TWI780530B - 一種具阻水氣特性的矽膠薄膜 - Google Patents
一種具阻水氣特性的矽膠薄膜 Download PDFInfo
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- TWI780530B TWI780530B TW109142315A TW109142315A TWI780530B TW I780530 B TWI780530 B TW I780530B TW 109142315 A TW109142315 A TW 109142315A TW 109142315 A TW109142315 A TW 109142315A TW I780530 B TWI780530 B TW I780530B
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Abstract
本發明係提供一種具阻水氣特性的矽膠薄膜,其係經由固化一可固化矽樹脂組成物而形成,其中該可固化矽樹脂組成物包含10至25重量份的線性聚矽氧烷;40至55重量份的一第一矽樹脂,其中用於表示第一矽樹脂的平均單元結構式至少具有R1
SiO3/2
單體以及R2 2
SiO2/2
單體,且該R1
SiO3/2
單體於平均單元結構式中所占的莫耳分率係介於0.60至0.75;15至30重量份的一第二矽樹脂;15至25重量份的含矽氫鍵之聚矽氧烷;10至40重量份的微層片以及一鉑族金屬系催化劑。
Description
本發明係有關於一種具阻水氣特性的矽膠薄膜,其可用以封裝光學半導體裝置,特別是可應用於發光二極體LED (Light Emitting Diode)之封裝的矽膠薄膜。
相較於傳統照明,發光二極體(Light Emitting Diode, LED)具有體積小、發光效率高、壽命長、安全性高、操作反應時間快、色彩豐富、無熱輻射及無水銀等有毒物質汙染的優點,因此目前正迅速地蓬勃發展。其應用面相當多元,例如建築照明、消費式手持照明、零售展示照明、居住用照明等等。
一般的LED封裝結構中包含支架、設置於支架上的LED晶片以及封裝膠。因矽膠具有良好的耐熱、耐光等特性,在現有技術中常使用矽膠做為LED的封裝材料。然而,因矽膠中的Si-O-Si鍵角較大,因此矽膠薄膜的阻水氣特性較差,容易使LED中的螢光粉或量子點(Quantum dot)因受潮而導致顏色發生變化或光衰退。雖已知可利用增加矽膠之交聯密度或添加奈米粒子來增加矽膠之阻水氣特性,但前述方法對於阻氣性的提升效果相當有限。此外,因矽膠之熱膨脹係數(CTE)較大,在進行無機薄膜的濺鍍製程中會產生較大的熱應力,而不容易在矽膠表面得到緻密平整的無機薄膜,故並不建議在矽膠上濺鍍無機薄膜來提升矽膠的阻水氣性。
現有的阻氣膜結構係以聚乙烯對苯二甲酸酯(PET)或聚萘二甲酸乙二醇酯(PEN)等具有較佳阻水氣特性的高分子材料做為基板,再利用原子層沉積法製備氧化鋁薄膜於高分子基板上而形成。然而因聚乙烯對苯二甲酸酯(PET)或聚萘二甲酸乙二醇酯(PEN)其柔軟性及可塑性皆不足以被應用於高端LED產品中的的晶片級封裝製程(Chip Scale Package,CSP)。
因此,仍需要一種新穎的具阻水氣特性的矽膠薄膜,除了可以提供足夠的阻水氣特性,具有高加工性可應用於LED封裝製程且仍能維持做為LED封裝材料所需的光學性質。
本發明係提出一種具阻水氣特性的矽膠薄膜,此具阻水氣特性的矽膠薄膜具有足夠的阻水氣特性以及高加工性,適用於LED產品中的的晶片級封裝製程(Chip Scale Package,CSP),且仍能維持做為LED封裝材料所需的光學性質,例如高可見光穿透率以及低霧度。
本發明提出之具阻水氣特性的矽膠薄膜,其係經由固化一可固化矽樹脂組成物而形成,前述可固化矽樹脂組成物包含:10至25重量份的一線性聚矽氧烷,其平均單元結構式至少具有一個與矽原子鍵結之芳基與二個與矽原子鍵結之烯基;40至55重量份的一第一矽樹脂,其平均單元結構式至少具有R1
SiO3/2
單體以及R2 2
SiO2/2
單體,其中R1
及R2
為經取代的或未取代之烷基、經取代的或未取代之烯基或經取代的或未取代之芳基,且於此平均單元結構式中,前述R1
SiO3/2
單體所占的莫耳分率係介於0.60至0.75之間,矽原子鍵結之烯基相對於所有與矽鍵結之官能基之莫耳數比值為0.03至0.15;15至30重量份的一第二矽樹脂,其平均單元結構式至少具有R3
SiO3/2
以及R4 3
SiO1/2
之單體,其中R3
及R4
為經取代的或未取代之烷基、經取代的或未取代之烯基或經取代的或未取代之芳基;15至25重量份的至少一含矽氫鍵之聚矽氧烷,其化學結構式為:HR5 2
SiO(SiR6 2
O)n
SiR5 2
H,其中R5
為經取代的或未取代的烷基或氫原子,R6
