TWI359267B - Radiation differaction sensor,its uses and the pro - Google Patents
Radiation differaction sensor,its uses and the pro Download PDFInfo
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- TWI359267B TWI359267B TW096146877A TW96146877A TWI359267B TW I359267 B TWI359267 B TW I359267B TW 096146877 A TW096146877 A TW 096146877A TW 96146877 A TW96146877 A TW 96146877A TW I359267 B TWI359267 B TW I359267B
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Classifications
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- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/47—Scattering, i.e. diffuse reflection
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/47—Scattering, i.e. diffuse reflection
- G01N21/4788—Diffraction
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/7703—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator using reagent-clad optical fibres or optical waveguides
- G01N2021/7706—Reagent provision
- G01N2021/7723—Swelling part, also for adsorption sensor, i.e. without chemical reaction
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
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1359267 九、發明說明: 【發明所屬之技術領域】 本發明係關於由輻射繞射材料製造之感測器,更具體而 言係關於當與活化劑組合物接觸時展示繞射波長變化之輻 射繞射感測器。 【先前技術】 基於輻射繞射材料之結晶膠體陣列已用於多種目的。結 晶膠體陣列(CCA)係單分散膠體粒子之三維有序陣列。該
等粒子通常由聚合物乳膠(例如聚苯乙烯)或無機材料(例如 一乳化梦)組成。 此等粒子之膠體分散粒子液可形成晶格間距相當於紫 外、可見或紅外輻射之波長的結晶結構。該等結晶結構已 用於對來自廣譜入射輻射之經選擇波長的窄帶進行濾波, 同時允許毗鄰之輻射波長透過。已藉由將粒子分散於液體 介質中粒子來產生先前裝置,藉此該等粒子自對準成一有 序陣列。該等粒子藉由相互聚合或引人使該等粒子溶脹及 融合在一起之溶劑來融合在一起。 在CCA其他應用中,有序陣列固定於基質中且當固定轉 列繞射可見光譜中之H射時可用作著色劑。或者,cca經 製造用以繞射輻射以用作濾光器、光轉換器及光限制器。 儘管該等CCA使錄定粒子間距,但當粒子間距回應刺潔 而變化時CCA可用作感測器。 最近’此等感測器已由含右力p #咖丄 有在水凝膠中聚合之CCA的
凝膠製得。圍繞CCA之該等水魁股Λ A 寺尺凝膠聚合物回應特定的外 126822.doc 1359267 刺激而改變構造°例如,該水凝膠之體積回應刺激而改 變’該刺激包括化學品(例如溶液中的金屬離子及有機分 子,例如葡萄糖)之存在,此使得該等裝置可用於化學分 析。在基於水凝膠之裝置中,單分散高度帶電的膠體粒子 分散於低離子強度液體介質中。該等粒子由於其靜電荷而 自組裝成CCA。根據布拉格定律(如帕i吟該等有序 結構繞射輻射,其中反射滿足布拉格條件之輻射而不滿足 布拉格條件之毗鄰光譜區則透過該裝置。 根據布拉格;t律,繞射韓射之粒子的有序週期性陣 足方程: mX=2ndsin Θ 其中m係-整數,、經反射輻射之波長,及_陣列之有 效折射率’ d係粒子層間的距離’及㊀係反射輻射與粒子層 平面所成的角度。入射輕射在陣列中粒子最上層粒子處以 角度㊀部分地反射至第一層平面且部分地透過下伏粒子 層。儘管同時吸收-些入射輻射,但一部分透射輕射在陣 列中粒子第二層粒子處以角度㊀部分地經反射且部分地透 過下伏粒子層。此以角度㊀部分反射及部分透過下伏粒子 層之特性在整個陣列厚度中延續。繞射輕射之波長⑷可藉 由尺寸d(其可為每層中粒子平面“間的距離)來控制 初’繞射波長λ與填充粒子陣列之粒子粒徑成正比。然 而’在週期性有序陣列中當粒子層間之距離⑷增加時,繞 射輕射之波長亦增加。感測器裝置回應特定化學物質增加 粒子層間之空間距離而增加該裝置中之空間體積板子二 126822.doc 而改變繞射輻射之波長。 在基於水凝膠之CCA中,當水凝膠體積改變時,該cca 之繞射波長亦改變。該等基於水凝膠iCCA裝置通常包含
