TW379246B - Electronic coating materials using mixed polymers - Google Patents

Electronic coating materials using mixed polymers Download PDF

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Publication number
TW379246B
TW379246B TW085106559A TW85106559A TW379246B TW 379246 B TW379246 B TW 379246B TW 085106559 A TW085106559 A TW 085106559A TW 85106559 A TW85106559 A TW 85106559A TW 379246 B TW379246 B TW 379246B
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TW
Taiwan
Prior art keywords
coating
weight
substrate
coated
resin
Prior art date
Application number
TW085106559A
Other languages
English (en)
Inventor
Loren Andrew Haluska
Keith Winton Michael
Original Assignee
Dow Corning
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Publication date
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Publication of TW379246B publication Critical patent/TW379246B/zh

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
    • C04B41/5035—Silica
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • C04B41/87—Ceramics
    • 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
    • H01L21/02134—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 the material comprising hydrogen silsesquioxane, e.g. HSQ
    • H—ELECTRICITY
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    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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    • H01L21/02107—Forming insulating materials on a substrate
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    • H01L21/02337—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment treatment by exposure to a gas or vapour
    • H01L21/0234—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment treatment by exposure to a gas or vapour treatment by exposure to a plasma
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    • 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
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    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02296—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer
    • H01L21/02318—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment
    • H01L21/02356—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment treatment to change the morphology of the insulating layer, e.g. transformation of an amorphous layer into a crystalline layer
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    • 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
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/312—Organic layers, e.g. photoresist
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    • 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
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/314—Inorganic layers
    • H01L21/316—Inorganic layers composed of oxides or glassy oxides or oxide based glass
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    • H01—ELECTRIC ELEMENTS
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    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
    • H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
    • H01L23/291—Oxides or nitrides or carbides, e.g. ceramics, glass
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
    • H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
    • H01L23/293—Organic, e.g. plastic
    • H01L23/295—Organic, e.g. plastic containing a filler
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00844—Uses not provided for elsewhere in C04B2111/00 for electronic applications
    • H—ELECTRICITY
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    • 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
    • H01L21/02219—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 nitrogen
    • H01L21/02222—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 nitrogen the compound being a silazane
