TWI578029B - Manufacturing method of wavelength-selective shielding films,and wavelength-selective shielding films and selective light-shielding composites manufactured thereby - Google Patents
Manufacturing method of wavelength-selective shielding films,and wavelength-selective shielding films and selective light-shielding composites manufactured thereby Download PDFInfo
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本發明係有關於一種光波長選擇性遮蔽膜、選擇性遮光複合體及製造光波長選擇性遮蔽膜的方法,且特別是有關於一種可遮蔽波長為700nm至1100nm之光線的光波長選擇性遮蔽膜、選擇性遮光複合體及製造光波長選擇性遮蔽膜的方法。 The present invention relates to a light wavelength selective masking film, a selective light shielding composite, and a method for fabricating a light wavelength selective masking film, and more particularly to a wavelength selective masking of light that can shield light having a wavelength of 700 nm to 1100 nm. A film, a selective light-shielding composite, and a method of producing a light wavelength selective masking film.
利用近紅外光作為夜視或偵測光源在軍事活動中已行之有年,隨著光學技術的發展與民眾對夜間攝影的需求,具備近紅外光成像與夜視功能的攝影裝置應運而生,例如具備夜視功能的監視器與近紅外光行車夜視輔助系統。然而,此等攝影裝置卻被濫用而衍生了攝影偷拍的問題。 The use of near-infrared light as a night vision or detection light source has been in military activities for many years. With the development of optical technology and the demand for night photography, people with near-infrared light imaging and night vision have emerged. For example, a night vision function monitor and a near infrared light travel night vision assist system. However, these photographic devices have been abused to create the problem of sneak shots.
目前可遮蔽近紅外光的衣物或織品,例如迷彩軍服,多以印染塗料或調整衣物顏色分佈的方式行之,但印染塗料易因清洗脫落而造成功能消減,而迷彩樣式難以滿足一般民生市場對織品或衣物的外觀需求,也不利軍事人員於非綠色植被環境進行偽裝。 At present, clothing or fabrics that can block near-infrared light, such as camouflage uniforms, are mostly printed or dyed or adjusted to the color distribution of the clothes. However, the printing and dyeing coatings are easy to reduce due to cleaning and falling off, and the camouflage style is difficult to meet the general livelihood market. The appearance requirements of fabrics or clothing are also unsuitable for military personnel to camouflage in non-green vegetation environments.
因此,如何使衣物或織品具有遮蔽近紅外光的功能、不易因清洗而脫落,且在顏色上能有別於迷彩樣式,以滿足一般民生市場對織品或衣物的外觀需求,或者有利於軍事人員於非綠色植被環境進行偽裝,係相關業者努力的目標。 Therefore, how to make clothing or fabric have the function of shielding near-infrared light, is not easy to fall off due to cleaning, and can be different from the camouflage pattern in color, to meet the appearance requirements of fabrics or clothes in the general livelihood market, or to benefit military personnel. Camouflage in a non-green vegetation environment is the goal of the relevant industry.
本發明之一目的是提供一種光波長選擇性遮蔽膜,其包含高分子塑料以及複數個含氧化鎢粉體,可用以遮蔽波長為700nm至1100nm之光線,可依實際需求調整顏色,並具有耐水洗、製程簡單的優點。 An object of the present invention is to provide a light wavelength selective masking film comprising a polymer plastic and a plurality of tungsten oxide-containing powders, which can be used to shield light having a wavelength of 700 nm to 1100 nm, can be adjusted according to actual needs, and have resistance. The advantages of washing and simple process.
本發明之又一目的是提供一種選擇性遮光複合體,包含前述的光波長選擇性遮蔽膜及布料層,可用以遮蔽波長為700nm至1100nm之光線,並可經由進一步裁製,應用於軍用反偵測物品、衣物或寢具用織物等等。 A further object of the present invention is to provide a selective light-shielding composite comprising the above-mentioned optical wavelength selective masking film and cloth layer, which can be used to shield light having a wavelength of 700 nm to 1100 nm, and can be further tailored for use in military anti- Detect items, fabrics for clothing or bedding, and more.
依照本發明之一態樣之一實施方式,提供一種光波長選擇性遮蔽膜,包含高分子塑料以及複數個含氧化鎢粉體,含氧化鎢粉體分散於高分子塑料中,含氧化鎢粉體的平均粒徑為50nm至1500nm,含氧化鎢粉體的通式為W1-XMXOY,M為鎂(Mg)、鋯(Zr)、鉻(Cr)、錳(Mn)、鐵(Fe)、釕(Ru)、鈷(Co)、銠(Rh)、銥(Ir)、鎳(Ni)、鈀(Pd)、鉑(Pt)、銅(Cu)、銀(Ag)、金(Au)、鋅(Zn)、鎘(Cd)、鋁(Al)、鎵(Ga)、銦(In)、鉈(Tl)、矽(Si)、鍺(Ge)、錫(Sn)、鉛(Pb)、銻(Sb)、硼(B)、氟(F)、磷(P)、硫(S)、硒(Se)、溴(Br)、碲(Te)、鈦(Ti)、鈮(Nb)、釩(V)、鉬(Mo)、鉭(Ta)、錸(Re)、鈹(Be)、鉿(Hf)、鋨(Os)、鉍(Bi)或碘(I),X與Y滿足以下關係式:0<X0.3;以及 2.2Y3。 According to an embodiment of the present invention, there is provided a light wavelength selective masking film comprising a polymer plastic and a plurality of tungsten oxide-containing powders, wherein the tungsten oxide powder is dispersed in a polymer plastic, and the tungsten oxide powder is contained. The average particle diameter of the body is 50 nm to 1500 nm, and the formula containing tungsten oxide powder is W 1-X M X O Y , and M is magnesium (Mg), zirconium (Zr), chromium (Cr), manganese (Mn), Iron (Fe), ruthenium (Ru), cobalt (Co), rhodium (Rh), iridium (Ir), nickel (Ni), palladium (Pd), platinum (Pt), copper (Cu), silver (Ag), Gold (Au), zinc (Zn), cadmium (Cd), aluminum (Al), gallium (Ga), indium (In), germanium (Tl), germanium (Si), germanium (Ge), tin (Sn), Lead (Pb), antimony (Sb), boron (B), fluorine (F), phosphorus (P), sulfur (S), selenium (Se), bromine (Br), tellurium (Te), titanium (Ti), Niobium (Nb), vanadium (V), molybdenum (Mo), tantalum (Ta), niobium (Re), niobium (Be), niobium (Hf), niobium (Os), niobium (Bi) or iodine (I), X and Y satisfy the following relationship: 0<X 0.3; and 2.2 Y 3.
