TWI232467B - Paste for circuit connection, anisotropic conductive paste and uses thereof - Google Patents
Paste for circuit connection, anisotropic conductive paste and uses thereof Download PDFInfo
- Publication number
- TWI232467B TWI232467B TW091134757A TW91134757A TWI232467B TW I232467 B TWI232467 B TW I232467B TW 091134757 A TW091134757 A TW 091134757A TW 91134757 A TW91134757 A TW 91134757A TW I232467 B TWI232467 B TW I232467B
- Authority
- TW
- Taiwan
- Prior art keywords
- mass
- curing agent
- circuit connection
- mass percent
- anisotropic conductive
- Prior art date
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- 239000003795 chemical substances by application Substances 0.000 claims abstract description 120
- 239000010419 fine particle Substances 0.000 claims abstract description 95
- 239000003822 epoxy resin Substances 0.000 claims abstract description 75
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 75
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000002245 particle Substances 0.000 claims abstract description 50
- 150000008065 acid anhydrides Chemical class 0.000 claims abstract description 36
- 239000003054 catalyst Substances 0.000 claims description 36
- 239000007822 coupling agent Substances 0.000 claims description 35
- 239000013589 supplement Substances 0.000 claims description 33
- 239000002518 antifoaming agent Substances 0.000 claims description 19
- 239000013530 defoamer Substances 0.000 claims description 19
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 18
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 14
- 239000000178 monomer Substances 0.000 claims description 14
- 239000004593 Epoxy Substances 0.000 claims description 11
- 150000008064 anhydrides Chemical class 0.000 claims description 11
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 8
- 125000003700 epoxy group Chemical group 0.000 claims description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 7
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- 238000000034 method Methods 0.000 abstract description 25
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- 150000001346 alkyl aryl ethers Chemical class 0.000 description 4
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- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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
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Description
1232467 玖、發明說明 【發明所屬之技術領域】 本發明係關於可使用於連接平面顯示器,諸如液晶顯示 器、電激發光顯示器及電漿顯示器,電荷偶合裝置(CCD) 及半導體裝置,諸如互補金屬氧化物半導體(CMOS)用之電 路之微觀布線的電路連接膏及各異向性導電膏。本發明亦 關於使用電路連接膏或各異向性導電膏於連接電路布線之 方法。 【先前技術】 近來電視接收機、個人電腦及行動電話用之液晶顯示器 的趨勢朝向細度及小型化,因此驅動器積體電路中之布線 係以較窄的節距設置。爲確保高生產性,其上安裝積體電 路之帶式載體封裝(TCP; tape carrier package)及液晶顯示 器基板之布線係在諸如200 °C之溫度、2 MPa之壓力及10 至3 0秒之時間之嚴苛的熱壓縮黏合條件下連接。 在此種布線的連接中,習知使用諸如揭示於:TP-A-3 ( 1 99 1 )/4 67 07中之包含分散於樹脂中之導電性微細顆粒以 提供各異向性之各異向性導電薄膜。然而,各異向性導電 薄膜有成本的問題:由於薄膜製造涉及隔離物薄膜,使得 各異向性導電薄膜昂貴,且需提供專門的自動剝離機器以 塗布薄膜,因而製造成本高。此外,各異向性導電薄膜無 法展現足夠的黏合強度,且會在熱及潮濕的條件下發生連 接可靠度的降低。 用於解決問題的材料包括在室溫下爲液態之電路連接 312/發明說明書(補件)/92-02/91134757 1232467 膏、各異向性導電膏及各異向性導電性黏著劑,其如揭示 於 JP’-A- 6 2( 1 9 87)/40 1 8 3、JP-A-62( 1 9 87 )/7 62 1 5 及 JP-A-62( 1 9 87)/ 1 76 1 39。然而,此等電路連接膏、各異向性 導電膏及各異向性導電性黏著劑之黏度在熱壓縮黏合程序 中隨溫度之急遽上升而大大減小。結果,由於在熱壓縮黏 合時之液體流動,而發生空隙及滲出污染。存在於電路連 接膏、各異向性導電膏及各異向性導電性黏著劑中之導電 性顆粒部分凝聚,而在壓縮方向中造成導電失效。此外, 於電路連接膏、各異向性導電膏等等固化之後,其由於殘 留於固化產物中之氣泡,而無法在高溫及高濕下維持連接 可靠度。此外,固化產物雖然強度高,但其沒有可修復性。 因此,須要當在諸如200 °C之溫度、2MPa之壓力及1〇 至3 0秒之時間之嚴苛的熱壓縮黏合條件下固化時,可不含 氣泡且具高黏合可靠度、連接可靠度及可修復性之材料。 【發明內容】 本發明之一目的爲提供儲存安定性及分配器塗布性質優 異,在熱壓縮黏合下可不含空隙、氣泡及滲出,且在高溫 及高濕下可固化同時可確保高黏合及連接可靠度且具可修 復性之電路連接膏及各異向性導電膏。本發明之另一目的 爲提供此等膏之使用方法。 本發明之電路連接膏包括: (I) 30至80質量百分比之環氧樹脂, (II) 10至50質量百分比之選自酸酐固化劑(ΠA)及酚系 固化劑(IIB)之固化劑.,及 9 312/發明說明書(補件)/92-02/91134757 1232467 (III) 5至25質量百分比之高軟化點微細顆粒。 本發明之電路連接膏包括: (I) 30至79.9質量百分比之環氧樹脂, (II) 10至50質量百分比之選自酸酐固化劑(ΠA)及酚系 固化劑(IIB)之固化劑, (III) 5至25質量百分比之高軟化點微細顆粒,及 (V) 0.1至20質量百分比之消泡劑。 本發明之電路連接膏包括: (I) 30至79.8質量百分比之環氧樹脂, (II) 10至50質量百分比之選自酸酐固化劑(ΠA)及酚系 固化劑(IIB)之固化劑, (III) 5至25質量百分比之高軟化點微細顆粒,及 (VI) 0.1至5質量百分比之偶合劑。 本發明之電路連接膏包括: (I) 30至79.8質量百分比之環氧樹脂, (II) 10至50質量百分比之選自酸酐固化劑(IIA)及酚系 固化劑(IIB)之固化劑, (III) 5至25質量百分比之高軟化點微細顆粒, (V) 0.1至20質量百分比之消泡劑,及 (VI) 0.1至5質量百分比之偶合劑。 本發明之各異向性導電膏包括: (I) 30至80質量百分比之環氧樹脂, (II) 10至50質量百分比之選自酸酐固化劑(IIA)及酚系 固化劑(IIB)之固化劑, 10 312/發明說明書(補件)/92-02/91134757 1232467 (ΠΙ) 5至25質量百分比之高軟化點微細顆粒,及 (IV) 0.1至25質量百分比之導電性顆粒。 