TW200830052A - Composition for formation of film, method for production of patterned film, and insulation film for electronic device - Google Patents

Composition for formation of film, method for production of patterned film, and insulation film for electronic device Download PDF

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Publication number
TW200830052A
TW200830052A TW096138351A TW96138351A TW200830052A TW 200830052 A TW200830052 A TW 200830052A TW 096138351 A TW096138351 A TW 096138351A TW 96138351 A TW96138351 A TW 96138351A TW 200830052 A TW200830052 A TW 200830052A
Authority
TW
Taiwan
Prior art keywords
film
component
photosensitive composition
composition
condensate
Prior art date
Application number
TW096138351A
Other languages
Chinese (zh)
Inventor
Taku Sasaki
Kenichi Azuma
Shigeru Nakamura
Yasunari Kusaka
Original Assignee
Sekisui Chemical Co Ltd
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Publication date
Application filed by Sekisui Chemical Co Ltd filed Critical Sekisui Chemical Co Ltd
Publication of TW200830052A publication Critical patent/TW200830052A/en

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04—Polysiloxanes
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/004—Photosensitive materials
    • G03F7/075—Silicon-containing compounds
    • G03F7/0757—Macromolecular compounds containing Si-O, Si-C or Si-N bonds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
    • H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
    • H01L21/02123—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon
    • H01L21/02126—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon the material containing Si, O, and at least one of H, N, C, F, or other non-metal elements, e.g. SiOC, SiOC:H or SiONC
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
    • H01L21/02205—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition
    • H01L21/02208—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si
    • H01L21/02214—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si the compound comprising silicon and oxygen
    • H01L21/02216—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si the compound comprising silicon and oxygen the compound being a molecule comprising at least one silicon-oxygen bond and the compound having hydrogen or an organic group attached to the silicon or oxygen, e.g. a siloxane
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof  ; Multistep manufacturing processes therefor
    • H01L29/40—Electrodes ; Multistep manufacturing processes therefor
    • H01L29/43—Electrodes ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
    • H01L29/49—Metal-insulator-semiconductor electrodes, e.g. gates of MOSFET
    • H01L29/4908—Metal-insulator-semiconductor electrodes, e.g. gates of MOSFET for thin film semiconductor, e.g. gate of TFT
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof  ; Multistep manufacturing processes therefor
    • H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
    • H01L29/68—Types of semiconductor device ; Multistep manufacturing processes therefor controllable by only the electric current supplied, or only the electric potential applied, to an electrode which does not carry the current to be rectified, amplified or switched
    • H01L29/76—Unipolar devices, e.g. field effect transistors
    • H01L29/772—Field effect transistors
    • H01L29/78—Field effect transistors with field effect produced by an insulated gate
    • H01L29/786—Thin film transistors, i.e. transistors with a channel being at least partly a thin film
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/70—Siloxanes defined by use of the MDTQ nomenclature

Abstract

Disclosed are: a composition for forming a film, which has excellent storage stability and image-developing property and can produce a patterned film having excellent insulation performance; a method for producing a patterned film by using the composition; and an insulation film for an electronic device. Specifically disclosed are: a composition for forming a film, which comprises (A) an alkoxysilane condensation product produced by reacting a component (X) comprising phenyl ethoxysilane and/or phenyl trimethoxysilane, a component (Y) comprising methyl triethoxysilane and/or methyl trimethoxysilane and a component (Z) comprising triethoxysilane and/or trimethoxysilane at any ratio falling within an area enclosed with a solid line P1 connecting coordinate points A17, A28, A29 and A18 in the three-component phase diagram shown in Fig. 1, and (B) an acid generator which can generate an acid upon being exposed to an external stimulation such as light or heat; a method for producing a patterned film by using the composition; and an insulation film for an electronic device.