高百分比的水,例如約30體積%。該等基於水凝膠之ccA 易碎且當CCA之水含量改變時其光學性能易於發生顯著變 化。 為克服該等基於水凝膠CCA之缺點,已使用一種方法來 裝備基於水凝膠之CCA,該方法係使圍繞cca之水凝勝基 質脫水且然後用可聚合單體回填該陣列。將單體聚合以生 成基本上無水的聚合結晶膠體陣列。該等陣列回應一些環 士兄刺激(例如廢應力)(由此改變晶格間距)來改變C c a之繞 射波長。 然而,s亥專基於水凝膠之CCA的先前系統具有明顯的製 造及處理缺點《需要一種更強壯的CCA,其回應所施加化 學品刺激及諸如此類展示輻射繞射性質且去除該等刺激後 其實質上可恢復其初始光學特徵。 【發明内容】 本發明係關於一種輻射繞射感測器,其包括在基板上形 成之粒子有序週期性陣列及塗敷於粒子陣列上之固體基質 組合物,其中該基質組合物係經選擇以對活化劑有回應, 以便暴露於該活化劑時使由感測器所繞射之輻射波長自第 一波長位移至第二波長。本發明亦包括一種製造感測器之 方法,其包括在基板上形成粒子之有序週期性陣列;用基 質塗敷該粒子陣列;及固化該基質以使該等粒子固定於該 126822.doc 基質中粒子’"該基質經選擇以對活化劑有回應,以便 暴露於該活化劑時使由感測器繞射之輻射波長位移。 本發明亦包括-種鑑別物件之方法,其包括在基板上形 成粒子之有序週期性陣列;用基質塗敷該粒子陣列;固化 該基質以使該等粒子陣列固定於該基質中以製造一種在第 -波長處繞射輻射之感測器;將該感測器應用於物件;及 使該感測器與活化劑接觸,以便該活化劑使繞射波長位 移,其中該位移繞射波長表明該物件之真實性。 【實施方式】 本發明包括輻射繞射感測器,λ中該等感測器繞射在可 見及/或非可見光譜中之輻射,1包括其製造方法。該等 輻射繞射感測器包括固持於聚合基f中之粒子有序週期性 陣列。該陣列包括複數個粒子層且滿足布拉格定律: mX=2ndsin Θ 其中m係-整數,祕陣列之有效折射率及d係粒子層之間 距’及λ係以角度㊀自粒子層平面反射之㈣波長。本文所 用繞射輻射之”一"個波長包括電磁輻射光譜之一個頻帶。 例如,提及波長600奈米可包括59〇至61〇奈米。 各種組合物可用於該等粒子,其包括(但不限於)有機聚 合物’例如聚苯乙;)#、聚胺基甲酸酯、丙烯酸系聚合物、 醇酸聚合物、聚_、含石夕氧燒之聚合物、聚硫化物、含環 氧之聚合物,及無機材料例如金屬氧化物(例如氧化鋁、 二氧化矽、氧化鋅、或二氧化鈦)或半導體例如鎘。另 外,該等粒子可具有核_殼結構,其中核可由與上文所述 126822.doc 1359267 整體粒子相同的材料製成。殼可由與核材料相同之聚合物 製成’而對於特定核-殼粒子之陣列粒子殼之聚合物不同 於核材料粒子。核材料及殼材料可具有不同的折射率。另 外,殼之折射率可隨殼厚度在整個殼厚度上以折射率梯度 的形式變化。該殼材料並非膜形成材料,因此該殼材料保 持在適當位置以圍繞各粒子核而不形成殼材料之膜以使 該等核-殼粒子在聚合基保持為離散粒子。 通常,該等粒子一般係球形。對於核·殼粒子,核之直 徑可構成總粒子粒徑的70至95%或總粒子粒徑的鳩而殼 構成粒子粒徑的剩餘部分且具有徑向厚度尺寸。 在實施例中,具有整體結構(非核·殼)之粒子係在表面 活化劑之存在下藉由乳液聚合產生,此獲得帶電粒子之分 散液。適用於乳膠粒子分散液之表面活化劑包括(但不限 於)苯乙烯磺酸鈉、丨_烯丙氧基-2-羥丙基磺酸鈉(可以 SIPOMER COPS-I購自Rhodia&司)、丙浠酿胺丙基續酸 醋^及婦丙基續酸鈉。特別有用之表面活化劑係彼等在粒 子分散液之分散流體(例如水)中稍微溶解者。該等帶電粒 子係藉由諸如超遽、透析或離子交換等技術自分散液中去 除不期望材料(例如未反應的單體、小聚合物、水、引發 劑:表面活化劑、未結合的鹽及粗粒子(聚結粒子”而純化 以裝付帶電粒子之單分散液。超濾尤其適合於純化帶電粒 子。當粒子與諸如鹽或副產寺勿等其他㈣一起存於分散液 中時可降低帶電粒子之排斥力;因此將該粒子分散液 、、屯化至大體上僅含有帶電粒子,其然後容易彼此排斥並形 126822.doc 1359267 成^有序陣列。 去除過量原料、副產物、溶劑及諸如此類後,帶電粒子 之靜電排斥可使該等粒子自身對準成有序陣列。將粒子之 經純化分散液施加於基板上並乾燥之《施加於基板上之粒 子为散液可含有10-70體積%之帶電粒子或3〇·65體積%之 帶電粒子。可藉由浸塗、噴塗、刷塗、輥塗、幕塗、流塗 或壓模塗佈將該分散液施加於基板上至所期望厚度。該濕 塗層可具有4-50微米(例如40微米)之厚度。乾燥後,該材 料可大體上僅含有自對準成布拉格陣列且因此繞射輻射之 粒子。 該基板可為諸如金屬薄板或箔(例如鋁箔)、紙或聚酯或 聚對苯二甲酸乙二酯(PET)之膜(或薄板)等撓性材料,或諸 如玻璃或塑料等非撓性材料^撓性"意指該基板可經受諸 如彎曲、拉伸、壓縮及諸如此類之機械應力而無顯著不可 逆變化。一種合適的基板係微孔薄板。一些微孔薄板之實 例揭示於美國專利第4,833,172號;第4,861,644號及第 6,1 14,023號中,其以引用的方式併入本文中。市售微孔薄 板係由PPG Industries公司以商品名TESLIN銷售。