TWI500736B - 用於各向異性導電黏合膜之組成物、各向異性導電黏合膜以及半導體裝置 - Google Patents
用於各向異性導電黏合膜之組成物、各向異性導電黏合膜以及半導體裝置 Download PDFInfo
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- TWI500736B TWI500736B TW101140765A TW101140765A TWI500736B TW I500736 B TWI500736 B TW I500736B TW 101140765 A TW101140765 A TW 101140765A TW 101140765 A TW101140765 A TW 101140765A TW I500736 B TWI500736 B TW I500736B
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- Taiwan
- Prior art keywords
- anisotropic conductive
- conductive adhesive
- acrylate
- diacrylate
- resin
- Prior art date
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- 239000000203 mixture Substances 0.000 title claims description 77
- 239000002313 adhesive film Substances 0.000 title claims description 54
- 239000004065 semiconductor Substances 0.000 title claims description 6
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- 230000001070 adhesive effect Effects 0.000 claims description 61
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical group OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims description 36
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Classifications
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
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- H—ELECTRICITY
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/12—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances organic substances
- H01B1/124—Intrinsically conductive polymers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L25/08—Copolymers of styrene
- C08L25/12—Copolymers of styrene with unsaturated nitriles
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- C08L55/00—Compositions of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08L23/00 - C08L53/00
- C08L55/02—ABS [Acrylonitrile-Butadiene-Styrene] polymers
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- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
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- C09J133/062—Copolymers with monomers not covered by C09J133/06
- C09J133/068—Copolymers with monomers not covered by C09J133/06 containing glycidyl groups
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- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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- C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/385—Acrylic polymers
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- C09J7/00—Adhesives in the form of films or foils
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
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- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
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- H—ELECTRICITY
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- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H01L23/48—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor
- H01L23/482—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor consisting of lead-in layers inseparably applied to the semiconductor body
- H01L23/4827—Materials
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- H—ELECTRICITY
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- H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