Description

200830052 九、發明說明： 【發明所屬之技術領域】 本發明係關於一種包含烷氧矽烷之縮合物、以及藉由熱 或光等之刺激而產生酸之酸產生劑的膜形成用組成物，更 詳細而言，係關於一種可獲得儲存穩定性優良且絕緣性能 " 優良的膜的膜形成用組成物、使用其之圖案膜之製造方法 、 及電子機器用絕緣膜。 【先前技術】 (； 、 於製造半導體等之電子元件時，藉由微細圖案形成法， 構成保護膜或閘極絕緣膜等。構成該等膜時，係使用例如 包含燒氧矽烷之縮合物等之感光性樹脂組成物。 下述專利文獻1中，作為圖案形成中所使用之感光性樹 脂組成物之一例，揭示有以（1)鹼溶性矽氧烷聚合物亦即烷 氧夕燒之縮合物、（2)藉由光產生催速劑之化合物以及（3) ;谷知]為主成为之感光性樹脂組成物。專利文獻1中，作為 ( (1)烷氧矽烷之縮合物，使用鹼溶性矽氧烷聚合物，該鹼溶 性矽氧烷聚合物係自於烷氧矽烷中添加水及觸媒進行加水 分解縮合後所得之反應溶液中去除水及觸媒而獲得。 • 專利文獻1中，作為（1)烷氧矽烷之縮合物之原料，較好 / 的是使用由〜莫耳％之甲基三甲氧矽烷、〇〜40莫耳％ 之苯基二甲氧矽烷、以及〇〜4〇莫耳％之二甲基二甲氧矽烷 構成之組成物。 專利文獻··曰本專利特開平〇6_148895號公報 【發明内容】 125692.doc 200830052 然而’專利文獻1之感光性樹脂組成物，有時由於構成 院氧石夕烧之縮合物之烷氧矽烷的種類及調配量，而使長期 保管時劣化且膠化。亦即，專利文獻丨之感光性樹脂組成 物之儲存穩定性不足。 又’亦要求於使感光性樹脂組成物曝光且硬化而形成硬 化物膜時所獲得之硬化物膜之絕緣性能優良。然而，先前 之感光性樹脂組成物之儲存穩定性或者硬化後之硬化物膜 之絕緣性能中的任一種性能均不足。 本發明係黎於上述先前技術之現狀而開發，且其目的在 於提供一種可獲得儲存穩定性優良且絕緣性能優良之膜的 膜形成用組成物、使用其之圖案膜之製造方法及電子機器 用絕緣膜。 根據本發明，提供一種膜形成用組成物，其特徵在於包 含烷氧矽烷之縮合物（A)以及藉由外部刺激而產生酸之酸 產生劑（B)，上述烷氧矽烷之縮合物（A)係將含苯基三乙氧 石夕燒及/或苯基三甲氧矽烷之成分（χ)、含曱基三乙氧石夕烧 及/或甲基三甲氧矽烷之成分（γ)與含三乙氧矽烷及/或三甲 氧石夕烧之成分（Ζ)，以圖1之三成分圖中連接座標α17、 Α28、Α29及Α18之實線P1所包圍區域内的比率反應而成。 本發明之膜形成用組成物之某一特定態樣中，烷氧矽烷 之縮合物（A)係將成分（x)、成分（γ)與成分（z)以圖8之三成 刀圖中連接座標A2、A28、A29及A30之實線P2所包圍區 域内的比率反應而得之烷氧矽烷之縮合物。 本發明之膜形成用組成物之其他特定態樣中，烷氧矽烷 125692.doc 200830052 ^縮合物⑷係、將成分（X)、成分⑺與成分（Z)以圖9之三成 刀圖中連接座標A31、A28、A29及A33之實線P3所包圍區 域内的比率反應而得之烷氧矽烷之縮合物。 又，根據本發明，提供一種圖案膜之製造方法，其特徵 在於：其係使用有本發明之膜形成用組成物的圖案膜之製 U方法，膜形成用組成物係包含曝光即產生酸之光酸產生 劑作為酸產生劑（B)之感光性組成物，上述圖案膜之製造 方法包含以下步驟：於基板上形成含感光性組成物之感光 性組成物層；根據所形成之圖案，使感光性組成物層選擇 性地曝光，藉由自光酸產生劑所產生之酸之作用，使曝光 部之感光性組成物層硬化，使曝光部之感光性組成物層不 溶於顯影液；以及於曝光部之感光性組成物層不溶於顯影 液後，利用顯影液使感光性組成物層顯影，去除未曝光部 之感光性組成物層。 本發明之電子機器用絕緣膜，係使用本發明之膜形成用 組成物所形成。 (發明之效果） 本發明之膜形成用組成物包含燒氧石夕烧之縮合物（A)， 且忒燒氧石夕烧之縮合物（A)係將成分（X)〜(z)以圖1之三成分 圖中連接座標A17、A28、A29及A18之實線P1所包圍區域 内的比率反應而得，故而，上述膜形成用組成物之儲存穩 定性優良。進而，本發明中，膜形成用組成物更含有藉由 光或熱等外部刺激而產生酸之酸產生劑（B)，故而，例如 可藉由對膜形成用組成物施加外部刺激而產生酸並進行硬 125692.doc 200830052 化，來獲得絕緣性能優良之膜。 本發明之圖案膜之製造方法中，於基板上形成包含作為 本舍明之膜形成用組成物之感光性組成物的感光性組成物 層，選擇性地曝光感光牲組成物層，於使曝光部之感光性 組成物層不溶於顯影液後，利用顯影液使感光性組成物層 顯影，故而，使用已長期保管之感光性組成物時，亦可形 成良好的圖案膜。進而，於顯影時，可容易地去除未曝光 部之感光性組成物層，且可獲得絕緣性能優良之圖案膜。 本發明之電子機器用絕緣膜係使用本發明之膜形成用組 成物而形成，故而，絕緣性能優良。 【實施方式】 以下，說明本發明之詳情。 本申請案發明者們發現，為了實現上述課題，可藉由如 下構成來提高膜形成用組成物之儲存穩定性，且獲得絕緣 性能優良之膜，從而開發出本發明’上述構成中含有烷氧 矽烷之縮合物（A)以及藉由外部刺激而產生酸之酸產生劑 (B) ’上述烷氧矽烷之縮合物（A)係使含特定烷氧矽烷之成 分（X)〜(Z)以圖1之三成分圖中連接座標八17、A28、am及 A18之實線Pi所包圍區域内的比率反應而得者。 本發明之膜形成用組成物，含有烷氧矽烷之縮合物（A) 以及藉由外部刺激而產生酸之酸產生劑（B)。 作為上述外部刺激，可列舉熱、可見光或紫外光等光、 超音波、微波等。當外部刺激為光日夺，本發明之膜形成用 組成物係藉由曝光而感光之感光性組成物。而當外部刺激 125692.doc 200830052 為熱時’本發明之膜形成用組成物係含有熱酸產生劑之膜 形成用組成物。以下，分為幾個部分詳述該等情形。 (作為膜形成用組成物之感光性組成物） 當本發明之膜形成用組成物係於曝光即進行感光之感光 性組成物時，使用曝光即產生酸之光酸產生劑作為上述酸 產生劑（B)。 上述烷氧矽烷之縮合物（A)係將含苯基三乙氧砍燒及/或 苯基二甲氧矽烷之成分（X)、含甲基三乙氧矽烷及/或甲基 二甲氧石夕烧之成分[Y]、與含三乙氧矽烷及/或三甲氧石夕烧 之成分（Z)，以圖1之三成分圖中連接座標ai7、A28、A29 及A1 8之實線p 1所包圍區域内的比率反應而得者。 亦即，上述烷氧矽烷之縮合物（A)係將成分（χ)、成分 (Υ)及成分（Ζ)以下述表1所示之三成分圖中連接座標Αΐ7、 Α28、Α29及Α18之直線所包圍區域内的比率反應而得者。 [表1] 成分（X) 成分（Υ) 成分（Ζ) Α17 62.5 37.5 0 Α28 1 99 0 Α29 12.5 75 12.5 Α18 37.5 50 12.5 單位為莫耳重量％ 較好的是，上述成分（X)為苯基三乙氧矽烷。較好的 是’上述成为（Υ)為甲基三乙氧矽烷。較好的是，上述成 125692.doc •10- 200830052 分（z)為三乙氧矽烷。 根據下述實驗例可知有如下趨勢：於獲得上述烷氧矽烷 之縮合物（A)時，成分（X)之調配比例越高，則感光性組成 物之儲存穩定性越高。又，亦有成分之調配比例越低 則感光性組成物之儲存穩定性越高之趨勢。尤其是，成分 (Z)之調配比例越低則感光性組成物之儲存穩定性越高之 趨勢顯著。 此原因在於’成分（X)之反應性低於成分及成分〇之 反應性，成分（Y)之反應性低於成分之反應性。成分 缺乏反應性，故而，使用較多成分（X)而獲得之烷氧矽烷 之縮合物（Α)於保存時難以進行Si〇H基的縮合反應。另一 方面，成分（Z)之反應性較高，故而，使用較多成分（z)而 獲得之烷氧矽烷之縮合物（A)於保存時易於進行SiOH基的 縮合反應。故而，為了提高感光性組成物之儲存穩定性， 較好的是，降低成分（Y)或成分（Z)之調配比例，而提高成 分（X)之調配比例。 又，成分（X)之反應性低於成分（Y)及成分（Z)之反應性， 成分（Y)之反應性低於成分（z)之反應性。故而，所使用之 成分（X)之比率越高，則經縮合而獲得之烷氧矽烷之縮合 物（A)中SiOH基的殘留量越大，故而，存在於經曝光而形 成感光性組成物之硬化物膜時絕緣性能降低之趨勢。另一 方面，當提高成分（Y)及成分（Z)之調配比例，降低成分（X) 之調配比例時，則縮合反應容易結束，可減少經縮合而獲 得之烷氧矽烷之縮合物（A)中SiOH基之存在量，故而，存 125692.doc -11 - 200830052 在感光性組成物之硬化物膜之絕緣性能提高的趨勢。 故而’為了提高感光性組成物之硬化物膜之絕緣性能， 較好的是，降低成分（X)之調配比例而提高成分（γ)及成分 (z)之调配比例。又’為了提而圖案膜之絕緣性能，較好 的是’提高成分（Y)之調配比例而降低成分（X)之調配比 例。 故而，本發明中，為了提高感光性組成物之儲存穩定性 且獲得絕緣性能優良之硬化物膜，而使用烧氧石夕烧之縮合 物（A)，且該烷氧矽烷之縮合物（A)係使成分（χ)〜(z)以三成 分圖中由連接座標A17、A28、A29及A18之實線P1包圍的 區域内的比率進行反應而獲得。 再者，根據下述實驗例可知有如下趨勢：於獲得上述烷 氧矽烷之縮合物（A)時，若成分（γ)之調配比例較高，則感 光性組成物之顯影性降低。尤其是，當僅單獨使用成分 (Y)之情形時，於形成圖案膜時，於顯影後會產生殘渣， 從而無法獲得良好的圖案化性能。故而，為了充分獲得顯 衫性’必須使成为（Y)之調配比例不過高，且成分（γ)之調 配比例為99莫耳重量。/。以下。 又，根據下述實驗例可知，較好的是，上述烷氧矽烷之 縮合物（A)係以如下方式而獲得的烷氧矽烷之縮合物， 即，使成分（X)、成分（Y)以及成分（2)，以下述表2所示之 圖8之二成分圖中由連接座標A2、A28、A29及A30的實線 P2包圍的區域内的比率進行反應。於使用該烷氧矽烷之縮 合物之情形時，可進一步提高絕緣性能。 125692.doc 12 200830052 [表2][Technical Field] The present invention relates to a film-forming composition comprising a condensate of alkoxysilane and an acid generator which generates an acid by stimulation with heat or light, and the like. Specifically, it relates to a composition for forming a film which is excellent in storage stability and excellent in insulation performance, a method for producing a pattern film using the same, and an insulating film for an electronic device. [Previous Art] When manufacturing an electronic component such as a semiconductor, a protective film or a gate insulating film is formed by a fine pattern forming method. When the film is formed, for example, a condensate containing a burnt oxane is used. In the following Patent Document 1, as an example of the photosensitive resin composition used for pattern formation, condensation of (1) an alkali-soluble sulfoxylate polymer, that is, alkoxylation is disclosed. (1) a compound which generates an accelerating agent by light, and (3); a known photosensitive resin composition. In Patent Document 1, as (a) a condensate of alkoxydecane, it is used. An alkali-soluble siloxane polymer obtained by removing water and a catalyst from a reaction solution obtained by adding water and a catalyst to alkoxysilane to hydrolyze and condense. • Patent Document 1 In the above, as the raw material of the (1) alkoxy decane condensate, it is preferred to use methyl methoxide, 〇 〜 40 mol % of phenyl dimethoxy decane, and 〇 〜 4 〇 mol% dimethyl dimethoxy decane In the case of the photosensitive resin composition of Patent Document 1, the condensate constituting the oxidized stone of the hospital may be formed by the method of the present invention. The type and the amount of the alkoxysilane are deteriorated and gelled during long-term storage. That is, the storage stability of the photosensitive resin composition of the patent document is insufficient. Further, it is required to expose the photosensitive resin composition. Further, the cured film obtained by hardening to form a cured film has excellent insulating properties. However, any of the storage stability of the prior photosensitive resin composition or the insulating property of the cured film after hardening is insufficient. The present invention has been developed in accordance with the state of the art of the prior art, and it is an object of the invention to provide a film-forming composition which can provide a film excellent in storage stability and excellent in insulation performance, a method for producing a pattern film using the same, and an electronic device. Insulating film. According to the present invention, there is provided a film forming composition characterized by comprising a condensate (A) of alkoxy decane An acid generator (B) which generates an acid by external stimulation, and the condensate (A) of the alkoxydecane contains a component (χ) containing phenyl triethoxylate and/or phenyltrimethoxydecane, a component (γ) containing decyl triethoxylate and/or methyltrimethoxy decane and a component (Ζ) containing triethoxy decane and/or trimethoxine, in the composition diagram of FIG. The ratio of the coordinates in the region surrounded by the solid line P1 of the coordinates α17, Α28, Α29 and Α18 is reacted. In a specific aspect of the film-forming composition of the present invention, the alkoxysilane condensate (A) will be Condensation of alkoxysilane obtained by reacting the component (x), the component (γ) and the component (z) in a ratio in the region surrounded by the solid line P2 of the coordinates A2, A28, A29 and A30 in the third graph of Fig. 8. In another specific aspect of the film-forming composition of the present invention, the alkoxy decane 125692.doc 200830052 ^ condensate (4) system, the component (X), the component (7) and the component (Z) are formed into a graph of FIG. The condensate of the alkoxy oxane obtained by reacting the ratio in the region surrounded by the solid line P3 of the coordinates A31, A28, A29 and A33. Moreover, according to the present invention, there is provided a method for producing a pattern film, which is characterized in that a film for forming a film for forming a film of the present invention is used, and the film forming composition contains an acid which is exposed to light. The photoacid generator is a photosensitive composition of the acid generator (B), and the method for producing the pattern film includes the steps of: forming a photosensitive composition layer containing a photosensitive composition on a substrate; and forming a pattern according to the formed pattern The photosensitive composition layer is selectively exposed, and the photosensitive composition layer of the exposed portion is cured by the action of an acid generated by the photo-acid generator, so that the photosensitive composition layer of the exposed portion is insoluble in the developer; After the photosensitive composition layer in the exposed portion is insoluble in the developer, the photosensitive composition layer is developed by the developer to remove the photosensitive composition layer in the unexposed portion. The insulating film for an electronic device of the present invention is formed using the film-forming composition of the present invention. (Effects of the Invention) The film-forming composition of the present invention contains a condensate (A) of oxysphate, and the condensate (A) of strontium oxysulfide is a component (X) to (z). In the composition diagram of the third component of Fig. 1, the ratio in the region surrounded by the solid line P1 connecting the coordinates A17, A28, A29, and A18 is obtained, and therefore, the film forming composition is excellent in storage stability. Further, in the present invention, the film-forming composition further contains an acid generator (B) which generates an acid by external stimulation such as light or heat. Therefore, for example, an external stimulus can be applied to the film-forming composition to generate an acid. And carry out the hard 125692.doc 200830052 to obtain a film with excellent insulation performance. In the method for producing a patterned film of the present invention, a photosensitive composition layer containing a photosensitive composition as a film-forming composition of the present invention is formed on a substrate, and the photosensitive composition layer is selectively exposed to expose the exposed portion. When the photosensitive composition layer is insoluble in the developer, the photosensitive composition layer is developed by the developer. Therefore, when a photosensitive composition that has been stored for a long period of time is used, a favorable pattern film can be formed. Further, at the time of development, the photosensitive composition layer of the unexposed portion can be easily removed, and a pattern film excellent in insulating properties can be obtained. The insulating film for an electronic device of the present invention is formed by using the film-forming composition of the present invention, and therefore has excellent insulating properties. [Embodiment] Hereinafter, the details of the present invention will be described. The inventors of the present invention have found that the above-described configuration can improve the storage stability of the film-forming composition and obtain a film having excellent insulating properties by the following configuration, thereby developing the present invention. a condensate of decane (A) and an acid generator (B) which generates an acid by external stimulation. The condensate (A) of the above alkoxy decane is a component (X) to (Z) containing a specific alkoxy decane. In the composition diagram of the third part of Fig. 1, the ratios in the region surrounded by the solid line Pi of the joints VIII, A28, am and A18 are obtained. The film-forming composition of the present invention contains an alkoxysilane condensate (A) and an acid generator (B) which generates an acid by external stimulation. Examples of the external stimulus include light such as heat, visible light, or ultraviolet light, ultrasonic waves, microwaves, and the like. When the external stimulus is light, the film-forming composition of the present invention is a photosensitive composition which is photosensitive by exposure. When the external stimuli 125692.doc 200830052 is hot, the film forming composition of the present invention contains a film forming composition of a thermal acid generator. In the following, the situation is detailed in several parts. (Photosensitive composition as a film-forming composition) When the film-forming composition of the present invention is a photosensitive composition which is exposed to light upon exposure, an acid generating agent which generates an acid by exposure is used as the acid generator. (B). The alkoxy decane condensate (A) is a component (X) containing phenyl triethoxy decane and/or phenyl dimethoxy decane, methyl triethoxy decane and/or methyl dimethyl oxygen. The composition of the stone shochu [Y], and the composition (Z) containing triethoxy decane and/or methicone, in the composition of Fig. 1 three, the solid lines connecting coordinates ai7, A28, A29 and A1 8 The ratio in the area surrounded by p 1 reacts. That is, the condensate (A) of the alkoxy decane is a component (χ), a component (Υ), and a component (Ζ) which are linked to coordinates Αΐ7, Α28, Α29, and Α18 in the three-component diagram shown in Table 1 below. The ratio in the area enclosed by the straight line reacts. [Table 1] Ingredient (X) Ingredient (Υ) Ingredient (Ζ) Α17 62.5 37.5 0 Α28 1 99 0 Α29 12.5 75 12.5 Α18 37.5 50 12.5 Unit is mol% by weight It is preferred that the above component (X) is benzene Base triethoxy decane. Preferably, the above-mentioned (Υ) is methyltriethoxydecane. Preferably, the above-mentioned 125692.doc •10-200830052 minutes (z) is triethoxydecane. According to the following experimental examples, it is understood that when the condensate (A) of the alkoxysilane is obtained, the higher the compounding ratio of the component (X), the higher the storage stability of the photosensitive composition. Further, the lower the blending ratio of the components, the higher the storage stability of the photosensitive composition. In particular, the lower the blending ratio of the component (Z), the higher the storage stability of the photosensitive composition is. The reason for this is that the reactivity of the component (X) is lower than the reactivity of the component and the component ,, and the reactivity of the component (Y) is lower than the reactivity of the component. Since the component is not reactive, the condensate of alkoxysilane obtained by using a large amount of the component (X) is difficult to carry out the condensation reaction of the Si〇H group at the time of storage. On the other hand, since the reactivity of the component (Z) is high, the condensate (A) of the alkoxysilane obtained by using a large amount of the component (z) is liable to undergo a condensation reaction of the SiOH group during storage. Therefore, in order to improve the storage stability of the photosensitive composition, it is preferred to reduce the blending ratio of the component (Y) or the component (Z) and to increase the blending ratio of the component (X). Further, the reactivity of the component (X) is lower than that of the component (Y) and the component (Z), and the reactivity of the component (Y) is lower than that of the component (z). Therefore, the higher the ratio of the component (X) to be used, the larger the residual amount of the SiOH group in the condensate (A) obtained by condensation, and thus the photosensitive composition is formed by exposure. The tendency of the insulation property to decrease when the cured film is cured. On the other hand, when the blending ratio of the component (Y) and the component (Z) is increased and the blending ratio of the component (X) is lowered, the condensation reaction is easily completed, and the condensate of the alkoxysilane obtained by the condensation can be reduced (A) The amount of the SiOH group present therein, therefore, the tendency of the insulating property of the cured film of the photosensitive composition to be improved by 125692.doc -11 - 200830052. Therefore, in order to improve the insulating properties of the cured film of the photosensitive composition, it is preferred to reduce the blending ratio of the component (X) to increase the blending ratio of the component (γ) and the component (z). Further, in order to improve the insulating properties of the pattern film, it is preferred to increase the blending ratio of the component (Y) and reduce the blending ratio of the component (X). Therefore, in the present invention, in order to improve the storage stability of the photosensitive composition and obtain a cured film having excellent insulating properties, an oxysulfide condensate (A) and an alkoxy condensate (A) are used. The components (χ) to (z) are obtained by reacting the ratios in the region surrounded by the solid line P1 connecting the coordinates A17, A28, A29, and A18 in the three-component diagram. Further, according to the following experimental examples, when the condensate (A) of the alkoxysilane is obtained, when the compounding ratio of the component (γ) is high, the developability of the photosensitive composition is lowered. In particular, when the component (Y) is used alone, when the pattern film is formed, a residue is generated after development, so that good patterning performance cannot be obtained. Therefore, in order to sufficiently obtain the visibility, it is necessary to make the ratio of (Y) too high, and the ratio of the component (γ) is 99 mol. /. the following. Moreover, it is understood from the following experimental examples that the condensate (A) of the alkoxy oxane is a condensate of alkoxy decane obtained as follows, that is, the component (X) and the component (Y). Further, the component (2) is reacted in a ratio in a region surrounded by a solid line P2 connecting the coordinates A2, A28, A29 and A30 in the component diagram of Fig. 8 shown in Table 2 below. In the case of using the alkoxydecane condensate, the insulation property can be further improved. 125692.doc 12 200830052 [Table 2]

進而，根據下述實驗例可知， 之縮合物（A)係以如下方式而獲Further, according to the following experimental examples, the condensate (A) was obtained as follows.

較好的是，上述烷氧矽烷 得的烷氧矽烷之縮合物， 即，使成分（X)、成分〇〇以及成分（2)，以下述表3所示之 圖9之三成分®中由連接座標A31、A28、A29及A33的實線 P3包圍的區域内的比率進行反應。於使用該烷氧矽烷之縮 合物之情形時，可進一步提高絕緣性能。 [表3] 成分（X) 成分CY) 成分（Ζ) Α31 20 80 0 Α28 1 99 0 Α29 ~~12.5 75 12.5 Α33 20 ~67.5 12.5 單位為莫耳重詈％ 上述烷氧矽烷之縮合物（A)係縮合有2種以上之烷氧矽烷 者。烷氧矽烷之縮合物（A)之重量平均分子量較好的是5〇〇 以上。烷氧矽烷之縮合物（A)可為使上述成分（χ)〜〇以上 述比率進行反應後而獲得者，且亦可為少量的、成分 (X) (Ζ)以外的、具有其他官能基之烧氧⑦烧或烧氧基數 125692.doc -13- 200830052 不同之烷氧矽烷等烷氧矽烷。烷氧矽烷之縮合物（A)可僅 單獨使用1種，亦可併用2種以上。 感光性組成物，除上述烷氧矽烷之縮合物（A)外，更含 有曝光即產生酸之光酸產生劑。 上述曝光即產生酸之酸產生劑（B)並無特別限定，可列 舉：Midori化學公司製造之商品名為「TPS-105」（CAS No.66003-78-9)、「TPS-109」（CAS No. 144317-44-2) > 「MDS-105」（CAS No.116808-67-4)、「MDS-205」（CAS No.81416-37-7)、「DTS-105」（CAS Ν〇·111281_12-0)、 「NDS-105」（CAS Νο·195057-83-1)、「NDS-165」（CAS No.316821-98-4)等銃鹽化合物；「DPI-105」（CAS No.66003-76-7)、「DPI-106」（CAS No.214534-44-8)、Preferably, the condensate of the alkoxydecane obtained from the alkoxysilane, that is, the component (X), the component hydrazine, and the component (2) are represented by the component of Fig. 9 bis as shown in Table 3 below. The ratio in the region surrounded by the solid line P3 connecting the coordinates A31, A28, A29, and A33 is reacted. In the case of using the alkoxydecane condensate, the insulation property can be further improved. [Table 3] Ingredient (X) Ingredient CY) Ingredient (Ζ) Α31 20 80 0 Α28 1 99 0 Α29 ~~12.5 75 12.5 Α33 20 ~67.5 12.5 Unit is Molar 詈% The condensate of the above alkoxy decane (A ) is a condensation of two or more alkoxysilanes. The weight average molecular weight of the alkoxysilane condensate (A) is preferably 5 Å or more. The alkoxysilane condensate (A) may be obtained by reacting the above components (χ) to 〇 at the above ratio, and may be a small amount, other than the component (X) (Ζ), having other functional groups. The calcined oxygen is burned or the number of alkoxy groups is 125692.doc -13- 200830052 Alkoxy decane such as alkoxy oxane. The alkoxysilane condensate (A) may be used alone or in combination of two or more. The photosensitive composition contains, in addition to the alkoxysilane condensate (A), a photoacid generator which is exposed to generate acid. The acid generator (B) which generates the acid is not particularly limited, and the product name "TPS-105" (CAS No. 66003-78-9) and "TPS-109" manufactured by Midori Chemical Co., Ltd. CAS No. 144317-44-2) > "MDS-105" (CAS No. 116808-67-4), "MDS-205" (CAS No. 81416-37-7), "DTS-105" (CAS Ν〇·111281_12-0), "NDS-105" (CAS Νο·195057-83-1), "NDS-165" (CAS No.316821-98-4) and other strontium salt compounds; "DPI-105" ( CAS No.66003-76-7), "DPI-106" (CAS No.214534-44-8),

