TW513487B - Method for producing anti-reflection plated film by sputtering and wet-type plated film - Google Patents
Method for producing anti-reflection plated film by sputtering and wet-type plated film Download PDFInfo
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513487513487
發明領域 本發明係有關於一種用於陰極射線管(CRT )破填爲 f之鍍膜製造方法,此鍍膜包含一光學效果層系統,具^有 f的抗反射以及低電阻效應。更具體地來說,本發明^供 「種結合真空濺鍍及溼式鍍膜的製造方法,其中真空賤錢 過,提供高導電性氧化層,溼式製程係用傳統旋轉鍍膜形 成氧化矽表面層。 發明背景 美國專利4, 921,7 6 0號揭示一種在Ce02層跟合成物脂 間’具有良好的附著特性的多層抗反射層鍍膜。這個多層 膜的系統包括了下列物質:Ce02、A1203、Zr02、Si02、 T i 0 2跟T a 2 0 5。在這多層系統中的薄膜全都是由真空蒸鍍 或是濺錢過程所產生,並且其中有三到五層薄膜。舉例來 說,一個五層結構的總厚度約為3 5 8 0埃。在這個五層結構 中最厚的兩層薄膜分別為Ce02 ( 1360埃)以及Si02 ( 1220 埃)。 美國專利5,1 0 5,3 1 0號揭示一種藉由反應濺鍍 (reactive sputtering)且設計用在線上鍍膜機器的多層 抗反射鍍膜。而這個多層膜結構包含了 Ti 02、Si 02、FIELD OF THE INVENTION The present invention relates to a method for manufacturing a coating film for fusing a cathode ray tube (CRT) with f. The coating film includes an optical effect layer system with anti-reflective effect and low resistance effect. More specifically, the present invention provides a "manufacturing method combining vacuum sputtering and wet coating, in which a vacuum is used to provide a highly conductive oxide layer, and a wet process uses a conventional spin coating to form a silicon oxide surface layer BACKGROUND OF THE INVENTION U.S. Patent No. 4,921,760 discloses a multi-layer antireflection coating with good adhesion characteristics between the Ce02 layer and the synthetic grease. The system of this multilayer film includes the following materials: Ce02, A1203, Zr02, Si02, T i 0 2 and T a 2 0 5. The films in this multilayer system are all produced by vacuum evaporation or money spattering, and there are three to five layers of films. For example, a five The total thickness of the layer structure is approximately 3 580 angstroms. The two thickest films in this five-layer structure are Ce02 (1360 angstroms) and Si02 (1220 angstroms). US Patent 5, 10 5, 3 1 0 No. reveals a multilayer anti-reflection coating by reactive sputtering and designed for use in an on-line coating machine. This multilayer film structure includes Ti 02, Si 02,
Zn0、Zr02跟Ta205。在這多層系統中的薄膜全都是由真空 蒸鍍或是濺鍍過程所產生,並且其中有四到六層薄膜。舉 例來說,一個六層結構的總厚度約為4 7 0 〇埃。且在這個六 層結構中最厚的兩層薄膜分別為zn〇 ( 1 3 7 0埃)以及Si 02 (1 3 6 0 埃)。 美國專利5, 091,244號跟5, 40 7, 73 3揭示一種新式的導Zn0, Zr02 and Ta205. The films in this multilayer system are all produced by a vacuum evaporation or sputtering process, and there are four to six layers of films. For example, the total thickness of a six-layer structure is approximately 4700 Angstroms. And the two thickest films in this six-layer structure are zn0 (1,370 angstroms) and Si 02 (1,360 angstroms). U.S. Patent Nos. 5,091,244 and 5,40 7,73 3 disclose a new type of guide
513487 銮號 89107402 五、發明說明(2) 電性光衰減抗反射層鍍膜。這些專利之範圍主要揭露一種 可提供導電、光衰減及反光表面的某些過渡元素氮化物材 料。這個多層結構包含了 TiN、NbN、Sn02、Si〇2、 A 1 203、跟Nb205。在這個多層結構中的薄膜材料為氮化物 及氧化物。在此多層結構中有三到四個薄膜。在專利中的 例子,一個四層結構的總厚度約為1 6 1 〇埃,且其中最厚的 兩層薄膜分別為211〇( 6 5 0埃)以及8丨〇2 ( 8 2 0埃)。這兩、 層薄膜對於可見光的穿透率都低於百分之五十。所有的X薄 膜都是由真空蒸鍍或是錢鍍過程所產生。 、 美國專利5,1 4 7,1 2 5號揭示一種使用氧化鋅,以提供 對於波長小於3 8 0奈米(nm )抗紫外光的多層抗反射膜。 這個多層系統包括了 Ti02、Si02、ZnO跟MgF2。所有的薄 膜是由真空蒸鍍或是濺鍍過程所產生。在這個多層系統中 有四到六個薄膜層。在專利中的例子裡,一個五層結構的 、’、心尽度約為7350埃。且其中最主要的兩層薄膜分別為 (43 9 0埃)及j|gF2 ( 1 3 2 0埃)。所有薄膜都是由真空蒸鍍 或是濺鍍過程所產生。 …、又 美國專利5,1 7 0,2 9 1號揭示一種具有光學效應及高抗 反射效應的四層結構。這些層乃是由熱解(pyr〇litic)方 式、電漿化學氣相沉積法、濺鍍法及化學沉積法所形成。 其包含了 Si〇2、Ti02 ' A1203、ZnS、MgO 及 Bi203。在專利 所說明的範例中,一個四層結構的總厚度約為2 4 8 0埃。最 主要的兩層薄膜分別為Ti 〇2 ( 1 04 0埃)及Si 02 ( 940埃 美國專利5,2 1 6,5 4 2號揭示一種具有高抗反射的五層513487 銮 89107402 V. Description of the invention (2) Electrical light attenuation anti-reflection layer coating. The scope of these patents primarily discloses a certain transition element nitride material that provides a conductive, light-attenuating, and reflective surface. This multilayer structure contains TiN, NbN, Sn02, SiO2, A1 203, and Nb205. The thin film materials in this multilayer structure are nitrides and oxides. There are three to four films in this multilayer structure. In the example in the patent, the total thickness of a four-layer structure is about 1610 angstroms, and the two thickest films are 2110 (650 angstroms) and 8 丨 2 (8 20 angstroms) respectively. . Both of these thin films have a transmittance of less than 50 percent for visible light. All X films are produced by vacuum evaporation or coin plating processes. U.S. Patent No. 5,14,1,25 discloses a multilayer anti-reflection film using zinc oxide to provide anti-ultraviolet light for wavelengths less than 380 nanometers (nm). This multilayer system includes Ti02, Si02, ZnO and MgF2. All films are produced by vacuum evaporation or sputtering processes. There are four to six thin film layers in this multilayer system. In the example in the patent, a five-layer structure, ′, and the endurance are about 7350 angstroms. And the two most important thin films are (4,390 angstroms) and j | gF2 (1,320 angstroms). All films are produced by vacuum evaporation or sputtering processes. ..., and U.S. Patent No. 5,170,29.1 discloses a four-layer structure with optical effect and high anti-reflection effect. These layers are formed by a pyrolitic method, a plasma chemical vapor deposition method, a sputtering method, and a chemical deposition method. It contains Si02, Ti02 'A1203, ZnS, MgO and Bi203. In the example described in the patent, the total thickness of a four-layer structure is about 2480 Angstroms. The two main thin films are Ti 〇2 (104 0 angstroms) and Si 02 (940 angstroms. US Patent No. 5, 2 1 6, 5 4 2 discloses a five-layer with high anti-reflection.
