TW201932304A - Water-vapor barrier laminate, water-vapor barrier structure - Google Patents
Water-vapor barrier laminate, water-vapor barrier structure Download PDFInfo
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本發明是有關於一種積層體，特別是指一種水氣阻障積層體及包含其的阻水氣用結構體。The present invention relates to a laminate, and more particularly to a water vapor barrier laminate and a water blocking gas structure comprising the same.
水氣阻障封裝的技術廣泛應用於食品、藥物保存及電子產品等，根據世界封裝組織(World Packaging Organization, WPO)近年來統計，全世界封裝費用已高達5.6 兆美金。隨著電子產品日新月異，厚重的玻璃基板逐漸被輕、薄、可撓曲且可塑性高的軟性塑膠基板取代，軟性電子裝置如電子紙、染料敏化太陽能電池(DSSCs)、有機太陽能電池(OPV)及有機發光二極體(OLED)等相關發展勢在必行。然而，此類產品卻存在可靠性疑慮，有機太陽能電池或是有機發光二極體的元件內部設置著高敏感的有機材料以及易氧化的陰極金屬，空氣中的水氣若透過軟性塑膠基板滲透至元件內部將導致上述材料的劣化及老化。因此，為延長產品使用壽命，需使用水氣阻障膜阻擋水氣穿透至元件內部，以防止元件內部的有機材料劣化及陰極金屬老化。此外，水氣阻障膜在商業化應用上還需具備高透光等性質。Water-blocking packaging technology is widely used in food, drug storage and electronic products. According to recent statistics from the World Packaging Organization (WPO), packaging costs worldwide have reached 5.6 trillion US dollars. As electronic products change with each passing day, heavy glass substrates are gradually replaced by soft, thin, flexible and highly flexible soft plastic substrates, such as electronic paper, dye-sensitized solar cells (DSSCs), and organic solar cells (OPV). And related developments such as organic light-emitting diodes (OLEDs) are imperative. However, such products have reliability concerns. The components of organic solar cells or organic light-emitting diodes are internally provided with highly sensitive organic materials and oxidizable cathode metals. The moisture in the air penetrates through the flexible plastic substrate. The inside of the component will cause deterioration and aging of the above materials. Therefore, in order to prolong the service life of the product, a water vapor barrier film is used to block the penetration of moisture into the interior of the component to prevent deterioration of the organic material inside the component and aging of the cathode metal. In addition, the water vapor barrier film needs to have high light transmission properties in commercial applications.
因此，本發明之第一目的，即在提供一種具有較佳的水氣阻隔效果以及較高的光穿透率的阻水氣用結構體。Accordingly, a first object of the present invention is to provide a water blocking gas structure having a preferred water vapor barrier effect and a high light transmittance.
於是，本發明阻水氣用結構體，包含： 一個可撓性基板；以及 一個水氣阻障積層體，包括至少一個有機-無機複合層單元，該有機-無機複合層單元含有： 一個有機層，設置在該可撓性基板的表面並含有交錯堆疊設置的多層的聚乙烯亞胺膜以及多層的聚丙烯酸膜，其中，每一聚乙烯亞胺膜的pH值範圍為1至8，每一聚丙烯酸膜的pH值範圍為6至14，及 一個無機層，設置於該有機層之相反於該可撓性基板的表面，且為一種選自於氧化鋁、鋅錫氧化物或上述任意組合的金屬氧化物。Accordingly, the water blocking gas structure of the present invention comprises: a flexible substrate; and a water vapor barrier laminate comprising at least one organic-inorganic composite layer unit, the organic-inorganic composite layer unit comprising: an organic layer a polyethyleneimine film disposed on the surface of the flexible substrate and comprising a plurality of layers of polyethyleneimine film and a plurality of layers of polyacrylic acid film, wherein each polyethyleneimine film has a pH ranging from 1 to 8, each The polyacrylic film has a pH in the range of 6 to 14, and an inorganic layer disposed on the surface of the organic layer opposite to the flexible substrate, and is selected from the group consisting of alumina, zinc tin oxide, or any combination thereof. Metal oxides.
因此，本發明之第二目的，即在提供一種具有較佳的水氣阻隔效果以及較高的光穿透率的水氣阻障積層體。Accordingly, a second object of the present invention is to provide a water vapor barrier laminate having a preferred moisture barrier effect and a high light transmittance.