依據前述之光波長選擇性遮蔽膜,光波長選擇性遮蔽膜對於波長為700nm至1100nm之光線的遮蔽率可大於40%。依據本發明一實施例,光波長選擇性遮蔽膜對於波長為700nm至1100nm之光線的遮蔽率可大於60%。光波長選擇性遮蔽膜的厚度可為0.005mm至1mm。 According to the aforementioned light wavelength selective masking film, the light wavelength selective masking film can have a shielding ratio of more than 40% for light having a wavelength of 700 nm to 1100 nm. According to an embodiment of the invention, the optical wavelength selective masking film may have a shielding ratio of more than 60% for light having a wavelength of 700 nm to 1100 nm. The light wavelength selective masking film may have a thickness of 0.005 mm to 1 mm.
依據前述之光波長選擇性遮蔽膜,高分子塑料的重量以100重量份計,含氧化鎢粉體的重量可為1重量份至20重量份。含氧化鎢粉體的平均粒徑可為50nm至400nm。高分子塑料可選自聚氨基甲酸酯(polyurethane;PU)、熱可塑性彈性體(thermoplastic elastomer;TPE)、熱可塑性橡膠彈性體(thermoplastic rubber;TPR)、熱塑性聚氨基甲酸酯(thermoplastic urethane;TPU)、聚丙烯(polypropylene;PP)、聚乙烯(polyethylene;PE)、聚四氟乙烯(polytetrafluoroethylene;PTFE)、聚對苯二甲酸乙二酯(polyethylene terephthalate;PET)及聚醯胺(polyamide;PA)所組成之群組。依據本發明一實施例,高分子塑料可為聚氨基甲酸酯。 The weight of the polymer plastic may be from 1 part by weight to 20 parts by weight based on 100 parts by weight, based on the weight of the optical wavelength selective masking film. The tungsten oxide-containing powder may have an average particle diameter of 50 nm to 400 nm. The polymer plastic may be selected from the group consisting of polyurethane (PU), thermoplastic elastomer (TPE), thermoplastic rubber (TPR), and thermoplastic polyurethane (thermoplastic urethane; TPU), polypropylene (PP), polyethylene (PE), polytetrafluoroethylene (PTFE), polyethylene terephthalate (PET) and polyamide (polyamide; Group of PA). According to an embodiment of the invention, the polymer plastic may be a polyurethane.
依照本發明之一態樣之另一實施方式,提供一種選擇性遮光複合體,包含布料層與光波長選擇性遮蔽膜,布料層包含一表面,光波長選擇性遮蔽膜覆蓋布料層的表面。光波長選擇性遮蔽膜包含高分子塑料以及複數個含氧化鎢粉體,含氧化鎢粉體分散於高分子塑料中,含氧化鎢粉體的平均粒徑為50nm至1500nm,含氧化鎢粉體的通式為W1-XMXOY,M為鎂、鋯、鉻、錳、鐵、釕、鈷、銠、銥、鎳、鈀、鉑、銅、銀、金、鋅、鎘、鋁、鎵、銦、鉈、矽、鍺、錫、鉛、銻、硼、氟、磷、硫、硒、溴、碲、鈦、鈮、釩、鉬、鉭、錸、鈹、鉿、鋨、鉍或碘,X與Y滿足以下關係式:0<X0.3,及2.2Y3。 According to another embodiment of an aspect of the present invention, a selective light-shielding composite comprising a cloth layer and a light wavelength selective masking film, the cloth layer comprising a surface, and a light wavelength selective masking film covering the surface of the cloth layer is provided. The light wavelength selective masking film comprises a polymer plastic and a plurality of tungsten oxide-containing powders, wherein the tungsten oxide powder is dispersed in the polymer plastic, and the tungsten oxide powder has an average particle diameter of 50 nm to 1500 nm and contains tungsten oxide powder. The general formula is W 1-X M X O Y , and M is magnesium, zirconium, chromium, manganese, iron, lanthanum, cobalt, lanthanum, cerium, nickel, palladium, platinum, copper, silver, gold, zinc, cadmium, aluminum. , gallium, indium, antimony, bismuth, antimony, tin, lead, antimony, boron, fluorine, phosphorus, sulfur, selenium, bromine, antimony, titanium, antimony, vanadium, molybdenum, niobium, tantalum, niobium, tantalum, niobium, tantalum Or iodine, X and Y satisfy the following relationship: 0<X 0.3, and 2.2 Y 3.
依據前述之選擇性遮光複合體,光波長選擇性遮蔽膜對於波長為700nm至1100nm之光線的遮蔽率可大於40%。依據本發明一實施例,光波長選擇性遮蔽膜對於波長為700nm至1100nm之光線的遮蔽率可大於60%。光波長選擇性遮蔽膜的厚度可為0.005mm至1mm。 According to the selective light-shielding composite described above, the light-wavelength selective masking film can have a shielding ratio of more than 40% for light having a wavelength of 700 nm to 1100 nm. According to an embodiment of the invention, the optical wavelength selective masking film may have a shielding ratio of more than 60% for light having a wavelength of 700 nm to 1100 nm. The light wavelength selective masking film may have a thickness of 0.005 mm to 1 mm.
依據前述之光波長選擇性遮蔽膜,高分子塑料的重量以100重量份計,含氧化鎢粉體的重量可為1重量份至20重量份。含氧化鎢粉體的平均粒徑可為50nm至400nm。高分子塑料可選自聚氨基甲酸酯、熱可塑性彈性體、熱可塑性橡膠彈性體、熱塑性聚氨基甲酸酯、聚丙烯、聚乙烯、聚四氟乙烯、聚對苯二甲酸乙二酯及聚醯胺所組成之群組。依據本發明一實施例,高分子塑料可為聚氨基甲酸酯。 The weight of the polymer plastic may be from 1 part by weight to 20 parts by weight based on 100 parts by weight, based on the weight of the optical wavelength selective masking film. The tungsten oxide-containing powder may have an average particle diameter of 50 nm to 400 nm. The polymer plastic may be selected from the group consisting of polyurethane, thermoplastic elastomer, thermoplastic rubber elastomer, thermoplastic polyurethane, polypropylene, polyethylene, polytetrafluoroethylene, polyethylene terephthalate and A group consisting of polyamines. According to an embodiment of the invention, the polymer plastic may be a polyurethane.
