TW202212479A - 硬化性聚有機矽氧烷組成物及電子零件 - Google Patents
硬化性聚有機矽氧烷組成物及電子零件 Download PDFInfo
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- TW202212479A TW202212479A TW110119849A TW110119849A TW202212479A TW 202212479 A TW202212479 A TW 202212479A TW 110119849 A TW110119849 A TW 110119849A TW 110119849 A TW110119849 A TW 110119849A TW 202212479 A TW202212479 A TW 202212479A
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- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 1
- QLNOVKKVHFRGMA-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical group [CH2]CC[Si](OC)(OC)OC QLNOVKKVHFRGMA-UHFFFAOYSA-N 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
- 239000005051 trimethylchlorosilane Substances 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 125000005023 xylyl group Chemical group 0.000 description 1
- 125000006839 xylylene group Chemical group 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
- NDKWCCLKSWNDBG-UHFFFAOYSA-N zinc;dioxido(dioxo)chromium Chemical compound [Zn+2].[O-][Cr]([O-])(=O)=O NDKWCCLKSWNDBG-UHFFFAOYSA-N 0.000 description 1
- CHJMFFKHPHCQIJ-UHFFFAOYSA-L zinc;octanoate Chemical compound [Zn+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O CHJMFFKHPHCQIJ-UHFFFAOYSA-L 0.000 description 1
- 150000003755 zirconium compounds Chemical class 0.000 description 1
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Abstract
本發明之硬化性聚有機矽氧烷組成物係包含:(a)聚有機矽氧烷,係在一分子中具有2個以上之硬化性官能基;(b)交聯劑,係在一分子中具有2個以上與前述(a)的硬化性官能基具有反應性之交聯基;(c)硬化觸媒,係可使前述(a)及(b)之交聯反應觸媒化;(d)顏料,係其本身不發出螢光;及(e)UV追蹤劑。同組成物係成為容易確認是否對於同系顏色之基材被均勻施用的接著劑。
Description
本發明係關於一種容易確認被施用於基材之狀態的硬化性聚有機矽氧烷組成物。又,亦有關一種該組成物對基材之施用狀態的確認方法。
係自以往已知有各種在室溫進行硬化而產生橡膠狀彈性體之室溫硬化性聚有機矽氧烷組成物。該組成物係有LCD(Liquid Crystal Display)等電性電子機器的塗覆材或灌封材等用途。在該用途係使用藉由與空氣中之水分接觸而產生硬化反應之類型者,且硬化時釋出對於金屬類之腐蝕小的醇或丙酮等。如此之組成物係作業性為良好之外,電極或配線的腐蝕之虞少,又,接著性等亦優異。有時依據零件而被要求遮光性、隱蔽性,但在該情況,可藉由添加顏料來進行對應,故普遍地被使用(例如,日本特開2007-169356號公報)。又,從操作性、深部硬化性之觀點而言,使用聚有機矽氧烷組成物之接著劑係亦採用將組成物分成主劑與硬化劑之兩種,而在使用時進行混合之二液型的形態。
在基材之接著中,為確保接著之強度、可靠性,作為接著劑之聚有機矽氧烷組成物必需對於基材發揮均勻地接著力。包含主劑與硬化劑的二液型的情形,就用以發揮均勻的接著力之前提而言,在施用於基材之前,必須均勻
地混合主劑與硬化劑,故吾人正在研究混合狀態之確認手段(日本特開2019-143074號公報)。
[先前技術文獻]
[專利文獻]
[專利文獻1]日本特開2007-169356號公報
[專利文獻2]日本特開2019-143074號公報
可容易確認對基材之施用狀態,係與避免因接著力之不足等產生不良品之風險相關連,在電子零件等構件之製造中為有利作用的因素。
如日本特開2007-169356號公報,有時在接著劑調配顏料等而進行著色,但另一方面,基材之種類亦包含其顏色而為各式各樣。依據基材之種類,亦有聚矽氧接著劑與基材為同系顏色。基材與接著劑為同系顏色時,以可見光所進行的判別有時難以確認施用之狀態。若無法確認是否有均勻地進行施用,則有與基材之接著成為不完全之虞,對製品之可靠性亦造成不良影響。在以往之接著劑中,當施用與基材同顏色之接著劑時,難以確認是否確實地被施用。只能耗費時間以目視進行確認,或者只能使用不同的顏色之接著劑。