- H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
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- H01L24/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
- H01L24/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
- C08F222/10—Esters
- C08F222/1006—Esters of polyhydric alcohols or polyhydric phenols
- C08F222/102—Esters of polyhydric alcohols or polyhydric phenols of dialcohols, e.g. ethylene glycol di(meth)acrylate or 1,4-butanediol dimethacrylate
- C08F222/1025—Esters of polyhydric alcohols or polyhydric phenols of dialcohols, e.g. ethylene glycol di(meth)acrylate or 1,4-butanediol dimethacrylate of aromatic dialcohols
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F230/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
- C08F230/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing phosphorus
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- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
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- C—CHEMISTRY; METALLURGY
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
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- C09J2301/00—Additional features of adhesives in the form of films or foils
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- C09J2301/00—Additional features of adhesives in the form of films or foils
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- C09J2301/314—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive layer and/or the carrier being conductive
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
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- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
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Description
本發明係關於一種用於各向異性導電黏合膜之組成物及一種各向異性導電黏合膜。更特別地,本發明係有關於一種各向異性導電黏合膜,其包含作為一聚合物黏結劑系統之具有一環氧官能基的丙烯酸酯共聚物以及作為一固化系統之具有高反應性且在固化後形成一強結構的丙烯酸酯。此黏合膜所具有之該聚合物黏結劑系統與該固化系統之間的固體含量比例為40:60至60:40,且因此在160至200℃下,於5秒或更少的連接時間期間,避免氣泡的發生,而此在一環氧膜中未被知曉。另外,此膜展現了高黏合強度、連接可靠性,及尺寸穩定性。
隨著近來趨勢朝向大而薄之顯示器,在電極與電路間的間距變得精確。一各向異性導電黏合膜擔任非常重要的角色以作為連接微細電路端子的一配線材料。於是,此種各向異性導電膜在作為一電連接材料上,獲得廣大的
注目。
各向異性導電黏合膜要求連接可靠性以供作為一接合材料。至於連接電阻、黏合強度或類似者,依膜的儲存條件而定,在初始狀態測量之膜電阻能夠增加或其黏合強度能夠減少,藉此減損了連接可靠性。進而,氣泡可能產生於使用此膜之端子中,造成連接可靠性的降低。
環氧樹脂黏合劑具有高黏合強度及優異的抗水性或耐熱性,且因而係廣泛地使用於不同的領域,例如,用於電氣及電子目的和建築物。然而,環氧樹脂黏合劑須要在140至180℃下加熱約20秒或在180至210℃下加熱約10秒。當當電極寬度及電極間距由於電子設備領域之高密度電路而變窄時,當線路的連接係以含有環氧樹脂之傳統電路連接材料所完成時,線路可與適當位置脫離、分隔或偏離。據此,需要一種用於一各向異性導電黏合劑組成物,其於10秒或更少的連接時間內達到所欲之特性,較佳地係5秒或更少,以改善生產效能。
傳統的各向異性導電膜具有相當高之一黏結劑系統相對於一固化系統的重量比例,致使在固化後之尺寸穩定性降低。此一低尺寸穩定性對一電極高度高(25μm或更高)之撓性印刷電路板(FPC)而言是一嚴重的問題。因此,有必要發展一用於電極高度高之FPC的具有改良之固化後黏合強度及尺寸穩定性之各向異性導電黏合膜,例如玻璃上膜(FOG)。
再者,對於各向異性導電黏合膜的需求增加,其
改良FPC中的填充比例以在未產生氣泡之下增進黏合強度及連接可靠性。
日本專利第3587859號揭露一含有環氧樹脂之自由基固化劑連接膜,而此樹脂並不足以黏合到玻璃上。日本專利公開案第2010-123418A號揭露黏合劑,其中含有陽離子固化劑及環氧樹脂的第一層是設置於玻璃側上,含有自由基固化劑、丙烯酸系樹脂及環氧化合物之第二層為PI側,以及該等層中之一的最低熔化黏度為另一層之最低熔化黏度的10倍。再者,韓國專利申請案第2009-7026218號揭露一黏合劑,其具有二層間最大放熱波峰溫度之差異為20℃或更低。
然而,這些傳統之黏合劑組成物具有顯著的高黏結劑系統相對於固化系統之重量比例,且因此呈現降低之固化後尺寸穩定性及與玻璃基材之黏合性不足。
本發明的目的係提供一各向異性導電黏合膜,其具有較高之固化系統相對於黏結劑系統的含量比例,藉此改良固化後之尺寸穩定性。
此外,本發明的目的係提供一各向異性導電黏合膜,其解決了氣泡的發生並增進填充比例以改良黏合強度及連接可靠性。
再者,本發明的目的係提供一各向異性導電黏合膜,其使得在160到200℃下,在5秒或較少之連接時間內能
夠快速低溫固化,以降低加壓時間,增進填充比例以改良黏合強度及連接可靠性,且不容許氣泡發生。