本發明之各異向性導電膏包括: U) 30至79.9質量百分比之環氧樹脂, (Π) 10至50質量百分比之選自酸酐固化劑(IIA)及酚系 固化劑(IIB)之固化劑, (III) 5至25質量百分比之高軟化點微細顆粒, (IV) 〇·1至25質量百分比之導電性顆粒,及 (V) 0.1至20質量百分比之消泡劑。 本發明之各異向性導電膏包括: (I) 30至79.8質量百分比之環氧樹脂, (II) 10至50質量百分比之選自酸酐固化劑(πa)及酚系 固化劑(IIB)之固化劑, (III) 5至25質量百分比之高軟化點微細顆粒, (IV) 0.1至25質量百分比之導電性顆粒,及 (VI) 0.1至5質量百分比之偶合劑。 本發明之各異向性導電膏包括: (I) 30至79.8質量百分比之環氧樹脂, (II) 10至50質量百分比之選自酸酐固化劑(IIA)及酚系 固化劑(IIB)之固化劑, (III) 5至25質量百分比之高軟化點微細顆粒, (IV) 0.1至25質量百分比之導電性顆粒, (V) 0.1至20質量百分比之消泡劑,及 (VI) 0.1至5質量百分比之偶合劑。 312/發明說明書(補件)/92-02/91134757 1232467 電路連接膏及各異向性導電膏可更包括固化催化劑 (VII)。 環氧樹脂(I)每分子平均具有至少1至6個環氧基及具有 100至7 000之根據GPC以聚苯乙烯計的平均分子量較佳。 酸酐固化劑(ΠA)係酿酸或順丁燒二酸衍生物較佳。 酚系固化劑(ΠΒ)係酚系酚醛型環氧(nov〇iak)固化劑較 佳。 高軟化點微細顆粒(III)以具有60至150 °C之軟化溫度及 0.01至2微米之原粒子大小較佳,及其係經由使(甲基)丙 烯酸甲酯及除(甲基)丙烯酸甲酯外之可共聚合單體共聚合 而製得,且包含30至70質量百分比之(甲基)丙烯酸甲酯 更佳。 導電性顆粒(IV)之表面以包含金或鎳較佳。 消泡劑(V)爲聚矽酮較佳,其係具有-80至0°C之軟化溫 度,且以具0.05至5微米之原粒子大小之顆粒存在於電路 連接膏或各異向性導電膏中之經矽酮改質之彈性體。經矽 酮改質之彈性體係希望經由將含矽酮基團接枝至環氧樹脂 而製得之彈性體。 電路連接膏或各異向性導電膏以具有30至400帕斯卡· 秒(Pa · s)之在25 °C下之黏度較佳。 電路連接膏或各異向性導電膏之使用方法包括利用電路 連接膏或各異向性導電膏使形成於一基板上之電路布線與 形成於另一基板上之電路布線連接。 根據本發明,可利用即使係在高溫及高濕下仍可具有高 . 312/發明說明書(補件)/92-02/91〗34757 •Ht / 12 1232467 黏合及連接可靠度之電路連接膏或各異向性導電膏使布線 彼此牢固連接。 可將電路連接膏或各異向性導電膏之使用方法應用至任 何一種電路材料、液晶顯示器、有機電激發光顯示器、電 發顯示器、電荷偶合裝置及半導體裝置。 根據本發明,可製得儲存安定性及分配器塗布性質優 異’在熱壓縮黏合下可不含空隙、氣泡及滲出,且在高溫 及高濕下可固化同時可確保高黏合及連接可靠度且具可修 復性之電路連接膏及各異向性導電膏。經由使用本發明之 電路連接膏或各異向性導電膏,不會於布線中產生短路, 且可維持在相鄰布線之間的絕緣性質。 【實施方式】 以下係本發明之詳細說明。 本發明之電路連接膏係說明於下之樹脂組成物。在本發 明’以下的樹脂組成物1至4皆爲電路連接膏(樹脂組成 物)。 本發明之各異向性導電膏係說明於下之樹脂組成物。在 本發明,以下的樹脂組成物5至8皆爲各異向性導電膏(樹 脂組成物)。 本發明之第一電路連接膏包括(1)30至80質量百分比之 環氧樹脂,(11)10至50質量百分比之選自酸酐固化劑(ΠΑ) 及酚系固化劑(IIB)之固化劑,及(111)5至25質量百分比之 高軟化點微細顆粒(以下稱爲樹脂組成物1)。 本發明之第二電路連接膏包括(1)30至79.9質量百分比 13 312/發明說明書(補件)/92-02/91134757 1232467 之環氧樹脂,(II) 1 0至5 0質量百分比之選自酸酐固化劑 (11六)及酚系固化劑(116)之固化劑,(111)5至25質量百分比 之高軟化點微細顆粒,及(V)O. 1至20質量百分比之消泡劑 (以下稱爲樹脂組成物2)。 本發明之第三電路連接膏包括(1)30至79.8質量百分比 之環氧樹脂,(11)10至5〇質量百分比之選自酸酐固化劑 (ΠΑ)及酚系固化劑(ΙΙΒ)之固化劑,(πΐ)5至25質量百分比 之高軟化點微細顆粒,及(V I) 0 · 1至5質量百分比之偶合劑 (以下稱爲樹脂組成物3)。 本發明之第四電路連接膏包括(1)30至79.8質量百分比 之環氧樹脂,(11)10至50質量百分比之選自酸酐固化劑 (IIA)及酚系固化劑(ΙΙΒ)之固化劑,(ΙΠ)5至25質量百分比 之高軟化點微細顆粒,(V) 0 · 1至2 0質量百分比之消泡劑, 及(VI)O.l至5質量百分比之偶合劑(以下稱爲樹脂組成物 4)。 本發明之第一各異向性導電膏包括(1)30至80質量百分 比之環氧樹脂,(11)10至50質量百分比之選自酸酐固化劑 (IIA)及酚系固化劑(IIB)之固化劑,(111)5至25質量百分比 之高軟化點微細顆粒,及(IV )0.1至25質量百分比之導電 性顆粒(以下稱爲樹脂組成物5)。 本發明之第二各異向性導電膏包括(1)30至79.9質量百 分比之環氧樹脂,(11)10至50質量百分比之選自酸酐固化 劑(IIA)及酚系固化劑(IIB)之固化劑,(111)5至25質量百分 比之高軟化點微細顆粒,(IV)O.l至25質量百分比之導電 14 312/發明說明書(補件)/92-02/91134757 1232467 性顆粒’及(V) 0.1至20質量百分比之消泡劑(以下稱爲樹 脂組成物6)。 本發明之第三各異向性導電膏包括(1)30至79.8質量百 分比之環氧樹脂,(11)10至50質量百分比之選自酸酐固化 劑(IIA)及酚系固化劑(ΠΒ)之固化劑,(111)5至25質量百分 比之高軟化點微細顆粒,(IV )0.1至25質量百分比之導電 性顆粒,及(VI)〇.l至5質量百分比之偶合劑(以下稱爲樹 脂組成物7)。 本發明之第四各異向性導電膏包括(1)30至79.8質量百 分比之環氧樹脂,(11)10至50質量百分比之選自酸酐固化 劑(IIA)及酚系固化劑(IIB)之固化劑,(111)5至25質量百分 比之高軟化點微細顆粒,(IV )0.1至25質量百分比之導電 性顆粒,(V)0.1至20質量百分比之消泡劑,及(VI)0.1至5 質量百分比之偶合劑(以下稱爲樹脂組成物8)。 樹脂組成物1至8可更包括固化催化劑(VII)。 以上的組成可製得儲存安定性及分配器塗布性質優異, 且在熱壓縮黏合下可不含空隙、氣泡及滲出之電路連接膏 及各異向性導電膏。其之固化產物即使係在高溫及高濕下 仍展現高黏合及連接可靠度,且具有可修復性。電路連接 膏及各異向性導電膏具有在壓縮固化方向中之導電性及在 其他方向中之絕緣性質的特性。以下詳細說明成份(I)至 (VII)。 環氣樹脂(I) 以1 00質量百分比之電路連接膏或各異向性導電膏(樹 15 312/發明說明書(補件)/92-02/91134757 1232467 脂組成物1至8)計,環氧樹脂(I)之量爲30至80質量百分 比,以40至70質量百分比較佳,50至65質量百分比更 佳。當樹脂組成物包含稍後說明之消泡劑(V)時,環氧樹脂 (I)係以30至79.9質量百分比使用,以40至69.9質量百 分比較佳,50至64.9質量百分比更佳。當樹脂組成物包含 稍後說明之偶合劑(VI)、或消泡劑(V)及偶合劑(VI)之組合 時,環氧樹脂(I)係以30至79.8質量百分比使用,以40至 6 9.8質量百分比較佳,50至64.8質量百分比更佳。 當環氧樹脂(I)係以樹脂組成物(100質量百分比)計爲30 質量百分比或以上使用時,可藉由電路連接膏及各異向性 導電膏之固化產物而確保黏合及連接可靠度,及在80質量 百分比或以下時,可確保電路連接膏及各異向性導電膏之 固化產物的可修復性。可修復性係可使基板再利用的性 質,即當於利用電路連接膏或各異向性導電膏使電極彼此 連接之後發生一些問題,及需使黏合電極釋放、洗滌及再 次連接時,可使經固化之膏自基板諸如玻璃基板分離,而 不會殘留的性質。 使用於本發明之環氧樹脂(I)係習知之環氧樹脂,且希望 其每分子平均包含1至6個環氧基,以平均1.2至6個較 佳,平均1.7至6個更佳。當環氧樹脂(I)每分子平均包含 1至6個環氧基時,電路連接膏及各異向性導電膏可在高 溫及高濕下展現充分的黏合及連接可靠度。 希望環氧樹脂(I)根據凝膠滲透層析術(以下稱爲GPC)以 聚苯乙烯計具有100至7000之平均分子量,以150至3000 16 312/發明說明書(補件)/92-02/91134757 1232467 較佳,3 5 0至2000更佳。以上之根據GPC以聚苯乙烯計之 平均分子量之範圍由於電路連接膏及各異向性導電膏可具 有優異的分配器塗布性質而爲較佳。在本發明,環氧樹脂 (I)可爲一環氧樹脂具有以上範圍之每分子之環氧基及另 一環氧樹脂具有以上範圍之以聚苯乙烯計之平均分子量之 環氧樹脂的任何組合。 環氧樹脂(I)在室溫下可爲液態或固態。環氧樹脂(I)之例 子包括單官能環氧樹脂(1-1)及多官能環氧樹脂(1-2),且可 使用選自此等樹脂之一或多種樹脂的組合。 單官能環氧樹脂(1-1)之例子包括脂族單縮水甘油基醚化 合物、芳族單縮水甘油基醚化合物、脂族單縮水甘油基酯 化合物、芳族單縮水甘油基酯化合物、脂環單縮水甘油基 酯化合物、含氮單縮水甘油基醚化合物、單縮水甘油丙基 聚矽氧烷化合物及單縮水甘油基烷。 脂族單縮水甘油基醚化合物包括由聚伸烷基單烷基醚與 環氧氯丙烷之反應所製得之化合物及由脂族醇與環氧氯丙 烷之反應所製得之化合物。