TWI549829B - 用於光伏陣列之抗反射膜 - Google Patents
用於光伏陣列之抗反射膜 Download PDFInfo
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- TWI549829B TWI549829B TW103110061A TW103110061A TWI549829B TW I549829 B TWI549829 B TW I549829B TW 103110061 A TW103110061 A TW 103110061A TW 103110061 A TW103110061 A TW 103110061A TW I549829 B TWI549829 B TW I549829B
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Classifications
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- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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- C—CHEMISTRY; METALLURGY
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- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
- G02B1/111—Anti-reflection coatings using layers comprising organic materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0216—Coatings
- H01L31/02161—Coatings for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/02167—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells
- H01L31/02168—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells the coatings being antireflective or having enhancing optical properties for the solar cells
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/10—Homopolymers or copolymers of propene
- C08J2423/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2433/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2433/08—Homopolymers or copolymers of acrylic acid esters
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Description
本發明係有關一種抗反射膜，尤其有用於製作光伏模組。
有多種方法用以最小化白光伏陣列浪費之可見光反射，包括應用低介電常數層於陣列表面。舉例而言，美國專利U.S.Pat.No.7,604,866揭示包括二氧化矽粒子之膜以達減少可見光反射之目的。然而，上述及其他方法均不能最小化位於膜-玻璃介面處之表面反射。
鑑於上述問題，本發明係提供一種抗反射膜，其尤其有用於製作光伏模組。
