TW201808851A - 中性色彩之抗反射玻璃基材及其製造方法 - Google Patents
中性色彩之抗反射玻璃基材及其製造方法 Download PDFInfo
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Abstract
本發明係關於藉由離子植入製造中性色彩之抗反射玻璃基材之方法,其包含將N2
源氣體離子化,以便形成N之單電荷及多電荷離子之混合物,藉由利用包含在20 kV與25 kV之間之加速電壓A加速並將離子劑量設定在包含在6 × 1016
個離子/cm2
與-5.00 × 1015
× A/kV + 2.00 × 1017
個離子/cm2
之間之值而形成N之單電荷及多電荷離子束。本發明進一步係關於中性色彩之抗反射玻璃基材,其包含根據此方法利用單電荷及多電荷離子之混合物藉由離子植入處理之區域。
Description
本發明係關於中性色彩之抗反射玻璃基材及其製造方法。本發明亦係關於中性色彩之抗反射玻璃基材的用途,特別是用作為窗用玻璃(glazing)的用途。
大多數抗反射玻璃基材係藉由在玻璃表面上沈積塗層而獲得。光反射率之降低係藉由單層獲得,該單層之折射率低於玻璃基材之折射率或具有折射率梯度。高性能抗反射玻璃基材係藉由多層之堆疊獲得,其利用干涉效應以在整個可見範圍內獲得光反射率之顯著降低。施加至基材兩側之此高性能抗反射層堆疊能使典型玻璃基材之光反射率自約8%降低至4%或甚至更小。然而,其需要多層沈積步驟,該步驟具有高度組成及層厚度控制,從而使其成為困難且由此昂貴之製程。此外,通常藉由物理氣相沈積來沈積之單一中性色彩之抗反射層且尤其多層堆疊與玻璃自身相比,對機械及/或化學侵蝕更敏感。單層抗反射層通常在反射中呈現非中性之色彩且中性色彩之多層抗反射塗層需要甚至更大數目之層,從而使得所得層堆疊甚至更敏感。 另一種抗反射玻璃基材已揭示於FR1300336中。在此,抗反射效應係藉由以10原子%之濃度將稀有氣體之重離子植入玻璃基材之表面中深達100 nm或200 nm之深度而獲得。然而,稀有氣體相對昂貴,且在玻璃基材中達到植入稀有氣體離子之此等高濃度的需要會增加對玻璃網絡產生重大損壞之風險。此外,該等玻璃基材在反射中並非中性。 因此業內需要提供製造中性色彩之抗反射玻璃基材之簡單、廉價的方法。
根據本發明之一個態樣,本發明之主題係提供生產中性色彩之抗反射玻璃基材之方法。 根據本發明之另一態樣,本發明之主題係提供中性色彩之抗反射玻璃基材。
本發明係關於生產中性色彩之抗反射玻璃基材之方法,其包含以下操作: ● 提供N2
源氣體, ● 將該N2
源氣體離子化,以便形成N之單電荷離子及多電荷離子之混合物, ● 利用加速電壓使該N之單電荷離子及多電荷離子之混合物加速,以便形成N之單電荷離子及多電荷離子之束,其中該加速電壓A係包含在20 kV與25 kV之間且劑量D係包含在6 × 1016
個離子/cm2
與-5.00 × 1015
× A/kV + 2.00 × 1017
個離子/cm2
之間, ● 提供玻璃基材, ● 將該玻璃基材定位於該N之單電荷及多電荷離子束之軌跡中。 本發明者已驚訝地發現,提供包含以相同特定加速電壓加速且在此特定劑量下施加至玻璃基材之N之單電荷及多電荷離子之混合物之離子束的本發明方法導致反射率降低。有利地,所得玻璃基材之反射率自約8%減小至至多6.5%、較佳至多6%、更佳至多5.5%。最令人驚訝的是達成此低程度之反射率,而植入N之濃度在整個植入深度上低於2原子%,且此外由反射中a*及b*之色坐標表示之反射中之色彩係中性的(即,-1 ≤ a* ≤ 1且-1 ≤ b* ≤ 1),或甚至極中性的(即,-0.3 ≤ a* ≤ 0.3且-0.3 ≤ b* ≤ 0.3)。 根據本發明,將N2
源氣體離子化,以便形成N之單電荷離子及多電荷離子之混合物。經加速單電荷離子及多電荷離子之束可包含不同量之不同N離子。較佳地,經加速單電荷及多電荷離子之束包含N+
、N2+
及N3+
。 各別離子之實例性流顯示於下表1中(以毫安培量測)。 表1