在日本特開2019-143074號公報之方法,即使可確認混合狀態,是否亦被均勻地施用則無法被判斷,而難以正確地評估施用之狀態。
[發明之目的]
本發明之目的在於提供一種被著色之聚矽氧接著劑,且容易確認是否對於同系顏色之基材被均勻地施用之接著劑、及使用同接著劑之施用狀態的確認方法。
本發明人等發現係藉由併用其本身不發出螢光之顏料與UV追蹤劑,即使施用於同系顏色之基材時,亦可在UV光下簡單地確認屬於接著劑之組成物的施用狀態。亦即,本發明主要的一態樣係一種硬化性聚有機矽氧烷組成物,係包含:(a)聚有機矽氧烷,係在一分子中具有2個以上之硬化性官能基;(b)交聯劑,係在一分子中具有2個以上與前述(a)之硬化性官能基具有反應性之交聯基;(c)硬化觸媒,係可催化前述(a)及(b)之交聯反應;(d)顏料,係其本身不發出螢光;及(e)UV追蹤劑。又,本發明之另一態樣係一種確認硬化性聚有機矽氧烷組成物對基材的施用狀態之方法,其係包含:提供前述組成物之步驟;提供與該組成物之色差(△E)為20以下之基材的步驟;使該組成物施用於該基材之步驟;及對施用於該基材之該組成物照射紫外線之步驟。
藉由本發明,可提供一種容易確認是否對於同系顏色之基材被均勻地施用之接著劑。又,提供一種方法,其係以硬化性聚有機矽氧烷組成物作為接著劑,確認接著劑與同系顏色對基材的施用狀態。
[發明之詳細說明]
以下,有關本發明之組成物,詳細說明每一項目。又,在本說明書中,表示數值範圍之波浪線「至」係包含在其前後所記載之數值作為下限值及上限值的意義而使用。
在本說明書中使用時,所謂「有機基」係意指含有碳之基。有機基之價數係藉由以n作為任意之自然數而記載為「n價之」來表示。因此,例如所謂「1價之有機基」係意指僅具有1個鍵結鍵之含有碳的基。鍵結鍵係可具有碳以外之元素。未特別明示價數時,只要為發明所屬技術領域者,可從文脈把握適合的價數。
在本說明書中使用時,所謂「烴基」係意指包含碳及氫之基,並使1個之氫原子從分子脫離之基。如此之烴基並無特別限定,但可列舉可藉由1個或多於1個之取代基取代的碳原子數1至20之烴基,例如,脂肪族烴基、芳香族烴基等。上述「脂肪族烴基」係可為直鏈狀、分枝鏈狀或環狀之任一者,亦可為飽和或不飽和之任一者。又,烴基係可包含1個或多於1個之環構造。又,如此之烴基係可於其末端或分子鏈中具有1個或多於1個之氮原子(N)、氧原子(O)、硫黃原子(S)、矽原子(Si)、醯胺鍵、磺醯基鍵、矽氧烷鍵、羰基、羰氧基等之雜原子或包含雜原子的構造。
在本說明書中使用時,「烴基」之取代基並無特別限定,但例如,可列舉鹵素原子;可被1個或多於1個之鹵素原子所取代之選自C1-6烷基、C2-6烯基、C2-6炔基、C3-10環烷基、C3-10不飽和環烷基、5至10員之雜環基、5至10員之不飽和雜環基、C6-10芳基及5至10員之雜芳基的基。
在本說明書中,烷基及苯基只要無特別記載,可為非取代,亦可為被取代。如此之基的取代基並無特別限定,但例如,可列舉選自鹵素原子、C1-6烷基、C2-6烯基及C2-6炔基之1個或多於1個之基。
[硬化性聚有機矽氧烷組成物]
‧成分(a)
本發明之硬化性聚有機矽氧烷組成物係包含至少1種之在分子內具有2個以上之硬化性官能基的聚有機矽氧烷作為成分(a)。成分(a)係發揮作為硬化性聚有機矽氧烷組成物之基質聚合物。在此,所謂「硬化性官能基」係指可產生硬化反應之官能基。硬化反應之機制並無特別限制,而可採用一般被使用於樹脂之硬化的方法。硬化反應係特別採用縮合反應或加成反應。在一分子中所含有的各種之硬化性官能基係以相同的官能基為佳,但若為產生同種之硬化反應的官能基,即使為相異的種類之官能基,亦可混合在相同分子內。硬化性官能基較佳係至少一個一個地存在於成分(a)之分子主鏈之兩末端。又,在此,在本說明書中,所謂成分(a)之分子主鏈係表示在成分(a)之分子中相對最長的鍵結鏈。
成分(a)之分子骨架只要矽氧烷鍵結為主骨架者即可,並無特別限制。矽氧烷骨架可被2價之有機基中斷。在此,在說明矽氧烷化合物之構造中,有時依據如以下之簡稱記載矽氧烷化合物之構造單元。以下,有時將此等之構造單元分別稱為「M單元」「D單元」等。
M:-Si(CH3)3O1/2
MH:-SiH(CH3)2O1/2
MVi:-Si(CH=CH2)(CH3)2O1/2
D:Si(CH3)2O2/2
DH:SiH(CH3)O2/2
T:Si(CH3)O3/2
Q:SiO4/2
以下,在本說明書中,矽氧烷化合物係組合上述之構造單元而建構者,但可至少部分地包含上述構造單元之甲基取代成如氟之鹵素、如苯基之烴基等其他的基者。又,例如記載為DH 20D20時,並非意指DH單元連續20個之後D單元連續20個,而理解為各別之單元可任意地排列。矽氧烷化合物可藉由T單元或Q單元三維地取得各式各樣的構造。因而,成分(a)可採用直鏈狀、分枝鏈狀、環狀、此等構造之組合等任意的分子骨架。成分(a)較佳係具有直鏈狀之分子骨架。
在本發明之一態樣中,成分(a)係例示以下述式(1)所表示之直鏈狀聚有機矽氧烷。
(Ra)3-pRpSi-O-(Si(R)r(Ra)2-rO)n-SiRq(Ra)3-q‧‧‧(1)(式中,
Ra係分別獨立地為硬化性官能基,
R係分別獨立地為1價之有機基,
p及q係分別獨立地為0、1或2,
r係分別獨立地為0、1或2,
n係在23℃之黏度為0.01至50Pa‧s之數)R係以具有烴基,尤其烷基、烯基、芳基為較佳。從調控折射率等物性之觀點而言,R之至少一部分可為苯基等芳基、乙烯基等烯基。從取得之容易性而言,特別佳係使用R全部為如甲基之聚有機矽氧烷。有關硬化性官能基之位置較佳係在