第5頁 513487 Λ 修正 曰 案號 89107402 五、發明說明(3) 膜結構。其製程利用一個厚度約為i奈米(nm )的附著層 (Ni、Cr或NiCr)。其它的四層膜則由Sn〇2、Zr〇2、Page 5 513487 Λ Amendment No. 89107402 V. Description of the invention (3) Membrane structure. The process uses an adhesion layer (Ni, Cr, or NiCr) with a thickness of about 1 nanometer (nm). The other four-layer film consists of Sn〇2, Zr〇2,
ZnO 、 Ta205 、 NiO 、 Cr〇2 、 Ti02 、 Sb2〇3 、 In2〇3 、 A12〇3 、ZnO, Ta205, NiO, Cr〇2, Ti02, Sb2O3, In2O3, A12〇3,
Si 02、TiN跟ZrN組成。在專利中的例子裡,一個五層結構 的·=厚度約為2 33 7埃。1其中最主要的兩層薄膜分別為 1 _500埃)及31〇2(138了埃)。這兩層薄膜對於可見 率都低於百分之三十。戶斤有薄膜都是由真空蒸鍍 或疋錢鍍過程所產生。 美國專利5, 541,77 0號揭示一福七人7兩、當成μ μ > 減抗反射層膜。這是一個四或 匕3 了電ν層的先哀 φ ,且古一 ^ = a五層的糸統。在這個系統 二;折射率光吸收的金屬如Cr、μ〇 :12〇广气膜η。而其它”或四層結構為⑽、IT。、 材科a气& 寻j顯不了此層狀系統中最主要的 材料為虱化物及氮化物,而唯一 氺璺辇> # , ^ , 的金屬在抗反射膜中做為 =政:膜用。戶斤有薄膜都是由真空蒸鐘或是…程 Ξί。,利:說明的範例卜個五層結構的總厚度 、、’、.、、 矣,其隶主要的兩層薄膜分別為ΙΤ0 ( 334埃)' S1 0 2 ( 7 2 〇埃)。而這個層狀系統對於可見光的穿透率低 於百分之六十。 一 美國專利5,3 6 2,5 52號揭示一種包含三層導電金屬氧 化層的六層抗反射膜。此系統包含了 S i 〇 2、I Τ 0、N b 2 0 5跟 Ta20’且在導電金屬氧化層總共約一個可見光波長的厚度 裡可邊也包含在薄膜中。在專利中六層結構的例子裡,最 主要的兩層薄膜分別為Si 02 ( 8 54埃)跟IT〇 ( 1 9 7 5埃)。 所有薄獏都是由真空蒸鍍或是濺鍍過程所產生。Si 02, TiN and ZrN. In the example in the patent, the thickness of a five-layer structure is approximately 2 33 7 Angstroms. 1 The two most important films are 1-500 angstroms) and 3102 (138 angstroms). Both films are less than 30% for visibility. Household thin films are produced by vacuum evaporation or coin plating. U.S. Patent No. 5,541,77 0 discloses that one fortune, seven people, and two are regarded as μ μ > Antireflection layer film. This is a five-layered system with four or three layers of electric ν, and the ancient one ^ = a. In this system II; the refractive index of light-absorbing metals such as Cr, μ0: 120 wide air film η. And the other "or four-layer structure is ⑽, IT., Material science and gas, and the main material in this layered system is lice and nitride, and the only 氺 璺 辇 >#, ^, The metal is used as an anti-reflection film in the anti-reflection film: the film is used. All the thin films are made of vacuum bells or ... Cheng Yi., Lee: The illustrated example, the total thickness of a five-layer structure ,,,,,,, ,, 矣, its main two layers are ITO (334 Angstroms) 'S1 0 2 (72 Angstroms). And this layered system has a transmittance of less than 60% for visible light. Patent No. 5,3 6 2,5 52 discloses a six-layer anti-reflection film including three conductive metal oxide layers. This system includes S i 〇2, I T 0, N b 2 0 5 and Ta20 'and is conductive. The metal oxide layer can also be included in the film in a thickness of about one visible wavelength. In the example of the six-layer structure in the patent, the two main films are Si 02 (85 54 Angstroms) and IT 0 (19). 7 5 Angstroms). All thin layers are produced by vacuum evaporation or sputtering.