聚伸烷基單烷基醚具有1至6 個碳原子之烷基或烯基,諸如乙二醇單烷基醚、二乙二醇 單烷基醚、三乙二醇單烷基醚、聚乙二醇單烷基醚、丙二 醇單烷基醚、二丙二醇單烷基醚、三丙二醇單烷基醚及聚 丙二醇單烷基醚。脂族醇之例子包括正丁醇、異丁醇、正 辛醇、2-乙基己醇、二羥甲基丙烷單烷基醚、羥甲基丙烷 二烷基醚、甘油二烷基醚、二羥甲基丙烷單烷基酯、羥甲 基丙烷二烷基酯及甘油二烷基酯。 17 312/發明說明書(補件)/92-02/91134757 1232467 芳族單縮水甘油基醚化合物包括由芳族醇或經烷二 如乙二醇或丙二醇改質之芳族醇與環氧氯丙烷之反應 得之化合物。芳族醇之例子包括酚、苯甲醇、二甲苯 萘酚。 脂族單縮水甘油基酯化合物包括由脂族二羧酸單烷 環氧氯丙烷之反應所製得之化合物,及芳族單縮水甘 酯化合物包括由芳族二羧酸單烷酯與環氧氯丙烷之反 製得之化合物。 多官能環氧樹脂(1-2)之例子包括脂族多價縮水甘油 化合物、芳族多價縮水甘油基醚化合物、脂族多價縮 油基酯化合物、芳族多價縮水甘油基酯化合物、脂族 縮水甘油基醚酯化合物、芳族多價縮水甘油基醚酯化 物、脂環族多價縮水甘油基醚化合物、脂族多價縮水 基胺化合物、芳族多價縮水甘油基胺化合物、內醯脲 縮水甘油基化合物、酚醛型環氧多價縮水甘油基醚化 物、環氧化二烯聚合物、3,4-環氧基-6-甲基環己基甲 3,4-環氧基-6-甲基環己烷碳酸酯及雙(2,3-環氧環戊基 脂族多價縮水甘油基醚化合物包括由聚烷二醇與環 丙烷之反應所製得之化合物及由多價醇與環氧氯丙烷 應所製得之化合物。聚烷二醇之例子包括乙二醇、二 醇、三乙二醇、聚乙二醇、丙二醇、二丙二醇、三丙 及聚丙二醇。多價醇之例子包括二羥甲基丙烷、三羥 丙烷、螺二元醇及甘油。 芳族多價縮水甘油基醚化合物包括由芳族二醇或經 312/發明說明書(補件)/92-02/91134757 醇諸 所製 酚及 酯與 油基 應所 基釀 水甘 多價 合 甘油 多價 合 基、 )醚。 氧氯 之反 乙二 二醇 甲基 烷二 18 1232467 醇諸如乙二醇或丙二醇改質之芳族二醇與環氧氯丙烷之反 應所製得之化合物。芳族二醇之例子包括雙酚A、雙酚S、 雙酚F及雙酚AD。 脂族多價縮水甘油基酯化合物包括由脂族二羧酸諸如己 二酸或伊康酸與環氧氯丙烷之反應所製得之化合物。 芳族多價縮水甘油基酯化合物包括由芳族二羧酸諸如間 苯二酸、對苯二甲酸或1,2,4,5-苯四酸與環氧氯丙烷之反 應所製得之化合物。 脂族多價縮水甘油基醚酯化合物及芳族多價縮水甘油基 醚酯化合物包括由羥基二羧酸化合物與環氧氯丙烷之反應 所製得之化合物。 脂族多價縮水甘油基胺化合物包括由脂族二胺諸如聚乙 二胺與環氧氯丙烷之反應所製得之化合物。 芳族多價縮水甘油基胺化合物包括由芳族二胺諸如二胺 基二苯基甲烷、苯胺或間二甲苯二胺與環氧氯丙烷之反應 所製得之化合物。 內醯脲多價縮水甘油基化合物包括由內醯脲或其衍生物 與環氧氯丙烷之反應所製得之化合物。 酚醛型環氧多價縮水甘油基醚化合物包括由衍生自酚或 甲酚及甲醛之酚醛型環氧樹脂與環氧氯丙烷之反應所製得 之化合物,及由多酚諸如聚烯基酚或其共聚物與環氧氯丙 烷之反應所製得之化合物。 環氧化二烯聚合物包括環氧化聚丁二烯及環氧化聚異戊 二烯。 19 312/發明說明書(補件)/92-02/91134757 1232467 固化劑(II) 酸酐固化劑(11A ) 以1 00質量百分比之電路連接膏或各異向性導電膏(樹 脂組成物1至8)計’酸酐固化劑(πA)之量爲10至50質量 百分比’以10至40質量百分比較佳,1〇至30質量百分 比更佳。當酸酐固化劑(IIA)係以樹脂組成物(1 00質量百分 比)計爲1 0質量百分比或以上使用時,樹脂組成物之固化 產物在高溫及高濕下將具有優異的黏合及連接可靠度,及 在5 0質量百分比或以下時,可防止樹脂組成物之黏度提 高,因而可獲致優異的工作性及塗布性質。 酸酐固化劑(IIA)在室溫下可爲液體或固體。對於優異的 工作性及塗布性質,使用液態固化劑爲較佳。 使用於本發明之酸酐固化劑(ΠA)可爲習知之酸酐固化 劑,諸如鄰苯二甲酸酐、順丁烯二酸酐、四氫化鄰苯二甲 酸酐、六氫化鄰苯二甲酸酐、4 -甲基四氫化鄰苯二甲酸酐、 雙環庚烯二甲酸酐、HET酐、四溴鄰苯二甲酸酐、偏苯三 甲酸酐、1,2,4,5-苯四酸酐及二苯基酮四羧酸酐。其中使用 衍生自鄰苯二甲酸或順丁烯二酸之酸酐爲較佳。此等酸酐 固化劑(IIA )可個別或結合使用。 酚系固化劑(IIB) 以1 00質量百分比之電路連接膏或各異向性導電膏(樹 脂組成物1至8)計,酚系固化劑(IIB)之量爲10至50質量 百分比,以10至40質量百分比較佳,10至30質量百分 比更佳。當酚系固化劑(II B)係以樹脂組成物(1〇〇質量百分 20 312/發明說明書(補件)/92-02/91134757 1232467 比)計爲1 〇質量百分比或以上使用時,樹脂組成物之固化 產物在高溫及高濕下將具有優異的黏合及連接可靠度,及 在50質量百分比或以下時,可防止樹脂組成物之黏度提 高,因而可獲致優異的工作性及塗布性質。 酚系固化劑(II Β)在室溫下可爲液體或固體,且可個別或 結合使用具至少兩官能基之酚系固化劑。關於酚系固化劑 (ΙΙΒ),可使用揭示於JP-A-6(1994)/100667中之酚系固化 劑。明確的例子包括苯基化合物或萘化合物與醛、酮、芳 族化合物或脂環族化合物之縮合物。苯基化合物之例子包 括酚、甲酚、乙酚及丙酚。萘化合物之例子包括萘酚及 /3 -萘酚。醛之例子包括甲醛(福馬林)及三聚甲醛。酮之例 子包括丙酮及苯乙酮。芳族化合物之例子包括苯二甲基及 二乙烯苯。脂環族化合物之例子包括二環戊二烯。 酚系固化劑(ΙΙΒ)可爲習知之酚系固化劑,以衍生自酚或 甲酚及甲醛之酚系酚醛型環氧固化劑較佳。 高軟化點微細顆粒(ΙΤΠ 使用於電路連接膏及各異向性導電膏(樹脂組成物1至 8)中之在軟化溫度或以上熔融於樹脂組成物中之高軟化點 微細顆粒(III)可提高糊黏度而控制其之流度,且可賦予電 路連接膏及各異向性導電膏可修復性。 以樹脂組成物(1 00質量百分比)計,高軟化點微細顆粒 (III)之量爲5至25質量百分比,以10至20質量百分比較 佳,13至18質量百分比更佳。當高軟化點微細顆粒(ΠΙ) 係以樹脂組成物(1 〇〇質量百分比)計爲5質量百分比或以 21 312/發明說明書(補件)/92-02/91134757 1232467 上使用時,可抑制在熱壓縮黏合下之空隙及滲出的發生, 及在25質量百分比或以下時,電路連接膏或各異向性導電 膏之黏度不會增加至阻礙塗布工作的程度,因而可獲致優 異的工作性,諸如分配器塗布性質。 高軟化點微細顆粒(III)可爲具有60至150 °C之軟化溫 度,以70至120 °C較佳,及0.01至2微米之原粒子大小, 以0· 1至1微米較佳之習知之高軟化點微細顆粒。在本發 明,高軟化點微細顆粒(III)可爲一微細顆粒具有以上範圍 之軟化溫度及另一微細顆粒具有以上範圍之原粒子大小之 微細顆粒的任何組合。原粒子大小係指不再可機械分離之 顆粒的大小。軟化溫度爲60 °C或以上較佳,由於該溫度可 使電路連接膏及各異向性導電膏在室溫下具有優異的儲存 安定性。當軟化溫度爲150°C或以下時,在150至200°C下 之熱壓縮黏合程序中可抑制電路連接膏及各異向性導電膏 之流動,且亦可賦予可修復性。高軟化點微細顆粒(III)之 原粒子大小以工作性諸如分配器塗布性質及連接可靠度的 觀點來看爲0.01至2微米較佳。 高軟化點微細顆粒(III)可經由製備高軟化點微細顆粒 (III)之乳液,及將溶液噴霧乾燥而製得。乳液可經由使單 體,例如(甲基)丙烯酸甲酯,以30至70質量百分比之量 與70至30質量百分比之其他可共聚合單體共聚合而製 得。此處使用之可共聚合單體爲多官能單體較佳。經由使 用多官能單體,可於乳液微細顆粒中形成輕度交聯的結構。 當將由乳液製得之高軟化點微細顆粒(III)使用於電路連 22 312/發明說明書(補件)/92-02/91134757 1232467 接膏及各異向性導電膏中時,可進一步改良電路連接膏及 各異向性導電膏之室溫儲存安定性,且可進一步抑制由熱 壓縮黏合所造成之空隙及滲出的發生。 單體之例子包括丙烯酸酯,諸如(甲基)丙烯酸甲酯、(甲 基)丙烯酸乙酯、(甲基)丙烯酸丙酯、(甲基)丙烯酸丁酯、(甲 基)丙烯酸2-乙基己酯、(甲基)丙烯酸戊酯、(甲基)丙烯酸 十六酯、(甲基)丙烯酸十八酯、(甲基)丙烯酸丁氧乙酯、(甲 基)丙燒酸苯氧乙酯、(甲基)丙烯酸2-羥乙酯及(甲基)丙烯 酸縮水甘油酯;丙烯酸系醯胺;酸單體,諸如(甲基)丙烯 酸、伊康酸及順丁烯二酸之單體;及芳族乙烯基化合物, 諸如苯乙烯及苯乙烯衍生物。 用於在乳液微細顆粒中形成輕度交聯結構之多官能單體 的例子包括二乙烯苯、二丙烯酸酯及共軛二烯,諸如1,3-丁二烯、1,3-戊二烯、異戊二烯、i,3 -己二烯及氯丁二烯。 使乳液微細顆粒在其之表面輕度交聯的範例方法包括經 由金屬交聯乳液微細顆粒之表面層之環氧基、羧基及胺基 的離子交聯聚合物交聯。藉由如以上所形成之在乳液微細 顆粒中之輕度交聯結構,微細顆粒在室溫下變得較不溶解 於環氧樹脂(I)或溶劑等等中,且可增進電路連接膏及各異 向性導電膏之儲存安定性。 導電性顆粒(IV) 以樹脂組成物(1 0 0質量百分比)計,使用於各異向性導電 膏(樹脂組成物5至8)中之導電性顆粒(IV)之量爲0.1至25 質量百分比,以1至20質量百分比較佳,2至15質量百 23 312/發明說明書(補件)/92-02/91134757 1232467 分比更佳。當導電性顆粒(IV)係以樹脂組成物(100質量百 分比)計在0.1及25質量百分比之間使用時’可賦予各異 向性導電膏充分的導電性。 使用於各異向性導電膏中之導電性顆粒(IV)可爲習知之 導電性顆粒。明確的例子包括貴金屬諸如金、鎳、銀及鉑 之導電性顆粒;貴金屬合金諸如銀-銅合金、金-銅合金及 鎳合金之導電性顆粒;及經由將有機聚合物微細顆粒諸如 聚苯乙烯微細顆粒塗布前述之貴金屬及貴金屬合金而製得 之導電性顆粒。較佳者爲金或鎳之導電性貴金屬顆粒,及 經塗布金或鎳之貴金屬塗層之有機聚合物微細顆粒。