依照本發明之另一態樣之一實施方式,提供一種光波長選擇性遮蔽膜的製造方法,包含以下步驟。提供一高分子塑料液體,高分子塑料液體包含高分子塑料。提供一粉體漿料,粉體漿料包含複數個含氧化鎢粉體,含氧化鎢粉體的平均粒徑為50nm至1500nm,含氧化鎢粉體的通式為W1-XMXOY,M為鎂、鋯、鉻、錳、鐵、釕、鈷、銠、銥、鎳、鈀、鉑、銅、銀、金、鋅、鎘、鋁、鎵、銦、鉈、矽、鍺、錫、鉛、銻、硼、氟、磷、硫、硒、溴、碲、鈦、鈮、釩、鉬、鉭、錸、鈹、鉿、鋨、鉍或碘,X與Y滿足以下關係式:0<X0.3,及2.2Y3。混合高分子塑料液體與粉體漿料以形成混合液。塗佈混合液於基材上以形成液狀膜。乾燥液狀膜以獲得光波長選擇性遮蔽膜。 According to an embodiment of another aspect of the present invention, a method of fabricating a light wavelength selective masking film comprising the following steps is provided. A polymer plastic liquid is provided, and the polymer plastic liquid comprises a polymer plastic. A powder slurry is provided. The powder slurry comprises a plurality of tungsten oxide-containing powders, the tungsten oxide powder has an average particle diameter of 50 nm to 1500 nm, and the tungsten oxide powder has a general formula of W 1-X M X O Y , M are magnesium, zirconium, chromium, manganese, iron, lanthanum, cobalt, lanthanum, cerium, nickel, palladium, platinum, copper, silver, gold, zinc, cadmium, aluminum, gallium, indium, antimony, bismuth, antimony, Tin, lead, antimony, boron, fluorine, phosphorus, sulfur, selenium, bromine, antimony, titanium, antimony, vanadium, molybdenum, niobium, tantalum, niobium, tantalum, niobium, tantalum or iodine, X and Y satisfy the following relationship: 0<X 0.3, and 2.2 Y 3. The polymer plastic liquid is mixed with the powder slurry to form a mixed liquid. The mixture is applied to a substrate to form a liquid film. The liquid film is dried to obtain a light wavelength selective masking film.
依據前述之光波長選擇性遮蔽膜的製造方法,高分子塑料液體可更包含丁酮或水。 According to the aforementioned method for producing a light wavelength selective masking film, the polymer plastic liquid may further comprise methyl ethyl ketone or water.
依據前述之光波長選擇性遮蔽膜的製造方法,粉體漿料可更包含丁酮或水。 According to the aforementioned method for producing a light wavelength selective masking film, the powder slurry may further comprise methyl ethyl ketone or water.
依據前述之光波長選擇性遮蔽膜的製造方法,高分子塑料的重量以100重量份計,含氧化鎢粉體的重量可為1重量份至20重量份。混合液的黏度可為20000cps至38000cps。基材係一離型紙或一布料層。 According to the above method for producing a light wavelength selective masking film, the weight of the polymer plastic may be from 1 part by weight to 20 parts by weight based on 100 parts by weight of the tungsten oxide powder. The viscosity of the mixture may range from 20,000 cps to 38,000 cps. The substrate is a release paper or a cloth layer.
100‧‧‧含氧化鎢粉體製備方法 100‧‧‧ Preparation method of tungsten oxide powder
110‧‧‧步驟 110‧‧‧Steps
111~113‧‧‧步驟 111~113‧‧‧Steps
120‧‧‧步驟 120‧‧‧Steps
130‧‧‧步驟 130‧‧‧Steps
140‧‧‧步驟 140‧‧‧Steps
150‧‧‧步驟 150‧‧‧ steps
200‧‧‧含氧化鎢粉體製備方法 200‧‧‧ Preparation method of tungsten oxide powder
210‧‧‧步驟 210‧‧‧Steps
220‧‧‧步驟 220‧‧‧Steps
230‧‧‧步驟 230‧‧‧Steps
300‧‧‧光波長選擇性遮蔽膜 300‧‧‧Light wavelength selective masking film
310‧‧‧高分子塑料 310‧‧‧Polymer plastic
320‧‧‧含氧化鎢粉體 320‧‧‧Tungsten oxide powder
400‧‧‧光波長選擇性遮蔽膜的製造方法 400‧‧‧Method for manufacturing optical wavelength selective masking film
410‧‧‧步驟 410‧‧‧Steps
420‧‧‧步驟 420‧‧ steps
430‧‧‧步驟 430‧‧ steps
440‧‧‧步驟 440‧‧‧Steps
450‧‧‧步驟 450‧‧‧Steps
500‧‧‧選擇性遮光複合體 500‧‧‧Selective shading complex
600‧‧‧布料層 600‧‧‧ cloth layer
d‧‧‧厚度 D‧‧‧thickness
第1圖係依照本發明一實施方式之含氧化鎢粉體製備方法的步驟流程圖;第2圖係第1圖中步驟110的步驟流程圖;第3圖係依照本發明另一實施方式之含氧化鎢粉體製備方法的步驟流程圖;第4圖係繪示依照本發明又一實施方式的一種光波長選擇性遮蔽膜的示意圖;第5圖係第4圖之光波長選擇性遮蔽膜的製造方法的步驟流程圖;以及第6圖係繪示依照本發明再一實施方式的一種選擇性遮光複合體的剖面示意圖;以及第7圖係純氧化鎢與實施例1、實施例4與實施例7的粉碎的氧化鎢鈦團塊的外觀圖。 1 is a flow chart showing the steps of a method for preparing a tungsten oxide-containing powder according to an embodiment of the present invention; FIG. 2 is a flow chart showing the steps of step 110 in FIG. 1; and FIG. 3 is a view showing another embodiment of the present invention. A flow chart of steps for preparing a tungsten oxide powder; FIG. 4 is a schematic view showing a light wavelength selective masking film according to still another embodiment of the present invention; and FIG. 5 is a light wavelength selective masking film of FIG. FIG. 6 is a schematic cross-sectional view showing a selective light-shielding composite according to still another embodiment of the present invention; and FIG. 7 is a pure tungsten oxide and Embodiment 1 and Embodiment 4 An external view of the pulverized tungsten oxide titanium agglomerate of Example 7.
本發明提供一種含氧化鎢粉體,含氧化鎢粉體的平均粒徑為50nm至1500nm,含氧化鎢粉體的通式為W1-XMXOY,M為鎂、鋯、鉻、錳、鐵、釕、鈷、銠、銥、鎳、鈀、鉑、銅、銀、金、鋅、鎘、鋁、鎵、銦、鉈、矽、鍺、錫、鉛、銻、硼、氟、磷、硫、硒、溴、碲、鈦、鈮、釩、鉬、鉭、錸、鈹、鉿、鋨、鉍或碘,X與Y滿足以下關係式:0<X0.3,及2.2Y3。 The invention provides a tungsten oxide-containing powder, wherein the tungsten oxide powder has an average particle diameter of 50 nm to 1500 nm, the tungsten oxide powder has a general formula of W 1-X M X O Y , and M is magnesium, zirconium and chromium. Manganese, iron, antimony, cobalt, antimony, bismuth, nickel, palladium, platinum, copper, silver, gold, zinc, cadmium, aluminum, gallium, indium, antimony, bismuth, antimony, tin, lead, antimony, boron, fluorine, Phosphorus, sulfur, selenium, bromine, antimony, titanium, antimony, vanadium, molybdenum, niobium, tantalum, niobium, tantalum, niobium, tantalum or iodine, X and Y satisfy the following relationship: 0<X 0.3, and 2.2 Y 3.
依據M的種類,含氧化鎢粉體可使用化學還原方法或物理性混合研磨方法製備而成,其中化學還原方法可為溶膠凝膠法。 Depending on the type of M, the tungsten oxide-containing powder may be prepared by a chemical reduction method or a physical mixed grinding method, wherein the chemical reduction method may be a sol-gel method.