為經取代或未取代的芳基或經取代的或未取代的烷基,n為大於等於0之整數;10至40重量份的微層片(microsheet);以及一鉑族金屬系催化劑,其中,此具阻水氣特性的矽膠薄膜之水氣穿透率(WVTR)小於40gm-2
day-1
,可見光穿透率大於92%且霧度小於4%。
根據本發明之一實施方式,前述微層片之一長徑比係介於10至200之間,前述微層片之一長度係介於0.1微米(μm)至25微米(μm)之間。
根據本發明之一實施方式,前述微層片可以是雲母、黏土、層狀雙氫氧化合物、磷酸氫鈣之至少之一或其組合。
根據本發明之一實施方式,此具阻水氣特性的矽膠薄膜之25℃-50℃熱膨脹係數(CTE)係介於20ppm至60ppm之間,80℃-100℃熱膨脹係數(CTE)係介於50ppm至150ppm之間,且表面的算術平均高度(Sa)係介於0.01微米(µm)至0.15微米(µm)間。
根據本發明之另一實施方式,前述可固化矽樹脂成物可選擇性地進一步包括接著劑、抑制劑、觸變劑、抗沉降劑、無機填料、螢光粉或其組合。
根據本發明之一實施方式,於前述可固化矽樹脂成物中的無機填料包括一氣相二氧化矽。
根據本發明之又一實施方式,前述具阻水氣特性的矽膠薄膜可選擇性地更包括一無機鍍膜層,其位於前述具阻水氣特性的矽膠薄膜之一表面上。
根據本發明之一實施方式,前述無機鍍膜層係藉由濺鍍法(Sputter Deposition)或原子層沉積法(Atomic Layer Deposition,ALD)形成於前述具阻水氣特性的矽膠薄膜之一表面上。
根據本發明之又一實施方式,前述無機鍍膜層之厚度係介於10奈米(nm)至300奈米(nm)之間。
根據本發明之又一實施方式,前述無機鍍膜層包括二氧化矽(SiO2
)、三氧化二鋁(Al2
O3
)或二氧化鉿(HfO2
)。
根據本發明之又一實施方式,前述具阻水氣特性的矽膠薄膜之水氣穿透率(WVTR)小於0.5gm-2
day-1
。
本發明另提出一種光學半導體裝置,其中此光學半導體裝置係由前述具阻水氣特性的矽膠薄膜封裝而成。
為了使本發明揭示內容的敘述更加詳盡與完備,下文針對了本發明的實施態樣與具體實施例提出了說明性的描述;但這並非實施或運用本發明具體實施例的唯一形式。以下所揭露的各實施例,在有益的情形下可相互組合或取代,也可在一實施例中附加其他的實施例,而無須進一步的記載或說明。
本發明之優點、特徵以及達到之技術方法將參照例示性實施例進行更詳細地描述而更容易理解,且本發明或可以不同形式來實現,故不應被理解僅限於此處所陳述的實施例,相反地,對所屬技術領域具有通常知識者而言,所提供的實施例將使本揭露更加透徹與全面且完整地傳達本發明的範疇,且本發明將僅為所附加的申請專利範圍所定義。
而除非另外定義,所有使用於後文的術語(包含科技及科學術語)與專有名詞,於實質上係與本發明所屬該領域的技術人士一般所理解之意思相同,而例如於一般所使用的字典所定義的那些術語應被理解為具有與相關領域的內容一致的意思,且除非明顯地定義於後文,將不以過度理想化或過度正式的意思理解。
本發明提出之具阻水氣特性的矽膠薄膜,其係經由固化一可固化矽樹脂組成物而成,其中該可固化矽樹脂組成物包含:10至25重量份的一線性聚矽氧烷,其平均單元結構式至少具有一個與矽原子鍵結之芳基與二個與矽原子鍵結之烯基;40至55重量份的一第一矽樹脂,其平均單元結構式至少具有R1
SiO3/2
單體以及R2 2
SiO2/2
單體,其中R1
及R2
為經取代的或未取代之烷基、經取代的或未取代之烯基或經取代的或未取代之芳基,且於此平均單元結構式中,該R1
SiO3/2
單體所占的莫耳分率係介於0.60至0.75之間,且矽原子鍵結之烯基相對於所有與矽鍵結之官能基之莫耳數比值為0.03至0.15,其中R1
及R2
為經取代的或未取代之烷基、經取代的或未取代之烯基或經取代的或未取代之芳基;15至30重量份的一第二矽樹脂,其平均單元結構式至少具有R3
SiO3/2
以及R4 3
SiO1/2
之單體,其中R3
及R4
為經取代的或未取代之烷基、經取代的或未取代之烯基或經取代的或未取代之芳基;15至25重量份的至少一含矽氫鍵之聚矽氧烷,其化學結構式為:HR5 2
SiO(SiR6 2
O)n
SiR5 2
H,其中R5
為經取代的或未取代的烷基或氫原子,R6
為經取代或未取代的芳基或經取代的或未取代的烷基,n為大於等於0之整數;10至40重量份的微層片(microsheet);以及一鉑族金屬系催化劑。
於本發明之具阻水氣特性的矽膠薄膜的可固化矽樹脂組成物中,藉由添加特定比例的微層片來提升矽膠薄膜的阻水氣特性,且仍能維持高可見光穿透率以及低霧度等做為LED封裝材料所需的光學性質以及必要之加工性。