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    • H01L21/02282—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process liquid deposition, e.g. spin-coating, sol-gel techniques, spray coating
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    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/0001—Technical content checked by a classifier
    • H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
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    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
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    • Y10T428/12861—Group VIII or IB metal-base component
    • Y10T428/12931—Co-, Fe-, or Ni-base components, alternative to each other
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Plasma & Fusion (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Silicon Polymers (AREA)
  • Paints Or Removers (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Formation Of Insulating Films (AREA)

Description

經濟部中央標準局員工消費合作衽印裝 弟^106559號專利申請案 中文說明書修正頁(88年9月） ϋ 五；發明説明（8 ) ' - ? ；
i I '佳之黏附遮土j修改表面之填料或懸浮劑。黏附性増進劑包 括，.例如，如縮水甘油氧基丙基三甲氧基矽烷、硫醇基S 基三曱氧基矽烷、與乙烯基三乙醯氧基矽烷之矽烷。通常 以〇. 1至5重量％之量而使用。懸浮劑可包括，例如，纖維 素、黏土、發煙矽石、硬脂酸鹽等。其以足以懸浮任何填 料之量而使用（例如，丨_25重量％)。這些與其他之视情 形成份對熟悉此技藝者為已知的。 同 依照本發明之方法，H_樹脂、聚矽氮烷、與任何視情 形成份塗布於基材之表面。其以任何方法完成，但是較= 方法涉及溶解或分散H-樹脂、聚矽氮烷、與任何視情形 成份於溶劑中。此混合物然後塗布於基材之表面。各2有 利疋方法，如攪拌及/或加熱，然後可用以溶解或分散物 料及產生更均勻之塗布物料。可使用之溶劑包括任何試劑 或試劑混合物，其溶解或分散H _樹脂與聚矽氮烷以形成 均質液體混合物，而不影響生成之塗層。這些溶劑包括， 例如，如苯或甲苯之芳族烴、如正庚烷或十二烷之烷屬 烴、酮、酯、甘油酯或環形二甲基聚矽氧烷，以足以溶解 /分散以上物料至塗布之所需濃度之量。通常，使用足夠 〜以上溶劑，以形成樹脂之〇丨_ 8 〇重量％混合物，較佳為 I - 5 〇重量％。 此混合物然後藉旋塗、浸塗、喷塗、或流塗而塗覆於基 材表面。然而，其他之同等方式亦視為在本發明之範圍 内。 刎然後自塗層之沉積而生成之被塗覆基材蒸發。可使 -11 - 振張尺度家辟（CNS )喊格（2iGx29 ) xi衣 , ϊ 訂 ϊ—. ~ 線 . 气 身 {請先閱讀背面之注意事項再填寫本頁) 發月係關於使用氫倍半矽氧烷樹脂樹脂) 合物’在電子基材上形成塗層之方法。這心 如供具有獨特性質與特徵之塗層。 二、，·且口 何生自陶堯塗層之H_樹脂在如電子裝置之基材上 用，在此技藝爲已知的。例如，1^ 4,756,977專利揭亍 在電子基材上形成氧化碎塗層之方法，其中1樹脂之溶 :塗布於基材，繼而在空氣中於2〇〇_1〇〇〇七之，度加埶： 塗覆基材。然而，此專利並未敘述使用樹脂之混合物以來 成塗層。 、 y 類似地，聚矽氮烷之使用以在電子裝置上形成陶瓷塗 層，此技藝爲已知的。例如，w〇 93/〇2472與Μ) 5,358,739專利敎示在電予基材上形成塗層之方法，其中 树月曰塗布於電子基材上，繼而加熱被塗覆基材以轉化成爲 陶资。這些公告亦未敎示使用聚合物之混合物。 - 吾人已發現可用之塗層可由H _樹脂與聚矽氮烷之混合 物形成。 經濟部中央標準局員工消費合作社印製 本發明提供在電子基材上形成塗層之方法，並且申請塗 覆之基材。本方法包含首先在基材上塗布包含1〇至9〇重 量％之Η -樹脂與9 0至1 0重量％之聚珍氮垸之複合材。被 塗覆之基材然後在足以轉化複合材成爲陶瓷塗層之溫度加 熱。 本發明亦介紹稀釋於用以形成各種型式之塗層之溶劑， 包含10至90重量％之Η-樹脂與90至10重量。/。之聚矽氮烷 之塗覆複合材。 -4· 本紙張尺度適用中圉國家標準（CNS ) Α4说格（210Χ297公釐） 五 、發明説明（ 本發明基於所需塗層由包含H， 材形成之發現。自其衍生之塗層可比衍 厚（例如，> 1微米），而且亦可裂解及無孔。 、月曰 此=這些優點’本塗層在電子基材特別有價値。例如， 印T用作為保毁塗層、介電塗層、層間介電層等。 =使用之名詞"陶资塗層，，敘述加熱氫倍半硬氧燒與聚 ⑻二二合物後得到之硬塗層。此塗層含（非晶氧切 2 ’及並非完全無殘餘碳、料(S1_0H)'氮(S1_ )或虱又似非晶氧化矽物料。名詞II電子基材”表示包 /但非限於如石夕基裝置、碎化錯基裝置、焦面陣列、光 :裝置、光伏打電池、與光學裝置之電子裝置或電子電 在本發明之方法，陶资塗層藉由包含塗布包含H-樹脂 與聚錢貌之塗覆複合材於基材上，然後在足以轉化複合 材成馬陶究之溫度加熱被塗覆基材之方&，形成於電子基 材上。 .經濟部中央橾準局負工消費合作社印製 可用於本發明-樹脂包括式HSi(OH)x(〇R)y〇z/2之氫 矽氧烷樹脂，其中各r分別爲有機基或經^代有，其 在經氧原子鍵結於矽時，形成可水解取代基，x=0_2， y = 0-2 ’ z=l_3 ’ x + y + z = 3。r之實例包括如甲基、乙 基、丙基、與丁基之烷基；如苯基之芳基；及如烯丙基或 乙缔基之缔基。這些樹脂可完全縮合（Hsi〇 或其可 j. , 3 / 2 ’ η 僅那份水解（即，含—些Si_〇R)及/或部份縮合（即，含一 二Si-OH)雖然此結構並未表示，由於涉及其形成或處 -5- 本紙張认適用中國國家橾準(CNS)A4^{ri0x297^ft 經濟部中央標準局貝工消費合作社印裝 A7 ____________B7_ 五、發明説明（3 ) 〜--- 理之各種因素，這些樹脂可含有少量(例如，少於… 矽原子，其具有〇或2個連接之氫原子。 以上之Η·樹脂及其製法在此技藝爲已知的。例如，us_ A 3,615,272專利敎示幾乎完全縮合^樹脂之製造（其可含 達100-300 ppm之石夕醇），其藉由包含在苯續酸水合物之ς 解介質水解三氣石夕燒，然後以水或水性疏酸清洗生成樹脂 乙方法。同樣的，US-A 5,0 10,159專利提供包-含在芳基磺 酸水合物之解解介質水解氫矽烷，以形成樹脂，其然後接 觸中和劑之替代方法。 ' 其他之或碎氧燒樹脂，如US-A 4,999,397專利所述者. JP-A 59- 178749、60-86017、與 63-107122 專利所述者； 或任何其他同等之氫矽氧烷，在此亦作用。 用於本發明之聚矽氮烷（或矽氮烷聚合物）通常在此技藝 爲已知的，而且其結構並非特別地嚴格。本發明之聚矽氮 烷通常含有[R2SINH]、[RSi(NH)3/2]及/或[R3Si(NH)1/2]@ 之單元，其中各尺分別選自包括氫原子、含1至2〇個碳原 子之基基團、芳基基團、與晞基基團之组。自然地，用 於本發明之聚梦氮燒可含其他之;5夕氮燒單元。此單元之實 例包括[MeSi(NH)3/2]、[Me2SiNH]、[ViSiSi(NH)3/2]、 [Vi2SiNH]、[PhMeSiNH]、[PhViSiNH]、[MeViSiNH]、 [HSi(NH)3/2]、與[H2SiNH]。聚矽氮烷之混合物亦可用於 本發明之實務。 本發明之聚矽氮烷藉此技藝已知之技術而製備。用以製 備聚矽氮烷之實際方法並不嚴格。適當之矽氮烷聚合物或 -6- 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） C請先«'讀背面之注意事項再¾寫本頁) .裝· -訂— A7 B7 經濟部中央標準局員工消費合作社印製 五、發明説明（4 聚珍氮燒可藉US-A 4,540,8〇3與4,543,344專利之方法製 備。其他適當之聚矽氮烷可藉US-Α 4,3 12,970、 4,340,619、4,395,460、4,404，153、4,482,689、 4,397,828 、4,543,344、4,656,300、4,689,252 、與 5,〇3〇,744專利之方法製備。