根據本發明,關鍵離子植入參數係離子加速電壓及離子劑量。 選擇玻璃基材於單電荷及多電荷離子束之軌跡中之定位,使得獲得一定量之每表面積離子或離子劑量。離子劑量或劑量表示為離子數目/平方公分。出於本發明之目的,離子劑量係單電荷離子及多電荷離子之總劑量。離子束較佳提供單電荷及多電荷離子之連續流。離子劑量係藉由控制基材向離子束之暴露時間來控制。根據本發明,多電荷離子係攜帶一個以上正電荷之離子。單電荷離子係攜帶單個正電荷之離子。 在本發明之一個實施例中,定位包含使玻璃基材及離子植入束相對於彼此移動,以便逐步處理一定表面積之玻璃基材。較佳地,玻璃基材及離子植入束以包含於0.1 mm/s與1000 mm/s之間之速度相對於彼此移動。以適當方式選擇玻璃相對於離子植入束之移動速度,以控制試樣在束中之滯留時間,該時間影響所處理區域之離子劑量。 本發明之方法可易於按比例放大以便處理超過1 m2
之大基材,例如藉由利用本發明之離子束連續掃描基材表面,或例如藉由形成多離子源之陣列以單遍次或多遍次處理在其整個寬度上移動之基材。 本發明者已發現,提供經相同加速電壓加速之包含單電荷及多電荷離子之混合物之離子束的離子源尤其有用,此乃因其可提供較單電荷離子劑量低之多電荷離子之劑量。看起來中性色彩之抗反射玻璃基材可利用此一束中提供之單電荷離子(具有較高劑量及較低植入能量)及多電荷離子(具有較低劑量及較高植入能量)之混合物獲得。以電子伏特(eV)表示之植入能量係藉由將單電荷離子或多電荷離子之電荷與加速電壓相乘來計算。 在本發明之較佳實施例中,位於所處理區域下方之所處理玻璃基材區域之溫度小於或等於玻璃基材之玻璃轉換溫度。此溫度受(例如)束之離子流、經處理區域在束中之滯留時間及基材之任何冷卻手段影響。 在本發明之一個實施例中,同時或相繼使用若干離子植入束來處理玻璃基材。 在本發明之一個實施例中,每玻璃基材之表面單位面積之總離子劑量係藉由離子植入束之單次處理獲得。 在本發明之另一實施例中,每玻璃基材之表面單位面積之總離子劑量係藉由一或多個離子植入束之若干次連續處理獲得。 在較佳實施例中,玻璃基材在其兩個面上皆利用本發明之方法處理,以便最大化低反射率效應。 本發明之方法較佳在真空室中在包含在10-2
毫巴(mbar)與10-7
毫巴之間、更佳地10-5
毫巴與10-6
毫巴之間之壓力下實施。 用於實施本發明方法之實例性離子源係來自Quertech Ingénierie S.A.之Hardion + RCE離子源。 反射率係在使用照明體D65及2°觀測角經本發明之離子植入方法處理之基材之側量測。反射中之色彩係在照明體D65下使用10°觀測角使用CIELAB色坐標a*及b*表示,並在經本發明方法處理之基材之側量測。CIE L*a*b*或CIELAB係由國際照明委員會(International Commission on Illumination)所指定之色彩空間。 本發明亦係關於N之單電荷及多電荷離子之混合物使玻璃基材之反射率減小且同時使反射中之色彩保持中性之用途,單電荷及多電荷離子之混合物係在有效降低玻璃基材之反射率且同時使反射中之色彩保持中性之離子劑量及加速電壓下植入玻璃基材中。 有利地,N之單電荷及多電荷離子之混合物係在有效使玻璃基材之反射率降低至至多6.5%、較佳地至多6%、更佳地至多5.5%之離子劑量及加速電壓下植入玻璃基材中。同時使反射中之色彩保持中性,即-1 ≤ a* ≤ 1且-1 ≤ b* ≤ 1。 玻璃基材之反射率在處理之前係約8%。 更有利地,N之單電荷及多電荷離子之混合物係用於使玻璃基材之反射率降低至至多6.5%、較佳地至多6%、更佳地至多5.5%。同時使反射中之色彩保持極中性,即-0.3 ≤ a* ≤ 0.3且-0.3 ≤ b* ≤ 0.3。 根據本發明,N之單電荷及多電荷離子之混合物較佳包含N+
、N2+
及N3+
。 根據本發明,有效降低玻璃基材之反射率且同時使反射中之色彩保持中性之加速電壓及離子劑量較佳地包含在以下範圍中: 表2
本發明亦係關於經離子植入之玻璃基材,其具有降低之反射率,其中N之單電荷及多電荷離子之混合物已根據本發明之方法經植入。 有利地,經離子植入之本發明之玻璃基材具有至多6.5%、較佳地至多6%、更佳地至多5.5%之反射率。其亦在反射中具有中性色彩,即-1 ≤ a* ≤ 1且-1 ≤ b* ≤ 1、較佳地-0.3 ≤ a* ≤ 0.3且-0.3 ≤ b* ≤ 0.3。 在本發明之較佳實施例中,植入本發明玻璃基材中之離子係N之單電荷及多電荷離子。 根據本發明之另一較佳實施例,N之單電荷及多電荷離子之混合物所包含N3+