於是，本發明水氣阻障積層體，包含： 至少一個有機-無機複合層單元，該有機-無機複合層單元包括： 一個有機層，含有交錯堆疊設置的多層的聚乙烯亞胺膜以及多層的聚丙烯酸膜，其中，該等聚乙烯亞胺膜的pH值範圍為1至8，該等聚丙烯酸膜的pH值範圍為6至14，及 一個無機層，設置於該有機層的表面且為一種選自於氧化鋁、鋅錫氧化物或上述任意組合的金屬氧化物。Therefore, the water vapor barrier laminate of the present invention comprises: at least one organic-inorganic composite layer unit, the organic-inorganic composite layer unit comprising: an organic layer comprising a plurality of layers of polyethyleneimine film arranged in a staggered stack and a plurality of layers a polyacrylic film, wherein the polyethyleneimine film has a pH in the range of 1 to 8, the polyacrylic film has a pH in the range of 6 to 14, and an inorganic layer is disposed on the surface of the organic layer and is A metal oxide selected from the group consisting of alumina, zinc tin oxide, or any combination thereof.
本發明之功效在於：該阻水氣用結構體透過該水氣阻障積層體的該有機層及該無機層互相搭配，且該有機層含有交錯堆疊設置的多層聚乙烯亞胺膜以及多層聚丙烯酸膜，能使該阻水氣用結構體及該水氣阻障積層體具有較佳的水氣阻隔效果，以及較高的光穿透率。The effect of the present invention is that the water-blocking gas structure penetrates the organic layer of the water vapor barrier laminate and the inorganic layer, and the organic layer contains a plurality of layers of polyethyleneimine film and multi-layer polymerization The acrylic film enables the water-blocking gas structure and the water-gas barrier laminate to have a better water vapor barrier effect and a high light transmittance.
以下就本發明內容進行詳細說明：The details of the present invention are described below:
較佳地，該阻水氣用結構體的其中一實施態樣，是該水氣阻障積層體包含二個堆疊設置在該可撓性基板的表面的有機-無機複合層單元，且該等有機-無機複合層單元的該等有機層與該等無機層是交錯地堆疊設置。Preferably, in one embodiment of the water-blocking gas structure, the moisture barrier layer comprises two organic-inorganic composite layer units stacked on a surface of the flexible substrate, and the same The organic layers of the organic-inorganic composite layer unit are stacked in a staggered manner with the inorganic layers.
較佳地，該阻水氣用結構體的又一實施態樣，是該水氣阻障積層體包含三個堆疊設置在該可撓性基板的表面的有機-無機複合層單元，且該等有機-無機複合層單元的該等有機層與該等無機層是交錯地堆疊設置。Preferably, in another embodiment of the water-blocking gas structure, the moisture barrier layer comprises three organic-inorganic composite layer units stacked on a surface of the flexible substrate, and the same The organic layers of the organic-inorganic composite layer unit are stacked in a staggered manner with the inorganic layers.
較佳地，該阻水氣用結構體的另一實施態樣，是該水氣阻障積層體包含五個堆疊設置在該可撓性基板的表面的有機-無機複合層單元，且該等有機-無機複合層單元的該等有機層與該等無機層是交錯地堆疊設置。Preferably, in another embodiment of the water-blocking gas structure, the moisture barrier layer comprises five organic-inorganic composite layer units stacked on a surface of the flexible substrate, and the same The organic layers of the organic-inorganic composite layer unit are stacked in a staggered manner with the inorganic layers.
較佳地，該阻水氣用結構體中，與該可撓性基板接觸的為聚乙烯亞胺膜，與無機層接觸的為聚丙烯酸膜。Preferably, in the water-blocking gas structure, a polyethyleneimine film is in contact with the flexible substrate, and a polyacrylic film is in contact with the inorganic layer.
較佳地，該水氣阻障積層體的其中一實施態樣，是該水氣阻障積層體包含二個堆疊設置的有機-無機複合層單元，且該等有機-無機複合層單元中的該等有機層與該等無機層是交錯地堆疊設置。Preferably, in one embodiment of the water vapor barrier laminate, the water vapor barrier laminate comprises two stacked organic-inorganic composite layer units, and the organic-inorganic composite layer unit The organic layers are stacked in a staggered manner with the inorganic layers.
較佳地，該水氣阻障積層體的又一實施態樣，是該水氣阻障積層體包含三個堆疊設置的有機-無機複合層單元，且該等有機-無機複合層單元中的該等有機層與該等無機層是交錯地堆疊設置。Preferably, in another embodiment of the water vapor barrier laminate, the water vapor barrier laminate comprises three stacked organic-inorganic composite layer units, and the organic-inorganic composite layer unit The organic layers are stacked in a staggered manner with the inorganic layers.