其他適 合的撓性基板包括天然皮革、合成皮革、經整飾天然皮 革、經整飾合成皮革、絨面革、乙烯基耐綸、乙烯乙酸乙 烯酯發泡體(EVA發泡體)、熱塑性胺基甲酸酯(τρυ)、流體 填充的囊狀物、聚烯煙及聚稀烴摻合物、聚乙酸乙烯酯及 共5^物、5^氯乙稀及共聚物、胺基甲酸醋彈性體、合成織 物及天然織物。 126822.doc 在某些實施例中,該等撓性基板係可壓縮基板0 "可壓 縮基板"及類似術語係指能夠經受壓縮變形且壓縮變形停 止後恢復至實質上相同形狀之基板。 術語"壓縮變形"意指一種使基板體積在至少一個方向上 至少暫時降低之機械應力。"EVA發泡體••可包括開孔發泡 體及/或閉孔發泡體《"開孔發泡體"意指該發泡體包括複數 個互連氣室;"閉孔發泡體"意指該發泡體包括離散的閉合 孔。EVA發泡體可包括平薄板或板或模製eVA發泡體,例 如鞋中底。不同類型之EVA發泡體可具有不同類型之表面 孔隙率。模製EVA可包括緻密表面或"表皮",而平薄板或 板可展示多孔表面。本發明之聚胺基曱酸酯基板包括基於 芳香族、脂肪族及混合(混合實例係聚矽氧聚醚或聚酯胺 基甲酸酯及聚矽氧碳酸酯胺基甲酸酯)聚酯或聚醚之熱塑 I1 生胺基曱酸酯。"塑料"係指任何常用熱塑性或熱固性合成 材料,其包括熱塑性烯烴("ΤΡ0")(例如聚乙烯及聚丙烯及 其摻合物)、熱塑性胺基甲酸酯、聚碳酸酯、薄板狀模製 化合物、反應注射成型化合物、基於丙烯腈的材料、耐 綸、及諸如此類。一種特定塑料係包括聚丙烯及EpDM(乙 烯丙婦二稀單體)之Τρο。 在本發明之另一實施例中,核_殼粒子係藉將核單體與 引發刀政在溶液中以製得核粒子的方式製造。將殼單體 連同礼化劑及/或表面活化劑(如上文針對整體粒子者所述) 加至核粒子分散液中,以使殼單體聚合於核粒子上。將 核从粒子为散液如上文所述實施純化以製得僅帶電核-殼 126822.doc 12 比 9267 粒子之分散液,然後當將粒子其施加於基板上時在基板上 形成有序陣列。 將基板上經乾燥的粒子(整體或核·殼)陣列藉由以下固定 於聚合基質中:利用包括單體或其他聚合物前體材料之流 . 冑可固化基質組合物塗敷該粒子陣列,,然後固化該基質組 _ D物。如美國專利第6,894,086號(以引用的方式併入本文 中)所揭示’已在乾燥陣列中自對準之粒子可與流體可固 化基質組合物(例如紫外(UV)可固化組合物)相互穿插。可 藉由次塗、喷塗、刷塗、親塗、凹板塗佈、幕塗、流塗、 槽模塗佈、或喷墨塗佈將該可固化基質組合物材料塗敷至 乾燥粒子陣列上。塗敷係指聚合物前體材料覆蓋整個陣列 且填充至少一些粒子間的間隙。該基質組合物係經固化 (例如藉由暴露於uv輻射)以固定填充粒子之陣列。可使用 其他固化機制以粒子使基質組合物固定在粒子周圍。 對於具有核-殼粒子之輻射繞射感測器,當該陣列與流 • 冑可固化基質組合物相互穿插時’-些基質單體可擴散至 殼中,藉此可增加殼厚度(及粒子粒徑)直至基質組合物固 化為止。溶劑亦可擴散至殼中並引起膨脹。溶劑最終可將 - 自陣列中去除,但此因溶劑之膨脹可影響殼之最終尺寸。 - I體穿插至該陣列中與單體固化之間的時間長度部分地決 定殼的溶脹度。 本發明之輻射繞射感測器係非凝膠狀且實質上為固體。 非凝膠狀係指該輻射繞射感測器不含有流化材料(例如 水),且不為水凝膠。如熟悉此項技術者所瞭解’即使產 126822.doc •13· ^0/ 生與^發明所主張不同之產品,產品感測器亦並非由水凝 ,得纟#實施例中,本發明賴射繞射感測器實質上 ♦子及聚合基質與一些可能的殘餘溶劑且因此實質 上為固體。在該輻射繞射感測器中粒子與聚合物基質之體 積比通常為約25:75至約80:20。 該轄射繞㈣測器可以各種方式應用於物件中。該輻射 =㈣測H可在基板上製造且然後自該基板移除並粉碎成 微粒形式,例如薄片形式。經粉碎之轄射繞射感測器可以 、加劑形式併入塗敷組合物(例如油漆或墨水)中以應用於 物件。或者,該輻射繞射感測器可直接應用於物件,藉此 :基板為物件表面’例如製品之包裝及/或外殼。舉例而 。’製-可包括消費品(包括醫藥產品或食品),其中該基 板為商品之包裝。或者,該物件自身可藉由將粒子陣列直 接應用於物件外殼(例如電子裳置之外殼)或直接應用於商 品(例如服裝、鞋類、運動裝備及諸如此類)而用作基板。 類似地’該物件可為辨識文件、法律文件或其他需要驗證 其真實性之文件。 此外,該辖射繞射感㈣器可製成薄膜&薄板之形式盆 然後經由(例如)黏著劑或諸如此類施加於物件 :、 該等在基板上製造感測器之方法係不同於其他襲造感測号 之技術’其t該等其他技術並不先直接在基板上形成有序 陣列,然後用基質材料塗敷該陣列。 忒輻射繞射感測器對一種或多種使基質在不同波長下繞 射之活化劑的存在有回應。根據本發明,選擇基質組合物 126822.doc 1359267 以便基質與特定活化劑之接觸改變基質尺寸及/或改變基 質之折射率。若尺寸改變,則陣列中粒子間及/或粒子層 之間的空間距離亦可能改變。本文所用之"活化劑"係任何 可使基質尺寸及/或折射率改變之材料。"改變基質尺寸,,及 類似術語意指基質擴張(即"溶脹")或縮小(即"收縮")以回應 活化劑。"改變基質折射率"意指改變基質之有效折射率以 回應活化劑’從而改變由感測器所繞射之輻射波長及/或 強度。有可能改變基質之折射率而不改變其尺寸,反之亦 然。該活化劑可為(例如)化學物質(例如水或有機溶劑)、 或含有溶質或氣體之液體。