請參照第1圖,其係依照本發明一實施方式之含氧化鎢粉體製備方法100的步驟流程圖。含氧化鎢粉體製備方法100屬於化學還原方法,在本實施方式中以M為鈦,說明如何以溶膠凝膠法製備含氧化鎢粉體。第1圖中,含氧化鎢粉體製備方法100包含步驟110、步驟120、步驟130、步驟140與步驟150。 Please refer to FIG. 1 , which is a flow chart of the steps of the method 100 for preparing tungsten oxide powder according to an embodiment of the present invention. The method for producing tungsten oxide-containing powder 100 is a chemical reduction method. In the present embodiment, M is titanium, and how to prepare a tungsten oxide-containing powder by a sol-gel method. In FIG. 1, the tungsten oxide-containing powder preparation method 100 includes a step 110, a step 120, a step 130, a step 140, and a step 150.
步驟110是提供二氧化鈦(TiO2)溶膠凝膠。請同時參照第2圖,其係第1圖中步驟110的步驟流程圖。第2圖中,步驟110包含步驟111、步驟112與步驟113。步驟111是形成溶膠,其係將去離子水、酒精(C2H5OH)與硝酸(HNO3)予以混合攪拌而得。步驟112是形成含鈦凝膠,其係將正丁氧基鈦(C16H36O4Ti)與酒精予以混合攪拌而得。步驟113是進行一攪拌步驟,其係將溶膠與含鈦凝膠予以混合攪拌,以形成二氧化鈦溶膠凝膠。 Step 110 is to provide a titanium dioxide (TiO 2 ) sol gel. Please refer to FIG. 2 at the same time, which is a flow chart of the steps of step 110 in FIG. In FIG. 2, step 110 includes step 111, step 112, and step 113. Step 111 is to form a sol obtained by mixing and stirring deionized water, alcohol (C 2 H 5 OH) and nitric acid (HNO 3 ). Step 112 is to form a titanium-containing gel obtained by mixing and stirring titanium n-butoxide (C 16 H 36 O 4 Ti) with alcohol. Step 113 is a stirring step of mixing and stirring the sol with the titanium-containing gel to form a titania sol gel.
請復參照第1圖,步驟120是提供氧化鎢(WO3)懸浮液,其係將氧化鎢與溶劑混合,並進行濕式研磨,以獲得氧化鎢懸浮液。溶劑可為乙醇,進行濕式研磨可更添加分散劑,藉以避免細化的氧化鎢產生團聚,濕式研磨可在10℃至50℃、以300rpm至1000rpm的轉速進行4小時至24小時。步驟120與步驟130的順序可對調。 Referring to Figure 1, step 120 provides a tungsten oxide (WO 3 ) suspension which is mixed with a solvent and wet-milled to obtain a tungsten oxide suspension. The solvent may be ethanol, and the wet grinding may be further added with a dispersant to avoid agglomeration of the refined tungsten oxide. The wet grinding may be carried out at 10 to 50 ° C for 4 to 24 hours at 300 rpm to 1000 rpm. The order of step 120 and step 130 can be reversed.
步驟130是混合二氧化鈦溶膠凝膠與氧化鎢懸浮液,以形成二氧化鈦/氧化鎢複合溶液。二氧化鈦的含量可佔二氧化鈦與氧化鎢總含量的20wt%至50wt%。 Step 130 is to mix a titania sol gel with a tungsten oxide suspension to form a titanium dioxide/tungsten oxide composite solution. The content of titanium dioxide may be from 20% by weight to 50% by weight based on the total content of titanium dioxide and tungsten oxide.
步驟140是加熱二氧化鈦/氧化鎢複合溶液,以形成氧化鎢鈦團塊。具體來說,可先進行乾燥步驟再進行燒結步驟,乾燥步驟可以50℃至150℃進行0.1小時至2小時,使二氧化鈦/氧化鎢複合溶液的溶劑蒸發以獲得乾燥粉末,燒結步驟可以700℃至1300℃進行1小時至8小時,使二氧化鈦與氧化鎢互相掺雜,以形成氧化鎢鈦團塊。 Step 140 is to heat the titanium dioxide/tungsten oxide composite solution to form a tungsten tungsten oxide agglomerate. Specifically, the drying step may be followed by a sintering step, and the drying step may be performed at 50 ° C to 150 ° C for 0.1 hour to 2 hours to evaporate the solvent of the titanium dioxide / tungsten oxide composite solution to obtain a dry powder, and the sintering step may be 700 ° C to Titanium dioxide and tungsten oxide are doped with each other at 1300 ° C for 1 hour to 8 hours to form a tungsten tungsten oxide agglomerate.
步驟150是研磨氧化鎢鈦團塊,以獲得含氧化鎢粉體。具體來說,步驟150可將氧化鎢鈦團塊先進行初步粉碎,再與溶劑混合,並進行濕式研磨,溶劑可為丁酮(C4H8O)或水,水可為純水或去離子水,濕式研磨可在10℃至50℃、以300rpm至1000rpm的轉速進行4小時至24小時。 Step 150 is to grind the tungsten oxide titanium agglomerate to obtain a tungsten oxide-containing powder. Specifically, in step 150, the tungsten tungsten oxide agglomerate may be firstly pulverized, mixed with a solvent, and subjected to wet grinding. The solvent may be methyl ethyl ketone (C 4 H 8 O) or water, and the water may be pure water or Deionized water, wet milling can be carried out at 10 ° C to 50 ° C, at 300 rpm to 1000 rpm for 4 hours to 24 hours.
步驟150的產物為一粉體漿料,即含氧化鎢粉體與溶劑的混合液,可直接以粉體漿料進行光波長選擇性遮蔽膜的製造,亦可將粉體漿料進行進一步的處理,例如噴霧造粒,以獲得乾燥的含氧化鎢粉體,關於噴霧造粒係習用技術,在此不予贅述。此外,由於溶膠凝膠法為習用技術,本領域具有通常知識者可依據M的種類,調整實驗的方法,在此將不予贅述。 The product of step 150 is a powder slurry, that is, a mixture containing tungsten oxide powder and a solvent, and the optical wavelength selective mask film can be directly processed by the powder slurry, and the powder slurry can be further processed. The treatment, for example, spray granulation, to obtain a dried tungsten oxide-containing powder, and the spray granulation conventional technique will not be described herein. In addition, since the sol-gel method is a conventional technique, those skilled in the art can adjust the method of the experiment according to the kind of M, and will not be described herein.
請參照第3圖,其係依照本發明另一實施方式之含氧化鎢粉體製備方法200的步驟流程圖。含氧化鎢粉體製備方法200屬於物理性混合研磨方法,在本實施方式中以M為鈦,說明如何以物理性混合研磨方法製備含氧化鎢粉體。第3圖中,含氧化鎢粉體製備方法200包含步驟210、步驟220與步驟230。 Please refer to FIG. 3, which is a flow chart of the steps of the method for preparing a tungsten oxide-containing powder according to another embodiment of the present invention. The method for preparing tungsten oxide-containing powder 200 is a physical mixing and polishing method. In the present embodiment, M is titanium, and how to prepare a tungsten oxide-containing powder by a physical mixing and polishing method. In FIG. 3, the tungsten oxide-containing powder preparation method 200 includes a step 210, a step 220, and a step 230.