較佳地，該水氣阻障積層體的另一實施態樣，是該水氣阻障積層體包含五個堆疊設置的有機-無機複合層單元，且該等有機-無機複合層單元中的該等有機層與該等無機層是交錯地堆疊設置。Preferably, in another embodiment of the water vapor barrier laminate, the water vapor barrier laminate comprises five stacked organic-inorganic composite layer units, and the organic-inorganic composite layer unit The organic layers are stacked in a staggered manner with the inorganic layers.
較佳地，該水氣阻障積層體中，與該可撓性基板接觸的為聚乙烯亞胺膜，與無機層接觸的為聚丙烯酸膜。Preferably, in the water vapor barrier laminate, a polyethyleneimine film is in contact with the flexible substrate, and a polyacrylic film is in contact with the inorganic layer.
該可撓性基板的材質沒有特別限制，例如但不限於：聚酯樹脂(polyester resin)、聚丙烯酸酯樹脂(polyacrylate resin)、聚烯烴樹脂(polyolefin resin)、聚碳酸酯樹脂(polycarbonate resin)、聚氯乙烯、聚醯亞胺樹脂(polyimide resin)或聚乳酸(polylactic acid)等。聚酯樹脂例如但不限於：聚對苯二甲酸乙二酯(polyethylene terephthalate，PET)，或聚萘二甲酸乙二酯(polyethylene naphthalate，PEN)等。聚丙烯酸酯樹脂例如但不限於：聚甲基丙烯酸甲酯(polymethyl methacrylate，PMMA)等。該聚烯烴樹脂例如但不限於：聚乙烯或聚丙烯等。可選擇性地對該可撓性基板的表面進行改質處理，改質處理的具體方式例如但不限於以氧氣電漿對該可撓性基板的表面進行改質。該可撓性基板的厚度沒有特別限制，例如但不限於50至200 mM。The material of the flexible substrate is not particularly limited, and is not limited to, for example, a polyester resin, a polyacrylate resin, a polyolefin resin, a polycarbonate resin, or the like. Polyvinyl chloride, polyimide resin or polylactic acid. The polyester resin is, for example but not limited to, polyethylene terephthalate (PET), or polyethylene naphthalate (PEN). The polyacrylate resin is, for example but not limited to, polymethyl methacrylate (PMMA) or the like. The polyolefin resin is, for example but not limited to, polyethylene or polypropylene. The surface of the flexible substrate can be selectively modified, and the specific modification method is, for example, but not limited to, modifying the surface of the flexible substrate with oxygen plasma. The thickness of the flexible substrate is not particularly limited, and is, for example, but not limited to, 50 to 200 mM.
該有機-無機複合層單元的該有機層能提昇該可撓性基板的表面平坦程度，進而使該阻水氣用結構體及該水氣阻障積層體具有較佳的水氣阻隔效果及良好的光穿透率。該有機層含有交錯堆疊設置的多層的聚乙烯亞胺膜以及多層的聚丙烯酸膜，其中，聚乙烯亞胺膜的pH值範圍為1至8以使聚乙烯亞胺膜陽離子化，聚丙烯酸膜的pH值範圍為6至14以使聚丙烯酸膜陰離子化，並透過交錯設置聚乙烯亞胺膜與聚丙烯酸膜，陽離子化的聚乙烯亞胺膜與陰子化的聚丙烯酸膜能夠藉由陰陽離子的相吸作用而成膜。且相較於僅堆疊聚乙烯亞胺膜或僅堆疊聚丙烯酸膜，採用交錯地堆疊該等聚乙烯亞胺膜與該等聚丙烯酸膜的結構設計，能使該有機層有效改善該可撓性基板的表面平坦程度。較佳地，為使該阻水氣用結構體及該水氣阻障積層體具有更佳的水氣阻隔效果，該有機層中含有交錯堆疊設置的十層的聚乙烯亞胺膜以及十層的聚丙烯酸膜。要說明的是，該聚乙烯亞胺膜及該聚丙烯酸膜的數目也可以皆大於十層，而不會損害水氣阻隔效果及光穿透率，但考量到成本與水氣阻隔效果之間的平衡，該聚乙烯亞胺膜的數目為十層以及聚丙烯酸膜的數目為十層。其中，每一聚乙烯亞胺膜的厚度範圍例如但不限於1至5 nm。每一聚丙烯酸膜的厚度範圍例如但不限於1至5 nm。The organic layer of the organic-inorganic composite layer unit can improve the surface flatness of the flexible substrate, thereby further improving the water vapor barrier effect and the water vapor barrier structure and the water vapor barrier laminate. Light penetration rate. The organic layer comprises a multi-layered polyethyleneimine film arranged in a staggered stack and a multilayer polyacrylic film, wherein the polyethyleneimine film has a pH in the range of 1 to 8 to cationize the polyethyleneimine film, and the polyacrylic film The pH range is 6 to 14 to anionize the polyacrylic acid film, and the polyethyleneimine film and the polyacrylic acid film are interlaced, and the cationized polyethyleneimine film and the negatively colored polyacrylic acid film can be used for yin and yang. The phase attraction of ions forms a film. And by stacking the polyethyleneimine films and the structural design of the polyacrylic acid films in a staggered manner compared to stacking only the polyethyleneimine film or only stacking the polyacrylic acid film, the organic layer can effectively improve the flexibility. The surface of the substrate is flat. Preferably, in order to make the water-blocking gas structure and the water-gas barrier layered body have better water vapor barrier effect, the organic layer contains ten layers of polyethyleneimine film and ten layers which are arranged in a staggered stack. Polyacrylic film. It should be noted that the number of the polyethyleneimine film and the polyacrylic acid film may also be greater than ten layers without impairing the moisture barrier effect and the light transmittance, but considering the cost and the moisture barrier effect. The balance is that the number of the polyethyleneimine films is ten layers and the number of polyacrylic acid films is ten layers. Wherein, the thickness of each polyethyleneimine film ranges, for example but is not limited to 1 to 5 nm. The thickness of each polyacrylic film is, for example, but not limited to, 1 to 5 nm.