選擇基質以對特定活化劑有回 應。"回應"活化劑意指該活化劑改變基質之尺寸及/或改變 基質之折射率。在某些實施例中,當活化劑與感測器基質 接觸時’該活化劑變得與基質結合且使基質體積增加。此 基質體積之增加使得粒子層擴展。根據布拉格定律,粒子 間距(d)之增加可使繞射輻射之波長(λ)自初始或第一波長 (λ〗)改變至可能較初始波長更長的第二波長(λ2)。或者,在 其他實施例中該第二波長(人2)可較初始波長(人^短。波長λι 及入2可藉由選擇粒子組合物、粒子徑、基質組合物及/或活 化劑組合物來調節。粒子及基質組合物決定該感測器之有 效折射率(η) 〇粒子粒徑決定陣列層間之起始間距(d)。選 擇基質組合物及活化劑組合物以便活化劑展示與基質之充 分親和力以保持在基質内,而使得基質繞射一不同波長。 波長λ丨及λ?兩者皆可在輻射之可見光譜中,以藉由可見色 位移來展示活化劑之存在性^ χ 1及λ2兩者皆可在不可見光 126822.doc •15- 1359267 譜中,其中可用適合的儀器來檢測波長位移。或者,〜可 在不可見光譜(UV或IR)而λ2在可見光譜中,其中當感測器 與活化劑接觸時顯示顏色。同樣,λ,可在可見光譜而“在 不可見光譜中’以便感測器與活化劑接觸時,繞射光之顏 色消失。任何其他波長組合亦在本發明範圍内。 去除活化劑(例如藉由蒸發)後,感測器基質可至少實質 上恢復至初始繞射波長(即λ!)。實質上意指繞射波長恢復 至其初始波長的約5-10奈米内。理論上,完全去除活化劑 後’基質將恢復至其初始繞射波長。然而,實際上,一些 活化劑可殘留在基質内,因此對於某些基質及活化劑對, 該繞射波長不可能完全恢復至其初始波長。在任一情況 下,當感測器完全恢復或實質恢復至其初始狀態後,該感 測器用於檢測活化劑是否存在。去除活化劑後基質至少實 質上恢復至其初始繞射波長可為介於立即至逐步間之任一 速率。在某些實施例中’感測器可為其中活化劑不能容易 地自基質去除以使感測器恢復至其初始狀態之單一應用設 計。 在一實施例中’基質組合物係水溶性或親水性丙烯酸系 聚合物,其中活化劑係水。適於製造水溶性或親水性基質 之單體包括(但不限於)乙氧基化15三羥甲基丙烷三丙烯酸 醋、乙氧基化2〇三羥甲基丙烷三丙烯酸酯、聚乙二酵(600) 二丙烯酸酯、聚乙二醇(4〇0)二丙烯酸酯、聚乙二醇(200) 二丙烯酸酯、及丙烯酸。 其他適於製造水溶性或親水性聚合物基質之單體可包括 126822.doc -16 - 1359267 聚乙一醇(1000)二丙烯酸酯甲氧基聚乙二醇(35〇)單丙烯 甲氧基聚乙二醇(35〇)單甲基丙烯酸酯、甲氧基聚乙 —醇(550)單甲基丙烯酸酯、甲氧基聚乙二醇(55〇)單丙烯 馱§曰、乙氧基化3〇雙酚A二丙烯酸酯、丙烯酸2(2_乙氧基乙 氧基)乙基醋、丙烯醯胺、丙烯酸羥乙基酯、丙烯酸羥丙 基画曰聚乙一醇(600)二甲基丙烯酸酯、聚乙二醇(4〇〇)二 甲基丙烯醆酯、乙氧基化3〇雙酚A二甲基丙烯酸酯、甲基 丙烯酸羥乙基酯、及甲基丙烯酸羥丙基酯。
由該等單體製成之水溶性或親水性聚合物可用水溶脹。 將水施加於本發明具有水溶性或親水性聚合物基質之輻射 繞射感❹可使得粒子間之歸吸水並溶脹。水溶脹可增 加粒子間之空間距離(布拉格定律之變量⑷),從而使繞射 轄射波長增加。
或者,該基質可為由有機溶劑溶脹之組合物。適合有機 心劑可溶服基質材料係對有機溶劑具有親和力之聚合物, 此思味者該基質聚合物係藉由有機溶劑溶脹至繞射輕射波 之隻化可檢測的程度。適合有機溶劑可溶脹聚合物係由 以下列非限制單體製得:烧氧基化己二醇二丙烯酸醋、乙 ,基化3三羥曱基丙烷三丙烯酸酯、異戊四醇四丙烯酸 酯、異戊四醇三丙烯酸酯、丙氧基化3三羥甲基丙烷三丙 烯酉“曰、丙氧基化6三羥甲基丙烷三丙烯酸酯、丁二醇 二丙烯酸酯、乙氧基化3雙酚A二丙烯酸醋、三羥甲基丙烷 ^丙埽酸醋、丙氧基化2新戊二醇:丙稀^旨、乙氧基化3 二羥甲基丙烷三丙烯酸醋、乙氧基化6三羥甲基丙烷三丙 126822.doc 1359267 烯酸酯、乙氧基化9三羥甲基丙烷三丙烯酸酯、乙氧基化3 雙盼A一甲基丙烯醆酯、新戊二醇二丙烯酸酯、及1,6-己 二醇二丙烯酸酯。 其他適於製造有機溶劑可溶脹丙烯酸系聚合物基質之單 體可包括丙氧基化3三丙烯酸甘油基酯、丙烯酸硬脂基 酯、丙烯酸四氫糠基酯、丙烯酸月桂酯、丙烯酸2苯氧乙 基醋、丙稀酸異癸酯、丙烯酸異辛基酯、丙烯酸辛基酯、 丙烯酸癸酯、丙烯酸十三烷基酯、己内酯丙烯酸酯、乙氧 基化4壬基酚丙烯酸酯、丙烯酸異冰片酯、丙烯酸丁基 酉旨、四乙二醇二丙烯酸酯、三乙二醇二丙烯酸酯、二-三 經曱基丙烧四丙烯酸酯、乙氧基化4異戊四醇四丙烯酸 酯、丙烯酸乙酯、丙烯酸2-乙基己基酯、苯.