon compound (mainly silanol (Si(OH)4)) by CVD, and then modifies the film into a silicon oxide film by an oxidation reaction. A flowable silicon compound film can easily fill narrow spaces, offering the advantages of excellent filling properties and being less likely to produce voids. [Prior art documents] [Patent documents]

[0005] [Patent Document 1] Japanese Patent Application Laid-Open No. 2012-231007 Summary of the Invention [Problem to be solved by the invention]

[0006] However, in the fluidity CVD method described in Patent Document 1, after forming a silicon compound film on a substrate, it is necessary to carry out an oxidation annealing treatment at a high temperature to promote an oxidation reaction.

[0007] Therefore, the method of Patent Document 1 has problems in that the volumetric shrinkage of the silicon compound film causes shrinkage and voids in the resulting planarization film, thereby reducing the planarization film's flatness, and in that the volumetric shrinkage of the silicon compound film causes shrinkage stress in the resulting planarization film, thereby reducing the film strength of the planarization film. Furthermore, the method of Patent Document 1 also has problems in that the high-temperature oxidation annealing causes thermal changes in the substrate and surrounding structures, making it inapplicable to substrates and structures with low heat resistance. Furthermore, the method of Patent Document 1 requires two or more steps, such as the formation of a silicon compound film and the subsequent oxidation annealing treatment, resulting in low productivity.

[0008] Therefore, the present invention has been made in consideration of the above-mentioned problems, and aims to provide a method for producing a planarizing film, a material for a planarizing film, and a planarizing film that are highly productive and capable of forming a planarizing film with excellent flatness on the uneven surface of a substrate with low heat resistance. [Means for solving the problem]

[0009] According to one aspect of the present disclosure, A method for producing a planarization film, comprising forming a planarization film on a substrate having an uneven surface from a planarization film material by a PECVD (plasma-enhanced chemical vapor deposition) method, the method comprising: The planarization film material is an organosilane compound in which an unsaturated aliphatic hydrocarbon group is bonded to a Si atom; an oxidizing agent, The formation of the planarization film is forming an unsolidified film derived from the planarization film material on the substrate and solidifying the film sequentially or simultaneously; The method for producing a planarizing film is provided, wherein the formation and solidification of the unsolidified film are both performed by chemical reactions excited by plasma.

[0010] According to one aspect of the present disclosure, a planarization film material used for a planarization film that flattens an uneven surface of a substrate includes: Monosilane represented by formula (1), A disiloxane represented by formula (2): A cyclic siloxane represented by formula (3), and A planarization film material is provided, which contains one or more organosilane compounds selected from the group consisting of trisiloxanes represented by formula (4):

[0011] [ka]

[0012] In formula (1), R 1 represents an alkenyl group having 1 to 10 carbon atoms or an alkynyl group having 1 to 10 carbon atoms, R 2 is an alkoxy group having 1 to 10 carbon atoms, a hydroxyl group, or a hydrogen atom, R 3 is a phenyl group, a benzyl group, or a linear, branched, or cyclic alkyl group having 1 to 10 carbon atoms, a is an integer from 1 to 4, b is an integer from 0 to 3, a+b is an integer from 2 to 4.

[0013] [ka]

[0014] In formula (2), R 4 represents an alkenyl group having 1 to 10 carbon atoms or an alkynyl group having 1 to 10 carbon atoms, R 5 is an alkoxy group having 1 to 10 carbon atoms, a hydroxyl group, or a hydrogen atom, R 6 is a phenyl group, a benzyl group, or a linear, branched, or cyclic alkyl group having 1 to 10 carbon atoms, c is an integer from 1 to 3, d is an integer from 0 to 2, c+d is an integer from 1 to 3.

[0015] [ka]

[0016] In formula (3), R 7 represents an alkenyl group having 1 to 10 carbon atoms or an alkynyl group having 1 to 10 carbon atoms, R 8 is an alkoxy group having 1 to 10 carbon atoms, a hydroxyl group, or a hydrogen atom, R 9 is a phenyl group, a benzyl group, or a linear, branched, or cyclic alkyl group having 1 to 10 carbon atoms, e is 1 or 2; f is 0 or 1, e+f is 1 or 2, n is an integer of 2 to 6.

[0017] [ka] In formula (4), R 10 and R 13 are an alkenyl group having 1 to 10 carbon atoms and an alkynyl group having 1 to 10 carbon atoms, respectively; R 11 and R 14 are each an alkoxy group having 1 to 10 carbon atoms, a hydroxyl group, or a hydrogen atom, R 12 and R 15 are each a phenyl group, a benzyl group, or a linear, branched, or cyclic alkyl group having 1 to 10 carbon atoms, g is an integer from 0 to 3, i is an integer from 0 to 2, g+i is an integer from 1 to 5, h is an integer from 0 to 3; j is an integer from 0 to 2, g+h are integers from 0 to 3, i+j is an integer between 0 and 2.

[0018] According to one aspect of the present disclosure, A planarization film is provided, which is made of components derived from the planarization film material.

[0019] According to one aspect of the present disclosure, An electronic device is provided that includes the planarization film.