其中，該聚乙烯亞胺膜是由聚乙烯亞胺溶液所形成，該聚乙烯亞胺溶液的濃度範圍例如但不限於0.1至5wt%，該聚乙烯亞胺溶液的pH值範圍例如但不限於1至8。該聚乙烯亞胺溶液的製備方式沒有特別限制，可採用現有的聚乙烯亞胺溶液的製備方式，例如可使用鹽酸調整該聚乙烯亞胺溶液的pH值。Wherein, the polyethyleneimine film is formed by a polyethyleneimine solution, the concentration of the polyethyleneimine solution is, for example, but not limited to, 0.1 to 5 wt%, and the pH range of the polyethyleneimine solution is, for example but not limited to, 1 to 8. The preparation method of the polyethyleneimine solution is not particularly limited, and a preparation method of the existing polyethyleneimine solution may be employed. For example, the pH of the polyethyleneimine solution may be adjusted using hydrochloric acid.
該聚丙烯酸膜是由聚丙烯酸溶液所形成，該聚丙烯酸溶液的濃度範圍例如但不限於0.01至0.5wt%，該聚丙烯酸溶液的pH值範圍例如但不限於6至14。該聚丙烯酸溶液的製備方式沒有特別限制，可採用現有的聚丙烯酸溶液的製備方式，例如可使用氫氧化鈉調整該聚丙烯酸溶液的pH值。The polyacrylic acid film is formed of a polyacrylic acid solution having a concentration ranging, for example, but not limited to, 0.01 to 0.5% by weight, and the pH of the polyacrylic acid solution is, for example but not limited to, 6 to 14. The preparation method of the polyacrylic acid solution is not particularly limited, and a preparation method of the existing polyacrylic acid solution may be employed. For example, the pH of the polyacrylic acid solution may be adjusted using sodium hydroxide.
在該有機層中，該等聚丙烯酸膜可為相同或不同，該等聚乙烯亞胺膜可為相同或不同。In the organic layer, the polyacrylic acid films may be the same or different, and the polyethyleneimine films may be the same or different.
該無機層的材質為選自於氧化鋁、鋅錫氧化物或上述任意組合的金屬氧化物。該無機層的厚度範圍例如但不限於為50至100 nm。形成該無機層的方式例如但不限於使用該金屬氧化物對應的靶材進行濺鍍沉積，進行濺鍍的方式例如但不限於直流式磁控濺鍍或射頻式磁控濺鍍。The material of the inorganic layer is a metal oxide selected from the group consisting of alumina, zinc tin oxide, or any combination thereof. The thickness of the inorganic layer is, for example but not limited to, 50 to 100 nm. The manner of forming the inorganic layer is, for example but not limited to, sputtering deposition using a target corresponding to the metal oxide, and sputtering is performed, for example, but not limited to, direct current magnetron sputtering or radio frequency magnetron sputtering.
且當該水氣阻障積層體包含二個以上的有機-無機複合層單元時，該等有機層可為相同或不同，該等無機層可為相同或不同。And when the water vapor barrier laminate comprises two or more organic-inorganic composite layer units, the organic layers may be the same or different, and the inorganic layers may be the same or different.