再者,本發明的目的係提供一各向異性導電黏合膜,其在黏合強度上具有非常低的下降速率,及在可靠性測試後的連接點電阻上具有低的上升速率,且因此確保優異的可靠性。
再者,本發明的目的係提供一各向異性導電黏合膜,其具有改良之尺寸穩定性、連接可靠性,及黏合強度,且避免氣泡發生於一具有高度高(25μm或更高)電極之撓性印刷電路板(FPC)。
本發明之一方面係提供一種各向異性導電黏合劑組成物,其所具有之該聚合物黏結劑系統與該固化系統之間的固體含量比例為40:60至60:40,及在100℃或更低溫度下的熱膨脹係數為150ppm/℃或更低。
本發明之另一方面係提供一種各向異性導電黏合劑組成物,其包含:丙烯酸酯共聚物;至少一苯乙烯-丙烯腈樹脂、丙烯腈-丁二烯橡膠、胺基甲酸乙酯丙烯酸酯樹脂、酯胺基甲酸乙酯樹脂,及除了胺基甲酸乙酯丙烯酸酯樹脂及酯胺基甲酸乙酯樹脂以外的胺基甲酸乙酯樹脂;經異三聚氰酸環氧乙烷改質之二丙烯酸酯;及雙酚茀二丙烯酸酯。
本發明之又另一方面係提供一種半導體裝置,其包括一各向異性導電黏合膜,該膜所具有之聚合物黏結劑系統與固化系統之間的固體含量比例為40:60至60:40,且具
有25μm或更高之高度之藉由黏合膜結合之電極。
本發明之又另一方面係提供一種各向異性導電膜,其具有利用方程式1計算之大於0且為40%或更低的黏合強度下降速率,以及藉由方程式2計算之大於0且為20%或更低的連接點電阻上升速率(connection resistance increasing rate)。
方程式1:黏合強度下降速率(%)=|(A-B)/A|×100
方程式2:連接點電阻上升速率(%)=|(C-D)/C|×100
(於方程式1,A係在80℃及1MPa下初步加壓1秒且在180℃及3MPa下最終加壓5秒後的黏合強度,及B係在初步加壓、最終加壓及在85℃及85%RH下進行可靠性測試250小時後之黏合強度。)
(於方程式2,C係在80℃及1MPa下初步加壓1秒且在180℃及3MPa下最終加壓5秒後的連接點電阻,及D係在初步加壓、最終加壓及在85℃及85%RH下進行可靠性測試250小時後之連接點電阻。)
本發明所提供之各向異性導電膜具有700gf/cm或更高的可靠性測試後黏合強度以及2.5Ω或更低的可靠性測試後連接點電阻。
本發明所提供之各向異性導電黏合膜,其不容許在初步加壓及最終加壓之後或在可靠性測試之後發生氣泡。
如上所述,根據本發明之各向異性導電黏合劑組成物或膜在固化後呈現適切的尺寸穩定性且不容許氣泡發
生,藉此提供改良之連接可靠性及穩定性。
此各向異性導電黏合劑組成物或膜避免FPC中的氣泡發生,該FPC具有高度高(25μm或更高)之電極且增加填充比例以呈現恰當的黏合強度、連接可靠性及尺寸穩定性。
再者,本發明使得在160到200℃下,於5秒或更少之連接時間內快速低溫固化以降低加壓時間,藉此提升生產效率。
此各向異性導電黏合劑組成物或膜在黏合強度方面具有非常低的下降速率且在可靠性測試後連接點電阻方面具有低的上升速率,以及不容許氣泡發生。
本發明之一方面係提供一各向異性導電黏合劑組成物,其所具有之該聚合物黏結劑系統與該固化系統之間的固體含量比例為40:60至60:40,以及在100℃或更低下的熱膨脹係數為150ppm/℃或更低。該各向異性導電黏合劑組成物包括作為聚合物黏結劑系統之丙烯酸酯共聚物及作為固化系統之雙酚茀二丙烯酸酯及經異三聚氰酸環氧乙烷改質之二丙烯酸酯。於此,以固體含量表示,以各向異性導電黏合劑組成物之總量為基準,雙酚茀二丙烯酸酯及經異三聚氰酸環氧乙烷改質之二丙烯酸酯之總量為25至
50wt%,較佳為25至50wt%。
本發明增加固化系統相對於聚合物黏結劑系統之含量比例,使得該聚合物黏結劑系統與該固化系統之間的固體含量比例為40:60至60:40,藉此改良固化後之尺寸穩定性。固化後尺寸穩定性可以基於固化後熱膨脹係數評估。在本實施例中,各向異性導電黏合劑組成物在100℃或更較的溫度下,具有150ppm/℃或更低的熱膨脹係數,較佳地為130ppm/℃或更低,且更佳為110ppm/℃或更低。在本發明中,熱膨脹係數係定義為在固化之各向異性導電膜設置於TMA(TA儀器)之探針上後,當溫度以10℃/min自25℃升高至250℃時,測量之每單位溫度及單位長度之伸展長度。熱膨脹係數可藉由檢測器顯示之圖形的梯度來測量。
在本發明中,聚合物黏結劑系統與固化系統之間的重量比例係調整至1:1,藉此同時提供適當之連接可靠性及尺寸穩定性。
本發明之另一方面提供各向異性導電黏合劑組成物,其包括丙烯酸酯共聚物;苯乙烯-丙烯腈樹脂、丙烯腈-丁二烯橡膠、胺基甲酸乙酯丙烯酸酯樹脂、酯胺基甲酸乙酯樹脂,及除了胺基甲酸乙酯丙烯酸酯樹脂與酯胺基甲酸乙酯樹脂之外的胺基甲酸乙酯樹脂中至少一者;經異三聚氰酸環氧乙烷改質之二丙烯酸酯;及雙酚茀二丙烯酸酯。
苯乙烯-丙烯腈樹脂、丙烯腈-丁二烯橡膠、胺基甲酸乙酯丙烯酸酯樹脂、酯胺基甲酸乙酯樹脂,或除了胺基甲酸乙酯丙烯酸酯樹脂與酯胺基甲酸乙酯樹脂之外的胺
基甲酸乙酯樹脂可具有100℃或較高之玻璃轉化溫度(Tg)。
以固體含量表示,以各向異性導電黏合劑組成物之總量為基準,雙酚茀二丙烯酸酯及經異三聚氰酸環氧乙烷改質之二丙烯酸酯之總量為25至50wt%。
以各向異性導電黏合劑組成物之總量為基準,雙酚茀二丙烯酸酯及經異三聚氰酸環氧乙烷改質之二丙烯酸酯之總量被調整為25至50wt%,藉此不僅達到各向異性導電黏合劑組成物的快速低溫固化,亦改良固化產物之模數以同時增進組成物的連接可靠性及尺寸穩定性。
包括丙烯酸酯共聚物及苯乙烯-丙烯腈樹脂、丙烯腈-丁二烯橡膠、胺基甲酸乙酯丙烯酸酯樹脂、酯胺基甲酸乙酯樹脂及除了胺基甲酸乙酯丙烯酸酯樹脂與酯胺基甲酸乙酯樹脂之外的胺基甲酸乙酯樹脂中至少一者的聚合物黏結劑系統,相對於包括雙酚茀二丙烯酸酯及經異三聚氰酸環氧乙烷改質之二丙烯酸酯的固化系統之固體含量比例為40:60至60:40,較佳為45:55至55:45。
根據本發明之各向異性導電黏著劑組成物又包括含有(甲基)丙烯酸酯基之化合物、有機過氧化物,及導電粒子,其通常使用於各向異性導電黏著劑組成物。
以固體含量表示,以固體含量的總量為基準,各向異性導電黏著劑組成物可包括20至40wt%之丙烯酸酯共聚物;1至20wt%之苯乙烯-丙烯腈樹脂、丙烯腈-丁二烯橡膠、胺基甲酸乙酯丙烯酸酯樹脂、酯胺基甲酸乙酯樹脂,及除了胺基甲酸乙酯丙烯酸酯樹脂及酯胺基甲酸乙酯樹脂
以外的之胺基甲酸乙酯樹脂中至少一者;5至25wt%之經異三聚氰酸環氧乙烷改質之二丙烯酸酯;5至25wt%之雙酚茀二丙烯酸酯;1至5wt%之含有(甲基)丙烯酸酯基之化合物;1至10wt%之有機過氧化物;及1至10wt%之導電粒子。
本發明之又另一方面係提供一半導體裝置,其包含一各向異性導電黏合膜,該膜所具有之該聚合物黏結劑系統與該固化系統之間的固體含量比例為40:60至60:40,以及具有25μm或更高之高度的藉由黏合膜結合之電極。
該各向異性導電黏合膜可包括作為該聚合物黏結劑系統之丙烯酸酯共聚物以及作為該固化系統之雙酚茀二丙烯酸酯及經異三聚氰酸環氧乙烷改質之二丙烯酸酯。
因為對滿足用於具有25μm或更高電極之FPC的各向異性導電黏合膜的填充比例有所限制,維持黏合強度及尺寸穩定性即非常重要。在本發明中,該各向異性導電黏合膜包括作為固化系統之雙酚茀二丙烯酸酯及經異三聚氰酸環氧乙烷改質之二丙烯酸酯,且以固體含量表示,依據黏合膜之總量為基準調整其固體含量為25至50wt%,以致使該裝置兼具適當之黏合強度及尺寸穩定性。