[0020] According to one aspect of the present disclosure, A coating film is provided that includes the planarizing film. [Effects of the Invention]

[0021] According to one aspect of the present disclosure, it is possible to provide a method for producing a planarizing film, a material for a planarizing film, and a planarizing film, which are highly productive and capable of forming a planarizing film with excellent flatness on an uneven surface of a substrate having low heat resistance. [Brief explanation of the drawings]

[0022] [Figure 1] 1 is a schematic cross-sectional view of a silicon wafer with a line and space pattern, which is a substrate having an uneven surface on which a planarizing film of one embodiment according to the present invention is formed, showing the state before the planarizing film is formed. [Figure 2] 1 is a schematic cross-sectional view of a silicon wafer with a line and space pattern, which is a substrate having an uneven surface on which a planarizing film of one embodiment according to the present invention is formed, showing the state after the planarizing film has been formed. FIG. [Figure 3] 1 is an electron microscope photograph showing a cross section of a silicon wafer having a line and space pattern on which the planarization film of Example 1 has been formed. DETAILED DESCRIPTION OF THE INVENTION

[0023] Each aspect of the present disclosure will be described in detail below.

[0024] <Method of manufacturing planarizing film> The method for producing a planarizing film of the present invention comprises forming a planarizing film that flattens a substrate having an uneven surface from a planarizing film material by a PECVD (plasma-enhanced chemical vapor deposition) method, the planarizing film comprising an organosilane compound in which an unsaturated aliphatic hydrocarbon group is bonded to a Si atom, and an oxidizing agent, and the planarizing film is formed by sequentially or simultaneously forming and solidifying an unsolidified film derived from the planarizing film material on the substrate, and both the formation and solidification of the unsolidified film are due to chemical reactions excited by plasma.

[0025] This allows the planarization film material, an organosilane compound in which an unsaturated aliphatic hydrocarbon group is bonded to a silicon atom, and an oxidizer, contained in the planarization film material, to undergo various chemical reactions, such as polymerization reactions at the carbon-carbon double or triple bonds contained in the unsaturated aliphatic hydrocarbon group and polycondensation reactions of the organosilane compound with the plasma-activated oxidizer. This allows an unsolidified film derived from the planarization film material to be formed on the uneven surface of the substrate. The unsolidified film thus formed conforms to the unevenness on the substrate surface, and more preferably is formed to be able to flow over the uneven surface, thereby having the effect of planarizing the unevenness on the substrate surface. Furthermore, since solidification of the unsolidified film proceeds following or simultaneously with the formation of the unsolidified film, the planarization film can be formed without the need for a separate process such as high-temperature oxidation annealing. Therefore, a planarization film manufacturing method, a planarization film material, and a planarization film can be provided that are highly productive and capable of forming a planarization film with excellent flatness on the uneven surface of a substrate with low heat resistance.

[0026] <<Organosilane compounds>> The planarization film material used in the preparation of the planarization film of the present invention contains an organosilane compound in which an unsaturated aliphatic hydrocarbon group is bonded to a Si atom. The organosilane compound may have two or more reactive groups bonded to the Si atom, including the unsaturated aliphatic hydrocarbon group. Examples of the reactive group include unsaturated aliphatic hydrocarbon groups such as alkenyl and alkynyl groups, as well as one or more groups selected from the group consisting of alkoxy groups, hydroxyl groups, and hydrogen atoms. Among these organosilane compounds, the following are particularly preferred: Monosilane represented by formula (1), A disiloxane represented by formula (2): A cyclic siloxane represented by formula (3), and Trisiloxane represented by formula (4) It is preferable that the composition contains one or more organic silane compounds selected from the group consisting of:

[0027] [ka]

[0028] In formula (1), R 1 represents an alkenyl group having 1 to 10 carbon atoms or an alkynyl group having 1 to 10 carbon atoms, R 2 is an alkoxy group having 1 to 10 carbon atoms, a hydroxyl group, or a hydrogen atom, R 3 is a phenyl group, a benzyl group, or a linear, branched, or cyclic alkyl group having 1 to 10 carbon atoms, a is an integer from 1 to 4, b is an integer from 0 to 3, a+b is an integer from 2 to 4.

[0029] [ka]

[0030] In formula (2), R 4represents an alkenyl group having 1 to 10 carbon atoms or an alkynyl group having 1 to 10 carbon atoms, R 5 is an alkoxy group having 1 to 10 carbon atoms, a hydroxyl group, or a hydrogen atom, R 6 is a phenyl group, a benzyl group, or a linear, branched, or cyclic alkyl group having 1 to 10 carbon atoms, c is an integer from 1 to 3, d is an integer from 0 to 2, c+d is an integer from 1 to 3.

[0031] [ka] In formula (3), R 7 represents an alkenyl group having 1 to 10 carbon atoms or an alkynyl group having 1 to 10 carbon atoms, R 8 is an alkoxy group having 1 to 10 carbon atoms, a hydroxyl group, or a hydrogen atom, R 9 is a phenyl group, a benzyl group, or a linear, branched, or cyclic alkyl group having 1 to 10 carbon atoms, e is 1 or 2; f is 0 or 1, e+f is 1 or 2, n is an integer of 2 to 6.

[0032] [ka]

[0033] In formula (4), R 10 and R 13 are an alkenyl group having 1 to 10 carbon atoms and an alkynyl group having 1 to 10 carbon atoms, respectively; R 11 and R 14 are each an alkoxy group having 1 to 10 carbon atoms, a hydroxyl group, or a hydrogen atom, R 12and R 15 are each a phenyl group, a benzyl group, or a linear, branched, or cyclic alkyl group having 1 to 10 carbon atoms, g is an integer from 0 to 3, i is an integer from 0 to 2, g+i is an integer from 1 to 5, h is an integer from 0 to 3; j is an integer from 0 to 2, g+h are integers from 0 to 3, i+j is an integer between 0 and 2.