上述式(1)中,r為2之聚有機矽氧烷,亦即,硬化性官能基至少1個1個地僅存在於分子之兩末端的直鏈狀聚有機矽氧烷。
(產生縮合反應之硬化性官能基)
成分(a)係在一分子中具有2個以上之可利用於矽氧烷樹脂之硬化反應的官能基者。若依據硬化反應之類型進行分類,在一個態樣中,上述成分(a)係可為具有2個以上與選自由羥基及可水解的基所成的群中之至少一個基鍵結的Si原子之聚有機矽氧烷。此時,羥基及/或可水解的基成為相當於前述式(1)之基Ra的硬化性官能基。
所謂「可水解的基」係在本說明書中使用時,意指可接受水解反應之基,亦即,意指可藉由水解反應從化合物之主骨架脫離之基。可水解的基之例係可列舉-OR’、-OCOR’、-O-N=CR’2、-NR’2、-NHR’、鹵素原子(此等式中,R’係表示取代或非取代之碳原子數1至4的烷基)等,較佳係-OR’(亦即,烷氧基)。在R’之例係包含甲基、乙基、丙基、異丙基、正丁基、異丁基等非取代烷基;氯甲基等取代烷基。其等之中,以烷基為佳,特別以非取代烷基為較佳,以甲基或乙基為更佳。羥基並無特別限定,但可為可水解的基進行水解所產生者。鹵素原子可列舉氟原子、氯原子、溴原子、碘原子,此等之中,以氯原子為較佳。
具有產生縮合反應之硬化性官能基的聚有機矽氧烷較佳係在前述式(1)中,p及q為0或1,且r為2,亦即,僅在分子末端各具有2個或3個、計4個或6個之可水解的基,尤其具有烷氧基者。
就產生縮合反應之類型的成分(a)而言,滿足以上之條件的較佳例係可列舉兩末端以甲基二甲氧基矽基、或三甲氧基矽基封鏈之直鏈狀聚有機矽氧烷等。可
利用來作為如此的成分(a)之聚有機矽氧烷係可利用所市售者。又,可使用藉由公知之反應導入硬化性官能基之聚有機矽氧烷。
(產生加成反應之硬化性官能基)
在另一態樣中,上述成分(a)係亦可為具有2個以上之Si原子的化合物,該Si原子係與具有藉由加成反應進行硬化之(甲基)丙烯醯基或乙烯基的脂肪族不飽和鍵,尤其烯基之基鍵結。產生加成反應之硬化性官能基係以乙烯基為更佳。此時,脂肪族不飽和基成為相當於前述式(1)之基Ra的硬化性官能基。
具有產生加成反應之硬化性官能基的聚有機矽氧烷較佳係在前述式(1)中,p及q為2,且r為2,亦即,僅在分子末端具有1個1個地,計2個之可加成反應的基,尤其具有乙烯基者。
就產生縮合反應之類型的成分(a)而言,滿足以上之條件的較佳之例係可列舉兩末端以二甲基乙烯基矽基封鏈的直鏈狀之聚有機矽氧烷等。可利用來作為如此的成分(a)之聚有機矽氧烷係可利用所市售者。又,可使用藉由公知之反應導入硬化性官能基之聚有機矽氧烷。
成分(a)之調配量係只要為硬化性聚有機矽氧烷組成物可操作之黏度的範圍之量即可,並無特別限制。以成分(a)之量作為基準,在以下個別所示之較佳的範圍內,可適當設定其他之成分的調配量。
‧成分(b)
在本發明之硬化性組成物的交聯劑係在一分子中具有2個以上與前述成分(a)具有之硬化性官能基具有反應性之交聯基者(以下,有時僅稱為「成分(b)」)。藉由包含交聯劑,從硬化性組成物所得到之硬化物之物性,例如拉伸強度或彈性率為良好。成分(b)具有之交聯基係可使用對一般利用於聚矽氧之硬化反應的反
應具活性的官能基,依照前述成分(a)具有之反應性官能基而決定。例如,前述成分(a)具有之反應性官能基可進行羥基或烷氧基等縮合反應之官能基時,係可採用直接鍵結於矽之如羥基或烷氧基的水解性基作為交聯基。前述成分(a)具有之反應性官能基可進行乙烯基等加成反應之官能基時,係可採用直接鍵結於矽之氫原子,亦即,Si-H基作為交聯基。成分(b)在每一分子具有之交聯基的數係為在成分(a)間形成交聯構造,必須為2個以上,但為藉由交聯反應產生網目狀構造,故以3個以上為較佳。各別之交聯基係可鍵結於相同之矽原子,亦可鍵結於相異的矽原子。
成分(b)可為僅具有1個矽之化合物,亦即,矽烷之衍生物,可為具有2個以上之矽的化合物。具有2個以上之矽的化合物時,成分(b)較佳係具有藉由各矽原子以氧所交聯的矽氧烷鍵結經連結之構造。包含2個以上之矽原子的成分(b)之分子骨架可為直鏈狀、分枝鏈狀、環狀之任一者。
<<產生縮合型反應之交聯劑>>
前述成分(a)產生縮合型之反應的聚有機矽氧烷時,成分(b)係具有至少2個與Si原子鍵結之羥基或水解性基的化合物(惟,相當於前述成分(a)者除外)或其部分水解縮合物。水解性基係例示如甲氧基、乙氧基、丙氧基、丁氧基之烷氧基;如2-甲氧基乙氧基、2-乙氧基乙氧基之取代烷氧基;如異丙烯氧基之烯氧基、如甲基乙基酮肟基之酮肟根(ketoximato)基、乙醯氧基等,可為互相相同,亦可為相異。各別之水解性基係可鍵結於相同之矽原子,亦可鍵結於相異之矽原子。例如,亦可使用具有與Si原子鍵結之羥基或水解性基以矽氧烷鍵連結的構造之化合物作為交聯劑。水解性基以外之鍵結於矽原子之基可分別獨立地為1價之有機基。
因容易取得對應之矽化合物,故1價之有機基係以烴基為較佳,尤其,以甲基、乙烯基、苯基為較佳。
更具體的成分(b)係例如,可列舉以式(2):
R1 aSi(OR2)4-a (2)(式中,R1係分別獨立地為取代或非取代之1價之烴基,R2係分別獨立地為氫原子或1價之有機基,a為0、1或2)所表示之有機矽化合物或其部分水解縮合物。R2係分別獨立地為氫原子或1價之有機基。1價之有機基係意指含有1價之碳的基。如此之1價的有機基並無特別限定,但可列舉1價之烴基。烴基係與上述為相同意義。
R1較佳係分別獨立地為碳原子數1至12之取代或非取代的1價烴基。具體而言,R1可列舉甲基、乙基、丙基、異丙基、丁基、異丁基、第三丁基、戊基、新戊基、己基、庚基、辛基、壬基、癸基等烷基;環戊基、環己基、環庚基等環烷基;苯基、甲苯基、二甲苯基、萘基等芳基;苯甲基、苯基乙基、苯基丙基等芳烷基;乙烯基、烯丙基、丙烯基、丁烯基等烯基;乙炔基、丙炔基等炔基;及,此等基之氫原子的一部分或全部以氟、氯、溴等鹵素原子取代後的基(例如,氯甲基、溴乙基、氯丙基、三氟丙基、3,3,4,4,5,5,6,6,6-九氟己基)等。從容易取得性、獲得優異之交聯反應速度而言,R1係以甲基或乙烯基為較佳。