本發明之膜包括具有(a)0.75至15微米之平均粒子直徑以及(b)從粒子之中心至表面連續變化之折射率之聚合物粒子；以及包括聚烯烴之連續聚合相，其中，於400至800奈米測量之該等聚合物粒子與該連續聚合相間之平均折射率差係不大於0.02。
除另行具體限定外，百分比為重量百分比(wt%)，以及溫度為攝氏溫標(℃)。除另行具體限定外，折射率(RI)值於其中波長為589.29奈米之鈉P線，於20℃測定。聚合物粒子包括有機聚合物，較佳為加成聚合物，且較佳係實質為球形。平均粒子直徑D50係定義為以粒子大小分析儀器所測定之粒子大小分布之中位數值，分析儀器較佳為庫爾特計數器(Coulter counter)。玻璃轉相溫度(Tg)值係使用福斯公式(Fox equation)自均聚物之Tg值計算而得；參見美國物理學會公告(Bulletin of the American Physiced Society)1，3，123頁(1956)。一種在整個粒子中其組成有變化之聚合物粒子之Tg為該粒子中不同組成之Tg值之重量平均。多階段聚合物之單體重量百分比乃針對各階段加以計算，係基於加入該階段之聚合混合物中之單體總重量計。以下用語“(甲基)丙烯酸系”係指丙烯酸系或甲基丙烯酸系，而用語“(甲基)丙烯酸酯”係指丙烯酸酯甲基丙烯酸酯。用語“(甲基)丙烯醯胺”係指丙烯醯胺(AM)或甲基丙烯醯胺(MAM)。“丙烯酸系單體”包括丙烯酸(AA)、甲基丙烯酸(MAA)、AA及MAA之酯類、衣康酸(IA)、巴豆酸(CA)、丙烯醯胺(AM)、甲基丙烯醯胺(MAM)以及AM及MAA之衍生物，如：烷基(甲基)丙烯醯胺。AA及MAA之酯類包括，但不限於，烷基酯(alkyl)、羥基烷基酯、磷烷基(phosphoalkyl)酯及磺基烷基(sulfoalkyl)酯，例如：甲
基丙烯酸甲酯(MMA)、甲基丙烯酸乙酯(EMA)、甲基丙烯酸丁酯(BMA)、甲基丙烯酸羥乙酯(HEMA)、丙烯酸羥乙酯(HEA)、甲基丙烯酸羥丙酯(HPMA)、丙烯酸羥丁酯(HBA)、丙烯酸甲酯(MA)、丙烯酸乙酯(EA)、丙烯酸丁酯(BA)、丙烯酸2-乙基己酯(EHA)、甲基丙烯酸環己酯(CHMA)、丙烯酸苄酯(BzA)以及甲基丙烯酸磷烷基酯(phosphoalkyl methacrylate)(如：PEM)。“苯乙烯系單體”包括苯乙烯、α-甲基苯乙烯或2-、3-或4-烷基苯乙烯，包括甲基-及乙基-苯乙烯；較佳係苯乙烯。
用語“乙烯基單體”(vinyl monomers)係指單體中包括連接雜原子如氮或氧之碳-碳雙鍵。例示之乙烯基單體包括，但不限於，乙酸乙烯酯、乙烯基甲醯胺、乙烯基乙醯胺、乙烯基吡咯烷酮，乙烯基己內醯胺，長鏈鏈烷酸乙烯酯，新癸酸乙烯酯及硬脂酸乙烯酯。用語“聚烯烴”係指烯烴之聚合物或共聚物，較佳具有2至10碳原子、2至8個碳原子、2至4個碳原子之烯烴，較佳為丙烯或乙烯。較佳地，該連續聚合相包括至少75wt%、85wt%，較佳至少95wt%，較佳至少98wt%的聚烯烴。較佳地，聚烯烴包括烯烴共聚物，特別是乙烯與他種烯烴(優選具有3至8個碳原子之烯烴)之共聚物；較佳他種烯烴總量為0至90wt%、2至50wt%或3至40wt%。較佳地，聚烯烴之平均分子量係50,000至500,000，較佳70,000至300,000。較佳地，聚烯烴之玻璃轉相溫度(Tg)小於25℃，較佳小於10℃。較佳地，聚烯烴之熔點不高於200℃，較佳不高於190℃，
較佳不高於180℃；較佳聚烯烴之熔點係至少100℃。
較佳地，該聚合物粒子具有至少1微米之平均粒子直徑，較佳至少1.5μm，較佳至少2μm，較佳至少2.5μm，較佳至少3，較佳至少3.5微米；較佳地，該等聚合物粒子之平均粒子直徑不大於12微米，較佳不大於10μm，較佳不大於8μm，較佳不大於6μm，較佳不大於5.5微米。較佳地，該等聚合物粒子具有顯示為單模之粒子大小分布；較佳該粒子大小分布之半高寬為0.1至3微米，較佳0.2至1.5微米。所述膜可包括具有不同平均直徑之粒子，限制條件為具各平均直徑之粒子具有如上所述之粒子大小分布。粒子大小分布係以粒子大小分析儀器測定。