該各向異性導電黏合膜中之該聚合物黏結劑系統與該固化系統之間的固體含量比例為40:60至60:40。
各向異性導電黏合膜可具有5秒或更少之160至200℃下連接時間,可在該連接時間內避免氣泡發生,且可增加填充比例以加強黏合強度及連接可靠性。
此裝置可包括一玻璃上膜(FOG)型式。
本發明之又另一方面提供一種各向異性導電膜,其具有利用方程式1計算之大於0且為40%或更低的黏合強度下降速率,以利用方程式2計算之大於0且為20%或更低的連接點電阻上升速率。
方程式1:黏合強度下降速率(%)=|(A-B)/A|×100
方程式2:連接點電阻上升速率(%)=|(C-D)/C|×100,其中A係在80℃及1MPa下初步加壓1秒且在180℃及3MPa下最終加壓5秒後的黏合強度,B係在初步加壓、最終加壓及在85℃及85%RH下進行可靠性測試250小時後之黏合強度,C係在80℃及1MPa下初步加壓1秒且在180℃及3MPa下最終加壓5秒後的連接點電阻,以及D係在初步加壓、最終加壓及在85℃及85%RH下進行可靠性測試250小時後之連接點電阻。
各向異性導電黏合膜具有700gf/cm或更高的可靠性測試後黏合強度及2.5Ω或更低的在靠性測試後連接點電阻,藉此提供優異的可靠性且不容許連接失敗。
各向異性導電黏合膜在初步加壓及最終加壓之後及/或在可靠性測試之後,不容許氣泡發生。
各向異性導電黏合膜係放置在部分由玻璃面板形成的電路上且在上述條件下接受初步加壓。然後,於移除離形膜之後,將FPCB置放在該膜上並在上述條件下接受最終加壓。
黏合強度可藉由本技術領域一般已知的任何方法量測量。舉例而言,將已加壓部分分成10mm片段,且基質或晶片彎折成90°,接著測量黏合強度同時在恆定速率下
提升負載晶胞。較佳地,使用通用試驗機(H5KT,Hounsfield)測量90°處的黏合強度。
連接點電阻可藉由本技術領域一般已知的任何方法測量,舉例而言,使用2點探針法。2點探針法可使用電阻檢測器,及使用連接到檢測器的二探針測量兩點之間的電阻。當此電阻檢測器被施與1mA時,利用所測得的電壓計算電阻。
各向異性導電黏合膜當已固化同時以10℃/min將溫度自30℃升高至250℃時,具有1×106
gf/cm2
或更高的最小模數。
各向異性導電黏合膜中之該聚合物黏結劑系統與該固化系統之間的固體含量比例為40:60至60:40。該聚合物黏結劑系統包括丙烯酸酯共聚物,及該固化系統包括雙酚茀二丙烯酸酯及經異三聚氰酸環氧乙烷改質之二丙烯酸酯。
本發明之又另一方面係提供一各向異性導電黏合劑組成物,其以固體含量表示,以該各向異性導電黏合劑組成物的總量為基準,所具有之雙酚茀二丙烯酸酯及經異三聚氰酸環氧乙烷改質之二丙烯酸酯的總量為25至50wt%。
根據本發明之各向異性導電黏合劑組成物或膜在160至200℃下,具有5秒或更少之連接時間。該連接時間意指用於電路連接之最終加壓的時間,其係在160至200℃及3MPa下進行5秒或更短。
根據本發明各向異性導電黏合膜在初步加壓及最終加壓之後及/或在可靠性測試之後不容許氣泡發生,藉此提供高連接可靠性。
氣泡的發生可藉由本技術領域一般已知的任何方法評估。在本發明中,利用顯微鏡觀察端子之間氣泡的形式,且氣泡發生面積為膜總面積的5%或更少時視為無氣泡發生。
根據本發明之各向異性導電黏合膜有1×104
gf/cm2
或更大的最小模數,且當已固化時同時以10℃/min自30℃升高溫度至250℃時,具有1×106
gf/cm2
或更小的最小模數。
根據本發明之各向異性導電黏合劑組成物或膜可用於具有25μm或更高之高度的電極之FPC。
在下文中,將詳細描述根據本發明之各向異性導電黏合劑組成物的每一成分。
<各向異性導電黏合劑組成物>
聚合物黏結劑系統
(a)丙烯酸酯共聚物
丙烯酸酯共聚物的種類無特別的限制,且其所屬技術領域中具有通常知識者一般已知的任何丙烯酸酯共聚物可用在本發明。特別地,可使用藉由作為主要單體之丙烯酸乙酯(EA)/丙烯腈(AN)與環氧官能基反應所製備之丙烯酸酯共聚物,且可使用具有100,000至700,000g/mol之重量平均分子量,較佳為200,000至600,000g/mol,及更佳為300,000至500,000g/mol的丙烯酸酯共聚物。丙烯酸酯共聚物的例子
可包括藉由丙烯酸單體的聚合反應獲得之丙烯酸酯共聚物,該丙烯酸單體例如丙烯酸乙酯、丙烯酸甲酯、丙烯酸丙酯、丙烯酸丁酯、丙烯酸己酯、丙烯酸辛酯、月桂基丙烯酸酯、甲基丙烯酸酯及其等之改質物,例如,丙烯酸酯、丙烯酸、甲基丙烯酸及甲基丙烯酸甲酯及其等之改質物,但不限於此。
丙烯酸酯共聚物必然包括一羥基或羧基,具有1至100mgKOH/g的酸價,及可選擇性地進一步包括一環氧基或烷基。
丙烯酸酯共聚物與固化系統的雙酚茀二丙烯酸酯或經異三聚氰酸環氧乙烷改質之二丙烯酸酯相容以形成一溶液,且因此不分離。
再者,丙烯酸酯共聚物對玻璃面板有好的黏合性,藉此作為一膜形成劑且尤其提供避免於高電極中產生玻璃界面上氣泡的功效。
(b)至少一個苯乙烯-丙烯腈樹脂、丙烯腈-丁二烯橡膠、胺基甲酸乙酯丙烯酸酯樹脂、酯胺基甲酸乙酯樹脂,及除了胺基甲酸乙酯丙烯酸酯樹脂及酯胺基甲酸乙酯樹脂以外的胺基甲酸乙酯樹脂。
(b1)苯乙烯-丙烯腈樹脂
在苯乙烯聚合物中,苯乙烯-丙烯腈樹脂具透明性及耐熱性,特別優異的電及機械特性、化學抗性、尺寸穩定性、除了丙酮之外的溶劑抗性,及光學透明性。因此,其廣泛地被使用在各種電子材料、建築物、醫療設備,或其類似者。苯乙烯-丙烯腈樹脂通常被合成或製備成苯乙烯-丙烯腈
共聚物及一苯乙烯-丙烯腈-苯乙烯共聚物,其可藉由一般方法製備,例如,乳化聚合反應、懸浮液聚合反應,及整體聚合反應。隨著丙烯腈含量的增加,苯乙烯-丙烯腈樹脂呈現優異的物理特性及特徵,但在加工過程中具有降低之可加工性及熱穩定性。因此,與其他製程相較,提供優異透明性及其他物理特性的連續整體聚合反應除了特殊狀況之外被廣泛使用,例如,備製具有高丙烯腈含量之苯乙烯-丙烯腈(SAN)樹脂。苯乙烯-丙烯腈樹脂的例子包括AP系列之SAN樹脂(第一毛織株式會社(Cheil Industries,Inc.))、SAN系列之SAN樹脂(錦湖石油化學株式會社(Kumho Petrochemical Co.,Ltd.))、Lustran系列之SAN樹脂(拜耳(Bayer)),及LuranS系列之丙烯腈-苯乙烯-丙烯腈(ASA)樹脂的(巴斯夫(BASF)),其等可在市面上購得。
苯乙烯-丙烯腈樹脂具有100至150℃的Tg,較佳為110至130℃,及具有50,000至150,000g/mol的重量平均分子量,較佳為70,000至120,000g/mol。
(b2)丙烯腈-丁二烯橡膠
丙烯腈-丁二烯橡膠為藉由丙烯腈及丁二烯的乳化聚合反應製備之共聚物。對於共聚物中丙烯腈及丁二烯的含量及聚合方法無特別限制。丙烯腈-丁二烯橡膠可具有50,000至2,000,000g/mol的重量平均分子量。
經羧基改質之丙烯腈-丁二烯橡膠可使用於本發明。羧基提高樹脂混合物的穩定性,因此改良與其他樹脂及添加物的相容性及可供增進可加工性,例如,可塗覆性。再者,極性上的增加增進黏合強度及且改良抗溼性及耐熱
性。
經羧基改質之丙烯腈-丁二烯橡膠具有2,000至270,000g/mol之重量平均分子量,10至60wt%之丙烯腈含量,及1至20wt%之羧基含量。較佳地,經羧基改質之丙烯腈-丁二烯橡膠具有3,000至250,000g/mol之重量平均分子量及20至50 wt%之丙烯腈含量。