R2係分別獨立地為氫原子或1價之有機基。如此之1價之有機基並無特別限定,但可列舉1價之烴基。烴基係與上述為相同的意義。R2係以CH3-、C2H5-、C3H7-、CF3CH2-、CH3CO-、CH2=C(CH3)-、CH3CH2C(CH3)=N-、(CH3)2N-、(C2H5)2N-、CH2=C(OC2H5)-、(CH3)2C=C(OC8H17)-、或
a係以1或2為較佳。
成分(b)具有之交聯基如上述式,可鍵結於相同的矽原子,但亦可鍵結於相異的矽原子。例如,由鍵結於矽之OR2基所構成的構造為2個如以2價之有機基連結的構造之化合物亦可利用作為成分(b)。2價之有機基係由矽氧烷鍵結所構成的2價之基以外,亦可為2價之烴基。2價之烴基,具體而言,可例示亞甲基、伸乙基、伸丙基、甲基伸乙基、伸丁基、六亞甲基等伸烷基;伸環己基等伸環烷基、伸苯基、伸甲苯基、伸二甲苯基、伸萘基、伸聯苯基等伸芳基;以鹵素原子等取代此等基之氫原子的一部分或全部的基;及此等之取代或非取代之伸烷基、伸芳基之組合。其中,2價之烴基係以亞甲基、伸乙基、伸丙基、伸丁基、六亞甲基、伸環己基及伸苯基為較佳,尤其,以伸乙基、伸丙基、伸丁基及伸苯基為較佳。
成分(b)係亦可為具有2個以上之基R2的環狀之矽氧烷。在此情形,基R2係可直接鍵結於形成矽氧烷環之矽原子,亦可不鍵結於形成矽氧烷環之矽原子。環狀之矽氧烷較佳係以環員數為6至10,以8為更佳。亦即,較佳係形成含有3至5個,尤其4個之由Si-O所構成的單元之環。
在較佳的態樣中,成分(b)係例示四甲氧基矽烷、甲基三甲氧基矽烷、乙烯基三甲氧基矽烷、苯基三甲氧基矽烷、四乙氧基矽烷、甲基三乙氧基矽烷、乙烯基三乙氧基矽烷、苯基三乙氧基矽烷、四丙氧基矽烷、四異丙氧基矽烷、二甲基二甲氧基矽烷、乙烯基甲基二甲氧基矽烷、二甲基二乙氧基矽烷及3-氯丙
基三甲氧基矽烷以及如其等之部分水解縮合物之含有烷氧基的化合物;肆(2-乙氧基乙氧基)矽烷、甲基參(2-甲氧基乙氧基)矽烷、乙烯基(2-乙氧基乙氧基)矽烷及苯基參(2-甲氧基乙氧基)矽烷以及如其等之部分水解縮合物之含有取代烷氧基之化合物;甲基三丙烯氧基矽烷、甲基三異丙烯氧基矽烷、乙烯基三異丙烯氧基矽烷、苯基三異丙烯氧基矽烷、二甲基二異丙烯氧基矽烷及甲基乙烯基二異丙烯氧基矽烷以及如其等之部分水解縮合物之含有烯氧基之化合物;甲基三乙醯氧基矽烷及如其等之部分水解縮合物之含有醯氧基之化合物等。
就交聯性之點而言,成分(b)較佳係不具有其他之反應性官能基,但交聯基以外可具有反應性官能基。如此之交聯劑係不僅有助於交聯反應(縮合反應),亦可發揮接著賦予劑功能。在此,其他之反應性官能基可列舉第一級胺基、環氧基、(甲基)丙烯醯基、(甲基)丙烯醯氧基、氫硫基、異氰酸基等。
如此之具有與成分(a)的交聯基以外之反應性官能基的交聯劑例如,可例示如3-胺基丙基三甲氧基矽烷、3-胺基丙基三乙氧基矽烷、3-胺基丙基三異丙氧基矽烷、3-胺基丙基三乙醯胺矽烷、N-(2-胺基乙基)-3-胺基丙基三甲氧基矽烷、N-(2-胺基乙基)-3-胺基丙基三乙氧基矽烷、N-甲基-3-胺基丙基三甲氧基矽烷、N-苯基-3-胺基丙基三甲氧基矽烷、N,N-二甲基-3-胺基丙基三甲氧基矽烷之取代或非取代之含有胺基的矽烷;如3-環氧丙氧基丙基三甲氧基矽烷、3-環氧丙氧基丙基三乙氧基矽烷、3-環氧丙氧基丙基甲基二甲氧基矽烷、3,4-環氧基環己基乙基三甲氧基矽烷之含有環氧基的矽烷;如3-異氰酸基丙基三甲氧基矽烷、3-異氰酸基丙基三乙氧基矽烷、3-異氰酸基丙基甲基二甲氧基矽烷之含有異氰酸基的矽烷;如參(3-三甲氧基矽基丙基)三聚異氰酸酯、參(3-三乙氧基矽基丙基)三聚異氰酸酯等之參(3-三烷氧基矽基丙基)三聚異氰酸酯之三聚異氰酸酯化合物;
雜氮矽三環(Silatrane)之氧被1個碳取代之具有碳雜氮矽三環骨架的矽烷化合物;如3-丙烯醯氧基丙基三甲氧基矽烷、3-甲基丙烯醯氧基丙基三甲氧基矽烷、3-丙烯醯氧基丙基甲基二甲氧基矽烷、3-甲基丙烯醯氧基丙基甲基二甲氧基矽烷、3-甲基丙烯醯氧基丙基甲基二乙氧基矽烷之含有(甲基)丙烯醯氧基的矽烷;如3-氫硫基丙基三甲氧基矽烷之含有氫硫基的矽烷;及含有第一級胺基的矽烷與含有環氧基的矽烷之混合物或者反應物。
<<產生加成反應之交聯劑>>
成分(a)為具有乙烯基等之不飽和基作為硬化性官能基時,成分(b)之交聯基可列舉Si-H鍵結。具有如此之交聯基的交聯劑係使用含有氫基的矽氧烷之氫聚有機矽氧烷。氫聚有機矽氧烷係具有Si-H鍵結之矽氧烷化合物,且成為交聯劑之成分。氫聚有機矽氧烷代表性係在分子中具有2個以上之以下述式(3)所示之單元。
(Rb)x(RC)ySiO(4-x-y)/2 (3)(式中,
Rb係氫原子,
RC係C1-6烷基(例如,甲基、乙基、丙基、丁基、戊基、己基,較佳係甲基)或苯基;
x係1或2;
y係0至2之整數,惟,x+y為1至3)
在氫聚有機矽氧烷中之矽氧烷骨架係可列舉環狀、分枝狀、直鏈狀者,但較佳係環狀或直鏈狀之骨架,更佳係直鏈狀之骨架。氫聚有機矽氧烷之主鏈係以直鏈狀之骨架為較佳,但可為具有經分枝之構造作為取代基之骨架。又,一分子所含有的鍵結在矽原子的氫基(亦即,與Si-H鍵結等價)之數必須為至