本發明將就以下實施例來作進一步說明，但應瞭解的是，該實施例僅為例示說明之用，而不應被解釋為本發明實施之限制。The present invention will be further illustrated by the following examples, but it should be understood that this embodiment is intended to be illustrative only and not to be construed as limiting.
在本發明被詳細描述之前，應當注意在以下的說明內容中，類似的元件是以相同的編號來表示。Before the present invention is described in detail, it should be noted that in the following description, similar elements are denoted by the same reference numerals.
參閱圖1及圖2，本發明阻水氣用結構體的第一實施例，包含一個可撓性基板1，及一個設置在該可撓性基板1表面的水氣阻障積層體2。該水氣阻障積層體2包括一個有機-無機複合層單元21，且該有機-無機複合層單元21含有一個有機層22及一個無機層23。其中，該有機層22設置在該可撓性基板1的表面並含有交錯堆疊設置的十層的聚乙烯亞胺膜221及十層的聚丙烯酸膜222(參閱圖2)。該無機層23設置於該有機層22之相反於該可撓性基板1的表面。且因該可撓性基板1的表面是帶負電，所以在該有機層22中，與該可撓性基板1的表面接觸的為陽離子化的聚乙烯亞胺膜221。以及與該無機層23接觸的為陰離子化的聚丙烯酸膜222。Referring to Figures 1 and 2, a first embodiment of the water-blocking gas structure of the present invention comprises a flexible substrate 1 and a water vapor barrier laminate 2 disposed on the surface of the flexible substrate 1. The water vapor barrier laminate 2 includes an organic-inorganic composite layer unit 21, and the organic-inorganic composite layer unit 21 contains an organic layer 22 and an inorganic layer 23. The organic layer 22 is disposed on the surface of the flexible substrate 1 and includes ten layers of polyethyleneimine film 221 and ten layers of polyacryl film 222 (see FIG. 2). The inorganic layer 23 is disposed on the surface of the organic layer 22 opposite to the flexible substrate 1. Further, since the surface of the flexible substrate 1 is negatively charged, a cationized polyethyleneimine film 221 is in contact with the surface of the flexible substrate 1 in the organic layer 22. And an anionized polyacrylic film 222 that is in contact with the inorganic layer 23.
在該第一實施例中，該可撓性基板1的材質為聚對苯二甲酸乙二酯(PET)或聚萘二甲酸乙二酯(PEN)。該無機層的材質為氧化鋁(Al2 O3 )或鋅錫氧化物(ZTO)。In the first embodiment, the flexible substrate 1 is made of polyethylene terephthalate (PET) or polyethylene naphthalate (PEN). The material of the inorganic layer is alumina (Al 2 O 3 ) or zinc tin oxide (ZTO).
以下先以該可撓性基板1的材質為聚對苯二甲酸乙二酯(PET)，以及該無機層的材質為氧化鋁(Al2 O3 )的態樣詳細說明製備該第一實施例的方式：Hereinafter, the first embodiment is prepared by using the material of the flexible substrate 1 as polyethylene terephthalate (PET) and the material of the inorganic layer being alumina (Al 2 O 3 ). The way:
[步驟1] 該可撓性基板1的前處理：將一個經過底漆(primer)處理的聚對苯二甲酸乙二酯膜(厚度為1251μm)先以去離子水沖洗，然後，將該聚對苯二甲酸乙二酯膜浸泡在乙醇中並以超音波震盪清洗3分鐘。接著，將清洗過後的該聚對苯二甲酸乙二酯膜置於烘箱中以80°C烘乾。將烘乾的該聚對苯二甲酸乙二酯膜以氧氣電漿進行表面改質(電漿功率為50W，工作壓力為100 mtorr，電漿處理的時間為2分鐘)，得到該可撓性基板1。[Step 1] Pretreatment of the flexible substrate 1 : A primer-treated polyethylene terephthalate film (thickness: 1251 μm) was first rinsed with deionized water, and then the polymerization was carried out. The ethylene terephthalate film was immersed in ethanol and washed with ultrasonic shock for 3 minutes. Next, the washed polyethylene terephthalate film was placed in an oven and dried at 80 °C. The dried polyethylene terephthalate film is surface-modified with oxygen plasma (plasma power is 50 W, working pressure is 100 mtorr, plasma treatment time is 2 minutes), and the flexibility is obtained. Substrate 1.