在本發明之一實施例中,適合之微層片可以例如是雲母、黏土、層狀雙氫氧化合物、磷酸氫鈣、氮化硼之至少之一或其組合。適合之微層片之一長徑比係介於10至200之間,且較佳係介於50至200之間。適合之微層片之長度係介於0.1微米(μm)至25微米(μm)之間,且較佳係介於2微米(μm)至25微米之間。適合之微層片之厚度係介於10奈米(nm)至1000奈米(nm)之間,且較佳係介於10奈米(nm)至400奈米(nm)之間。
在本發明之一較佳實施例中,可固化矽樹脂中的微層片可經矽膠改質以提高微層片的疏水性質,以避免微層片在可固化矽樹脂中發生聚集現象。在本發明之一較佳實施例中,可固化矽樹脂中的微層片可以是經甲基矽酮處理之雲母層片。
在本發明之可固化矽樹脂組成物中,微層片(microsheet)之添加量可介於10至40重量份之間,當微層片的添加量過高,則會使具阻水氣特性的矽膠薄膜霧度太高而影響LED的發光效率。當添加量過低,則無法有效提升具阻水氣特性的矽膠薄膜之阻水氣特性,且會因無法有效降低矽膠之熱脹係數(CTE),熱脹係數(CTE)過高時在後續形成無機鍍膜層後可能會有龜裂現象,而無法維持必須的阻水氣性質。
在本發明之一實施例中,第一矽樹脂之平均單元結構式至少具有R1
SiO3/2
單體以及R2 2
SiO2/2
單體,其中,R1
及R2
為經取代的或未取代之烷基、經取代的或未取代之烯基或經取代的或未取代之芳基。此經取代的或未取代的芳基例如可為苯基、甲苯基、二甲苯基或萘基,較佳為苯基。此經取代的或未取代的烯基例如可為乙烯基、丙烯基、烯丙基、丁烯基、戊烯基或是己烯基,較佳為乙烯基。除了經取代的或未取代的芳基與經取代的或未取代的烯基以外,其餘與矽原子鍵結之官能基可為經取代的或未取代的烷基,例如可為甲基、乙基、丙基、異丙基、丁基、異丁基、叔丁基、戊基、新戊基、己基、環己基、辛基、壬基或癸基,較佳為甲基。
在本發明之一實施例中,為了提高具阻水氣特性的矽膠薄膜的耐熱性以及硬度,於第一矽樹脂之平均單元結構式中,除了封端基單體以外,與矽原子鍵結之芳基相對於所有與矽鍵結之官能基之莫耳數比值至少為0.48以上。第一矽樹脂的重量平均分子量可介於500至200,000之間,且較佳為介於1,000至190,000之間。
於本發明之一較佳實施例中,用於表示第一矽樹脂的平均單元結構式,其可例如由(PhSiO3/2
)0.7
(Me2
SiO2/2
)0.15
(ViMeSiO2/2
)0.15
及用於封端之單體ViMe2
SiO1/2
所組成。上述Ph表示苯基,Me表示甲基,Vi表示乙烯基。
於本發明之另一較佳實施例中,用於表示第一矽樹脂的平均單元結構式,其可例如由(PhSiO3/2
)0.7
(Me2
SiO2/2
)0.2
(ViMeSiO2/2
)0.1
及用於封端之單體ViMe2
SiO1/2
所組成。
線性聚矽氧烷可提高與第一矽樹脂及第二矽樹脂之該些矽樹脂間的加工性與所製得之具阻水氣特性的矽膠薄膜的柔韌性。在本發明之一實施例中,適合的線性聚矽氧烷之平均單元結構式至少具有一個與矽原子鍵結之芳基與二個與矽原子鍵結之烯基。前述芳基可為取代的或未取代之芳基,如可為苯基、甲苯基、二甲苯基或萘基,較佳為苯基。前述烯基可為經取代的或未取代之烯基,例如可為乙烯基、丙烯基、烯丙基、丁烯基、戊烯基或是己烯基,較佳為乙烯基。除了芳基與烯基以外,其餘與矽原子鍵結之官能基可為經取代的或未取代的烷基,例如可為甲基、乙基、丙基、異丙基、丁基、異丁基、叔丁基、戊基、新戊基、己基、環己基、辛基、壬基或癸基,較佳為甲基。
為了提高具阻水氣特性的矽膠薄膜的耐熱性、硬度以及折射率,故於可固化矽樹脂組成物中,線性聚矽氧烷之平均單元結構式中,除了封端基單體以外,與矽原子鍵結之芳基相對於所有與矽鍵結之官能基之莫耳數比值至少為0.4以上。且線性聚矽氧烷的添加量可為10至25重量份,較佳為14至20重量份。
於本發明之一較佳實施例,用以表示線性聚矽氧烷的平均單元結構式如下所示:由(PhMeSiO2/2
)0.8
(Me2
SiO2/2
)0.1
(ViMeSiO2/2
)0.1
及用於封端之單體ViMe2
SiO1/2
所組成,上述Ph表示苯基,Me表示甲基,Vi表示乙烯基。線性聚矽氧烷的重量平均分子量可在介於1,000至200,000之間,且較佳為介於1,000至160,000之間。線性聚矽氧烷於25℃的黏度未受限制,較佳範圍為6,000 mPa.s至10,000 mPa.s。在本發明之一較佳實施例中,線性聚矽氧烷於25℃的黏度為6420 mPa.s。
於形成具阻水氣特性的矽膠薄膜之可固化矽樹脂組成物中,用於表示第二矽樹脂之平均單元結構式至少具有R3
SiO3/2
以及R4 3
SiO1/2
之單體,其中R3
為經取代的或未取代的芳基、經取代的或未取代的烷基或經取代的或未取代的烯基。R4