之量小於N+
及N2+
各自之量。在本發明之更佳實施例中,N之單電荷及多電荷離子之混合物包含40%-70%之N+
、20%-40%之N2+
及2%-20%之N3+
。 有利地,離子之植入深度可包含在0.1 µm與1 µm之間、較佳地0.1 µm與0.5 µm之間。 本發明中所使用之玻璃基材通常係片材狀玻璃基材,其具有兩個相對主要表面。本發明之離子植入可在該等表面之一個或兩個上實施。本發明之離子植入可在玻璃基材之一部分表面或整個表面上實施。 在另一實施例中,本發明亦係關於納入本發明抗反射玻璃基材之窗用玻璃(glazing),無論其係單片式、層壓式或具有插入氣體層之多片式。 該等窗用玻璃可用作內部及外部建築窗用玻璃二者,及作為物體之保護玻璃(例如,面板、顯示視窗)、玻璃家具(例如,櫃檯、冷凍展示櫃等)、以及作為汽車窗用玻璃(例如,層壓式擋風玻璃)、鏡子、電腦之防眩光螢幕、顯示器及裝飾性玻璃。 納入本發明抗反射玻璃基材之窗用玻璃可具有令人關注的額外性質。因此,其可係具有安全功能之窗用玻璃,例如,層壓式窗用玻璃。其亦可係具有防盜、隔音、防火或抗菌功能之窗用玻璃。 窗用玻璃亦可以使得利用本發明方法在其一個面上處理之基材包含沈積於其另一面上之層堆疊之此一方式選擇。層堆疊可具有特定功能,例如遮陽或吸熱功能,或亦具有防紫外、抗靜電(例如,輕微導電、經摻雜金屬氧化物層)及低發射功能(例如,基於銀之層或經摻雜氧化錫層)。其亦可係具有防污性質之層(例如,極細TiO2
層)或具有防水功能之疏水有機層或具有抗凝功能之親水層。 層堆疊可係具有鏡功能之含銀塗層,且所有組態皆係可能的。因此,在具有鏡功能之單片式窗用玻璃之情形下,所關注的是本發明之抗反射玻璃基材之定位,其中經處理面作為面1 (即,在觀看者所定位之側上)及銀塗層在面2上(即,在鏡附接至牆之側上),由此本發明之抗反射堆疊防止反射影像之分裂。 在雙層窗用玻璃之情形下(其中,根據慣例,玻璃基材之面係自最外面開始編號),由此可使用經抗反射處理之面作為面1且面2上之其他功能層用於防紫外或遮陽及面3用於低發射層。在雙層窗用玻璃中,由此可具有至少一個抗反射面作為基材之一個面及提供附加功能之至少一個層或層堆疊。雙層窗用玻璃亦可具有若干經抗反射處理之面,尤其地至少在面2、3或4上。對於單片式窗用玻璃1,可沈積與抗反射面相關之抗靜電功能層。 基材亦可經歷表面處理、具體地酸蝕(磨砂),離子植入處理可在經蝕刻之面上或在相對面上實施。 基材或與其相關之彼等之一者亦可係經印刷、裝飾性玻璃類型或可經絲網製程印刷。 納入本發明抗反射玻璃基材之尤其令人關注的窗用玻璃係具有層壓結構之窗用玻璃,該層壓結構具有兩個玻璃基材且包含聚合物型組裝片材,該組裝片材在本發明之抗反射玻璃基材(其中經離子植入處理之表面背向聚合物組裝片材)與另一玻璃基材之間。聚合物組裝片材可來自聚乙烯醇縮丁醛(PVB)類型、聚乙酸乙烯酯(EVA)類型或聚環己烷(COP)類型。較佳地,另一玻璃基材係本發明之抗反射玻璃基材。 具體地具有兩個經熱處理(即,彎曲及/或回火)之基材的此組態使得可獲得汽車窗用玻璃且尤其具有極有利性質之擋風玻璃。標準要求汽車所具有之擋風玻璃在垂直入射中具有至少75%之高光傳輸。由於將經熱處理之抗反射玻璃基材納入習用擋風玻璃之層壓結構中,故窗用玻璃之光傳輸尤其經改良,使得其能量傳輸可藉由其他方式略有降低,同時仍然保持在光傳輸標準內。由此,可(例如)藉由玻璃基材之吸收作用改良擋風玻璃之遮陽效應。可使標準層壓式擋風玻璃之光反射值自8%達到小於5%。 本發明之玻璃基材可係任一厚度之玻璃片材,其具有經表示為玻璃總重量之重量%之以下組成範圍: SiO2
35% - 85%, Al2
O3
0% - 30%, P2
O5
0% - 20%, B2
O3
0% - 20%, Na2
O 0% - 25%, CaO 0% - 20%, MgO 0% - 20%, K2