步驟210是混合二氧化鈦、氧化鎢與溶劑並進行濕式研磨,以形成二氧化鈦/氧化鎢複合溶液,溶劑可為丁酮或水,水可為純水或去離子水,且步驟210可在10℃至50℃、以300rpm至1000rpm的轉速進行4小時至24小時。 Step 210 is mixing titanium dioxide, tungsten oxide and a solvent and performing wet grinding to form a titanium dioxide/tungsten oxide composite solution, the solvent may be methyl ethyl ketone or water, the water may be pure water or deionized water, and step 210 may be 10 ° C. The temperature is carried out at 50 ° C, from 300 rpm to 1000 rpm for 4 hours to 24 hours.
步驟220是加熱二氧化鈦/氧化鎢複合溶液,以形成氧化鎢鈦團塊。具體來說,可先進行乾燥步驟再進行燒結步驟,乾燥步驟可以50℃至150℃進行0.1小時至2小時,使二氧化鈦/氧化鎢複合溶液的溶劑蒸發以獲得乾燥粉末,燒結步驟可以700℃至1300℃進行1小時至8小時,使二氧化鈦與氧化鎢互相掺雜,以形成氧化鎢鈦團塊。 Step 220 is to heat the titanium dioxide/tungsten oxide composite solution to form a tungsten tungsten oxide agglomerate. Specifically, the drying step may be followed by a sintering step, and the drying step may be performed at 50 ° C to 150 ° C for 0.1 hour to 2 hours to evaporate the solvent of the titanium dioxide / tungsten oxide composite solution to obtain a dry powder, and the sintering step may be 700 ° C to Titanium dioxide and tungsten oxide are doped with each other at 1300 ° C for 1 hour to 8 hours to form a tungsten tungsten oxide agglomerate.
步驟230是研磨氧化鎢鈦團塊,以獲得含氧化鎢粉體。具體來說,步驟230可將氧化鎢鈦團塊先進行初步粉碎,再與溶劑混合,並進行濕式研磨,溶劑可為丁酮或水,水可為純水或去離子水,濕式研磨可在10℃至50℃、以300rpm至1000rpm的轉速進行4小時至24小時。 Step 230 is grinding the tungsten tungsten oxide agglomerate to obtain a tungsten oxide-containing powder. Specifically, in step 230, the tungsten tungsten oxide agglomerate may be firstly pulverized, mixed with a solvent, and subjected to wet grinding. The solvent may be methyl ethyl ketone or water, and the water may be pure water or deionized water, wet grinding. It can be carried out at 10 ° C to 50 ° C for 4 hours to 24 hours at 300 rpm to 1000 rpm.
步驟230的產物為一粉體漿料,即含氧化鎢粉體與溶劑的混合液,可直接以粉體漿料進行光波長選擇性遮蔽膜的製造,亦可將粉體漿料進行進一步的處理,例如噴霧造粒,以獲得乾燥的含氧化鎢粉體,關於噴霧造粒係習用技術,在此不予贅述。 The product of the step 230 is a powder slurry, that is, a mixture containing the tungsten oxide powder and the solvent, and the optical wavelength selective mask film can be directly processed by the powder slurry, and the powder slurry can be further processed. The treatment, for example, spray granulation, to obtain a dried tungsten oxide-containing powder, and the spray granulation conventional technique will not be described herein.
本發明的含氧化鎢粉體,對於波長為700nm至1100nm之光線具有遮蔽效果。已知近紅外光的波長範圍為780nm至3000nm,因此,本發明的含氧化鎢粉體可遮蔽部份的近紅外光,而可應用於製作近紅外線的反偵測物品,此外,藉由選擇M的種類、M的含量以及控制前述燒結步驟的溫度與時間,可調整含氧化鎢粉體顏色的深淺,使含氧化鎢粉體所製成的產品可滿足一般民生市場對織品或衣物的外觀需求,並有利於軍事人員於非綠色植被環境進行偽裝。 The tungsten oxide-containing powder of the present invention has a shielding effect on light having a wavelength of from 700 nm to 1100 nm. It is known that the near-infrared light has a wavelength ranging from 780 nm to 3000 nm. Therefore, the tungsten oxide-containing powder of the present invention can shield part of the near-infrared light, and can be applied to the near-infrared anti-detection article, and further, by selecting The type of M, the content of M, and the temperature and time of controlling the sintering step, the color of the tungsten oxide-containing powder can be adjusted, and the product made of the tungsten oxide powder can satisfy the appearance of the fabric or clothing in the general livelihood market. Demand and facilitate military personnel to camouflage in non-green vegetation environments.
請參照第4圖,其係繪示依照本發明又一實施方式的一種光波長選擇性遮蔽膜300的示意圖,光波長選擇性遮蔽膜300包含高分子塑料310以及複數個含氧化鎢粉體320,含氧化鎢粉體320分散於高分子塑料310中,關於含氧化鎢粉體320請參照前文,在此不予贅述。 Please refer to FIG. 4 , which is a schematic diagram of a light wavelength selective masking film 300 including a polymer plastic 310 and a plurality of tungsten oxide containing powders 320 according to still another embodiment of the present invention. The tungsten oxide-containing powder 320 is dispersed in the polymer plastic 310. For the tungsten oxide-containing powder 320, please refer to the foregoing and will not be described here.
光波長選擇性遮蔽膜300對於波長為700nm至1100nm之光線的遮蔽率可大於40%。依據本發明一實施例,光波長選擇性遮蔽膜300對於波長為700nm至1100nm之光線的遮蔽率可大於60%。光波長選擇性遮蔽膜300的厚度d可為0.005mm至1mm。 The light wavelength selective masking film 300 may have a shielding ratio of more than 40% for light having a wavelength of 700 nm to 1100 nm. According to an embodiment of the present invention, the optical wavelength selective masking film 300 may have a shielding ratio of more than 60% for light having a wavelength of 700 nm to 1100 nm. The thickness d of the light wavelength selective masking film 300 may be 0.005 mm to 1 mm.