為經取代的或未取代的芳基、經取代的或未取代的烷基或經取代的或未取代的烯基。上述經取代的或未取代的芳基例如可為苯基、甲苯基、二甲苯基、或萘基,較佳為苯基。上述經取代的或未取代的烯基例如可為乙烯基、丙烯基、烯丙基、丁烯基、戊烯基或是己烯基,較佳為乙烯基。除了經取代的或未取代的芳基與經取代的或未取代的烯基以外,其餘與矽原子鍵結之官能基為經取代的或未取代的烷基,例如可為甲基、乙基、丙基、異丙基、丁基、異丁基、叔丁基、戊基、新戊基、己基、環己基、辛基、壬基或癸基,較佳為甲基。
為了提高具阻水氣特性的矽膠薄膜的耐熱性及硬度,於可固化矽樹脂組成物中,第二矽樹脂中除封端基單體以外,與矽原子鍵結之芳基相對於與矽鍵結之所有官能基之莫耳數比值至少為0.25以上。
於本發明之一較佳實施例中,用於表示第二矽樹脂的平均單元結構式如以下所式:(PhSiO3/2
)0.5
(ViMe2
SiO1/2
)0.5
。上述Ph表示苯基,Me表示甲基,Vi表示乙烯基。第二矽樹脂的重量平均分子量可介於100至10,000之間,且較佳為介於500至5,000之間。
於本發明之形成具阻水氣特性的矽膠薄膜之可固化矽樹脂組成物中,用以表示含矽氫鍵之聚矽氧烷之化學結構式為: HR5 2
SiO(SiR6 2
O)n
SiR5 2
H,其中R5
為經取代的或未取代的烷基或氫原子,R6
為經取代或未取代的芳基或經取代的或未取代的烷基,且n為大於等於0之整數。
上述經取代的或未取代的芳基例如可為苯基、甲苯基、二甲苯基、或萘基,較佳為苯基。取代的或未取代的烷基例如可為甲基、乙基、丙基、異丙基、丁基、異丁基、叔丁基、戊基、新戊基、己基、環己基、辛基、壬基或癸基,較佳為甲基。
於本發明之一較佳實施例中,用於表示含矽氫鍵之聚矽氧烷的平均單元結構式如下所式:(Ph2
SiO2/2
)1
(HMe2
SiO1/2
)2
。上述Ph表示苯基,Me表示甲基。含矽氫鍵之聚矽氧烷的重量平均分子量可介於100至5,000之間,且較佳為介於100至1,000之間。
適合之鉑族金屬系催化劑可例如為鉑-型式催化劑、銠-型式催化劑或鈀-型式催化劑,較佳為鉑-型式催化劑,常用的催化劑可例如為H2
PtCl6
‧mH2
O,K2
PtCl6
,KHPtCl6
‧mH2
O,K2
PtCl4
,K2
PtCl4
‧mH2
O或PtO2
‧mH2
O (m為正整數)等。亦或該些催化劑與鏈烯烴、醇或含有乙烯基的有機聚矽氧烷之間的錯合物,例如可為鉑(0)-2,4,6,8-四甲基-2,4,6,8-四乙烯基環四矽氧烷複合體溶液(Platinum(0)-2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane complex solution)或辛醇絡鉑化合物(Platinum-Octanal/Octanol Complex),但不限於此。上述該些鉑族金屬系催化劑可單獨使用或合併使用。鉑族金屬系催化劑的添加量為線性聚矽氧烷、第一矽樹脂、第二矽樹脂及含矽氫鍵之聚矽氧烷之重量份總和的1ppm至50ppm,較佳為3 ppm至10ppm。
於本發明之一較佳實施例,所使用的鉑族金屬系催化劑為辛醇絡鉑化合物,其使用量為線性聚矽氧烷、第一矽樹脂、第二矽樹脂及含矽氫鍵之聚矽氧烷之重量份總和的4.3ppm。
另,於本發明之形成具阻水氣特性的矽膠薄膜之可固化矽樹脂組成物中,進一步還可包括觸變劑、抑制劑、抗沉降劑、無機填料、螢光粉、量子點或其組合。
上述無機填料是用以增加具阻水氣特性的矽膠薄膜的耐熱性,亦可作為防止螢光粉沈降的抗沈降劑,此外,也作為反射粒子之用途。該些無機填料例如可為氣相法二氧化矽、氣相法二氧化鈦等增強型無機填充劑以及碳酸鈣、矽酸鈣、二氧化鈦、氧化鈦、氧化鋅等非增強型無機填充劑。
於本發明之一實施例中,於形成具阻水氣特性的矽膠薄膜的可固化矽樹脂組成物中,其包括氣相二氧化矽,該氣相二氧化矽添加量相對100重量份之線性聚矽氧烷、第一矽樹脂、第二矽樹脂及含矽氫鍵之聚矽氧烷之總和,係為0.1至5重量份。
本發明所提出的具阻水氣特性的矽膠薄膜具有良好的阻水氣性質、適當的光學性質,其水氣穿透率(WVTR)可小於40gm-2
day-1
,可見光穿透率可大於92%,霧度可小於4%。此外,本發明所提出的具阻水氣特性的矽膠薄膜具有良好的加工性,其25℃-50℃熱膨脹係數(CTE)可介於20ppm至60ppm之間,80℃-100℃熱膨脹係數(CTE)可介於50ppm至150ppm之間,且表面的算術平均高度(Sa)可介於0.01微米(µm)至0.15微米(µm)間,有利於形成後續的無機鍍膜層。
在本發明之另一實施例中,具阻水氣特性的矽膠薄膜之一表面上更具有一無機鍍膜層,以進一步降低矽膠薄膜之阻水氣性質。
無機鍍膜層可包含但不限於二氧化矽(SiO2
)、三氧化二鋁(Al2
O3
)或二氧化鉿(HfO2
),在本發明之一實施例中,無機鍍膜層可為三氧化二鋁(Al2
O3
)鍍膜層。在本發明之另一實施例中,無機鍍膜層可為三氧化二鋁(Al2
O3