若經羧基改質之丙烯腈-丁二烯橡膠之重量平均分子量小於2,000g/mol,熱穩定性惡化。若經羧基改質之丙烯腈-丁二烯橡膠之重量平均分子量大於270,000g/mol,組成物具有不良的溶劑溶解度,在製備溶液時具有增加的黏度而使可操作性惡化,且呈現降低之黏合強度。再者,若經羧基改質之丙烯腈-丁二烯橡膠之丙烯腈含量小於10wt%,組成物的溶解度降低。若經羧基改質之丙烯腈-丁二烯橡膠之丙烯腈含量大於60wt%,組成物具有不合適的電絕緣性。
可使用任何通常使用於此領域的經羧基改質之丙烯腈-丁二烯橡膠,而無特別限制,及市面上可購得之經羧基改質之丙烯腈-丁二烯橡膠的例子包括Vamac MR,Vamac Ultra IP,VMX30380(杜邦公司(E.I.Du Pont de Nemours and Company))、N34、Nipol NBR、1072及1072CGX(日本瑞翁株式會社(Zeon Co.,Ltd.))。
以固體含量表示,依據各向異性導電黏合劑組成物之總量為基準,丙烯腈-丁二烯橡膠的存在量為2至10wt%,較佳為4至8wt%,更佳為5至7wt%,以作為聚合物
黏結劑系統之成分。若丙烯腈-丁二烯橡膠的量少於2wt%,組成物對於被黏附物的黏合強度降低。若丙烯腈-丁二烯橡膠的量大於10wt%,因為高分子量,可以使樹脂在熱加壓時的流動性降低。
(b3)胺基甲酸乙酯樹脂
胺基甲酸乙酯樹脂為除了胺基甲酸乙酯丙烯酸酯樹脂及酯胺基甲酸乙酯樹脂以外之具有一胺基甲酸乙酯鍵的聚合物樹脂,其係藉由異佛酮二異氰酸酯與聚四亞甲基二醇之聚合反應所製備,但不限於此。
胺基甲酸乙酯樹脂有50,000至2,000,000 g/mol之重量平均分子量。
胺基甲酸乙酯樹脂的說明性化學結構為利用包括至少一有機二異氰酸酯、至少一多元醇,及/或至少一雙官能鏈延長劑之混合物製備的樹脂。
有機二異氰酸酯的例子包括間-伸苯基二異氰酸酯及對-伸苯基二異氰酸酯、氯伸苯基二異氰酸酯、α,α'-二甲苯二異氰酸酯、2,4-甲苯二異氰酸酯及2,6-甲苯二異氰酸酯、2,4-甲苯二異氰酸酯及2,6-甲苯二異氰酸酯的混合物、甲苯胺二異氰酸酯、六亞甲基二異氰酸酯、1,5-萘二異氰酸酯、異佛酮二異氰酸酯;環脂族二異氰酸酯,例如亞甲基雙(環己基異氰酸酯)包括4,4'-異構物、2,4'-異構物及其等之混合物,及其等之所有的幾何異構物,包括反式/反式、順式/反式、順式/順式及其等之混合物,伸環己基二異氰酸酯(1,2-、1,3-或1,4-)、1-甲基-2,5-伸環己基二異氰酸酯、1-甲
基-2,4-伸環己基二異氰酸酯、1-甲基-2,6-伸環己基二異氰酸酯、4,4'-異亞丙基雙(環己基異氰酸酯)、4,4'-二異氰酸酯二環己基,其等之所有幾何異構物及混合物,及其類似物。
再者,此有機二異氰酸酯包括亞甲基雙(異氰酸苯酯)改質之形式。有機二異氰酸酯之較佳例子包括芳香族及脂肪族二異氰酸酯。
多元醇的例子包括聚醚二元醇、聚酯二元醇、羥基端之聚碳酸酯、羥基端之聚丁二烯-丙烯腈共聚物、二烷基氧化物例如環氧乙烷或氧化丙烯、二烷基矽氧烷之羥基端共聚物,及胺基端之聚丁二烯-丙烯腈共聚物,或其等之組合。
雙官能鏈延長劑的例子包括鏈中具有C2至C10的脂肪族直鏈及支鏈二元醇。此二元醇包括乙二醇、1,3-丙二醇、1,4-丁二醇、1,5-戊二醇、1,6-己二醇、新戊二醇;1,4-環己烷二甲醇;對苯二酚雙(羥乙基)醚、伸環己基二醇(1,4-,1,3-,及1,2-異構物)、亞異丙基雙(環己醇);二甘醇、二丙烯甘醇、乙醇胺、N-乙基二甲醇胺;及其混合物。
(b4)胺基甲酸乙酯丙烯酸酯樹脂
由於分子鏈中的胺基甲酸乙酯基,胺基甲酸乙酯丙烯酸酯樹脂具有100℃或較低的玻璃轉化溫度(Tg)以改進流動性及顯示出高黏合強度。特別地,當胺基甲酸乙酯丙烯酸酯樹脂被使用於各向異性導電膜時,固化表現被改善而降低了連接過程的溫度。
胺基甲酸乙酯丙烯酸酯樹脂包括二異氰酸酯、多元醇、二元醇及丙烯酸酯,但不限於此。
二異氰酸酯包括芳香族、脂肪族、脂環族二異氰酸酯,及其等之混合物。二異氰酸酯的例子包括四亞甲基-1,4-二異氰酸酯、六亞甲基-1,6-二異氰酸酯、伸環己基-1,4-二異氰酸酯、亞甲基雙(4-環己基二異氰酸酯)、異佛酮二異氰酸酯,及4,4’-亞甲基雙(環己基異氰酸酯),其可單獨使用或以混合物的形式使用。
多元醇包括聚酯多元醇、聚醚多元醇,及聚碳酸酯多元醇,其具有至少二羥基在其分子鏈中,但不限於此。聚酯多元醇較佳地可得自於二羧酸化合物及二元醇化合物的縮合反應。在此,二羧酸化合物的例子包括丁二酸、戊二酸、異苯二甲酸、己二酸、辛二酸、壬二酸、癸二酸、十二烷二羧酸、六氫酞酸、對苯二甲酸、鄰苯二甲酸、四氯酞酸、1,5-萘二羧酸、富馬酸、馬來酸、伊康酸、檸康酸、中康酸,及四氫酞酸。二元醇化合物的例子包括乙二醇、丙二醇、1,3-丙二醇、1,3-丁二醇、1,4-丁二醇、1,5-戊二醇、1,6-己二醇、新戊二醇、二甘醇、二丙烯甘醇、三甘醇、四甘醇、二丁二醇、2-甲基-1,3-戊二醇、2,2,4-三甲基-1,3-戊二醇,及1,4-環己烷二甲醇。聚醚多元醇的例子包括聚乙二醇、聚丙二醇,及聚四甘醇。在聚醚多元醇,多元醇具有400至10,000g/mol的重量平均分子量,較佳為400至3,000g/mol。聚碳酸酯多元醇的例子包括衍生自聚伸烷基碳酸酯及矽氧烷之聚碳酸酯多元醇。
二元醇包括1,3-丙二醇、1,3-丁二醇、1,4-丁二醇、1,5-戊二醇、1,6-己二醇、新戊二醇、二甘醇、二丙烯甘醇、三甘醇、四甘醇、二丁二醇、2-甲基-1,3-戊二醇、2,2,4-三甲基-1,3-戊二醇,及1,4-環己烷二甲醇。
丙烯酸酯包括羥基丙烯酸酯或胺丙烯酸酯。
包括上述四成份的胺基甲酸乙酯丙烯酸酯樹脂係藉由加成聚合反應所製備致使二異氰酸酯基(NCO)相對於羥基(OH)的莫耳比例是1.04至1.6且多元醇含量在除了丙烯酸酯外之三成份中係70%或較少,接著是藉由加成聚合反應合成之胺基甲酸乙酯的末端官能基的反應,亦即二異氰酸酯基與羥基丙烯酸酯或胺丙烯酸酯以0.1至2.1莫耳比例的反應。再者,使剩餘的異氰酸酯基進行與醇類的反應,藉此最終產生胺基甲酸乙酯丙烯酸酯樹脂。在此,加成聚合係由在本技術領域一般已知的任何方法來進行。同樣地,加成聚合可被進行於溫度90℃及1 atm的壓力使用錫系催化劑達5小時,但不限於此。
胺基甲酸乙酯丙烯酸酯樹脂具有1,000至100,000g/mol之重量平均分子量及包括至少一個丙烯酸酯之末端官能基。
胺基甲酸乙酯丙烯酸酯樹脂具有20,000至100,000g/mol之重量平均分子量,較佳為20,000至40,000g/mol。
(b5)酯胺基甲酸乙酯樹脂
酯胺基甲酸乙酯樹脂係具有胺基甲酸乙酯基及酯基機
化合物的組合。酯胺基甲酸乙酯化合物具有胺基甲酸乙酯基及酯基在其主鏈。酯胺基甲酸乙酯化合物係,例如,藉由聚酯多元醇及二異氰酸酯之反應所獲得。藉此反應獲得之酯胺基甲酸乙酯化合物通常亦也被稱為聚酯胺基甲酸乙酯樹脂。
二異氰酸酯的例子包括芳香族、脂環族,或脂肪族二異氰酸酯,例如2,4-甲伸苯基二異氰酸酯(TDI)、4,4'-二苯甲烷二異氰酸酯(MDI)、1,6-六亞甲基二異氰酸酯(HDI),及異佛酮二異氰酸酯(IPDI)。
聚酯多元醇係具有多個酯基及多個羥基之聚合物。聚酯多元醇係,例如,藉由二羧酸及二元醇之反應所獲得。二羧酸的例子包括芳香族或脂肪族二羧酸,例如對苯二甲酸、異苯二甲酸、己二酸,及癸二酸。二元醇的例子包括二醇,例如乙二醇、丙二醇、1,4-丁二醇、己二醇、新戊二醇、二甘醇,及三甘醇。