光波長選擇性遮蔽膜300中,高分子塑料310的重量以100重量份計,含氧化鎢粉體320的重量可為1重量份至20重量份,依據本發明一實施例,含氧化鎢粉體320的重量可為1重量份至5重量份。高分子塑料310可選自聚氨基甲酸酯、熱可塑性彈性體、熱可塑性橡膠彈性體、熱塑性聚氨基甲酸酯、聚丙烯、聚乙烯、聚四氟乙烯、聚對苯二甲酸乙二酯及聚醯胺所組成之群組。依據本發明一實施例,高分子塑料310可為聚氨基甲酸酯。 In the light wavelength selective masking film 300, the weight of the polymer plastic 310 may be 1 part by weight to 20 parts by weight based on 100 parts by weight of the tungsten oxide powder 320, and according to an embodiment of the present invention, the tungsten oxide powder is contained. The body 320 may have a weight of from 1 part by weight to 5 parts by weight. The polymer plastic 310 may be selected from the group consisting of polyurethane, thermoplastic elastomer, thermoplastic rubber elastomer, thermoplastic polyurethane, polypropylene, polyethylene, polytetrafluoroethylene, polyethylene terephthalate. And a group consisting of polyamines. According to an embodiment of the invention, the polymer plastic 310 may be a polyurethane.
請參照第5圖,其係第4圖之光波長選擇性遮蔽膜300的製造方法400的步驟流程圖。第5圖中,光波長選擇性遮蔽膜300的製造方法400包含步驟410、步驟420、步驟430、步驟440與步驟450。 Please refer to FIG. 5, which is a flow chart of the method of manufacturing the optical wavelength selective masking film 300 of FIG. In FIG. 5, the method 400 for manufacturing the optical wavelength selective masking film 300 includes a step 410, a step 420, a step 430, a step 440, and a step 450.
步驟410是提供高分子塑料液體,高分子塑料液體包含高分子塑料310。前述高分子塑料液體可為高分子塑料310的熔融態或者為高分子塑料310 與溶劑相混所形成的高分子塑料溶液。依照本發明一實施例,高分子塑料溶液為聚氨基甲酸酯與丁酮或水相混所形成。 Step 410 is to provide a polymer plastic liquid, and the polymer plastic liquid comprises a polymer plastic 310. The polymer plastic liquid may be a molten state of the polymer plastic 310 or a polymer plastic 310 A polymer plastic solution formed by mixing with a solvent. According to an embodiment of the invention, the polymer plastic solution is formed by mixing a polyurethane with methyl ethyl ketone or water.
步驟420是提供粉體漿料,粉體漿料可為前述步驟150的產物或前述步驟230的產物,粉體漿料包含複數個含氧化鎢粉體320。粉體漿料中的溶劑可為丁酮或水,水可為純水或去離子水。 Step 420 is to provide a powder slurry. The powder slurry may be the product of the foregoing step 150 or the product of the foregoing step 230. The powder slurry comprises a plurality of tungsten oxide-containing powders 320. The solvent in the powder slurry may be methyl ethyl ketone or water, and the water may be pure water or deionized water.
步驟430是混合高分子塑料液體與粉體漿料以形成混合液。混合液中,高分子塑料310的重量以100重量份計,含氧化鎢粉體320的重量為1重量份至20重量份,且混合液的黏度可為20000cps至38000cps,其中黏度大小隨塗佈設備及塗佈方式有所不同,當黏度適中將使混合液的流動性適中,方便控制塗佈厚度、均勻性並維持穩定塗佈速度。 In step 430, the polymer plastic liquid and the powder slurry are mixed to form a mixed liquid. In the mixed solution, the weight of the polymer plastic 310 is 100 parts by weight, the weight of the tungsten oxide-containing powder 320 is 1 part by weight to 20 parts by weight, and the viscosity of the mixed liquid may be 20,000 cps to 38000 cps, wherein the viscosity varies depending on the coating. The equipment and coating method are different. When the viscosity is moderate, the fluidity of the mixture is moderate, and it is convenient to control the coating thickness and uniformity and maintain a stable coating speed.
步驟440是塗佈混合液於基材上以形成液狀膜。基材可為離型紙或布料層,當基材為離型紙,易於將基材與最終獲得的光波長選擇性遮蔽膜分離,而可得到獨立的光波長選擇性遮蔽膜,若基材為布料層,即可獲得本發明之選擇性遮光複合體。 Step 440 is to apply a mixed solution to the substrate to form a liquid film. The substrate can be a release paper or a cloth layer. When the substrate is a release paper, the substrate can be easily separated from the finally obtained wavelength selective masking film, and an independent light wavelength selective shielding film can be obtained. The layer, the selective light-shielding composite of the present invention can be obtained.
步驟450是乾燥液狀膜以獲得光波長選擇性遮蔽膜300。 Step 450 is to dry the liquid film to obtain a light wavelength selective masking film 300.
本發明的光波長選擇性遮蔽膜300具有以下優點:(1)藉由添加含氧化鎢粉體,可遮蔽部份的近紅外光,而可應用於製作軍事用的反偵察產品與民生用的反偷拍、反偷窺產品等。(2)藉由選擇M的種類、M的含量以及控制前述燒結步驟的溫度與時間,可調整含氧化鎢粉體顏色的深淺,進而可調整光波長選擇性遮蔽膜300的顏色,使其滿足一般民生市場對織品或衣物的外觀需求,並有利於軍事人員於非綠色植被環境,例如雪地,進行偽裝。(3)藉由將含氧化鎢粉體320分散於高分子塑料310中,含氧化鎢粉體320不易因清洗而脫落,意即 光波長選擇性遮蔽膜300不易因清洗而使功能消減。(4)光波長選擇性遮蔽膜300係使用塗佈方式形成,具有製程簡單的優點,並有利於製作大面積的光波長選擇性遮蔽膜300。(5)光波長選擇性遮蔽膜300可視實際需求塗佈於不同的基材上,可擴大其應用範圍。 The optical wavelength selective masking film 300 of the present invention has the following advantages: (1) by adding tungsten oxide powder, a part of the near-infrared light can be shielded, and can be applied to the production of anti-reconnaissance products for military use and livelihood. Anti-sneak shots, anti-peeping products, etc. (2) By selecting the type of M, the content of M, and controlling the temperature and time of the sintering step, the color of the tungsten oxide-containing powder can be adjusted, and the color of the selective wavelength masking film 300 can be adjusted to satisfy the color. The general needs of the people's livelihood market for fabrics or clothing, and for military personnel to camouflage in non-green vegetation environments, such as snow. (3) By dispersing the tungsten oxide-containing powder 320 in the polymer plastic 310, the tungsten oxide-containing powder 320 is less likely to fall off due to cleaning, that is, The light wavelength selective shielding film 300 is less likely to be functionally reduced by cleaning. (4) The optical wavelength selective masking film 300 is formed by a coating method, has an advantage of a simple process, and is advantageous for fabricating a large-area light wavelength selective masking film 300. (5) The optical wavelength selective masking film 300 can be applied to different substrates according to actual needs, and the application range can be expanded.