乙烯、丙烯 腈、三羥曱基丙烷三丙烯酸酯、甲基丙烯酸甲酯、甲基丙 烯酸丁酯、甲基丙烯酸環己基酯、曱基丙烯酸異冰片酯、 甲基丙烯酸月桂基酯、聚丙二醇單甲基丙烯酸酯、丙氧基 化2甲基丙烯酸烯丙基酯、甲基丙烯酸烯丙基酯、乙氧基 甲基丙烯酸十六烷基酯、乙氧基甲基丙烯酸硬脂基酯、乙 氧基化2甲基丙烯酸羥乙基酯、乙氧基化5甲基丙烯酸羥乙 基酯、乙氧基化1〇甲基丙稀酸經乙基酯、乙氧基化4壬基盼 甲基丙烯酸酯、乙氧基三甘醇曱基丙烯酸酯、甲基丙烯酸 四氫糠基酯、甲基丙烯酸異癸基酯、曱基丙烯酸月桂基 酯、甲基丙烯酸硬脂基酯、曱基丙烯酸2-苯氧乙基酯、甲 基丙烯酸縮水甘油酯、甲基丙烯酸異冰片酯、甲基丙烯酸 十三烷基酯、環己烷二甲醇二甲基丙烯酸酯、乙氧基化4 126822.doc -18· 1359267 雙酚A二甲基丙烯酸酯、乙氧基化8雙酚A二甲基丙烯酸 酯、二乙二醇二甲基丙烯酸酯、乙二醇二甲基丙烯酸酯、 四乙二醇二甲基丙烯酸酯、丨,4-丁二醇二甲基丙烯酸酯、 1,6-己二醇二甲基丙烯酸酯、新戊二醇二甲基丙烯酸酯、 1,3-丁二醇二甲基丙烯酸酯、乙氧基化2雙酚人二〒基丙烯 酸酯、乙氧基化10雙酚A二甲基丙烯酸酯、乙氧基化6雙酚 A二甲基丙烯酸酯、脂族胺基甲酸酯丙烯酸酯、脂族胺基 甲酸酯寡聚物、丙烯酸系寡聚物、聚醚丙烯酸酯寡聚物、 聚丁二烯二f基丙烯酸酯寡聚物、二丙烯酸酯寡聚物、三 丙烯酸醋寡㈣、聚醋丙職醋寡聚#、環氧基丙烯酸醋 及芳香族胺基甲酸酯丙烯酸酯。 適合的有機溶劑包括脂族烴(例如石油醚、戊院、己 烷庚烷及異十二烷);環脂族烴(例如環己烷、甲基環己 烷二乙基環己烷、四氫萘及十氫萘);祐及類箱(例如木材 松節油、松油、α-蔽烯、β_㈣、二戊稀及d_宇稀);芳香 例如笨、甲苯、二甲苯、乙基苯、異丙苯、均三甲 苯、假茴香烯、連三曱苯、繳花醇及苯乙烯);氯化烴(例 如-氣甲烷、二氣曱烷、氣乙烷、12_二氣乙烷、“,卜三 氯=烷、三氣乙烯、全氣乙烯及丨,2·二氣丙烷);醇(例如 甲醇、乙醇、丙醇、異丙醇、丁醇、第二丁醇、第三-丁 醇、戍醇、異戊醇、己醇、庚醇、辛醇、壬醇、甲基異丁 基曱醇、2-乙基丁醇、異辛醇、2_乙基己醇、異壬醇、異 :醇:二異丁基甲醇、環己醇、甲基環己醇、三甲基環己 醇节醇、甲基节醇、糖醇、四氣祿醇、及二丙㈣ 126822.doc -19- 1359267 酮(例如丙酮、曱基乙基酮、甲基丙基酮、甲基異丙基 酮、甲基丁基酮、甲基異丁基酮、甲基戊基酮、甲基異戊 基酮、二乙酮、乙基丁基酮、乙基戊基酮、二異丙基酮、 二異丁基酮、環己酮、甲基環己酮、二甲基環己酮、三甲 基環己酮、異亞丙基丙酮、異佛爾酮、及乙醯丙酮);酯 (例如甲酸曱酯、甲酸乙酯、甲酸丁酯、曱酸異丁酯、乙 酸甲酯、乙酸丙酯、乙酸異丙酯、乙酸丁酯、乙酸異丁 酯、乙酸第二丁酯、乙酸戊酯、乙酸異戊酯、乙酸己酯、 乙酸庚酯、乙酸2·乙基己基酯、乙酸環己酯、乙酸苄酯、 丙二醇二乙酸酯、丙酸甲酯、丙酸乙酯、丙酸丙酯、丙酸 丁酯、丙酸戊酯、丁酸乙酯、丁酸丙酯、丁酸丁酯、丁酸 異丁酯、丁酸戊酯、異丁酸甲酯、異丁酸乙酯、異丁酸異 丙酯、異丁酸異丁酯、乳酸甲酯、乳酸乙酯、乳酸異丙 酯、乳酸丁酯、羥乙酸丁酯、甲基甘醇乙酸酯、乙基甘醇 乙酸酯、丁基甘醇乙酸酯、乙基二甘醇乙酸醋、丁基二甘 酵乙&L自曰、乙酸曱氧基丙自旨、乙酸乙氧基丙g旨、乙酸3_甲 氧基丁酯、3-乙氧基丙酸乙酯、二元酯、碳酸乙二酯、碳 酸丙二酯及丁内酯);甘醇醚(例如甲基甘醇、乙基甘醇、 丙基甘醇、異丙基甘醇、丁基甘醇、己基甘醇、苯基甘 醇、甲基二甘醇、乙基二甘醇、丁基二甘醇、己基二甘 醇、甲基三甘醇、乙基三甘醇、丁基三甘醇、丁基四甘 醇、1-曱氧基-2·丙醇、乙氧基丙醇、異丙氧基丙醇、丁氧 基丙醇、異丁氧基丙醇、第三_ 丁氧基丙_、苯氧丙醇、 甲基二丙二醇、異丙基二丙二醇、丁基二丙二醇、曱基三 126822.doc •20· 1359267 丙一醇、丁基三丙二醇、二甘醇二甲基醚及二丙二醇二曱 醚),醚(例如二乙醚、二異丙醚、二丁醚、曱基第三丁 醚、四氫呋喃、二氧雜環己烷、2,2-二甲基-4-羥甲基_i,3_ —氧雜環己烷及1,2-環氧丙烷);及其他溶劑(例如二甲基 縮經、二曱基甲醯胺、二甲基乙醯胺、二甲亞艰、環丁 碾、二硫化碳、糠醛、硝基乙烷、丨·硝基丙烷、2硝基丙 烷、N-甲基吡咯啶酮、N•乙基吡咯啶酮、N_環己基吡咯啶 酮、N-(2-羥乙基)吡咯啶酮、丨,3_二曱基_2·咪唑啶酮及六 亞甲基磷酸三醯胺)。該等有機溶劑亦可用於使水溶性或 親水性丙烯酸系聚合物基質溶脹。 在另一實施例中,可選擇聚合物基質以使該基質回應特 定活化劑繞射不同波長’例如溶液中之金屬離子、有機分 子(例如葡萄糖)、溶液中之氣體、各種來源之抗原、各種 來源之抗體、及病毒(例如HIV)。例如,具有酸官能團之 聚合物基質可與含有鹼之活化劑組合物反應,或其中該基 質具有鹼官能團且活化劑具有酸官能團之相反情況。可選 擇聚合物基質以使該基質回應各種活化劑而溶脹、收縮或 者改變尺寸及/或折射率。該基質可包括當暴露於其中時 抗體結合至其之抗原。類似地,感測器可基於酵素及基板 對、螯合劑、錯合劑或適配子。對於某些感測器,活化劑 與基質之結合可足夠強以使活化劑保持吸引結合至該基 質及/或在基質内而幾乎不會使感測器恢復至其初始狀 態。在此等實施例中,活化劑與基質之間可產生共價鍵或 離子鍵。熟悉此項技術者應瞭解,本文所揭示各種實施例 126822.doc •21 · 1359267 及本發明範圍内之其他實施例將在環境、醫藥、冶金及化 學領域中有多種應用。 應瞭解’藉由選擇特定基質組合物及適合的活化劑可調 即基質之繞射波長。本發明之輻射繞射感測器可用於各種 應用令,其包括標記或辨識物件(例如在醫藥包裝上用於 鑑別醫藥來源),用於鑑別文件或諸如此類之安全裝置, 作為感測器用於感測化學物質之存在或用作新奇物件(例 如玩具)。本發明之輻射繞射感測器可單獨提供或連同用 於接觸感測器之活化劑—起以套組形式提供,該活化劑改 變繞射輻射至位移波長。 本發明之感測器可用於鑑別物件,例如用以鑑別文件或 裝置或用以辨識商品之來源。若該感測器對活化劑有回 應,則認為帶有本發明感測器之文件(例如安全卡)係真實 的。"