TWI473830B - 半導體密封用樹脂組成物及半導體裝置 - Google Patents
半導體密封用樹脂組成物及半導體裝置 Download PDFInfo
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- TWI473830B TWI473830B TW99106880A TW99106880A TWI473830B TW I473830 B TWI473830 B TW I473830B TW 99106880 A TW99106880 A TW 99106880A TW 99106880 A TW99106880 A TW 99106880A TW I473830 B TWI473830 B TW I473830B
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- resin
- general formula
- epoxy resin
- resin composition
- phenol
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- 239000004065 semiconductor Substances 0.000 title claims description 109
- 239000011342 resin composition Substances 0.000 title claims description 95
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- 238000010276 construction Methods 0.000 claims description 2
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Classifications
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- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/62—Alcohols or phenols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
- C08G59/22—Di-epoxy compounds
- C08G59/24—Di-epoxy compounds carbocyclic
- C08G59/245—Di-epoxy compounds carbocyclic aromatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/62—Alcohols or phenols
- C08G59/621—Phenols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- 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
- H01L21/50—Assembly of semiconductor devices using processes or apparatus not provided for in a single one of the subgroups H01L21/06 - H01L21/326, e.g. sealing of a cap to a base of a container
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Description
本發明係關於半導體密封用樹脂組成物及半導體裝置。
作為樹脂密封半導體裝置的手法,有轉移成型、壓縮成形、射出成形等,於更一般的轉移成形中,通常,半導體密封用樹脂組成物以錠劑形態供給至成形機。錠劑狀的半導體密封用樹脂組成物係將環氧樹脂、硬化劑、硬化促進劑,無機填充材等使用輥或押出機等進行熔融混練,冷卻後粉碎,並加壓成型(打錠)成圓柱或長方體形狀之錠劑而可得。於半導體密封用樹脂組成物的量產步驟中,係使用單發式或旋轉式之打錠機連續地進行錠劑成型,此時,有時錠劑發生裂開和缺口、或在打錠機內之成型金屬模具內面附著樹脂組成物且錠劑表面呈粗澀狀態之外觀不良等不適。發生裂痕和缺口的錠劑,在封裝成形步驟中將導致搬送不良和未填充不良,外觀不良有時在輸送中成為錠劑裂開、缺口的原因。作為減低上述裂開、缺口和外觀不良之手法,已提案有例如將打錠機內的成型金屬模具之表面粗度適化,控制環境溫度和金屬模具溫度的方法等(例如,參照專利文獻1、專利文獻2、專利文獻3)。
另一方面,近年以電子機器之小型化、輕量化、高性能化之市場動向為背景,半導體元件之高積體化年年發展,且安裝方式亦由插入安裝移轉成表面安裝。半導體封裝形態係以表面安裝型之QFP(Quad Flat Package)所代表之可因應於小型、輕量且多針化的類型登場,更且,多針化,金屬線佈線的狹窄間距化、以及在1個包裝內積層晶片的構造已登場。於此種半導體裝置中,因為樹脂密封部分的厚度薄,且金屬線密度增大,因此相較於先前的半導體裝置,有易發生未填充和空隙、金屬線流動等之封裝成形步驟之成形不良的傾向。於是,由提高流動特性的目的高言,一般進行對環氧樹脂及硬化劑使用低分子量者和結晶性者之手法。
但是,配合低分子量、或結晶性環氧樹脂和硬化劑時,雖然樹脂組成物的流動性提高,且成形產率提高,但於錠劑打錠成型步驟中易發生裂開、缺口和外觀不良,即使以上述的打錠法亦無法充分改善錠劑成型性,而有封裝成形性和錠劑成型性無法兩相成立的情形。
專利文獻1:日本專利第2551548號公報
專利文獻2:日本專利特開平8-52734號公報
專利文獻3:日本專利特開平10-175210號公報
本發明係提供不損害錠劑打錠產率,且封裝成形時的流動性、成形性優良的半導體密封用樹脂組成物及使用其之半導體裝置。
本發明之半導體密封用樹脂組成物係含有環氧樹脂(A)和硬化劑(B)與無機填充劑(C)的半導體密封用樹脂組成物,其特徵為,上述環氧樹脂(A)為包含具下述一般式(1)構造之環氧樹脂(A1):
[化1]
(其中,於上述一般式(1)中,R1及R3為碳數1~5之烴基,彼此可為相同或亦可為相異。R2表示直接鍵、碳數1~5之烴基、-S-、-O-之任一者。a及b為0~4之整數,彼此可為相同或亦可為相異)上述硬化劑(B)為包含下述一般式(2)所示之酚樹脂(B1):
[化2]
(其中,於上述一般式(2)中,c為0~20之整數)以膠滲透層析之面積法測定,一般式(2)所示之酚樹脂(B1)全量中所含之c=1成分的含有比例,以面積分率計為40%以上,且c≧4成分之含有比例,以面積分率為20%以下。