請參照第6圖,其係繪示依照本發明再一實施方式的一種選擇性遮光複合體500的剖面示意圖,選擇性遮光複合體500包含布料層600與光波長選擇性遮蔽膜300,布料層600包含二表面(圖未標號),光波長選擇性遮蔽膜覆300蓋布料層600的其中一表面(圖未標號)。關於光波長選擇性遮蔽膜300請參照前文,在此不予贅述。 Please refer to FIG. 6 , which is a cross-sectional view of a selective light-shielding composite 500 according to another embodiment of the present invention. The selective light-shielding composite 500 includes a cloth layer 600 and a light wavelength selective shielding film 300 , and a cloth layer The 600 includes two surfaces (not labeled), and the light wavelength selective masking film covers 300 one of the surfaces of the cloth layer 600 (not labeled). The light wavelength selective shielding film 300 is referred to the foregoing and will not be described herein.
布料層600可為針織物、梭織物及非織物,布料層600的材質可為但不限於聚酯、尼龍、聚丙烯、聚乙烯、聚丙烯腈、天絲棉(Lyocell)、嫘縈、毛、麻、蠶絲等。藉此,選擇性遮光複合體500可裁製成具有遮蔽部份的近紅外光的機能性衣物或寢具用織物等。 The fabric layer 600 can be a knitted fabric, a woven fabric and a non-woven fabric. The material of the fabric layer 600 can be, but not limited to, polyester, nylon, polypropylene, polyethylene, polyacrylonitrile, Lyocell, enamel, wool. , hemp, silk, etc. Thereby, the selective light-shielding composite 500 can be cut into a functional clothing having a shielding portion of near-infrared light, a fabric for bedding, or the like.
製備實施例1的光波長選擇性遮蔽膜。 The optical wavelength selective masking film of Example 1 was prepared.
首先,以化學還原方法製備含氧化鎢粉體,步驟如下。 First, a tungsten oxide-containing powder is prepared by a chemical reduction method as follows.
提供二氧化鈦(TiO2)溶膠凝膠:分別秤取0.752克的去離子水、7.209克的酒精與4.359克的硝酸後置入燒杯中,利用磁石攪拌機在常溫下混合攪拌10分鐘,以形成溶膠;分別秤取7.445克的正丁氧基鈦與7.890克的酒精後置入 燒杯中,利用磁石攪拌機在常溫下混合攪拌10分鐘,以形成含鈦凝膠;將溶膠與含鈦凝膠利用磁石攪拌機在常溫下混合攪拌24小時,以形成二氧化鈦溶膠凝膠。 Providing titanium dioxide (TiO2) sol gel: 0.752 g of deionized water, 7.209 g of alcohol and 4.359 g of nitric acid were respectively weighed into a beaker, and mixed with a magnet mixer at room temperature for 10 minutes to form a sol; Weighing 7.445 grams of titanium n-butoxide with 7.890 grams of alcohol and placing it In a beaker, the mixture was stirred at room temperature for 10 minutes using a magnet mixer to form a titanium-containing gel; the sol and the titanium-containing gel were mixed and stirred at room temperature for 24 hours using a magnet mixer to form a titania sol gel.
提供氧化鎢懸浮液:分別秤取10克的氧化鎢粉體、90克的酒精、2克的高分子型分散劑(型號為DS-06,購買自穩好高分子化學工業)與150克的鋯球後置入濕式珠磨機(型號:TYBS-2F2R;廠商:台溢實業有限公司)的球磨罐中,在室溫下,以300rpm的轉速進行8小時,以形成氧化鎢懸浮液。 Provide tungsten oxide suspension: 10 grams of tungsten oxide powder, 90 grams of alcohol, 2 grams of polymer dispersant (model DS-06, purchased self-stabilizing polymer chemical industry) and 150 grams The zirconium ball was placed in a ball mill jar of a wet bead mill (model: TYBS-2F2R; manufacturer: Taiyi Industrial Co., Ltd.) at room temperature for 8 hours at 300 rpm to form a tungsten oxide suspension.
混合二氧化鈦溶膠凝膠與氧化鎢懸浮液:二者混合比例為二氧化鈦的含量佔二氧化鈦與氧化鎢總含量的30wt%,利用磁石攪拌機在常溫下混合攪拌1小時,以形成二氧化鈦/氧化鎢複合溶液。 The titanium dioxide sol gel and the tungsten oxide suspension are mixed: the content of the titanium dioxide is 30% by weight of the total content of titanium dioxide and tungsten oxide, and the mixture is stirred and stirred at room temperature for 1 hour by a magnet mixer to form a titanium oxide/tungsten oxide composite solution.
加熱二氧化鈦/氧化鎢複合溶液:可分兩階段進行,先進行乾燥步驟,再進行燒結步驟。乾燥步驟是將二氧化鈦/氧化鎢複合溶液放入真空烘箱(型號:DOV-30;廠商:瀚基科技股份有限公司)中,以80℃進行0.5小時至1小時,使二氧化鈦/氧化鎢複合溶液的溶劑蒸發以獲得乾燥粉末。燒結步驟是以700℃的溫度進行1小時,使二氧化鈦與氧化鎢互相掺雜,以形成氧化鎢鈦團塊。 Heating the titanium dioxide/tungsten oxide composite solution: it can be carried out in two stages, followed by a drying step followed by a sintering step. The drying step is to place the titanium dioxide/tungsten oxide composite solution in a vacuum oven (model: DOV-30; manufacturer: 瀚基科技股份有限公司) at 80 ° C for 0.5 hour to 1 hour to make the titanium dioxide / tungsten oxide composite solution The solvent was evaporated to obtain a dry powder. The sintering step was carried out at a temperature of 700 ° C for 1 hour to dope the titanium oxide and the tungsten oxide to form a tungsten tungsten oxide agglomerate.
研磨氧化鎢鈦團塊:將氧化鎢鈦團塊先以研缽與杵進行初步粉碎,再分別秤取10克經初步粉碎的氧化鎢鈦團塊、90克的丁酮(試藥級,購買自景明化工)與150克的鋯球後置入濕式珠磨機(型號:TYBS-2F2R;廠商:台溢實業有限公司)的球磨罐中,在室溫下,以300rpm的轉速進行8小時,以形成包含含氧化鎢粉體的粉體漿料。 Grinding tungsten oxide titanium agglomerate: The tungsten tungsten oxide agglomerate is firstly pulverized with mortar and pestle, and then 10 g of the initially pulverized tungsten oxide titanium agglomerate and 90 g of methyl ethyl ketone are separately weighed (test drug grade, purchased From Jingming Chemical) and 150 g of zirconium ball into a wet bead mill (model: TYBS-2F2R; manufacturer: Taiyi Industrial Co., Ltd.) in a ball mill tank, at room temperature, at 300 rpm for 8 hours To form a powder slurry containing tungsten oxide-containing powder.
接著,製備光波長選擇性遮蔽膜,步驟如下。 Next, a light wavelength selective masking film is prepared, and the steps are as follows.
提供高分子塑料液體:在此高分子塑料液體為30克的溶劑型聚氨基甲酸酯(工業級;分子式為(C8H12N2O2.C6H14O3)X;4X21;購買自嘉良特化股份有限公司)。 Providing a polymer plastic liquid: the polymer plastic liquid is 30 g of a solvent-type polyurethane (industrial grade; the molecular formula is (C 8 H 12 N 2 O 2 .C 6 H 14 O 3 ) X ; 4 X 21; purchased from Jialiang Special Chemical Co., Ltd.).