以下所述之折射率差對係絕對值。較佳地，於800nm至2500nm測量之該聚合物粒子與該連續聚合相間之折射率差(即差之絕對值)係至少0.04，較佳至少0.06、較佳至少0.08、較佳至少0.1。較佳地，於800nm至2500nm測量之該聚合物粒子與該連續聚合相間之折射率差(即差之絕對值)係不大於0.2，較佳不大於0.17，較佳不大於0.15。較佳地，於400nm至800nm測量之該聚合物粒子與該連續聚合相間之折射率差係不大於0.015，較佳不大於0.01，較佳不大於0.005，較佳不大於0.003。較佳地，該聚合物粒子之折射率係1.43至1.55，較佳1.45至1.53，較佳1.46至1.52，較佳1.47至1.51。較佳地，該連續聚合相之折射率係1.4至1.6，較佳1.45至1.55較佳1.47至1.53，較佳1.48至1.52。較佳地，在紅外光區(即800至2500
奈米)之該聚合物粒子之折射率係大於該連續聚合相之折射率。用以計算折射率差之GRIN粒子之折射率係於粒子表面處之折射率。
所述膜中之該聚合物粒子係一種具有徑向折射率梯度之粒子(“GRIN”粒子，參見如美國專利申請案US 20090097123)。較佳地，GRIN粒子具有中心高於表面之折射率。較佳地，GRIN粒子之中心折射率係1.51至1.63，較佳1.52至1.60，較佳1.53至1.59，較佳1.54至1.59；以及表面折射率係1.45至1.43，較佳1.46至1.52，較佳1.47至1.51。於另一較佳具體實施例中，GRIN粒子具有中心低於表面之折射率。GRIN粒子可具有核心，該核心係衍生自用以產生GRIN粒子之聚合物種子。較佳地，GRIN粒子之核心係不大於粒子之95wt%，較佳不大於80wt%，較佳不大於60wt%、40wt%或20wt%。
較佳地，該連續聚合相包括0.5至15wt%之該聚合物粒子，基於整個膜之重量計；較佳至少1wt%較佳至少1.5wt%、較佳至少2wt%、較佳至少3wt%、較佳至少5wt%；較佳不大於12wt%，較佳不大於10wt%，較佳不大於9wt%。該連續聚合相係連續，就意義而言存有連接聚合物中所有部位之不間斷路徑。
較佳地，該聚合物粒子包括至少60%丙烯酸系單體之聚合殘基，較佳至少65%，至少70%，至少75%，至少80%。較佳地，該聚合物粒子包括至少70%丙烯酸系以及苯乙烯系單體之聚合殘，較佳至少90%，至少95%，
至少97%。較佳地，該聚合物粒子亦包括0至5%酸單體之聚合殘基(如：AA、MAA、IA或CA)，較佳0.5至4% AA及/或MAA，且亦可包括小量乙烯基單體之聚合殘基。
交聯劑係具有兩個或更多個乙烯系不飽和基之單體、偶合劑(如：矽烷)或離子交聯劑(如：金屬氧化物)。具有兩個或更多個乙烯系不飽和基之單體之交聯劑可包括如二乙烯基芳香化合物、二-，三-及四-(甲基)丙烯酸酯、二-，三-及四-烯丙基醚或酯化合物以及(甲基)丙烯酸烯丙酯。上述單體之較佳實施例包括二乙烯基苯(DVB)、三羥甲基丙烷二烯丙基醚、四烯丙基季戊四醇、三烯丙基季戊四醇、二烯丙基季戊四醇、苯二甲酸二烯丙酯、馬來酸二烯丙酯、氰尿酸三烯丙酯、雙酚A二烯丙基醚、烯丙基蔗糖、亞甲基雙丙烯醯胺、三羥甲基丙烷三丙烯酸酯、甲基丙烯酸烯丙基酯(ALMA)、乙二醇二甲基丙烯酸酯(EGDMA)、己烷-1,6-二醇二丙烯酸酯(HDDA)以及丁二醇二甲基丙烯酸酯。較佳地，經聚合之交聯劑殘基之量在該聚合物粒子中不超過8%，較佳不超過6%較佳不超過5%；較佳地，至少0.1%，較佳至少0.5%，較佳至少1%，較佳至少2%。較佳地，若交聯劑存在，其具有分子量100至250，較佳110至230，較佳110至200，較佳115至160。較佳地，交聯劑係雙官能或三官能，亦即，它們分別是二乙烯系或三乙烯系不飽合，優選雙官能。
較佳地，所述膜包括複數本發明之聚合物粒子，其係藉由擠壓聚烯烴以及聚合物粒子之混合物所形
成。較佳地，適用所述膜之基板係玻璃、木材、皮革或諸如聚對苯二甲酸乙二酯之透光塑料；較佳係玻璃或透光塑料，較佳玻璃。較佳地，用於本案之塑料及玻璃之折射率由聚偏二氟乙烯之最小值1.4變化至掺雜有氧化鉈(Tl2O)之玻璃之1.8。所述膜樣本亦可塗布有黏著層以供多層結構中之膜對膜積層及改善其與基板之接觸。