第6頁 513487 -----案號89107402 年月日 _修正____ 五、發明說明(4) 美國專利5,5 7 9,1 6 2號揭示一種如橡膠般具有溫度靈 敏性質之基板的四層抗反射層薄膜。其中有一層為快速沉 積且不會將大量的熱傳遞給基板的直流反應歲鐘金屬乳化 物。此層狀系統包括了 Sn02、Si02、跟ITO。就一個四層 結構的例子來說,最主要的兩層薄膜分別為S η 0 2 ( 7 6 3埃 )跟S i 02 ( 9 4 0埃)。所有薄膜都是由真空蒸鍍或是濺鍍 過程所產生。 美國專利5, 728, 45 6號與5, 78 3, 049號揭示一個能夠改 善沉積在塑膠膜上的抗反射薄膜。此多層膜是隨著真空濺 錢過程中,利用滾轉機鑛膜而成。此系統包含了 I T 〇、S i 0 跟一個覆蓋在可溶解氟聚合物層上的薄潤滑層。在專利中 的例子,一個六層的結構總厚度約為2 6 3 0埃。最主要的兩 層薄膜為ΙΤΌ ( 888埃)跟Si 02 ( 8 6 9埃)。 由上敘述,可清楚看出在這些具有高抗反射效應及高 可見光穿透率(大於百分之九十)的薄膜系統中,所有薄 膜皆是由真空蒸鍍及(或)濺鍍過程所產生。另一方面, 在這類系統裡面最主要的高折射率材料層的厚度約在7 〇 〇 埃至2 0 0 〇埃之間,而最主要的低折射率材料層的厚度約在 7 0 0埃至1 4 0 0埃之間。 發明總論 本發明的主要目的是藉由濺鍍的過程提供一個抗靜電 (anti-static)薄膜並且結合利用溼式過程如旋轉錢膜、 喷濺鍍膜等的抗反射薄膜。 製作透明導電氧化薄膜層的過程在工業大量生產中具Page 6 513487 ----- Case No. 89107402 Date _ Amendment ____ V. Description of the Invention (4) US Patent No. 5,5 7 9, 1 6 2 discloses a substrate with temperature sensitive properties like rubber Four anti-reflection layer films. One of these layers is a DC reaction metal emulsion that rapidly deposits and does not transfer a large amount of heat to the substrate. This layered system includes Sn02, Si02, and ITO. In the case of a four-layer structure, the two main thin films are S η 0 2 (763 Angstroms) and Si 02 (94 Angstroms). All films are produced by vacuum evaporation or sputtering processes. U.S. Patent Nos. 5,728,45 6 and 5,78 3,049 disclose an anti-reflective film capable of improving deposition on a plastic film. This multi-layer film is formed by using a roller ore film in the process of vacuum sputtering. This system consists of I T 0, S i 0 and a thin lubricating layer overlying a soluble fluoropolymer layer. In the example in the patent, the total thickness of a six-layer structure is approximately 2630 angstroms. The most important two layers are ITO (888 Angstroms) and Si 02 (86 Angstroms). From the above description, it can be clearly seen that in these thin film systems with high anti-reflection effect and high visible light transmittance (greater than 90%), all thin films are subjected to vacuum evaporation and / or sputtering produce. On the other hand, the thickness of the most important layer of high refractive index material in this type of system is between about 700 Angstroms and 2000 Angstroms, and the thickness of the most important layer of low refractive index material is about 700 Angstroms. Angstroms to 14 0 0 Angstroms. SUMMARY OF THE INVENTION The main object of the present invention is to provide an anti-static film through a sputtering process and an anti-reflection film using a wet process such as a spinning film, a sputter coating, and the like. The process of making a transparent conductive oxide film layer is useful in industrial mass production.
第7頁 513487 _案號891ί)74Π?_年月日_修正 五、發明說明(5) 有高可靠性’且長久以來一直為半導體、顯示器、建材玻 璃及塑膠板等工業所需要。因為利用濺鍍過程來製做低電 阻性且高透明導電氧化層薄膜比溼式過程來得容易(不論 是旋轉鍍膜或是喷濺鍍膜)。本發明提供了 一個結合抗反 射的抗靜電大量生產系統,或是線上的物理氣相沉積跟溼 式鍍膜。一些眾所周知的導電氧化膜如Sn02、ZnO、Page 7 513487 _Case No.891ί) 74Π? _YearMonthDay_Amendment V. Description of the Invention (5) High Reliability 'and has been required by industries such as semiconductors, displays, building materials, glass, and plastic boards for a long time. This is because it is easier to make a low-resistance and highly transparent conductive oxide film by using the sputtering process than the wet process (whether it is a spin coating or a sputter coating). The invention provides an antistatic mass production system combining anti-reflection, or physical vapor deposition on line and wet coating. Some well-known conductive oxide films such as Sn02, ZnO,
In203 、 Sn02 : F 。 Sn02 : Sb , In203 : Sn 、 ZnO : A1 、In203, Sn02: F. Sn02: Sb, In203: Sn, ZnO: A1,
