TW201809033A - 低介電常數材料與其前驅物 - Google Patents
低介電常數材料與其前驅物 Download PDFInfo
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- TW201809033A TW201809033A TW105123850A TW105123850A TW201809033A TW 201809033 A TW201809033 A TW 201809033A TW 105123850 A TW105123850 A TW 105123850A TW 105123850 A TW105123850 A TW 105123850A TW 201809033 A TW201809033 A TW 201809033A
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- 150000003949 imides Chemical class 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- ZQMHJBXHRFJKOT-UHFFFAOYSA-N methyl 2-[(1-methoxy-2-methyl-1-oxopropan-2-yl)diazenyl]-2-methylpropanoate Chemical compound COC(=O)C(C)(C)N=NC(C)(C)C(=O)OC ZQMHJBXHRFJKOT-UHFFFAOYSA-N 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
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- 239000000178 monomer Substances 0.000 description 1
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- QYZFTMMPKCOTAN-UHFFFAOYSA-N n-[2-(2-hydroxyethylamino)ethyl]-2-[[1-[2-(2-hydroxyethylamino)ethylamino]-2-methyl-1-oxopropan-2-yl]diazenyl]-2-methylpropanamide Chemical compound OCCNCCNC(=O)C(C)(C)N=NC(C)(C)C(=O)NCCNCCO QYZFTMMPKCOTAN-UHFFFAOYSA-N 0.000 description 1
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- FOKCKXCUQFKNLD-UHFFFAOYSA-N pent-1-enyl hypofluorite Chemical compound C(CC)C=COF FOKCKXCUQFKNLD-UHFFFAOYSA-N 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000005054 phenyltrichlorosilane Substances 0.000 description 1
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- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 125000000446 sulfanediyl group Chemical group *S* 0.000 description 1
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- 229920003002 synthetic resin Polymers 0.000 description 1
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- GQIUQDDJKHLHTB-UHFFFAOYSA-N trichloro(ethenyl)silane Chemical compound Cl[Si](Cl)(Cl)C=C GQIUQDDJKHLHTB-UHFFFAOYSA-N 0.000 description 1