「DPI-109」（CAS No.194999-82-1)、「DPI-201」（CAS No.6293-66-9)、「BI-105」（CAS No. 1 54557-16-1)、「MPI-105」（CAS No.1 15298-63-0) 、「MPI-106」（CAS"DPI-109" (CAS No. 194999-82-1), "DPI-201" (CAS No. 6293-66-9), "BI-105" (CAS No. 1 54557-16-1), " MPI-105" (CAS No.1 15298-63-0), "MPI-106" (CAS

No.260061-46-9)、「MPI-109」（CAS No.260061-47-0)、 「BBI-105」（GAS Νο·84563-54-2)、「BBI-106」（CAS No.185 195-30-6)、「BBI-109」（CAS No.194999-85-4)、 「BBI-110」（CAS No.213740-80-8)、「BBI-201」（CAS No.l42342-33-4)等碘鹽化合物；Midori化學公司製造之商 品名為「NAI-106」（萘二曱醯亞胺樟腦磺酸鹽、CAS No.83697-56-7)、「NAI-100」（CAS No.83697-53-4)、 「NAI_1002」（CAS Ν〇·76656_48-9)、「ΝΑΙ-1004」（CAS No.83697-60-3)、Γ NAI-101」（CAS No.555 1-72-4)、「NAI- 125692.doc -14- 200830052 105」（CASN〇.85342_62-7)、「NAI-109」（CASN〇.171417-91-7)、「NI-101」（CAS Νο·13 1526-99-3)、「ΝΙ-105」（CAS No.85342-63-8)、「NDI-101」（CAS No. 141714-82-1) > 「NDI-105」（CAS No.133710-62-0)、「NDI-106」（CAS No.210218-57-8)、r NDI-109」（CAS No.30753 1-76-6)、 「PAI-01」（CAS No.175 12-88-8)、「PAI-101」（CAS No.82424-53-1)、「PAI-106」（CAS No.202419-88-3) > 「PAI-1001」（CAS No.193222-02-5)、「SI-101」（CAS No.55048-39-0)、「SI-105」（CAS No.34684-40-7)、rSI-106」（CASNo.l79419-32-0)、「SI-109」（CASNo.252937-66-9)、「PI-105」（CAS Νο·41580-58-9)、「PI-106」（CAS No.83697-51-2)，汽巴精化公司製造之商品名為 「CGI1397」、「CGI1325」、「CGI1380」、「CGI1311」、 「CGI263」、「CGI268」等磺酸酯化合物；Midori化學公司 製造之商品名為「DTS200」（CAS No.203573-06-2)、 Rhodia Japan公司製造之商品名為 「RHODORSIL PHOTOINITIATOR-2074」（CAS No.178233-72-2)等以 BF4-為對離子之化合物等。酸產生劑（B)可單獨使用，亦可併 用2種以上。 除作為該等光敏劑之酸產生劑（B)外，為了進一步提高 靈敏度，可進而添加敏化劑。 上述敏化劑並無特別限定，具體而言，可較佳地使用例 如：二苯甲酮、p，p’-四曱基二胺基二苯曱酮、p，pf-四乙基 胺基二苯甲酮、2-氣噻噸酮、蒽酮、9·乙氧基蒽、蒽、 125692.doc -15· 200830052 芘、茈、硫二苯胺、二笨基乙二酮、吖啶橙、苯幷黃素、 Setoflavine-T、9，10_二苯基蒽、9-苐酮、苯乙酮、菲、 硝基第、5-硝基苊、苯醌、2-氣-4-硝基苯胺、N-乙醯·對 硝基苯胺、對硝基苯胺、N-乙醯-4-硝基-1-萘胺、苦基 胺、蒽醌、2-乙基蒽醌、2_第三丁基蒽醌、丨，2_苯蒽醌、 3-曱基-1，3 - 一氮_1，9 -苯蒽酮、二亞苄丙酮、ι，2_萘酉昆、 3,3’-羧基-雙（5,7-二甲氧基羰基香豆素）以及蔻等。 較理想的疋’相對於1 〇〇重量份的烧氧石夕燒之縮合物 (A) ’上述曝光即產生酸之酸產生劑（B)之含有比例為 〇·〇5〜50重量份之範圍。當酸產生劑（B)未滿〇〇5重量份 時’有時靈敏度不充分，難以形成圖案膜等膜。當酸產生 劑（B)超過50重量份時，有時難以均勻地塗佈感光性組成 物，進而導致於顯影後產生殘渣。 可於感光性組成物中進而添加適當的溶劑。藉由添加溶 劑’可提供能夠容易地進行塗佈之感光性組成物。 上述溶劑只要能溶解烷氧矽烷之縮合物（A)，則並無特 別限定，可列舉：苯、二甲苯、甲苯、乙苯、苯乙烯、三 甲苯、二乙苯等芳香族碳氫化合物；環己烷、環己烯、雙 戊稀、正戊烧、異戊烷、正己烷、異己烷、正庚烷、異庚 燒、正辛燒、異辛烷、正壬烷、異壬烷、正癸烷、異癸 炫*、四氫化萘、角鯊烯等飽和或不飽和碳氫化合物；二乙 、 一 -Γ ~r~ a·. 丙轉、二-異丙鱗、二丁醚、乙基丙基_、二苯 鱗' 二 7 一齡一 一 G 一醇二甲醚、二乙二醇二乙醚、二乙二醇二丁 、 一 7 一 〇 一醇曱基乙基醚、二丙二醇二甲醚、二丙二醇二 125692.doc -16 - 200830052 乙驗、二丙二酿-_ , 知一丁喊、二丙二醇甲基乙基醚、乙二醇二 曱、乙二醇-7⑽ 予一乙醚、乙二醇二丙醚、乙二醇曱基乙基 鱗、四氫TJ夫喃、〗4 一 一 > 0 ，.二噁烷、丙二醇單甲基醚乙酸酯、乙 一醇單乙基鱗乙酿π W 齩酉曰、二丙二醇曱基醚乙酸酯、二乙二醇 單乙基乙酸_、其 G基％己烷、甲基環己烷、對薄荷烷、 正薄荷烷、間薄苻栌 , 寻仃烷、二丙醚、二丁醚等醚類；丙酮、甲 基乙，同、甲基異丁基酮、二甲酮、二丙酮、甲基戊基 :衣戊嗣、％己嗣、環庚酮等酮類；乙酸乙醋、乙酸甲 知乙^ 丁酉曰、乙酸丙醋、乙酸環己醋、乙酸曱基賽璐 蘇、乙酸乙基賽路蘇、乙酸丁基賽路蘇、乳酸乙醋、乳酸 丙酉日、乳酸丁酉旨、受丨而充 礼馱異戊自曰、硬脂酸丁酯等酯類等。該 等溶劑可單獨使用，亦可併用2種以上。 上述+劑之_比例係’例如於基板上塗敷感光性組成 物而形成感光性組成物層時，以均勾塗敷之方式加以適當 卩可車乂好的& ’感光性組成物之濃度以固形分濃度 計’為〇.5〜70重量％，更好的是，為2〜50重量％左右。 可視需要而於感光性組成物中進而添加其他添加劑。如 上所述之添加劑可列舉：填充劑、顏料、㈣、均染劑、 夕烷偶口』、消泡劑、抗靜電劑、紫外線吸收劑、pH值調 正4 〃政劑、分散助劑、表面改質劑、塑化劑、塑化促 進劑、防流掛劑等。 本^明之圖案臈之製造方法中，依次進行如下步驟··於 基板上形成感光性組成物層之步驟；曝光感光性組成物層 之步驟；以及顯影感光性組成物層之步驟。具體而言，依 125692.doc -17- 200830052 人進行如下各步驟：於基板上形成包含作為本發明之膜形 成用組成物的感光性組成物的感光性組成物層的步驟；根 據所形成之圖案，選擇性地曝光感光性組成物層，藉由自 光酸產生劑產生之酸之作用，於曝光部中使感光性組成物 g更化使曝光部之感光性組成物層不溶於顯影液之步 驟，以及於曝光部之感光性組成物層不溶於顯影液後，利 用頌衫液使感光性組成物層顯影，去除未曝光部之上述感 光性組成物層之步驟。 本I明之圖案膜之製造方法中，首先，例如圖2(約所 不，於基板上，形成包含作為本發明之膜形成用組成物之 感光性組成物的感光性組成物層1。 關於形成上述感光性組成物層丨之方法，並無特別限 疋，可列舉例如將感光性組成物付與至圖2所示之基板2上 而形成感光性組成物層丨之方法。此時之具體方法可使用 、般的塗敷方法，例如，浸塗、滾塗、棒塗、刷塗、噴 塗、旋塗、擠壓塗敷、凹板塗敷等。作為塗敷有感光性組 成物之基板2 ’可根據用途而使用石夕基板、玻璃基板、金 屬板塑料板等。$光性組成物層1之厚度，根據用途而 有所不同，但10 nm〜1〇 μιη為基準。 塗敷於基板2上之感光性組成物層i較理想的是，當為了 使烧氧㈣之縮合物⑷溶解而使用溶劑時，為了使該溶 hJ乾秌而進行加熱處理。加熱處理溫度一般為 C 200 C可根據溶劑之沸點或蒸氣壓力作適當選擇。 '、人如圖2⑻所不，曝光感光性組成物層1。於曝光 125692.doc -18- 200830052 時，使用例如與圖案形狀相應之光罩3等。於已曝光之感 光性組成物層1A中，自光酸產生劑產生酸。另一方面，於 未曝光之感光性組成物層⑺中，未自光酸產生劑產生酸。 藉由於已曝光之感光性組成物層1A中自光酸產生劑產生 之酸的作用，使烷氧矽烷之縮合物（A)交聯。若烷氧矽烷 之縮合物（A)交聯，則感光性組成物層1A硬化。其結果 為，曝光部之感光性組成物層丨八不溶於顯影液。 於曝光時，作為用以照射紫外線或可見光等活性能量線 之光源，並無特別限定，可使用超高壓水銀燈、深紫外線 燈、高壓水銀燈、低壓水銀燈、金屬_素燈、準分子雷射 等。該等.光源可根據感光性組成物之構成成分之感光波長 而適當選擇。光之照射能量係取決於所期望之膜厚及感光 性組成物之構成成分，但一般而言為10〜3000 mJ/cm2之範 圍。當小於10 mJ/cm2時，曝光部之感光性組成物層以有 日才不處充分硬化，而當大於3〇〇〇 mJ/cm2時，可能導致曝 光時間過長，圖案膜之每小時之製造效率可能會降低。 其次’利用顯影液使感光性組成物層顯影ΙΑ、1B。藉 由利用顯影液進行顯影，使未曝光部之感光性組成物層1B ’谷解於顯影液中後去除，從而獲得圖案膜1C。 於選擇性地曝光感光性組成物層1後，利用顯影液使感 光性組成物層顯影丨A、1B，藉此，使未曝光部之感光性 、、且成物層1B溶解於顯影液中後去除，而曝光部之感光性組 成物層1A保留於基板2上。從而獲得圖案膜1C。因已去除 未曝光部之感光性組成物層1B，故該圖案係被稱為負型圖 125692.doc -19- 200830052 案者。 此處’所謂顯影’除包含將曝光部之感光性組成物層ia 及未曝光部之感光性組成物層1B浸潰於鹼性水溶液等顯影 液中的操作外’亦包含制顯影液處理感光性組成物層 ΙΑ、1B之各種操作’ ，利用顯影液沖洗該感光性組成 物層ΙΑ、1B之表面之操作，或者，將顯影液喷射於上述 感光性組成物層ΙΑ、1B之表面之操作等。 7再者，戶斤謂_液係於選擇性地曝光感光性组成物層i 後溶解未曝光部之感光性組成物1B之液體。因曝光部之感 光性組成物層1A硬化，故不會溶解於顯影液。顯影液並不 限於鹼性水溶液，亦可使用酸性水溶液或各種溶劑。溶劑 可列舉上述各種溶劑。酸性水溶液可列舉草酸、犧酸、醋 酸等。 曰 顯影液無須防爆設備，且因腐蝕等所產生之設備負擔亦 較少，故而，較好的是使用鹼性水溶液。例如，可列舉四 甲基氫氧化銨水溶液、矽酸鈉水溶液、氫氧化鈉水溶液、 虱氧化鉀水溶液等鹼性水溶液。顯影所須要之時間取決於 感光性組成物層之厚度及溶劑種類，但為了高效地顯影且 提高製造效率，較好的是丨秒〜10分鐘之範圍。較好的是， 於顯影後，利用蒸餾水清洗圖案膜，來去除殘留於膜上之 鹼性水溶液等顯影液。 再者，於上述曝光時，亦可曝光基板2上之感光性組成 物層1之整個表面。此時，可獲得基板2上之感光性組成物 層1之整個表面均硬化的硬化物膜。 125692.doc •20- 200830052 (含有熱酸產生劑之膜形成用組成物） 本發明之膜形成用組成物中，可代替曝光即產生酸之光 酸產生劑，而使用熱處理時產生酸之熱酸產生劑。除酸產 生劑（B)不同之外，含有熱酸產生劑之膜形成用組成物可 以與上述感光性組成物相同的方式而構成。 上述熱酸產生劑並無特別限定，可列舉例如鑌鹽等。 更好的是，上述熱酸產生劑為選自重氮鹽、銨鹽、鱗 鹽、埃鹽、疏鹽、砸鹽、鉀鹽及績酸g旨所組成之群中之至 少1種。No.260061-46-9), "MPI-109" (CAS No.260061-47-0), "BBI-105" (GAS Νο·84563-54-2), "BBI-106" (CAS No. 185 195-30-6), "BBI-109" (CAS No. 194999-85-4), "BBI-110" (CAS No. 213740-80-8), "BBI-201" (CAS No. l42342) -33-4) Iodine salt compound; manufactured by Midori Chemical Co., Ltd. under the trade name "NAI-106" (naphthalene diimide camphor sulfonate, CAS No. 83697-56-7), "NAI-100" (CAS No. 83697-53-4), "NAI_1002" (CAS Ν〇 76665_48-9), "ΝΑΙ-1004" (CAS No. 83697-60-3), Γ NAI-101" (CAS No. 555) 1-72-4), "NAI-125692.doc -14- 200830052 105" (CASN〇.85342_62-7), "NAI-109" (CASN〇.171417-91-7), "NI-101" ( CAS Νο·13 1526-99-3), "ΝΙ-105" (CAS No. 85342-63-8), "NDI-101" (CAS No. 141714-82-1) > "NDI-105" ( CAS No.133710-62-0), "NDI-106" (CAS No. 210218-57-8), r NDI-109" (CAS No. 30753 1-76-6), "PAI-01" (CAS No.175 12-88-8), "PAI-101" (CAS No.82424-53-1), "PAI-106" (CAS No. 202419-88-3) > "PA I-1001" (CAS No. 193222-02-5), "SI-101" (CAS No.55048-39-0), "SI-105" (CAS No. 34684-40-7), rSI-106 (CAS No.l79419-32-0), "SI-109" (CAS No. 252937-66-9), "PI-105" (CAS Νο·41580-58-9), "PI-106" (CAS No) .83697-51-2), sulfonate compounds such as "CGI1397", "CGI1325", "CGI1380", "CGI1311", "CGI263", "CGI268" manufactured by Ciba Specialty Chemicals; Midori Chemical Co., Ltd. The product name is "DTS200" (CAS No. 203573-06-2), and the product name "RHODORSIL PHOTOINITIATOR-2074" (CAS No. 178233-72-2) manufactured by Rhodia Japan Co., Ltd. Compounds and the like. The acid generator (B) may be used singly or in combination of two or more. In addition to the acid generator (B) as the photosensitizer, in order to further improve the sensitivity, a sensitizer may be further added. The sensitizer is not particularly limited, and specifically, for example, benzophenone, p,p'-tetradecyldiaminodibenzophenone, p,pf-tetraethylamino group can be preferably used. Benzophenone, 2-air thioxanthone, anthrone, 9·ethoxy hydrazine, hydrazine, 125692.doc -15· 200830052 hydrazine, hydrazine, thiodiphenylamine, dipyridylethylenedione, acridine orange, Benzoflavin, Setoflavine-T, 9,10-diphenylhydrazine, 9-fluorenone, acetophenone, phenanthrene, nitro, 5-nitroindole, benzoquinone, 2-ox-4-nitro Aniline, N-acetamidine p-nitroaniline, p-nitroaniline, N-acetylindole-4-nitro-1-naphthylamine, picrylamine, anthracene, 2-ethylhydrazine, 2_third Butyl hydrazine, hydrazine, 2_phenylhydrazine, 3-mercapto-1,3-nitroso-1,9-benzophenone, dibenzylideneacetone, ι,2-naphthoquinone, 3,3' -Carboxy-bis(5,7-dimethoxycarbonylcoumarin) and hydrazine. Preferably, the 疋' is relative to 1 part by weight of the oxysulfide condensate (A). The above-mentioned exposure, that is, the acid generating agent (B) is contained in an amount of 5 to 50 parts by weight. range. When the acid generator (B) is less than 5 parts by weight, the sensitivity may be insufficient, and it may be difficult to form a film such as a pattern film. When the acid generator (B) exceeds 50 parts by weight, it may be difficult to uniformly apply the photosensitive composition, which may cause residue after development. Further, a suitable solvent can be added to the photosensitive composition. A photosensitive composition which can be easily applied can be provided by adding a solvent '. The solvent is not particularly limited as long as it can dissolve the alkoxysilane condensate (A), and examples thereof include aromatic hydrocarbons such as benzene, xylene, toluene, ethylbenzene, styrene, trimethylbenzene, and diethylbenzene; Cyclohexane, cyclohexene, dipentane, n-pentane, isopentane, n-hexane, isohexane, n-heptane, isoheptane, n-octyl, isooctane, n-decane, isodecane, Saturated or unsaturated hydrocarbons such as n-decane, isoindole*, tetrahydronaphthalene, squalene; diethyl, mono-oxime ~r~ a·. propane, di-isopropyl scale, dibutyl ether, Ethyl propyl _, diphenyl squaring ' 2 7 one age one by one G glycerol dimethyl ether, diethylene glycol diethyl ether, diethylene glycol dibutyl, a 7-nonyl decyl decyl ethyl ether, two Propylene glycol dimethyl ether, dipropylene glycol II 125692.doc -16 - 200830052 乙验,二丙二酿-_ , Zhiyi Ding shout, dipropylene glycol methyl ethyl ether, ethylene glycol dioxime, ethylene glycol-7 (10) Monoethyl ether, ethylene glycol dipropyl ether, ethylene glycol decyl ethyl sulphate, tetrahydro TJ phoran, 〗 4 _ _ 0, dioxane, propylene glycol monomethyl ether acetate, ethyl alcohol B鳞B brewed π W 齩酉曰, dipropylene glycol decyl ether acetate, diethylene glycol monoethyl acetic acid _, its G-based hexane, methyl cyclohexane, p-menthane, n-menthane, between Thin 苻栌, looking for ethers such as decane, dipropyl ether, dibutyl ether; acetone, methyl ethyl, iso, methyl isobutyl ketone, dimethyl ketone, diacetone, methyl amyl: pentylene, Ketones such as hexanone and cycloheptanone; ethyl acetate, acetic acid, ketone, butyl acetonide, propylene acetate, cyclohexyl vinegar, acesulfame acetate, ethyl celecoxib acetate, acetate butyl Lu Su, lactic acid ethyl acetate, lactic acid propionate day, lactic acid butyl sputum, sputum and sputum, sulphur, butyl sulphate and other esters. These solvents may be used singly or in combination of two or more. The ratio of the above-mentioned + agent is, for example, when a photosensitive composition is applied onto a substrate to form a photosensitive composition layer, and the coating is appropriately applied to the coating. The solid content concentration is '5 to 70% by weight, more preferably 2 to 50% by weight. Further additives may be further added to the photosensitive composition as needed. The additives mentioned above may be exemplified by fillers, pigments, (4), leveling agents, oxirane couples, antifoaming agents, antistatic agents, ultraviolet absorbers, pH adjustment agents, dispersing aids, Surface modifier, plasticizer, plasticizer, anti-sagging agent, etc. In the method for producing a pattern of the present invention, the following steps are carried out: a step of forming a photosensitive composition layer on a substrate; a step of exposing the photosensitive composition layer; and a step of developing the photosensitive composition layer. Specifically, according to 125692.doc -17-200830052, the following steps are carried out: a step of forming a photosensitive composition layer containing a photosensitive composition as a film-forming composition of the present invention on a substrate; The pattern is selectively exposed to the photosensitive composition layer, and the photosensitive composition g is made to be insoluble in the exposed portion by the action of an acid generated from the photoacid generator, so that the photosensitive composition layer of the exposed portion is insoluble in the developer In the step of dissolving the photosensitive composition layer in the exposed portion in the developing solution, the photosensitive composition layer is developed by the shirting liquid to remove the photosensitive composition layer in the unexposed portion. In the method for producing a patterned film of the present invention, first, for example, a photosensitive composition layer 1 containing a photosensitive composition which is a composition for forming a film of the present invention is formed on a substrate. The method of the photosensitive composition layer is not particularly limited, and for example, a method in which a photosensitive composition is applied to the substrate 2 shown in Fig. 2 to form a photosensitive composition layer 。 is exemplified. The method can be applied by a general coating method such as dip coating, roll coating, bar coating, brush coating, spray coating, spin coating, extrusion coating, gravure coating, etc. as a substrate coated with a photosensitive composition. 2 'It is possible to use Shishi substrate, glass substrate, metal plate plastic plate, etc. depending on the application. The thickness of the optical composition layer 1 varies depending on the application, but is based on 10 nm to 1 〇μιη. It is preferable that the photosensitive composition layer i on the substrate 2 is subjected to heat treatment in order to dissolve the condensed product (4) in order to dissolve the oxidized product (4), and the heat treatment temperature is generally C 200. C can be based on the boiling point or vapor of the solvent For the appropriate selection. ', the person as shown in Figure 2 (8) does not expose the photosensitive composition layer 1. When the exposure 125692.doc -18- 200830052, for example, the mask 3 corresponding to the shape of the pattern, etc. In the composition layer 1A, an acid is generated from the photoacid generator. On the other hand, in the unexposed photosensitive composition layer (7), no acid is generated from the photoacid generator. By the exposed photosensitive composition layer 1A The action of the acid generated by the photoacid generator causes the alkoxysilane condensate (A) to crosslink. When the alkoxysilane condensate (A) is crosslinked, the photosensitive composition layer 1A is hardened. The photosensitive composition layer of the exposed portion is insoluble in the developer. The light source for irradiating the active energy rays such as ultraviolet rays or visible light is not particularly limited, and an ultrahigh pressure mercury lamp, a deep ultraviolet lamp, or a high voltage can be used. Mercury lamps, low-pressure mercury lamps, metal-based lamps, excimer lasers, etc. These light sources can be appropriately selected depending on the photosensitive wavelength of the constituent components of the photosensitive composition. The irradiation energy of the light depends on the desired film thickness and feeling. The constituent component of the composition is generally in the range of 10 to 3000 mJ/cm 2 . When it is less than 10 mJ/cm 2 , the photosensitive composition layer of the exposed portion is not sufficiently hardened at all times, and when it is larger than 3 When 〇〇〇mJ/cm2, the exposure time may be too long, and the manufacturing efficiency per hour of the pattern film may be lowered. Next, the photosensitive composition layer is developed by a developing solution, 1B. Development by using a developing solution The photosensitive composition layer 1B' of the unexposed portion is removed in the developer and then removed to obtain the pattern film 1C. After the photosensitive composition layer 1 is selectively exposed, the photosensitive composition layer is formed by the developer After the development of the 丨A and 1B, the photosensitive layer of the unexposed portion is removed, and the resultant layer 1B is dissolved in the developer, and then removed, and the photosensitive composition layer 1A of the exposed portion remains on the substrate 2. Thereby, the pattern film 1C is obtained. Since the photosensitive composition layer 1B of the unexposed portion has been removed, the pattern is referred to as a negative pattern 125692.doc -19-200830052. Here, the term "development" includes the process of immersing the photosensitive composition layer ia of the exposed portion and the photosensitive composition layer 1B of the unexposed portion in a developing solution such as an alkaline aqueous solution. The operation of the composition layer ΙΑ, the various operations of 1B, the operation of rinsing the surface of the photosensitive composition layer ΙΑ, 1B with a developer, or the operation of spraying the developer onto the surface of the photosensitive composition layer 1, 1B Wait. In addition, the liquid is a liquid which dissolves the photosensitive composition 1B of the unexposed portion after selectively exposing the photosensitive composition layer i. Since the photosensitive composition layer 1A of the exposed portion is hardened, it is not dissolved in the developer. The developer is not limited to an alkaline aqueous solution, and an acidic aqueous solution or various solvents may also be used. The solvent can be exemplified by the above various solvents. Examples of the acidic aqueous solution include oxalic acid, acid, and acetic acid.曰 The developer does not require explosion-proof equipment, and the equipment burden due to corrosion is small. Therefore, it is preferred to use an alkaline aqueous solution. For example, an alkaline aqueous solution such as a tetramethylammonium hydroxide aqueous solution, a sodium citrate aqueous solution, a sodium hydroxide aqueous solution or a potassium cesium hydroxide aqueous solution can be mentioned. The time required for development depends on the thickness of the photosensitive composition layer and the kind of the solvent, but in order to efficiently develop and improve the production efficiency, it is preferably in the range of leap seconds to 10 minutes. Preferably, after the development, the pattern film is washed with distilled water to remove a developing solution such as an alkaline aqueous solution remaining on the film. Further, at the time of the above exposure, the entire surface of the photosensitive composition layer 1 on the substrate 2 can be exposed. At this time, a cured film in which the entire surface of the photosensitive composition layer 1 on the substrate 2 is hardened can be obtained. 125692.doc • 20-200830052 (Composition for forming a film containing a thermal acid generator) The film-forming composition of the present invention can be used as a photoacid generator which generates an acid instead of exposure, and generates heat of acid when heat treatment is used. Acid generator. The film-forming composition containing a thermal acid generator may be formed in the same manner as the above-mentioned photosensitive composition, except for the acid generator (B). The thermal acid generator is not particularly limited, and examples thereof include a phosphonium salt. More preferably, the thermal acid generator is at least one selected from the group consisting of a diazonium salt, an ammonium salt, a scale salt, an arsenic salt, a salty salt, a cerium salt, a potassium salt, and a chloric acid.

上述熱酸產生劑之具體例可列舉：重氮鹽（s· LSpecific examples of the above thermal acid generator include diazonium salts (s·L)

Schlesinger，Photogr· Sci. Eng·，18, 387(1974)、T. S· Bal et al，Polymer, 21，423(1980)中有明確揭示）；銨鹽（美國專利 第4069055號、美國專利第4069056號、美國專利再發行第 27992號之各說明書及日本專利特開平4-365049號公報中 有明確揭示）；鱗鹽（D. C. Necker et al，Macromolecules， 17, 2468 (1984)、C· S· Wen et al，Teh，Pr〇c. Conf· Rad，Schlesinger, Photogr. Sci. Eng., 18, 387 (1974), T. S. Bal et al, Polymer, 21, 423 (1980); ammonium salts (US Patent No. 4069055, US Patent No. No. 4069056, U.S. Patent Reissue No. 27,992, and Japanese Patent Laid-Open No. Hei-4-365049, the disclosure of which is incorporated herein by reference. Wen et al, Teh, Pr〇c. Conf· Rad,

Curing ASIA，p478 Tokyo, 〇ct(1988)、美國專利第 4069055 號、美國專利第4069056號之各說明書中有明確揭示）；峨 鹽（J. V· Crivello et al，Macromorecules, 10 (6)，1307 (1977)、Chem. & Eng· News，Nov. 28, p3 1 (1988)、歐州專 利104143號、美國專利第339049號、美國專利第410201號 之各說明書以及曰本專利特開平2-150848號、日本專利特 開平2-296514號之各公報中有明確揭示）；銕鹽（j· V.Curing ASIA, p478 Tokyo, 〇 ct (1988), U.S. Patent No. 4,609, 055, and U.S. Patent No. 4,609, 056, each of which is expressly incorporated by reference in its entirety herein; 1307 (1977), Chem. & Eng· News, Nov. 28, p3 1 (1988), European Patent No. 104143, US Patent No. 339049, US Patent No. 410201, and Japanese Patent Laid-Open No. 2- No. 150848, Japanese Patent Laid-Open No. 2-296514, each of which is explicitly disclosed); 銕 salt (j·V.