[步驟2]該有機層22的製備：使用一浸塗機(dip coater)將步驟1得到的該可撓性基板1以下降速率50 mm/min緩慢地浸入濃度為2 wt%且pH值為7的聚乙烯亞胺溶液中後停留1分鐘，然後，以拉升速率20 mm/min將該可撓性基板1從聚乙烯亞胺溶液中拉起，以在該可撓性基板1的表面上形成第一層的聚乙烯亞胺膜221。接著，將該可撓性基板1以下降速率50 mm/min緩慢地浸入濃度為0.2 wt%且pH值為7的聚丙烯酸溶液中後停留1分鐘，然後，以拉升速率25 mm/min將該可撓性基板1從聚丙烯酸溶液中拉起，以在該第一層的聚乙烯亞胺膜221上形成第一層的聚丙烯酸膜222。重複地進行上述步驟，以在該可撓性基板1上形成交錯堆疊設置的十層的聚乙烯亞胺膜221及十層的聚丙烯酸膜222的該有機層22。最後，以去離子水沖洗該有機層2，2再用氮氣吹乾該有機層22。其中，該有機層22中，每一聚乙烯亞胺膜221的pH值為7以及厚度為100nm，每一聚丙烯酸膜222的pH值為7以及厚度為100nm。[Step 2] Preparation of the organic layer 22: The flexible substrate 1 obtained in the step 1 was slowly immersed at a dropping rate of 50 mm/min at a concentration of 2 wt% and a pH value using a dip coater. After staying in the polyethyleneimine solution of 7 for 1 minute, the flexible substrate 1 was pulled up from the polyethyleneimine solution at a pulling rate of 20 mm/min to be on the surface of the flexible substrate 1. A first layer of polyethyleneimine film 221 is formed thereon. Next, the flexible substrate 1 was slowly immersed in a polyacrylic acid solution having a concentration of 0.2 wt% and a pH of 7 at a dropping rate of 50 mm/min, and then left for 1 minute, and then, at a pulling rate of 25 mm/min. The flexible substrate 1 is pulled up from the polyacrylic acid solution to form a first layer of polyacrylic film 222 on the first layer of polyethyleneimine film 221. The above steps are repeatedly performed to form the organic layer 22 of the ten-layer polyethyleneimine film 221 and the ten-layer polyacryl film 222 which are alternately stacked on the flexible substrate 1. Finally, the organic layer 2 was rinsed with deionized water, and the organic layer 22 was again dried with nitrogen. In the organic layer 22, each of the polyethyleneimine films 221 has a pH of 7 and a thickness of 100 nm, and each polyacrylic acid film 222 has a pH of 7 and a thickness of 100 nm.
[步驟3]該無機層23(Al2 O3 )的製備：使用直流式磁控濺鍍設備(DC magnetron sputtering system，廠商為高敦股份有限公司，型號為R-24K08- SPUTTERING)在該有機層22上形成該無機層23(Al2 O3 )。其中，濺鍍靶材為氧化鋁(廠商為凱達森實業有限公司，純度為99.9%，尺寸為直徑 2吋，厚度為3 mm)，電源器為射頻電源器(RF power)，濺鍍時的背景壓力為5.0×10-6 Torr，工作壓力1×10-3 Torr，功率為150W，該無機層23(Al2 O3 )的厚度為100 nm。[Step 3] Preparation of the inorganic layer 23 (Al 2 O 3 ): using a DC magnetron sputtering system (manufactured by Gao Dun Co., Ltd., model R-24K08-SPUTTERING) in the organic The inorganic layer 23 (Al 2 O 3 ) is formed on the layer 22. Among them, the sputtering target is alumina (the manufacturer is Kaidasen Industrial Co., Ltd., the purity is 99.9%, the size is 2吋, the thickness is 3 mm), the power supply is RF power, during sputtering The background pressure was 5.0 × 10 -6 Torr, the working pressure was 1 × 10 -3 Torr, the power was 150 W, and the thickness of the inorganic layer 23 (Al 2 O 3 ) was 100 nm.