- ORVMIVQULIKXCP-UHFFFAOYSA-N trichloro(phenyl)silane Chemical compound Cl[Si](Cl)(Cl)C1=CC=CC=C1 ORVMIVQULIKXCP-UHFFFAOYSA-N 0.000 description 1
- FRGPKMWIYVTFIQ-UHFFFAOYSA-N triethoxy(3-isocyanatopropyl)silane Chemical compound CCO[Si](OCC)(OCC)CCCN=C=O FRGPKMWIYVTFIQ-UHFFFAOYSA-N 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 1
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 239000005050 vinyl trichlorosilane Substances 0.000 description 1
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Abstract
本揭露提供之低介電常數材料的前驅物,包括:(a)清漆組合物;5-30重量份的(b)聚四氟乙烯與聚矽氧烷的複合微粉;以及0.05-3重量份的(c)界面活性劑,其中(a)清漆組合物包括:(a1)100重量份的聚苯醚樹脂、20至30重量份的三烯丙基異氰脲酸酯、與0.01至0.03重量份的引發劑;(a2)100重量份的聚苯醚樹脂、20至30重量份的橡膠、20至30重量份的三烯丙基異氰脲酸酯、與0.01至0.03重量份的引發劑;或者(a3)100重量份的聚醯胺醯亞胺與雙馬來醯亞胺之共聚物。
Description
本揭露關於低介電常數材料,更特別關於其前驅物之組成。
隨著電子資訊產品逐漸向著高頻化、高速化方向發展,具有低介電常數(Dk)和低介電損耗(Df)的絕緣材料在印製電路板用基板的應用逐漸受到重視。
聚四氟乙烯(PTFE)具有許多獨特的特性,如耐高溫、耐化學性、離型性、低吸水性及絕緣性,尤其是具有極低的介電常數(Dk)和介電損耗(Df),在高頻覆銅板的應用已經有多年的歷史。一般含PTFE覆銅板的應用可以分為兩種,一種是將玻纖布含浸於PTFE乳液中,另一種則是混合PTFE乳液與無機陶瓷粉。
除了PTFE外,聚苯醚、BT樹脂、氰酸酯樹脂亦常作為低介電常數(Dk)和低介電損耗(Df)覆銅板的黏著材料。然而上述材料製成的覆銅板其介電常數,高於PTFE製成的覆銅板的介電常數。此外,可在清漆組合物如聚苯醚樹脂、雙馬來醯亞胺(BMI)與三嗪(BT,Bismaleimide Triazine)的聚合物樹脂、氰酸酯樹脂、聚醯胺醯亞胺及其衍生物、或環氧樹脂系統中,加入PTFE以降低介電常數和介電損耗。然而上述樹脂是屬於油性系統,通常不可能與PTFE乳液相容,因此只能加入PTFE微粉來達到目的。然而
一般小粒徑的PTFE微粉(平均粒徑約在4-10μm)雖容易均勻分散在一般有機高分子中,但其低分子量(約在10萬以下)會提高介電常數與介電損耗。至於高分子量的PTFE微粉(分子量高於200萬),其平均粒徑範圍過大(介於30-500μm之間)而不易均勻分散在一般油性樹脂系統中,容易團聚,在樹脂中分佈不均,造成電性能不一致。
綜上所述,目前亟需新的低介電常數材料與其前驅物,以改善高分子量之PTFE微粉與清漆組合物的相容性。
本揭露一實施例提供之低介電常數材料的前驅物,包括:(a)清漆組合物;5-30重量份的(b)聚四氟乙烯與聚矽氧烷的複合微粉;以及0.05-3重量份的(c)界面活性劑,其中(a)清漆組合物包括:(a1)100重量份的聚苯醚樹脂、20至30重量份的三烯丙基異氰脲酸酯、與0.01至0.03重量份的引發劑;(a2)100重量份的聚苯醚樹脂、20至30重量份的橡膠、20至30重量份的三烯丙基異氰脲酸酯、與0.01至0.03重量份的引發劑;或者(a3)100重量份的聚醯胺醯亞胺與雙馬來醯亞胺之共聚物。
本揭露一實施例提供之低介電常數材料的前驅物,包括:(a)清漆組合物;5-30重量份的(b)四氟乙烯與聚矽氧烷的複合微粉;以及0.05-3重量份的(c)介面聚活性劑。若(b)聚四氟乙