[0034] In particular, R 1 , R 4 , R 7 , R 10 and R 13 are preferably an alkenyl group having 1 to 5 carbon atoms and an alkynyl group having 1 to 5 carbon atoms, respectively.

[0035] In the formulas (1) to (4), examples of the linear, branched, or cyclic alkyl group having 1 to 10 carbon atoms include a methyl group, an ethyl group, an n-propyl group, an isopropyl group, an n-butyl group, an isobutyl group, a sec-butyl group, a t-butyl group, a 2-ethylhexyl group, a cyclopropyl group, a cyclobutyl group, and a cyclohexyl group.

[0036] In the formulas (1) to (4), examples of the alkenyl group having 1 to 10 carbon atoms include a vinyl group, an allyl group, a propenyl group, an isopropenyl group, a butenyl group, a hexenyl group, and a cyclohexenyl group.

[0037] In the formulas (1) to (4), examples of the alkynyl group having 1 to 10 carbon atoms include an ethynyl group, a 1-propynyl group, and a 2-propynyl group.

[0038] In the formulas (1) to (4), examples of the alkoxy group having 1 to 10 carbon atoms include a methoxy group, an ethoxy group, an n-propoxy group, an isopropoxy group, an n-butoxy group, an isobutoxy group, a sec-butoxy group, a t-butoxy group, an n-pentyloxy group, a sec-pentyloxy group, a t-pentyloxy group, a neopentyloxy group, an n-hexyloxy group, an n-heptyloxy group, an n-octyloxy group, and a 2-ethylhexyloxy group.

[0039] Among the compounds represented by formulas (1) to (4), compounds 1 to 7296 described below are more preferred. The abbreviations for compounds 1 to 7296 are as follows: Me: methyl group Et: ethyl group n Pr: n-propyl group i Pr: isopropyl group n Bu: n-butyl group i Bu: isobutyl group sec Bu: sec-butyl group t Bu: t-butyl group OH: hydroxy group OMe: methoxy group OEt: Ethoxy group O n Pr: n-propoxy group O i Pr: isopropoxy group O n Bu: n-butoxy group O i Bu: isobutoxy group O sec Bu: sec-butoxy group O t Bu: t-butoxy group

[0040] Thus, for example, in the case of compound 1, the monosilane represented by formula (1) (i.e., SiR 1 a R 2b R 3 (4-(a+b)) ) and R 1 is a vinyl group, a is 2, and R 2 The number of alkoxy groups, hydroxy groups, and hydrogen atoms corresponding to R is 0 (i.e., b is 0), 3 is a methyl group, and (4-(a+b)) is 2 (i.e., (a+b) is 2). In other words, compound 1 is a monosilane represented by Si(C2H3)2(CH3)2.

[0041] Among the compounds represented by formulas (1) to (4), compounds having a molecular weight of 400 or less are preferred from the viewpoint of vapor pressure.

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[0707] Particularly preferred organic silane compounds include tetravinylsilane, trivinylsilane, divinylsilane, vinylsilane, tetraallylsilane, triallylsilane, diallylsilane, allylsilane, methyltrivinylsilane, ethyltrivinylsilane, triallylmethylsilane, triallylethylsilane, dimethyldivinylsilane, diallyldimethylsilane, diethyldivinylsilane, diallyldiethylsilane, methyldivinylsilane, diallylmethylsilane, ethyldivinylsilane, diallylethylsilane, methylvinylsilane, and allylmethylsilane. Silane, ethyl vinyl silane, allyl ethyl silane, dimethyl vinyl silane, allyl dimethyl silane, diethyl vinyl silane, allyl diethyl silane, tetraethynyl silane, triethynyl silane, diethynyl silane, ethynyl silane, triethynyl methyl silane, diethynyl dimethyl silane, diethynyl methyl silane, ethynyl dimethyl silane, ethynyl methyl silane, methoxy dimethyl vinyl silane, ethoxy dimethyl vinyl silane, diethyl methoxy vinyl silane, diethoxy ethyl vinyl silane, ethynyl methoxy dimethyl silane, dimethy dimethoxymethylvinylsilane, ethyldimethoxyvinylsilane, dimethoxy-n-propylvinylsilane, isopropyldimethoxyvinylsilane, diethoxymethylvinylsilane, diethoxyethylvinylsilane, diethoxy-n-propylvinylsilane, diethoxyisopropylvinylsilane, allyldimethoxymethylsilane, allylethyldimethoxysilane, allyldimethoxy-n-propylsilane, allylisopropyldimethoxysilane, allyldiethoxymethylsilane, allyldiethoxyethylsilane, allyldiethoxy-n-propylsilane, allyldiethoxyisopropylsilane, ethynyldimethoxymethylsilane, trimethoxyvinylsilane, triethoxyvinylsilane, tri-n-propoxyvinylsilane, triisopropoxyvinylsilane, tri-n-butoxyvinylsilane, tri-s-butoxyvinylsilane, triisobutoxyvinylsilane, tri-t-butoxyvinylsilane, allyltrimethoxysilane, allyltriethoxysilane, allyltri-n-propoxysilane, allyltriisopropoxysilane, allyltri-n-butoxysilane, allyltri-s-butoxysilane,Allyltriisobutoxysilane, allyltri-t-butoxysilane, ethynyltrimethoxysilane, methoxymethyldivinylsilane, ethoxymethyldivinylsilane, ethylmethoxydivinylsilane, ethoxyethyldivinylsilane, diethynylmethoxymethylsilane, methoxytrivinylsilane, ethoxytrivinylsilane, n-propoxytrivinylsilane, isopropoxytrivinylsilane, triethynylmethoxysilane, dimethoxydivinyl Nylsilane, diethoxydivinylsilane, di-n-propoxydivinylsilane, diisopropoxydivinylsilane, di-n-butoxydivinylsilane, di-s-butoxydivinylsilane, diisobutoxydivinylsilane, di-t-butoxydivinylsilane, diallyldimethoxysilane, diallyldiethoxysilane, diallyldi-n-propoxysilane, diallyldiisopropoxysilane, diallyldi-n-butoxysilane, diallyldi-s-butoxy Dimethylsilane, Diallyldiisobutoxysilane, Diallyldi-t-butoxysilane, Diethynyldimethoxysilane, Methoxymethylvinylsilane, Ethoxymethylvinylsilane, Ethylmethoxyvinylsilane, Ethoxyethylvinylsilane, Allylmethoxymethylsilane, Allylethoxymethylsilane, Allylethylmethoxysilane, Allylethoxyethylsilane, Methoxyvinylsilane, Ethoxyvinylsilane, Allylmethoxysilane, Allylethoxyethylsilane Examples of such siloxanes include 2,4,6-trivinylcyclotrisiloxane, 2,4,6-trimethyl-2,4,6-trivinylcyclotrisiloxane, 2,4,6-triethyl-2,4,6-trivinylcyclotrisiloxane, 2,4,6-tri-n-propyl-2,4,6-trivinylcyclotrisiloxane, 2,4,6-triisopropyl-2,4,6-trivinylcyclotrisiloxane, and 1,5-divinylhexamethyltrisiloxane.