可使用具廣泛多種官能及分子量之水系或溶劑系之丙烯酸系聚合物及樹脂來黏著多層。較佳地，黏著劑係自水或溶劑中之膠體聚合物分散體製備而得，以產生高固體含量(30至50% w/w)之溶液或懸浮液。較佳地，於使用黏著劑前，基板藉由曝露於放電電場處理以達降低表面能及提升黏著之目的。較佳地，塗布有黏著劑之基板係以範圍自80至170℃之梯度溫度，在烘箱中乾燥10至15分鐘。
較佳地，該黏著劑組成物係由低玻璃轉相溫度之丙烯酸系聚合物(較佳Tg低於25℃)以及呈輕度交聯形態之球體型式之丙烯酸系聚合物之混合物所製備，該球體之直徑範圍自最小值0.85微米至最大值30微米。較佳地，該球體之丙烯酸系聚合物已交聯；較佳地，已聚合之交聯劑殘基之總量係介於4至20%。較佳地，第一聚合階段包括一或多種下列單體：乙二醇二丙烯酸酯、丙二醇二丙烯酸酯、以及四亞甲基二醇二丙烯酸酯。較佳地，第二階段包括4至20%之一或多種下列交聯劑部分(moiety)：二乙二醇雙(碳酸烯丙酯)、甲基丙烯酸烯丙酯、乙二醇二
甲基丙烯酸酯、丙二醇二甲基丙烯酸酯以及四亞甲基二醇二甲基丙烯酸酯。
該黏著劑組成物經設計為待施加於粗糙或平滑表面，該表面係廣佈大的突出物，該等大突出物限制該表面形貌之完全覆蓋。該黏著劑之溶劑型溶液或水分散液得以不同方式施加於基板上。較佳地，若該基板為硬質且廣佈表面不規則物(呈高深寬比粒子之形態)，該黏著劑係以凹印塗佈機塗布於該表面。或者，該黏著劑珠組成物可調配各種黏結劑(binder)，以產生水性或溶劑型塗布組成物，其可施加(例如：以噴霧或輥塗、噴墨或印刷)於適當之基板。該等分散之粒子之最有效益之幾何配置係其中粒子呈面心立方或六方緊密堆積配置於基板上之單層球體。
當黏著劑珠組成物以水分散液之形態而加以施加時，較佳的黏結劑包括諸如氨基矽烷、環氧樹脂、環氧矽烷、烷基矽烷、脂肪酸或矽油之塗布劑。較佳氨基矽烷係氨乙基氨丙基三甲氧基矽烷以及丙烯酸纖維素溶液。其他適用水性黏結劑包括選自丙烯酸系、諸如乙酸乙烯酯或乙酸乙烯酯-乙烯之乙烯、聚氨酯、矽氧烷、天然橡膠、諸如苯乙烯-丁二烯嵌段共聚物(SBR)之合成橡膠聚合物、蛋白質聚合物、纖維素類聚合物及其混合物或其組合(如：丙烯酸系聚氨酯之(共)聚物)。
當該珠組成物係溶劑安定性，該黏著劑組成物可藉溶劑澆鑄施加。使用於溶劑澆鑄之溶劑包括甲基乙基酮、甲基異丁基酮、乙酸乙酯、乙酸丁酯、甲苯、異
丙醇、乙醇、以及二甲苯及甲苯。
該黏著劑組成物亦可包括下列者之任一或全部：防腐劑、抗氧化劑、氫化木松香縮水甘油酯、玉米或馬鈴薯澱粉、乙二醇、1,3-丙二醇、1,4丁二醇、戊二醇、己二醇、1,2丙二醇、甘油、2,3-丁二醇、1,3-丁二醇、二乙二醇甘油酯、三甘醇、聚乙二醇、乙烯脲、尿素、山梨醇以及甘露糖醇。諸如松香及萜烯酚(terpene phenol)之增黏樹脂亦可加入上述混合組成物中。
或者，該黏著劑可為基於阿爾法聚烯烴以及乙烯之共聚物。較佳為以氫化烴增黏劑增黏之調配物。該黏著劑調配物可為矽烷以改善對玻璃基板之附著性。在一些具體實施例中，所述膜可於多結構中使得可撕掉一層而露出新表面。在此具體實施例中，較佳每層之厚度小於100微米，較佳小於50微米；以及總層數大於2，較佳大於3，較佳大於5，較佳大於7。在多層構形之具體實施例中，較佳為於該等膜間有該黏著劑層。較佳於400至800奈米測量之該膜與黏著劑之平均折射率差不大於0.02，較佳不大於0.01較佳不大於0.005。該黏著層之乾厚度較佳係小於50微米，較佳小於20微米。
較佳地，所述膜之總厚度，不論是否為多層所組成，係10微米至2毫米，較佳15微米至2毫米，較佳20微米至1.5毫米。
較佳地，該等聚合物粒子以習知之乳化聚合技術製備在水性介質中，接著噴霧乾燥所得之聚合物乳
膠。噴霧乾燥法典型地產生具有1至15微米平均直徑之聚合物粒子團塊。較佳地，此等團塊係無需減縮尺寸而直接分散於包括聚烯烴之聚合物中，以於擠壓機中藉由融溶混練過程產生所述膜，較佳擠壓溫度係190至250℃，較佳195至240℃，較佳200至230℃。
所述GRIN粒子通過噴霧乾燥法而與水性介質分離。
比較例1