Crivello et al，Polymer J. 17，73 (1985)、J· V· Crivello et 125692.doc -21 - 200830052 al，J. Org. Chem·，43，3055 (1978)、W\ R. Watt et al，J.Crivello et al, Polymer J. 17, 73 (1985), J. V. Crivello et 125692.doc -21 - 200830052 al, J. Org. Chem., 43, 3055 (1978), W\R. Watt et al , J.

Polymer Sci.3 Polymer Chem. Ed., 22, 1789 (1984) ' J. V. Crivello et al，PolymerBull·，14，279 (1985)、J· V. Crivello et al5 Macromorecules，14 (5)，1141 (1981)、J. V· Crivel. l〇 et al5 J· Polymer Sci·，Polymer Chem. Ed.，17，2877 (I979)、歐州專利37〇693號、歐州專利3902114號、歐州專 利233567號、歐州專利297443號、歐州專利297442號、美 國專利第4933377號、美國專利第161811號、美國專利第 41〇2〇1號、美國專利第339(M9號、美國專利第4760013 號、美國專利第4乃4444號、美國專利第2833827號、德國 專利第29CM626號、德國專利第3604580號、德國專利第 3604581號之各說明書中有明確揭示）；硒鹽（j· V. et al5 Macromorecules, 10 (6)5 1307 (1977) ^ J. V. Crivello et al5 J. Polymer Sci.5 Polymer Chem. Ed.? 173 1047 (1979) 中有明確揭示）；以及钟鹽（c· s. Wen et al，Teh，Polymer Sci.3 Polymer Chem. Ed., 22, 1789 (1984) 'JV Crivello et al, Polymer Bull, 14, 279 (1985), J. V. Crivello et al 5 Macromorecules, 14 (5), 1141 (1981) , J. V. Crivel. l〇et al5 J· Polymer Sci·, Polymer Chem. Ed., 17, 2877 (I979), European Patent No. 37〇693, European Patent No. 3902114, European Patent No. 233567, European Patent 297443 No. 297442, U.S. Patent No. 297, 443, U.S. Patent No. 4,933,377, U.S. Patent No. 1,161,811, U.S. Patent No. 4,112, U.S. Patent No. 339 (M9, U.S. Patent No. 4,760,013, U.S. Patent No. 4, 4,444 U.S. Patent No. 2,833, 827, German Patent No. 29 CM 626, German Patent No. 3, 604, 580, and German Patent No. 3,605,581, each of which is expressly incorporated by reference; selenium salt (j. V. et al5 Macromorecules, 10 (6) 5 1307 (1977) ^ JV Crivello et al5 J. Polymer Sci.5 Polymer Chem. Ed.? 173 1047 (1979) clearly disclosed); and clock salt (c·s. Wen et al, Teh,

Conf. Rad· Curing ASIA，p478 T〇ky〇, 〇ct (1988)中有明確 揭示）。作為鑌鹽之對陰離子之示例，可列舉Bp*·、 CF3s〇3_、C4F9S〇3·、c8Fi7S〇3.以及cH3S〇3.等。又，作為 光酸產生劑而列舉之化人舲介 ' 化口物亦可用作熱酸產生劑。該等熱 酸產生劑可單獨使用，，亦可併用2種以上。 較理想的是，相對於100重 里切之坑乳石夕燒之縮合物 (A)，上述熱酸產生劑冬 王㈤之3有比例為0·05〜5〇重量 圍。當熱酸產生劑未滿〇.〇5重 專巳 ^ ^^, 置里伤¥，有時不能充分產生 酸，而當超過50重量份時，有 座生 有T難以均勻地塗佈臈形成用 125692.doc -22- 200830052 組成物，從而膜厚不均勻。 當使膜形成用組成物硬化而形成硬化物膜時，於上述圖 案膜之製造步驟中，可不使形成於基板2上之膜形成用組 成物層曝光，而進行熱處理。 亦即，可於在基板2上形成包含本發明之膜形成用組成 物之膜形成用組成物層後，對該膜形成用組成物層進行熱 處理’藉由自酸產生劑（B)產生之酸之作用，使膜形成用 組成物層硬化。 (膜形成用組成物之用途） 使用膜形成用組成物而形成之膜可用於各種用途。此 處，所謂「使用膜形成用組成物而形成之膜」係指，將熱 或光等外部刺激施加於膜形成用組成物而導入交聯構造後 所獲得之膜。 本發明之膜形成用組成物可較佳地用於在各種裝置中形 成圖案膜等膜，但上述膜形成用組成物可較佳地用於電子 機器之絕緣膜。作為電子機器之絕緣膜，藉由使用由上述 膜形成用、组成物而形成之膜，彳有效地提高絕緣膜之形狀 穩定性。作為如上所述之電子機器之絕緣膜的示例，可列 舉例如，液晶顯示元件中用以保護薄膜電晶體（TFT，丁Conf. Rad· Curing ASIA, p478 T〇ky〇, 〇ct (1988) is clearly disclosed). Examples of the counter anion of the onium salt include Bp*·, CF3s〇3_, C4F9S〇3·, c8Fi7S〇3., and cH3S〇3. Further, as a photoacid generator, a chemical substance can also be used as a thermal acid generator. These thermal acid generators may be used singly or in combination of two or more. Preferably, the proportion of the above-mentioned thermal acid generator dongwang (5) 3 is 0.05 to 5 〇 围 相对 相对 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 When the thermal acid generator is not full, 〇5 heavy 巳^ ^^, 里 伤 ¥ ¥, sometimes not enough to produce acid, and when it exceeds 50 parts by weight, it is difficult to uniformly coat 臈 formation With 125692.doc -22- 200830052 composition, the film thickness is not uniform. When the film forming composition is cured to form a cured film, the film forming composition layer formed on the substrate 2 can be subjected to heat treatment without exposing the film forming composition layer in the film forming step. In other words, after the film formation composition layer containing the film formation composition of the present invention is formed on the substrate 2, the film formation composition layer is subjected to heat treatment "by the acid generator (B). The action of the acid hardens the film forming composition layer. (Use of Composition for Film Formation) A film formed using the film formation composition can be used for various purposes. Here, the "film formed using the film-forming composition" is a film obtained by applying an external stimulus such as heat or light to the film-forming composition and introducing the cross-linking structure. The film-forming composition of the present invention can be preferably used for forming a film such as a pattern film in various apparatuses, but the film-forming composition can be preferably used for an insulating film of an electronic device. As the insulating film of the electronic device, the film formed by the above-mentioned film forming composition is used, and the shape stability of the insulating film is effectively improved. As an example of the insulating film of the electronic device as described above, for example, a liquid crystal display element for protecting a thin film transistor (TFT, D

Film Transistor)之TFT保言蒦絕緣膜、以及彩色遽光器中用 以保護濾光片之保護絕緣膜等。 又，本發明之膜形成用組成物可更佳地用於構成半導體 元件之層間絕緣膜或者保護膜。 圖3係模式地表示具傷由本發明之感光性組成物構成之 125692.doc • 23 - 200830052 保護膜以及層間絕緣膜的半導體元件之正視剖面圖。 圖3所示之半導體元件11中，於基板12之上表面中央設 置有閘電極13。以覆蓋閘電極13之方式，於基㈣之上表 面上形成有閘極絕緣膜14。於閘極絕緣膜丨4上設置有源電 極15以及汲電極16。以覆蓋源電極丨5之一部分以及汲電極 16之一部分的方式，於閘極絕緣膜14上形成有半導體層 17。進而，以覆蓋源電極15及汲電極16之未被半導體層17 覆盍之部分以及半導體層17的方式，形成有保護膜18。半 ‘體元件11中，上述閘極絕緣膜14及保護膜18係使用本發 明之膜形成用組成物而形成之膜。 本發明之膜形成用組成物，可用於例如有機EL(ElectroFilm Transistor) is a TFT-protected insulating film and a protective insulating film for protecting a filter in a color chopper. Further, the film-forming composition of the present invention can be more preferably used for forming an interlayer insulating film or a protective film of a semiconductor element. Fig. 3 is a front cross-sectional view schematically showing a semiconductor element having a protective film and an interlayer insulating film, which is composed of a photosensitive composition of the present invention, 125692.doc. 23 - 200830052. In the semiconductor device 11 shown in Fig. 3, a gate electrode 13 is provided at the center of the upper surface of the substrate 12. A gate insulating film 14 is formed on the upper surface of the base (4) so as to cover the gate electrode 13. The active electrode 15 and the ytterbium electrode 16 are provided on the gate insulating film 4. A semiconductor layer 17 is formed on the gate insulating film 14 in such a manner as to cover a portion of the source electrode 丨5 and a portion of the ytterbium electrode 16. Further, a protective film 18 is formed so as to cover the portion of the source electrode 15 and the germanium electrode 16 which are not covered by the semiconductor layer 17 and the semiconductor layer 17. In the half body element 11, the gate insulating film 14 and the protective film 18 are formed by using the film forming composition of the present invention. The film-forming composition of the present invention can be used, for example, in an organic EL (Electro)

Luminescence，電致發光）元件之tft保護膜、 IC(Integrated Circuit，積體電路）晶片之層間保護膜、感測 器之絕緣層等各種電子機器用絕緣保護膜。 以下，藉由列舉本發明之實施例及比較例，可明確本發 明。再者，本發明並非限定於以下實施例者。 首先，準備實施例1〜15及比較例1〜13之感光性組成物。 實施例1〜15及比較例1〜13中，成分（X)係使用苯基三乙氧 矽烷，成分（Y)係使用甲基三乙氧矽烷，成分（z)係使用三 乙氧矽烧。 (實施例1) 準備調配有50莫耳重量％之苯基三乙氧石夕烧、以及5〇莫 耳重量％之甲基三乙氧矽烷的烷氧矽烷組成物。 其後，於附帶冷卻管之1〇〇 ml之燒瓶中，添加26 g所獲 125692.doc •24- 200830052 得之烷氧矽烷組成物、0 06 g草酸、6.7 g水、以及I7g二乙 二醇。使用半圓型機械攪拌器攪拌溶液，利用加熱包於 3〇°C反應6小時。之後，使用蒸發器去除由與水之縮合反 應所生成之乙醇及殘餘的水，獲得烷氧矽烷之縮合物 (A1) 〇 混合100重量份的上述烷氧矽烷之縮合物（A1)以及2重量 份的作為光酸產生劑（B1)之DTS_2〇〇(Midori化學公司製 造），獲得作為膜形成用組成物之感光性組成物。 (實施例2〜8) 除將構成烷氧矽烷組成物之各成分（χ)〜(z)之調配比例 設為下述表4所示的比率以外，以與實施例丨相同之方式， 獲得烷氧矽烷之縮合物（A2)、（A16)〜(A21)。 除使用如此所獲得之各烷氧矽烷之縮合物（A2)、 (A16)〜(A21)以外，以與實施例i相同之方式，獲得感光性 組成物。 (實施例9〜15) 除將構成烷氧矽烷組成物之各成分（χ)〜(ζ)之調配比例 认為下述表4所示的比率以外，以與實施例1相同之方式， 獲得烷氧矽烷之縮合物（Α27)〜(Α33)。 除使用如此所獲得之各烷氧矽烷之縮合物（Α27)〜(Α33) 以外，以與實施例1相同之方式，獲得感光性組成物。 (比較例1〜13) 除將構成烷氧矽烷組成物之各成分（χ)〜(ζ)之調配比例 没為下述表4所示的比率以外，以與實施例丨相同之方式， 125692.doc -25- 200830052 獲得烷氧矽烷之縮合物（A3)〜(A 1 5)。 除使用如此所獲得之烷氧矽烷之縮合物（A3)〜(A1 5)以 外，以與實施例1相同之方式，獲得感光性組成物。 [表4] 烷氧矽 烧之縮 合物 成分(X) 苯基三 乙氧矽烷 (莫耳重量％) 成分⑺ 甲基三 乙氧矽烷 (莫耳重量％) 成分(Z) 三乙氧石夕烧 (莫耳重量％) 實施例1 A1 50 50 - 實施例2 A2 25 75 - 實施例3 A16 10 90 - 實施例4 A17 62.5 37.5 - 實施例5 A18 37.5 50 12.5 實施例6 A19 37.5 56.25 6.25 實施例7 A20 50 43.75 6.25 實施例8 A21 25 68.2 6.8 實施例9 A27 5 95 - 實施例10 A28 1 99 - 實施例11 A29 12.5 75 12.5 實施例12 A30 25 62.5 12.5 實施例13 A31 20 80 - 實施例14 A32 20 73.75 6.25 實施例15 A33 20 67.5 12.5 比較例1 A3 100 - - 比較例2 A4 75 25 比較例3 A5 75 - 25 125692.doc -26- 200830052 比較例4 Α6 50 25 25 比較例5 Α7 50 - --------------- 50 比較例6 Α8 25 50 ---—^. 25 比較例7 Α9 25 25 50~^ 比較例8 Α10 25 - 75 比較例9 All - 100 ~~' ~~---—— 比較例10 A12 - 75 一 ~~~~^ 25 比較例11 A13 - 50 50 ^ 比較例12 A14 - 25 75 ~^ 比較例13 A15 - - 100~ 又，圖4表示描繪烷氧矽烷組成物的各成分（X)〜(Z)的調 配比例的三成分圖，上述烧氧石夕烧組成物的各成分 (X)〜(Z)用於構成實施例1〜15及比較例1〜13中所使用之燒 氧矽烷之縮合物（A1)〜(A21)、（A27)〜(A33)。Luminescence (electroluminescence) element tft protective film, IC (Integrated Circuit) wafer interlayer protective film, sensor insulation layer and other insulating protective films for electronic equipment. Hereinafter, the present invention will be clarified by exemplifying the examples and comparative examples of the present invention. Furthermore, the invention is not limited to the following examples. First, the photosensitive compositions of Examples 1 to 15 and Comparative Examples 1 to 13 were prepared. In Examples 1 to 15 and Comparative Examples 1 to 13, phenyltriethoxysilane was used as the component (X), methyltriethoxysilane was used as the component (Y), and triethoxy oxime was used as the component (z). . (Example 1) An alkoxydecane composition having 50 mol% of phenyltriethoxylate and 5 mol% of methyltriethoxydecane was prepared. Thereafter, in a 1 ml flask equipped with a cooling tube, 26 g of the obtained alkoxysilane composition of 125692.doc •24-200830052, 0 06 g of oxalic acid, 6.7 g of water, and I7g of diethylene were added. alcohol. The solution was stirred using a semicircular mechanical stirrer, and reacted at 3 ° C for 6 hours using a heating pack. Thereafter, the ethanol and the residual water generated by the condensation reaction with water are removed using an evaporator to obtain a condensate of the alkoxydecane (A1), 100 parts by weight of the above condensate of the alkoxydecane (A1), and 2 parts by weight. A DTS 2 oxime (manufactured by Midori Chemical Co., Ltd.) as a photoacid generator (B1) was obtained, and a photosensitive composition as a film-forming composition was obtained. (Examples 2 to 8) The same procedure as in Example 丨 was carried out except that the blending ratio of each component (χ) to (z) constituting the alkoxydecane composition was set to the ratio shown in Table 4 below. Alkoxysilane condensate (A2), (A16) to (A21). A photosensitive composition was obtained in the same manner as in Example i except that the condensates (A2) and (A16) to (A21) of the alkoxy oxane thus obtained were used. (Examples 9 to 15) In the same manner as in Example 1, except that the ratio of each component (χ) to (ζ) constituting the alkoxysilane composition was considered to be the ratio shown in Table 4 below. Alkoxysilane condensate (Α27)~(Α33). A photosensitive composition was obtained in the same manner as in Example 1 except that the condensates (Α27) to (Α33) of the respective alkoxysilanes thus obtained were used. (Comparative Examples 1 to 13) In the same manner as in Example 除 except that the ratio of the components (χ) to (ζ) constituting the alkoxysilane composition was not the ratio shown in Table 4 below, 125692 .doc -25- 200830052 Obtain a condensate of alkoxy decane (A3) ~ (A 1 5). A photosensitive composition was obtained in the same manner as in Example 1 except that the alkoxysilane condensates (A3) to (A1 5) thus obtained were used. [Table 4] Alkoxylated condensate component (X) Phenyltriethoxy decane (mol% by weight) Component (7) Methyltriethoxy decane (mol%) Component (Z) Triethoxylate Burning (mol% by weight) Example 1 A1 50 50 - Example 2 A2 25 75 - Example 3 A16 10 90 - Example 4 A17 62.5 37.5 - Example 5 A18 37.5 50 12.5 Example 6 A19 37.5 56.25 6.25 Implementation Example 7 A20 50 43.75 6.25 Example 8 A21 25 68.2 6.8 Example 9 A27 5 95 - Example 10 A28 1 99 - Example 11 A29 12.5 75 12.5 Example 12 A30 25 62.5 12.5 Example 13 A31 20 80 - Example 14 A32 20 73.75 6.25 Example 15 A33 20 67.5 12.5 Comparative Example 1 A3 100 - - Comparative Example 2 A4 75 25 Comparative Example 3 A5 75 - 25 125692.doc -26- 200830052 Comparative Example 4 Α6 50 25 25 Comparative Example 5 Α7 50 - --------------- 50 Comparative Example 6 Α8 25 50 ---—^. 25 Comparative Example 7 Α9 25 25 50~^ Comparative Example 8 Α10 25 - 75 Comparative Example 9 All - 100 ~~' ~~---- Comparative Example 10 A12 - 75 One~~~~^ 25 Comparative Example 11 A13 - 50 50 ^ Comparative Example 12 A14 - 25 75 ~^ Comparative Example 13 A15 - - 100 ~ Again, the picture 4 is a three-component diagram showing the blending ratio of each component (X) to (Z) of the alkoxysilane composition, and each component (X) to (Z) of the above-described calcined stone composition is used to constitute Example 1. The condensates (A1) to (A21) and (A27) to (A33) of the oxyalkylene oxide used in -15 and Comparative Examples 1 to 13.