少3個以上,但每一分子之平均以5個以上為較佳,以8個以上為更佳。對於在氫聚有機矽氧烷中之其他的條件、氫基以外之有機基、鍵結位置、聚合度、構造等並無特別限定,但為直鏈狀之構造時,若聚合度為10至100,尤其,為15至70之範圍,所得到之組成物的操作性有更提升之傾向,故為較佳。可使用之氫聚有機矽氧烷之具體例係包含8個以上之具有Si-H鍵結的單元(MH或DH單元),且聚合度為15至70之範圍的具有直鏈狀骨架之氫聚有機矽氧烷。
相對於前述成分(a)之硬化性官能基,尤其,如乙烯基之不飽和基1個,氫聚有機矽氧烷之調配量較佳係經直接鍵結於矽原子之氫原子為0.7至5.0個之量。若少於0.7個,有時不以充分的速度進行硬化,若超過5.0個,有時硬化物變得太硬,又,亦對硬化後之物性造成不良影響。硬化性官能基為乙烯基時,在分子內具有一個乙烯基之聚有機矽氧烷之量,亦可以該氫聚有機矽氧烷具有之Si-H鍵結與不飽和鍵結,尤其,乙烯基之物質量的比(H/Vi比)進行調整。H/Vi比係以0.7至2.0之範圍為較佳,以0.8至1.5之範圍為更佳。藉由使H/Vi比設為0.7以上,可達成以充分的速度之硬化,又,亦可抑制過剩的滲出。又,藉由使H/Vi比設為2.0以下,可以充分的量達成組成物之硬化,並適度地維持硬度。
在一態樣中,交聯劑(b)之分子量為1000以下,較佳係600以下,更佳係250以下。交聯劑之分子量的下限值可為90以上,亦可為120以上。
成分(b)係只要為具有與成分(a)之反應性官能基對應的交聯基,可僅使用1種,若為可引起同種之反應者,可同時使用2種以上。
交聯劑(b)係在在硬化性組成物中,相對於成分(a)100質量份,例如,可含有0.1質量份以上,具體而言,係可含有0.3質量份以上,可含有30質量份以下,具體而言,可含有20質量份以下,更具體而言,可含有10質量份以下。
從交聯性之觀點而言,成分(b)對成分(a)之合計含量係以0.1質量%以上為較佳,更佳係0.3質量%以上,又,以30質量%以下為較佳,更佳係20質量%以下,特佳係10質量%以下。
在硬化性組成物中,相對於成分(a)之反應性官能基1莫耳,成分(b)係例如,可包含交聯基1莫耳以上,具體而言,可包含2莫耳以上。相對於成分(a)之反應性官能基1莫耳,成分(b)係例如,可包含交聯基30莫耳以下,具體而言,可包含20莫耳以下,更具體而言,可包含10莫耳以下。
相對於成分(a)之反應性官能基1莫耳,成分(b)係例如,可在1至30莫耳之範圍包含交聯基,具體而言,係可包含2至20莫耳之範圍。
‧成分(c)
在本發明之硬化性組成物中的硬化觸媒係可催化前述成分(a)與成分(b)之交聯反應的化合物(以下,有時僅稱為「成分(c)」)。前述成分(a)與成分(b)之交聯反應為縮合反應的情形,可使用已知作為縮合觸媒者,前述成分(a)與成分(b)之交聯反應為加成反應的情形,可使用加成硬化觸媒。
<<縮合觸媒>>
作為成分(c)之縮合觸媒係促進上述成分(a)與成分(b)之水解縮合的成分。縮合觸媒可使用金屬系觸媒、有機酸系觸媒、無機酸系觸媒、鹼系觸媒等。從組成物之硬化速度的觀點而言,縮合觸媒係以金屬系觸媒為較佳。
在上述金屬系觸媒所含有的金屬原子,例如,可列舉鈦、鋯、錫等。尤其,以有機錫化合物或烷氧基鈦類為較佳。金屬系觸媒之一態樣,就配位基而言,可使用烷氧化物,較佳係具有碳原子數1至4,更佳係具有碳原子數1至
3之烷氧化物的化合物。若使用如此之觸媒,容易溶解或分散於硬化性組成物,有助於促進均勻的縮合反應。
較佳的金屬系觸媒係辛酸鐵、辛酸錳、辛酸鋅、萘甲酸錫、辛酸錫、油酸錫之羧酸金屬鹽;二乙酸二丁基錫、二辛酸二丁基錫、二月桂酸二丁基錫、二油酸二丁基錫、二乙酸二苯基錫、氧化二丁基錫、二甲氧化二丁基錫、二丁基雙(三乙氧基矽氧基)錫、二月桂酸二辛基錫、二新癸酸二甲基錫之有機錫化合物;如四乙氧基鈦、四丙氧基鈦、四異丙氧基鈦、四正丁氧基鈦、四異丁氧基鈦、二異丙氧基鈦雙(乙基乙醯基乙酸酯)、1,3-丙烷二氧鈦雙(乙基乙醯基乙酸酯)之有機鈦類;鋁參乙醯丙酮、鋁參乙基乙醯基乙酸酯、二異丙氧基鋁乙基乙醯基乙酸酯、三乙氧基鋁等有機鋁;四乙醯丙酮鋯、四異丙氧基鋯、四丙氧基鋯、四正丁氧基鋯、四異丁氧基鋯、三丁氧基鋯乙醯丙酮、三丁氧基鋯硬脂酸酯等有機鋯化合物。
上述有機酸系觸媒例如,可列舉具有羧酸、磺酸、磷酸之化合物,具體而言,可列舉乙酸、三氟乙酸、甲烷磺酸、甲苯磺酸、烷基磷酸等。又,無機酸系觸媒例如,可列舉鹽酸、硫酸等。
上述鹼系觸媒例如,可例示氨、三乙基胺、二乙基胺等胺化合物,二甲基羥基胺、二乙基羥基胺等二烷基羥基胺,四甲基胍、含有胍基的矽烷或者矽氧烷等胍基化合物。
在本發明之硬化性組成物中,相對於成分(a)100質量份,上述縮合觸媒係以含有0.01至10.0質量份為較佳,以含有0.03至5.0質量份為更佳。
上述縮合觸媒係可僅使用1種,亦可同時使用2種以上。
<<加成硬化型觸媒>>
前述成分(a)及(b)為藉由加成反應產生交聯反應之組合時,可使用加成硬化型之觸媒作為硬化觸媒。代表性的例係可列舉鉑觸媒。鉑觸媒係使前述成分(a)之硬化性官能基與前述成分(b)之氫基反應,用以獲得硬化物之硬化觸媒。該鉑化合物係例示氯化鉑酸、鉑烯烴錯合物、鉑乙烯基矽氧烷錯合物、鉑磷錯合物、鉑醇錯合物、鉑黑等。相對於前述成分(a),就鉑元素而言,其調配量係成為0.1至1000ppm之量。若低於0.1ppm,不會充分硬化,又,即使超過1000ppm,尤其,無法期待硬化速度之提升。又,為了獲得更長的操作時間,依據用途係可藉由添加反應抑制劑,抑制觸媒之活性。就公知之鉑族金屬用的反應抑制劑而言,可列舉2-甲基-3-丁炔-2-醇、1-乙炔-2-環己醇等乙炔醇,馬來酸二烯丙酯。
‧成分(d)
在本發明之硬化性組成物中,包含作為著色劑之顏料(以下,有時僅稱為「成分(d)」)。顏料係只要為與在本發明之硬化性組成物所含有的其他成分不具有反應性,且為有顏色之無機物或有機物,一般處理作為顏料者,可使用公知者。在此,所謂「有顏色」係意指產生至少一部分之可見光線的吸收或散射,亦即,並非透明。顏料係可為源自天然者,亦可為人工所合成或調製者。惟,顏料本身為不發出螢光者。