當該可撓性基板1的材質為聚萘二甲酸乙二酯(PEN)，以及該無機層23的材質為鋅錫氧化物(ZTO)的態樣時，基本上是依照上述的方式製備該第一實施例，差別在於將該可撓性基板1的材質換成為聚萘二甲酸乙二酯，以及改變該無機層23的製備方式。其中，該無機層23(ZTO)的製備方式說明如下：When the material of the flexible substrate 1 is polyethylene naphthalate (PEN), and the material of the inorganic layer 23 is zinc tin oxide (ZTO), the preparation is basically performed according to the above manner. The first embodiment differs in that the material of the flexible substrate 1 is changed to polyethylene naphthalate, and the manner of preparation of the inorganic layer 23 is changed. The preparation method of the inorganic layer 23 (ZTO) is as follows:
[步驟3]該無機層23(ZTO)的製備：使用直流式磁控濺鍍設備(DC magnetron sputtering system，廠商為高敦股份有限公司，型號為R-24K08- SPUTTERING)在該有機層22上形成該無機層23(ZTO)。其中，濺鍍靶材為鋅錫靶材(廠商為凱達森實業有限公司，純度為99.99%，尺寸為直徑 2吋，厚度為3 mm)，電源器為直流電源器(RF power)，濺鍍時的背景壓力為5.0×10-6 Torr，工作壓力1×10-3 Torr，功率為30W，該無機層23(ZTO)的厚度為100 nm。[Step 3] Preparation of the inorganic layer 23 (ZTO): On the organic layer 22, a DC magnetron sputtering system (manufactured by Gaodun Co., Ltd., model R-24K08-SPUTTERING) was used. This inorganic layer 23 (ZTO) is formed. Among them, the sputtering target is a zinc-tin target (the manufacturer is Kadison Industrial Co., Ltd., the purity is 99.99%, the size is 2吋, the thickness is 3 mm), and the power supply is DC power, splashing. The background pressure at the time of plating was 5.0 × 10 -6 Torr, the working pressure was 1 × 10 -3 Torr, the power was 30 W, and the thickness of the inorganic layer 23 (ZTO) was 100 nm.
參閱圖3，本發明阻水氣用結構體的第二實施例，與該第一實施例不同之處在於，該水氣阻障積層體包含二個堆疊設置在該可撓性基板1表面的有機-無機複合層單元2，且該等有機-無機複合層單元2的該等有機層22與該等無機層23是交錯地堆疊設置。Referring to FIG. 3, a second embodiment of the water-blocking gas structure of the present invention is different from the first embodiment in that the water vapor barrier laminate comprises two stacked layers disposed on the surface of the flexible substrate 1. The organic-inorganic composite layer unit 2, and the organic layers 22 of the organic-inorganic composite layer units 2 and the inorganic layers 23 are alternately stacked.
參閱圖4，本發明阻水氣用結構體的第三實施例，與該第一實施例不同之處在於，該水氣阻障積層體包含三個堆疊設置在該可撓性基板1的表面的有機-無機複合層單元2，且該等有機-無機複合層單元2的該等有機層22與該等無機層23是交錯地堆疊設置。Referring to FIG. 4, a third embodiment of the water blocking gas structure of the present invention is different from the first embodiment in that the water vapor barrier laminate comprises three stacked surfaces disposed on the flexible substrate 1. The organic-inorganic composite layer unit 2, and the organic layers 22 of the organic-inorganic composite layer unit 2 and the inorganic layers 23 are alternately stacked.
參閱圖5，本發明阻水氣用結構體的第四實施例，與該第一實施例不同之處在於，該水氣阻障積層體包含五個堆疊設置在該可撓性基板1的表面的有機-無機複合層單元2，且該等有機-無機複合層單元2的該等有機層22與該等無機層23是交錯地堆疊設置。Referring to FIG. 5, a fourth embodiment of the water blocking gas structure of the present invention is different from the first embodiment in that the water vapor barrier laminate comprises five stacked surfaces disposed on the flexible substrate 1. The organic-inorganic composite layer unit 2, and the organic layers 22 of the organic-inorganic composite layer unit 2 and the inorganic layers 23 are alternately stacked.
上述第二、第三及第四實施例中各層的材質及製備方式是與第一實施例中的材質及製備方式相同，於此不再贅述。The materials and preparation methods of the layers in the second, third and fourth embodiments are the same as those in the first embodiment, and will not be described again.
依據以下所述的性質評價方式量測上述各實施例的水氣阻隔效果以及穿透率，結果整理如表1。The water vapor barrier effect and the penetration rate of the above respective examples were measured in accordance with the property evaluation methods described below, and the results are summarized in Table 1.
1.水氣透過率 (Water Vapor Transmission Rate，WVTR)1. Water Vapor Transmission Rate (WVTR)
將待測的阻水氣用結構體置於水氣滲透量測儀(廠商型號為AQUATRAN® Model 2 G)的樣品槽中。測量時在樣品槽的一側利用溼度計(為該水氣滲透量測儀內建)控制濕度並且通入氮氣，當氮氣攜帶水氣滲透過待測的阻水氣用結構體到達另一側時，會進入庫侖電量五氧化二磷傳感器以偵測滲透水氣的含量，藉此分析待測的阻水氣用結構體的水氣透過率。其中，量測的條件為：溫度為37.8℃，相對溼度為90%，樣品槽流量設定為20 sccm。The structure of the water-blocking gas to be tested is placed in a sample tank of a moisture gas permeability meter (manufacturer model AQUATRAN ® Model 2 G). During the measurement, the humidity is controlled on one side of the sample tank (for the built-in moisture meter) to control the humidity and nitrogen is introduced. When the nitrogen gas carries the water vapor permeating through the structure of the water-blocking gas to be tested, it reaches the other side. At the time, the Coulomb pentoxide pentoxide sensor is detected to detect the osmotic water content, thereby analyzing the water vapor transmission rate of the water blocking gas structure to be tested. Among them, the measurement conditions were as follows: the temperature was 37.8 ° C, the relative humidity was 90%, and the sample tank flow rate was set to 20 sccm.