本發明之半導體密封用樹脂組成物,可作成上述酚樹脂(B1)以膠滲透層析之面積法測定,上述一般式(2)所示之酚樹脂(B1)全量中所含之c=0成分的含有比率,以面積分率計為16%以下者。
本發明之半導體密封用樹脂組成物,可作成上述環氧樹脂(A1)係將烷基取代或未取代之雙酚、雙酚A、雙酚F、雙酚S、雙酚A/D、氧基雙酚所組成群中選出之酚化合物予以二環氧丙基醚化的結晶性環氧樹脂者。
本發明之半導體密封用樹脂組成物,可作成上述環氧樹脂(A1)為具有熔點者,將此熔點設為TA1
,上樹酚樹脂(B1)之軟化點設為TB1
時,兩者溫度差之絕對值|TA1
-TB1
|為35℃以下者。
本發明之半導體密封用樹脂組成物,可用於作為錠劑狀型式而藉由轉移成形法將半導體元件密封者。
本發明之半導體裝置,其特徵為,係以上述半導體密封用樹脂組成物之硬化物將半導體元件密封而得。
若根據本發明,則可得到不損害錠劑成型性,且封裝成形時之流動性、成形性優良的半導體密封用樹脂組成物。
本發明係藉由含有環氧樹脂(A)與硬化劑(B)與無機填充劑(C)之半導體密封用樹脂組成物,上述環氧樹脂(A)係含有具一般式(1)所示構造之環氧樹脂(A1),上述硬化劑(B)係含有一般式(2)所示之酚樹脂(B1),以膠滲透層析之面積法測定,一般式(2)所示之酚樹脂(B1)之全量中所含之c=1成分的含有比例係以面積分率計為40%以上,且c≧4成分之含有比例以面積分率計為20%以下,則可取得錠劑成型性和封裝成形性之平衡優異的半導體密封用樹脂組成物。以下,詳細說明關於本發明。
首先,說明關於半導體密封用樹脂組成物。本發明之半導體密封用樹脂組成物中,使用具有下述一般式(1)所示構造之環氧樹脂(A1)作為環氧樹脂(A)。於一般式(1)中,取代基R1及R3為碳數1~5之烴基,彼此可為相同或亦可為相異,R2為直接鍵、碳數1~5之烴基,-S-、-O-之任一者,a及b為0~4之整數,彼此可為相同或亦可為相異。具有一般式(1)所示構造之環氧樹脂(A1)由於分子量小,故熔融黏度低,且可表現良好的流動性。作為此種環氧樹脂,可列舉例如,烷基取代或未取代之雙酚、雙酚A、雙酚F、雙酚S、雙酚A/D、氧基雙酚等之二環氧丙基醚化合物,作為市售品可列舉新日鐵化學(股)製YSLV-80XY(四甲基雙酚F型環氧)、同YSLV-120TE(下述式(3)所示之烷基取代型雙酚S型環氧樹脂)、Japan Epoxy Resin製YX4000H(四甲基雙酚之環氧樹脂)、Japan Epoxy Resin製YL6810(雙酚A型環氧樹脂)等。
[化3]
(其中,上述一般式(1)中,R1及R3為碳數1~5之烴基,彼此可為相同或亦可為相異。R2表示直接鍵、碳數1~5之烴基、-S-、-O-之任一者。a及b為0~4之整數,彼此可為相同或亦可為相異)
[化4]
具有一般式(1)所示構造之環氧樹脂(A1),若為上述之構造,則無特別限定,為具有熔點者,其熔點較佳為40℃以上,更佳45℃以上。熔點之下限值若為上述範圍內,則在環氧樹脂原料之輸送和保存中以發生黏連,損害作業性之虞較少。又,關於熔點的上限值亦無特別限定,以140℃以下為佳,且以125℃以下為更佳。熔點之上限值若為上述範圍內,則因熔融混練中之樹脂熔融不足引起硬化性不良等不適之虞較少。
本發明之半導體密封用樹脂組成物中,在不致損害因使用具有一般式(1)所示構造之環氧樹脂(A1)而得之效果之範圍下,可併用其他環氧樹脂。作為可併用之環氧樹脂,可列舉苯酚酚醛清漆型環氧樹脂、甲酚酚醛清漆型環氧樹脂等之酚醛清漆型環氧樹脂;三苯酚甲烷型環氧樹脂、烷基改質三苯酚甲烷型環氧樹脂等之多官能環氧樹脂;具有伸苯基骨架之苯酚芳烷基型環氧樹脂、萘酚芳烷基型環氧樹脂、具有伸聯苯骨架之苯酚芳烷基型環氧樹脂、具有伸苯基骨架之萘酚芳烷基型環氧樹脂等之芳烷基型環氧樹脂;二羥基萘型環氧樹脂、將萘酚或二羥基萘之二聚物予以環氧丙基醚化而得之環氧樹脂等之萘酚型環氧樹脂;三環氧丙基三聚異氰酸酯、單烯丙基二環氧丙基三聚異氰酸酯等之含有三核之環氧樹脂:二環戊二烯改質酚型環氧樹脂等之有橋環狀烴化合物改質酚型環氧樹脂、甲氧基萘型環氧樹脂、二氫蒽醌型環氧樹脂,若考慮作為半導體密封用樹脂組成物的耐濕信賴性,則以離子性雜質之Na+
離子和Cl-
離子極少者為佳,且由硬化性方面而言,環氧當量以100g/eq以上、500g/eq以下為佳。
於併用其他環氧樹脂之情況中,作為具有一般式(1)所示構造之環氧樹脂(A1)的配合比例,相對於全環氧樹脂(A),以25質量%以上為佳,以45質量%以上為更佳,以60質量%以上為特佳。配合比例若為上述範圍內,則可取得提高流動性的效果。
關於環氧樹脂(A)全體之配合比例的下限值並無特別限定,但於總半導體密封用樹脂組成物中,以2質量%以上為佳,且以4質量%以上為更佳。配合比例之下限值若為上述範圍內,則引起流動性降低等之虞較少。又,關於環氧樹脂(A)全體之配合比例的上限值,亦無特別限定,但於總半導體密封用樹脂組成物中,以15質量%以下為佳,且以13質量%以下為更佳。配合比例的上限值若為上述範圍內,則引起耐焊錫性降低等之虞較少。
本發明之半導體密封用樹脂組成物含有下述一般式(2)所示之酚樹脂(B1)作為硬化劑(B),並且使用以膠滲透層析之面積法測定,相對於一般式(2)所示之酚樹脂(B1)全量,c=1成分之含有比例以面積分率計為40%以上,且c≧4成分之含有比例以面積分率計為20%以下者。更且,一般式(2)所示之酚樹脂(B1)全量中所含之c=0成分之含有比例以面積分率計為16%以下為佳。此處,所謂一般式(2)所示之酚樹脂(B1)的全量,意指不論c=1成分、c≧4成分、c=0成分之含有比例為何,半導體密封用樹脂組成物中所含之1種或數種之一般式(2)所示之酚樹脂的合計。於一般式(2)所示之酚樹脂(B1)中,一般式(2)之c=0成分雖為低黏度者,但因一分子中的羥基為2個,故尤其在與環氧樹脂(A1)般之2官能環氧樹脂進行熔融混練時,因為分子彼此間的凝集力不夠充分,故有錠劑的強度降低的可能性,且硬化後亦難以取得交聯構造。c=1之成分,為次於c=0的低黏度,且因一分子內具有3個羥基,故容易熔融混練,並且以樹脂組成物狀態與環氧樹脂(A1)般之2官能環氧樹脂之間表現良好的凝集力,於硬化後亦可形成立體交聯構造。隨著c數增加,黏度變高,缺乏熔融混練性和流動性,尤其在重複單位為c≧4,進一步經由本身的立體阻礙,與環氧樹脂(A1)般之2官能環氧樹脂之間的反應性有較缺乏之傾向。本發明之半導體密封用樹脂組成物,關於一般式(2)所示之酚樹脂(B1)全量中所含之c=1成分的含有比例下限值,較佳係以面積分率計為40%以上,且以50%以上為更佳,以55%以上為特佳。c=1成分之含有比例的下限值若為上述範圍內,則引起錠劑打錠產率降低之虞較少,且,可提高樹脂組成物的流動性。關於c=1成分之含有比例的上限值,並無特別限定,較佳係以面積分率計為85%以下,且以80%以下為更佳。c=1成分之上限值若為上述範圍內,則一般式(2)所示之酚樹脂(B1)的合成產率過度變低而造成高成本化之虞較少。關於一般式(2)所示之酚樹脂(B1)全量中所含之c≧4成分之含有比例的上限值,並無特別限定,較佳係以面積分率計為20%以下,且以15%以下為更佳。c≧4成分之含有比例的上限值若為上述範圍內,則引起流動性降低之虞較少。關於一般式(2)所示之酚樹脂(B1)全量中所含之c=0成分的含有比例上限值,並無特別限定,較佳係以面積分率計為16%以下,且以12%以下為更佳。c=0成分之含有比例的上限值若為上述範圍內,則引起錠劑成型時之裂開、缺口和外觀不良之虞較少。另外,上述各成分之含有比例,可根據後述之膠滲透層析面積法測定求出。