[0708] <<Oxidizing agent>> The planarizing film material used to prepare the planarizing film of the present invention must contain an oxidizing agent. The oxidizing agent may be oxygen, ozone, nitrogen oxides, carbon dioxide, carbon monoxide, hydrogen peroxide, etc. The oxidizing agent may be a mixture of two or more of these.

[0709] <<Alcohol, water>> The planarizing film material used to prepare the planarizing film of the present invention may further contain one or more members selected from the group consisting of alcohols and water.

[0710] Among these, examples of alcohols include monohydric alcohols such as methanol, ethanol, n-propyl alcohol, isopropyl alcohol, n-butyl alcohol, isobutyl alcohol, sec-butyl alcohol, t-butyl alcohol, n-pentyl alcohol, n-amyl alcohol, t-amyl alcohol, n-hexyl alcohol, 2-hexanol, 3-hexanol, 2-methyl-1-pentanol, 3-methyl-1-pentanol, 4-methyl-1-pentanol, 2-methyl-2-pentanol, n-heptyl alcohol, n-octyl alcohol, and 2-ethylhexyl alcohol, as well as polyhydric alcohols such as 1,2-ethanediol. Here, the planarization film material may be a mixture of two or more of these alcohols, or a mixture of one or more of these alcohols with water.

[0711] On the other hand, the planarization film material used in the production of the planarization film of the present invention may be one that is substantially free of alcohol and water. Here, "substantially free of" alcohol and water is not limited to one that is free of alcohol and water, but also includes one to which alcohol and water are not intentionally added. In other words, when "substantially free of" alcohol and water, the planarization film material may contain alcohol and water as impurities, and more specifically, the planarization film material may contain alcohol and water. It may be contained in a proportion of 0.1% by volume or less.

[0712] <<Base material>> The substrate (film formation substrate) on which the planarizing film is formed may have an uneven surface. By using a substrate having an uneven surface, a planarizing film that flattens the uneven surface can be formed using the above-mentioned planarizing film material.

[0713] Here, the material of the substrate is not particularly limited, and examples thereof include ceramic substrates such as metal oxides, metal nitrides, metal nitride oxides, and silicon oxides; crystalline substrates such as silicon; metallic substrates such as metals and alloys; plastic substrates; and glass substrates.

[0714] Among these, examples of plastic substrates include polyethylene terephthalate, polyethylene naphthalate, polycarbonate, polyimide, cycloolefin polymer, polyethylene, polypropylene, polystyrene, polyvinyl chloride, ABS (Acrylonitrile butadiene styrene) resin, methacrylic resin, modified polyphenylene ether, polyamide, polyacetal, polybutylene terephthalate, polyarylate, polysulfone, polyethersulfone, polyamideimide, polyetherimide, polyphenylene sulfide, polyetheretherketone, and fluororesin.

[0715] The substrate may be a substrate in which a material different from the substrate is carried on the substrate, or a substrate in which one or more layers are laminated on the surface of the substrate.