所謂 將有機聚合物微細顆粒塗布金或鎳之貴金屬塗層係指有機 聚合物微細顆粒之表面包含金或鎳。市售的產品包括 Sekisui Fine Chemicals Division, Seki sui Chemical Co., Ltd 之Micropearl AU™系列。導電性顆粒之顆粒大小範圍係自 2至20微米較佳。 消泡劑(V) 使用於電路連接膏及各異向性導電膏(樹脂組成物2、4、 6及8)中之消泡劑(V)可爲習知之消泡劑。明確言之,可舉 矽酮消泡劑及氟消泡劑爲例。使用矽酮消泡劑爲較佳,及 聚砂酮更佳。 以樹脂組成物(1 0 0質量百分比)計,消泡劑(V)之量爲〇. 1 至20質量百分比,以0.1至15質量百分比較佳,〇.5至15 質量百分比更佳。當消泡劑(V)係以〇 · 1質量百分比或以上 使用於樹脂組成物(1 0 0質量百分比)中時,電路連接膏及各 讎 312/發明說明書(補件)/92-02/91134757 24 1232467 異向性導電膏幾乎不會有氣泡產生且於固化之後不含氣 泡,及在20質量百分比或以下時,電路連接膏及各異向性 導電膏將具有優異的分配器塗布性質及黏著力,且可抑制 於固化後之氣體障壁性質的減小。 聚矽酮爲經矽酮改質之彈性體較佳。當聚矽酮爲彈性體 時,電路連接膏及各異向性導電膏之固化產物更能抵抗外 部物理衝擊及熱驟變試驗中之熱應變。當聚矽酮爲經矽酮 改質之彈性體時,外部物理衝擊及熱驟變試驗中之熱應變 可再更經減輕。矽酮改質係指含官能基之矽酮接枝鍵結至 彈性體。 聚矽酮係經由將含矽酮基團接枝至與作爲電路連接膏或 各異向性導電膏之成份之環氧樹脂(I)不同之環氧樹脂而 製備得之經矽酮改質之彈性體較佳。一般而言,環氧樹脂 及矽酮彼此具低相容性,而易產生相分離。因此,將包含 經接枝環氧樹脂之經矽酮改質之彈性體使用作爲聚矽酮, 以致聚矽酮可均勻地分散於電路連接膏及各異向性導電膏 中〇 希望聚矽酮具有-80至0°C之軟化溫度,以-80至-20 °C較 佳,_80至-40°C更佳。當軟化溫度在以上範圍內時,可改 良減輕外部物理衝擊及熱驟變試驗中之熱應變的效應,因 而可確保高的黏合強度。 希望聚矽酮係具0.0 5至5微米之原粒子大小,以0.1至 3.5微米較佳,〇·1至2微米更佳之似橡膠聚合物的微細顆 粒。當原粒子大小爲0 · 0 5微米或以上時,聚矽酮不會於電 25 312/發明說明書(補件)/92-02/91134757 1232467 路連接膏及各異向性導電性顆粒中凝聚,且膏之黏度經安 定化’而可有優異的工作性,諸如分配器塗布性質。利用 具有* 5微米或以下之原粒子大小的聚矽酮,含有聚矽酮之 電路連接膏及各異向性導電膏將具有優異的工作性,諸如 分配器塗布性質,且於固化之後可確保高黏合強度。在本 發明’聚矽酮可爲一聚矽酮具有以上範圍之軟化溫度及另 一聚砂酮具有以上範圍之原粒子大小之聚矽酮的任何組 製備聚矽酮之範例方法包括使用矽酮橡膠之微細顆粒的 方法;揭示於JP-A-60(1985)/72957中之方法;將雙鍵引入 至環氧樹脂,使雙鍵與可與雙鍵反應之含氫矽酮反應,因 而產生接枝產物,及使矽酮橡膠單體在接枝產物之存在下 聚合之方法;將雙鍵引入至環氧樹脂,及使雙鍵與可與雙 鍵聚合之含乙烯基之矽酮橡膠單體反應,因而產生接枝產 物之方法;及使矽酮橡膠單體在以上之接枝產物之存在下 聚合的方法。較佳者爲產生接枝產物之方法及在接枝產物 之存在下不使用矽酮橡膠之微細顆粒而產生矽酮橡膠顆粒 之方法。利用此等方法製得之聚矽酮當經分散時僅造成黏 度的輕微增加,因此可得到良好的分配器塗布性質。 將含矽酮基團接枝至環氧樹脂之經矽酮改質之彈性體可 良好地製造如下:加入於分子中具有甲氧基之矽酮中間 體,以與經引入丙烯酸殘基之環氧樹脂及丙烯酸酯化合物 之共聚物反應,因而產生經改質環氧樹脂及矽酮樹脂之接 枝產物,及將雙組份冷固化矽酮橡膠加至接枝產物。 親 312/發明說明書(補件)/92-02/91134757 26 1232467 更明確言之,在具氧大氣諸如空氣中將丙烯酸或甲基丙 烯酸加至環氧樹脂,諸如雙酚F,以產生具有雙鍵之經引 入(甲基)丙烯酸殘基之環氧樹脂。使經引入丙烯酸殘基之 環氧樹脂與丙烯酸酯化合物,諸如丙烯酸羥乙酯或丙烯酸 丁酯,在自由基聚合引發劑諸如偶氮雙異丁腈之存在下共 聚合,而製得共聚物。加入於分子中具有甲氧基之矽酮中 間體以與共聚物在催化劑諸如月桂酸二丁錫之存在下反 應,因而經由去甲醇作用產生經改質環氧樹脂及矽酮樹脂 之接枝產物。及加入雙組份冷固化矽酮橡膠,以與接枝產 物反應,因而製得其中矽酮橡膠之交聯微細顆粒經均勻分 散之經矽酮改質之彈性體。 偶合劑(VI) 利用使用於電路連接膏及各異向性導電膏(樹脂組成物 3、4、7及8)中之偶合劑(VI)於提高在樹脂組成物與基板 之間之黏著力及增進.在形成於一基板上之電路布線與形成 於另一基板上之電路布線之間的黏著力。以樹脂組成物 (100質量百分比)計,其係以0.1至5質量百分比使用,以 0 · 1至4質量百分比較佳,0. 1至3質量百分比更佳。當以 樹脂組成物(100質量百分比)計,偶合劑(VI)係以0.1質量 百分比或以上使用時,在電路連接膏或各異向性導電膏與 基板之間之黏著力增加,及在5質量百分比或以下時,經 固化之膏將具有足夠的硬度,且可降低對周圍組件的污染。 偶合劑(VI)可爲習知之偶合劑。明確的例子包括三烷氧 矽烷化合物及甲基二烷氧矽烷化合物。三烷氧矽烷化合物 27 312/發明說明書(補件)/92-02/91134757 1232467 包括r -縮水甘油氧丙基三甲氧矽烷、γ-縮水甘油氧丙基三 乙氧矽烷、胺丙基三甲氧矽烷、γ-胺丙基三乙氧矽烷、 Ν-胺乙基-γ-亞胺丙基三甲氧矽烷、γ-硫醇丙基三甲氧矽烷 及γ-異氰酸丙基三乙氧矽烷。甲基二烷氧矽烷化合物包括 縮水甘油氧丙基甲基二甲氧矽烷、γ-縮水甘油氧丙基甲 基二乙氧矽烷、γ-胺丙基甲基二甲氧矽烷、胺丙基甲基 二乙氧矽烷、Ν-胺乙基-γ-亞胺丙基甲基二甲氧矽烷、r-硫醇丙基甲基二甲氧矽烷及異氰酸丙基甲基二乙氧矽烷。 固化催I,劑(VII) 使用於電路連接膏及各異向性導電膏(樹脂組成物1至 8)中之固化催化劑(VII)在環氧樹脂(I)及酸酐固化劑(ΙΙΑ) 或酚系固化劑(ΙΙΒ)之反應中作爲催化劑,且明確言之,其 之添加目的係要使樹脂組成物於非常短的時間內固化。固 化催化劑(VII)可選自熟知之環氧固化催化劑。尤其,使用 將可在40 °C或以上之加熱溫度下引發熱固化之潛在的環 氧固化催化劑較佳。固化催化劑(VII)並不包含酸酐固化劑 (IIA)及酚系固化劑(IIB)。 將可在40°C或以上之加熱溫度下引發熱固化之潛在固 化催化劑的例子包括二氰二醯胺,其之衍生物及二醯肼化 合物,諸如己二酸二醯肼及間苯二酸酯二醯胼。亦可使用 咪唑化合物之衍生物及其之經改質產物,即咪唑固化催化 劑。咪唑固化催化劑之例子包括咪唑衍生物,諸如2-甲基 咪唑、2-乙基-4-甲基咪唑及2-正十五基咪唑;經咪唑改質 之衍生物,諸如咪唑化合物及芳族酸酐之錯合物及咪唑化 28 312/發明說明書(補件)/92-02/91134757 1232467 合物及環氧樹脂之加成物;及微膠囊化的經改質產物。 微膠囊化的經改質產物,即微膠囊化的咪唑固化催化 劑,包括於微小外殻中囊封爲芯材之2-甲基咪唑、2-乙基 -4 -甲基咪唑及2 -正十五基咪唑。 以100質量百分比之樹脂組成物(1-8)計,希望固化催化 劑(VII)係以15質量百分比或以下使用,以1至10質量百 分比較佳。不多於15質量百分比之量產生固化環氧樹脂之 特性,以致可得到高黏合可靠度。 在將單獨的固化催化劑(VII)使用於電路連接膏及各異 向性導電膏中,同時未使用酸酐固化劑(IIA)或酚系固化劑 (IIB)之情況中,樹脂組成物將經由環氧樹脂(I)之離子聚合 作用固化,但其之性質可能較利用酸酐固化劑(IIA)或酚系 固化劑(II B)之固化產物不足夠。 其他添加劑 可將其他添加劑,諸如無機塡料及溶劑,加至電路連接 膏及各異向性導電膏(樹脂組成物1至8)。 無機塡料之添加目的爲黏度控制及降低固化產物之熱應 力’且其可選自熟知之無機化合物。無機塡料之例子包括 碳酸鈣、碳酸鎂、硫酸鋇、硫酸鎂、矽酸鋁、矽酸鉻、氧 化鐡、氧化鈦、氧化鋁(鋁氧)、氧化鋅、二氧化矽、鈦酸 鉀、高嶺土、滑石、粉狀石綿、粉狀石英、雲母及玻璃纖 維。 希望無機塡料之顆粒大小爲2微米或以下,以〇. 〇 1至1 微米較佳,但如其不會影響電路連接膏及各異向性導電膏 29 312/發明說明書(補件)/92-02/91134757 Π7刀 1232467 之導電性,則其並不受限於此。希望無機塡料係以樹脂組 成物(100質量百分比)計40質量百分比或以下使用,以5 至30質量百分比較佳,但如其不會影響電路連接膏及各異 向性導電膏之導電性,則其之量並不特別受限於此。 無機塡料係部分或完全經以無機塡料(丨〇 〇質量百分比) S十爲1至50質量百分比之量的環氧樹脂⑴及/或偶合劑 (VI)接枝改質較佳。換言之,使用於本發明之無機塡料以 具有1至5 0 %之以利用重複溶劑淸潔測得之重量增加表示 的接枝百分比較佳。 用於測得接枝百分比之重複溶劑淸潔係進行如下。使經 πβ分或完全接枝改質之無機塡料以10至20倍質量之以下 溶劑潤濕及過濾5至1 0次。未參與接枝改質之環氧樹脂⑴ 及偶合劑(VI)經由此過濾而被洗掉。溶劑之例子包括環氧 樹脂(I)及偶合劑(VI)之良好溶劑,諸如丙酮、甲基乙基酮、 甲醇、乙醇、甲苯及二甲苯。於過濾之後,將殘留的無機 塡料乾燥及稱重。測得値爲經接枝改質之無機塡料的乾質 量。將測量値代至下式,以求得重量增加。除了重複溶劑 淸潔之外,接枝百分比亦可使用前述溶劑利用連續索司勒 (Soxhlet)萃取而測得。 [式] 接枝百分比(%)··[(於接枝改質後之無機塡料的乾質量-於 接枝改質前之無機塡料的乾質量)/於接枝改質前之無機 塡料的乾質量]X 100。 溶劑之明確例子包括酮溶劑,諸如甲基乙基酮、甲基異 1232467 丁基酮及環己酮;醚溶劑,諸如二乙二醇二甲基醚、甲基 卡必醇、乙基卡必醇及丁基卡必醇;乙酸乙酯、二乙二醇 二乙酸酯及烷氧基二乙二醇單乙酸酯。