O 0% - 20%,及 BaO 0% - 20%。 本發明之玻璃基材較佳地係選自以下各項中之玻璃片材:鈉鈣玻璃片材、硼矽酸鹽玻璃片材或鋁矽酸鹽玻璃片材。在尤佳實施例中,玻璃片材係透明玻璃片材。 本發明之玻璃基材較佳在經受離子植入之側不具有塗層。 本發明之玻璃基材可係在離子植入處理後將被切成其最終尺寸之大玻璃片材,或其可係已經切成其最終大小之玻璃片材。 有利地,本發明之玻璃基材可係浮製玻璃基材。本發明之離子植入方法可在浮製玻璃基材之空氣側及/或浮製玻璃基材之錫側上實施。較佳地,本發明之離子植入方法係在浮製玻璃基材之空氣側上實施。 在本發明之實施例中,玻璃基材可係先前經化學加強之玻璃基材。 光學性質係使用Hunterlab Ultrascan Pro分光光度計量測。 具體實施例之詳細說明 離子植入實例係使用用於生成單電荷及多電荷離子束之RCE離子源根據下表中所詳述之各參數製備。所使用離子源係來自Quertech Ingénierie S.A.之Hardion+ RCE離子源。 所有試樣具有10 × 10 cm2
之大小,且藉由使玻璃基材以介於20 mm/s與30 mm/s間之速度位移穿過離子束而在整個表面上經處理。 使正在處理之玻璃基材之區域之溫度保持在小於或等於玻璃基材之玻璃轉換溫度的溫度下。 對於所有實例,植入皆在真空室中在10-6
毫巴壓力下實施。 將N之離子植入4 mm規則透明鈉鈣玻璃及鋁矽酸鹽玻璃基材中。在利用本發明之離子植入方法植入前,玻璃基材之反射率係約8%。關鍵植入參數及光學量測值可在下表中發現。 表4
如自本發明之實例E1至E6可見,所選用於離子植入之關鍵參數(其中加速電壓A係包含在20 kV與25 kV之間且劑量D係包含在6 × 1016
個離子/cm2
與-5.00 × 1015
× A/kV + 2.00 × 1017
個離子/cm2
之間)一方面導致至多6.5%、至多6.0%或甚至至多5.5%之降低反射率,且另一方面導致該等實例之反射中之色彩為中性,即-1 ≤ a* ≤ 1且-1 ≤ b* ≤ 1。針對實例E3、E4及E5所選之關鍵植入參數產生極中性的反射中之色彩,即-0.3 ≤ a* ≤ 0.3且-0.3 ≤ b* ≤ 0.3。 此外,對本發明之實例E1至E6進行XPS量測並發現,植入之N離子的原子濃度在整個植入深度上低於8原子%。
Claims (14)
- 一種生產中性色彩之抗反射玻璃基材之方法,其包含以下操作: a) 提供N2 源氣體, b) 將該N2 源氣體離子化,以便形成N之單電荷離子及多電荷離子之混合物, c) 利用加速電壓使該N之單電荷離子及多電荷離子之混合物加速,以便形成單電荷離子及多電荷離子之束,其中該加速電壓A係包含在20 kV與25 kV之間且劑量D係包含在6 × 1016 個離子/cm2 與-5.00 × 1015 × A/kV + 2.00 × 1017 個離子/cm2 之間, d) 提供玻璃基材, e) 將該玻璃基材定位於該N之單電荷及多電荷離子束之軌跡中。
- 如請求項1之生產中性色彩之抗反射玻璃基材之方法,其中所提供之該玻璃基材具有經表示為該玻璃總重量之重量%之以下組成範圍: SiO2 35% - 85%, Al2 O3 0% - 30%, P2 O5 0% - 20%, B2 O3 0% - 20%, Na2 O 0% - 25%, CaO 0% - 20%, MgO 0% - 20%, K2 O 0% - 20%,及 BaO 0% - 20%。
- 如請求項2之生產中性色彩之抗反射玻璃基材之方法,其中該玻璃基材係選自鈉鈣玻璃片材、硼矽酸鹽玻璃片材或鋁矽酸鹽玻璃片材。
- 一種N之單電荷及多電荷離子之混合物使玻璃基材之反射率減小且同時使反射中之色彩保持中性之用途,該單電荷及多電荷離子之混合物係以有效降低該玻璃基材之反射率且同時使該反射中之色彩保持中性之離子劑量及加速電壓植入該玻璃基材中。
- 如請求項4之N之單電荷及多電荷離子之混合物使玻璃基材之反射率減小且同時使反射中之色彩保持中性之用途,其中該單電荷及多電荷離子之混合物係以有效使該玻璃基材之反射率降低至至多6.5%,且同時使該反射中之色彩保持中性(使得 -1 ≤ a* ≤ 1且-1 ≤ b* ≤ 1)之離子劑量及加速電壓植入該玻璃基材中。