)/二氧化鉿(HfO2
)鍍膜層。
無機鍍膜層可藉由濺鍍法(Sputter Deposition)或原子層沉積法(Atomic Layer Deposition,ALD)形成於具阻水氣特性的矽膠薄膜之一表面上。
在本發明之一實施例中,無機鍍膜層之厚度可介於10奈米(nm)至300奈米(nm)之間,且較佳係介於20奈米(nm)至30奈米(nm)之間。且此具有無機鍍膜層之具阻水氣特性的矽膠薄膜之一水氣穿透率(WVTR)可小於0.5gm-2
day-1
。
本發明提出一種光學半導體裝置,其中此光學半導體裝置係利用前述具阻水氣特性的矽膠薄膜封裝而成。
下述實施例係用來進一步說明本發明,但本發明之內容並不受其限制。
實施例
製備例1:線性聚矽氧烷(化合物1)的製備方法
將3499.92克(19.13 mole)的甲基苯基二甲氧基矽烷(phenylmethyl dimethoxysilane,購自恆橋產業股份有限公司,台灣),288.48克(2.4 mole)的二甲基二甲氧基矽烷(Dimethyldimethoxysilane,購自恆橋產業股份有限公司,台灣),以及317.28克(2.4 mole)的甲基乙烯基二甲氧基矽烷(Methylvinyldimethoxysilane,購自六和化工股份有限公司,台灣)加至反應槽中並於室溫下攪拌形成一均勻混和溶液。將此混和溶液滴入濃度5%的硫酸水溶液(5337.4克)中得到一反應溶液,接著將此反應溶液加熱至75℃以進行水解,待反應完全後以去離子水進行萃取使有機層達到中性,最後移除溶劑以製得一水解產物。
將上述水解產物、69.52克(0.374 mole)的二乙烯基四甲基二矽氧烷(Divinyltetramethyldisiloxane,購自六和化工股份有限公司,台灣)以及5.88克的四甲基氫氧化銨(Tetramethyl ammonium hydroxide,商品名L09658,購自Alfa Aesar,美國)置於反應槽中,於反應槽中通入氮氣,並於室溫下均勻攪拌以製得一反應溶液。將此反應溶液加熱至95℃,待反應完全後,進行除鹼以完成化合物1的製備。化合物1之平均單元結構式係由(PhMeSiO2/2
)0.8
(Me2
SiO2/2
)0.1
(ViMeSiO2/2
)0.1
及用於封端之單體ViMe2
SiO1/2
所組成。上述Ph表示苯基,Me表示甲基,Vi表示乙烯基。
製備例2:第一矽樹脂(化合物2)的製備方法
將2685克(13.5mole)的苯基三甲氧基矽烷(phenyl-trimethoxysilane,購自六和股份有限公司,台灣),349克(2.9mole)的二甲基二甲氧基矽烷 (Dimethyldimethoxysilane,購自恆橋產業股份有限公司,台灣),以及384克(2.9 mole)的甲基乙烯基二甲氧基矽烷(Methylvinyldimethoxysilane,購自六和化工股份有限公司,台灣)置於反應槽中,於室溫下攪拌以製得均勻混合溶液。將混和溶液滴入濃度5%的硫酸水溶液(4579克)中以製得一反應溶液,接著將此反應溶液加熱至75℃進行水解,待反應完全後,以去離子水進行萃取使有機層達到中性,最後移除溶劑以製得一水解產物。
將上述水解產物、21.39克(0.11 mole)的二乙烯基四甲基二矽氧烷(Divinyltetramethyldisiloxane,購自六和化工股份有限公司,台灣)、22.74克的氫氧化鉀以及2274克的甲苯置於反應槽中,於反應槽中通入氮氣,並於室溫下攪拌以製得一反應溶液。接著將此反應溶液加熱至95℃。待反應完全後,以去離子水進行萃取使有機層達到中性,最後移除溶劑以完成化合物2的製備。化合物2之平均單元結構式係由(PhSiO3/2
)0.7
(Me2
SiO2/2
)0.15
(ViMeSiO2/2
)0.15
及用於封裝之單體ViMe2
SiO1/2
所組成。
製備例3:第一矽樹脂(化合物3)的製備方法
將2776克(14 mole)的苯基三甲氧基矽烷(phenyl-trimethoxysilane,購自六和股份有限公司,台灣),480.88克(4mole)的二甲基二甲氧基矽烷 (Dimethyldimethoxysilane,購自恆橋產業股份有限公司,台灣),以及264.46克(2 mole)的甲基乙烯基二甲氧基矽烷(Methylvinyldimethoxysilane,購自六和化工股份有限公司,台灣)置於反應槽中,於室溫下攪拌以製得均勻混合溶液。將混和溶液滴入濃度5%的硫酸水溶液中以製得一反應溶液,接著將此反應溶液加熱至75℃進行水解,待反應完全後,以去離子水進行萃取使有機層達到中性,最後移除溶劑以製得一水解產物。