[0716] The surface of the substrate is provided with an uneven surface. The uneven surface is not particularly limited, but a typical example is a surface having a line-and-space pattern. Here, the line-and-space pattern is a pattern in which line portions (linear convex portions having a predetermined width) and space portions (linear concave portions having a predetermined width) are alternately arranged adjacent to each other. The widths of the line portions and space portions are both in the range of 2 μm to 100 μm, and multiple sets of line portions and space portions having the same width (e.g., A μm) may be arranged adjacent to each other. Furthermore, adjacent to this repeating structure of line portions and space portions having the same width (e.g., A μm), another repeating structure of line portions and space portions having the same width (e.g., B μm) may be arranged, with a flat portion of a predetermined width sandwiched between them. Furthermore, the height of the step between the line portions and space portions in the line-and-space pattern is not particularly limited, but is in the range of 1 μm to 3 μm.

[0717] When forming a planarizing film, the substrate is supplied to a chamber (film formation chamber) of a film formation apparatus using a PECVD method. Here, the method of transporting the substrate to the film formation chamber is not particularly limited, and known methods such as a batch method, a single-wafer method, and a roll-to-roll method can be used.

[0718] <<Formation of planarization film>> The planarizing film material is formed by the PECVD method. At this time, if the raw materials constituting the planarizing film material are in a state other than gas, they are all gasified before being supplied to the film formation chamber where the substrate is placed.

[0719] Here, methods for gasifying planarization film materials other than gases include, for example, a method in which the raw material is placed in a heated thermostatic chamber and gasified by reducing the pressure using a vacuum pump or the like; a method in which the raw material is placed in a heated thermostatic chamber and gasified by blowing in a carrier gas such as helium, neon, argon, krypton, xenon or nitrogen; and a method in which the planarization film material is sent, either as is or in the form of a solution obtained by dissolving the planarization film material in a solvent, to a vaporizer, heated, and gasified in the vaporizer (liquid injection method).

[0720] In particular, when the planarization film material is dissolved in a solvent and gasified, examples of the solvent that dissolves the planarization film material include ethers such as 1,2-dimethoxyethane, diglyme, triglyme, dioxane, tetrahydrofuran, and cyclopentyl methyl ether; and hydrocarbons such as hexane, cyclohexane, methylcyclohexane, ethylcyclohexane, heptane, octane, nonane, decane, benzene, toluene, ethylbenzene, and xylene.

[0721] The planarizing film material, which is in a gaseous state or has been gasified into a gaseous state, is supplied to the film forming chamber with all, some, or none of the constituent components mixed together.

[0722] The planarization film material, such as an organosilane compound, supplied to the film formation chamber is excited by plasma generated in the film formation chamber, causing various chemical reactions, such as polymerization reactions at carbon-carbon double or triple bonds contained in unsaturated aliphatic hydrocarbon groups and polycondensation reactions of the organosilane compound with a plasma-converted oxidizing agent, thereby forming an unsolidified film derived from the planarization film material on the substrate. Furthermore, the unsolidified film is solidified by the plasma to form the planarization film. Here, the formation and solidification of the unsolidified film derived from the planarization film material on the substrate can be carried out sequentially or simultaneously. More specifically, both the formation and solidification of the unsolidified film can be carried out by chemical reactions excited by plasma. Here, the plasma-excited chemical reaction may proceed solely by plasma excitation, or plasma excitation may be combined with light irradiation or heating of the substrate. In particular, from the perspective of increasing productivity, it is preferable that the formation and solidification of the unsolidified film be carried out in a single process.

[0723] The source of the plasma that excites the chemical reaction of the planarization film material is not particularly limited, and plasma generated using a radio frequency (RF) power source can be used. More specifically, capacitively coupled plasma, inductively coupled plasma, helicon wave plasma, surface wave plasma, electron cyclotron resonance plasma, etc. can be used.

[0724] Here, the power density applied to the electrodes of the PECVD apparatus to generate plasma is 0.01 W / cm 2 It is preferable that the value is equal to or greater than 0.01 W / cm 2 More than 100W / cm 2 The following range is more preferable:

[0725] Furthermore, the temperature of the substrate surface (particularly the surface on which the planarizing film is formed) when the planarizing film is formed is not particularly limited, but is preferably 300°C or lower, more preferably in the range of -100°C to 300°C, and even more preferably in the range of 0°C to 200°C. On the other hand, the surface temperature of the substrate when the planarizing film is formed is preferably equal to or lower than the heat resistance temperature of the substrate. In particular, the surface temperature of the substrate is preferably within these temperature ranges while the formation and solidification of the unsolidified film are proceeding.

[0726] The atmospheric pressure during the formation of the flattening film is not particularly limited, but is preferably in the range of 0.01 Pa or more and 101325 Pa or less, and particularly preferably in the range of 1 Pa or more and 10000 Pa or less.

[0727] Furthermore, when forming a planarizing film from a planarizing film material, the film formation conditions can be appropriately adjusted based on the surface temperature of the substrate, the atmospheric pressure, the flow rate of the organosilane compound, the presence or absence and flow rate of alcohol or water, the flow rate of the oxidizing agent, the presence or absence and flow rate of a carrier gas such as helium, and the like. Here, when forming the planarizing film, the flow rate of the organosilane compound constituting the planarizing film material supplied during film formation is X [sccm], the flow rate of one or more selected from the group consisting of alcohol and water is Y [sccm], and the flow rate of the oxidizing agent is Z [sccm]. The ratio of Y to X (Y / X ratio) is preferably 20 or less, more preferably 10 or less. The ratio of Z to X (Z / X ratio) is preferably 20 or less, more preferably 10 or less. In particular, by reducing one or both of the Y / X ratio and the Z / X ratio, the planarization rate of the planarizing film can be further increased. On the other hand, the lower limit of the Z / X ratio must be greater than 0, preferably 0.01 or greater. The lower limit of the Y / X ratio is not particularly limited and may be 0.