- 如請求項5之N之單電荷及多電荷離子之混合物使玻璃基材之反射率減小且同時使反射中之色彩保持中性之用途,其中該單電荷及多電荷離子之混合物係以有效使該玻璃基材之反射率降低至至多6.5%且同時使該反射中之色彩保持中性(使得 -0.3 ≤ a* ≤ 0.3且-0.3 ≤ b* ≤ 0.3)之離子劑量及加速電壓植入該玻璃基材中。
- 如請求項4至6中任一項之N之單電荷及多電荷離子之混合物使玻璃基材之反射率減小且同時使反射中之色彩保持中性之用途,其中該加速電壓A係包含在20 kV與5 kV之間且該劑量D係包含在6 × 1016 個離子/cm2 與-5.00 × 1015 × A/kV + 2.00 × 1017 個離子/cm2 之間。
- 一種中性色彩之抗反射玻璃基材,其係藉由如請求項1至3中任一項之方法生產。
- 一種單片式窗用玻璃、層壓式窗用玻璃或具有插入氣體層之多片式窗用玻璃,其包含如請求項8之中性色彩之抗反射玻璃基材。
- 如請求項9之窗用玻璃,其進一步包含遮陽、吸熱、防紫外、抗靜電、低發射、加熱、防污、安全、防盜、隔音、防火、抗霧、防水、抗菌或鏡構件。
- 如請求項9或10中任一項之窗用玻璃,其中該抗反射玻璃基材係經磨砂、印刷或經絲網製程印刷。
- 如請求項9或10之窗用玻璃,其中該基材係經著色、回火、加強、彎曲、摺疊或紫外過濾。
- 如請求項9或10之窗用玻璃,其具有包含聚合物型組裝片材之層壓式結構,該組裝片材經插入於本發明之抗反射玻璃基材(其中經離子植入處理之表面背向該聚合物組裝片材)與另一玻璃基材之間。
- 如請求項13之窗用玻璃,其中該窗用玻璃係汽車擋風玻璃。
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EP (1) | EP3442922B1 (zh) |
JP (1) | JP6948344B2 (zh) |
KR (1) | KR102309419B1 (zh) |
CN (1) | CN109476535B (zh) |
BR (1) | BR112018070860A2 (zh) |
CA (1) | CA3019269A1 (zh) |
EA (1) | EA201892161A1 (zh) |
ES (1) | ES2883165T3 (zh) |
PL (1) | PL3442922T3 (zh) |
SG (1) | SG11201808096PA (zh) |
TW (1) | TW201808851A (zh) |
WO (1) | WO2017178170A1 (zh) |
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EP3146086B1 (en) * | 2014-05-23 | 2019-10-02 | Quertech | Single- and/or multi-charged gas ion beam treatment method for producing an anti-glare sapphire material |
JP6410906B1 (ja) * | 2017-09-26 | 2018-10-24 | デクセリアルズ株式会社 | 偏光素子及び光学機器 |
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FR1300336A (fr) | 1961-06-23 | 1962-08-03 | Carnaud & Forges | Perfectionnements à la fabrication dés emballages métalliques tels que boîtes de conserve |
JPH0323238A (ja) * | 1989-06-19 | 1991-01-31 | Nippon Sheet Glass Co Ltd | ガラス基材の表面改質法 |
CN100365161C (zh) * | 2004-12-01 | 2008-01-30 | 深圳国家863计划材料表面工程技术研究开发中心 | 单mevva离子源渗注镀复合处理工艺 |