溶劑之量並無特殊 之限制,且溶劑係以於電路連接膏及各異向性導電膏固化 之後不會殘留於其中之量使用。 本發明之電路連接膏及各異向性導電膏之製備並無特殊 之限制,以下係一例子。利用道耳吞混合機(Dalt〇n,s mixer) 在室溫下將前述之環氧樹脂(I)、固化劑(II)、高軟化點微 細顆粒(III)、消泡劑(V)及偶合劑(VI)預捏合,然後再利用 三輥磨捏合。爲製備電路連接膏,將固化催化劑(VII)加至 以上之混合物並與其混合,利用道耳吞混合機將所得混合 物在真空中捏合及脫氣。爲製備各異向性導電膏,將導電 性顆粒(IV)及固化催化劑(VII)加至以上之混合物並與其混 合,利用道耳吞混合機將所得混合物在真空中捏合及脫氣。 希望如此製備得之電路連接膏及各異向性導電膏具有 30至400帕斯卡•秒之在25 °C下之黏度,以40至200帕 斯卡•秒較佳,5 0至1 5 0帕斯卡•秒更佳(e Η ·型黏度計, 2.5 rpm)。藉由30帕斯卡•秒或以上之膏黏度,可抑制在 利用熱壓縮黏合固化時之樹脂流動(其係氣泡產生的原 因),及藉由4 0 0帕斯卡•秒或以下,可達到優異的分配器 電 導 性 向 異 各 及 。 膏 質接 性連 布路 塗電 細 電路連接膏及各異向性導電膏之用途係與電路布線之連 接相關。在此將說明連接液晶顯示器之電路布線之方法。 312/發明說明書(補件)/92-02/91134757 : 1232467 如圖1所示,步驟1包括利用分配器將電路連接膏或各 異向性導電膏塗布於液晶顯示器基板之預定區域上。在步 驟2中,使液晶顯示器基板與TCP、經安裝1C之電路基板 對準。在步驟3中,經由於固定狀態中熱壓,而使電路連 接膏或各異向性導電膏固化。經由此等步驟1至3而在液 晶顯示器基板與TCP之間形成導電電路。 在步驟1之電路連接膏或各異向性導電膏之分配器塗布 中,可將整個分配器在20至5 0°C下預熱。電路連接膏或 各異向性導電膏可利用電腦控制塗布,諸如在分配器塗布 中,或以人工塗布至適當區域。 在步驟3之經由於固定狀態中熱壓而使電路連接膏或各 異向性導電膏固化中,希望將熱壓用之電熱板控溫於1 00 至3 00 °C,以120至25 0 °C較佳。熱壓中之壓縮壓力係0.1 至5 MPa,在此壓力下電極接點經均等地熱壓。在加壓中, 可將一橡膠氈或其類似物插置於電極與壓台面之間。 經由利用本發明之電路連接膏或各異向性導電膏使液晶 顯示器基板與TCP之布線以上述方式連接,可達成連接, 而可僅於熱壓縮黏合之方向中有導電性。因此,可維持在 相鄰布線之間的絕緣性質,且可使布線以高連接可靠度連 接。 雖然已於液晶顯示器上說明連接電路布線之方法,但此 方法亦可應用至其他平面顯示器,諸如有機電激發光顯示 器及電漿顯示器之電路布線的連接。可將電路連接膏及各 異向性導電膏使用於電路材料、電荷偶合裝置(CCD)及半 32 312/發明說明書(補件)/92-02/91134757 1232467 導體裝置諸如CMOS之布線的連接。 (實施例) 本發明將由以下實施例作更詳細說明,但不應將本發明 解釋爲受限於實施例。 實施例及比較實施例中之試驗及測量係利用以下方法進 行。 1 .儲存安定性之試驗 測量電路連接膏或各異向性導電膏之25 °C下之黏度,並 將其使用作爲標準。將電路連接膏或各異向性導電膏置於 聚乙烯容器中,及將容器密閉及儲存於-1 0°C下之恒溫槽 中。30天後測量25 t下之黏度,及以黏度增加爲基準而評 估儲存安定性。 A A :低於1 0 % B B : 1 0 %至低於5 0 % C C ·· 5 0 %或以上 2 .塗布件質之試驗 將電路連接膏或各異向性導電膏塡裝至10-cc之注射器 中並脫氣。利用分配器(MUSA SHI ENGINEERING,INC.之 S H〇TM AS TER)在4公分/秒之速率下塗布膏,及基於以下 標準而評估塗布性質。 AA :無滲出,無牽絲及良好的外觀 B B :無滲出,無牽絲但不良的外觀 CC :由於顯著低劣的塗布性質而導致滲出及牽絲 3.膠凝時間測量 33 312/發明說明書(補件)/9102/91134757 1232467 將1克量之電路連接膏或各異向性導電膏置於15CTC之 電熱板上,並以刮勺攪拌。測量自將樹脂組成物置於電熱 板上至最終牽絲的時間,因而測得膠凝時間。 4.黏合強度測量 手[J 用分配器(MUSASHI ENGINEERING, INC.之 SHOTM AS TER)使1克量之電路連接膏或各異向性導電膏於 低鹼性玻璃板上牽引。利用2 3 0°C之陶瓷工具以2 MPa之 壓力使玻璃板壓縮於試驗TAB (帶材自動黏合)薄膜上並與 其層合30秒。於在恒溫爐中在25 °C及50% RH(相對濕度) 下儲存24小時後,利用拉伸強度試驗儀(Intesco Corporation製造)測量剝離強度(黏合強度:克/公分)。 5 .空隙之確認 利用分酉己器(MUSAS HI ENGINEERING,INC.之 SHOTM AS TER)使1克量之電路連接膏或各異向性導電膏於 低鹼性玻璃板上牽引。利用230°C之陶瓷工具以2 MPa之 壓力使玻璃板壓縮於試驗TAB薄膜上並與其層合30秒。 於冷卻後,利用顯微鏡觀察接點,及基於以下標準進行評 估。 AA :無空隙,無滲出及良好的外觀 BB :在凸塊之間觀察到一些空隙及不良的外觀 CC :於整個接點中產生空隙及滲出 6 .氣泡產生之確認 利用分配器(MUSAS HI ENGINEERING, INC.之 SHOTM AS TER)將1克量之電路連接膏或各異向性導電膏塗 34 312/發明說明書(補件)/92-02/91134757 1232467 布至低鹼性玻璃板。利用230°C之陶瓷工具以2 MPa之壓 力使玻璃板壓縮於試驗TAB薄膜上並與其層合3〇秒。於 冷卻後,利用顯微鏡觀察接點,及基於以下標準進行評估。 AA :無氣泡及良好的外觀 B B :在凸塊之間觀察到一些氣泡 CC :於整個接點中觀察到氣泡 7.導電性測量 利用分配器(MUSASHI ENGINEERING, INC.之 S Η OTM AS TER)將1克量之電路連接膏或各異向性導電膏塗 布至具有ITO(銦錫氧化物)布線之低鹼性玻璃板。利用230 °C之陶瓷工具以2 MPa之壓力使玻璃板壓縮於試驗TAB薄 膜上並與其層合30秒。於層合之後立即測量在ITO電極與 試驗TAB薄膜上之電極之間的電阻(Ω),及於在60 °C及95% RH下儲存600小時後,再次測量電極之間的電阻。 8 .布線短路之試驗 利用分配器(MUSASHI ENGINEERING,INC.之 S H〇TM AS TER)使1克量之電路連接膏或各異向性導電膏於 具有ITO布線之低鹼性玻璃板上牽引。利用230 °C之陶瓷 工具以2 MPa之壓力使玻璃板壓縮於試驗TAB薄膜上並與 其層合30秒。於冷卻之後,檢查相鄰ITO電極之間的導電 性,並基於以下標準進行評估。 AA :確保絕緣 BB :導電 9.可修復件試験 35 312/發明說明書(補件)/92-02/91134757 1232467 利用分配器(MUSA SHI ENGINEERING,INC·之 S H〇TM AS TER)使1克量之電路連接膏或各異向性導電膏於 低鹼性玻璃板上牽引。利用230 °C之陶瓷工具以2 MPa之 壓力使玻璃板壓縮於試驗TAB薄膜上並與其層合30秒。 於冷卻後,以溶劑洗滌層合物,並將試驗TAB薄膜剝離。 然後利用顯微鏡觀察低鹼性玻璃板之表面,並基於以下標 準進行評估。 AA :無樹脂殘留及良好的外觀 B B :樹脂部分殘留及不良的外觀 CC :樹脂殘留於整個表面上 [合成實施例1 ] 高軟化點微細顆粒之合成 將4 00克之離子交換水置於設有攪拌器、氮氣入口、溫 度計及迴流冷凝器之1 000毫升的四頸燒瓶中。邊攪拌邊將 1.0克之烷基二苯基醚二磺酸鈉引入至燒瓶,然後再將其 加熱至65 °C。邊將溫度維持於65 °C及繼續攪拌,邊加入 0.4克之過硫酸鉀,隨後再4小時連續逐滴加入經由利用 均化器將包含1.2克之第三-十二烷基硫醇、156克之丙烯 酸正丁酯、4.0克之二乙烯苯、3.0克之烷基二苯基醚二磺 酸鈉及200克之離子交換水之溶液乳化而製備得之混合溶 液。當逐滴添加完成時,進一步進行反應2小時,及將2 3 2 克之甲基丙烯酸甲酯一次加入。於進行反應1小時後,將 8克丙烯酸於1小時之期間內連續加入’並在6 5 °C之恒溫 下進行反應2小時,隨後再冷卻。利用氫氧化鉀將生成溶 ή Ms W發明說明書(補件)/92-02/91134757 36 1232467 液中和至pH = 7,因而製得含40.6質量百分比固體之乳液。 利用噴霧乾燥機將1 000克之乳液噴霧乾燥,而得具0.1 % 或以下之濕氣含量之約400克的高軟化點微細顆粒。高軟 化點微細顆粒具有8 0 °C之軟化溫度。 利用次微米顆粒分析儀(購自Beckman Coulter,Inc.之 N4PLUS)測量高軟化點微細顆粒之顆粒大小,測得其爲180 奈米。 [合成實施例2] 低軟化點微細顆粒之合成 將4 00克之離子交換水置於設有攪拌器、氮氣入口、溫 度計及迴流冷凝器之1 000毫升的四頸燒瓶中。邊攪拌邊將 1.0克之烷基二苯基醚二磺酸鈉引入至燒瓶,然後再將其 加熱至651。邊將溫度維持於65 °C及繼續攪拌,邊加入 0.4克之過硫酸鉀,隨後再4小時連續逐滴加入經由利用 均化器將包含1.2克之第三-十二烷基硫醇、156克之丙烯 酸正丁酯、4.0克之二乙烯苯、3.0克之烷基二苯基醚二磺 酸鈉及200克之離子交換水之溶液乳化而製備得之混合溶 液。當逐滴添加完成時,進一步進行反應2小時,及將1 42 克之甲基丙烯酸甲酯及90克之丙烯酸正丁酯一次加入。於 進行反應1小時後,將8克丙烯酸於1小時之期間內連續 加入,並在65 °C之恒溫下進行反應2小時,隨後再冷卻。 利用氫氧化鉀將生成溶液中和至pH = 7,因而製得含40.6 質量百分比固體之乳液。 