Cd2Sn〇4 、 In203 — ZnO 、 Sn02 — ZnO 跟 In203 — Mg〇 等都是相 當高成本、低效能(高電阻)、低使用率(約百分之三至 百分之五)從溼式鍍膜過程中所得到的化學溶液。粗略地 估算由氧化物所組成的陰極射線管(CRT )傳統系統,其 所需要做為抗靜電效果(103〜105Q/square)及光學抗反 射等效薄膜的厚度約為2 0 0奈'米(nm) ( IT0 : 1〇〇奈米 (nm ),氧化矽:1 〇〇奈米(nm ))。實驗顯示對於如 IT0、ΑΤΟ、IZ0跟AZ0等厚度大於100奈米(nm)之導電氧 化物的溼式鍍膜,由於烘烤的動作使其具有低平整度、高 電阻性 '低穿透率及高成本。在導電氧化物的濺鍍過程 中’厚度要低於50奈米(nm)以符合電阻值(1〇〜1〇), 在光學抗反射效應中很重要的薄膜平整度小於百分之三, 且該薄膜也比溼式製程製作出來的材料還硬(9 Η )。另外 一方面,在溼式製程中對於厚度相當敏感的基板溫度跟烘 烤的過程也長了 2 0〜3 0分鐘,而這個短周期的過程對於大 量生產的過程是相當困難的。本發明提供了由pVD系統所 沉積而成的三層氧化物以及由溼式製程所沉積的氧化矽的 anti - static系統抗反射能力。因為高導電氧化層與擴散Cd2Sn〇4, In203 — ZnO, Sn02 — ZnO, and In203 — Mg〇 are all quite high cost, low efficiency (high resistance), low usage (about 3% to 5%) from the wet coating process The resulting chemical solution. Roughly estimate the traditional system of cathode ray tube (CRT) composed of oxide, which needs to be antistatic effect (103 ~ 105Q / square) and the thickness of the optical anti-reflection equivalent film is about 200 nanometers. (Nm) (IT0: 100 nanometers (nm), silicon oxide: 1000 nanometers (nm)). Experiments have shown that for wet-type coatings of conductive oxides with thicknesses greater than 100 nanometers (nm), such as IT0, ATTO, IZ0, and AZ0, due to the baking action, they have low flatness, high resistivity, and low transmissivity. High cost. During the sputtering process of conductive oxides, the thickness should be less than 50 nanometers (nm) to meet the resistance value (10 ~ 10), and the flatness of the film, which is important in the optical anti-reflection effect, is less than three percent. And the film is harder than the material produced by the wet process (9 Η). On the other hand, in the wet process, the substrate temperature and baking process, which are quite sensitive to the thickness, also took 20 to 30 minutes longer, and this short cycle process is quite difficult for mass production. The invention provides the anti-static system anti-reflective ability of the three-layer oxide deposited by the pVD system and the silicon oxide deposited by the wet process. Because of the highly conductive oxide layer and diffusion
513487 _案號89107402_年月曰 修正_ 五、發明說明(6) 保護氧化層被PVD所包含,此多層系統在氧化矽的溼式薄 膜製程中保持了低電阻性以及低抗反射能力。本發明也提 供了可以用在陰極射線管(CRT )表面鍍膜之抗反射層薄 膜,具有高導電性及抗靜電性。 本發明的抗反射層薄膜裡有四層的結構,最接近基板 的稱為第一層,第二至第四層以此類推。每一層都以厚度 或是光學厚度來描述其特性。光學厚度是由每一層的厚度 乘上其折射率而來,且其通常以我們所設計的波長的分數 來表示。在我們的發明裡所使用的波長約為5 2 0奈米(nm )° 第一層或是最裡面的那一層是由透明導電氧化物所組 成。一般來說此透明導電氧化物較常用I TO,因為它對於 可見光的吸收很小,其在可見光波長5 2 0奈米(nm )之折 射率約為1. 8 5至2. 1,光學厚度約為我們所設計波長的六 分之一至十分之一。 第二層為一氧化材料。一般來說由於Si02對於可見光 不會吸收,其在可見光波長5 2 0奈米(nm )之折射率為 1. 4 5至1. 5,而實際厚度在我們所設計的波長約為1 0 0至 300奈米(nm)。 第三層也是氧化材料,此氧化層的折射率類似I TO, 一般來說由於SnO 2對於可見光不會吸收,其在可見光波長 5 2 0奈米(nm )之折射率為1 · 8 5至2 · 1,而實際厚度在我們 所設計的波長約為4 0 0至6 0 0奈米(nm )。而第四層和第二 層相同,唯一的差別是在於第二層是由藏鍵方式形成,而 第四層是在TE I S溶液裡由溼式過程所產生。一般來說我們513487 _Case No. 89107402_Year Month Amendment _ V. Description of the Invention (6) The protective oxide layer is included by PVD. This multilayer system maintains low resistance and low anti-reflection ability in the wet film process of silicon oxide. The present invention also provides an anti-reflection layer film that can be applied to the surface of a cathode ray tube (CRT), which has high electrical conductivity and antistatic properties. The antireflection layer film of the present invention has a four-layer structure. The one closest to the substrate is called the first layer, the second to fourth layers and so on. Each layer is characterized by its thickness or optical thickness. Optical thickness is the thickness of each layer multiplied by its refractive index, and it is usually expressed as a fraction of the wavelength we design. The wavelength used in our invention is about 5 20 nanometers (nm) ° The first or innermost layer is composed of a transparent conductive oxide. Generally, this transparent conductive oxide is more commonly used because it has a small absorption of visible light, and its refractive index at the visible light wavelength of 5 2 0 nm (nm) is about 1. 8 5 to 2.1, optical thickness About one-sixth to one-tenth of the wavelength we design. The second layer is an oxide material. In general, since Si02 does not absorb visible light, its refractive index at the visible light wavelength of 5 2 0 nanometers (nm) is 1.4 to 1.5, and the actual thickness is about 1 0 0 at the wavelength we designed. Up to 300 nanometers (nm). The third layer is also an oxidizing material. The refractive index of this oxide layer is similar to that of TO. Generally, since SnO 2 does not absorb visible light, its refractive index at the visible light wavelength of 5 2 0 nm (nm) is 1.85 to 2 · 1, and the actual thickness at our designed wavelength is about 400 to 600 nanometers (nm). The fourth layer is the same as the second layer, the only difference is that the second layer is formed by the hidden bond method, and the fourth layer is produced by the wet process in the TEI S solution. Generally we