烯與聚矽氧烷的複合微粉之比例過低,則介電常數無法降低。若(b)聚四氟乙烯與聚矽氧烷的複合微粉之比例過高,則半固化片在壓合後的粘接力過低。若(c)界面活性劑之比例過低,則聚四氟乙烯和聚矽氧烷複合粉末無法很好地分散。若(c)界面活性劑之比例過高,則影響壓合形成的層壓板的介電損耗性能。本揭露所使用的界面活性劑,主要的功能是能降低本發明樹脂組成物的表面張力,幫助聚四氟乙烯與聚矽氧烷的複合微粉可以均勻分散在樹脂組成物。界面活性劑通常是非離子型氟系界面活性劑,如杜邦Capstone FS3100,日本AGC清美化學的氟系界面活劑S-386,S-611、及非離子型矽系界面活性劑,如Momentive的CoatOSil* 1211,優先選擇非離子型氟系界面活性劑。
在一實施中,(a)清漆組合物包括(a1)100重量份的聚苯醚樹脂、20至30重量份的三烯丙基異氰脲酸酯(TAIC)、與0.01至0.03重量份的引發劑;(a2)100重量份的聚苯醚樹脂、20至30重量份的橡膠、20至30重量份的TAIC、與0.01至0.03重量份的引發劑;或者100重量份的(a3)聚醯胺醯亞胺與雙馬來醯亞胺之共聚物。若TAIC的比例過低,則壓合形成的層壓板的玻璃轉換溫度(Tg)不夠高且耐熱性差。若TAIC的比例過高,則降低壓合形成的層壓板的介電性能。在一實施例中,聚苯醚樹脂為末端為甲基丙烯醯氧基的聚苯醚樹脂(如Sabic公司所售之SA-9000)、末端乙烯苄基醚的聚苯醚樹脂(如三菱瓦斯化學所售OPE-2st)、或上述之組合。在一實施例中,橡膠包括聚丁二烯、苯乙烯-丁二烯-苯乙烯嵌段聚合物(SBS)、短鏈聚甲基苯乙烯、或上述之組合。若橡膠之比例過低,則影響壓合形成的層壓板的介電性能。若橡膠之比例過高,
則會降低壓合形成的層壓板的Tg。在一實施例中,引發劑可為偶氮類如2,2’-偶氮二雙(2,4-二甲基正戊腈)(2,2’-azobis(2,4-dimethyl valeronitrile))、二甲基-2,2’-偶氮雙(2-丙酸甲酯)(dimethyl 2,2’-azobis(2-methylpropionate)、2,2-偶氮雙異丁腈(2,2-azobis isobutyronitrile)、2,2-偶氮雙(2-甲基異丁腈)(2,2-azobis(2-methylisobutyronitrile))、1,1’-偶氮雙(環己烷-1-腈)(1,1’-azobis(cyclohexane-1-carbonitrile))、2,2’-偶氮雙[N-2-丙基-2-甲基丙醯胺](2,2’-azobis[N-(2-propenyl)-2-methyl propionamide])、1-[(氰基-1-甲基乙基)-偶氮基]甲醯胺(1-[(cyano-1-methylethyl)azo]formamide)、2,2’-偶氮雙(N-丁基-2-甲基丙醯胺)(2,2’-azobis(N-butyl-2-methylpropionamide))、2,2’-偶氮雙(N-環己基-2-甲基丙醯胺)(2,2’-azobis(N-cyclohexyl-2-methylpropionamide)、或其他合適之偶氮類引發劑;過氧化物類包括苯甲醯基過氧化物(benzoyl peroxide)、1,1-雙(第三丁基過氧基)環己烷(1,1-bis(tert-butyl peroxy)cyclohexane)、2,5-雙(第三丁基過氧基)-2,5-二甲基環己烷(2,5-bis(tert-butylperoxy)-2,5-dimethylcyclohexane)、2,5-雙(第三丁基過氧基)-2,5-二甲基-3-環己快(2,5-bis(tert-butylperoxy)-2,5-dimethyl-3-cyclo-hexyne)、過氧化二叔丁基(Di-t-butyl peroxide)、雙(1-(第三丁基過氧基)-1-甲基乙基)苯(bis(1-(tert-butylpeorxy)-1-methy-ethyl)benzene)、第三丁基過氧化氫(tert-butyl hydroperoxide)、第三丁基過氧化物(tert-butyl peroxide)、第三丁基過氧基苯甲酸(tert-butyl
peroxybenzoate)、茴香基過氧化氫(Cumene hydroperoxide)、環己酮基過氧化物(cyclohexanone peroxide)、二茴香基過氧化物(dicumyl peroxide)、月桂基過氧化物(lauroyl peroxide)、或其他合適之過氧化物。上述之引發劑除可單一使用外,亦可混合使用,端視需要而定。若引發劑之比例過低,則會降低反應物的交聯密度,進而降低壓合形成的層壓板的Tg,若引發劑之比例過高,則反應速率過快,不易操作。