利用噴霧乾燥機將1 000克之乳液噴霧乾燥,而得具0.1% 37 312/發明說明書(補件)/92-〇2/91134757 1232467 或以下之濕氣含量之約400克的低軟化點微細顆粒。低車欠 化點微細顆粒具有40°C之軟化溫度。 利用合成實施例1所使用之次微米顆粒分析儀測量低軟 化點微細顆粒之顆粒大小,測得其爲1 80奈米。 [合成實施例3] 矽酮彈性體(A)之合成 於設有攪拌器、氣體入口、溫度計及冷凝器之2000毫升 的四頸燒瓶中加入600克之於分子中具有兩環氧基之雙酚 F 環氧樹月旨(DAINIPPON INK AND CHEMICALS, INCORPORATED製造之EPICLON 830S)、12克之甲基丙燦 酸、1克之二甲基乙醇胺及50克之甲苯。邊引入空氣邊在 1 1 0 °C下進行反應5小時,因而於分子中引入雙鍵。然後加 入5克之丙烯酸羥酯、10克之丙烯酸丁酯及1克之偶氮雙 異丁腈,及在70°C下進行反應3小時,並再在90°C下反應 1小時。接下來於真空中在1 1 0 °C下將甲苯移除。然後加入 70克之於分子中具有甲氧基之砂酮中間體(Dow Corning To ray Silicone Co.,Ltd.)及 0.3 克之二月桂酸二丁錫,及在 1 50 °C下進行反應1小時。爲移除產生的甲醇,再多進行反 應1小時。於生成的接枝產物中加入300克量之冷固化雙 組份矽酮橡膠(Shin· Etsu Silicones製造之KE-1204)的1比 1混合物,並進行反應2小時,因而製得其中之交聯矽酮 橡膠微細顆粒經均勻分散的矽酮彈性體(A)。 使矽酮彈性體(A)在光固化催化劑之存在下於低溫下快 速固化。利用電子顯微鏡觀察固化產物之破裂橫剖面中的 38 312/發明說明書(補件)/92-02/91134757 1232467 將高軟化點微細顆粒(III)改爲於合成實施例2中合成得之 低軟化點微細顆粒,及其他成份係以表1所示量使用。結 果示於表2。 如表2所示,實施例1至9之電路連接膏經試驗評估爲 有利。
實施例 比較賓 Σ施例 1 2 3 4 5 6 7 8 9 1 2 組成物(重量份數) (I)環氧樹脂 58 60 60 60 58 60 30 79 40 63 57 (IIA)酸酐固化劑 12 14 14 14 13 15 25 10 50 17 10 (III)高軟化點微細顆粒 15 15 15 21 15 21 25 6 5 - - 低軟化點微細顆粒 - - - - 15 (V)消泡劑 矽酮A 10 10 - - 10 - 17 2 3 15 13 ϊ夕酮B - - 10 - - - - - - - - (VI)偶合劑 1 1 1 1 - - 1 1 1 1 1 (VII)固化催化劑 4 - - 4 4 4 2 2 1 4 4 總計 100 100 100 100 100 100 100 100 100 100 100 酸酐固化劑:RIKACID MH-700(New Japan Chemical Co., Ltd.) 高軟化點微細顆粒:軟化溫度=80 °C 低軟化點微細顆粒:軟化溫度=40°C 矽酮A :矽酮彈性體(A) 矽酮 B :直鏈矽酮 DC 3 037 (Shin-Etsu Silicones) 固化催化劑:經咪唑改質之微膠囊化化合物 41 326\總檔\91 \91134757W1134757(¾抱 V1 1232467 93. 5. 替換頁 表2
實施例 比較實施例 1 2 3 4 5 6 7 8 9 1 2 評估項目 (1)儲存安定性 AA AA AA AA AA AA AA AA AA AA CC (2)塗布性質 AA AA AA AA AA AA AA AA AA AA CC (3)膠凝時間(秒) 14 27 26 12 14 1 12 24 20 26 14 13 (4)黏合強度(g/cm) 1250 1150 910 930 830 870 940 1010 970 560 470 (5)空隙 AA AA AA AA AA AA AA AA AA CC BB (6)氣泡產生 AA AA AA BB AA BB AA AA AA BB AA ⑺導電性 於層合之後立即測量 10Ω 10Ω 10Ω 10Ω 10Ω 10Ω 10Ω 10Ω 10Ω 10Ω 16Ω 於在60°C及95%RH 下儲存600小時後 10Ω 10Ω 11Ω 10Ω 10Ω 11Ω 10Ω 10Ω 11Ω 17Ω 32 Ω (8)布線短路 AA AA AA AA AA AA AA AA AA AA AA (9)可修復性 AA AA AA AA AA AA AA AA AA CC BB
[實施例1 0 ] 在室溫下先利用道耳吞混合機將環氧樹脂(I):雙酚A環 氧樹脂、酸酐固化劑(IIA):氫化4-甲基鄰苯二甲酸酐(New Japan Chemical Co·,Ltd.製造之 RIKA CID MH-700)、高軟化 點微細顆粒(III):於合成實施例1中合成得之高軟化點微 細顆粒、消泡劑(V):於合成實施例3中合成得之矽酮彈性 體(A)、及偶合劑(VI) : r -縮水甘油氧丙基三甲氧矽烷 (Shin-Etsu Silicones製造之ΚΒΜ·403)預捏合,然後再利用 三輥磨捏合。於將導電性顆粒(IV) : M i c r 〇 p e a r 1 Au-205(Sekisui Chemical Co.,Ltd.製造;比重 2.67)及固化 催化劑(VII):經咪唑改質之微膠囊化化合物(Asahi Kasei Epoxy Corporation 製造之 NOVACURE HX3748)與捏合產物 混合之後’利用道耳吞混合機在真空中將混合物捏合並脫 氣。成份之添加量不於表3。 利用前述之試驗方法評估如此製得之各異向性導電膏。 42 326V總檔\91 \91134757\91134757(替換)-1 1232467 93. 5. 17 替換頁 結果示於表4。 [實施例Π] - 以與實施例1 〇相同之方式製備及評估各異向性導電 膏,除了未使用固化催化劑(VII),及其他成份係以表3所 示量使用。結果示於表4。 [實施例1 2 ] 以與實施例1 〇相同之方式製備及評估各異向性導電 膏,除了將消泡劑(V)由矽酮彈性體(A)改爲直鏈矽酮B (Shin-Etsu Silicones製造之〇〇3037),及其他成份係以表3 所示量使用。結果示於表4。 [實施例1 3 ] 以與實施例1 〇相同之方式製備及評估各異向性導電 膏,除了未使用偶合劑(VI),及其他成份係以表3所示量 使用。結果示於表4。 [實施例14] 以與實施例1 0相同之方式製備及評估各異向性導電 < 膏,除了未使用偶合劑(VI)及消泡劑(V),及其他成份係以 表3所示量使用。結果示於表4。 [實施例15] 以與實施例1 〇相同之方式製備及評估各異向性導電 膏,除了未使用偶合劑(VI)、消泡劑(V)及固化催化劑 (VII),及其他成份係以表3所示量使用。結果示於表4。 [實施例1 6〜1 8 ] 除了以表3所示組成之外,以與實施例1 〇相同之方 43 326\總檔\91 \91134757\91134757(替換)-1 1232467 替換頁 式製備及評估各異向性導電膏。評估結果示於表2。 [比較實施例3 ] 以與實施例1 〇相同之方式製備及評估各異向性導電 膏,除了未使用高軟化點微細顆粒(ΙΠ),及其他成份係以 表3所示量使用。結果示於表4。 [比較實施例4] 以與實施例1 〇相同之方式製備及評估各異向性導電 膏,除了將高軟化點微細顆粒(III)改爲於合成實施例2中 合成得之低軟化點微細顆粒,及其他成份係以表3所示量 使用。結果示於表4。 [比較實施例5 ] 以與實施例1 0相同之方式製備及評估各異向性導電 賞,除了成份係以表3所不量使用。結果示於表4。 如表4所示,實施例1 0至1 8之各異向性導電膏經試驗 評估爲有利。 表3
Wmm ~— 比較實施例 10 11 12 13 14 15 16 17 」8 3 4 5 組成物(重量份數) (I)環氧樹脂 49 52 49 50 53 55 30 79 40 55 49 27 (IIA)酸酐固化劑 15 17 15 15 17 20 12 10 50 19 15 51 (III)高軟化點微細顆 15 15 15 15 20 20 25 6 ς Q 粒 j 0 低軟化點微細顆粒 - - - - - - - • 15 (IV)導電性顆粒 5 5 5 5 5 5 25 1 0.1 5 5 5 (V)消泡劑 石夕酮A 10 10 - 10 - - 5 3 15 10 3 矽酮B - 10 - - - - - (VI)偶合劑 1 1 1 - - - 1 Γ 1 0.9 1 1 1 (VII)固化催化劑 5 - 5 5 5 - 2 3 1 5 5 5 總計 100 100 100 100 100 100 100 100 ^ 100 100 100 100 44 326\總檔\91\91134757\91134757(替換)-1 1232467 5. 1 7 替換頁 酸酐固化劑·· RIKACID MH-700(New Japan Chemical Co.,
Ltd.) 高軟化點微細顆粒:軟化溫度=80t 低軟化點微細顆粒:軟化溫度=4(TC 矽酮A :矽酮彈性體(A) 矽酮 B :直鏈矽酮 DC3037 (Shin-Etsu Silicones) 固化催化劑:經咪唑改質之微膠囊化化合物 表4