顏料之具體的例係可列舉碳黑(黑色)、氧化鈦、鋅白、鉛白、硫酸鋇(白色)、鉛丹、氧化鐵(紅色)、黃鉛、鋅黃(黃色)、普魯士藍(藍色)等。此等之顏料係可1種類單獨使用,亦可混合2種類以上而使用。顏料之種類係與施用組成物之基材皆有關連,但較佳係選自碳黑、氧化鈦、氧化鐵及此等之混合物所成的群。
顏料只要為可在組成物中均勻地混合之量即可,含量並無特別限制,亦可依顏料之濃度調節組成物之顏色,尤其亮度。在本發明之硬化性組成物中,相對於成分(a)100質量份,以含有0.01至10質量份為較佳,以含有0.1至5質量份為更佳。
‧成分(e)
在本發明之硬化性組成物係含有UV追蹤劑(以下,有時僅稱為「成分(e)」)。UV追蹤劑係吸收紫外線而產生螢光之化合物。UV追蹤劑係吸收比440nm更短之波長的光,以發出螢光,尤其藍色至紫色之螢光的無色之化合物。UV追蹤劑例如,可使用如2,5-噻吩二基雙(5-第三丁基-1,3-苯并噁唑)之苯并噁唑衍生物、二苯乙烯衍生物、咪唑衍生物、香豆素衍生物、如若丹明之螢光素衍生物等一般所知的化合物。具體的市售品可列舉BASF公司製之TinopaL OB等。
在本發明之硬化性組成物中,相對於成分(a)100質量份,成分(e)之添加量係以含有0.001至1質量份為較佳,以含有0.005至0.1質量份為更佳。相對於成分(a)100質量份,若添加量太少於0.001質量份,照射紫外線時之螢光會不充分,有時難以確認施用狀態。
[硬化性聚有機矽氧烷組成物]
本發明之硬化性聚有機矽氧烷係含有上述成分(a)至(e)。尤其,藉由以硬化方法所產生的分類,可分類成濕氣硬化型與加成硬化型。
(濕氣硬化型之聚有機矽氧烷組成物)
藉由濕氣(水分)進行硬化之類型的聚有機矽氧烷組成物,該組成物係各別具有作為上述成分(a)之聚有機矽氧烷,其係具有產生縮合反應之硬化性官能基;
作為上述成分(b)之具有至少2個與Si原子鍵結之羥基或水解性基的化合物;具有作為上述成分(c)之縮合觸媒。
尤其,可列舉如下之硬化性聚有機矽氧烷組成物為例,該組成物係前述(a)為在一分子中具有2個以上之羥基及/或烷氧基的聚有機矽氧烷,前述(b)為以式R1 aSi(OR2)4-a(其中,R1係分別獨立地為1價之有機基,R2係分別獨立地為氫原子或1價之有機基,a係0、1或2)所表示之矽烷或其水解縮合物,前述(c)為縮合觸媒。
(加成硬化型之聚有機矽氧烷組成物)
藉由對不飽和鍵結之加成反應進行硬化的類型之聚有機矽氧烷組成物,該組成物係分別地:具有作為上述成分(a)之聚有機矽氧烷,其係具有產生加成反應之硬化性官能基;具有作為上述成分(b)之聚有機氫矽氧烷;具有作為上述成分(c)之鉑觸媒。
尤其,可列舉硬化性聚有機矽氧烷組成物為例,該硬化性聚有機矽氧烷組成物係前述(a)為在一分子中具有2個以上之烯基的聚有機矽氧烷,前述(b)為在一分子中具有3個以上之鍵結於矽原子的氫原子之氫聚有機矽氧烷,前述(c)為鉑化合物。
本發明之聚有機矽氧烷組成物係各成分被均勻地混合,且只要具有可施用於基材的程度之流動性,其性狀並無特別之限制。從操作性之觀點而言,聚有機矽氧烷組成物之黏度較佳係主要可藉由成分(a)之黏度進行調控,且為0.1至100Pa‧s之範圍。又,聚有機矽氧烷組成物較佳係各成分全部被混合之狀態的一液型之組成物。在一液型之組成物中,為了防止在保存狀態之硬化,可以乾燥狀態進行保存或添加反應抑制劑,其方法係發明所屬技術領域者為公知。
本發明之硬化性聚有機矽氧烷組成物係只要無損其目的/硬化者,可調配公知之其他成分。就添加劑而言,可適當調配阻燃劑、填充材、接著賦予劑、耐熱賦予劑、稀釋劑、有機溶劑等。又,亦可調配不相當於前述成分(a)之矽氧烷樹脂。就如此之樹脂而言,可列舉僅具有1個之硬化性官能基的聚有機矽氧烷、不具有如二甲基矽氧烷之硬化性官能基的聚有機矽氧烷等。此等樹脂之中,不具有反應性之樹脂係可使用來作為稀釋劑。
<填充劑>
硬化性聚有機矽氧烷組成物係可更含有填充劑。填充劑可例示煙霧質二氧化矽、燒成二氧化矽、二氧化矽氣凝膠、沈澱二氧化矽、矽藻土、粉碎二氧化矽、熔融二氧化矽、石英粉末、煙霧質氧化鈦、氧化鐵、氧化鋅、氧化鈦、氧化鋁等氧化物;使此等之表面以三甲基氯矽烷、二甲基二氯矽烷、六甲基二矽氮烷、八甲基環四矽氧烷等疏水化劑經處理者;碳酸鈣、碳酸鎂、碳酸鋅等碳酸鹽;鋁矽酸、矽酸鈣等矽酸鹽;滑石;玻璃棉、雲母微粉末等複合氧化物;碳黑、銅粉、鎳粉等導電性填充劑;聚甲基倍半矽氧烷、聚苯乙烯、聚氯乙烯、聚丙烯等合成樹脂粉末;石綿、玻璃纖維、有機纖維等纖維質填充劑。此等填充劑係依照塗佈作業性、及硬化所得到之橡膠狀彈性體所需要的物性而選擇。
填充劑為粒狀之填充劑時,從分散性、硬化性組成物之流動性及硬化物高的機械性強度之觀點而言,其平均粒徑係以100μm以下為較佳,更佳係50μm,尤佳係10μm以下。平均粒徑之測定值係藉由雷射繞射/散射法所測定之中值徑(d50)。
在硬化性聚有機矽氧烷組成物中,相對於成分(a)100質量份,填充劑係例如,可包含200質量份以下,具體而言,可包含1至100質量份,更具體而言,可包含1至50質量份。
<接著賦予劑>
硬化性聚有機矽氧烷組成物係可更包含接著賦予劑。接著賦予劑係提升組成物的硬化物對玻璃、金屬、塑膠等基材之密著性的成分。亦可使用具有在前述之交聯劑中的可水解的基以外之官能基的化合物作為接著賦予劑。具體而言,可列舉含有胺基的矽烷、三聚異氰酸酯、碳雜氮矽三環化合物。更具體的例可列舉乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷、3-環氧丙氧基丙基三甲氧基矽烷、3-環氧丙氧基丙基三乙氧基矽烷、3-環氧丙氧基丙基甲基二甲氧基矽烷、3,4-環氧基環己基乙基三甲氧基矽烷、3-丙烯醯氧基丙基三甲氧基矽烷、3-甲基丙烯醯氧基丙基三甲氧基矽烷、3-丙烯醯氧基丙基甲基二甲氧基矽烷、3-甲基丙烯醯氧基丙基甲基二甲氧基矽烷、3-甲基丙烯醯氧基丙基甲基二乙氧基矽烷等。