在一實施例中,(a3)聚醯胺醯亞胺與雙馬來醯亞胺之共聚物中,聚醯胺醯亞胺是由二苯基甲烷二異氰酸酯(MDI)和偏苯三酸酐(TMA)聚合而成。雙馬來醯亞胺可為4,4’-雙馬來醯亞胺二苯甲烷、雙(3-乙基-5-甲基-4-馬來醯亞胺基苯基)甲烷、或上述之組合。聚醯胺醯亞胺與雙馬來醯亞胺的重量比介於70:100到70:50之間。若雙馬來醯亞胺的比例過低,則所形成的層壓板其層與層之間容易分層,層壓板機械強度低,且層壓板子容易變形。若雙馬來醯亞胺的比例過高,組合物放久之後則,會有部分的雙馬來醯亞胺沉澱出來,影響組合物儲存安定性,此外因交聯密度太高,也會造成所形成的層壓板太脆。
本揭露一實施例提供之聚四氟乙烯(PTFE)與聚矽氧烷的複合微粉中,PTFE與聚矽氧烷之重量比介於95:5至90:10之間。若PTFE之比例過低,聚矽氧烷相對量過大,造成聚四氟乙烯(PTFE)與聚矽氧烷的複合微粉本身的介電常數及介電損耗偏高,降低介電常數及介電損耗的效果。若PTFE之比例過高,則PTFE與聚矽氧烷所形成的複合材料不夠硬,無法順利使用氣流粉碎的方法,將其粒徑有效的降低到平均粒徑為2-10微米,粒徑會過大,
同時也會造成分散性不好,會影響層壓板的成形性和粘接性,半固化片的外觀也會不好。PTFE的重均分子量可介於200萬至500萬之間。上述PTFE與聚矽氧烷的複合微粉其平均粒徑(D50)可介於2μm至10μm之間。若複合微粉的平均粒徑過大,則會造成半固化片的外觀不佳,不平坦且有顆粒狀PTFE存在再辦固化片的表面。
在本揭露一實施例中,PTFE與聚矽氧烷的複合微粉其製備方法包括:將100重量份的PTFE與10~40重量份的矽烷混合均勻。視混合情況可加入適當的溶劑來潤濕PTFE,且溶劑沒有特別限定,只要能潤濕PTFE的溶劑皆可,比如醇類如甲醇、乙醇、異丙醇,或苯類如甲苯或二甲苯。
在其他實施例中,可進一步將60~80%的矽烷替換為矽溶膠,以進一步提高複合材料的耐熱性。若矽溶膠的添加量過高,則會影響矽烷在PTFE中的反應速率,矽烷在水解縮合的反應過程中容易凝膠。矽烷可滲透至PTFE的孔隙之間,經水解縮合反應(原位聚合)形成網狀結構的聚矽氧烷,可防止PTFE進一步聚集,以達分散PTFE的效果。另一方面,聚矽氧烷可包覆PTFE的表面以硬化PTFE,使其易於粉碎。若矽烷的用量過高,則所形成的複合微粉中聚矽氧烷量過多,而失去PTFE的特性。若矽烷的用量過低,則矽烷無法包覆PTFE,造成PTFE分散效果不佳,亦造成包覆聚矽氧烷的PTFE不夠脆,而無法以一般的氣流粉碎法製備微粉。
接著將占PTFE和矽烷總重之0.1~0.0001%重量份的催化劑加入上述混合物後混合均勻,再加水使矽烷於PTFE中進行
原位聚合反應,以形成聚矽氧烷。催化劑並無特別限定,只要能催化矽烷水解的觸媒皆可,比如硫酸、鹽酸、甲酸、醋酸、檸檬酸、胺類、氫氧化鉀、或氫氧化鈉。若催化劑用量過高,則水解縮合反應速率過快,反應不易控制,容易造成矽烷凝膠產生粒子。若催化劑用量過低,則水解縮合反應速率過慢,反應時間過長。水與矽烷的莫耳比介於0.5:1至3:1之間。若水的用量過高,則會造成反應相分離;若水的用量過少,則使矽烷水解不充分,殘留過多的矽烷,影響產物效果。
在本揭露一實施例中,上述原位聚合反應的溫度介於室溫(約25℃)至45℃之間,且反應時間介於4小時至16小時之間。若原位聚合反應的溫度過高及/或反應時間過長,則水解縮合反應不易控制。若原位聚合反應的溫度過低及/或反應時間過短,則矽烷無法充分進行水解縮合反應。
在本發明一實施例中,PTFE優選為由四氟乙烯(TFE)單體經懸浮聚合或分散聚合所製備的PTFE,其重均分子量介於200萬至500萬之間,具有較好的不粘黏性。上述PTFE可為懸浮聚合,由於懸浮聚合不使用含氟界面活性劑,因此不含PFOA。上述PTFE可進一步包含少量能改善烘烤(熔結)期間之成膜能力的共聚單體改性劑如全氟烯烴,特別是六氟丙烯(HFP)或全氟(烷基乙烯基)醚,其中烷基含有1~5個碳原子,優選為全氟(丙基乙烯基)醚(PPVE)、全氟(甲基乙烯基)醚(PMVE)。上述改性劑的用量不足以讓PTFE具有熔融加工性,而上述共聚物稱為改性PTFE。一般改性劑的用量低於3wt%,優選低於1wt%。聚四氟乙烯的型態為粉狀或凝聚狀,粒徑在20~260μm左右。值得注意的是,上述PTFE
完全不含全氟辛酸(PFOA)。