[化5]
(其中,上述一般式(2)中,c為0~20之整數)
本發明中,一般式(2)所示之酚樹脂(B1)為上述之構造,c==1成分、c≧4成分之含有比例若為上述之範圍,則無特別限定,但一般式(2)所示之酚樹脂(B1)的軟化點下限值較佳為50℃以上,且以60℃以上為更佳。軟化點之下限值若為上述範圍內,則在環氧樹脂原料之輸送和保存中難以發生黏連,損害作業性之虞較少。又,關於軟化點之上限值並無特別限定,但以140℃以下為佳,以125℃以下為更佳。軟化點之上限值若為上述範圍內,則少因熔融混練中之樹脂熔融不足造成硬化性不良等不適之虞較少。
一般式(2)所示之酚樹脂(B1)中之一般式(2)之c=1成分的含有比例、c≧4成分之含有比例及c=0成分之含有比例,可如下述般算出。進行一般式(2)所示之酚樹脂(B1)的膠滲透層析(GPC)測定,求出對應檢測出之波峰之各成分的換算PS分子量,並且由檢測出之波峰面積比可算出對應檢測出之波峰之各成分的含有比例(面積分率)。
本發明中之膠滲透層析(GPC)的測定係如下進行。GPC裝置係由泵、噴射器、保護柱、管柱及檢測器所構成,且於溶劑使用四氫呋喃(THF)。泵之流速以0.5ml/分鐘進行測定。比其更高之流速將使目的分子量的檢測精確度降低故為不佳。又,為了依上述流速以良好精確度進行測定,必須使用流量精確度良好的泵,流量精確度以0.10%以下為佳。保護柱為市售的保護柱(例如,東梭(股)製TSK GUARD COLUMN HHR-L:直徑6.0mm、管長40mm)、管柱為直列連接數根之市售的聚苯乙烯膠柱(東梭(股)製TSK-GEL GMHHR-L:直徑7.8mm、管長30mm)。檢測器使用差示折射率計(RI檢測器,例如,WATERS公司製差示折射率(RI)檢測器W2414)。於測定前,使保護柱、管柱及檢測器內部安定於40℃。試料係準備調整至濃度3~4mg/ml之環氧樹脂(A)的THF溶液,並將其由約50~150微升注射器注入並進行測定。於試料解析時,使用以單分散聚苯乙烯(以下PS)標準試料作成的標準線。標準線係將PS分子量之對數值與PS之波峰檢測時間(保持時間)進行繪點,並且使用回歸三次式者。作為標準線作成用之標準PS試料,係使用昭和電工(股)製Shodex Standard SL-105系列之編號S-1.0(波峰分子量1060)、S-1.3(波峰分子量1310)、S-2.0(波峰分子量1990)、S-3.0(波峰分子量2970)、S-4.5(波峰分子量4490)、S-5.0(波峰分子量5030)、S-6.9(波峰分子量6930)、S-11(波峰分子量10700)、S-20(波峰分子量19900)。
本發明中,酚樹脂(B1)以一般式(2)之構造表示,c=1成分、c≧4成分之份量若為上述之範圍,則對於聚合方法和成分量之調整方法並無特別限制。作為聚合方法例,可列舉將酚與甲醛於酸觸媒下聚縮合後,將殘留單體及水分蒸餾除去的方法,但亦可使用市售之苯酚酚醛清漆樹脂。又,為了調整一般式(2)之c=1成分、c≧4成分、c=0成分之份量,可使用混合後述之蒸餾、水洗、萃取、管柱層析分級、或混合既定之分子量分佈之苯酚酚醛清漆等之手法。
上述之酚,可使用市售之酚單體或經溶劑稀釋酚之溶液等,但由費用方面而言以工業用酚為佳。上述甲醛可使用對甲醛、三烷、甲醛水溶液等作為甲醛發生源的物質、或者、該等甲醛之溶液。通常,由作業性和費用方面而言以使用甲醛水溶液為佳。又,此外作為合成原料,亦可使用預先將酚與甲醛於酸觸媒下聚縮合的聚合物、該等之蒸餾物、萃取物、分子量分級物、罐出物,其他亦可併用市售之雙酚F和苯酚酚醛清漆樹脂無妨。
作為上述之酸觸媒,可使用通常苯酚酚醛清漆樹脂合成中所公知的酸觸媒。例如,可使用硫酸、鹽酸、磷酸、亞磷酸等之無機酸、或草酸、甲酸、有機膦酸、對甲苯磺酸、二甲基硫酸等之有機酸、醋酸鋅、醋酸鎳等,其可單獨、或亦可組合使用2種以上。其中,草酸、鹽酸因可由酚樹脂中輕易除去觸媒故為佳。
關於酚與甲醛之聚縮合中的酚(P)與甲醛(F)的反應莫耳比(F/P莫耳比)及反應溫度,並無特別限制,通常,F/P莫耳比為0.05~0.7莫耳之範圍,且反應溫度以50~150℃之範圍反應為佳。此處,降低反應莫耳比(F/P莫耳比)、或反應溫度,可減低平均分子量,且可調底c≧4成分之份量。
作為以上述以蒸餾調整分子量之方法,並無特別限制,可列舉例如常壓蒸餾、減壓蒸餾、水蒸氣蒸餾等之手法。蒸餾操作之溫度以50℃以上、250℃以下之蒸餾操作為佳,此處蒸餾溫度未滿50℃時,蒸餾效率變差,由生產性觀點而言為不佳,超過250℃時,因為引起苯酚酚醛清漆樹脂的分解和高分子量化,故不佳。具體而言,分別經由100~150℃之常壓蒸餾可將水分有效除去,以150~200℃、5000Pa之條件減壓蒸餾可將酚單體成分有效除去,以200~250℃、5000Pa之條件減壓水蒸氣蒸餾可將一般式(2)之c=0成分有效除去,藉由將其適當組合,可提高一般式(2)之c=1成分的含有比例。
作為以上述以水洗調整分子量之方法,具體而言,係於苯酚酚醛清漆樹脂中、或將苯酚酚醛清漆樹脂以有機溶劑溶解者中,加水,於常壓或加壓下,以20~150℃之溫度攪拌後,以靜置或離心分離使水相與有機相分離,並將水相除去至系統外,則可減低水相中溶解之低分子量成分、主要為酚單體成分與一般式(2)之c=0成分。經由該等操作,結果可調整一般式(2)之c=1成分量。
作為以上述以萃取調整分子量之方法,係將甲苯、二甲苯等之對於酚樹脂之溶解性低的非極性溶劑,添加至苯酚酚醛清漆樹脂、苯酚酚醛清漆樹脂水溶液、或於醇等之極性溶劑中溶解的酚樹脂中,於常壓或加壓下,以20~150℃之溫度攪拌後,以靜置或離心分離使非極性溶劑相與其他成分相分離,並將非極性溶劑相除去至系統外,則可除去溶解於非極性溶劑相的高分子量成分。進行該等操作,結果可減低、調整c≧4成分之份量。
作為以上述以分級管柱調整分子量之方法,可在分液漏斗、填充了聚苯乙烯膠的分級管柱中,直列接續折射率(RI)檢測器、分液捕集用閥,並由分液漏斗供給苯酚酚醛清漆樹脂之四氫呋喃溶液後,供給四氫呋喃洗提液,偵測折射率(RI)圖表,檢測出既定之波峰後,捕集直到消失為止之間的萃取溶液,則可採集任意的分子量成分。