實施例 比較實施1 列 10 11 12 13 14 15 16 17 18 3 4 5 評估項目 (1)儲存安定性 AA AA AA AA AA AA AA AA AA AA CC BB ⑵塗布性質 AA AA AA AA AA AA AA AA AA AA CC BB (3)膠凝時間(秒) 17 32 16 18 15 28 29 27 28 18 15 16 (4)黏合強度 (g/cm) 1430 1320 1010 950 1020 1060 910 980 930 760 280 920 (5)空隙 AA AA AA AA AA AA AA AA AA CC BB AA (6)氣泡產生 AA AA AA AA BB BB AA AA AA BB AA AA ⑺導電性 於層合之後立即測量 5Ω 5Ω 5Ω 5Ω 5Ω 5Ω 5Ω 5Ω 5Ω 10Ω 10Ω 5Ω 於在60°C及95%RH下 儲存600小時後 5Ω 5Ω 5Ω 6Ω 5Ω 6Ω 5Ω 6Ω 7Ω 16Ω 15Ω 8Ω (8)布線短路 AA AA AA AA AA AA AA AA AA AA AA AA (9)可修復性 AA AA AA AA AA AA AA AA AA CC BB CC
[實施例1 9 ] 在室溫下先利用道耳吞混合機將環氧樹脂(I):雙酚A環 氧樹脂、酚系固化劑(IIB) ··酚/對二甲苯二醇二甲基醚聚 縮合物(Mitsui Chemicals,Inc.製造之 MILEX LLL)、高軟化 點微細顆粒(III):於合成實施例1中合成得之高軟化點微 細顆粒、消泡劑(V):於合成實施例3中合成得之矽酮彈性 體(A)、及偶合劑(VI) : 7 -縮水甘油氧丙基三甲氧矽烷 (Shin-Etsu Silicones製造之KBM-403)預捏合,然後再利用 45 326V總檔 \91\91134757\91134757(替換)-1 1232467 ¥•換1 三輥磨捏合。於將固化催化劑(VII):經咪唑改質之微膠囊 化化合物(Asahi Kasei Epoxy Corporation 製造之 NOVACURE HX 3748)與捏合產物混合之後,利用道耳吞混 合機在真空中將混合物捏合並脫氣。成份之添加量示於表 5 ° 利用前述之試驗方法評估如此製得之電路連接膏。結果 示於表6。 [實施例20] 以與實施例1 9相同之方式製備及評估電路連接膏,除了 未使用固化催化劑(VII),及其他成份係以表5所示量使 用。結果示於表6。 [實施例2 1 ] 以與實施例1 9相同之方式製備及評估電路連接膏,除了 未使用固化催化劑(VII),將消泡劑(V)由矽酮彈性體(A)改 爲直鏈矽酮B(Shin-Etsu Silicones製造之DC3037),及其他 成份係以表5所示量使用。結果示於表6。 [實施例22] 以與實施例1 9相同之方式製備及評估電路連接膏,除了 未使用消泡劑(V),及其他成份係以表5所示量使用。結果 示於表6。 [實施例23] 以與實施例1 9相同之方式製備及評估電路連接膏,除了 未使用偶合劑(VI),及其他成份係以表5所示量使用。結 果示於表6。 46 326\總檔\91 \91134757\91134757(替換)-1 1232467 uu· 〇· j| 7 替換頁 [實施例24] 以與實施例1 9相同之方式製備及評估電路連接膏,除了 _ 未使用偶合劑(VI)及消泡劑(V),及其他成份係以表5所示 量使用。結果示於表6。 [實施例25〜27] 除了以表5所示組成之外,以與實施例1 9相同之方 式製備及評估電路連接膏。評估結果示於表6。 [比較實施例6] 以與實施例19相同之方式製備及評估電路連接膏,除了 未使用局軟化點微細顆粒(111)’及其他成份係以表5所示 量使用。結果示於表6。 [比較實施例7 ] 以與實施例1 9相同之方式製備及評估電路連接膏,除了 將高軟化點微細顆粒(III)改爲於合成實施例2中合成得之 低軟化點微細顆粒,及其他成份係以表5所示量使用。結 果示於表6。 如表6所示,實施例1 9至27之電路連接膏經試驗評估 爲有利。 47 326V總檔\91 \91134757\91134757(替換)-1 1232467 从 ί>· 17 替換頁
實施例 比較實施例 19 20 21 22 23 24 25 26 27 6 7 組成物(重量份數) (I)環氧樹脂 53 55 55 55 53 55 30 79 40 58 52 (IIB)酚系固化劑 17 19 19 19 18 20 25 10 50 22 15 (III)高軟化點微細顆粒 15 15 15 21 15 21 25 6 5 - - 低軟化點微細顆粒 - - 15 (V)消泡劑 矽酮A 10 10 10 17 2 3 15 13 矽酮B - - 10 - - - - - - - - (VI)偶合劑 1 1 1 1 - - 1 1 1 1 1 (VII)固化催化劑 4 - - 4 4 4 2 2 1 4 4 總計 100 100 100 100 100 100 100 100 100 100 100 酚系固化劑:MILEX LLL (Mitsui Chemicals,Inc.) 高軟化點微細顆粒:軟化溫度=80 °C 低軟化點微細顆粒:軟化溫度=40 °C 矽酮A :矽酮彈性體(A) 矽酮 B :直鏈矽酮 DC 3 03 7 (Shin-Etsu Silicones) 固化催化劑:經咪唑改質之微膠囊化化合物 表6
實施例 比較實施例 19 20 21 22 23 24 25 26 27 6 7 評估項目 (1)儲存安定性 AA AA AA AA AA AA AA AA AA AA CC (2)塗布性質 AA AA AA AA AA AA AA AA AA AA CC (3)膠凝時間(秒) 14 27 26 12 14 12 21 19 20 14 13 (4)黏合強度(g/cm) 1350 1250 960 980 880 920 910 990 880 660 320 (5)空隙 AA AA AA AA AA AA AA AA AA CC BB (6)氣泡產生 AA AA AA BB AA BB AA AA AA BB AA ⑺導電性 於層合之後立即測量 10Ω 10Ω 10Ω 10Ω 10Ω 10Ω 10Ω 10Ω 10Ω 10Ω 18Ω 於在60°C及95%RH 10Ω 10Ω 11Ω 10Ω 10Ω 11Ω 10Ω 10Ω 11Ω 18Ω 35 Ω 下儲存600小時後 (8)布線短路 AA AA AA AA AA AA AA AA AA AA AA (9)可修復性 AA AA AA AA AA AA AA AA AA CC BB
[實施例2 8 ] 在室溫下先利用道耳吞混合機將環氧樹脂(I):雙酚A環 326\總檔\91 \91134757\91134757(替換)· 1 48 1232467 W頁17 氧樹脂、酚系固化劑(IIB):酚/對二甲苯二醇二甲基醚聚 縮合物(Mitsui Chemicals, Inc.製造之 MILEX LLL)、高軟化 點微細顆粒(III):於合成實施例1中合成得之高軟化點微 細顆粒、消泡劑(V):於合成實施例3中合成得之矽酮彈性 體(A )、及偶合劑(VI) : 7 -縮水甘油氧丙基三甲氧矽烷 (Shin-Etsu Silicones製造之KBM-403)預捏合,然後再利用 三輥磨捏合。於將導電性顆粒(IV) : Micropearl Au-205 (Sekisui Chemical Co·,Ltd.製造;比重2·67)及固化催化劑 (VII):經咪唑改質之微膠囊化化合物(Asahi Kasei Epoxy Corporation製造之NOVACURE HX3748)與捏合產物混合之 後,利用道耳吞混合機在真空中將混合物捏合並脫氣。成 份之添加量不於表7。 利用前述之試驗方法評估如此製得之各異向性導電膏。 結果示於表8。 [實施例29] 以與實施例2 8相同之方式製備及評估各異向性導電 膏,除了未使用固化催化劑(VII),及其他成份係以表7所 示量使用。結果示於表8。 [實施例30] 以與實施例2 8相同之方式製備及評估各異向性導電 膏,除了將消泡劑(V)由矽酮彈性體(A)改爲直鏈矽酮B (Shi n- Etsu Silicones製造之DC3037),及其他成份係以表7 所示量使用。結果示於表8。 [實施例31] ' 49 326\總檔\91\91134757\91134757(替換)-1 1232467 — Α 替換頁 以與實施例2 8相同之方式製備及評估各異向性導電 膏,除了未使用偶合劑(VI),及其他成份係以表7所示量 使用。結果示於表8。 [實施例3 2 ] 以與實施例2 8相同之方式製備及評估各異向性導電 膏,除了未使用偶合劑(VI)及消泡劑(V),及其他成份係以 表7所示量使用。結果示於表8。 [實施例33] 以與實施例28相同之方式製備及評估各異向性導電 膏,除了未使用偶合劑(VI)、消泡劑(V)及固化催化劑 (VII),及其他成份係以表7所示量使用。結果示於表8。 [實施例3 4〜3 6 ] 除了以表7所示組成之外,以與實施例2 8相同之方式製 備及評估各異向性導電膏。評估結果示於表8。 [比較實施例8 ] 以與實施例28相同之方式製備及評估各異向性導電 膏,除了未使用高軟化點微細顆粒(ΠΙ),及其他成份係以 表7所示量使用。結果示於表8。 [比較實施例9 ] 以與實施例28相同之方式製備及評估各異向性導電 膏,除了將高軟化點微細顆粒(ΠΙ)改爲於合成實施例2中 合成得之低軟化點微細顆粒,及其他成份係以表7所示量 使用。結果示於表8。 [比較實施例10] 50 326\總檔 \91\91134757\91134757(替換)-1 1232467 替換頁 以與實施例28相同之方式製備及評估各異向性導電 膏,除了成份係以表7所示量使用。結果示於表8。 如表8所示,實施例2 8至3 6之各異向性導電膏經試驗 評估爲有利。 表7 實施例 比較實施例 28 29 30 31 32 33 34 35 36 8 9 10 組成物(重量份 數) ⑴環氧樹脂 49 52 49 50 53 55 30 79 40 55 49 27 (IIB)酚系固化 劑 15 17 15 15 17 20 12 10 50 19 15 51 (III)高軟化點微 細顆粒 低軟化點微細 顆粒 15 15 15 15 20 20 25 6 5 - 15 8 (IV)導電性顆粒 5 5 5 5 5 5 25 1 0.1 5 5 5 (V)消泡劑 石夕酮A 10 10 10 5 3 15 10 3 矽酮B - - 10 - - - - - - - - - (VI)偶合劑 1 1 1 - - - 1 1 0.9 1 1 1 (VII)固化催化 劑 5 - 5 5 5 - 2 3 1 5 5 5 總計 100 100 100 100 100 100 100 100 100 100 100 100 酉分系固化劑·· MILEX LLL (Mitsui Chemicals,Inc·) 高軟化點微細顆粒:軟化溫度=80 °C 低軟化點微細顆粒:軟化溫度=40 °C 矽酮A :矽酮彈性體(A) 石夕酮 B :直鏈 5夕酮 DC3037 (Shin-Etsu Silicones) 固化催化劑:經咪唑改質之微膠囊化化合物 51 326\總檔\91 \91134757\91134757(替換)-1 1232467 肋· 5· 17 替換頁 表8