在一實施例中,矽烷為R1 mR2 nSi(OR3)4-m-n、R4 jR5 kSiCl4-j-k、或上述的組合,其中m、n、j、k各自為0或正整數,m+n=0至2的整數,且j+k=0至3的整數。R1、R2、R4、與R5各自選自H、C1-6的烷基(如甲基、乙基、丙基、或丁基)、C3-6的環烷基(如環戊基或環己基)、C2-6的烯基(如乙烯基或丙烯基)、芳香基(如苯基)、鹵化C1-6的烴基(如氯甲基或γ-氯丙基)、胺基(如γ-胺丙基)、甲基丙烯醯氧基(如γ-甲基丙烯醯氧基丙基或γ-縮水甘油醚氧基丙基)、環氧基(如3,4-環氧環己烷乙基)、巰基(如γ-巰丙基)、硫基、脲基(如γ-脲丙基)、或異氰酸基(如γ-異氰酸基丙基)。R3為C1-3的烷基如甲基、乙基、或丙基。在本發明一實施例中,矽烷可以為甲基三甲氧基矽烷、甲基三乙氧基矽烷、苯基三甲氧基矽烷、苯基三乙氧基矽烷、乙烯基三甲氧基矽烷、正矽酸乙酯、聚矽酸乙酯(TEOS-40)、正矽酸甲酯、γ-胺丙基三乙氧基矽烷、N-(γ-胺乙基)-γ-胺丙基三甲氧基矽烷、3-(2,3-環氧丙氧基)丙基三甲氧基矽烷、2-(3,4-環氧環己烷)乙基三甲氧基矽烷、3-(甲基丙烯醯氧)丙基三甲氧基矽烷、γ-巰丙基三甲氧基矽烷、γ-脲丙基三乙氧基矽烷、γ-異氰酸基丙基三乙氧基矽烷、四氯矽烷、甲基三氯矽烷、苯基三氯矽烷、甲基苯基二氯矽烷、乙烯基三氯矽烷、或上述的組合。在本發明一實施例中,矽烷優選為苯基三甲氧基矽烷,乙烯基三甲氧基矽烷、正矽酸乙酯、3-(2,3-環氧丙氧基)丙基三甲氧基矽烷、3-(甲基丙烯醯氧)丙基三甲氧基矽烷、或上述的組合。
接下來,乾燥聚矽氧烷與聚四氟乙烯的混合物。舉例來說,可先升溫除水混合物至無水分脫出為止,再將以100目濾
布過濾混合物得濕粉。接著將濕粉於200℃至300℃下烘乾2小時至4小時即得乾粉。烘乾主要的目的除了要除去水及溶劑外,另外一個目的是要使聚矽氧烷的矽醇基(Si-OH)減少,避免殘留過多的矽醇基,影響到介電常數和介電損耗。秤重乾粉可得矽含量,公式如下:聚矽氧烷%=[(乾粉重-聚四氟乙烯重)/乾粉重]×100%。
最後物理粉碎乾粉如氣流粉碎,即可得PTFE與聚矽氧烷的複合微粉,其平均粒徑(D50)介於2.0μm至10μm之間,且PTFE與聚矽氧烷之重量比介於95:5至90:10之間。複合微粉中的PTFE其重均分子量,與一開始採用之PTFE之重均分子量實質上相同。上述物理粉碎法如氣流粉碎分級法只會粉碎複合材料,而不會裂解其中的PTFE。
在一實施例中,還可添加30重量份的阻燃劑至介電材料之前驅物中,其中阻燃劑並不特別限定,滿足阻燃要求即可,例如溴系阻燃劑如十溴二苯乙烷等,或是磷氮系阻燃劑如.環狀苯氧基磷腈化合物等。
在本發明一實施例中,還可進一步添加0.5-1重量份的矽烷偶聯劑和20-40重量份的二氧化矽至介電材料之前驅物中。上述矽烷偶聯劑可為(3-環氧丙氧丙基)三甲氧基矽烷、(3-環氧丙氧丙基)三乙氧基矽烷、3-(甲基丙烯醯氧)丙基三甲氧基矽烷、或上述之組合。矽烷偶聯劑可在無機物質和有機物質的介面之間架起「分子橋」,把兩種性質懸殊的材料連接在一起,以提高複合材料的性能和增加粘接強度的作用。不同樹脂系統需選擇不同的矽烷偶聯劑。以聚苯醚系統為例,可優先採用3-(甲基丙烯醯氧)丙基三甲氧基矽烷作為矽烷偶聯劑。在介電材料之前驅物中添
加二氧化矽如熔融型二氧化矽,有助於降低樹脂固化物的熱膨脹係數並降低成本。
上述低介電常數材料之介電常數介於3.4至3.8之間,且介電損耗介於0.002至0.015之間。與直接採用PTFE微粉與清漆組合物之前驅物相較,採用PTFE與聚矽氧烷之複合微粉與清漆組合物之前驅物所形成的低介電常數材料具有較低的介電常數與介電損耗。
為讓本揭露之上述和其他目的、特徵、和優點能更明顯易懂,以實施例說明如下。
實施例
本發明所用的藥品名稱及來源列舉如下,但不僅限於所列藥品:
PTFE粉:
CGM 031B,購自中昊晨光化工研究院有限公司,平均粒徑介於70μm至90μm之間。
CGM 031C,購自中昊晨光化工研究院有限公司,平均粒徑介於130μm至260μm之間。
CGM 16(F),購自中昊晨光化工研究院有限公司,平均粒徑介於25μm。
含矽化合物:
苯基三甲氧基矽烷:購自Wacker之XL70。
(3-環氧丙氧丙基)三甲氧基矽烷:購自Dow Corning之Z 6040。
3-(甲基丙烯醯氧)丙基三甲氧基矽烷:購自Evonic的Dynasylan MEMO。
正矽酸乙酯:購自Wacker之TES 28。
氧化矽溶膠:購自阿克蘇之Levasil CT20 DH。
二苯基甲烷二異氰酸酯:購自日本Nippon polyurethane Industry Co.Ltd Millionate MT.