安全卡,,包括可鑑別其持有者之身份或允許其進入一 設施之文件或裝置(例如為佩章形式)。該安全卡可識別該 卡(例如,光-識別卡或護照)的持有者或可用作指示允許其 持有者進入安全設施之文件或裝置。例如,一安全卡可顯 不為真的且當應用合適活化劑後,卡上之感測器將展示繞 射輻射之波長位移。偽造安全卡將不能展示該波長位移。 同樣,對於在帶有本發明感測器之包裝中所提供的物品 (例如醫藥產品)’消費者可藉由將適合的活化劑應用於其 來測試包裝的真實性。認為對活化劑無回應之包裝係偽造 的,而認為對活化劑有回應之包裝係真實的。其他消費品 可(例如)在成品(例如電子裝置)之外殼上或在衣物(例如鞋) 126822.doc -22- 1359267 表面上包括本發明感測器。該等消費品之真實性可藉由將 活化劑應用於其來測試或該感測器之活化可為物件之新穎 特徵。"物件"包括可應用本發明感測器之任何產品,其包 括但不限於彼等本文所討論者。 粒子之有序週期性陣列係形成於基板上且用基質塗敷, 使該基質如上文所述固化以製造感測器。在其上形成感測 器之基板可為薄膜或薄板,隨後將其應用於物件或另一表
面(例如微孔板或金屬箔之表面)。另外,物件之表面可基 板用於製造感測P在此情況下,有序週期性陣列係在該 物件表面上形成並將基質組合物塗敷於其上。該感測器可 經由遮罩應用於該物件的一部分以使該感測器定位於特定 位置。該物件粒子表面之任何剩餘部&可用纟適的塗敷组 合物塗敷或實質上塗敷以產生其中感測器暴露'而任何剩 餘基板均經塗敷之基板°例如,本發明感測器可應用於微 孔薄板’ ^該薄板之剩餘部分可經塗敷、層壓或類似處 理。可以此方式製備安全卡。另外,該感測器可與適合的 活化劑接觸’而該卡之剩餘部分藉由塗敷或層壓而免於磨 損或撕裂或諸如此類。 U於物件上之感測器與使繞射輻射波長位移之活化劑 接觸經位移波長可在可見光譜或不可見光譜中。去除活 化劑後感測器至少實質上恢復至其初始狀態。例如,親水 性丙稀酸系聚合物基質可藉由暴露於水而溶脹。若帶有感 測器之識別卡與水接觸,則會發生繞射波長之位移,從而 證實該識別卡之真實性。當水蒸發後,該繞射波長實質上 126822.doc •23· 恢復至其初始狀態。 表明確說明,否則本文所用所有數字(例如彼等 樣=範圍、數量或百分比者)可以如同以詞"約"開始 =理解’即使該術語並未明確出現。本文所列舉之任 意欲包括其中所包含的所有子範圍。複數涵蓋 ”二2亦然。例如’當本文(包括中請專利範圍)提到 個有序週期性陣列、"一種"基質、"一種"活化劑、及 f如此類時’可使用—個以上,且儘管提到改變基質之多 m ’但可能僅改變-個尺寸。同樣,本文所用術語 “物”意指預聚物、募聚物及均聚物及共聚物兩者;前 綴聚”係指兩個或更多。 輻射繞射感測器作為水印之該等實例性應用並非意欲限 制另外下列實例僅為說明本發明而非意欲加以限制。 實例 實例1 :可固化丙烯酸系基質 經由以下程序製備一種紫外輻射可固化有機組合物◊在 搜拌的Θ時將二苯基(2,4,6-三甲基苯甲醯基)氧化鱗及2_經 基2甲基本丙_ (購自Aidrich (Chemical有限公司,
Milwaukee,粘8,)之5〇/5〇摻合物(〇15克)添加於5 〇克乙氧 基化2〇一經甲基丙炫二丙稀酸g旨(購自Sartomer有限公司, Exton,Pa.)中。 實例2 :可固化丙烯酸系基質 經由以下程序製備一種紫外輻射可固化有機組合物。在 攪拌的同時將二苯基(2,4,6-三甲基苯甲醯基)氧化膦及2_羥 126822.doc -24- 1359267 基-2-甲基-苯丙酮(購自 Aldrich Chemical公司 ’ Milwaukee,
Wis·)之50/50摻合物(0.15克)添加於4.0克乙氧基化20三羥甲 基丙院三丙稀酸醋(購自Sartomer有限公司,Exton,Pa.) 中。然後在攪拌的同時於該混合物中加入丙烯酸(1.0 克)(購自Aldrich Chemical有限公司)。 實例3 :可固化丙烯酸系基質 經由以下程序製備一種紫外輻射可固化有機組合物。在 攪拌的同時將二苯基(2,4,6-三甲基苯甲醯基)氧化膦及2-羥 基-2-甲基-苯丙_ (購自Aldrich Chemical有限公司,
Milwaukee,Wis.)之5 0/5 0摻合物(0.15克)添加於5克丙氧基 化2新戊一醇二丙稀酸g旨(購自sartomer有限公司,Exton, Pa.)中。 實例4 :核-殼粒子之陣列 經由以下程序製備一種聚苯乙烯-二乙烯苯核/苯乙烯·曱 基丙烯酸甲酯-乙二醇二甲基丙烯酸酯_二乙烯苯殼粒子存 於水中之分散液。 將碳酸氫納(4·9克)(購自Aldrich Chemical有限公司)與 4090克去離子水混合並添加於12•升配有熱電偶加熱夾 套、搜拌器、回流冷凝器及氮氣人口之反應爸中。在授拌 的同時m合物用氮氣鼓泡43分鐘且然後用氣氣覆蓋。 在授拌的同時於该混合物中加入Aerc)sc)1 MA8(M(46 8克於 41〇克去離子水中)(購自一 一心公司),隨後用48 克去離子水清洗。你田k I 士 。 月无使用加熱夾套將該混合物加熱至約50 C。在授掉的同時加入! 7接错触 苯乙廊單體(832.8克)(購自Aldrich 126822.doc •25- 1359267