[0728] The thickness of the planarizing film formed by such a PECVD method is not particularly limited, but is preferably equal to or greater than the height of the steps on the uneven surface of the substrate. Here, the "thickness of the planarizing film" may refer to the thickness of the film formed on the flat portion of the substrate surface (i.e., the portion without unevenness) when the planarizing film is formed on a substrate having an uneven surface on part of the substrate surface.

[0729] The planarization film formed by the above process, which is primarily composed of silicon oxide, can be formed by using an organosilane compound in a gaseous state in a deposition chamber, in which an unsaturated aliphatic hydrocarbon group is bonded to a silicon atom, and an oxidizing agent. This allows a planarization film with high planarization performance to be formed at low temperatures and without post-treatment to harden the film.

[0730] <Materials for flattening film, flattening film> The planarizing film material of the present invention is a material for a planarizing film used for a planarizing film that flattens an uneven surface of a substrate, Monosilane represented by formula (1), A disiloxane represented by formula (2), and A cyclic siloxane represented by formula (3), and Trisiloxane represented by formula (4) one or more organosilane compounds selected from the group consisting of and an oxidizing agent. Here, the monosilane represented by formula (1), the disiloxane represented by formula (2), the cyclic siloxane represented by formula (3), and the trisiloxane represented by formula (4) are the same as those described above in <<Organosilane Compounds>>, including their definitions and preferred ranges, and therefore will not be described here.

[0731] Here, the planarizing film material preferably further contains, in addition to the above-mentioned organosilane compound, one or more species selected from the group consisting of alcohol and water.

[0732] The planarization film material of the present invention is preferably used for forming an organic electroluminescent device. The planarization film obtained has excellent planarity and high productivity, making it useful for forming an organic electroluminescent device. Furthermore, as described above, since no annealing treatment is required during the preparation of the planarization film, it is useful for use as a planarization film for an organic electroluminescent device.

[0733] The planarization film of the present invention contains at least a component derived from an organosilane compound among the above-mentioned planarization film materials. Here, the carbon concentration in the planarization film is preferably 12 atomic % or less. In particular, silicon oxide films with low carbon concentrations in the film have very high light transmittance, making them useful for optical components and displays.

[0734] Here, the planarization film is preferably an unannealed product. Since no annealing treatment is required, this contributes to the production of a planarization film that can be applied to objects with low heat resistance. With the planarization film material according to this embodiment, a planarization film with excellent flatness can be produced even on a substrate with low heat resistance, such as a plastic substrate. A planarization film that is an unannealed product has reduced volumetric shrinkage and small shrinkage stress. Furthermore, a planarization film that is an unannealed product reduces the impact of annealing on the substrate on which it is formed. Therefore, whether a planarization film is an unannealed product can be determined by observing traces of volumetric shrinkage, the impact of shrinkage stress, or the impact of annealing on the substrate.

[0735] Fig. 1 is a schematic cross-sectional view of a silicon wafer with a line and space pattern, which is a substrate having an uneven surface on which a planarizing film of one embodiment according to the present invention is formed, showing the state before the planarizing film is formed. Also, Fig. 2 is a schematic cross-sectional view of a silicon wafer with a line and space pattern, which is a substrate having an uneven surface on which a planarizing film of one embodiment according to the present invention is formed, showing the state after the planarizing film is formed.

[0736] As shown in Fig. 2, the planarizing film 2 is used to planarize the uneven surface 11 of the substrate 1, such as a silicon wafer with a line and space pattern. That is, as shown in Fig. 2, the upper surface of the planarizing film 2 is planarized after the planarizing film 2 is formed.

[0737] <Electronic devices, coating films (planarization film applications)> A planarizing film is formed for the purpose of filling grooves present in a substrate, filling around structures or particles protruding from the substrate, etc., to flatten the surface, etc. Therefore, the use of the planarizing film is not particularly limited, and it can be used, for example, in coating films, various electronic devices, etc.

[0738] That is, the electronic device of the present invention includes the above-mentioned planarization film. Here, the electronic device may include an organic electroluminescent element. Also, the coating film of the present invention includes the above-mentioned planarization film.

[0739] The coating film includes a planarizing film on the surface of a resin substrate, such as polyethylene terephthalate, cyclic olefin copolymer, polyacrylate, polycarbonate, polyethylene, polymethyl methacrylate, polyether ether ketone, polyethylene naphthalate, polyetherimide, polyimide, and triacetyl cellulose.

[0740] Examples of electronic devices include multilayer printed wiring boards; various displays such as thin film transistor (TFT) liquid crystal display elements and organic electroluminescent elements; photoelectric conversion elements such as solar cells and image sensors; various sensors such as optical sensors, temperature sensors, touch sensors, and pressure sensors; IC (integrated circuit) cards; and RFID (radio frequency identifiers).

[0741] The planarization film of the present invention does not require annealing treatment during its production, and therefore can be applied to planarization of substrates and structures with low heat resistance, such as plastic substrates and organic electroluminescent devices. Furthermore, the planarization film of the present invention has excellent light transmittance, and therefore can be suitably used in optical elements such as OLEDs and OLED displays. [Example]

[0742] The present invention will be described in more detail below with reference to examples, but the present invention is not limited to these examples.