(實施例1〜15及比較例1〜13之感光性組成物之評估） 以下，對實施例1〜15及比較例1〜13之各感光性組成物之 儲存穩定性、顯影性及絕緣性能進行評估。 (1)儲存穩定性之評估 首先，測定剛配製之各感光性組成物、亦即剛合成時之 烷氧矽烷之縮合物的經聚苯乙烯換算的重量平均分子量。 ?次，測定將各感光性組成物於_20。。冷凍保存7天後之烷 虱矽烷之縮合物的經聚苯乙烯換算的重量平均分子量。疋 量二天後之重量平均分子量較剛合成時之"平：分子 :下二1·5倍以下之情形設為「。」，將超過Μ倍且為2倍 月形設為「△」，將超過2倍之情形設為「X」，來對 125692.doc -27- 200830052 儲存穩定性進行評估。又，將7天後膠化之情形設為 「X」，來對儲存穩定性進行評估。 下述表5表示結果。 [表5] 烧氧石夕 烷之縮 合物 剛合成時之 重量平均分 子量Mwl 7天後之重 量平均分 子量Mw2 Mw2/Mwl 評估結果 實施例1 A1 835 1149 1.38 〇 實施例2 A2 957 1799 1.88 Δ 實施例3 A16 1090 2018 1.85 Δ 實施例4 A17 757 1021 1.35 〇 實施例5 A18 1276 2449 1.92 Δ 實施例6 A19 987 1441 1.46 〇 實施例7 A20 892 1266 1.42 〇 實施例8 A21 1103 2083 1.89 Δ 實施例9 A27 1065 2004 1.88 Δ 實施例10 A28 1095 1978 1.81 Δ 實施例11 A29 1324 2415 L82 Δ 實施例12 A30 1213 2114 1.74 Δ 實施例13 A31 1010 1879 1.86 Δ 實施例14 A32 1184 2190 1.85 Δ 實施例15 A33 1267 2243 1.77 Δ 比較例1 A3 617 829 1.34 〇 比較例2 A4 723 918 1.27 〇 比較例3 A5 883 1148 1.30 〇 比較例4 A6 1116 1874 1.68 Δ 125692.doc -28 - 200830052(Evaluation of Photosensitive Compositions of Examples 1 to 15 and Comparative Examples 1 to 13) The storage stability, developability, and insulating properties of the photosensitive compositions of Examples 1 to 15 and Comparative Examples 1 to 13 were as follows. to evaluate. (1) Evaluation of storage stability First, the polystyrene-equivalent weight average molecular weight of each of the photosensitive compositions immediately prepared, that is, the alkoxysilane condensate immediately after the synthesis, was measured. Then, each photosensitive composition was measured at -20. . The polystyrene-equivalent weight average molecular weight of the condensate of the alkyl decane after 7 days of storage. The weight average molecular weight after two days of sputum is set to "." in the case of "single: numerator: the next two 1-5 times or less, and it is more than Μ and the double-shaped moon is set to "△". The storage stability of 125692.doc -27- 200830052 was evaluated by setting "more than 2 times" to "X". Further, the case of gelation after 7 days was set to "X" to evaluate the storage stability. Table 5 below shows the results. [Table 5] Weight average molecular weight of the oxysulfan oxide condensate just after synthesis Mwl Weight average molecular weight after 7 days Mw2 Mw2/Mwl Evaluation result Example 1 A1 835 1149 1.38 〇 Example 2 A2 957 1799 1.88 Δ Implementation Example 3 A16 1090 2018 1.85 Δ Example 4 A17 757 1021 1.35 〇 Example 5 A18 1276 2449 1.92 Δ Example 6 A19 987 1441 1.46 〇 Example 7 A20 892 1266 1.42 〇 Example 8 A21 1103 2083 1.89 Δ Example 9 A27 1065 2004 1.88 Δ Example 10 A28 1095 1978 1.81 Δ Example 11 A29 1324 2415 L82 Δ Example 12 A30 1213 2114 1.74 Δ Example 13 A31 1010 1879 1.86 Δ Example 14 A32 1184 2190 1.85 Δ Example 15 A33 1267 2243 1.77 Δ Comparative Example 1 A3 617 829 1.34 〇Comparative Example 2 A4 723 918 1.27 〇Comparative Example 3 A5 883 1148 1.30 〇Comparative Example 4 A6 1116 1874 1.68 Δ 125692.doc -28 - 200830052