其他之聚矽氮烷包括ep_a 〇 351 747 與 0 332 374 專利者。 特佳之米碎氮燒爲在聚合物重複單元不具有碳者，因爲 生成之塗層具有極少之碳污染。如之末端嵌 段基在此聚合物爲可接受的，、因爲其通常在以後之熱解時 去除。 在此使用之最佳聚合物爲US_A七34…6^與4,54〇,8〇3專 利。前者專利之矽氮烷聚合物藉由在惰性，特別是無水氣 氛，以具有通式（R3’Si)2NH之二矽氮烷，在 之範圍之溫度，接觸及反應通式（ClxRySi)2之含二矽烷之 氣，或含二矽烷之氣之混合物，同時蒸餾揮發性副產物而 製備，其中R爲乙烯基、丨_3個碳原子之烷基、或苯基； R’爲乙烯基、氫原子、i-3個碳原子之烷基、或苯基；X 具有0.5-3之値；y具有0-2.5之値，而且x + y之和爲3。 其中之特佳具體實施例涉及甲基氣二梦燒與六甲基二石夕氮 烷之反應，以製造甲基聚二矽基氮烷。1；1八4,34〇,619專 利之產物矽氮烷聚合物可具有相當高氣離子含量，而且較 佳爲此濃度在用於本發明之前降低。此去除方法更詳細地 敘述於心4,772,516專利’其包含以氨處理聚合物：二 去除氣之時間。 ‘紙張尺度適用中國國家梯準< CNS )八4規格（21〇X297公釐） I 裳 - ,—訂-----祿 、 一 一： (請先W讀背面之注意事項再填寫本頁} 五、發明説明（5 A7 B7 經濟部中央標準局負工消賢合作社印装 /S-A 4,54G，8G3專利之發氮垸聚合物藉由包含在惰性實 質上無水氣氛，以二矽氮烷在25。(：至30(TC之溫度範圍接 觸及與三氣矽烷反應’同時蒸餾揮發性副產物之方法而製 備。用於本發明之二秒氮垸具有式（νι)2ΝΗ，其中义選 自包括乙締基、苯基、與含丨_3個碳原子之烷基基團、或 氫原子之组。此後者專利之特佳具體實施例涉及三氯矽烷 與六甲基二矽氮烷之反應，以製造氫聚矽氮垮。 此外，摻染硼心聚矽氮烷（即，聚硼矽氮烷或硼矽氮烷） 亦可用於本發明，並且包括於本聚矽氮烷之定義。這些硼 矽氮烷通常亦在此技藝爲已知的，而且其結構並未特別地 嚴格。這些聚合物之硼含量，同樣的，通常並不重要，因 此，可在廣泛範圍變化（例如，〇」_ 5 〇重量％ )。本發明之 爛石夕氮：^之主幹通常含有Si-B、Si-N、與B-N鍵，這些 原子疋其餘價數充滿分別選自包括氫原子；含1至2〇個碳 原子之烷基基團，如甲基、乙基、與丙基；如苯基之芳基 基團，及如乙烯基之烯基基固之組之基。較佳之硼秒氮燒 爲其中在聚合物之重複單元並無碳原子者，即，在聚合末 端可有碳原子。 特定的硼矽氮烷之實例包括，例如，Seyferth等人之 國陶竞協會期刊’ ？3, 213 1-2133 (199〇)，或諾斯之 Anorg· Chem. Org. Chem，16 (9), 618-21，（1961)所述者 US-A 4,9l〇，173、5，169,908、4,482,689、5,030,744、 4,604,3 67 所述者；或 EP A 0424 082 與 0 364 3 23 所述者。 製備此化合物之方法類似地在此技藝爲已知的，而且敘 請 先 閱 Λ 之 注 項 再一 裝 美 B. 與 頁 τι 絲 8- 發明説明（6 ) 返於以上之參考資科。然而，此方法之實例一般包含⑴ 以如（RSi(NH)].5)x或（（CH3)3Si)2NH之矽氮烷低聚物與三 自化《I反應’纟中汉選自包括氫原子、烴基團、或經取代 k基團^组，而且又爲2_2〇之整數；（2)以有機聚矽烷與 有機棚氮块反應；及（3 )如硼烷錯合物、環硼氧烷、硼烷 氧化物、及硼氮炔之硼化合物，與聚矽氮烷之反應。 ^佳聚合物包含US-A 5，169,908專利之硼修声氫聚梦氮 烷水口物。這些聚合物藉由以硼烷錯合物或二硼烷與氫矽 氮燒聚合物反應而製造。在此專利之更佳具體實施例，氯 聚石夕乳;fe特別藉由三氣料與六甲基二珍氮虎之反應而製 造，如US-A 4,540,803專利所述。 &如果需要，其他物料亦可加入本塗覆混合物。例如，所 二 ' 塗後複&材可含鉑、铑、或銅觸媒，以增加樹脂成爲 氧化石夕之轉化速率與程度。通常，任何之#、❺、或銅化