作為以上述以混合調整分子量之方法,並無特別限制,係使用酚與甲醛於酸觸媒下聚縮合之聚合物、將市售之苯酚酚醛清漆樹脂進行蒸餾、萃取、罐出、分級等操作後,將該等複數之樹脂以熔點以上之溫度熔融混合,或者,使用將溶解於溶劑後混合之溶劑予以減壓除去者,則亦可調整式(2)之c=1成分、c≧4成分、c=0成分之份量。此時,作為個別之單獨樹脂,亦可含有c=1成分、c≧4成分之份量超出上述範圍者。
本發明之半導體密封用樹脂組成物中,在不會損害使用酚樹脂(B1)所得效果之範圍中,可併用其他之硬化劑。作為可併用之硬化劑,可列舉例如聚加成型之硬化劑、觸媒型之硬化劑、縮合型之硬化劑等。作為聚加成型之硬化劑,例如,除了二伸乙基三胺(DETA)、三伸乙基四胺(TETA)、對二甲苯二胺(MXDA)等之脂肪族多胺、二胺基二苯基甲烷(DDM)、對-伸苯基二胺(MPDA)、二胺基二苯基碸(DDS)等之芳香族多胺以外,可列舉雙氰胺(DICY)、含有有機酸二醯肼等之多胺化合物;六氫苯二甲酸酐(HHPA)、甲基四氫苯二甲酸酐(MTHPA)等之脂環族酸酐、偏苯三酸酐(TMA)、均苯四甲酸酐(PMDA)、二苯酮四羧酸(BTDA)等之含有芳香族酸酐的酸酐;苯酚芳烷基樹脂、二環戊二烯改質酚樹脂等之酚樹脂系化合物;多硫化物、硫酯、硫醚等之聚硫醇化合物;異氰酸酯預聚合物、嵌段化異氰酸酯等之異氰酸酯化合物;含有羧酸之聚酯樹脂等之有機酸類等。作為本發明之半導體密封用樹脂組成物可併用的硬化劑,由耐燃性、耐濕性、電特性、硬化性、保存安定性等平衡方面而言,以酚樹脂系硬化劑為佳。酚樹脂系硬化劑為一分子內具有2個以上酚性羥基的單體、低聚物、聚合物全部,其分子量、分子構造並無特別限定,可列舉例如,甲酚酚醛清漆樹脂等之酚醛清漆型樹脂、三酚甲烷型酚樹脂等之多官能型酚樹脂;萜烯改質酚樹脂、二環戊二烯改質酚樹脂等之改質酚樹脂;具有伸苯基骨架及/或伸聯苯基骨架之苯酚芳烷基樹脂、具有伸苯基及/或伸聯苯基骨架之萘酚芳烷基樹脂等之芳烷基型樹脂;雙酚A、雙酚AD等之雙酚化合物等。其中,由硬化性之觀點而言,羥基當量以90g/eq以上、250g/eq以下者為佳。
關於硬化劑(B)全體之配合比例的下限值,並無特別限定,於全半導體密封用樹脂組成物中,較佳為0.8質量%以上,且以1.5質量%以上為更佳。配合比例之下限值若為上述範圍內,則可取得充分的流動性。又,關於硬化劑(B)全體之配合比例的上限值,亦無特別限定,於全半導體密封用樹脂組成物中,較佳為10質量%以下,且以8質量%以下為更佳。配合比例之上限值若為上述範圍內,則可取得良好的耐焊錫性。
又,在使用酚樹脂系硬化劑作為硬化劑(B)之情況,作為環氧樹脂全體與酚樹脂系硬化劑全體之配合比率,較佳係環氧樹脂(A)全體之環氧基數(EP)與酚樹脂系硬化劑全體之酚性羥基數(OH)的當量比(EP)/(OH)為0.8以上、1.3以下。當量比若為此範圍,則在半導體密封用樹脂組成物成形時可取得充分的硬化性。又,當量比若為此範圍,則樹脂硬化物可取得良好的物性。
於本發明之半導體密封用樹脂組成物中,環氧樹脂(A1)為具有熔點者,將其熔點設為TA1
,一般式(2)所示之酚樹脂(B1)的軟化點設為TB1
時,兩者溫度差的絕對值|TA1
-TB1
|較佳為35℃以下,且以30℃以下為更佳。環氧樹脂(A1)之熔點與一般式(2)所示之酚樹脂(B1)之軟化度的溫度差,若為上述範圍,則可取得良好的錠劑成型性。雖然減少上述之溫度差,提高錠劑成型性、產率的理由雖未闡明,但認為在樹脂組成物之熔融混練步驟中,環氧樹脂(A1)與一般式(2)所示之酚樹脂(B1)可迅速熔融混合之結果,將提高冷卻後之環氧樹脂與硬化劑的凝集力。另一方面,結晶性環氧樹脂的熔點過高時,無法快速進行熔融,與硬化劑成分的混合不足,結晶性環氧樹脂之熔點過低時,雖比其他成分易於低溫下熔融,但加熱混合中未加以充分的剪切,與硬化劑的混合、凝集力不足。又,關於與環氧樹脂(A1)及酚樹脂(B1)併用之其他環氧樹脂及硬化劑之軟化點或熔點之下限值,較佳為50℃以上為佳,且以60℃以上為更佳。又,關於與環氧樹脂(A1)及酚樹脂(B1)併用之其他環氧樹脂及硬化劑之軟化點或熔點的上限值,並無特別限定,較佳為140℃以下,且以125℃以下為更佳。與環氧樹脂(A1)及酚樹脂(B1)併用之其他環氧樹脂及硬化劑之軟化點或熔點若為上述範圍內,則因熔融混練中之樹脂熔融不足引起錠劑之外觀不良和缺損等不適之虞較少。
本發明之半導體密封用樹脂組成物中,可進一步使用(C)無機填充劑。作為本發明之半導體密封用樹脂組成物可使用之無機填充劑(C),可使用一般半導體密封用樹脂組成物所用者。可列舉例如,熔融二氧化矽、球狀二氧化矽、結晶二氧化矽、氧化鋁、氮化矽、氮化鋁等。作為無機填充劑(C)之粒徑,若考慮對於金屬模具的填充性,則較佳為0.01μm以上、150μm以下。
作為無機填充劑(C)之含有比例的下限值,較佳為半導體密封用樹脂組成物全體的75質量%以上,且以80質量%以上為更佳,以83質量%以上為特佳。無機填充劑(C)之含有比例的下限值若為上述範圍內,則半導體密封用樹脂組成物可取得良好的錠劑成型性,作為其硬化物物性,不致增加吸濕量、強度降低,並且可取得良好的耐焊錫裂開性。又,作為無機填充劑(C)之含有比例的上限值,以半導體密封用樹脂組成物全體之93質量%以下為佳,且以91質量%以下為更佳,以90質量%以下為特佳。無機填充劑(C)之含有比例的上限值若為上述範圍內,則不致損害流動性,可取得良好的成形性。
本發明之半導體密封用樹脂組成物中,可進一步使用硬化促進劑(D)。硬化促進劑(D)若為促進環氧樹脂之環氧基與含有2個以上酚性羥基之化合物的酚性羥基進行反應者即可,可利用一般之半導體密封用樹脂組成物所使用者。作為具體例,可列舉有機膦、四取代鏻化合物、磷酸甜菜鹼化合物、膦化合物與醌化合物之加成物、鏻化合物與矽烷化合物之加成物等之含磷原子之化合物;1,8-二吖雙環(5,4,0)十一碳烯-7、苄基二甲基胺、2-甲基咪唑等之含氮原子之化合物。其中,以含磷原子之化合物為佳,由流動性和硬化性平衡之觀點而言,以四取代鏻化合物、磷酸甜菜鹼化合物、膦化合物與醌化合物之加成物、鏻化合物與矽烷化合物之加成物等之具有潛伏性的觸媒為更佳。若考慮流動性方面,則以四取代鏻化合物為特佳,若考慮半導體密封用樹脂組成物之硬化物熱時低彈性係數,則以磷酸甜菜鹼化合物、膦化合物與醌化合物之加成物為特佳,若考慮潛伏的硬化性,則以鏻化合物與矽烷化合物之加成物為特佳。
作為本發明之半導體密封用樹脂組成物可使用之有機膦,可列舉例如乙基膦、苯基膦等之第1膦;二甲基膦、二苯基膦等之第2膦;三甲基膦、三乙基膦、三丁基膦、三苯基膦等之第3膦。
作為本發明之半導體密封用樹脂組成物可使用之四取代鏻化合物,可列舉例如下述一般式(4)所示之化合物等。
[化6]
(其中,上述一般式(4)中,P表示磷原子。R4、R5、R6及R7表示芳香族基或烷基。A表示芳香環上具有至少1個由羥基、羧基、硫醇基中選出之任一種官能基的芳香族有機酸之陰離子。AH表示芳香環上具有至少1個由羥基、羧基、硫醇基中選出之任一種官能基的芳香族有機酸。x、y為1~3之整數,z為0~3之整數,且x=y)