513487 _案號891Q7402_年月日__ 五、發明說明(7) 稱此材料為氧化矽。其折射率為1 . 4 5至I 5 5之間且其光學 厚度在我們所設計的波長約為四分之一個波長。 在本發明的較佳具體實例中,四層膜的結構中的第一 層為I TO,在樣本一中其厚度為40奈米(nm),在樣本二 中其厚度為25奈米(nm)。第二層為Si02,在樣本一中厚 度為20奈米(nm),在樣本二中厚度為25奈米(nm)。第 三層為SnO,在樣本一中厚度為40奈米(nm ),樣本二中 厚度為55奈米(nm)。第四層為氧化矽,在樣本一與樣本 二中厚度同為85奈米(nm)。 本發明可實現前述目標,也就是從I TO薄膜中得到1 0 2 Ω/square至103Q/square,而且在可見光400奈米(nm) 至700奈米(nm)的範圍裡,可以在玻璃或是塑膠基板上 得到低的反射頻譜。在這個四層的光學薄膜層裡面,在波 長範圍40 0奈米(nm)至7 0 0奈米(nm)的任何波長其反射 都小於百分之五。我們很容易就可以說明此製程具有可靠 性、簡單、易控制且具有經濟效應。以這樣的製程製作低 電阻、高硬度且中性抗反射膜變為相當可能。大量生產或 是i η- 1 i ne濺鍍系統將用來沉積可以做為低電阻、高光學 特性及高s c r a t c h電阻的第一 '二、三層的薄膜。而渔式 鍍膜系統將被用來沉積第四層氧化矽層,且可用降低成 本。 此外,本發明中的層狀系統對於電磁屏蔽(EM I sh i e 1 d )具有高導電性、對於光學觀點來說具有低反射特 性、對於表面鍍膜具有高scratch電阻、並且可以降低成 本。舉例來說,我們可以利用濺鍍製程及溼式製程的結513487 _Case No. 891Q7402_Year Month Day__ 5. Description of the invention (7) This material is called silicon oxide. Its refractive index is between 1.45 and I 5 5 and its optical thickness is about a quarter of the wavelength we designed. In a preferred embodiment of the present invention, the first layer in the four-layer film structure is ITO, and its thickness is 40 nanometers (nm) in sample one, and its thickness is 25 nanometers (nm) in sample two. ). The second layer is Si02, with a thickness of 20 nanometers (nm) in sample one and a thickness of 25 nanometers (nm) in sample two. The third layer is SnO, with a thickness of 40 nanometers (nm) in sample one and a thickness of 55 nanometers (nm) in sample two. The fourth layer is silicon oxide with a thickness of 85 nanometers (nm) in sample one and sample two. The present invention can achieve the foregoing objective, that is, to obtain 1 02 Ω / square to 103Q / square from the I TO film, and in the range of visible light from 400 nanometers (nm) to 700 nanometers (nm), it can be used in glass or It is the low reflection spectrum obtained on the plastic substrate. In this four-layer optical film layer, the reflection is less than five percent at any wavelength in the wavelength range of 400 nanometers (nm) to 700 nanometers (nm). We can easily explain that this process is reliable, simple, easy to control and economical. It is quite possible to produce a low-resistance, high-hardness, and neutral anti-reflection film by such a process. A mass-produced or i η-1 in ne sputtering system will be used to deposit the first two, three layers of thin films that can be used as low resistance, high optical characteristics, and high scr a t c h resistance. The fishery coating system will be used to deposit a fourth silicon oxide layer at a reduced cost. In addition, the layered system in the present invention has high conductivity for electromagnetic shielding (EM I sh e e d), low reflection characteristics from an optical standpoint, high scratch resistance for surface coating, and can reduce costs. For example, we can use the results of sputtering and wet processes.
第10頁 513487 _ 案號89107402_年月日 修正 __ 五、發明說明(8) 合,在陰極射線管(CRT )破璃基板上完成一個四層的抗 反射及anti-static層膜。此層狀系統可具有1 〇2 Ω /square至l〇3D/square的低電阻以讓TC09 9通過,並且其 硬度可以使付軍事標準MIL — C — 48497或MIL — C — 675的刻 劃測試,且其光學品質相當優異可以避免反射及假像的產 生。 此外,本發明可利用一 DC ' AC、RF磁控管濺鍍系統在 3m Toi:r(m=miii = 〇.001)氣壓的 Ar^〇2 混合氣體下, 由I TO、Si、Sn的靶材中提供第一、二、三層的薄膜濺 鍍。而第四層薄膜可以在330C且烘烤溫度2000C/30min的 情況下’由T E I S溶液裡利用旋轉濺鍍或是噴灑濺鍍等溼式 製程來鍍成。 本發明具有下列優點: 對於陰極射線管(CRT )的傳統溼式抗反射及抗靜電 鍍膜製程對於是很難通過T C 0 9 9,薄膜厚度跟品質對於溫 度相當敏感且會產生像是電阻及光學效應的問題。對於低 電阻渥式鍵臈製程所需用的化學溶液成本相當地高,並且 該電阻很難達到1〇2 Ω /square。本發明包含了利用濺鍍方 式所鑛成的二層氧化層及溼式鍍膜方式所鍍成的一層氧化 層,且有兩種型態的光學層狀系統,我們分別命名為樣本 一與樣本二。樣本一中,第一、二、三層氧化層的厚次分 別為40、20、40奈米(nm )。第四層氧化矽層的厚度則為 8 5奈米(nm )。因為利用真空濺鍍系統所鍍成的導電薄膜 層,其電阻可以低至102Ω /square。第二層也是利用濺鍍 系統鍍成,並且可以做為擴散阻障的保護層。第三層濺鍍Page 10 513487 _ case number 89107402_ year month day amendment __ V. Description of the invention (8) Combined, a four-layer anti-reflection and anti-static film is completed on the cathode ray tube (CRT) broken glass substrate. This layered system can have low resistance of 102 Ω / square to 103D / square to pass TC09 9 and its hardness can pass military standard MIL — C — 48497 or MIL — C — 675 scratch test , And its optical quality is quite excellent, which can avoid reflection and artifacts. In addition, in the present invention, a DC ′ AC, RF magnetron sputtering system can be used under a 3 m Toi: r (m = miii = 0.001) pressure Ar ^ 〇2 gas mixture from I