偏苯三酸酐(TMA):購自台灣恆洲貿易公司。
N-甲基吡咯烷酮(NMP):購自BASF。
二甲基乙醯胺(DMAC):購自杜邦公司。
4,4’-雙馬來醯亞胺二苯甲烷:購自日本Daiwakasei Industry Co.,LTD.之BMI-1000。
末端為甲基丙烯醯氧基的聚苯醚樹脂:購自Sabic的SA-9000。
三烯丙基異氰脲酸酯(Triallylisocyanurate,TAIC):購自中國湖南以翔化工有限公司。
聚丁二烯橡膠:購自Cray Valley的Ricon 153。
苯乙烯-丁二烯-苯乙烯嵌段聚合物(SBS):購自Kraton的D1155。
短鏈聚甲基苯乙烯:購自Eastman的F115。
溴系阻燃劑:購自Albemarle的Saytex 8010。
熔融型二氧化矽:購自台灣矽比科的Megasil 525。
引發劑:購自中國廣州沁豐化工有限公司的過氧化二叔丁基(Di-t-butyl peroxide)。
界面活性劑:購自日本AGC清美化學的氟界面活性劑S386。
玻璃布:購自台玻集團的玻璃纖維布2116。
下述實施例1至4為聚四氟乙烯與含矽化合物之複合微粉的製備方式。
實施例1
在反應容器中加入1000g之PTFE粉(CGM 031B),加入適量的甲醇,攪拌使PTFE粉全部潤濕,然後加入100g之苯基三甲氧基矽烷攪拌均勻,再加入0.01g之濃硫酸作催化劑混合均勻,最後加入10g之水,控制反應溫度不超過45℃反應4小時。
將上述混合液升溫至沸騰以除去水分,然後用100目濾布過濾得濕粉,於300℃烘乾濕粉4小時後得乾粉(秤重1053g)。經氣流粉碎分級乾粉,即得平均粒徑(D50)為10μm之聚四氟乙烯與聚矽氧烷的複合微粉。
實施例2
在反應容器中加入1000g之PTFE粉(CGM 031C),加入適量的甲醇,攪拌使PTFE粉全部潤濕,然後加入120g之3-(甲基丙烯醯氧)丙基三甲氧基矽烷攪拌均勻,再加入1g之鹽酸作催化劑混合均勻,最後加入20g之水,控制反應溫度不超過45℃反應6小時。
將上述混合液升溫至沸騰以除去水分,然後用100目濾布過濾得濕粉,於200℃烘乾濕粉4小時後得乾粉(秤重1064g)。經氣流粉碎分級乾粉,即得平均粒徑(D50)為6.0μm之聚四氟乙烯與聚矽氧烷的複合微粉。
實施例3
在反應容器中加入1000g之PTFE粉(CGM 16(F)),加入適量的甲醇,攪拌使PTFE粉全部潤濕,然後加入200g之3-(2,3-環氧丙氧基)丙基三甲氧基矽烷攪拌均勻,再加入0.1之g鹽酸作催化劑混
合均勻,最後加入40g之水,控制反應溫度不超過45℃反應16小時。
將上述混合液升溫至沸騰以除去水分,然後用100目濾布過濾得濕粉,於200℃下烘乾濕粉2小時後得乾粉(秤重1098g)。經氣流粉碎分級乾粉,即得平均粒徑(D50)為4.0μm之聚四氟乙烯與聚矽氧烷的複合微粉。
實施例4
在反應容器中加入1000g之PTFE粉(CGM 031B),加入適量的異丙醇,攪拌使PTFE粉全部潤濕,然後加入160g之正矽酸乙酯和240g之氧化矽溶膠攪拌均勻,再加入1.2g之濃硫酸作催化劑混合均勻,最後加入20g水,控制反應溫度不超過45℃反應12小時。
將上述混合液升溫至沸騰除去水分,然後用100目濾布過濾得濕粉,於300℃下烘乾濕粉4小時後得乾粉(秤重1110g)。經氣流粉碎分級乾粉,即得平均粒徑(D50)為2.0μm之聚四氟乙烯與聚矽氧烷的複合微粉。
實施例5
100g之聚苯醚(SA-9000)、100g之甲苯、20g之三烯丙基異氰脲酸酯(TAIC)、20g之實施例1製備的PTFE與聚矽氧烷的複合微粉、30g之阻燃劑、1g之3-(甲基丙烯醯氧)丙基三甲氧基矽烷偶聯劑、40g之二氧化矽、0.01g之引發劑、與0.2g之界面活性劑混合均勻。
實施例6
100g之聚苯醚(SA-9000)、100g之甲苯、30g之TAIC、20g之實施例2製備的PTFE與聚矽氧烷的複合微粉、30g之阻燃劑、1g之3-(甲基丙烯醯氧)丙基三甲氧基矽烷偶聯劑、40g之二氧化矽、0.03g之引發劑、與0.2g之界面活性劑混合均勻。
實施例7