一般式(4)所示之化合物,例如可如下進行處理而取得,但並非限定於此。首先,將四取代鹵基鏻與芳香族有機酸與鹼在有機溶劑中均勻混合,使此溶液系內發生芳香族有機酸陰離子。其次若加水,則可使一般式(4)所示之化合物沈澱。於一般式(4)所示之化合物中,結合至磷原子的R4、R5、R6及R7為苯基,且AH為芳香環上具有羥基的化合物,即酚類,且A較佳為該酚類之陰離子。
作為本發明之半導體密封用樹脂組成物可使用之磷酸甜菜鹼化合物,可列舉例如下述一般式(5)所示之化合物。
[化7]
(其中,上述一般式(5)中,X1表示碳數1~3之烷基,Y1表示羥基。f為0~5之整數,g為0~4之整數)
一般式(5)所示之化合物可例如如下處理而取得。首先,將第三膦之三芳香族取代膦與重氮鎓鹽接觸,經過使三芳香族取代膦與重氮鎓鹽所具有之重氮鎓基被取代的步驟而取得。但是並非限定於此。
作為本發明之半導體密封用樹脂組成物可使用之膦化合物與醌化合物的加成物,可列舉例如下述一般式(6)所示之化合物等。
[化8]
(其中,上述一般式(6)中,P表示磷原子。R8、R9及R10表示碳數1~12之烷基或碳數6~12之芳基,彼此可為相同或亦可為相異。R11、R12及R13表示氫原子或碳數1~12之烴基,彼此可為相同或亦可為相異,R11與R12亦可結合成為環狀構造)
作為膦化合物與醌化合物之加成物所用之膦化合物,可列舉例如三苯膦、三(烷基苯基)膦、三(烷氧基苯基)膦、三萘膦、三(苄基)膦等之芳香環上無取代或存在烷基、烷氧基等取代基者為佳,且作為烷基、烷氧基等之取代基可列舉具有碳數1~6之碳數者。由易於取得之觀點而言,以三苯膦為佳。
又,作為膦化合物與醌化合物之加成物所用之醌化合物,可列舉鄰-苯醌、對-苯醌、蒽醌類,其中亦以對-苯醌由保存安定性方面而言為佳。
作為膦化合物與醌化合物之加成物的製造方法,係藉由在有機第三膦與苯醌類兩者可溶解之溶劑中接觸、混合則可取得加成物。作為溶劑,以丙酮和甲基乙基酮等之酮類對於加成物之溶解性低者為佳。但並非限定於此。
於一般式(6)所示之化合物中,結合至磷原子之R8、R9及R10為苯基,且R11、R12及R13為氫原子之化合物,即加成了1,4-苯醌與三苯膦之化合物,於降低半導體密封用樹脂組成物之硬化物的熱時彈性係數方面而言為佳。
作為本發明之半導體密封用樹脂組成物可使用之鏻化合物與矽烷化合物之加成物,可列舉例如下述一般式(7)所示之化合物等。
[化9]
(其中,上述一般式(7)中,P表示磷原子,Si表示矽原子。R14、R15、R16及R17分別表示具有芳香環或雜環之有機基、或脂肪族基,彼此可為相同或亦可為相異。式中X2為與基Y2及Y3結合的有機基。式中X3為與基Y4及Y5結合的有機基。Y2及Y3表示質子供給性基釋出質子而成之基,且一分子內之基Y2及Y3與矽原子結合形成嵌合構造。Y4及Y5表示質子供給性基釋出質子而成之基,同一分子內之基Y4及Y5與矽原子結合形成嵌合構造。X2、及X3彼此可為相同或亦可為相異,Y2、Y3、Y4、及Y5彼此可為相同或亦可為相異。Z1為具有芳香環或雜環之有機基、或脂肪族基。
一般式(7)中,作為R14、R15、R16及R17,可列舉例如,苯基、甲基苯基、甲氧基苯基、羥苯基、萘基、羥萘基、苄基、甲基、乙基、正丁基、正辛基及環己基等,其中亦以苯基、甲基苯基、甲氧基苯基、羥苯基、羥萘基等之具有取代基的芳香族基或未取代之芳香族基為更佳。
又,一般式(7)中,X2係與Y2及Y3結合的有機基。同樣地,X3係與基Y4及Y5結合的有機基。Y2及Y3為質子供給性基釋出質子而成之基,同一分子內之基Y2及Y3與矽原子結合形成嵌合構造者。同樣地Y4及Y5為質子供給性基釋出質子而成之基,同一分子內之基Y4及Y5與矽原子結合形成嵌合構造者。基X2及X3彼此可為相同或亦可為相異,基Y2、Y3、Y4、及Y5彼此可為相同或亦可為相異。此種一般式(7)中之-Y2-X2-Y3-及-Y4-X3-Y5所示之基為質子供予體釋出2個質子而成之基所構成者,作為質子供予體,可列舉例如,兒萘酚、焦棓酚、1,2-二羥基萘、2,3-二羥基萘、2,2’-雙酚、1,1’-二-2-萘酚、水楊酸、1-羥基-2-萘酸、3-羥基-2-萘酸、氯冉酸、丹寧酸、2-羥苄基醇、1,2-環己二醇、1,2-丙二醇及甘油等,其中亦以兒茶酚、1,2-二羥基萘、2,3-二羥基萘為更佳。
又,一般式(7)中之Z1表示具有芳香環或雜環之有機基或脂肪族基,作為其具體例,可列舉甲基、乙基、丙基、丁基、己基及辛基等之脂肪族烴基和苯基、苄基、萘基及聯苯基等之芳香族烴基、環氧丙氧基丙基、氫硫丙基、胺丙基及乙烯基等之反應性取代基等,其中,以甲基、乙基、苯基、萘基及聯苯基係由熱安定性方面為更佳。
作為鏻化合物與矽烷化合物之加成物的製造方法,係在放入甲醇的燒瓶中,加入苯基三甲氧基矽烷等之矽烷化合物、2,3-二羥基萘等之質子供予體並溶解,其次於室溫攪拌下滴下甲醇鈉-甲醇溶液。更且,若於其中將預先準備之溴化四苯基鏻等之四取代鹵基鏻溶解於甲醇的溶液於室溫攪拌下滴下,則析出結晶。若將析出之結晶過濾、水洗、真空乾燥,則取得鏻化合物與矽烷化合物的加成物。但是,並非限定於此。
本發明之半導體密封用樹脂組成物可使用之硬化促進劑(D)的配合比例,較佳係於全樹脂組成物中為0.1質量%以上、1質量%以下。硬化促進劑(D)之配合比例若為上述範圍內,則可取得充分的硬化性。又,硬化促進劑(D)的配合比例若為上述範圍內,則可取得充分的流動性。
本發明中,可進一步使用構成芳香環之2個以上鄰接碳原子上分別結合了羥基的化合物(E)。經由使用構成芳香環之2個以上鄰接碳原子上分別結合了羥基的化合物(E)(以下,亦稱為「化合物(E)」),可作為促進環氧樹脂(A)與硬化劑(B)之交聯反應的硬化促進劑,即使使用不具有潛伏性之含磷原子的硬化促進劑,亦可抑制樹脂組成物之熔融混練中的反應,可安定取得半導體密封用樹脂組成物。又,化合物(E)亦具有降低半導體密封用樹脂組成物之熔融黏度,並提高流動性之效果。作為化合物(E),可使用下述一般式(8)所示之單環式化合物或下述一般式(9)所示之多環式化合物等,且該等化合物亦可具有羥基以外之取代基。
(其中,上述一般式(8)中,R18、R22任一者為羥基,一者為羥基時另一者為氫原子、羥基或羥基以外之取代基。R19、R20及R21為氫原子、羥基或羥基以外之取代基。
[化11]
(其中,上述一般式(9)中,R23、R29任一者為羥基,一者為羥基時另一者為氫原子、羥基或羥基以外之取代基。R24、R25、R26、R27及R28為氫原子、羥基或羥基以外之取代基)
作為一般式(8)所示之單環式化合物之具體例,可列舉例如,兒荼酚、焦培酚、沒食子酸、沒食子酸酯或其衍生物。又,作為一般式(9)所示之多環式化合物之具體例,可列舉例如,1,2-二羥基萘、2,3-二羥基萘及其衍生物。其中,由控制流動性和硬化性之容易度而言,以構成芳香環之2個鄰接碳原子分別結合了羥基的化合物為佳。又,考慮混練步驟之揮發時,作成母核係以低揮發性且秤量安定性高的萘環化合物為更佳。此時,化合物(E),具體而言,可設為例如,1,2-二羥基萘、2,3-二羥基萘及其衍生物等之具有萘環的化合物。該等化合物(E)可使用單獨1種且亦可併用2種以上。