比較例5 A7 1329 2213 1.67 Δ 比較例6 A8 1717 3880 2.26 X 比較例7 A9 2135 9394 4.40 X 比較例8 A10 2695 膠化 - X 比較例9 All 1217 5414 4.45 X 比較例10 A12 1808 膠化 - X 比較例11 A13 2871 膠化 - X 比較例12 A14 4236 膠化 - X 比較例13 A15 7009 朦化 - X 又，圖5表示於描緣有圖4所示之烧氧石夕烧組成物之各調 配成分（X)〜(Z)的調配比例的三成分圖中描繪儲存穩定性 的評估結果的圖。於由圖5之虛線Q包圍之區域内，儲存穩 定性之評估結果為「〇」或「Δ」。 (2)顯影性之評估 使用石夕晶圓基板，將各感光性組成物以旋轉數12 5 0 rpm 於該基板上旋塗20秒。塗敷後，利用100°C之加熱板乾燥2 分鐘，形成塗膜。 其次，經由具有特定圖案之光罩，使用紫外線照射裝 置，以照射能量為500 mJ/cm2之方式，以100 mW/cm2之紫 外線照度，對塗膜照射0.5秒之波長為365 nm之紫外線。 照射紫外線後，利用l〇〇°C之加熱板，對塗膜加熱2分鐘。 其後，將塗膜浸潰於四甲基氫氧化銨為2.38%之水溶液中 進行顯影。 觀察顯影時之未曝光部之感光性組成物有無溶解、以及 其圖案化的析像度。將未曝光部溶解且圖案化之析像度為 125692.doc -29- 200830052 1 5 μπι以下之情形設為「ο」，將未曝光部溶解且圖案化之 析像度超過1 5 μιη之情形設為「Δ」，將未曝光部未溶解而 產生殘渣之情形設為「X」，來對顯影性進行評估。 下述表6表示結果。 [表6] 烷氧矽烷之縮合物 有無溶解 析像度(μηι) 評估結果 實施例1 Α1 溶解 10 〇 實施例2 Α2 溶解 8 〇 實施例3 Α16 溶解 6 〇 實施例4 Α17 溶解 10 〇 實施例5 Α18 溶解 8 〇 實施例6 Α19 溶解 8 〇 實施例7 Α20 溶解 9 〇 實施例8 Α21 溶解 8 〇 實施例9 Α27 溶解 7 〇 實施例10 Α28 溶解 6 〇 實施例11 Α29 溶解 7 〇 實施例12 Α30 溶解 8 〇 實施例13 Α31 溶解 7 0 實施例14 Α32 - 溶解 7 〇 實施例15 Α33 溶解 7 〇 比較例1 A3 溶解 15 〇 比較例2 Α4 溶解 15 〇 125692.doc -30- 200830052 比較例3 A5 溶解 10 〇 比較例4 A6 溶解 10 〇 比較例5 A7 溶解 9 〇 比較例6 A8 溶解 8 〇 比較例7 A9 溶解 7 〇 比較例8 A10 溶解 6 〇 比較例9 All 產生殘渣 7 X 比較例10 A12 溶解 7 〇 比較例11 A13 溶解 7 〇 比較例12 A14 溶解 6 〇 比較例13 A15 溶解 5 〇 又，圖6表示於描繪有圖4所示之烧氧石夕烧組成物之各調 配成分（X)〜(Z)的調配比例的三成分圖中描繪顯影性的評 估結果的圖。於由圖6之虛線R包圍之區域内，顯影性之評 估結果為「〇」或「Δ」。 (3)絕緣性能之評估 使用表層上蒸鍍有鋁之玻璃基板，將各感光性組成物以 旋轉數1250 rpm於該玻璃基板上旋塗20秒。塗敷後，利用 100°C之加熱板乾燥2分鐘，形成塗膜。 其次，使用紫外線照射裝置，以照射能量為500 mJ/cm2 之方式，以100 mW/cm2之紫外線照度，對塗膜照射0.5秒 之波長為365 nm之紫外線。照射紫外線後，利用100°C之 加熱板，加熱2分鐘，進而，利用2 0 0 °C之加熱板，加熱6 0 125692.doc -31 - 200830052 分鐘。之後，再次於塗膜上蒸鍍鋁。 測定於已硬化之感光性組成物層中對已蒸鍍之鋁間施加 3 MV/cm之電壓時的洩漏電流。將洩漏電流為l〇xl(T7 A/cm2以下之情形設為「◎」，將超過1〇χ1〇-7 A/cm2且為 15xl(T7 A/cm2以下之情形設為「〇」，將超過15xl0·7 A/cm2 ^ 且為25x1 (T7 A/cm2以下之情形設為「Δ」，將超過25χ1(Γ7 、 A/cm2之情形設為「X」，來對絕緣性能進行評估。 下述表7表示結果。 [表7] 烷氧矽烷之縮合物 >'曳漏電流A/cm2 評估結果 實施例1 A1 24x10-7 Δ 實施例2 A2 14xl〇-7 〇 實施例3 A16 6.2xl0'7 ◎ 實施例4 A17 25 xlO·7 Δ 實施例5 A18 2〇xlO'7 Δ 實施例6 A19 18xl(T7 Δ 實施例7 A20 25xl〇·7 Δ 實施例8 A21 14xl〇·7 〇 實施例9 A27 4xl0'7 ◎ 實施例10 A28 3xl0'7 ◎ 實施例11 A29 6xl0·7 ◎ 實施例12 A30 14xl0·7 〇 實施例13 A31 9x1 (T7 ◎ 實施例14 A32 8xl0'7 ◎ 實施例15 A33 9xl0'7 ◎ 125692.doc -32- 200830052 比較例1 A3 715xl0·7 X 比較例2 A4 91xl〇·7 X 比較例3 A5 127xl0'7 X 比較例4 A6 29χ10·7 X 比較例5 A7 34x1 (Γ7 X 比較例6 A8 17xl0·7 Δ 比較例7 A9 17x1 Ο·7 Δ 比較例8 A10 19χ1(Γ7 Δ 比較例9 All 2x10"7 ◎ 比較例10 A12 2χ10·7 ◎ 比較例11 A13 3χ10·7 ◎ 比較例12 A14 3χ10·7 ◎ 比較例13 A15 3χ1〇·7 ◎ 又’圖7表示於描繪有圖4所示之烷氧矽烷組成物之各調 配成分（X)〜(Z)的調配比例的三成分圖中描繪絕緣性能的Comparative Example 5 A7 1329 2213 1.67 Δ Comparative Example 6 A8 1717 3880 2.26 X Comparative Example 7 A9 2135 9394 4.40 X Comparative Example 8 A10 2695 Gelation - X Comparative Example 9 All 1217 5414 4.45 X Comparative Example 10 A12 1808 Gelation - X Comparative Example 11 A13 2871 Gelation - X Comparative Example 12 A14 4236 Gelation - X Comparative Example 13 A15 7009 Deuteration - X Further, Fig. 5 shows that each of the compositions of the pyrotechnic composition shown in Fig. 4 was drawn. A graph showing the evaluation results of storage stability in the three-component diagram of the blending ratio of the components (X) to (Z). In the region surrounded by the broken line Q of Fig. 5, the evaluation result of the storage stability is "〇" or "Δ". (2) Evaluation of developability Using a Shihwa wafer substrate, each photosensitive composition was spin-coated on the substrate at a number of revolutions of 12 5 rpm for 20 seconds. After coating, it was dried by a hot plate at 100 ° C for 2 minutes to form a coating film. Next, the coating film was irradiated with ultraviolet rays having a wavelength of 365 nm at a wavelength of 500 mW/cm 2 by irradiation with an ultraviolet ray having a specific pattern by an ultraviolet ray irradiation device at an irradiation energy of 500 mJ/cm 2 . After the ultraviolet ray was irradiated, the coating film was heated for 2 minutes using a heating plate of 10 ° C. Thereafter, the coating film was immersed in an aqueous solution of tetramethylammonium hydroxide (2.38%) for development. The presence or absence of dissolution of the photosensitive composition in the unexposed portion at the time of development and the degree of resolution of the patterning were observed. The resolution in which the unexposed portion is dissolved and patterned is 125692.doc -29-200830052 1 5 μπι or less is set to "ο", and the unexposed portion is dissolved and the resolution of the pattern is more than 15 μm. When the amount of residue was not dissolved in the unexposed portion and the residue was formed as "X", the developability was evaluated. Table 6 below shows the results. [Table 6] Whether or not the alkoxysilane condensate has a dissolution resolution (μηι) Evaluation Results Example 1 Α1 Dissolution 10 〇 Example 2 Α 2 Dissolution 8 〇 Example 3 Α 16 Dissolution 6 〇 Example 4 Α 17 Dissolution 10 〇 Example 5 Α18 Dissolution 8 〇Example 6 Α19 Dissolution 8 〇Example 7 Α20 Dissolution 9 〇Example 8 Α21 Dissolution 8 〇Example 9 Α27 Dissolution 7 〇Example 10 Α28 Dissolution 6 〇Example 11 Α29 Dissolution 7 〇Example 12 Α30 Dissolution 8 〇 Example 13 Α31 Dissolution 7 0 Example 14 Α32 - Dissolution 7 〇Example 15 Α33 Dissolution 7 〇Comparative Example 1 A3 Dissolution 15 〇Comparative Example 2 Α4 Dissolution 15 〇125692.doc -30- 200830052 Comparative Example 3 A5 Dissolved 10 〇 Comparative Example 4 A6 Dissolved 10 〇 Comparative Example 5 A7 Dissolved 9 〇 Comparative Example 6 A8 Dissolved 8 〇 Comparative Example 7 A9 Dissolved 7 〇 Comparative Example 8 A10 Dissolved 6 〇 Comparative Example 9 All Residue 7 X Comparative Example 10 A12 Dissolved 7 〇 Comparative Example 11 A13 Dissolved 7 〇 Comparative Example 12 A14 Dissolved 6 〇 Comparative Example 13 A15 Dissolved 5 〇 Again, Figure 6 shows the burned oxygen stone group shown in Figure 4. Each component was adjusted with the (X) ~ (Z) of the three-component mixing proportion of the figures depicting the results of evaluation of developability. In the region surrounded by the broken line R of Fig. 6, the evaluation result of the developability is "〇" or "Δ". (3) Evaluation of insulating properties A glass substrate on which aluminum was vapor-deposited on the surface layer was used, and each photosensitive composition was spin-coated on the glass substrate at a number of revolutions of 1,250 rpm for 20 seconds. After coating, it was dried by a hot plate at 100 ° C for 2 minutes to form a coating film. Next, the coating film was irradiated with ultraviolet rays having a wavelength of 365 nm for 0.5 second at an irradiation intensity of 500 mJ/cm 2 using an ultraviolet irradiation device at a wavelength of 500 mJ/cm 2 . After the ultraviolet ray was irradiated, the mixture was heated for 2 minutes using a hot plate at 100 ° C, and further heated at 60 ° C for 30 ° 692 692 - doc - 31 - 200830052 minutes. Thereafter, aluminum was again evaporated on the coating film. A leakage current when a voltage of 3 MV/cm was applied between the vapor-deposited aluminum in the cured photosensitive composition layer was measured. The leakage current is l〇xl (the case of T7 A/cm2 or less is set to "◎", and it is more than 1〇χ1〇-7 A/cm2 and is 15xl (when T7 A/cm2 or less is set to "〇", More than 15xl0·7 A/cm2 ^ and 25x1 (when T7 A/cm2 or less is set to "Δ", it will exceed 25χ1 (Γ7, A/cm2 is set to "X") to evaluate the insulation performance. The results are shown in Table 7. [Table 7] Alkoxysilane condensate > 'Leakage current A/cm2 Evaluation result Example 1 A1 24x10-7 Δ Example 2 A2 14xl〇-7 〇 Example 3 A16 6.2xl0 '7 ◎ Example 4 A17 25 xlO·7 Δ Example 5 A18 2〇xlO'7 Δ Example 6 A19 18xl (T7 Δ Example 7 A20 25xl〇·7 Δ Example 8 A21 14xl〇·7 〇Example 9 A27 4xl0'7 ◎ Example 10 A28 3xl0'7 ◎ Example 11 A29 6xl0·7 ◎ Example 12 A30 14xl0·7 〇 Example 13 A31 9x1 (T7 ◎ Example 14 A32 8x10'7 ◎ Example 15 A33 9xl0'7 ◎ 125692.doc -32- 200830052 Comparative Example 1 A3 715xl0·7 X Comparative Example 2 A4 91xl〇·7 X Comparative Example 3 A5 127xl0'7 X Comparative Example 4 A6 29χ10·7 X Comparative Example 5 A7 34x1 ( Γ7 X ratio Example 6 A8 17xl0·7 Δ Comparative Example 7 A9 17x1 Ο·7 Δ Comparative Example 8 A10 19χ1 (Γ7 Δ Comparative Example 9 All 2x10"7 ◎ Comparative Example 10 A12 2χ10·7 ◎ Comparative Example 11 A13 3χ10·7 ◎ Comparative Example 12 A14 3χ10·7 ◎ Comparative Example 13 A15 3χ1〇·7 ◎ Further, Fig. 7 shows three components in which the blending ratios (X) to (Z) of the alkoxydecane composition shown in Fig. 4 are plotted. The figure depicts the insulation properties

評估結果的圖。於由圖7之虛線s包圍之區域内，絕緣性能 之評估結果為「◎」、r 〇」或「△」。 如圖5〜圖7所示’儲存穩定性、顯影性及絕緣性能 估結果均為「◎」、「。」或「△」之區域係圖i所示的由二 :圍：η?。又，儲存穩定性及顯影性之評估結果均 之區二J、且絕緣性能之評估結果為「@」或「。 :域係圖8所示的由實線p2包圍的區域。進而 」 顯影性之評估結果均為「。」《「△且⑺穩 之評估結果為「◎」 一」 < 緣性能 區域。 °。或係圖9所示的由實線P3包圍的 125692.doc -33 - 200830052 (實施例16) 代替2重量份之作為光酸產生劑（B1)之DTS-200(Midori 化學公司製造），使用0.5重量份之作為光酸產生劑（B2)之 NAI-105(Midori化學公司製造），除此以外，以與實施例6 相同之方式，獲得感光性組成物。 * (實施例1 6之感光性組成物之評估） ^ 以下，關於實施例16之感光性組成物，以與上述實施例 1〜15及比較例1〜13相同之方式，對（1)儲存穩定性、（2)顯 f 影性以及（3)絕緣性能進行評估。 下述表8表示結果。 [表8] 儲 存 穩 定 性 烷氧矽 烧之縮 合物 剛合成時之 重量平均分 子量Mwl 7天後之 重量平均 分子量 Mw2 Mw2/Mwl 評估結果 實施 例16 A19 987 1441 1.46 〇 顯 影 性 烷氧矽 烧之縮 合物 有無溶解 析像度 (μηι) 評估結果 / 實施 例16 A19 溶解 3 〇 絕 緣 性 能 烷氧矽 烧之縮 合物 泡漏電流 A/cm2 評估結果 / 實施 例16 A19 13χ10-7 〇 125692.doc -34- 200830052 (實施例17〜21) 實施例17〜21中，成分（X)係使用苯基三曱氧矽烷，成分 (Y)係使用甲基三甲氧矽烷，成分（Z)係使用三甲氧矽烷。 除將構成烷氧矽烷組成物之各成分（X)〜(Z)之調配比例 設為下述表9所示的比率以外，以與實施例1相同之方式， 獲得烷氧矽烷之縮合物（A22)〜(A26)。 除使用如此所獲得之烷氧矽烷之縮合物（A22)〜(A26)以 外，以與實施例1相同之方式，獲得感光性組成物。 [表9] 烷氧矽 烷之縮 合物 成分(X) 苯基三 乙氧矽烷 (莫耳重量％) 成分(Y) 甲基三 乙氧矽烷 (莫耳重量％) 成分(Z) 三甲氧矽烷 (莫耳重量％) 實施例17 A22 10 90 - 實施例18 A23 62.5 37.5 - 實施例19 A24 37.5 50 12.5 實施例20 A25 50 43.75 6.25 實施例21 A26 25 68.2 6.8 (實施例17〜21之感光性組成物之評估） 以下，關於實施例17〜21之各感光性組成物，以與上述 實施例1〜15及比較例1〜13相同之方式，對（1)儲存穩定 性、（2)顯影性以及（3)絕緣性能進行評估。 下述表10表示結果。 125692.doc -35- 200830052 [表 ι〇] 儲 存 穩 定 性 烷氧矽 烧之縮 合物 剛合成時 之重量平 均分子量 Mwl 7天後之重 量平均分 子量Mw2 Mw2/Mw 1 評估結果 實施例17 A22 1371 2632 1.92 Δ 實施例18 A23 890 1267 1.42 〇 實施例19 A24 1460 2840 1.95 Δ 實施例20 A25 953 1444 1.52 Δ 實施例21 A26 1132 2241 1.98 Δ 顯 影 性 烷氧矽 烧之縮 合物 有無溶解 析像度 (μηι) 評估結果 實施例17 A22 溶解 7 〇 實施例18 A23 溶解 10 〇 實施例19 A24 溶解 8 〇 實施例20 A25 溶解 8 〇 實施例21 A26 溶解 8 〇 絕 緣 性 能 烷氧矽 院之縮 合物 洩漏電流 A/cm2 評估結果 / 實施例17 A22 4.5χ10'7 ◎ 實施例18 A23 2〇xl 0'7 Δ 實施例19 A24 18χ10'7 Δ 實施例20 A25 21xl〇·7 Δ 實施例21 A26 llxlO·7 〇 125692.doc -36- 200830052 (實施例22) 混合100重量份的實施例1中所獲得之烷氧矽烷之縮合物 (A1)、以及1重量份的作為熱酸產生劑之ρΑΙ_ l〇l(Midori化學公司製造），而獲得臈形成用組成物。 (實施例23〜36及比較例14〜26) 代替100重量份之實施例1中所獲得的烷氧矽烷之縮合物 (A1)，而使用1〇〇重量份之下述表丨丨所示的案施例2〜15及 比較例1〜13中所獲得的烷氧矽烷之縮合物（A2)〜(A21)、 (A27)〜(A33)中的任一個，除此以外，以與實施例22相同 之方式，獲得膜形成用組成物。 (實施例22〜36及比較例14〜26之膜形成用組成物之評估） 使用表層上蒸鍍有銘之玻璃基板，料膜形成用組成物 以旋轉數1250 rpm於該玻璃基板上旋塗2〇秒。塗敷後，利 用100 °C之加熱板加熱2分鐘，形成塗膜。 其次，利用2GG°C之加熱板加熱6G分鐘，使膜形成用組 成物硬化。之後，再次於塗膜上蒸鍍鋁。 測疋於已硬化之膜形成用組成物層中對已蒸鍍之鋁間施 加3 MV/em之電壓時的茂漏電流，且以與上述實施例μ 及比較例1〜13相同之方式，對（3)絕緣性能進行評估。 下述表11表示結果。 125692.doc -37- 200830052 [表 ii] 烷氧矽烷之縮合物 洩漏電流A/cm2 評估結果 實施例22 A1 22x10'7 Δ 實施例23 A2 14xl〇-7 〇 實施例24 A16 7xl〇·7 ◎ 實施例25 A17 22x10-7 Δ 實施例26 A18 18xl0'7 Δ 實施例27 A19 16X10-7 Δ 實施例28 A20 25xl0'7 Δ 實施例29 A21 13X10'7 〇 實施例30 A27 4χ10'7 ◎ 實施例31 A28 3χ10·7 ◎ 實施例32 A29 5χ1(Τ7 ◎ 實施例33 A30 14χ10·7 〇 實施例34 A31 9x1 (Τ7 ◎ 實施例35 A32 9χ10·7 ◎ 實施例36 A33 8χ10_7 ◎ 比較例14 A3 826χ1〇·7 X 比較例15 A4 9〇χ10'7 X 比較例16 A5 135χ10'7 X 比較例17 A6 33 χΙΟ·7 X 比較例18 A7 37χ10'7 X 比較例19 A8 16x10'7 Δ 比較例20 A9 17χ10·7 Δ 比較例21 A10 18χ1〇·7 Δ 比較例22 All 2χ10'7 ◎ 125692.doc -38- 200830052A diagram of the results of the assessment. In the region surrounded by the broken line s of Fig. 7, the evaluation result of the insulation performance is "?", r?" or "?". As shown in Fig. 5 to Fig. 7, the areas where the storage stability, developability, and insulation performance evaluation results are "◎", ".", or "△" are shown by the following two: η?. In addition, the evaluation results of the storage stability and the developability are both in the second section, and the evaluation result of the insulation performance is "@" or ".: the region is surrounded by the solid line p2 shown in Fig. 8. Further" developability The evaluation results are all "." ""△ and (7) stable evaluation result is "◎" one" < edge performance area. °. Or, as shown in FIG. 9, 125692.doc -33 - 200830052 (Example 16) surrounded by a solid line P3, instead of 2 parts by weight of DTS-200 (manufactured by Midori Chemical Co., Ltd.) as a photoacid generator (B1), is used. A photosensitive composition was obtained in the same manner as in Example 6 except that 0.5 parts by weight of NAI-105 (manufactured by Midori Chemical Co., Ltd.) as a photoacid generator (B2) was used. (Evaluation of the photosensitive composition of Example 16) ^ The photosensitive composition of Example 16 was stored in (1) in the same manner as in the above Examples 1 to 15 and Comparative Examples 1 to 13 in the following. Stability, (2) visible shadow and (3) insulation performance were evaluated. Table 8 below shows the results. [Table 8] Storage stability Alkoxylated condensate condensate just after weight average molecular weight Mwl Weight average molecular weight after 7 days Mw2 Mw2/Mwl Evaluation result Example 16 A19 987 1441 1.46 〇 developable alkoxy oxime Whether or not the condensate has a dissolution resolution (μηι) Evaluation result / Example 16 A19 Dissolution 3 〇Insulation property Alkoxypyrene condensate bubble leakage current A/cm2 Evaluation result / Example 16 A19 13χ10-7 〇125692.doc - 34-200830052 (Examples 17 to 21) In Examples 17 to 21, the component (X) was phenyl trioxoxane, the component (Y) was methyltrimethoxysilane, and the component (Z) was trimethoxy. Decane. A condensate of alkoxy decane was obtained in the same manner as in Example 1 except that the ratio of the components (X) to (Z) constituting the alkoxysilane composition was a ratio shown in the following Table 9. A22) ~ (A26). A photosensitive composition was obtained in the same manner as in Example 1 except that the alkoxysilane condensates (A22) to (A26) thus obtained were used. [Table 9] Alkoxysilane condensate component (X) Phenyltriethoxy decane (mol% by weight) Component (Y) Methyltriethoxy decane (mol% by weight) Component (Z) Trimethoxy decane ( Molar wt%) Example 17 A22 10 90 - Example 18 A23 62.5 37.5 - Example 19 A24 37.5 50 12.5 Example 20 A25 50 43.75 6.25 Example 21 A26 25 68.2 6.8 (Photosensitive composition of Examples 17 to 21) Evaluation of the materials (1) Storage stability and (2) developability of each of the photosensitive compositions of Examples 17 to 21 in the same manner as in the above Examples 1 to 15 and Comparative Examples 1 to 13. And (3) evaluation of insulation properties. Table 10 below shows the results. 125692.doc -35- 200830052 [Table 〇] Storage stability Alkoxylated condensate weight average molecular weight Mwl just after synthesis Weight average molecular weight after 7 days Mw2 Mw2/Mw 1 Evaluation results Example 17 A22 1371 2632 1.92 Δ Example 18 A23 890 1267 1.42 〇 Example 19 A24 1460 2840 1.95 Δ Example 20 A25 953 1444 1.52 Δ Example 21 A26 1132 2241 1.98 Δ Developable alkoxylated condensate with or without dissolution resolution (μηι Evaluation Results Example 17 A22 Dissolution 7 〇 Example 18 A23 Dissolution 10 〇 Example 19 A24 Dissolution 8 〇 Example 20 A25 Dissolution 8 〇 Example 21 A26 Dissolution 8 〇Insulation Properties Alkoxy oxime condensate leakage current A /cm2 Evaluation Results / Example 17 A22 4.5χ10'7 ◎ Example 18 A23 2〇xl 0'7 Δ Example 19 A24 18χ10'7 Δ Example 20 A25 21xl〇·7 Δ Example 21 A26 llxlO·7 〇 125692.doc -36- 200830052 (Example 22) 100 parts by weight of the condensate (A1) of the alkoxydecane obtained in Example 1, and 1 part by weight of ρΑΙ as a thermal acid generator were mixed. L〇l (manufactured by Midori Chemical Co., Ltd.) to obtain a composition for forming a ruthenium. (Examples 23 to 36 and Comparative Examples 14 to 26) Instead of 100 parts by weight of the alkoxysilane condensate (A1) obtained in Example 1, the following formula is used in an amount of 1 part by weight. Any of the condensates (A2) to (A21) and (A27) to (A33) of the alkoxydecane obtained in Examples 2 to 15 and Comparative Examples 1 to 13, except for In the same manner as in Example 22, a film-forming composition was obtained. (Evaluation of Film Formation Compositions of Examples 22 to 36 and Comparative Examples 14 to 26) A glass substrate having a surface layer deposited thereon was used, and a film forming composition was spin-coated on the glass substrate at a number of revolutions of 1,250 rpm. Leap second. After coating, it was heated by a hot plate at 100 ° C for 2 minutes to form a coating film. Next, the film forming composition was cured by heating with a hot plate of 2 GG °C for 6 G minutes. Thereafter, aluminum was again evaporated on the coating film. The leakage current when a voltage of 3 MV/em was applied between the vapor-deposited aluminum in the hardened film-forming composition layer was measured, and in the same manner as in the above Example μ and Comparative Examples 1 to 13, (3) Evaluation of insulation properties. Table 11 below shows the results. 125692.doc -37- 200830052 [Table ii] Alkoxysilane condensate leakage current A/cm2 Evaluation result Example 22 A1 22x10'7 Δ Example 23 A2 14xl〇-7 〇 Example 24 A16 7xl〇·7 ◎ Example 25 A17 22x10-7 Δ Example 26 A18 18x10'7 Δ Example 27 A19 16X10-7 Δ Example 28 A20 25x10'7 Δ Example 29 A21 13X10'7 〇 Example 30 A27 4χ10'7 ◎ Example 31 A28 3χ10·7 ◎ Example 32 A29 5χ1 (Τ7 ◎ Example 33 A30 14χ10·7 〇 Example 34 A31 9x1 (Τ7 ◎ Example 35 A32 9χ10·7 ◎ Example 36 A33 8χ10_7 ◎ Comparative Example 14 A3 826χ1〇 · 7 X Comparative Example 15 A4 9〇χ10'7 X Comparative Example 16 A5 135χ10'7 X Comparative Example 17 A6 33 χΙΟ·7 X Comparative Example 18 A7 37χ10'7 X Comparative Example 19 A8 16x10'7 Δ Comparative Example 20 A9 17χ10·7 Δ Comparative Example 21 A10 18χ1〇·7 Δ Comparative Example 22 All 2χ10'7 ◎ 125692.doc -38- 200830052