藉由融熔擠壓製程從純聚合物樹脂顆粒製備片。該聚丙烯樹脂(Huntsman Reyen，折射率RI=1.8，玻璃轉相溫度Tg=-10℃，熔點Tm=173℃)於Leistritz擠壓機中以200至250℃範圍之料桶溫度融熔加工。融熔混練後進行製成顆粒、於真空烘箱中以60℃乾燥及於221至236℃間之溫度注模成型。此等衍生自注模成型之測試板係具下列尺寸：66.9毫米(mm)×66.9毫米×1.5毫米。此等片依據美國材料及試驗協會ASTM D10003-00(透光塑料之霧度和透光率標準測試法)及ASTM E313-00(從儀器量測色度坐標計算黃度及白度指數之標準測試法)測試法予以評估。數據如下表I所示。
實施例2至4
藉由融熔擠壓製程從GRIN粒子及聚合物樹脂之混合物製備片。將自下述聚合製製備且具鄰((丙烯酸苄酯/ALMA=76/4)//MMA/EA=16/4))組成之GRIN粒子(折射率
RI=1.56至1.49以及等於0.75微米之粒子大小直徑)與聚丙烯樹脂(Huntsman Reyen，折射率RI=1.49)乾混合，然後於Leistritz擠壓機中以200至225℃範圍料桶溫度融熔混練。該融熔混練使用80/120/300/120/80網孔之特殊濾網組合配置以產生該等GRIN粒子之終極分散體。融熔混練後進行製成顆料；於真空烘箱中以60℃乾燥及於221至236℃間之溫度注模成型。此等衍生自注模成型之測試板係具下列尺寸：66.9毫米×66.9毫米×1.5毫米。此等片依據美國材料及試驗協會ASTM D10003-00(透光塑料之霧度和透光率標準測試法)及ASTM E313-00(從儀器量測色度坐標計算黃度及白度指數之標準測試法)測試法予以評估。數據如下表I所示。
實施例5至7
藉由融熔擠壓製程從GRIN粒子與聚合物樹脂之混合物製成片。將自下述聚合製程製備且具鄰((丙烯酸苄酯/ALMA=76/4)//(苯乙烯=20))組成之GRIN粒子(折射率RI=1.56至1.59以及等於0.80微米之粒子大小直徑)與聚丙烯樹脂(Huntsman Reyen，折射率RI=1.49)乾混合，然後於Leistritz擠壓機中以200至225℃範圍料桶溫度融熔混練。該融熔混練使用80/120/300/120/80網孔之特殊濾網組合配置以產生該等GRIN粒子之終極分散體。融熔混練後進行製成顆粒、於真空烘箱中以60℃乾燥及於221至236℃間之溫度注模成型。此等衍生自注模成型之測試板係具下列尺寸：66.9毫米×66.9毫米×1.5毫米。此等片依據美國材料
及試驗協會ASTM D10003-00(透光塑料之霧度和透光率標準測試法)及ASTM E313-00(儀器量測色度坐標計算黃度及白度指數之標準測試法)測試法予以評估。測試數據如下表II所示。
實施例8(預-種子聚合物)
本實施例例示具0.25微米直徑之經交聯聚合物預-種子之製備，該預-種子係適於製造大種子粒子之水中分散體。下列A至C混合物係以去離子水製備：
混合物A1注入設有攪拌器和冷凝器且覆蓋氮氣之反應器，並加熱至83℃。加入10%乳化之混合物B1以及25%混合物C1於該反應器中。持溫於83℃並攪拌60分鐘後，以120分鐘將剩餘混合物B1以及混合物C1加入該反應器並伴隨攪拌。於83℃持續攪拌90分鐘後，將該
反應器之內容物冷卻至室溫。以布魯克海文儀器(Brookhaven Instrument)粒子大小分析儀器BI-90測量所得粒子預-種子之粒子大小為0.25微米。
實施例9(聚合物種子)
在本實施例中，使用丙烯酸正丁酯、苯乙烯及1-己硫醇使實施例8乳膠中之預-種子粒子成長至0.56微米。下列A2至G2混合物係以去離子水製備：
混合物A2加入實施例8之反應器中，攪拌並加熱至88℃。以氮氣替代該反應器中之空氣。當該反應器溫度穩定於88℃，混合物B2注入該反應器。乳化之混合物C2及D2以及混合物E2接著伴隨攪拌以300分鐘加入該反應器中於88℃持續攪拌90分鐘。將該反應器之內容物冷卻至65℃。加入混合物F2及G2且該反應器之內容物持溫於65℃並攪拌1小時後，將該反應器之內容物冷卻至室溫。以Brookhaven Instrument粒子大小分析儀器BI-90測量所得乳膠粒子之粒子直徑為0.56微米。