此種化合物(E)之配合比例,於全半導體密封用樹脂組成物中較佳為0.01質量%以上、1質量%以下,更佳為0.03質量%以上、0.8質量%以下,特佳為0.05質量%以上、0.5質量%以下。化合物(E)之配合比例的下限值若為上述範圍內,則可取得半導體密封用樹脂組成物充分的低黏度化和提高流動性效果。又,化合物(E)之配合比例的上限值若為上述範圍內,則引起半導體密封用樹脂組成物之硬化性降低和硬化物物性降低之虞較少。
於本發明之半導體密封用樹脂組成物中,為了提高環氧樹脂(A)與無機填充劑(C)的密合性,可進一步添加矽烷偶合劑等之密合輔助劑(F)。其例並無特別限定,可列舉環氧矽烷、胺基矽烷、脲矽烷、氫硫基矽烷等,若為在環氧樹脂與無機填充劑之間反應,並且提高環氧樹脂與無機填充劑的界面強度者即可。又,矽烷偶合劑係藉由與上述之化合物(E)併用,則亦可降低半導體密封用樹脂組成物的熔融黏度,提高流動性,提高化合物(E)之效果。
更具體而言,作為環氧矽烷,可列舉例如,γ-環氧丙氧丙基三乙氧基矽烷、γ-環氧丙氧丙基三甲氧基矽烷、γ-環氧丙氧丙基甲基二甲氧基矽烷、β-(3,4-環氧環己基)乙基二甲氧基矽烷等。又,作為胺基矽烷,可列舉例如,γ-胺丙基三乙氧基矽烷、γ-胺丙基三甲氧基矽烷、N-β(胺乙基)γ-胺丙基三甲氧基矽烷、N-β(胺乙基)γ-胺丙基甲基二甲氧基矽烷、N-苯基γ-胺丙基三乙氧基矽烷、N-苯基γ-胺丙基三甲氧基矽烷、N-β(胺乙基)r-胺丙基三乙氧基矽烷、N-6-(胺己基)-3-胺丙基三甲氧基矽烷、N-3-(三甲氧基甲矽烷丙基)-1,3-苯二甲烷等。又,作為脲矽烷,可列舉例如,γ-脲丙基三乙氧基矽烷、六甲基二矽氮烷等。又,作為氫硫基矽烷,可列舉例如,γ-氫硫丙基三甲氧基矽烷等。該等矽烷偶合劑可使用單獨1種且亦可併用2種以上。
作為本發明之半導體密封用樹脂組成物可使用之矽烷偶合劑等之密合輔助劑(F)的配合比例,較佳為全樹脂組成物中0.01質量%以上、1質量%以下,更佳為0.05質量%以上、0.8質量%以下,特佳為0.1質量%以上、0.6質量%以下。矽烷偶合劑等之密合輔助劑(F)的配合比例若為上述下限值以下,則環氧樹脂與無機填充劑的界面強度不致降低,於半導體裝置中可取得良好的耐焊錫裂開性。又,矽烷偶合劑等之密合輔助劑(F)的配合比例若為上述範圍內,則樹脂組成物之硬化物的吸水性不致增大,於半導體裝置中可取得良好的耐焊錫裂開性。
本發明之半導體密封用樹脂組成物中,除了上述成分以外,亦可適當配合碳黑、鐵丹、氧化鈦等之著色劑;巴西棕櫚蠟等之天然蠟、聚乙烯蠟等之合成蠟、硬脂酸和硬脂酸鋅等之高級脂肪酸及其金屬鹽類或石蠟等之脫模劑;矽酮油、聚矽氧膠等之低應力添加劑;氧化鉍水合物等之無機離子交換體;氫氧化鋁、氫氧化鎂等之金屬氫氧化物、和硼酸鋅、鉬酸鋅、呋咱(phosphazene)、三氧化銻等難燃劑等之添加劑。
本發明之半導體密封用樹脂組成物之製造方法並無特別限制,係將上述成分、及其他添加劑等以指定量配合者,例如使用混合器、噴射磨、球磨等在常溫下均勻粉碎、混合後,使用加熱輥、捏合機或擠壓機等之混練機將樹脂組成物一邊以90~120℃左右加溫一邊進行熔融混練,並將混練後之樹脂組成物冷卻、粉碎,取得顆粒或粉末狀之樹脂組成物。樹脂組成物之粉末或顆粒的粒度較佳為5mm以下。若超過5mm則引起打錠時填充不足,且錠劑重量的偏差變大。
更且,將所得樹脂組成物的粉末或顆粒予以打錠成型,則可取得錠劑。作為打錠成型所用之裝置,可使用單發式、或多連旋轉式打錠機。錠劑的形狀並無特別限定,但以圓柱狀為佳。打錠機的杵、臼及環境溫度並無特別限制,但以35℃以下為佳。若超過35℃則經由樹脂組成物反應而黏度上升,有損害流動性之虞。打錠壓力較佳為400×104
~3000×104
Pa之範圍。打錠壓力若超過上述之上限值,則在剛打錠後有發生破壞錠劑之虞,於未滿下限值之情況,因為無法取得充分的凝集力,故在輸送中有發生破壞錠劑之虞。打錠劑之杵、臼的金屬模具材質、表面處理並無特別限定,可使用公知的材質物質,作為表面處理之例,可列舉例如放電加工、脫模劑之塗敷、鍍敷處理、研磨等。
其次,說明關於本發明之半導體裝置。藉由本發明之半導體密封用樹脂組成物之硬化物將半導體元件密封以製造半導體裝置時,例如係在金屬模具室內設置搭載了半導體元件的導線框、電路基板等之後,將半導體密封用樹脂組成物以轉移成模、壓縮成模、注射成模等之成形方法予以成形硬化即可。
作為本發明之半導體裝置所密封之半導體元件,並無特別限定,可列舉例如,積體電路、大規模積體電路、電晶體、可變電阻、二極管、固體攝像元件等。
作為本發明之半導體裝置的形態,並無特別限定,可列舉例如,雙式直插式封裝(Dual Inline Package,DIP)、附塑膠‧導線之晶片載體(PLCC)、四列直插式扁平封裝(Quad Flat Package,QFP)、薄型四列直插式封裝(Low Profile Quad Flat Package,LQFP)、小型外殼(Small Qut-line Package,SOP)、小型J導線外殼(Small Qut-line J lead Package,SOJ)、薄小型外殼(Thin Small Out-line Package,TSOP、薄型四列直插式封裝(Thin Quad Flat Package,TQFP)、帶狀載體封裝(Tape Carrier Package,TCP)、球柵陣列(Ball Grid Array,BGA)、晶片尺寸封裝(Chip Size Package,CSP)等。
以轉移成模等之成形方法藉由半導體密封用樹脂組成物之硬化物將半導體元件密封之本發明的半導體裝置,係直接、或者以80℃至200℃左右之溫度,歷10分鐘至10小時左右之時間使其完全硬化後,搭載至電子機器等。
圖1係對於使用本發明之半導體密封用樹脂組成物之半導體裝置之一例,表示剖面構造之圖。在晶粒座3上,透過黏晶材硬化體2將半導體元件1固定。半導體元件1之電極墊與導線框5之間係經由金屬線4連接。半導體元件1係經由半導體密封用樹脂組成物之硬化體6被密封。
圖2係對於使用本發明之樹脂組成物之單面密封型之半導體裝置之一例,表示剖面構造之圖。於基板8上,透過阻焊劑7及黏晶材硬化體2將半導體元件1固定。半導體元件1之電極墊與基板8上之電極墊之間係經由金屬線4,透過阻焊劑7連接。藉由密封用樹脂組成物之硬化體6,僅將基板8之半導體元件1所搭載的單面側密封。使基板8上之電極墊與基板8上之非密封面側的焊錫球9在內部接合。