θ係成刀（x) (z)之二成分圖，表示本發明中所使用之 構成燒氧㈣之縮合物⑷以成分（χ)〜(ζ)之調配比例的 、生圖2(a)〜圖2⑷係用以說明使用本發明之感光性組成物製 ^圖案膜之方法中的各步驟的剖面圖。 圖3係表示具備由本發明之感光性組成物構成之保護膜 以及層間絕緣膜的半導體元件的正視剖面圖。 圖4表示描繪烷氧矽烷組成物的各成分（χ)〜(z)的調配比 例的三成分圖，上述烷氧矽烷組成物的各成分（X卜用 於構成實施例及比較例中所使用之烷氧矽烷之縮合物。 圖5係於描繪有圖4所示之烷氧矽烷組成物之各調配成分 (X) (Z)的调配比例的三成分圖中，描繪有儲存穩定性之 評估結果的圖。 圖6係於描繪有圖4所示之烷氧矽烷組成物之各調配成分 (X)〜(Z)的調配比例的三成分圖中，描繪有顯影性之評估 結果的圖。 圖7係於描繪有圖4所示之烷氧矽烷組成物之各調配成分 (X)〜(Z)的調配比例的三成分圖中，描繪有絕緣性能之評 估結果的圖。 125692.doc -39- 200830052 圖8係成分（X)〜(Z)之三成分圖，表示本發明中所使用之 構成烷氧矽烷之縮合物（A)的各成分（X)〜〇的調配比例的 較佳區域。 圖9係成分（X)〜(z)之二成分圖，表示本發明中所使用之 構成烷氧矽烷之縮合物（A)的各成分（χ)〜(z)的調配比例的 更佳區域。 【主要元件符號說明】 1 感光性組成物層 1A 曝光部之感光性組成物層 1B 未曝光部之感光性組成物層 1C 圖案膜 2 基板 3 光罩 11 半導體元件 12 基板 13 閘電極 14 閘極絕緣膜 15 源電極 16 >及電極 17 半導體層 18 保護膜 125692.docThe θ system is a two-component diagram of the knives (x) and (z), and shows that the condensate (4) constituting the sintered oxygen (IV) used in the present invention has a ratio of the components (χ) to (ζ), and the growth diagram 2(a) 2(4) is a cross-sectional view for explaining each step in the method of producing a pattern film using the photosensitive composition of the present invention. Fig. 3 is a front cross-sectional view showing a semiconductor element including a protective film composed of the photosensitive composition of the present invention and an interlayer insulating film. 4 is a three-component diagram showing the blending ratio of each component (χ) to (z) of the alkoxydecane composition, and each component of the alkoxydecane composition (Xb is used in the examples and comparative examples). The condensate of the alkoxy oxane. Fig. 5 is a three-component diagram depicting the blending ratio of each of the compounding components (X) (Z) of the alkoxydecane composition shown in Fig. 4, and the evaluation of storage stability is depicted. Fig. 6 is a diagram showing the results of evaluation of developability in a three-component diagram in which the blending ratios of the respective blending components (X) to (Z) of the alkoxydecane composition shown in Fig. 4 are plotted. Fig. 7 is a graph showing the evaluation results of the insulating properties in a three-component diagram in which the blending ratios of the respective blending components (X) to (Z) of the alkoxydecane composition shown in Fig. 4 are drawn. 125692.doc - 39-200830052 Fig. 8 is a three-component diagram of the components (X) to (Z), and is preferably a blending ratio of each component (X) to hydrazine constituting the alkoxysilane condensate (A) used in the present invention. Fig. 9 is a two component diagram of the components (X) to (z), showing the condensation of the constituent alkoxydecane used in the present invention. A more preferable region of the blending ratio of each component (χ) to (z) of the material (A) [Explanation of main component symbols] 1 Photosensitive composition layer 1A Photosensitive composition layer 1B of exposed portion photosensitive property of unexposed portion Composition layer 1C Pattern film 2 Substrate 3 Photomask 11 Semiconductor element 12 Substrate 13 Gate electrode 14 Gate insulating film 15 Source electrode 16 > Electrode 17 Semiconductor layer 18 Protective film 125692.doc

Claims (1)

200830052 十、申請專利範圍： 1 · 一種膜形成用組成物，其特徵在於包含烷氧石夕烧之縮合 物（A)以及藉由外部刺激而產生酸之酸產生劑（B)，上述 烷氧矽烷之縮合物（A)係將含苯基三乙氧秒烧及/或苯基 二甲氧石夕烧之成分（X)、含甲基三乙氧石夕燒及/或甲基三 甲氧矽烷之成分（Y)與含三乙氧矽燒及/或三甲氧石夕烧之 成分（Z)，以圖1之三成分圖中連接座標八17、a28、A29 及A1 8之實線P1所包圍區域内的比率反應而得。 2_如請求項1之膜形成用組成物，其中上述烷氧矽烷之縮 合物（A)係將上述成分（X)、上述成分（γ)與上述成分（z) 以圖8之二成分圖中連接座標A2、A28、A29及A3 0之實 線P2所包圍區域内的比率反應而得之烷氧矽烷之縮合 物。 3·如請求項1之膜形成用組成物，其中上述烷氧矽烷之縮 合物（A)係將上述成分（X)、上述成分（γ)與上述成分（z) 以圖9之二成分圖中連接座標A3i、A28、A29及A33之實 線P3所包圍區域内的比率反應而得之烷氧矽烷之縮合 物。 4. 一種圖案膜之製造方法，其特徵在於·· 其係使用請求項1至3中任一項之膜形成用組成物者， 上述膜形成用組成物係包含曝光即產生酸之光酸產生 劑作為上述酸產生劑（B)之感光性組成物； 上述製造方法包含以下步驟·· 於基板上形成含上述感光性組成物之感光性組成物 125692.doc 200830052 層； 根據所形成之圖案，使上述感光性組成物層選擇性 地曝光，藉由自上述光酸產生劑所產生之酸之作用，使 曝光部之上述感光性組成物層硬化，使曝光部之上述感 光性組成物層不溶於顯影液；以及 於使曝光部之上述感光性組成物層不溶於顯影液 後，利用顯影液使上述感光性組成物層顯影，去除未曝 光部之上述感光性組成物層。 5. 一種電子機器用絕緣膜，其係使用請求項丨至3中任一項 之膜形成用組成物所形成。 125692.doc200830052 X. Patent application scope: 1 . A composition for forming a film, characterized by comprising an alkoxylate condensate (A) and an acid generator (B) which generates an acid by external stimulation, the alkoxylate The condensate of decane (A) is a component (X) containing phenyl triethoxy sec-second and/or phenyl dimethyl sulphide, containing methyl triethoxylate and/or methyl trimethoxy The component (Y) of decane and the component (Z) containing triethoxy sulphur and/or samarium sulphate are connected to the solid line P1 of coordinates VIII17, a28, A29 and A1 8 in the composition diagram of Fig. 1 The ratio in the enclosed area is obtained by reaction. The composition for forming a film of claim 1, wherein the condensate (A) of the alkoxydecane is a component diagram of the component (X), the component (γ), and the component (z) shown in FIG. The condensate of the alkoxy decane obtained by reacting the ratio in the region surrounded by the solid line P2 of the coordinates A2, A28, A29 and A30. 3. The composition for forming a film according to claim 1, wherein the condensate (A) of the alkoxydecane is a component diagram of the component (X), the component (γ), and the component (z) as shown in FIG. The condensate of the alkoxy oxane obtained by reacting the ratio in the region surrounded by the solid line P3 of the coordinates A3i, A28, A29 and A33. A method of producing a pattern film, comprising: the film forming composition according to any one of claims 1 to 3, wherein the film forming composition comprises photoacid generation which generates an acid upon exposure. a photosensitive composition of the acid generator (B); the method for producing the method comprising the steps of: forming a photosensitive composition 125692.doc 200830052 layer containing the photosensitive composition on a substrate; The photosensitive composition layer is selectively exposed, and the photosensitive composition layer in the exposed portion is cured by the action of an acid generated from the photo-acid generator, so that the photosensitive composition layer in the exposed portion is insoluble. And after the photosensitive composition layer of the exposed portion is insoluble in the developer, the photosensitive composition layer is developed by a developer to remove the photosensitive composition layer in the unexposed portion. An insulating film for an electronic device, which is formed by using the film forming composition according to any one of claims 3 to 3. 125692.doc
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