酯胺基甲酸乙酯化合物具有100℃或更高的玻璃轉化溫度(Tg)。酯胺基甲酸乙酯化合物的玻璃轉化溫度(Tg)可藉由適當調節聚酯多元醇或二異氰酸酯的種類及分子量以調整至100℃或更高。
酯胺基甲酸乙酯化合物具有陰離子特性,得以進一步改善黏合強度。陰離子性酯胺基甲酸乙酯化合物可藉由在在聚酯多元醇與二異氰酸酯的反應中,使具有磺酸基或羧基之二元醇或二元胺共聚合至支鏈而獲得。亦即,酯胺基甲酸乙酯化合物可包含磺酸或二羧酸。
酯胺基甲酸乙酯化合物具有芳香基包括苯環或脂環基包括環己烷環。
可使用至少兩種酯胺基甲酸乙酯化合物的混合物。例如,結合藉由芳香族聚酯多元醇與脂肪族二異氰酸酯之反應所獲得之化合物及藉由脂肪族聚酯多元醇與芳香族二異氰酸酯之反應所獲得之化合物。
酯胺基甲酸乙酯化合物具有5,000至100,000g/mol之重量平均分子量。若酯胺基甲酸乙酯化合物之重量平均分子量低於5,000 g/mol,當此組成物成形為膜時,膜的成形性會趨於降低。若酯胺基甲酸乙酯化合物的重量平均分子量大於100,000 g/mol時,此組成物無法適當地溶於或相容於溶劑中,使得製備出用以成形為膜之塗層溶液有困難。
固化系統
(c)經異三聚氰酸環氧乙烷改質之二丙烯酸酯
經異三聚氰酸環氧乙烷改質之二丙烯酸酯具有低的反應溫度,在該溫度下固化開始和快速的反應速率,故而快速固化此各向異性導電黏合劑組成物。因此,經異三聚氰酸環氧乙烷改質之二丙烯酸酯可在連接時在低溫提供高的黏合強度及連接可靠性。
藉由示差掃描式量熱法(DSC)的評估,經異三聚氰酸環氧乙烷改質之二丙烯酸酯具有86至97℃之放熱波峰。特別地,經異三聚氰酸環氧乙烷改質之二丙烯酸酯較佳地具有92至95℃的放熱波峰,以使各向異性導電黏合膜充分地在短暫的最終加壓時間內被固化。若經異三聚氰酸
環氧乙烷改質之二丙烯酸酯之放熱波峰係低於86℃時,各向異性導電黏合膜組成物太早被固化,致使一電極無法被充分加壓。若經異三聚氰酸環氧乙烷改質之二丙烯酸酯之放熱波峰係高於97℃,此組成物無法在短時間內被固化,則無法確保連接點電阻的可靠性。
以固體含量表示,以各向異性導電黏合劑組成物之總量為基準,經異三聚氰酸環氧乙烷改質之二丙烯酸酯的存在量為10至30wt%,較佳為15至25wt%。若經異三聚氰酸環氧乙烷改質之二丙烯酸酯的量低於10wt%,組成物具有不良之連接可靠性。若經異三聚氰酸環氧乙烷改質之二丙烯酸酯的量高於30wt%,組成物有下降之黏合強度。
(d)雙酚茀二丙烯酸酯
由於茀的本質,雙酚茀二丙烯酸酯可供增加填充比例,控制組成物的流動性,及改善固化產物的模數,以增強可靠性。
雙酚茀二丙烯酸酯的例子包括雙酚茀環氧基二丙烯酸酯及雙酚茀胺基甲酸乙酯二丙烯酸酯。
雙酚茀二丙烯酸酯具有1,000至2,000g/mol之重量平均分子量,較佳為1,200至1,600g/mol,及更佳為1,300至1,500 g/mol。
較佳地,使用藉由化學式1表示之雙酚茀二丙烯酸酯:[化學式1]
其中R係獨立地為氫、烷基、烷氧基、芳香基或環烷基,m係獨立地為0至4之整數。
(e)含(甲基)丙烯酸酯基之化合物
含(甲基)丙烯酸酯基之化合物係自由基可聚合化合物,其中固化系統的一成份用以確保當自由基固化反應發生時介於連接層間的黏合強度及連接可靠性。
含(甲基)丙烯酸酯基之化合物包括(甲基)丙烯酸酯寡聚物及(甲基)丙烯酸酯單體。(甲基)丙烯酸酯寡聚物包括任何通用之(甲基)丙烯酸酯寡聚物,例如,胺基甲酸乙酯(甲基)丙烯酸酯、環氧基(甲基)丙烯酸酯、聚酯(甲基)丙烯酸酯、氟(甲基)丙烯酸酯、茀(甲基)丙烯酸酯、矽氧烷(甲基)丙烯酸酯、磷(甲基)丙烯酸酯、經馬來醯亞胺改質之(甲基)丙烯酸酯,及丙烯酸酯(甲基丙烯酸酯),其具有約1,000至100,000g/mol之重量平均分子量。
胺基甲酸乙酯(甲基)丙烯酸酯包括具有中間產物結構的分子,該中間產物結構係自聚酯多元醇、聚醚多元醇、聚碳酸酯多元醇、聚己內酯多元醇、開環之四氫呋喃-環氧丙烷共聚物、聚丁二烯二元醇、聚二甲基矽氧烷二
元醇、乙二醇、丙二醇、1,4-丁二醇、1,5-戊二醇、1,6-己二醇、新戊二醇、1,4-環己烷二甲醇、雙酚A、氫化雙酚A、2,4-甲苯二異氰酸酯、1,3-二甲苯二異氰酸酯、1,4-二甲苯二異氰酸酯、1,5-萘二異氰酸酯、1,6-己烷二異氰酸酯、異佛酮二異氰酸酯,及經雙酚A環氧丙烷改質之二丙烯酸酯合成。環氧基(甲基)丙烯酸酯包括具有中間產物結構的分子,該中間產物結構係選自於2-溴氫醌、間苯二酚、鄰苯二酚、雙酚A、雙酚F、雙酚AD、雙酚S、4,4'-二羥基聯苯基、雙(4-羥苯基)醚,及(甲基)丙烯酸酯寡聚物具有烷基、芳香基、羥甲基、丙烯基、脂環基、鹵素(四溴雙酚A),或硝基。此外,(甲基)丙烯酸酯寡聚物包括在其分子中含有至少兩個馬來醯亞胺基的化合物,例如,1-甲基-2,4-雙馬來醯亞胺苯、N,N'-間-伸苯基雙馬來醯亞胺、N,N'-對-伸苯基雙馬來醯亞胺、N,N'-間-1,2-伸聯苯基雙馬來醯亞胺、N,N'-4,4-雙伸苯基雙馬來醯亞胺、N,N'-4,4-(3,3'-二甲基雙伸苯)雙馬來醯亞胺、N,N'-4,4-(3,3'-二甲基二苯甲烷)雙馬來醯亞胺、N,N'-4,4-(3,3'-二乙基二苯甲烷)雙馬來醯亞胺、N,N'-4,4-二苯甲烷雙馬來醯亞胺、N,N'-4,4-聯苯丙烷雙馬來醯亞胺、N,N'-4,4-二苯醚雙馬來醯亞胺、N,N'-3,3'-二苯碸雙馬來醯亞胺、2,2-雙[4-(4-馬來酰亞胺苯氧基)]、2,2-雙[3-仲丁基-4-8(4-馬來酰亞胺苯氧基)苯基]丙烷、1,1-雙[4-(4-馬來酰亞胺苯氧基)苯基]癸烷、4,4'-亞環己基-雙[1-(4-馬來酰亞胺苯氧基)-2-環己基]苯,及2,2-雙[4-(4-馬來酰亞胺苯氧基)苯基]六氟丙烷所組成之組群。
(甲基)丙烯酸酯單體包括通用的(甲基)丙烯酸酯單體,例如,1,6-己二醇單(甲基)丙烯酸酯、2-羥乙基(甲基)丙烯酸酯、2-羥丙基(甲基)丙烯酸酯、2-羥丁基(甲基)丙烯酸酯、2-羥基-3-苯基環氧丙烷基(甲基)丙烯酸酯、1,4-丁二醇(甲基)丙烯酸酯、2-羥烷基(甲基)丙烯醯基磷酸、4-羥基環己基(甲基)丙烯酸酯、新戊二醇單(甲基)丙烯酸酯、三羥甲基乙烷二(甲基)丙烯酸酯、三羥甲基丙烷二(甲基)丙烯酸酯、季戊四醇三(甲基)丙烯酸酯、二季戊四醇五(甲基)丙烯酸酯、季戊四醇六(甲基)丙烯酸酯、二季戊四醇六(甲基)丙烯酸酯、甘油二(甲基)丙烯酸酯、t-水糠基(甲基)丙烯酸酯、異癸基(甲基)丙烯酸酯、2-(2-乙氧基乙基(甲基)丙烯酸酯、硬脂醯(甲基)丙烯酸酯、月桂基(甲基)丙烯酸酯、2-苯氧乙基(甲基)丙烯酸酯、異莰基(甲基)丙烯酸酯、十三基(甲基)丙烯酸酯、乙氧基化壬基苯酚(甲基)丙烯酸酯、乙二醇二(甲基)丙烯酸酯、二甘醇二(甲基)丙烯酸酯、三乙二醇二(甲基)丙烯酸酯、t-乙二醇二(甲基)丙烯酸酯、聚乙二醇二(甲基)丙烯酸酯、1,3-丁二醇二(甲基)丙烯酸酯、三伸丙二醇二(甲基)丙烯酸酯、乙氧基化雙酚A二(甲基)丙烯酸酯、環己烷二甲醇二(甲基)丙烯酸酯、苯氧基-t-乙二醇(甲基)丙烯酸酯、2-甲基丙烯醯氧乙基磷酸酯、二羥甲基三環癸烷二(甲基)丙烯酸酯、三羥甲基-丙烷苯甲酸丙烯酸酯、茀(甲基)丙烯酸酯,及酸磷氧乙基甲基丙烯酸酯(acid phosphoxyethyl methacrylate)。
以固體含量表示,以各向異性導電黏合劑組成物之總量為基準,含(甲基)丙烯酸酯基之化合物的存在量為1
至10wt%,較佳為1至5wt%。在此範圍內,儘管加壓溫度上升,組成物的黏合強度未下降,且儘管加壓溫度下降,可防止組成物之未固化,故能維持連接可靠性。
自由基固化劑