若根據本發明,則不致損害錠劑成型性,取得封裝成形時之流動性、成形性優異的半導體密封用樹脂組成物,因此適合使用於使用錠劑狀之半導體密封用樹脂組成物將半導體元件密封成形而得的半導體裝置,尤其是樹脂密封部分之厚度薄,且金屬線密度高,多針化、金屬線佈線間距狹窄化、或積層複數半導體晶片之構造的半導體裝置。
以下,以實施例具體說明本發明,但本發明並不限定於此等實施例。以下配合量為質量份。關於實施例、比較例所用之成分示於下。
又,以下列條件進行硬化劑1~5之膠滲透層析(GPC)測定。於苯酚酚醛清漆樹脂1之試料20毫克中加入溶劑四氫呋喃(THF)6毫升並充分溶解再供於GPC測定。GPC系統為使用WATERS公司製Module W2695、東梭(股)製TSK GUARD COLUMN HHR-L(直徑6.0mm、管長40mm、保護管柱)、東梭(股)製TSK-GEL GMHHR-L(直徑7.8mm、管長30mm、聚苯乙烯膠管柱)2根、WATERS公司製差示折射率(R1)檢測器W2414直列連接者。泵流速為0.5毫升/分鐘,管柱及差示折射率計內溫度為40℃,測定溶液由100微升注射器注入並且進行測定。試料解析時,使用以單分散聚苯乙烯(以下PS)標準試料作成的標準線。標準線係使用縮出PS分子量之對數值與PS之波峰檢測時間(保持時間),並且回歸3次式者。作為作成標準線之PS標準PS試料,係使用昭和電工(股)製Shodex Standard SL-105系列之編號S-1.0(波峰分子量1060)、S-1.3(波峰分子量1310)、S-2.0(波峰分子量1990)、S-3.0(波峰分子量2970)、S-4.5(波峰分子量4490)、S-5.0(波峰分子量5030)、S-6.9(波峰分子量6930)、S-11(波峰分子量10700)、S-20(波峰分子量19900)。
(環氧樹脂)
環氧樹脂1:四甲基雙酚F型環氧樹脂(東都化成(股)製、YSLV-80XY。環氧當量190、熔點80℃)
環氧樹脂2:雙酚A型環氧樹脂(Japan Epoxy Resin(股)製、YL6810。環氧當量172、熔點45℃)
環氧樹脂3:四甲基聯苯型環氧樹脂(Japan Epoxy Resin(股)製、YX4000H。環氧當量185、熔點107℃)
環氧樹脂4:下述式(3)所示之環氧樹脂(東都化成(股)製、YSLV-120TE。環氧當量240、熔點120℃)
環氧樹脂5:含有伸聯苯骨架之苯酚芳烷基型環氧樹脂(日本化藥股份有限公司製、NC3000、環氧當量276、軟化點58℃)
環氧樹脂6:二環戊二烯型環氧樹脂(大日本油墨化學工業股份有限公司製、HP7200L、環氧當量244、軟化點56℃)
環氧樹脂7:甲氧基萘型環氧樹脂(大日本油墨化學工業股份有限公司製、EXA7320、環氧當量251、軟化點58℃)
環氧樹脂8:二氫蒽醌型環氧樹脂(Japan Epoxy Resin(股)製商品名YX8800、當量180、熔點110℃)
[化12]
(硬化劑)
硬化劑1:下述一般式(2)所示之苯酚酚醛清漆樹脂(群榮化學(股)製、LV-70S。羥基當量104、軟化點67℃、c=1成分之含有比例63.8%、c≧4成分之含有比例4.4%、c=0成分之含有比例7.4%、數平均分子量332)
硬化劑2:下述一般式(2)所示之苯酚酚醛清漆樹脂(三井化學(股)製、VR-9305。羥基當量104、軟化點75.5℃、c=1成分之含有比例43.1%、c≧4成分之含有比例32.1%、c=0成分之含有比例7.7%、數平均分子量391)
硬化劑3:於具備攪拌機、溫度計、冷卻器之反應器中,裝入酚1700質量份、37%甲醛350質量份,並加入草酸17質量份後,將反應溫度一邊保持於95℃~105℃一邊反應4小時。其後,升溫至180℃,並以5000Pa之減壓度進行減壓蒸餾,除去未反應的酚並升溫至230℃為止,以5000Pa之減壓度並以水蒸氣量2g/min進行水蒸氣蒸餾,取得下述一般式(2)所示之苯酚酚醛清漆樹脂(羥基當量104、軟化點64.4℃、c=1成分之含有比例33.1%、c≧4成分之含有比例11.7%、c=0成分之含有比例19.4%、數平均分子量338)
硬化劑4:下述一般式(2)所示之苯酚酚醛清漆樹脂(住友Becklite(股)製、PR-HF-3、羥基當量104、軟化點80℃、c=1成分之含有比例14.5%、c≧4成分之含有比例46.5%、c=0成分之含有比例18.9%、數平均分子量437)
硬化劑5:於硬化劑3之合成中,除了於反應後之系統中加入雙酚F(試藥特級、4,4’-二羥基二苯基甲烷、和光純藥工業(股)製)80質量份,且水蒸氣蒸餾溫度由230℃變更成215℃以外,進行與硬化劑3同樣之合成操作,取得下述一般式(2)所示之苯酚酚醛清漆樹脂(羥基當量104、軟化點63.0℃、c=1成分之含有比例21.3%、c≧4成分之含有比例22.4%、c=0成分之含有比例32.1%、數平均分子量333)。
以凝膠滲透層析(GPC)測定之硬化劑1~5之各成分含量、數平均分子量、軟化點示於表1,硬化劑1及2之凝膠滲透層析(GPC)圖表示於圖3。硬化劑3~5之凝膠滲透層析(GPC)圖表分別示於圖4~6。
[化13]
(無機填充劑)
無機填充劑1:將電氣化學工業製熔融球狀Silica FB560(平均粒徑30μm)100質量份、Adomatix製合成球狀Silica SO-C2(平均粒徑0.5μm)6.5質量份、Adomatix製合成球狀二氧化矽SO-C5(平均粒徑30μm)7.5質量份予以預先摻混者。
硬化促進劑1:下述式(10)所示之硬化促進劑
[化14]
(矽烷偶合劑)
矽烷偶合劑1:γ-環氧丙氧基丙基三甲氧基矽烷(信越化學工業(股)製、KBM-403)
矽烷偶合劑2:γ-氫硫丙基三甲氧基矽烷(信越化學工業(股)製、KBM-803)
矽烷偶合劑3:N-苯基-3-胺丙基三甲氧基矽烷(信越化學工業(股)製、KBM-573)
(著色劑)
著色劑1:碳黑(三菱化學工業(股)製、MA600)
(脫模劑)
脫模劑1:巴西棕櫚蠟(日興Fine(股)製、Nikko Carnauba、熔點83℃)
[實施例1]
環氧樹脂1 8.19質量份
硬化劑1 4.31質量份
無機填充劑1 86.5質量份
硬化促進劑1 0.4質量份
矽烷偶合劑1 0.1質量份
矽烷偶合劑2 0.05質量份
矽烷偶合劑3 0.05質量份
著色劑1 0.3質量份
脫膜劑1 0.1質量份
於混合器中常溫溫合,並以85~100℃之加熱輥熔融混練,且延伸成片狀並冷卻後,以錘磨加以粉碎,取得粉末狀樹脂組成物。使用所得之樹脂組成物以下列方法評估。評估結果示於表2。
螺旋流動:使用低壓轉移成形機(Kotaki精機(股)製、KTS-15),於根據EMMI-1-66之測定螺旋流動用金屬模具中,以175℃、注入壓力6.9MPa、保壓時間120秒鐘之條件,注入粉末狀之樹脂組成物,測定流動長。螺旋流動為流動性的參數,數值大者,則流動性良好。單位為公分。
錠劑打錠成型性:將樹脂組成物使用粉末成型加壓機(玉川Machinery(股)製、S-20-A),調整成錠劑之完成重量15克、尺寸Φ