Chemical有限公司)。將該混合物加熱至6〇。。。在攪拌的同 時於該混合物中加入過硫酸鋼(購自線咖chemi_限 公司)(12.5克於144克去離子水中)。將混合物之溫度保持
Aldrich Chemica丨有限公司)(2〇5 4克)並將溫度在約6〇t下 保持2.3小時〇在攪拌的同時於混合物中加入叫(聚氧
乙烯(23)月桂基醚)(購自Aidrich Chemical有限公司)(5 〇克 於100克去離子水中)。然後,在攪拌的同時於混合物中加 入過硫酸鈉(購自Aldrich Chemical有限公司)(9. i克於9〇〇克 去離子水中)。在攪拌的同時於該反應混合物中加入苯乙 烯(200克)、曱基丙烯酸甲酯(478 8克)、乙二醇二甲基丙 稀酸酯(48克)及二乙烯苯(3〇2克)(均購自AldHch
Chemical 有限公司)之混合物。在攪拌的同時於該反應混合物中加 入Sipomer COPS-I(3-烯丙氧基_2_羥基-丨_丙烷磺酸82 7 克)(購自Rhodia公司,Cranbury, NJ.)且然後加入(1〇〇克)去
恆定40分鐘。在攪拌下 ’於混合物中加入二乙烯苯(購自 離子水。將混合物溫度在60。(:下保持約4.0小時。 將所得聚合物分散液經5微米過濾袋過濾。使用4英吋超 遽设利用2.41吳对聚二氣亞乙烯膜(兩者皆購自ρτι
Advanced Filtration公司,〇xnard,CA.)將該聚合物分散液 超滤且用螺動幫浦以約170毫升/秒之流速泵送。去除3〇〇〇 克超濾液後於該分散液中加入去離子水(2985克)。將該交 換重複數次直至用1 1348克去離子水替換11349克超濾液。 然後將額外的超濾液去除直至該混合物之固體含量為44 8 126822.doc •26- 1359267 經由槽模塗佈機(購自Frontier Industrial Technology公 司’ To wanda,PA)將該材料施加於2密耳厚的聚對苯二甲酸 乙二醋(PET)基板上並在180°F下乾燥40秒以得到約7微米 之乾燥厚度。利用Cary 500光譜儀(購自Varian公司)在518 奈米下量測所得材料之繞射光。 實例5 :水溶性固定陣列 用下拉桿將實例1中所製備材料施加於實例4之聚苯乙 烯-二乙烯苯核/苯乙烯_甲基丙烯酸甲酯_乙二醇二甲基丙 烯酸酯-二乙稀苯殼粒子之固定陣列上。然後將一片2密耳 厚的PET膜放置於實例丨之沈積材料上以完全覆蓋該材料。 在PET基板之頂部側使用輥以擴展並迫使實例i之uv可固 化塗層進入實例4之固定陣列的間隙空間中。使用1〇〇…汞 燈將樣品紫外輻射固化《然後將兩層PET分離。 當以垂直或〇度觀察時該膜對觀察者展示綠色而當以45 度或更大角度觀察時對觀察者展示藍色。使用Cary 5〇〇光 譜計量測該膜之繞射波長。隨後,將該膜暴露於水中並再 次量測繞射波長。將水蒸發後最後一次量測該膜。列於下 表1中之結果顯示,該材料之繞射波長隨水之施加而增加 且去除水後基本上恢復至其初始狀態。 表1 樣品 — ---繞射波長____ L 56〇¥i 初始狀態 ~~ 經水合(Η2〇) 602奋籴 經乾燥 558备朵 實例6:官能團可溶張固定陣列 126822.doc -27- 1359267 重複實例5之程序,只是用實例2之材料(含有酸基團)代 替實例1之材料。當以垂直或〇度觀察時該膜對觀察者展示 綠色而當以45度或更大角度觀察時對觀察者展示藍色。使 = Cary _光譜計量測該膜之繞射波長。隨後,將該膜暴 露於水中並再次量測該繞射波卩。將該膜暴露於5%鹼(二 甲基乙醇胺(DMEA))存於去離子水中之溶液中,並重新量 測繞射波長。將DMEA溶液蒸發後最後—次量測該膜。列
於表2之結果顯示’含有酸基團之膜的丙烯酸系聚合物基 質材料可由水及㈣者溶脹且去除水及㈣基本上恢復至 其初始狀態。 由於實例6之基質材料中包含酸官能團,故實例6之產物 不同於實例5之產物。當兩種產物與水接觸時皆溶脹,如 由繞射輻射波長自560奈求改變至6〇2奈米所證實。當實例 6之產物與驗(麵A)接觸時可進_步改變,如由繞射輕射 波長進一步增加至623奈米所證實。 表2
實例7 ·有機溶劑可溶脹固定陣列 重複實例5之程序’只是用奢 用實例3之材料代替實例1之材 料。當以垂直或0度觀察時該 、 联對械察者展示綠色而當以 45度或更大角度觀察時對觀察去思_ 祝祭者展不藍色。使用Cary 500 光譜計量測該膜之繞射波長。 ^隨後,將該骐暴露於水中並 126822.doc •28- 1359267 再次量測繞射波長,其中基本上沒有變化。然後將該膜暴 露於95%的變性乙醇中並量測繞射波長。將乙醇蒸發後最 後一次量測該膜。列於表3之結果顯示’該膜並不因水而 溶脹,而因乙醇溶脹且去除乙醇後幾乎恢復至其原始狀 態。 樣品 繞射i長 初始狀態 556奈米 經水合(H20) 556奈米 經乙醇暴露 - 610奈米 &醇蒸發後 __564奈米 如本文所證實,本發明之輻射繞射材料可用於感測水或 有機溶劑之存在。 儘管上文中闞述本發明之較佳實施例,但可對本發明實 施各種修改及改變而不㈣本發明之精神及範^本發明 之範圍定義於隨附申請專利範圍及其等效物中。 126822.doc 29-
Claims (1)