將上述水解產物、21.39克(0.11 mole)的二乙烯基四甲基二矽氧烷(Divinyltetramethyldisiloxane,購自六和化工股份有限公司,台灣)、22.74克的氫氧化鉀以及2274克的甲苯置於反應槽中,於反應槽中通入氮氣,並於室溫下攪拌以製得一反應溶液。接著將此反應溶液加熱至95℃。待反應完全後,以去離子水進行萃取使有機層達到中性,最後移除溶劑以完成化合物3的製備。化合物3之平均單元結構式係由(PhSiO3/2
)0.7
(Me2
SiO2/2
)0.2
(ViMeSiO2/2
)0.1
及用於封裝之單體ViMe2
SiO1/2
所組成。
製備例4:第二矽樹脂(化合物4)的製備方法
將2379.4克(12 mole)的苯基三甲氧基矽烷(Phenyltrimethoxysilane,購自六和化工股份有限公司,台灣),以及1118.4克(6 mole)的二乙烯基四甲基二矽氧烷(Divinyltetramethyldisiloxane,購自六和化工股份有限公司,台灣)置於反應槽中,於室溫下攪拌以製得均勻混和溶液。將此混和溶液滴入濃度5%的硫酸水溶液(4547.16克)中以製得一反應溶液,接著將此反應溶液加熱至75℃,以進行水解,待反應完全後,以去離子水進行萃取使有機層達到中性,最後移除溶劑以製得一水解產物。
將上述水解產物、1998克的甲苯以及10克的氫氧化鉀置於反應槽中,於反應槽中通入氮氣,並於室溫下均勻攪拌以製得一反應溶液。將此反應溶液進行加熱至85℃。待反應完全後,以去離子水進行萃取使有機層達到中性,最後移除溶劑以完成化合物4的製備。化合物4之平均單元結構式為(PhSiO3/2
)0.5
(ViMe2
SiO1/2
)0.5
。
製備例5:含矽氫鍵之聚矽氧烷(化合物5)的製備方法
將3432.04克(14 mole)的二苯基二甲氧基矽烷(Diphenyldimethoxysilane,購自六和化工股份有限公司,台灣),以及1880.62克(14 mole)的四甲基二矽氧烷(1,1,3,3-Tetramethyldisiloxane,購自恆橋產業有限公司,台灣)置於反應槽中,於室溫下攪拌以製得一均勻混和溶液。將混和溶液滴入濃度50%的硫酸水溶液(2669克)中以製得一反應溶液,接著將此反應溶液於室溫下反應4小時以進行水解。待反應完全後,以去離子水萃取使有機層達到中性,最後移除溶劑以完成化合物5的製備。化合物5之平均單元結構式係(Ph2
SiO2/2
)0.33
(HMe2
SiO1/2
)0.67
。
製備例6:含矽氫鍵之聚矽氧烷(化合物6)的製備方法
將2776克(14 mole)的苯基三甲氧基矽烷( phenyltrimethoxysilane ,購自六和化工股份有限公司,台灣),以及1880.62克(14 mole)的四甲基二矽氧烷(1,1,3,3-tetramethyldisilloxane,購自恆橋產業有限公司,台灣)置於反應槽中,於室溫下攪拌以製得均勻混和溶液。將混和溶液滴入質量濃度為50%的硫酸水溶液(2669克)中以製得反應溶液,接著將此反應溶液於室溫下反應4小時以進行水解。待反應完全後,以去離子水萃取使有機層達到pH值為中性,最後移除溶劑以完成含矽氫鍵的聚矽氧烷(化合物6)的製備,化合物6的平均單元結構式為(PhSiO3/2
)0.33
(HMe2
SiO1/2
)0.67
。
實施例1
首先,先於反應瓶中置入47.3克的化合物2、18.4克的化合物4、20克的化合物5,1000ppm(相對於100克的化合物1,化合物2,化合物4及化合物5的總和)的1-乙炔基環己醇作為抑製劑,以及1.5重量份的氣相二氧化矽(TS-720,購自Cabot Corp.,美國)以製得第一溶液。於另一反應瓶中置入14.3克的化合物1,以及4.3ppm(相對於100克的化合物1,化合物2,化合物4及化合物5的總和)的辛醇絡鉑化合物(PIatinum–Octanal/Octanol Complex,購自Gelest,美國)以形成第二溶液。將第一溶液、第二溶液、30克的經甲基矽酮處理之雲母層片(購自加全實業,台灣)、30克的溶劑甲苯以及與前述材料等重量的0.3mm鋯珠,以真空行星脫泡機Thinky ARV-310機型攪拌均勻,並於PET基材上進行塗布,再經80°C加熱15分鐘、150°C加熱3小時固化後,撕除PET基材,製得矽膠薄膜。矽膠薄膜厚度約為50微米(μm)。
實施例2
以相同於實施例1之方法製得矽膠薄膜,但將經甲基矽酮處理之雲母層片之使用量變更為40重量份,並將溶劑甲苯之使用量變更為35重量份。
實施例3