合物或其可溶解之錯合物可作用。例如，#乙醯基丙酮酸 ^姥觸媒之複合材’ Rhcl3[s(CH2CW 自欲西根州密德蘭之道康寧公司，或萘酸銅。這些觸媒基 於组合樹脂之重量（H_樹脂與聚梦氮垸），通常以5至1〇〇〇 ppm之銷、铑 '或銅之量而加入。 在本樹脂混合物加入粒狀填料亦爲合適的。例如，其 括各種無機與有機填料，特別是無機料，以各種形能 包^但不限於粉末、顆粒、屑、微球、與纖絲。無機^ 〈實例包括合成與天然物料，如各種金屬之氧化物、氣 物、硼化物、與碳化物’或非金屬，如玻璃、氧化銘、 五、發明説明（7 ) 化石夕、一氧化矽、衰 _ 氧化辞、氧化鶴、氧化：二：化欽' 氧化艇、氧㈣、 碳化珍仆 ’虱化矽、氮化鋁、二硼化鈦、 灭化硼、與氮化硼；碳 二 常數填料（例如，>12、. .弓，灭石π、鬲介電 鋅、與錳之金屬之鈦酸1’ H·、鉛、鑭、鐵、 如，鈦酸鋇、鈦心—乂鈮酸鹽，或鶴酸鹽，包括，例 麫、鈦醢妒；”鈮酸鉛、鈦酸鋰、鈦酸鳃、鈦酸鋇 乂、、锆、鈦酸鉛#、與鎢酸鉛；不透射缘物科 (防止射線穿透之物料)，★鋇'銘、銀、全-:科 錫、鈀、鳃、鎢H ，： t知、銻、 鹽、硫酸鹽、與氧化物：::鹽’包括，例如，如碳酸 餐科，如有機與無機顏料、氮化#末、碳化 透月 化鋁粉末 '氧化碎、盥氧仆 、 氮 ..』 ’、乳化鋁，防干擾物料（氧化時生瓿
:I如鎂m、與辞；磁性物料，如碳I :::二鐵質：羰基鐵、及如鐵，m、：： 全，包括目例T H'锆、錯、發、與鋅之金屬之合 至匕括，例如，Fe2〇 MnZn Π:物料，熱或電導塗層之二金與:他 二辞、路、銘等；鱗等。可使用如纖維素、聚 心、方族聚醢胺、酚樹脂等之—些有機物料。’、 用於本發明之任何填料之量可在廣泛範圍變化 通常填料以少於90體積％之量而使用，以確在夠 :樹=料，地’可使用較少量之填料(: 可存在於本塗覆複合材之其他物料包括，例如，爲了較 -10- ) 本纸張尺度適用中國國家梯準（CNS ) A4規格(210X297^ 經濟部中央標準局員工消費合作衽印裝 弟^106559號專利申請案 中文說明書修正頁(88年9月） ϋ 五；發明説明（8 ) ' - ? ；
i I '佳之黏附遮土j修改表面之填料或懸浮劑。黏附性増進劑包 括，.例如，如縮水甘油氧基丙基三甲氧基矽烷、硫醇基S 基三曱氧基矽烷、與乙烯基三乙醯氧基矽烷之矽烷。通常 以〇. 1至5重量％之量而使用。懸浮劑可包括，例如，纖維 素、黏土、發煙矽石、硬脂酸鹽等。其以足以懸浮任何填 料之量而使用（例如，丨_25重量％)。這些與其他之视情 形成份對熟悉此技藝者為已知的。 同 依照本發明之方法，H_樹脂、聚矽氮烷、與任何視情 形成份塗布於基材之表面。其以任何方法完成，但是較= 方法涉及溶解或分散H-樹脂、聚矽氮烷、與任何視情形 成份於溶劑中。此混合物然後塗布於基材之表面。各2有 利疋方法，如攪拌及/或加熱，然後可用以溶解或分散物 料及產生更均勻之塗布物料。可使用之溶劑包括任何試劑 或試劑混合物，其溶解或分散H _樹脂與聚矽氮烷以形成 均質液體混合物，而不影響生成之塗層。這些溶劑包括， 例如，如苯或甲苯之芳族烴、如正庚烷或十二烷之烷屬 烴、酮、酯、甘油酯或環形二甲基聚矽氧烷，以足以溶解 /分散以上物料至塗布之所需濃度之量。通常，使用足夠 〜以上溶劑，以形成樹脂之〇丨_ 8 〇重量％混合物，較佳為 I - 5 〇重量％。 此混合物然後藉旋塗、浸塗、喷塗、或流塗而塗覆於基 材表面。然而，其他之同等方式亦視為在本發明之範圍 内。 刎然後自塗層之沉積而生成之被塗覆基材蒸發。可使 -11 - 振張尺度家辟（CNS )喊格（2iGx29 ) xi衣 , ϊ 訂 ϊ—. ~ 線 . 气 身 {請先閱讀背面之注意事項再填寫本頁) 經濟部中央揉準局貝工消費合作杜印袈 五、發明説明（9 ) 2發万法’如藉由暴露於周圍環境之簡單 乾、藉由眞空或溫和加熱(例如，低於50。〇之應用、或 熱處理（早期階段時。應注意在使用旋塗時，旋轉驅除容 劑時，額外之乾燥期間最少。 雖然上迷万法王要注意在使用液體方式，熟悉此技藝 應了解，其他同筈夕士、土+ ^ 万法在此亦可使用，而且在本發明之 範圍内。 ，塗層然後-般藉由加熱至足夠溫度而轉化成陶瓷。溫度 通¥在50至lOOOCi範圍，毳熱解氣氛而定。較佳之溫 度在50至80(TC之範圍，而且更佳爲5〇_5〇{rc。加熱通 系進仃足以陶瓷化之時間，通常達6小時，少於3小時較 佳。 '以上t加熱可在由眞空至超大氣壓力之任何有效之大氣 壓力，及有效之氧化或非氧化氣態環境進行，如空氣： 〇2、臭氣、惰氣（N2等）、氨 '胺、水份、n2〇、與只2。 任何加熱方法，如通風烤箱、快速熱處理、加熱板、或 輻射或微波能量之使用，通常在此作用。此外，加熱速率 亦不嚴格，但是儘快加熱最實際及較佳。 藉由以上之方法，在基材上製造陶瓷塗層。塗層之厚度 通常大於0.5微米，而且經常大微米。這些塗層平滑各 種基材之不規則表面；其相當無缺陷；而且其具有優異之 黏著性性質》如此’其對許多電子應用特別有用，如介電 或保護層與導電層。 如果需要，額外之塗層可塗布於這些塗層上。