1359267 第096146877號專利申請案 中文申請專利範圍替換本(100年9月) 申請專利範圍·· ---- 種輻射繞射感測器,其包括: 十 在基板上所形成之粒子有序週期性陣列;及 塗敷於該粒子陣列上之固體基質組合物; 其中該基質組合物係經選擇以對活化劑有回應,以便 暴露於該活化劑時使由該感測器所繞射之輻射波長自第 一波長位移至第二波長。 2.如凊求項i之感測器,其巾當自該感測器去除該活化劑 時,該繞射輻射波長實質上恢復至該第一波長。 3:如請求们之感測器’其中該基f包括對水有回應之親 水性丙烯酸系聚合物。 1其中該基質包括對有機溶劑有回 其中該基板係薄膜。 其中該基板係微孔薄板。 其中s玄基板係物件之表面。 其中該表面係物件之包裝及/或外 4. 如請求項1之感測器 應之聚合物。 5. 如請求項1之感測器 6. 如請求項1之感測器 7. 如請求項1之感測器 8. 如請求項7之感測器 殼。 9. 一種製造感測器之方法,其包括: 在基板上形成粒子之有序週期性陣列; 用基質塗敷該粒子陣列;及 =該基質以將該粒子陣列固定於該基質内,其中該 經選擇以回應活化劑’以便暴露於該活化劑時使 由该感測器所繞射之轄射波長位移至位移波長。 126822-1000927.doc 10.如請求項9 u.如請求項10之方法其中該活化劑包括水。 入板 ,其中該基質包括親水性丙烯酸系聚 12.如請求項9之方法, 13·如請求項12之方法 之聚合物。 其中該活化劑包括有機溶劑。 ’其中該基質包括對有機溶劑有回應 14. 如請求項9之方 ,/、中該位移波長係在可見光譜中。 15. 如4求項9之方法 .,_ ’,、中該位移波長係在可見光譜以 16.如請求項9之方法,其進一 器。 步包括自該基板移除該感測 如-月求項16之方法,其進一步包括將該感測器粉碎成微 粒子形式。 ⑼求項9之方法,其中該活化劑包括與該基質反應之 官能團。 19’ -種物件,其具有根據請求項9之方法製造的感測器。 20· 一種鑑別物件之方法,其包括: 在基板上形成粒子之有序週期性陣列; 用基質塗敷該粒子陣列; 固化該基質而形成固體組合物,以將該粒子陣列固定 於"亥基質内以製造在第一波長繞射輕射之感測器; 將該感測器應用於物件上;及 使該感測器與活化劑接觸以便該活化劑使繞射波長位 移’其中該位移繞射波長表明該物件之真實性。 126822-1000927.doc 1359267 21. 如明求項20之方法,其中該位移波長係在 可見光譜t。 22. 如6月求項20之方法,其中該位移波長係在可見光譜以 外。 月求項20之方法,其中該基板係應用於該物件之膜。 24. 如請求項2〇之方法,其中該基板係該物件之表面。 25. 如請求項2〇之方法,其中該基㈣微孔薄板。 6.如明求項20之方法,其進一步包括將該活化劑自該感測 器去除以使繞射H射波長實f上恢復至該第—波長。 27·如請求項20之方法,其中該物件係安全卡。 又 28·如請求項20之方法,其中該基板為撓性。 29, 如请求項20之方法,其中該基板係EVA發泡體。 30. 如請求項20之方法,其中該基板係金屬。 126822-1000927.doc
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Also Published As
Publication number | Publication date |
---|---|
BRPI0720803A2 (pt) | 2014-03-04 |
CN101622524A (zh) | 2010-01-06 |
EP2122335A1 (en) | 2009-11-25 |
RU2009133272A (ru) | 2011-03-20 |
MX2009008457A (es) | 2009-08-17 |
JP2012215893A (ja) | 2012-11-08 |
NO20092971L (no) | 2009-09-04 |
KR101114588B1 (ko) | 2012-03-05 |
WO2008097397A1 (en) | 2008-08-14 |
US20080185498A1 (en) | 2008-08-07 |
PE20081239A1 (es) | 2008-10-10 |
CA2676734A1 (en) | 2008-08-14 |
JP2010518447A (ja) | 2010-05-27 |
AR064094A1 (es) | 2009-03-11 |
CL2007003492A1 (es) | 2008-07-04 |
RU2436072C2 (ru) | 2011-12-10 |
NZ578623A (en) | 2012-04-27 |
AU2007346613A1 (en) | 2008-08-14 |
CN101622524B (zh) | 2012-11-14 |
CA2676734C (en) | 2013-02-26 |
UA94646C2 (ru) | 2011-05-25 |
TW200837343A (en) | 2008-09-16 |
HK1137806A1 (en) | 2010-08-06 |
US7682530B2 (en) | 2010-03-23 |
UY30765A1 (es) | 2008-07-03 |
KR20090123872A (ko) | 2009-12-02 |
AU2007346613B2 (en) | 2011-02-24 |
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