實施例10(GRIN球體組成)
在本實施例中將實施例9乳膠之粒子擴大而產生5微米直徑之發散透鏡，係於第I階段使用丙烯酸正丁酯以及甲基丙烯酸烯丙酯，之後於第II階段與甲基丙烯酸甲酯以及丙烯酸乙酯共聚合。下列A3至G3混合物係以去離子水製備：
實施例8之反應器中加入A3，攪拌並加熱至90℃。以氮氣替代該反應器中之空氣。當該反應器溫度
穩定於90℃，混合物B3注入該反應器。混合物C3以均質機乳化後注入該反應器。該反應器於60℃攪拌1小時。混合物D3以均質機乳化後注入該反應器。於60℃攪動1小後，於放熱聚合反應發生同時，該反應器被逐漸加熱至65至70℃。到達峰溫度後，持續攪動，同時該反應器於30分鐘內冷卻至73℃。注入半數之混合物F3。然後以2小時將混合物E3以及剩餘之混合物F3及G3間分開地加入該反應器中。於將該反應器冷卻至室溫前，溫度維持在73至75℃之間並持續攪動1小時。以Coulter Corporation，多尺寸IIE粒子大小分析儀器測量所得乳膠粒子之直徑為5微米。
實施例11(純球體組成)
在本實施例中，使用甲基丙烯酸甲酯以及甲基丙烯酸烯丙酯將實施例9乳膠之粒子擴大而產生5微米直徑之會聚透鏡。下列A3至C3混合物係以去離子水製備：
實施例1之反應器中加入混合物A3，攪拌並加熱至60℃。以氮氣替代該反應器中之空氣。當該反應器溫度穩定於60℃，混合物B3注入該反應器。混合物C3以均質機乳化後注入該反應器。該反應器於60℃攪拌1小時。混合物D3以均質機乳化後注入該反應器。於60℃攪動1小後，於放熱聚合反應發生同時，該反應器被逐漸加熱至80℃。到達峰溫度後，於88℃持續攪動直至聚合反應呈現高於(>)92%轉化率。聚合反應後，該反應器於30分鐘內冷卻至73℃。於該反應器冷卻至室溫前，持溫在73至75℃之間並持續攪動1小時。以Coulter Corporation多尺寸IIE粒子大小分析儀器測量所得乳膠粒子之直徑為5微米。
得自上述聚合方案之該等5微米球體，藉由
Zess Jenval干涉顯微鏡(250-CF Series JENA)之幫助以干涉顯微術予以分析。自該等干涉條紋，正確測定及描述如前每顆球體之折射率隨其半徑之變化。使用本文所描述之相同種子粒子溶脹/聚合製程產生之具有2微米平均粒子大小之粒子係使用如上所述之Zess Jenval Interphako干涉顯微鏡及周知技術分析而測定該等粒子由中心至表面之折射率。本領域具有通常知識者將預期藉由相同種子粒子溶脹/聚合製程所產生之較小粒子展現相同之漸變折射率之性質且將認知具有0.3至1.9微米平均直徑之給定粒子所展現之折射率形貌(profile)可基於藉由相同方法及組成所產生5微米粒子之折射率形貌來間接測定。
Claims (8)
- 一種膜，包括：聚合物粒子，其具有(a)0.75至15微米之平均粒子直徑以及(b)從該粒子之中心至表面連續變化之折射率；以及連續聚合相，其包括聚烯烴；其中，於400至800奈米測量之該聚合物粒子與該連續聚合相間之平均折射率差係不大於0.02，以及該聚合物粒子與該聚烯烴之重量比為1.5：98.5至0.5：99.5。
- 如申請專利範圍第1項所述之膜，其中，該平均粒子直徑係1.5至10微米。
- 如申請專利範圍第3項所述之膜，其中，該聚合物粒子之折射率係1.45至1.53。
- 如申請專利範圍第3項所述之膜，其中，該聚烯烴包括具有2至8個碳原子之烯烴之聚合物或共聚物。
- 如申請專利範圍第4項所述之膜，其中，位於該聚合物粒子之中心之折射率折射率係1.52至1.60以及位於該聚合物粒子表面之折射率係1.46至1.52。
- 如申請專利範圍第5項所述之膜，其中，該連續聚合相包括1至12重量%之該聚合物粒子。
- 如申請專利範圍第6項所述之膜，其中，該平均粒子直徑係2至8微米。
- 如申請專利範圍第7項所述之膜，其中，該聚合物粒 子包括至少60%丙烯酸系及苯乙烯系單體之聚合殘基。
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