2.可見光穿透率(transmittance，T%)2. Visible light transmittance (transmittance, T%)
以 UV-VIS光譜儀(廠商型號為Agilent Cary 5000) 測量待測的阻水氣用結構體的可見光穿透度。測量方式詳述如下：先將UV-VIS光譜儀進行全光校正，再將待測的阻水氣用結構體置於載具後放入UV-VIS光譜儀的測量腔體。其中，量測的條件為：波長 450至750nm。The visible light transmittance of the water-blocking gas structure to be tested was measured by a UV-VIS spectrometer (manufacturer model Agilent Cary 5000). The measurement method is detailed as follows: First, the UV-VIS spectrometer is subjected to all-optical calibration, and then the structure for the water-blocking gas to be tested is placed in the measuring device and placed in the measuring chamber of the UV-VIS spectrometer. Among them, the measurement conditions are: a wavelength of 450 to 750 nm.
表1
表2
由表1及表2的結果證明，相較於對照例，第一實施例至第四阻水氣用結構體具有較佳的水氣阻隔效果以及較高的可見光穿透率。From the results of Tables 1 and 2, it was confirmed that the first to fourth water-blocking gas structures have a better water vapor barrier effect and a higher visible light transmittance than the comparative examples.
綜上所述，本發明阻水氣用結構體透過該水氣阻障積層體中的該有機層及該無機層互相搭配，且該有機層含有交錯堆疊設置的多層聚乙烯亞胺膜以及多層聚丙烯酸膜，能使該阻水氣用結構體及該水氣阻障積層體具有優異的水氣阻隔效果，以及高的光穿透率，故確實能達成本發明之目的。In summary, the water-blocking gas structure of the present invention is permeable to the organic layer and the inorganic layer in the water-vapor barrier laminate, and the organic layer comprises a plurality of layers of polyethyleneimine film and a plurality of layers arranged in a staggered stack. The polyacrylic acid film can provide the water vapor barrier structure and the water vapor barrier laminate with excellent water vapor barrier effect and high light transmittance, so that the object of the present invention can be achieved.
惟以上所述者，僅為本發明之實施例而已，當不能以此限定本發明實施之範圍，凡是依本發明申請專利範圍及專利說明書內容所作之簡單的等效變化與修飾，皆仍屬本發明專利涵蓋之範圍內。However, the above is only the embodiment of the present invention, and the scope of the invention is not limited thereto, and all the equivalent equivalent changes and modifications according to the scope of the patent application and the patent specification of the present invention are still The scope of the invention is covered.
1‧‧‧可撓性基板1‧‧‧Flexible substrate
2‧‧‧水氣阻障積層體2‧‧‧Water and gas barrier laminate
21‧‧‧有機-無機複合層單元21‧‧‧Organic-inorganic composite layer unit
22‧‧‧有機層22‧‧‧Organic layer
221‧‧‧聚乙烯亞胺膜221‧‧‧polyethyleneimine film
222‧‧‧聚丙烯酸膜222‧‧‧ polyacrylic film
23‧‧‧無機層23‧‧‧Inorganic layer
本發明之其他的特徵及功效，將於參照圖式的實施方式中清楚地呈現，其中： 圖1是本發明阻水氣用結構體的第一實施例的示意圖； 圖2是本發明阻水氣用結構體的有機層的局部放大的示意圖； 圖3是本發明阻水氣用結構體的第二實施例的示意圖； 圖4是本發明阻水氣用結構體的第三實施例的示意圖；及 圖5是本發明阻水氣用結構體的第四實施例的示意圖。BRIEF DESCRIPTION OF THE DRAWINGS Other features and advantages of the present invention will be apparent from the embodiments of the present invention, wherein: Figure 1 is a schematic view of a first embodiment of a water blocking gas structure of the present invention; FIG. 3 is a schematic view showing a second embodiment of the water blocking gas structure of the present invention; FIG. 4 is a schematic view showing a third embodiment of the water blocking gas structure of the present invention; And Fig. 5 is a schematic view showing a fourth embodiment of the water blocking gas structure of the present invention.
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