100g之聚苯醚(SA-9000)、100g之甲苯、25g之TAIC、5g之實施例3製備的PTFE與聚矽氧烷的複合微粉、30g之阻燃劑、1g之3-(甲基丙烯醯氧)丙基三甲氧基矽烷偶聯劑、40g之二氧化矽、0.02g之引發劑、與0.05g之界面活性劑混合均勻。
實施例8
100g之聚苯醚(SA-9000)、100g之甲苯、25g之TAIC、30g之實施例4製備的PTFE與聚矽氧烷的複合微粉、30g之阻燃劑、1g之3-(甲基丙烯醯氧)丙基三甲氧基矽烷偶聯劑、40g之二氧化矽、0.02g之引發劑、與3g之界面活性劑混合均勻。
實施例9
100g之聚苯醚、120g之甲苯、30g之TAIC、4g之聚丁二烯、8g之SBS、8g之短鏈聚甲基苯乙烯、30g之實施例1製備的PTFE與
聚矽氧烷的複合微粉、30g之阻燃劑、0.01g之引發劑、與0.3g之界面活性劑混合均勻。
實施例10
100g之聚苯醚、120g之甲苯、20g之TAIC、6g之聚丁二烯、12g之SBS、12g之短鏈聚甲基苯乙烯、30g之實施例2製備的PTFE與聚矽氧烷的複合微粉、30g之阻燃劑、0.03g之引發劑、與1.5g之界面活性劑混合均勻。
比較例1
100g之聚苯醚(SA-9000)、100g之甲苯、25g之TAIC、30g之阻燃劑、1g之3-(甲基丙烯醯氧)丙基三甲氧基矽烷偶聯劑、40g之二氧化矽、與0.02g之引發劑混合均勻。
比較例2
100g之聚苯醚(SA-9000)、100g之甲苯、25g之TAIC、30g之PTFE粉(CGM 031B)、30g之阻燃劑、1g之3-(甲基丙烯醯氧)丙基三甲氧基矽烷偶聯劑、40g之二氧化矽、0.02g引發劑、與0.3g之界面活性劑混合均勻。
比較例3
100g之聚苯醚、120g之甲苯、20g之TAIC、4g之聚丁二烯、8g之SBS、8g之短鏈聚甲基苯乙烯、30g之阻燃劑、1g之3-(甲基丙烯醯氧)丙基三甲氧基矽烷偶聯劑、與0.01g之引發劑混合均勻。
比較例4
100g之聚苯醚、120g之甲苯、20g之TAIC、4g之聚丁二烯、8g之SBS、8g之短鏈聚甲基苯乙烯、30g之PTFE粉(CGM 031B)、30g之阻燃劑、0.01g之引發劑、與1.5g之界面活性劑混合均勻。
實施例11
將203g之二苯基甲烷二異氰酸酯(MDI)和149.8g偏苯三酸酐(TMA)加入390g之N-甲基吡咯烷酮(NMP)中,在120℃反應3小時,然後再加入1.52g之TMA繼續反應1小時製得聚醯胺醯亞胺,再加入260g之NMP調節固含量至35%。
將100g之雙馬來醯亞胺加入到200g之上述聚醯胺醯亞胺溶液(固含量35%)中,在120℃下反應2小時形成PAI-BMI樹脂溶液,再加入40g之二甲基乙醯胺(DMAC)調節固含量至50%。
實施例12
取200g之實施例11製備的PAI-BMI樹脂溶液(固含量50%),加入20g之實施例1製備的PTFE與聚矽氧烷的複合微粉、與2g之界面活性劑混合均勻。
實施例13
將203g之MDI與149.8g之TMA加入390g之NMP中,在120℃反應3小時,然後再加入1.52g TMA繼續反應1小時,製得聚醯胺醯亞胺後,再加入260g之NMP調節固含量至35%。
將50g之雙馬來醯亞胺加入200g之上述的聚醯胺醯亞胺溶液(固含量35%)中,在120℃下反應2小時形成PAI-BMI樹脂溶液。
實施例14
取208g之實施例13的PAI-BMI樹脂溶液,加入30g之實施例4製備的PTFE與聚氧矽烷的複合微粉、與3g之界面活性劑混合均勻。
比較例5
取200g之實施例11的PAI-BMI樹脂溶液,加入20g之PTFE粉(CGM 031B)、與2g之界面活性劑混合均勻。
比較例6
取200g上述實施例11的PAI-BMI樹脂溶液。
半固化片與銅箔基板的製作方法
取第2與3表中的樹脂組合物,和其他配料混合後以篩網(100~200mesh)過濾,形成膠液狀的預浸料。接著以含浸機將玻璃纖維布含浸於預浸料中(含浸規格:2116),並將膠含量控制在50±2%。接著在170℃條件下烘烤上述含浸後的玻璃纖維布2-3min,製成半固化片。將6片上述半固化片堆疊後,測其介電常數及介電損耗,如第4與5表所示。接著在半固化片堆疊的雙側放上銅箔後再進行壓合(壓合溫度為210℃,壓合時間為150分鐘,壓合壓力為200psi),以製成銅箔基板。