在硬化性聚有機矽氧烷組成物中,相對於成分(a)100質量份,接著賦予劑係例如,可包含10質量份以下,具體而言,可包含0.01至10質量份,更具體而言,可包含0.1至5質量份。
<其他之樹脂>
硬化性聚有機矽氧烷組成物係可更包含不相當於前述成分(a)及(b)之矽氧烷樹脂。如此之樹脂亦可使用用以調整黏度之稀釋劑。如此之矽氧烷樹脂係可使用以下述式(4)所示之不具有硬化性官能基的矽氧烷。
(Ra)3-pRpSi-O-(SiR2O)n-SiR3‧‧‧(4)(式中,Ra、R、p、n係如在式(1)所定義)
所示之僅具有1個硬化性官能基的矽氧烷、或以式(5):
R3Si-O-(SiR2O)n-SiR3‧‧‧(5)(式中,R、n係如在式(1)所定義)可藉由使用如此的矽氧烷樹脂,調控硬化性聚有機矽氧烷組成物硬化時之硬度,或調控組成物之黏度,可對於操作性或所要求之物性廣泛地對應。
在硬化性聚有機矽氧烷組成物中,相對於成分(a)100質量份,如此的樹脂係例如,可包含50質量份以下,具體而言,可包含0.1至50質量份,更具體而言,可包含1至30質量份。
<溶劑>
硬化性聚有機矽氧烷組成物係可包含溶劑。此時,硬化性聚有機矽氧烷組成物係可依照其用途、目的而在適當的溶劑中溶解成所希望之濃度而使用。相對於硬化性聚有機矽氧烷組成物100質量份,上述溶劑之濃度係例如,可為80質量份以下,亦可為50質量份以下,亦可為30質量份以下,亦可為20質量份以下。從調整硬化性組成物之黏度的觀點而言,以包含溶劑為較佳。藉由包含溶劑,硬化性組成物之操作性可變得良好。又,由硬化性組成物所形成之硬化物的形狀之控制變得容易,例如,可容易形成厚度大的硬化物。
本發明之硬化性聚有機矽氧烷組成物因具有顏料,故為有顏色。顏料之種類如前述,並無特別限制,但可設計成包含與被施用之基材為同系顏色之顏料。尤其,在組成物中包含與施用組成物之基材的色差(△E)小之顏料。
所謂「色差」係使2個顏色之差異定量化為在顏色空間之距離者,藉由L*a*b*表色系中之顏色座標的距離來求得。在L*a*b*表色系中之組成物與
基材的色差(△E)係使基材之L*a*b*表色系之各值設為L*(b)、a*(b)、b*(b),使組成物之L*a*b*表色系之各值設為L*(c)、a*(c)、b*(c)值時,可藉由下式而求得。
△E={(L*(b)-L*(c))2+(a*(b)-a*(c))2+(b*(b)-b*(c))2}1/2其中,L*係使該顏色之亮度(0至100)設為參數化,a*係使該顏色之紅色-綠色間的位置(-128至+128)設為參數化,b*係使該顏色之黃色-藍色間的位置(-128至+128)設為參數化。
色差之定量方法係發明所屬技術領域者為公知,可使用一般可取得的分光色差計、測色色差計進行定量。
硬化性聚有機矽氧烷組成物與基材之色差(△E)係可大於20,但為了更顯著地表現本發明之效果,以20以下為較佳。硬化性聚有機矽氧烷組成物及基材之兩者皆使用相同的顏料,顏料以外之成分為無色透明,且若在顏料之濃度無較大的差,色差係可推定為20以下。或者,即使基材與組成物使用相異之顏料,亦可使兩者接觸並排時,若為無法以目視判斷兩者之境界或困難之狀態,色差係可推定為20以下。
[基材]
施用本發明之硬化性聚有機矽氧烷組成物的基材係在其材質並無特別限制。基材係可使用鋁、銅、鎳、鐵、黃銅、不銹鋼等金屬;環氧基樹脂、聚對苯二甲酸乙二酯、聚對苯二甲酸丁二酯(PBT)樹脂等聚酯樹脂、聚碳酸酯樹脂、丙烯酸樹脂、聚醯亞胺樹脂、酚樹脂、聚醯胺樹脂、聚苯硫醚(PPS)樹脂、改性聚苯醚(PPE)樹脂等工程塑膠;玻璃等。又,依需要,可對於空隙之壁面等依據常用方法而施予底漆處理。惟,為了與硬化性聚有機矽氧烷組成物為同系顏色之基材,較佳係容易混合顏料之塑膠材料。
在基材施用硬化性聚有機矽氧烷組成物之方法係可使用發明所屬技術領域者為公知之方法的浸漬法、刷毛塗佈法、噴塗法、點膠法等。又,組成物之施用厚度通常為0.01至3mm,較佳為0.05至2mm。
本發明之一態樣係有關一種確認硬化性聚有機矽氧烷組成物對基材的施用狀態之方法,該方法係包含:
(A)提供前述硬化性聚有機矽氧烷組成物之步驟;
(B)提供與該組成物之色差(△E)為20以下之基材的步驟;
(C)使該組成物施用於該基材之步驟;及
(D)對施用於該基材之該組成物照射紫外線之步驟。
藉由照射紫外線之步驟(D),可藉由目視更簡便地確認組成物之施用狀態。照射紫外線之步驟係由對組成物表面藉由紫外線照射裝置照射波長280至440nm,較佳係300至420nm,特別佳係340至400nm之紫外線所構成。一般可利用紫外線照射裝置,亦可使用市售之黑光燈。可藉由照射紫外線,依據觀察來自組成物表面之螢光,以目視確認對基材之施用狀態。
有關本發明之方法係至少包含上述步驟(A)至(D)之方法,但在步驟(C)或(D)之後,可包含使組成物硬化之步驟。使組成物硬化之方法係採用依據組成物中之成分(a)及(b)而異的方法。例如,具有成分(a)為可水解的基作為硬化性官能基時,組成物係可藉由空氣中之水分而硬化。此時,典型地係可藉由在室溫(23℃)、相對濕度50%之環境下放置1小時至72小時,空氣中之水分會進行水解反應,並使組成物硬化。成分(a)係具有含有不飽和鍵結之基作為硬化性官能基時,組成物係可藉由加熱至室溫乃至150℃而硬化。