TO, Si, Sn The target provides first, second and third layers of thin film sputtering. The fourth film can be deposited at 330C and a baking temperature of 2000C / 30min by using a wet process such as spin sputtering or spray sputtering in a T E I S solution. The invention has the following advantages: For the traditional wet anti-reflection and anti-static coating process of cathode ray tube (CRT), it is difficult to pass TC 0 99, the thickness and quality of the film are quite sensitive to temperature and produce resistance and optics. Problem of effects. The cost of the chemical solution required for the low-resistance W-bond process is quite high, and the resistance is difficult to reach 10 2 Ω / square. The present invention includes two oxide layers formed by sputtering and one oxide layer formed by wet coating. There are two types of optical layered systems. We named them Sample 1 and Sample 2 respectively. . In sample 1, the thickness of the first, second, and third oxide layers is 40, 20, and 40 nanometers (nm). The thickness of the fourth silicon oxide layer is 85 nanometers (nm). Because the conductive thin film layer formed by the vacuum sputtering system can have a resistance as low as 102Ω / square. The second layer is also deposited using a sputtering system and can be used as a protective barrier for diffusion barriers. Third layer sputtering
513487 _案號89107402_年月曰 修正_ 五、發明說明(9) 層SnO,利用化學溶液不容易蝕刻,因此其可以做為抗腐 蝕以及在其下之I TO的保護層。第四層氧化矽是由溼式製 程所鍍成,其相當容易製作且低成本。比較有趣的是,此 層狀系統的電組約為1 · 5 ’ 1 0 2 Ω / s q u a r e,且在4 0 0奈米 (nm)至700奈米(nm)之間的所有波長其反射率小於百 分之五,而平均反射率約為百分之零點五。對於陰極射線 管(CRT )應用來說,它具有極優異的性質。 在樣本二中,第一、二、三層氧化層的厚度分別為 2 5、3 0、5 5奈米(nm )。第四層氧化矽層厚度則為9 5奈米 (nm)。其電阻約為3.8’ 102D/square且其光學效應具 有寬頻的抗反射。平均反射率低於百分之零點五。本發明 是在玻璃上製作抗反射及anti-static薄膜,由三層錢鍵 層及一層具有高效能、易製作、低成本、經濟效益的製程 溼式鍍膜層所組成。 為使本發明之步驟,功效及特點更為人所瞭解,茲舉 實例並配合附圖,說明本發明之較佳實現方式: 較佳具體實例說明 在本發明中我們實現了上面所描述的目標,也就是在 陰極射線管(CRT )基板上藉由濺鍍及溼式製程所製成的 四層膜系統,以及在可見光波長400奈米(nm)至700奈米 (nm )之間的範圍裡可以得到低電阻及低反射率。這個多 層的系統由最靠近基板的那一層序列地編號,也就是說最 靠基板所鍍上的薄膜為第一層。而每一層的厚度以其實際 厚度(以奈米(nm)為單位)或是以可見光波長的分數 或是倍數型態做為表示的光學厚度來表示。513487 _Case No. 89107402_ Years and Months Amendment_ Five. Description of the Invention (9) The layer SnO is not easily etched by using a chemical solution, so it can be used as a protective layer against corrosion and I TO underneath. The fourth layer of silicon oxide is plated by a wet process, which is relatively easy to manufacture and low cost. What is more interesting is that the electrical group of this layered system is about 1 · 5 '1 0 2 Ω / square, and its reflectance is at all wavelengths between 400 nm (700 nm) and 700 nm (nm). Less than five percent, and the average reflectance is about 0.5 percent. For cathode ray tube (CRT) applications, it has extremely excellent properties. In Sample 2, the thicknesses of the first, second, and third oxide layers were 25, 30, and 55 nanometers (nm), respectively. The thickness of the fourth silicon oxide layer is 95 nanometers (nm). Its resistance is about 3.8 '102D / square and its optical effect has wide-band anti-reflection. The average reflectance is less than 0.5 percent. The invention is made of anti-reflection and anti-static film on glass, which is composed of three layers of money bonds and a wet-type coating layer with high-performance, easy-to-manufacture, low-cost and economic benefits. In order to make the steps, effects, and characteristics of the present invention more comprehensible, examples are given below in conjunction with the drawings to explain the preferred implementation of the present invention: The preferred specific examples illustrate that in the present invention we have achieved the objectives described above , That is, a four-layer film system made by sputtering and wet processes on a cathode ray tube (CRT) substrate, and a range of visible light wavelengths between 400 nm (nm) and 700 nm (nm) Here you can get low resistance and low reflectivity. This multi-layer system is serially numbered by the layer closest to the substrate, which means that the thinnest film deposited on the substrate is the first layer. The thickness of each layer is expressed by its actual thickness (in nanometers (nm)) or the optical thickness expressed as a fraction or multiple of the wavelength of visible light.