實施例 比較實施例 28 29 30 31 32 33 34 35 36 8 9 10 評估項目 (1)儲存安定性 AA AA AA AA AA AA AA AA AA AA CC BB (2)塗布性質 AA AA AA AA AA AA AA AA AA AA CC BB (3)膠凝時間 (秒) 14 27 12 10 12 23 26 21 24 14 12 9 (4)黏合強度 (g/cm) 1350 1250 980 880 920 950 880 910 870 660 320 890 (5)空隙 AA AA AA AA AA AA AA AA AA CC BB AA (6)氣泡產生 AA AA AA AA BB BB AA AA AA BB AA AA (7)導電性 於層合之後立 5Ω 5Ω 5Ω 5Ω 5Ω 5Ω 5Ω 5Ω 5Ω 10Ω 10Ω 5Ω 即測量 於在60°C及 95% RH下儲存 600小時後 5Ω 5Ω 5Ω 8Ω 7Ω 9Ω 5Ω 6Ω 7Ω 18Ω 16Ω 7Ω (8)布線短路 AA AA AA AA AA AA AA AA AA AA AA AA (9)可修復性 AA AA AA AA AA AA AA AA AA CC BB CC (發明之效果) 本發明提供儲存安定性及分配器塗布工作性優異之電路 連接膏及各異向性導電膏。 當將根據本發明之電路連接膏及各異向性導電膏使用於 在諸如200°C之溫度及10至30秒之時間之嚴苛的熱壓縮 黏合條件下連接布線以確保高生產力時,其可沒有空隙、 氣泡及滲出。膏之固化產物即使係在高溫高濕下亦可確保 高黏合及連接可靠性,且亦具有高可修復性。 【圖式簡單說明】 圖1係根據本發明之連接電路布線之方法的槪略流程 圖。 52 326\總檔\91 \91134757\91134757(替換)-1
Claims (1)
1232467 拾、申請專利範圍 1 · 一種電路連接膏,包括: (I) 30至80質量百分比之環氧樹脂, (II) 10至50質量百分比之選自酸酐固化劑(πA)及酚系固 化劑(IIB)之固化劑,及 (III) 5至25質量百分比之高軟化點微細顆粒。 2 . —種電路連接膏,包括: (I) 3 0至79.9質量百分比之環氧樹脂, (II) 10至50質量百分比之選自酸酐固化劑(IIA)及酚系固 化劑(IIB)之固化劑, (III) 5至25質量百分比之高軟化點微細顆粒,及 (V )0.1至20質量百分比之消泡劑。 3. —種電路連接膏,包括: (I) 30至79.8質量百分比之環氧樹脂, (II) 10至50質量百分比之選自酸酐固化劑(IIA)及酚系固 化劑(IIB)之固化劑, (III) 5至25質量百分比之高軟化點微細顆粒,及 (VI) 0.1至5質量百分比之偶合劑。 4. 一種電路連接膏,包括: (I) 30至79.8質量百分比之環氧樹脂, (II) 10至50質量百分比之選自酸酐固化劑(IIA)及酚系固 化劑(IIB)之固化劑, (III) 5至25質量百分比之高軟化點微細顆粒, (V )0.1至20質量百分比之消泡劑,及 312/發明說明書(補件)/92-02/91134757 53 1232467 (VI)0.1至5質量百分比之偶合劑。 5 . —種各異向性導電膏,包括·· (I) 30至80質量百分比之環氧樹脂, (II) 10至50質量百分比之選自酸酐固化劑(IIA)及酚系固 化劑(IIB)之固化劑, (III) 5至25質量百分比之高軟化點微細顆粒,及 (IV) 0.1至25質量百分比之導電性顆粒。 6 . —種各異向性導電膏,包括: (I) 30至79.9質量百分比之環氧樹脂, (II) 10至50質量百分比之選自酸酐固化劑(IIA)及酚系固 化劑(II B)之固化劑, (III) 5至25質量百分比之高軟化點微細顆粒, (IV )0.1至25質量百分比之導電性顆粒,及 (V) 0.1至20質量百分比之消泡劑。 7 . —種各異向性導電膏,包括: (I) 30至7 9.8質量百分比之環氧樹脂, (II) 10至50質量百分比之選自酸酐固化劑(ΠΑ)及酚系固 化劑(IIB)之固化劑, (III) 5至25質量百分比之高軟化點微細顆粒, (IV) 0.1至25質量百分比之導電性顆粒,及 (V 1)0.1至5質量百分比之偶合劑。 8.—種各異向性導電膏,包括: (I) 30至7 9.8質量百分比之環氧樹脂, (II) 10至50質量百分比之選自酸酐固化劑(IIA)及酚系固 54 312/發明說明書(補件)/92-02/91134757 1232467 化劑(IIB)之固化劑, (ΙΠ)5至25質量百分比之高軟化點微細顆粒, (IV )0. 1至25質量百分比之導電性顆粒, (V) O.l至20質量百分比之消泡劑,及 (VI) 0.1至5質量百分比之偶合劑。 9 ·如申請專利範圍第1項之電路連接膏,其更包括固化 催化劑(VII)。 1 〇.如申請專利範圍第1項之電路連接膏,其中該環氧樹 脂(I)每分子平均具有至少1至6個環氧基及具有100至 7 0 00之根據GPC以聚苯乙烯計的平均分子量。 1 1 .如申請專利範圍第1項之電路連接膏,其中該酸酐固 化劑(IIA)係鄰苯二甲酸或順丁烯二酸衍生物。 1 2.如申請專利範圍第1項之電路連接膏,其中該酚系固 化劑(IIB)係酚系酚醛型環氧(novolak)固化劑。 1 3.如申請專利範圍第1項之電路連接膏,其中該高軟化 點微細顆粒(III)具有60至150°C之軟化溫度及0.01至2微 米之原粒子大小。 1 4.如申請專利範圍第1項之電路連接膏,其中該高軟化 點微細顆粒(III)係經由使(甲基)丙烯酸甲酯及除(甲基)丙 烯酸甲酯外之可共聚合單體共聚合而製得,且其包含30 至70質量百分比之(甲基)丙烯酸甲酯。 1 5.如申請專利範圍第5項之各異向性導電膏,其中該導 電性顆粒(IV)之表面包含金或鎳。 1 6.如申請專利範圍第2項之電路連接膏,其中該消泡劑 55 312/發明說明書(補件)/92-02/91134757
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TWI550643B (zh) * | 2012-03-30 | 2016-09-21 | Taiyo Holdings Co Ltd | Conductive paste and conductive circuit |
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-
2002
- 2002-11-29 TW TW091134757A patent/TWI232467B/zh not_active IP Right Cessation
- 2002-11-29 KR KR10-2002-0075108A patent/KR100527990B1/ko not_active IP Right Cessation
- 2002-11-30 CN CNB021518866A patent/CN1228383C/zh not_active Expired - Fee Related
- 2002-12-02 US US10/307,282 patent/US6939431B2/en not_active Expired - Lifetime
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US9279070B2 (en) | 2010-07-06 | 2016-03-08 | Dexerials Corporation | Anisotropic conductive adhesive, method of producing the same, connection structure and producing method thereof |
TWI550643B (zh) * | 2012-03-30 | 2016-09-21 | Taiyo Holdings Co Ltd | Conductive paste and conductive circuit |
Also Published As
Publication number | Publication date |
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KR20040029932A (ko) | 2004-04-08 |
US6939431B2 (en) | 2005-09-06 |
CN1427035A (zh) | 2003-07-02 |
KR100527990B1 (ko) | 2005-11-09 |
TW200400518A (en) | 2004-01-01 |
CN1228383C (zh) | 2005-11-23 |
US20030144381A1 (en) | 2003-07-31 |
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