(f)有機過氧化物
有機過氧化物可以作為一固化劑,當被加熱或曝光時會產生自由基。有機過氧化物的例子包括,但不被限於,過氧月桂醯基、過氧t-丁基月桂酸酯、過氧1,1,3,3-t-甲基丁基-2-乙基己酸酯、2,5-二甲基-2,5-二(過氧2-乙基己醯基)己烷、過氧1-環己基-1-甲基乙基-2-乙基己酸酯、2,5-二甲基-2,5-二(過氧間-甲苯甲醯基)己烷、過氧t-丁基異丙基單碳酸酯、過氧t-丁基-2-乙己基單碳酸酯、過氧t-己基苯甲酸酯、過氧t-叔丁基醋酸酯、過氧二異丙苯、2,5-二甲基-2,5-二(過氧t-丁基)己烷、過氧t-丁基異丙苯、過氧t-己基新癸酸酯、過氧t-己基-2-乙基己酸酯、過氧t-丁基-2-2-乙基己酸酯、過氧t-丁基基異丁酸酯、1,1-雙(過氧t-丁基)環己烷、過氧t-己基異丙基單碳酸酯、過氧t-丁基-3,5,5-三甲基己酸酯、過氧t-丁基特戊酸酯、過氧異丙苯新癸酸酯、二異丙苯過氧化氫、異丙苯過氧化氫、異丁基過氧化物、2,4-二氯過氧化苯甲醯過氧化物、3,5,5-三甲基己醯基過氧化物、辛醯基過氧化物、硬脂醯基過氧化物、過氧化琥珀酸、苯甲醯基過氧化物、3,5,5-三甲基己醯基過氧化物、苯甲醯基過氧基甲苯、1,1,3,3-四甲基丁基過氧基新癸酸酯、1-環己基-1-甲基乙基過氧基新癸酸酯、二-n-丙基過氧基二碳酸酯、二異丙基過氧基碳酸酯、雙(4-t-丁基環己基)過氧基二碳酸酯、二
-2-乙氧基甲氧基過氧基二碳酸酯、二(2-乙基己基過氧化基)二碳酸酯、二甲氧基-丁基過氧化基二碳酸酯、二(3-甲基-3-甲氧基丁基過氧化基)二碳酸酯、1,1-雙(t-己基過氧化基)-3,3,5-三甲基環己烷、1,1-雙(t-己基過氧化基)環己烷、1,1-雙(t-丁基過氧化基)-3,3,5-三甲基環己烷、1,1-(t-丁基過氧化基)環十二烷、2,2-雙(t-丁基過氧化基)癸烷、t-丁基三甲基矽烷基過氧化物、雙(t-丁基)二甲基矽烷基過氧化物、t-丁基三丙烯基矽烷基過氧化物、雙(t-丁基)二丙烯基矽烷基過氧化物,及三(t-丁基)丙烯基矽烷基過氧化物。
作為有機過氧化物,可合宜地使用在40至100℃下具有5小時至15小時半衰期溫度之化合物。若有機過氧化物的半衰期溫度過低,其解離速率會很快,致使在室溫儲存困難。若半衰期溫度過高,聚合反應速率會變得很慢,而此難以合宜地用於快速固化。
以據固體含量表示,以各向異性導電黏合劑組成物之總量為基準,有機過氧化物的存在量為1至10wt%。在此範圍內,固化速率不會降低,故而不會使最終加壓的特性劣化,且可避免藉由加熱固化後之各向異性導電黏合膜的脆度增加,因此在再造期間可完全移除各向異性導電膜。
導電粒子
導電粒子包括任何通常已知之導電粒子,並無特別的限制。此導電粒子包括含金、銀、鎳、銅,及焊料之金屬粒子;碳粒子;塗覆有金、銀,及鎳之包括聚乙烯、聚丙烯、聚酯、聚苯乙烯及聚乙烯醇之樹脂的粒子或其等之改
質的樹脂粒子;及藉由塗覆絕緣粒子至該等已塗覆粒子的絕緣粒子。導電粒子視所採用的電路之間距及目的而定,可具有2至50μm之尺寸。
以固體含量表示,以各向異性導電黏合劑組成物之總量為基準,導電粒子的存在量為1至10wt%,較佳為1至5wt%。在此範圍內,導電粒子能展現其維持電路間的連接,維持絕緣性質的主要角色。
根據本發明用於各向異性導電黏合膜的組成物可進一步包括一用於染色之顏料、一染料、一聚合反應抑制劑、一矽烷偶合劑,或鑑於產品性質或可操作性之類似者以能獲得固化產品之所欲性質。這些成份可以此技藝領域通常所知之適量被加入。
在下文中,本發明的組成與功能將參照下述實施例更詳細說明。所提供之這些實施例僅係供例示說明之目的且不得以任何方式解釋成限制本發明。
未包括於本文中的細節將可容易地由熟習此技藝者所認知或理解,且省略其等之解釋。
實施例
實施例1:各向異性導電黏合膜之製備
(1)各向異性導電黏合劑組成物之製備
一種各向異性導電黏合劑組成物係藉由混合作為有機過氧化物之30wt%之含有環氧官能基的丙烯酸酯共聚物,溶於甲苯及甲乙酮(MEK)之5wt%的經羧基改質之丙烯腈-丁二烯橡膠(重量平均分子量:240,000g/mol,Nipol NBR,曾榮公司(Zeon Co.))、溶於MEK之15wt%之苯乙烯-丙烯腈
樹脂(Tg:120℃,重量平均分子量:100,000g/mol)、20wt%之經異三聚氰酸環氧乙烷改質之二丙烯酸酯(DSC放熱波峰:92至95℃)、20wt%之雙酚茀二丙烯酸酯(重量平均分子量:1,400g/mol)、1.5wt%之酸磷氧乙基甲基丙烯酸酯、2.5wt%磷酸丙烯酸酯(重量平均分子量:12,000g/mol)、溶於甲苯之1.0wt%的月桂醯過氧化物,及溶於甲苯之2.0wt%之苯甲醯過氧化物,及作為導電粒子之3wt%之塗覆具有4至6μm的平均直徑之鎳的導電聚合物球來製備。
(2)各向異性導電黏合膜之製備
根據本發明之一種各向異性導電黏合膜可輕易地以使用根據本發明之各向異性導電黏合劑組成物而無特殊設備或系統所製備。
將上述製備的各向異性導電黏合劑組成物溶於一例如甲苯之有機溶劑,並液化,之後在一導電粒子並不會粉碎的速度下攪拌該溶液一定時間。之後,將此溶液施覆至一離形膜達厚度10至15μm,隨後藉由乾燥一段時間以蒸發該有機溶劑,藉此產生一各向異性導電膜。
實施例2
除了該丙烯酸酯共聚物、該經異三聚氰酸環氧乙烷改質之二丙烯酸酯,及該雙酚茀二丙烯酸酯的含量分別變更為35wt%、15wt%,及25wt%之外,以與實施例1相同的方法製備根據實施例2各向異性導電膜。
實施例3
除了使用如下述所製備之胺基甲酸乙酯丙烯酸酯樹脂來取代經羧基改質之丙烯腈-丁二烯橡膠之外,以與實施例
1相同的方法製備實施例3之各向異性導電膜。
比較例1至3
除了使用茀苯氧基樹脂取代丙烯酸酯共聚物(比較例1)、使用二環戊丙烯酸酯取代經異三聚氰酸環氧乙烷改質之二丙烯酸酯(比較例2),或使用二環戊丙烯酸酯取代雙酚茀二丙烯酸酯(比較例3)之外,以與實施例1相同的方法製備實施例3之各向異性導電膜。
(A)丙烯腈-丁二烯橡膠:經羧基改質之丙烯腈-丁二烯橡膠,具有240,000g/mol之重量平均分子量,固體含量:25%(Nipol NBR,曾榮公司(Zeon Co.))。
(B)丙烯酸酯共聚物:AOF7001(重量平均分子量:350,000g/mol,含有環氧官能基,固體含量:18%,愛敬化學(Aekyung Chemical))。
(C)胺基甲酸乙酯丙烯酸酯樹脂:使用50vol%的MEK為溶劑,藉由在90℃及1atm下,在作為催化劑之二丁基錫二月桂酸酯存在下,與60vol%之多元醇及莫耳比例為1.0之羥基甲基丙烯酸酯/芳香族異氰酸酯聚合達5小時合成之聚胺基甲酸乙酯丙烯酸酯(重量平均分子量:100,000g/mol,Tg:110℃)。
(D)具有120℃之Tg及100,000g/mol之重量平均分子量
的苯乙烯-丙烯腈樹脂,固體含量:50%(第一毛織公司(Cheil Industries))。
(E)經異三聚氰酸環氧乙烷改質之二丙烯酸酯:具有DSC放熱波峰92至95℃之經異三聚氰酸環氧乙烷改質之二丙烯酸酯。
(F)具有1400g/mol之重量平均分子量之雙酚茀二丙烯酸酯。
(G)含(甲基)丙烯酸酯基之化合物
-酸磷氧乙基甲基丙烯酸酯
-具有12,000g/mol之重量平均分子量的磷酸丙烯酸酯。
(H)有機過氧化物:月桂醯過氧化物(固體含量:10%),苯甲醯過氧化物(固體含量:10%)
(I)導電粒子:具有平均直徑4至6μm之塗覆鎳之導電聚合球。
*雙酚A液體環氧樹脂:YP-50(JER Co.)