第12頁 513487 _案號89107402_年月曰 修正_ 五、發明說明(10) 本發明的具體層狀結構的如圖1所示。基板5由玻璃' 塑膠箔或是其它可看透的材料來組成。視覺的方向如箭頭 六所示。而連接基板五前端的為第一層1。以觀察者的方 向來看,接在基板上面的第一層1為第二層2。四層中的第 三層3則放在第二層2的上面。而最外面的第四層4則放在 第三層3的上面。而第一、二、三、四層組成了本發明的 層狀系統。 此光學層狀系統有兩種型態,分別命名為樣本一與樣 本二。在樣本一中第一層為ITO且其厚度為40奈米(nm )。在波長約為5 2 0奈米(nm )其折射率約為1 · 9 8。第二 層為Si02其厚度為20奈米(nm ),在波長約為5 2 0奈米 (nm )其折射率為1 · 4 6。S i 0 2被用做擴散阻障層。第三層 為Sn02且其厚度為40奈米(nm),在波長約為520奈米 (nm )其折射率為2. 00。這層SnO被用做化學物品的阻抗 層。第四層為氧化矽其厚度為85奈米(nm),在波長520 奈米(nm)其折射率為1.5。它也是在大氣壓力下唯一從 TE I S溶液中,唯一利用溼式鍍膜法所製成的薄膜。其它的 第一、二、三層則是利用真空濺鍍系統所鍍成。在樣本二 中其第一、二、三層的厚度分別為25、28、55奈米(nm )。第四層氧化矽的厚度為9 5奈米(nm )。在此樣本中具 有寬頻抗反射的光學特性。 圖二顯示了樣本一中層狀系統的頻譜。其反射率(以 百分比做為單位)乃是由玻璃的前面測量而得。可見光頻 譜範圍從4 0 0奈米(nm )至7 0 0奈米(nm )。點狀的曲線圖 顯示了以濺鍍方式所製成的第一、二、三層的反射特性。Page 12 513487 _Case No. 89107402_ Year Month Amendment _ V. Description of the invention (10) The specific layered structure of the present invention is shown in Figure 1. The substrate 5 is composed of glass' plastic foil or other transparent materials. The direction of vision is shown by arrow six. The first layer 1 is connected to the five front ends of the substrate. In the direction of the observer, the first layer 1 on the substrate is the second layer 2. The third layer 3 of the four layers is placed on top of the second layer 2. The outermost fourth layer 4 is placed on top of the third layer 3. The first, second, third, and fourth layers constitute the layered system of the present invention. There are two types of this optical layered system, named sample one and sample two. In sample one, the first layer is ITO and its thickness is 40 nanometers (nm). Its refractive index is about 1.98 at a wavelength of about 5 2 nanometers (nm). The second layer is SiO2 with a thickness of 20 nanometers (nm) and a refractive index of 1.46 at a wavelength of about 520 nanometers (nm). S i 0 2 is used as a diffusion barrier layer. The third layer is Sn02 and has a thickness of 40 nanometers (nm) and a refractive index of 2. 00 at a wavelength of about 520 nanometers (nm). This layer of SnO is used as a resistance layer for chemicals. The fourth layer is silicon oxide with a thickness of 85 nanometers (nm) and a refractive index of 1.5 at a wavelength of 520 nanometers (nm). It is also the only thin film made from the TE I S solution under atmospheric pressure by the wet coating method. The other first, second and third layers are deposited using a vacuum sputtering system. The thicknesses of the first, second and third layers in sample two are 25, 28 and 55 nanometers (nm), respectively. The thickness of the fourth layer of silicon oxide is 95 nanometers (nm). In this sample, it has broad-band anti-reflection optical properties. Figure 2 shows the spectrum of the layered system in Sample 1. The reflectance (in percent) is measured from the front of the glass. The visible light spectrum ranges from 400 nanometers (nm) to 700 nanometers (nm). The dotted graph shows the reflection characteristics of the first, second, and third layers made by sputtering.
第13頁 513487 案號 89107402 曰 修正 五、發明說明(11) 而此層狀系統的曲線圖清楚地顯示了在中心波長5 7 0奈米 (nm)至590奈米(nm)的範圍其具有極低的反射率(百 分之零點一),而在波長400奈米(nm)至700奈米(nm) 範圍中其反射率則低於百分之五。此層狀系統的電阻為1 · 36’ 102W/square,而錯筆(pencil)的硬度為9H。對於 CRT、CDT、FED、PDP等應用具有相當好的結果。附件一表 一顯示了從4 0 0奈米(nm )至7 0 0奈米(nm )間關於電阻、 船筆(p e n c i 1 )硬度、與C I E顏色的所有資料。 102W/square ,而船 二顯示了從4 0 0奈米 ‘錯筆(p e n c i 1 )硬 圖三顯示了樣本一中層狀系統的頻譜。其反射率(以 百分比做為單位)乃是由玻璃的前面測量而得。可見光頻 譜範圍從40 0奈米(nm)至700奈米(nm)。點狀的曲線圖 顯示了以濺鍍方式所製成的第一、二、三層的反射特性。 而此層狀系統的曲線圖清楚地顯示了在中心波長440奈米 (nm )至5 8 0奈米(nm )的範圍其具有極低的反射率(百 分之零點二)。在波長40 0奈米(nm )至7 0 0奈米(nm )範 圍裡,其具有寬頻光學抗反射特性,而其反射率低於百分 之五。此層狀系統的電阻值為3. 9 6 ’ 筆(p e n c i 1 )的硬度為9 Η。附件一 4 (nm )至7 0 0奈米(nm )間關於電阻 度、與C I E顏色的所有資料。 在Ar跟02所混合的反應氣體中的磁控管系統,第一、 二、三氧化層乃是由濺鍍方式所製成。第一、二、三層的 靶材分別為I TO、S i跟Sn。靶材到基板之間的距離為1 5公 分。在濺鍍的過程中並沒有加熱。第四層氧化矽層耐是在 室溫3 3 0 C下,利用旋轉鍍膜方式鍍成,且在大氣中以Page 13 513487 Case No. 89107402 Amendment V. Description of the Invention (11) The graph of this layered system clearly shows that it has a center wavelength in the range of 5 7 0 nm (nm) to 590 nm (nm). Very low reflectivity (0.1%), while the reflectance is less than 5% in the wavelength range of 400 nanometers (nm) to 700 nanometers (nm). The resistance of this layered system is 1.36 '102 W / square, and the hardness of the pencil is 9H. For CRT, CDT, FED, PDP and other applications have quite good results. Table 1 in Annex 1 shows all the information about resistance, boat hardness (pe n c i 1), and C I E color from 400 nanometers (nm) to 700 nanometers (nm). 