[0743] A planarizing film was formed on the substrate using a general CVD apparatus that performs film formation by the capacitively coupled PECVD method. Here, a silicon wafer with a diameter of 200 mm and a thickness of 725 μm and having a line and space pattern was used as the substrate for film formation, which is the base material. After forming a planarizing film on this silicon wafer, the planarizing performance was evaluated by observing the cross-sectional image of the area where the line and space pattern was formed.

[0744] The film formation temperature during the deposition of the flattening film was measured by attaching a vacuum thermopit 9MC (manufactured by AS ONE Corporation) to the surface of the substrate where the film was to be deposited. This temperature reading indicates the maximum temperature reached during film deposition.

[0745] The planarization performance of the planarization film was evaluated using the planarization rate expressed by the following formula. Planarization rate (%) = {1 - (step height between line and space portions after planarization film formation / step height between line and space portions before planarization film formation)} x 100 The step height between the line portion and the space portion before and after the formation of the planarizing film was roughly calculated by taking a cross-sectional image of the film using a JEOL field emission scanning electron microscope (FE-SEM) JSM-7600F. The flattening rate is the average value of measurements at two locations.

[0746] The thickness of the planarizing film was roughly calculated by taking a cross-sectional image of the film using a field emission scanning electron microscope (FE-SEM) (manufactured by JEOL Ltd., model number: JSM-7600F).

[0747] The film composition of the planarization film was analyzed using an X-ray photoelectron spectrometer (XPS) (ULVAC-PHI, Model: PHI5000 VersaProbeII).

[0748] The elastic modulus and hardness of the planarization film were calculated from the load-displacement curve obtained using a nanoindentation method employing a continuous stiffness measurement method, which is a method that can obtain data in the depth direction to reduce the influence of the substrate, using an ultra-microhardness tester (KLA-Tencor, model number: Nano Indenter G200X Inforce 50). Here, a triangular pyramidal indenter made of diamond was used as the indenter attached to the ultra-microhardness tester.

[0749] [Example 1] Formation of a planarizing film using isopropyldimethoxyvinylsilane and oxygen Isopropyldimethoxyvinylsilane (an organic silane compound) was synthesized using the method described in Japanese Patent No. 4438385. The resulting isopropyldimethoxyvinylsilane and oxygen (oxidant) were then supplied to a deposition chamber, and a planarizing film was formed on a silicon wafer substrate with a line-and-space pattern by PECVD under the following deposition conditions. During deposition, cooling water was circulated inside the substrate stage in the deposition chamber to cool the substrate stage. The deposition temperature of the planarizing film (the surface temperature of the substrate during deposition) was above room temperature (approximately 20°C) and below 40°C. The silicon wafer substrate had a line-and-space pattern formed as an uneven surface 11, as shown in FIG. 1. The uneven surface 11 of the substrate 1 had line portions 11a each with a width of 2 μm, space portions 11b each with a width of 1 μm, and a step height of 2 μm between the line portions 11a and space portions 11b.

[0750] <Film formation conditions> Isopropyldimethoxyvinylsilane supply flow rate: 14 sccm Oxygen supply flow rate: 20sccm Helium supply flow rate: 50sccm Pressure in deposition chamber: 133.3 Pa PECVD equipment power supply type: RF power supply Power frequency: 13.56MHz Power output: 80 W (power density applied to electrode: 0.25 W / cm 2 ) Type of plasma source in PECVD equipment: Capacitively coupled plasma Film formation time: 5 minutes

[0751] The thickness of the planarization film obtained was 4 μm. The planarization rate of the planarization film was 100%. The composition of the planarization film obtained was 33 atomic % silicon (Si), 56 atomic % oxygen (O), and 11 atomic % carbon (C). The elastic modulus of the planarization film obtained was 6 GPa, and the hardness was 0.7 GPa. The resulting silicon wafer with a line and space pattern on which the planarization film was formed was observed using an electron microscope. Figure 3 is an electron microscope photograph showing a cross section of the silicon wafer with a line and space pattern on which the planarization film of Example 1 was formed. As shown in Figure 3, it can be seen that the uneven surface 11 of the silicon wafer, which is the substrate 1, is planarized by the planarization film 2.

[0752] [Comparative Example 1] Formation of a planarizing film using t-butyltriethoxysilane and oxygen t-Butyltriethoxysilane (an organic silane compound) was synthesized based on the method described in K. Lin, RJ Wiles, CB Kelly, GHMDavies, and GA Molander, ACS Catalysis, 2017, Vol. 7, pp. 5129-5133. The resulting t-butyltriethoxysilane and oxygen (oxidant) were then supplied to a deposition chamber, and a planarizing film was deposited on the same line-and-space patterned silicon wafer as in Example 1 by PECVD under the deposition conditions shown below. The type of plasma source, power supply frequency, power output, and cooling of the substrate table of the PECVD apparatus were the same as in Example 1. The deposition temperature (surface temperature of the substrate during deposition) was above room temperature and below 40°C.