首先,先於反應瓶中置入47.84克的化合物3、19.53克的化合物4、15.96克的化合物5、2.05克的化合物6,1000ppm(相對於100克的化合物1,化合物3,化合物4,化合物5及化合物6的總和)的1-乙炔基環己醇作為抑製劑,以及1.5重量份的氣相二氧化矽(TS-720,購自Cabot Corp.,美國)以製得第一溶液。於另一反應瓶中置入14.53克的化合物1,以及4.3ppm(相對於100克的化合物1,化合物3,化合物4,化合物5以及化合物6的總和)的辛醇絡鉑化合物(PIatinum–Octanal/Octanol Complex,購自Gelest,美國)以形成第二溶液。將第一溶液、第二溶液、10克的經甲基矽酮處理之雲母層片(購自加全實業,台灣)、10克的溶劑甲苯以及與前述材料等重量的0.3mm鋯珠,以真空行星脫泡機Thinky ARV-310機型攪拌均勻,並於PET基材上進行塗布,再經80°C加熱15分鐘、150°C加熱3小時固化後,撕除PET基材,製得矽膠薄膜。矽膠薄膜厚度約為50微米(μm)。
實施例4
以相同於實施例3之方法製得矽膠薄膜,但將經甲基矽酮處理之雲母層片之使用量變更為30重量份,並將溶劑甲苯之使用量變更為37重量份。
實施例5
以相同於實施例3之方法製得矽膠薄膜,但將經甲基矽酮處理之雲母層片之使用量變更為40重量份,並將溶劑甲苯之使用量變更為37重量份。
比較例1
以相同於實施例1之方法製得矽膠薄膜,但未添加經甲基矽酮處理之雲母層片以及溶劑甲苯。
比較例2
以相同於實施例3之方法製得矽膠薄膜,但未添加經甲基矽酮處理之雲母層片以及溶劑甲苯。
比較例3
以相同於實施例1之方法製得矽膠薄膜,但將經甲基矽酮處理之雲母層片之使用量變更為50重量份,並將溶劑甲苯之使用量變更為45重量份。
以下,將本發明所提出的具阻水氣特性的矽膠薄膜依照下列方法進行評估測試,量測結果如下列表1所示。
水氣穿透率(WVTR)量測
水氣穿透率(WVTR)以Moconaquatran model 1 (量測範圍:5-5×10-5
gm-2
day-1
)依據ASTM F1249規則量測,量測面積0.5-5cm2
,於溫度25℃、濕度90%RH條件下進行量測。
熱膨脹係數(CTE)
依照ASTM E831規則,以熱機械分析儀(TMA from TA instrument)在氮氣環境中,以10℃/分鐘的升溫速率量測30-100℃範圍內的CTE,所用張力為0.0023N。
穿透率(T%)
以分光光度計(U4100,購自Hitachi,日本)量測380-700nm波長範圍內之光穿透率。
霧度量測
以霧度計(NDH2000,購自日本電色工司)量測矽膠薄膜之霧度。
表面粗糙度(Roughness, Sa)量測
使用Olympus OLS5000 3D雷射顯微鏡,以雷射共軛焦的原理,根據ISO25178規則量測矽膠薄膜表面的算術平均高度(Sa)。
表1:實施例1-實施例5以及比較例1-比較例2之矽膠薄膜特性測試結果
表1 | WVTR (gm-2 day-1 ) | 25-50℃ CTE(ppm) | 80-100℃ CTE(ppm) | 穿透率(%) | 霧度 (%) | 粗糙度 (μm) |
實施例1 | 18.88 | 37.7 | 144.5 | 97.19 | 0 | 0.039 |
實施例2 | - | 33.8 | 93.9 | 96.26 | 0 | 0.056 |
實施例3 | 38.64 | 56.5 | 140.4 | 98.43 | 0 | 0.014 |
實施例4 | 21.64 | 23.3 | 76.3 | 97.89 | 0 | 0.022 |
實施例5 | 17.78 | 22.4 | 52.4 | 97.41 | 3.38 | 0.112 |
比較例1 | 74.37 | 117.9 | 292.1 | 97.51 | 0 | 0.029 |
比較例2 | 63.76 | 92.2 | 258.4 | 98.24 | 0 | 0.01 |
比較例3 | 15.76 | 26.8 | 103 | 92.68 | 57.44 | 0.53 |
於表1所列之測試結果,實施例1至實施例5之矽膠薄膜因添加了微層片,故水氣穿透率皆小於比較例1及比較例2之矽膠薄膜。且實施例1至實施例5的之光穿透率皆仍大於96%,實施例1至實施例4之矽膠薄膜之霧度皆僅有0,顯見仍能具有良好的光學性質。此外,實施例1至實施例5之熱膨脹係數皆比比較例1及比較例2為低,故可具有更好的加工性以利後續形成無機鍍膜層。
實施例6
將實施例3所製得之矽膠薄膜進一步利用Syskey Technology之濺鍍設備,以氬氣做為工作氣體,在0.005 Torr的工作壓力下,以濺鍍法在薄膜表面形成一厚度約為50奈米(nm)之氧化鋁(Al2
O3
)鍍膜層。
實施例7
將實施例3所製得之矽膠薄膜以氧氣電漿進行前處理。接著,利用ALD設備(i-SA,購自Syskey Technology,台灣),以三甲基鋁(AlCH3
)3
以及四雙(乙基甲基氨)鉿(Tetrakis(ethylmethylamino)hafnium,TEMAHF)做為前驅物,水(H2