102W / square, while ship 2 shows the hardness from 400 nanometers ‘wrong pen (pe n c i 1). Figure 3 shows the spectrum of the layered system in sample 1. The reflectance (in percent) is measured from the front of the glass. The visible light spectrum ranges from 400 nanometers (nm) to 700 nanometers (nm). The dotted graph shows the reflection characteristics of the first, second, and third layers made by sputtering. The graph of this layered system clearly shows that it has a very low reflectance (0.2%) in the range of the center wavelength from 440 nanometers (nm) to 580 nanometers (nm). In the wavelength range of 400 nanometers (nm) to 700 nanometers (nm), it has broadband optical anti-reflection characteristics, and its reflectance is less than five percent. The resistance value of this layered system is 3. 9 6 ′ The pen (pe n c i 1) has a hardness of 9 Η. Attachment 1 All the information about electrical resistance and C I E color between 4 (nm) and 700 nanometers (nm). In the magnetron system in the reaction gas mixture of Ar and 02, the first, second and third oxide layers are made by sputtering. The targets of the first, second and third layers are I TO, Si and Sn, respectively. The distance from the target to the substrate is 15 cm. There was no heating during the sputtering process. The fourth silicon oxide layer is resistant to plating at room temperature 3 3 0 C by spin coating, and is
第14頁 513487Page 513 487
第15頁Page 15
513487附件 表1· 最小反射率 底波長 電阻値 鉛筆 (pencil ) 硬度 CIE 顏色(x,y) 0.02% 577.94η m 1.3 59 χ102Ω /□ 8H 〜9H (0.26761, 0.20798) 波長(奈米(nm)) _反射(百分比)_ CRT//IT0/Si02/Sn0 CRT//IT0/Si02/Sn0 Ί 2/SiOx __ 400 5.02 420 4.86 440 6.15 460 8.26 480 9.7 500 11.77 520 12.89 540 13.91 560 15.18 580 15.97 600 16.27 620 16.82 640 16.95 660 17.24 680 17.44 700 17.1 /751814 ./065347 H-...... 5 4 3 2 10 0.18 0.02 0.17 0.52 16 5 2 0 6 3 0 1 1 2 表2· 最小反射率 底波長 電阻値 Pencil硬度 CIE 顏色(x,y) 0.16% (W-b and) 440〜580 nm 3.96χ102Ω/ □ 8H 〜9H (0.31562, 0.12193) CRT//IT0/Si02/Sn0 Ύ CRT//IT0/Si02/Sn0 ,/SiOx 400 13.66 4.07 420 10.54 1.2 440 9.54 0.28 波長(奈米(nm)) _反射率(百分比) 16 513487 460 480 500 520 540 560 580 600 620 640 660 680 700 9.79 10.06 11.11 11.63 3 2 8 16 8 9 4 3 3 3 4 4 4 4 5 1 1X Ί -Η lx 1Χ ix-· 4 6 3 7 8 2 7 4 0.16 0.23 0.25 0.23 0.18 0.16 0.2 0.33 0.56 0.88 1.27 1.7 2.17 表 3 · \ 材料 厚, 度 鑛膜方式 原始 材料 鍍膜情況 樣本 樣本 第一 層 ITO 40nm 2 5 nm Sputt erin g ITO 3 mTorr 第二 層 Si02 2 Onm 2 8nm Sputterin g Si 3 mTorr 弟二 層 Sn02 40nm 5 5 nm Sputterin g Sn 3 mTorr 第四 層 Silica 8 5 nm 95nm Spin coating TEIS 覆蓋溫度:33°C 烘烤溫度:200°C /3 Omin513487 Attachment Table 1 · Minimum reflectance, bottom wavelength resistance, pencil hardness CIE color (x, y) 0.02% 577.94η m 1.3 59 χ102Ω / □ 8H ~ 9H (0.26761, 0.20798) Wavelength (nm (nm)) _Reflection (percent) _ CRT // IT0 / Si02 / Sn0 CRT // IT0 / Si02 / Sn0 Ί 2 / SiOx __ 400 5.02 420 4.86 440 6.15 460 8.26 480 9.7 500 11.77 520 12.89 540 13.91 560 15.18 580 15.97 600 16.27 620 16.82 640 16.95 660 17.24 680 17.44 700 17.1 / 751814 ./065347 H -...... 5 4 3 2 10 0.18 0.02 0.17 0.52 16 5 2 0 6 3 0 1 1 2 Table 2.Minimum reflectance bottom wavelength resistance値 Pencil hardness CIE color (x, y) 0.16% (Wb and) 440 ~ 580 nm 3.96 × 102Ω / □ 8H ~ 9H (0.31562, 0.12193) CRT // IT0 / Si02 / Sn0 Ύ CRT // IT0 / Si02 / Sn0, / SiOx 400 13.66 4.07 420 10.54 1.2 440 9.54 0.28 Wavelength (nanometer (nm)) _Reflectivity (percent) 16 513487 460 480 500 520 540 560 580 600 620 640 660 680 700 9.79 10.06 11.11 11.63 3 2 8 16 8 9 4 3 3 3 4 4 4 4 5 1 1X Ί -Η lx 1 × ix- · 4 6 3 7 8 2 7 4 0.16 0.23 0.25 0.23 0.18 0.16 0.2 0.33 0. 56 0.88 1.27 1.7 2.17 Table 3 \ Material thickness, degree of ore film method Raw material coating situation Sample sample First layer ITO 40nm 2 5 nm Sputt erin g ITO 3 mTorr Second layer Si02 2 Onm 2 8nm Sputterin g Si 3 mTorr Brother Two layers of Sn02 40nm 5 5 nm Sputterin g Sn 3 mTorr Fourth layer of Silica 8 5 nm 95nm Spin coating TEIS Covering temperature: 33 ° C Baking temperature: 200 ° C / 3 Omin
17 513487 圖式簡單說明 圖1為依 圖2顯示 為單位表 圖3顯示 為單位表 案號89107402_年月日 修正 據本發明之層狀系統的概略剖面圖; 了在樣本一中的層狀系統之反射曲線 示)與波長(以奈米n m )的關係圖。 了在樣本二中的層狀系統之反射曲線 示)與波長(以奈米nm )的關係圖。 (以百分比 (以百分比17 513487 Brief description of the diagram. Figure 1 shows the unit table according to Figure 2. Figure 3 shows the unit table. Case number 89107402_year, month, and day. A schematic cross-sectional view of the layered system according to the present invention; The reflection curve of the system is shown) as a function of wavelength (in nanometers). The relationship between the reflection curve of the layered system in sample 2 and the wavelength (in nanometers) is shown. (In percentage (in percentage
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WO2022156820A1 (en) * | 2021-01-25 | 2022-07-28 | Hong Kong Baptist University | Metal substrate coatings |
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