[0753] <Film formation conditions> t-Butyltriethoxysilane supply flow rate: 16 sccm Oxygen supply flow rate: 20sccm Helium supply flow rate: 20sccm Pressure in deposition chamber: 133.3 Pa Film formation time: 5 minutes

[0754] The thickness of the planarizing film obtained was 1 μm, and the planarization rate of the planarizing film was 0%. [Explanation of symbols]

[0755] 1 Base material 11 Uneven surface 11a Line section 11b Space section 2 Planarization film

Claims

1. A method for producing a planarization film, comprising forming a planarization film on a substrate having an uneven surface from a planarization film material by a PECVD (plasma-enhanced chemical vapor deposition) method, the method comprising: The planarization film material is an organosilane compound in which an unsaturated aliphatic hydrocarbon group is bonded to a Si atom; an oxidizing agent; Including, The formation of the planarization film is forming an unsolidified film derived from the planarization film material on the substrate and solidifying the film sequentially or simultaneously; The method for producing a planarizing film, wherein the formation and solidification of the unsolidified film are both by chemical reactions excited by plasma.

2. The method for producing a planarization film according to claim 1 , wherein the organosilane compound has two or more reactive groups bonded to a Si atom.

3. The method for producing a planarization film according to claim 1 or 2, wherein the planarization film material further contains alcohol or water.

4. The method for producing a planarization film according to claim 1 or 2, wherein the planarization film material is substantially free of alcohol and water.

5. The method for producing a planarization film according to claim 1 or 2, wherein the formation and solidification of the unsolidified film are carried out in a single process.

6. The method for producing a planarizing film according to claim 1 or 2, wherein the surface temperature of the substrate when the planarizing film is formed is 300° C. or less.

7. 3. The method for producing a planarization film according to claim 1, wherein the atmospheric pressure during the formation of the planarization film is in the range of 0.01 Pa or more and 101325 Pa or less.

8. 3. The method for manufacturing a planarization film according to claim 1 or 2, wherein, in forming the planarization film, a ratio of Y to X (Y / X ratio) is 20 or less and a ratio of Z to X (Z / X ratio) is 20 or less, where X [sccm] is a flow rate of the organosilane compound, Y [sccm] is a flow rate of one or more selected from the group consisting of alcohol and water, and Z [sccm] is a flow rate of the oxidizing agent, which are the planarization film materials.

9. A planarization film material used in the method for producing a planarization film according to claim 1, The planarization film material is Monosilane represented by formula (1), A disiloxane represented by formula (2): A cyclic siloxane represented by formula (3), and Trisiloxane represented by formula (4) one or more organosilane compounds selected from the group consisting of an oxidizing agent; A planarization film material comprising: 【Chemical 1】 In formula (1), R １ represents an alkenyl group having 1 to 10 carbon atoms or an alkynyl group having 1 to 10 carbon atoms, R ２ is an alkoxy group having 1 to 10 carbon atoms, a hydroxyl group, or a hydrogen atom, R ３ is a phenyl group, a benzyl group, or a linear, branched, or cyclic alkyl group having 1 to 10 carbon atoms, a is an integer from 1 to 4, b is an integer from 0 to 3; a+b is an integer of 2 to 4. 【Chemistry 2】 In formula (2), R ４ represents an alkenyl group having 1 to 10 carbon atoms or an alkynyl group having 1 to 10 carbon atoms, R ５ is an alkoxy group having 1 to 10 carbon atoms, a hydroxyl group, or a hydrogen atom, R ６ is a phenyl group, a benzyl group, or a linear, branched, or cyclic alkyl group having 1 to 10 carbon atoms, c is an integer from 1 to 3; d is an integer from 0 to 2, c+d is an integer of 1 to 3. 【Chemistry 3】 In formula (3), R ７ represents an alkenyl group having 1 to 10 carbon atoms or an alkynyl group having 1 to 10 carbon atoms, R ８ is an alkoxy group having 1 to 10 carbon atoms, a hydroxyl group, or a hydrogen atom, R ９ is a phenyl group, a benzyl group, or a linear, branched, or cyclic alkyl group having 1 to 10 carbon atoms, e is 1 or 2; f is 0 or 1; e+f is 1 or 2, n is an integer from 2 to 6. 【Chemistry 4】 In formula (4), R １０ and R １３ are an alkenyl group having 1 to 10 carbon atoms and an alkynyl group having 1 to 10 carbon atoms, respectively; R １１ and R １４ are each an alkoxy group having 1 to 10 carbon atoms, a hydroxyl group, or a hydrogen atom, R １２ and R １５ are each a phenyl group, a benzyl group, or a linear, branched, or cyclic alkyl group having 1 to 10 carbon atoms, g is an integer from 0 to 3; i is an integer from 0 to 2, g+i is an integer from 1 to 5, h is an integer from 0 to 3; j is an integer from 0 to 2, g+h are integers from 0 to 3, i+j is an integer from 0 to 2.

10. The planarization film material according to claim 9 , which is used in forming an organic electroluminescent device.

11. The planarization film material according to claim 9 , further comprising alcohol or water.

12. The planarization film material according to claim 9 , which is substantially free of alcohol or water.

13. A planarization film comprising at least a component derived from the organosilane compound of the planarization film material according to claim 9 .

14. The planarization film of claim 13 which is an annealed green film.

15. 14. The planarization film according to claim 13, wherein the carbon concentration in the planarization film is 12 atomic % or less.

16. An electronic device comprising the planarization film according to claim 13 .

17. 17. The electronic device of claim 16, further comprising an organic electroluminescent element.

18. A coating film comprising the planarizing film according to claim 13.

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