由第4與5表可知,本揭露的PTFE與聚矽氧烷的複合微粉,其PTFE雖具有高分子量的特性,但因表面經過聚矽氧烷的處理,經氣流粉碎後所得到的複合微粉,可以容易及均勻地分散在聚苯醚樹脂(或聚醯胺醯亞胺和雙馬來醯亞胺的共聚物)中,並
可以降低聚苯醚樹脂(或聚醯胺醯亞胺和雙馬來醯亞胺的共聚物)的介電常數(Dk)和介電損耗(Df)。一般高分子量的PTFE粉,不易分散在聚苯醚樹脂(或聚醯胺醯亞胺和雙馬來醯亞胺的共聚物)中,在分散的過程中,PTFE粉容易團聚,分散不均勻,造成半固化片的外觀不佳,不平坦且有顆粒狀PTFE。
在第4與5表中的測定方法如下:玻璃化溫度(Tg)測試方法採用美國電子電路成型標準(IPC standard),IPC-TM-650-2.4.25(DSC法)。
剝離強度(PS)測試:採用美國電子電路成型標準(IPC standard),IPC-TM-650-2.4.8中的「熱應力後」實驗條件,測試金屬蓋層的剝離強度。
浸錫耐熱性測試:使用50×50mm的銅箔基板,浸入288℃的焊錫中,記錄樣品分層起泡的時間。
耐濕熱性能(PCT)測試:採用壓力鍋蒸煮實驗(PCT),板材經壓力鍋(0.105Mpa)121℃,連續蒸煮120分鐘後,浸入288℃的焊錫中,記錄樣品分層起泡的時間。
介電常數及介電損耗測試方法:測試樣板的大小(長×寬×厚)為70mm×3.5mm×0.75mm,使用日本AET的儀器,測量2GHZ的介電常數和低介電損耗,使用的方法是依照JIS-Compliant C 2565的共振腔法(Resonant Cavity)。
雖然本揭露已以數個實施例揭露如上,然其並非用以限定本揭露,任何所屬技術領域中具有通常知識者,在不脫離本揭露之精神和範圍內,當可作任意之更動與潤飾,因此本揭露之保護範圍當視後附之申請專利範圍所界定者為準。
Claims (9)
- 一種低介電常數材料的前驅物,包括:(a)清漆組合物;5-30重量份的(b)聚四氟乙烯與聚矽氧烷的複合微粉;以及0.05-3重量份的(c)界面活性劑,其中(a)清漆組合物包括:(a1)100重量份的聚苯醚樹脂、20至30重量份的三烯丙基異氰脲酸酯、與0.01至0.03重量份的引發劑;(a2)100重量份的聚苯醚樹脂、20至30重量份的橡膠、20至30重量份的三烯丙基異氰脲酸酯、與0.01至0.03重量份的引發劑;或者(a3)100重量份的聚醯胺醯亞胺與雙馬來醯亞胺之共聚物。
- 如申請專利範圍第1項所述之低介電常數材料的前驅物,其中該聚苯醚為末端基為甲基丙烯醯氧的聚苯醚樹脂、末端乙烯苄基醚的聚苯醚樹脂、或上述之組合。
- 如申請專利範圍第1項所述之低介電常數材料的前驅物,其中該聚苯醚的分子量為2000-5000。
- 如申請專利範圍第1項所述之低介電常數材料的前驅物,其中(a3)聚醯胺醯亞胺與雙馬來醯亞胺中,聚醯胺醯亞胺與雙馬來醯亞胺的重量比介於70:100至70:50之間。
- 如申請專利範圍第1項所述之低介電常數材料的前驅物,其中該雙馬來醯亞胺包括4,4’-雙馬來醯亞胺二苯甲烷、雙(3-乙基-5-甲基-4-馬來醯亞胺基苯基)甲烷、或上述之組合。
- 如申請專利範圍第1項所述之低介電常數材料的前驅物,其中該橡膠包括聚丁二烯、苯乙烯-丁二烯-苯乙烯嵌段聚合物(SBS)、短鏈聚甲基苯乙烯、或上述之組合。
- 如申請專利範圍第1項所述之低介電常數材料的前驅物,其中聚四氟乙烯與聚矽氧烷的重量比介於95:5至90:10之間。
- 如申請專利範圍第1項所述之低介電常數材料的前驅物,其中聚四氟乙烯之重均分子量介於200萬至500萬之間。
- 如申請專利範圍第1項所述之低介電常數材料的前驅物,其中聚四氟乙烯與聚矽氧烷的複合微粉之平均粒徑(D50)介於2μm至10μm之間。
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