**茀苯氧基樹脂:FX293(東都化成股份有限公司(Tohto Kasei Co.,Ltd.))。
***二環戊丙烯酸酯:DCP-A(新中村化學(Shin Nakamura Chemical))
實驗實施例:黏合強度、熱膨脹係數,及模數的測量
根據實施例1至3及比較例1至3所製備之各向異性導電黏合膜相關於黏合強度、熱膨脹係數、連接點電阻,及模數之評估如下。
.初始黏合強度:1000gf/cm或更高
.可靠性測試後黏合強度:700gf/cm或更高
.初始連接點電阻:2Ω或更低
.可靠性測試後連接點電阻:2.5Ω或更低
.最小模數:1×104
gf/cm2
或更高
.在固化後之模數:1×106
gf/cm2
或更高
.熱膨脹係數:在100℃或更低溫度下為150ppm/℃或更低
評估方法
(1)黏合強度
評估每一種各向異性導電黏合膜之電路連接表現,使用FPCB(電極高度:28 μm,BH Flex Co.,Ltd.)及玻璃TEG(無圖案裸玻璃TEG,第一毛織公司(Cheil Industries)進行加壓。
各向異性導電黏合膜被放置部分由玻璃面板形成的電路上並在80℃及1MPa下接受初步加壓1秒。移除離形膜之後,FPCB被置放在該膜上並在180℃及3MPa下承受最終加壓8秒。已加壓部分被分成10 mm片段,且基板或晶片折成90°,接著使用通用試驗機(H5KT,Hounsfield)量測黏合強度同時以恆定速率提升負載晶胞。然後,評估可靠性,在恆定溫度及濕度留下電路連接產品,亦即,在85℃及85% RH達250小時,接著以上述方法量測黏合強度。
(2)連接點電阻
膜的連接點電阻係在初步加壓及最終加壓及在恆定溫度及濕度下儲存之後,藉由2點探針法在黏合強度測量所述
條件(1)下測得。2點探針法係使用電阻檢測器,及使用連接到檢測器之2點探針檢測界於兩點之間的電阻。當此電阻檢測器被施與1mA時,利用所測得的電壓計算電阻。
(3)熱膨脹係數
測量各向異性導電膜之熱膨脹係數係藉由安置固化膜於TMA(TA儀器公司(TA Instruments))的探針上。以10℃/min將溫度自25℃提高至250℃。熱膨脹係數係定義為每單位溫度及單位長度伸展之長度,其係藉由一檢測器顯示圖形梯度所測量而得。
(4)模數
使用ARES設備量測模數,同時以10℃/min將溫度自30℃提高至250℃。在5%形變及頻率1.0 rad/sec之下進行量測。
根據實施例1至3及比較例1至3之膜的測量結果係說明於表2。
O:與溶劑混合
X:不與溶劑混合
如表2所示,根據本發明之各向異性導電黏合劑組成物,在固化後顯示出合宜之尺寸穩定性及改良之連接可靠性和穩定性,且在於可靠性測試之後,黏合強度具有顯著低的下降速率及連接點電阻具有低的上升速率。
本發明使得能夠在160至200℃下,在5秒或更少之連接時間內進行快速低溫-固化,以降低加壓時間,藉此提升生產效率。
雖然已結合圖式提供一些實施例,但熟習此項技藝者將顯知該等實施例僅係作為例示說明,且各種修改、變化、改變及等效實施例可於未偏離本發明之精神及範圍下進行。本發明之範圍應僅受限於伴隨之申請專利範圍。
Claims (16)
- 一種各向異性導電黏著劑組成物,其具有之界於一聚合物黏結劑系統與一固化系統之間的固體含量比例為40:60至60:40,以及在100℃或更低之下的熱膨脹係數為150ppm/℃或更低,其中該聚合物黏結劑系統包含丙烯酸酯共聚物,及該固化系統包含雙酚茀二丙烯酸酯及經異三聚氰酸環氧乙烷改質之二丙烯酸酯。
- 如申請專利範圍第1項之各向異性導電黏著劑組成物,其中以固體含量表示,以該各向異性導電黏著劑組成物之總量為基準,該雙酚茀二丙烯酸酯及該經異三聚氰酸環氧乙烷改質之二丙烯酸酯之總量為25至50wt%。
- 一種各向異性導電黏著劑組成物包含:丙烯酸酯共聚物;至少一苯乙烯-丙烯腈樹脂、丙烯腈-丁二烯橡膠、胺基甲酸乙酯樹脂、胺基甲酸乙酯丙烯酸酯樹脂,及酯胺基甲酸乙酯樹脂;經異三聚氰酸環氧乙烷改質之二丙烯酸酯;以及雙酚茀二丙烯酸酯。
- 如申請專利範圍第3項之各向異性導電黏著劑組成物,其中該苯乙烯-丙烯腈樹脂、該丙烯腈-丁二烯橡膠、該胺基甲酸乙酯樹脂、該胺基甲酸乙酯丙烯酸酯樹脂,及該酯胺基甲酸乙酯樹脂具有100℃或更高之玻璃轉化溫度。
- 如申請專利範圍第3項之各向異性導電黏著劑組成物,其中以固體含量表示,以該各向異性導電黏著劑組成物 之總量為基準,該雙酚茀二丙烯酸酯及該經異三聚氰酸環氧乙烷改質之二丙烯酸酯之總量為25至50wt%。
- 如申請專利範圍第3至5項中任一項之各向異性導電黏著劑組成物,進一步包含:含(甲基)丙烯酸酯基之化合物、一有機過氧化物,及導電粒子。
- 如申請專利範圍第6項之各向異性導電黏著劑組成物,其中以固體含量表示,以該各向異性導電黏著劑組成物之總量為基準,該各向異性導電黏著劑組成物包含20至40wt%之該丙烯酸酯共聚物;1至20wt%之該至少一苯乙烯-丙烯腈樹脂、該丙烯腈-丁二烯橡膠、該胺基甲酸乙酯樹脂、該胺基甲酸乙酯丙烯酸酯樹脂,及該酯胺基甲酸乙酯樹脂;5至25wt%之該經異三聚氰酸環氧乙烷改質之二丙烯酸酯;5至25wt%之該雙酚茀二丙烯酸酯;1至5wt%之該含(甲基)丙烯酸酯基之化合物;1至10wt%之有機過氧化物;及1至10wt%之導電粒子。
- 一種半導體裝置,包含一各向異性導電黏合膜,該膜所具有之界於一聚合物黏結劑系統與一固化系統之間的固體含量比例為40:60至60:40,包含一丙烯酸酯共聚物作為該聚合物黏結劑系統,以及雙酚茀二丙烯酸酯及經異三聚氰酸環氧乙烷改質之二丙烯酸酯作為該固化系統,及具有25μm或更高之高度之藉由該黏合膜結合之電極。
- 如申請專利範圍第8項之半導體裝置,其中該各向異性導電黏合膜在160℃至200℃下具有5秒或更少之連接時間。
- 如申請專利範圍第8項之半導體裝置,其中該裝置包含 一玻璃上膜的型式(a film on glass form)。
- 一種各向異性導電黏合膜,具有藉由方程式1計算之大於0且為40%或更低的黏合強度下降速率,以及藉由方程式2計算之大於0且為20%或較少的一連接點電阻上升速率(connection resistance increasing rate):方程式1:黏合強度下降速率(%)=|(A-B)/A|×100 方程式2:連接點電阻上升速率(%)=|(C-D)/C|×100其中A係在80℃及1MPa下初步加壓1秒且在160℃及3MPa下最終加壓5秒後的黏合強度,B係在初步加壓、最終加壓及在85℃及85%下進行可靠性測試250小時後之黏合強度,以及C係在80℃及1MPa下初步加壓1秒且在160℃及3MPa下最終加壓5秒後的連接點電阻,及D係在初步加壓、最終加壓及在85℃及85%下進行可靠性測試250小時後之連接點電阻。
- 如申請專利範圍第11項之各向異性導電黏合膜,其中該各向異性導電黏合膜具有700gf/cm或更高的可靠性測試後黏合強度及2.5Ω或更低的可靠性測試後連接點電阻。
- 如申請專利範圍第11項之各向異性導電黏合膜,其中該各向異性導電黏合膜當固化同時以10℃/min將溫度自30℃提升至250℃時,具有1×106 gf/cm2 或更高的最小模數。
- 如申請專利範圍第11到13之任一項之各向異性導電黏合膜,其中在該各向異性導電黏合膜中,界於一聚合物黏結劑系統與一固化系統之間的固體含量比例為40:60至60:40。
- 如申請專利範圍第14項之各向異性導電黏合膜,其中該聚合物黏結劑系統包含一丙烯酸酯共聚物,及該固化系統包含雙酚茀二丙烯酸酯及經異三聚氰酸環氧乙烷改質之二丙烯酸酯。
- 一種各向異性導電黏著劑組成物,其以固體含量表示,以該各向異性導電黏著劑組成物之總量為基準,具有雙酚茀二丙烯酸酯及經異三聚氰酸環氧乙烷改質之二丙烯酸酯之總量為25至50wt%。
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JP6438102B2 (ja) * | 2017-10-19 | 2018-12-12 | デクセリアルズ株式会社 | 接続体、及び接続体の製造方法 |
KR102256785B1 (ko) * | 2018-12-05 | 2021-05-27 | 주식회사 엘지화학 | 점착제 조성물, 표면 보호 필름 및 유기 발광 전자 장치 제조 방법 |
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US9589696B2 (en) | 2017-03-07 |
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