其包括， 12- 卜紙張尺度適用中國國家標準（CNS )八4规格（210X297公釐） 裝 ^ 丨.I訂·；-------^ (請先W讀背面之注意事項再續寫本頁} 一 經濟部中央標準局—工消费合作社印裝 Α7 Β7 五、發明説明（ίο ) 例如，Si〇2塗層、Si〇2/陶瓷氧化物層、含矽塗層 '含矽 碳塗層、含矽氮塗層、矽氧氮塗層、含矽氮碳塗層及/或 鑽石狀碳塗層。此塗層之塗布方法在此技藝爲已知的，而 且許多敘述於US-A 4,756,977專利。特佳塗層爲藉矽雜環 丁板或二甲基矽貌之化學蒸氣沉積而塗布之碳化矽。此方 法更完全地敘述於US-A 5,011，706專利。 包括以下之非限制性實例，使得熟悉此技藝_者可更易於 了解本發明。 實例1 US-A 3,6 15,272專利之方法所製造之0.9克之氫倍半矽氧 燒樹脂’ US-A 4,540,803專利之方法所製造之0.2克之氫 聚矽氮烷（55.6重量％之固體於二甲苯），及6〇 ppmtpt (0.1克之乙醯基丙酮酸鉑），混合於8.8克之環形聚二甲基 梦氧坡。2.54平方公分之秒晶圓然後以此溶液在3〇〇〇 rpni 旋塗2 0秒。塗層在400 °C於空氣熱解3小時。塗廣之FTIR 光譜顯示塗層實質上轉化成爲氧化矽。塗層厚度爲0,5086 微米，而且折射率爲1.442 (8300拉目達）。 實例2 0.5克以上述前者之方法所製造之氫倍半梦氧院樹脂， 1.0克以上述後者之方法所製造之氫聚矽氮烷（55.6重量％ 之固體於二甲苯），3.0克之電漿氧化鋁微球（6微米）及0.4 克之縮水甘油氧基丙基三甲氧基矽烷，以超音波探針混合 於1克之環形聚二甲基矽氧烷，以形成塗層溶液。11.25平 方公分之氧化鋁板藉由使用7 5微米之畫棒而以溶液塗 -13- ^紙張尺度逋用中國國家梯準（CNS ) M規格（2ί0χ297公釐） ~ ----------裝--------Μ——訂；——.----Μ ί I (請先閲讀背面之注意事項再镇寫本頁) 五、發明説明（) A7 B7 覆。被塗覆之板風乾3小時25分鐘，繼而在400 °C於空氣 熱解1小時。熱解之塗層以顯微鏡檢驗，而且在ΙΌΟΟχ放 大未發現裂解。塗層厚度爲48.7微米。 ----------裝--：----- -訂：--^----诔 (請先閲讀背面之注意事項再續寫本頁) 經濟部中央標準局員工消費合作社印裝 -14- 本紙張尺度適用中國國家揉準（CNS ) Α4規格（210X297公釐）

Claims (1)

  1. ABCD 第85丨〇6559號專利申請案 中文申请專利範圍修正本(狀年9月)
    -------------------------------- ^ 丨.-：在電子基材上形成塗層之方法，包含在電子基材 上立布包3 10至90重1%之氫倍半矽氧烷樹脂盥Μ至 1 〇重量％之聚矽氮烷之塗覆複八 &複口材洛液，及被塗覆之 基材在足以轉化塗覆複合材 ^ Τ成為陶瓷塗層之溫度加 熱° 2, -種於電子基材上形成塗層之塗覆複合材，* 劑中稀釋成（^丨至“重量％固體之氫倍 0岭 ，聚物完’其中氣倍半峨樹脂與聚二= 1玍1 . 9之重量比例而存在。 .I -I I 二·- --r . I (請先閱讀背面之注意事項再填寫本頁) 訂·' ▲ 經濟部中央標隼局員工消費合作社印製 ABCD 第85丨〇6559號專利申請案 中文申请專利範圍修正本(狀年9月)
    -------------------------------- ^ 丨.-：在電子基材上形成塗層之方法，包含在電子基材 上立布包3 10至90重1%之氫倍半矽氧烷樹脂盥Μ至 1 〇重量％之聚矽氮烷之塗覆複八 &複口材洛液，及被塗覆之 基材在足以轉化塗覆複合材 ^ Τ成為陶瓷塗層之溫度加 熱° 2, -種於電子基材上形成塗層之塗覆複合材，* 劑中稀釋成（^丨至“重量％固體之氫倍 0岭 ，聚物完’其中氣倍半峨樹脂與聚二= 1玍1 . 9之重量比例而存在。 .I -I I 二·- --r . I (請先閱讀背面之注意事項再填寫本頁) 訂·' ▲ 經濟部中央標隼局員工消費合作社印製
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EP0750337A3 (en) 1997-05-14
US5635240A (en) 1997-06-03
EP0750337A2 (en) 1996-12-27
KR970000360A (ko) 1997-01-21
JPH0922903A (ja) 1997-01-21
US5776599A (en) 1998-07-07

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