O)做為氧化劑,以高純度氮氣作為吹掃氣和載氣,在25°C及9 Torr的工作壓力下,以原子層沉積法在矽膠薄膜表面上形成一厚度約為20奈米之三氧化二鋁(Al2
O3
)/二氧化鉿(HfO2
)鍍膜層。
實施例8
將實施例2所製得之矽膠薄膜以相同於實施例7之方法在矽膠薄膜上以原子層沉積法在矽膠薄膜表面上形成一厚度約為20奈米之三氧化二鋁(Al2
O3
)/二氧化鉿(HfO2
)鍍膜層。
上述實施例6至實施例8的具阻水氣特性的矽膠薄膜之詳細測試結果如下列表2所示。
表2:實施例6-實施例8之矽膠薄膜特性測試結果
表2 | WVTR (gm-2 day-1 ) |
實施例6 | 0.453 |
實施例7 | 0.259 |
實施例8 | 0.161 |
由表2所列之測試結果可知,矽膠薄膜之表面可再形成無機鍍膜層以進一步降低水氣穿透率。實施例6至實施例8在形成無機鍍膜層後水氣穿透率可進一步的下降至0.5 gm-2
day-1
以下。故本發明之具阻水氣特性的矽膠薄膜可同時具有良好的阻水氣性質且兼具優良的之可加工性。
綜上所述,雖然本發明已以較佳實施例揭露如上,然其並非用以限定本發明。本發明所屬技術領域中具有通常知識者,在不脫離本發明之精神和範圍內,當可作各種之更動與潤飾。因此,本發明之保護範圍當視後附之申請專利範圍所界定者為準。
無
Claims (13)
- 一種具阻水氣特性的矽膠薄膜,其係經由固化一可固化矽樹脂組成物而形成,該可固化矽樹脂組成物包含: 10至25重量份的一線性聚矽氧烷,其平均單元結構式至少具有一個與矽原子鍵結之芳基與二個與矽原子鍵結之烯基; 40至55重量份的一第一矽樹脂,其平均單元結構式至少具有R1 SiO3/2 單體以及R2 2 SiO2/2 單體,其中R1 及R2 為經取代的或未取代之烷基、經取代的或未取代之烯基或經取代的或未取代之芳基,於此平均單元結構式中,該R1 SiO3/2 單體所占的莫耳分率係介於0.60至0.75之間,且矽原子鍵結之烯基相對於所有與矽鍵結之官能基之莫耳數比值為0.03至0.15; 15至30重量份的一第二矽樹脂,其平均單元結構式至少具有R3 SiO3/2 以及R4 3 SiO1/2 之單體,其中R3 及R4 為經取代的或未取代之烷基、經取代的或未取代之烯基或經取代的或未取代之芳基; 15至25重量份的至少一含矽氫鍵之聚矽氧烷,其化學結構式為:HR5 2 SiO(SiR6 2 O)n SiR5 2 H,其中,R5 為經取代的或未取代的烷基或氫原子,R6 為經取代或未取代的芳基或經取代的或未取代的烷基,n為大於等於0之整數; 10至40重量份的微層片(microsheet);以及 一鉑族金屬系催化劑; 其中,該具阻水氣特性的矽膠薄膜之水氣穿透率(WVTR)小於40gm-2 day-1 ,可見光穿透率大於92%且霧度小於4%。
- 如請求項1之具阻水氣特性的矽膠薄膜,其中該微層片之一長徑比係介於10至200之間。
- 如請求項1之具阻水氣特性的矽膠薄膜,其中該微層片之一長度係介於0.1微米(μm)至25微米(μm)之間。
- 如請求項1之具阻水氣特性的矽膠薄膜,其中該微層片係選自由雲母、黏土、層狀雙氫氧化合物、磷酸氫鈣以及氮化硼所組成之群組之至少之一或其組合。
- 如請求項1之具阻水氣特性的矽膠薄膜,其中該具阻水氣特性的矽膠薄膜之25℃-50℃熱膨脹係數(CTE)係介於20ppm至60ppm之間,80℃-100℃熱膨脹係數(CTE)係介於50ppm至150ppm之間,且表面的算術平均高度(Sa)係介於0.01微米(µm)至0.15微米(µm)間。
- 如請求項1之具阻水氣特性的矽膠薄膜,其中該可固化矽樹脂成物進一步包括抑制劑、觸變劑、抗沉降劑、無機填料、螢光粉或其組合。
- 如請求項6之具阻水氣特性的矽膠薄膜,其中於可固化矽樹脂成物中的無機填料包括一氣相二氧化矽。
- 如請求項1之具阻水氣特性的矽膠薄膜更包括一無機鍍膜層,其位於該具阻水氣特性的矽膠薄膜之一表面上。
- 如請求項8之具阻水氣特性的矽膠薄膜,其中該無機鍍膜層係藉由濺鍍法(Sputter Deposition)或原子層沉積法(Atomic Layer Deposition,ALD)形成於該具阻水氣特性的矽膠薄膜之一表面上。
- 如請求項8之具阻水氣特性的矽膠薄膜,其中該無機鍍膜層之厚度係介於10奈米(nm)至300奈米(nm)之間。
- 如請求項8之具阻水氣特性的矽膠薄膜,其中該無機鍍膜層包括二氧化矽(SiO2 )、三氧化二鋁(Al2 O3 )或二氧化鉿(HfO2 )。
- 如請求項8之具阻水氣特性的矽膠薄膜,其中該具阻水氣特性的矽膠薄膜之水氣穿透率(WVTR)小於0.5gm-2 day-1 。
- 一種光學半導體裝置,其中該光學半導體裝置係由請求項1至請求項12中任一項具阻水氣特性的矽膠薄膜封裝而成。
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