18mm×高度約31mm,並以打錠壓力600Pa連續打錠200個。打錠後計數外觀不良、具有破損的錠劑,以不良率(%)表示。其次,將良品錠劑100個以內裝聚乙烯袋之瓦楞紙箱捆包,由30公分之高度落下3次後,實施同樣的外觀觀察,計數落下試驗後的不良率(%)。
金屬線流動量之測定:將錠劑化之密封材料以低壓轉移成形機於175℃、6.9MPa、120秒鐘之條件,將評估金屬線流量試驗用之280針QFP包裝(尺寸;28×28×2.4mmt、Cu導線框、試驗元件;9×9mm、金屬線:Au、1.2mils、5mm)各包裝成形10個,且成形的208針QFP包裝以軟X射線穿透裝置(Exlon International(股)製、型號PMS-160)觀察。作為金屬線流動量之計算方法,係將於1個包裝中最流動(變形)之金屬線流動量視為(F)、其金屬線長度視為(L),算出流動量=F/L×100(%),且10個包裝的平均值示於表2。另外,作為金屬線流動量之判定,未滿5%視為合格,5%以上視為不合格。
[實施例2~17、比較例1~8]
根據表2、表3、表4之配合,同實施例1處理製造樹脂組成物,並同實施例1處理評估。評估結果示於表2、表3、表4。另外,於實施例2、3中,製作將2種硬化劑預先根據表2之比率配合,並以100℃熔融混合,再予以粉碎者,加上與其他原料同時以混合器常溫混合,其後同實施例1處理取得粉末狀樹脂組成物。又,關於表2中記載之實施例2、3中的酚樹脂(B1)軟化點、及c=1成分、c≧4成分、c=0成分的含有比例,亦製作將2種硬化劑預先根據表2之比率配合,並以100℃熔融混合,再予以粉碎者,進行軟化點之測定和凝膠滲透層(GPC)測定。
實施例1~17為包含具有一般式(1)所示構造之環氧樹脂(A1)、一般式(2)所示之酚樹脂(B1),且以膠滲透層析之面積法測定,一般式(2)所示之酚樹脂(B1)全量中所含之c=1成分之含有比率為面積分率40%,且c≧4成分之含有比例為面積分率20%以下者,改變環氧樹脂(A1)之種和配合比例者,改變一般式(2)所示之酚樹脂(B1)中之c=1成分、c≧4成分之含有比例者,均為流動性(螺旋流動)、金屬線流動、鎵劑成型性之平衡優異的結果。
另一方面,雖然含有一般式(2)所示之酚樹脂(B1),但以凝膠滲透層析之面積法測定,一般式(2)所示之酚樹脂(B1)全量中所含之c≧4成分的含有比例為面積分率大幅超過20%的比較例1、3中,為流動性(螺旋流動)降低,且金屬線流動差的結果。又,雖然含有一般式(2)所示之酚樹脂(B1),但以凝膠滲透層析之面積法測定,一般式(2)所含示之酚樹脂(B1)全量中所含之c=1成分的含有比例係面積分率低於40%的比較例2、4中,為錠劑成型性差的結果。另外,比較例3亦為c=1成分之含有比例低於40%者,但因比較例3為c≧4成分之含有比例大幅超過20%者,故錠劑成型性為良好的結果。又,未使用具有一般式(1)所示構造之環氧樹脂(A1)的比較例5~7中,為流動性(螺旋流動)降低,且金屬線流動差的結果。更且,使用環氧樹脂6(二環戊二烯型環氧樹脂)的比較例6中,亦為錠劑成型差的結果。又,雖然未使用具有一般式(1)所示構造之環氧樹脂(A1)者,但使用結晶性環氧樹脂之環氧樹脂8(二氫蒽醌型環氧樹脂)的比較例8中,雖然金屬線流動取得良好之結果,但錠劑成型性為差的結果。
如上述之結果,僅含有具一般式(1)所示構造之環氧樹脂(A1)、一般式所示之酚樹脂(B1),且,以凝膠滲透層析之面積法測定,一般式(2)所示之酚樹脂(B1)全量中所含之c=1成分的含有比例以面積分率為40%以上、且c≧4成分之含有比例以面積分率為20%以下之情況,取得流動性(螺旋流動)、金屬線流動、鎵劑成型性之平衡優異的結果,可認為此效果係為組合含具一般式(1)所示構造之環氧樹脂(A1)、與含有一般式(2)所示之酚樹脂(B1)、且、以凝膠滲透層析之面積法測定,一般式(2)所示之酚樹脂(B1)全量中所含之c=1成分之含有比例以面積分率為40%以上、且c≧4成分之含有比例以面積分率為20%以下的相乘效果。
本申請係以平成21年3月11日申請之日本專利申請特願2009-057387作為基礎主張優先權,且其全部揭示於此處併入。
1...半導體元件
2...黏晶硬化體
3...晶粒座
4...金屬線
5...導線框
6...半導體密封用樹脂組成物之硬化體
7...阻焊劑
8...基板
9...焊錫球
圖1係關於使用本發明之半導體密封用樹脂組成物之半導體裝置的一例,表示剖面構造之圖。
圖2係關於使用本發明之半導體密封用樹脂組成物之單面密封型之半導體裝置的一例,表示剖面構造之圖。
圖3為硬化劑1及硬化劑2之GPC圖表。
圖4為硬化劑3之GPC圖表。
圖5為硬化劑4之GPC圖表。
圖6為硬化劑5之GPC圖表。
1...半導體元件
2...黏晶硬化體
3...晶粒座
4...金屬線
5...導線框
6...半導體密封用樹脂組成物之硬化體
Claims (5)
- 一種半導體密封用樹脂組成物,係含有環氧樹脂(A)與硬化劑(B)與無機填充劑(C)者,其特徵為,上述環氧樹脂(A)為含有具下述一般式(1)所示構造之環氧樹脂(A1):
- 如申請專利範圍第1項之半導體密封用樹脂組成物,其中,上述酚樹脂(B1)係以凝膠滲透層析之面積法進行測定,上述一般式(2)所示之酚樹脂(B1),全量中所含之c=0成分之含有比例以面積分率計為16%以下。
- 如申請專利範圍第1項之半導體密封用樹脂組成物,其中,上述環氧樹脂(A1)係將烷基取代或未取代之聯苯、雙酚A、雙酚F、雙酚S、雙酚A/D、氧基雙酚所組成群中選出之酚化合物予以二環氧丙基醚化的結晶性環氧樹脂。
- 如申請專利範圍第1項之半導體密封用樹脂組成物,其中,係用於作為錠劑狀型式而藉由轉移成形法密封半導體元件。
- 一種半導體裝置,其特徵為,以申請專利範圍第1至4項中任一項之半導體密封用樹脂組成物的硬化物將半導體元件進行密封而得。
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JP5716426B2 (ja) * | 2011-02-03 | 2015-05-13 | 住友ベークライト株式会社 | 樹脂成形体及びその製造方法、ならびに、電子部品装置 |
KR20180104168A (ko) * | 2011-05-13 | 2018-09-19 | 히타치가세이가부시끼가이샤 | 밀봉용 에폭시 수지 성형 재료 및 전자 부품 장치 |
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WO2019189023A1 (ja) * | 2018-03-27 | 2019-10-03 | 明和化成株式会社 | フェノール樹脂及びその製造方法、並びにエポキシ樹脂組成物及びその硬化物 |
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