利用本發明之方法而確認出施用狀態之構件係有效地利用於電性電子零件。尤其,就以顏料所進行之著色為常態之部分的零件而言,在要求遮光性、隱蔽性之零件中為有效,本發明之方法係對其等之製造為有利。
[實施例]
經由以下之實施例更具體地說明本發明之組成物及方法,但本發明係不受此等實施例之態樣所限定。
[實施例1]黑色之聚有機矽氧烷組成物
使用行星式混合機混合作為基質聚合物(成分(a))之甲基二甲氧基末端聚二甲基矽氧烷(黏度20Pas)100質量份、作為交聯劑(成分(b))之甲基三甲氧基矽烷1.1質量份、作為兼具接著賦予劑之交聯劑的3-胺基丙基三甲氧基矽烷0.44質量份及參[3-(三甲氧基矽基)丙基]三聚異氰酸酯0.66質量份、作為觸媒(成分(c))之二月桂酸二丁基錫0.38質量份、作為顏料(成分(d))之碳黑0.5質量份、作為UV追蹤劑(成分(e))之2,5-噻吩二基雙(5-第三丁基-1,3-苯并噁唑)0.013質量份、再者作為填充材之煙霧質二氧化矽14質量份及作為稀釋劑之二甲基矽氧烷(黏度0.1Pas)18質量份,獲得均勻的組成物之黑色的聚有機矽氧烷組成物。
[比較例1]黑色之聚有機矽氧烷組成物
除了未加入作為UV追蹤劑之2,5-噻吩二基雙(5-第三丁基-1,3-苯并噁唑)以外,其餘係與實施例1為相同方式,獲得黑色之聚有機矽氧烷組成物。
[實施例2]白色之聚有機矽氧烷組成物
除了將顏料從碳黑變更為二氧化鈦1.0質量份以外,其餘係與實施例1為相同方式,獲得白色之聚有機矽氧烷組成物。
[比較例2]白色之聚有機矽氧烷組成物
除了未加入作為UV追蹤劑之2,5-噻吩二基雙(5-第三丁基-1,3-苯并噁唑)以外,其餘係與實施例2為相同方式,獲得白色之聚有機矽氧烷組成物。將實施例1、2及比較例1、2中之組成物的組成彙整於表1中。
[實施例3、比較例3]
與實施例1相同地混合下述表2所示之調配的組成物,作為藉由加成反應進行硬化之類型的組成物,獲得作為均勻的組成物之灰色聚有機矽氧烷組成物。比較例3係除了未加入作為UV追蹤劑之2,5-噻吩二基雙(5-第三丁基-1,3-苯并噁唑)以外,其餘係與實施例3為相同的調配。
[施用狀態確認試驗]
準備聚苯硫醚(PPS)樹脂(Polyplastic公司製、黑色)、聚對苯二甲酸丁二酯(PBT)樹脂(Polyplastic公司製、白色)、改性聚苯醚(PPE)樹脂(SABIC公司製、灰色)作為施用各實施例及比較例之組成物的基材。使用Konica Minolta公司製色彩色差計CR-400所測定之各基材的色座標表示於以下之表3中。
分別在聚苯硫醚(PPS)樹脂(黑色)之基材上,使用不銹鋼之抹刀將實施例1及比較例1獲得之組成物施用成為10mm×25mm之長方形。將經施用之組成物在23℃、相對濕度50%之環境下放置3日,以使組成物硬化。在此,使用與基材為相同顏色彩色差計而測定組成物之色座標,算出與基材之色差。實施例及比較例1至3之組成物之色座標及與施用基材的色差係彙整於表4中。然後,對於基材照射室內照明(螢光燈)及UV光(波長375nm)。此時,以容易或困難評價是否可以目視判斷硬化物與基材之境界。
對於在實施例2及比較例2獲得之組成物分別施用於聚對苯二甲酸丁二酯(PBT)樹脂(白色)之基材上,進行與有關實施例1為相同之試驗。
對於在實施例3及比較例3獲得之組成物分別施用於改性聚苯醚(PPE)樹脂(灰色)之基材上,在100℃、烘箱中使其硬化1小時,進行與有關實施例1為相同樣之試驗。將各別之結果彙整於表4中。
從表2明顯可知,本發明之組成物係即使施用於同系顏色之基材時,亦可藉由紫外光確認出容易被施用之處與施用狀態。
[產業上之利用可能性]
本發明之組成物係可利用來作為容易確認對同系顏色基材的施用狀態之電性電子零件之封裝材、塗覆劑。又,本發明之方法係可組入於使用如此之封裝材或塗覆劑的電性電子零件之製造方法,並不僅可簡便地利用,亦可使用於可靠性高的零件之製造。尤其,可使用在被要求遮光性、隱蔽性的零件中。
Claims (7)
- 一種硬化性聚有機矽氧烷組成物,係包含:(a)聚有機矽氧烷,係在一分子中具有2個以上之硬化性官能基;(b)交聯劑,係在一分子中具有2個以上與前述(a)之硬化性官能基具有反應性之交聯基;(c)硬化觸媒,係可催化前述(a)及(b)之交聯反應;(d)顏料,係其本身不發出螢光;及(e)UV追蹤劑。
- 如請求項1所述之硬化性聚有機矽氧烷組成物,其中,前述(a)為在一分子中具有2個以上之羥基及/或水解性基的聚有機矽氧烷,前述(b)為在一分子中具有2個以上之羥基及/或水解性基的矽化合物或其水解縮合物,前述(c)為縮合觸媒。
- 如請求項1所述之硬化性聚有機矽氧烷組成物,其中,前述(a)為在一分子中具有2個以上之烯基的聚有機矽氧烷,前述(b)為在一分子中具有3個以上之鍵結於矽原子的氫原子之氫聚有機矽氧烷,前述(c)為鉑化合物。
- 如請求項1至3中任一項所述的硬化性聚有機矽氧烷組成物,係一液型之組成物。
- 如請求項1至4中任一項所述的硬化性聚有機矽氧烷組成物,其中,(d)顏料為選自由碳黑、氧化鈦、氧化鐵及此等之混合物所組成之群組中。
- 如請求項1至5中任一項所述的硬化性聚有機矽氧烷組成物,係與該硬化性聚有機矽氧烷組成物之色差(△E)為20以下之基材的接著用者。
- 一種確認硬化性聚有機矽氧烷組成物對基材的施用狀態之方法,係包含:提供如請求項1至6中任一項所述的硬化性聚有機矽氧烷組成物之步驟;提供與該硬化性聚有機矽氧烷組成物之色差(△E)為20以下之基材的步驟;將該硬化性聚有機矽氧烷組成物施用於該基材之步驟;及對施用於該基材之該硬化性聚有機矽氧烷組成物照射紫外線之步驟。
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