JP2007227424A (ja) * | 2006-02-21 | 2007-09-06 | Sumco Corp | Simoxウェーハの製造方法 |
CN103898469A (zh) * | 2012-12-26 | 2014-07-02 | 核工业西南物理研究院 | 一种低温高负载状况下材料表面的无界面强化处理方法 |
FR3002240B1 (fr) * | 2013-02-15 | 2015-07-10 | Quertech Ingenierie | Procede de traitement par un faisceau d'ions pour produire des materiaux en verre antireflet durable |
FR3003857B1 (fr) * | 2013-03-28 | 2015-04-03 | Quertech | Procede de traitement par un faisceau d'ions pour produire des materiaux en verre superhydrophiles. |
CN107074641B (zh) | 2014-10-24 | 2020-08-07 | 旭硝子欧洲玻璃公司 | 离子注入方法和离子注入的玻璃基板 |
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- 2017-03-13 CA CA3019269A patent/CA3019269A1/en not_active Abandoned
- 2017-03-13 CN CN201780022706.XA patent/CN109476535B/zh not_active Expired - Fee Related
- 2017-03-13 WO PCT/EP2017/055853 patent/WO2017178170A1/en active Application Filing
- 2017-03-13 ES ES17709997T patent/ES2883165T3/es active Active
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- 2017-03-13 US US16/092,395 patent/US11339089B2/en active Active
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US20200325067A1 (en) | 2020-10-15 |
EP3442922B1 (en) | 2021-06-02 |
KR20190116904A (ko) | 2019-10-15 |
CA3019269A1 (en) | 2017-10-19 |
KR102309419B1 (ko) | 2021-10-07 |
JP6948344B2 (ja) | 2021-10-13 |
EA201892161A1 (ru) | 2019-04-30 |
CN109476535A (zh) | 2019-03-15 |
EP3442922A1 (en) | 2019-02-20 |
WO2017178170A1 (en) | 2017-10-19 |
ES2883165T3 (es) | 2021-12-07 |
BR112018070860A2 (pt) | 2019-04-24 |
PL3442922T3 (pl) | 2022-01-03 |
CN109476535B (zh) | 2022-01-11 |
US11339089B2 (en) | 2022-05-24 |
SG11201808096PA (en) | 2018-10-30 |
JP2019513676A (ja) | 2019-05-30 |
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