提供粉體漿料:粉體漿料為前述以化學還原方法製備含氧化鎢粉體的最終產物,高分子塑料液體與粉體漿料的混合比例,以高分子塑料液體中的高分子塑料為100重量份計,粉體漿料中含氧化鎢粉體的重量為1重量份,以下將此氧鎢鈦粉體的含量以1wt%表式。 Providing a powder slurry: the powder slurry is the final product of preparing the tungsten oxide powder by the chemical reduction method, the mixing ratio of the polymer plastic liquid and the powder slurry, and the polymer plastic in the polymer plastic liquid is The weight of the tungsten oxide powder contained in the powder slurry was 1 part by weight based on 100 parts by weight, and the content of the oxytungsten titanium powder was expressed by 1 wt%.
混合高分子塑料液體與粉體漿料:係以行星攪拌脫泡機(型號:KK-50S;廠商:Mazerustar)以高速進行均勻混合與脫泡後以得到混合液。 The mixed polymer plastic liquid and the powder slurry were uniformly mixed and defoamed at a high speed by a planetary stirring defoaming machine (model: KK-50S; manufacturer: Mazerustar) to obtain a mixed liquid.
塗佈混合液於基材上:係將混合液倒在放置有離型紙的自動塗佈機(型號:Control Coater Model101;廠商:英國RK Print-Coat Instruments Ltd.)上,以等速向前推壓以形成厚度約30μm的液狀膜。 Coating the mixture on the substrate: pouring the mixture onto an automatic coater (Model: Control Coater Model 101; manufacturer: RK Print-Coat Instruments Ltd., UK) with release paper, pushing forward at a constant speed It was pressed to form a liquid film having a thickness of about 30 μm.
乾燥液狀膜:係將前述塗佈有液狀膜的離型紙放入真空烘箱(型號:DOV-30;廠商:瀚基科技股份有限公司)中,以80℃進行30分鐘,最後放入抽氣櫃中陰乾,即可獲得實施例1的光波長選擇性遮蔽膜(藉由重複前述塗佈混合液於基材上以及乾燥液狀膜的步驟,可控製所穫得的光波長選擇性遮蔽膜的厚度)。 Dry liquid film: The above-mentioned release paper coated with a liquid film is placed in a vacuum oven (model: DOV-30; manufacturer: Silicone Technology Co., Ltd.), at 80 ° C for 30 minutes, and finally put into pumping The light wavelength selective masking film of Example 1 can be obtained by drying in the gas cabinet (the wavelength selective masking film can be controlled by repeating the steps of coating the mixed liquid on the substrate and drying the liquid film) thickness of).
製備實施例2-13的光波長選擇性遮蔽膜:改變實施例1中二氧化鈦的含量佔二氧化鈦與氧化鎢總含量的比例(表一中簡記為二氧化鈦比例)、燒結步驟的溫度(表一中簡記為燒結溫度)及/或氧鎢鈦粉體與高分子塑料的比例關係(表一中簡記為氧鎢鈦粉體比例),列舉如下表一,其餘步驟與條件與實施例1相同,以獲得實施例2-13的波長選擇性遮蔽膜。 Preparation of the optical wavelength selective masking film of Examples 2-13: changing the ratio of the content of titanium dioxide in Example 1 to the total content of titanium oxide and tungsten oxide (abbreviated as titanium dioxide ratio in Table 1), the temperature of the sintering step (abbreviation in Table 1) The sintering temperature) and/or the ratio of the tungsten-tungsten titanium powder to the polymer plastic (abbreviated as the proportion of the tungsten-oxygen titanium powder in Table 1) are listed in Table 1 below, and the remaining steps and conditions are the same as in Example 1 to obtain Wavelength selective masking films of Examples 2-13.
請參照第7圖,其係純氧化鎢與實施例1、實施例4與實施例7的粉碎的氧化鎢鈦團塊的外觀圖,其中(a)為純氧化鎢的外觀圖,(b)、(c)與(d)分別是將實施例1、實施例4與實施例7進行至加熱二氧化鈦/氧化鎢複合溶液步驟所得的氧化鎢鈦團塊進行初步粉碎後所得的外觀圖。由第7圖可知,本發明的含氧化鎢粉體可藉由M的存在,改變純氧化鎢的顏色,此外,調整燒結溫度,亦可改變含氧化鎢粉體的顏色。 Please refer to FIG. 7 , which is an external view of the pure tungsten oxide and the pulverized tungsten-titanium oxide agglomerates of the first embodiment, the fourth embodiment and the seventh embodiment, wherein (a) is an external view of pure tungsten oxide, (b) (c) and (d) are external appearances obtained by subjecting Example 1, Example 4, and Example 7 to the preliminary pulverization of the tungsten-titanium oxide agglomerate obtained by the step of heating the titanium oxide/tungsten oxide composite solution. As can be seen from Fig. 7, the tungsten oxide-containing powder of the present invention can change the color of pure tungsten oxide by the presence of M, and can also change the color of the tungsten oxide-containing powder by adjusting the sintering temperature.
(一)光波長選擇性遮蔽膜對波長為700nm至1100nm之光線的遮蔽率分析:將實施例1-13的光波長選擇性遮蔽膜裁切成長×寬為5cm×3cm之大小,之後放入紫外光/可見光-近紅外光光譜儀(UV-Vis-NIR spectrotometer;型號:V-670;廠商:Jasco)的夾具中,測試波長為340nm至2500nm的穿透率,並由穿透率計算出遮蔽率,計算公式如下:遮蔽率=(100-光穿透率)。並將實施例1-13的光波長選擇性遮蔽對波長為700nm至1100nm之遮蔽率列於表二。由表二可知,實施例1-13的光波長選擇性遮蔽膜對於波長為700nm至1100nm之光線的遮蔽率皆大於60%。 (1) Shielding rate analysis of light wavelength selective masking film for light having a wavelength of 700 nm to 1100 nm: The light wavelength selective masking film of Example 1-13 was cut into a length × width of 5 cm × 3 cm, and then placed. In a fixture of UV-Vis-NIR spectrotometer (Model: V-670; Vendor: Jasco), the transmittance is measured at a wavelength of 340 nm to 2500 nm, and the transmittance is calculated by the transmittance. The rate is calculated as follows: masking rate = (100 - light transmittance). The optical wavelength selective masking of Examples 1-13 and the masking ratios of wavelengths of 700 nm to 1100 nm are listed in Table 2. As can be seen from Table 2, the light wavelength selective masking films of Examples 1-13 have a shielding ratio of more than 60% for light having a wavelength of 700 nm to 1100 nm.
(二)光波長選擇性遮蔽膜之拉伸性質分析:依照ASTM D638之標準進行測試,試驗規格為Type V進行拉伸之試驗,拉伸速率為100±25%mm/min,試驗結果列舉於表三。由表三可知,當M為鈦時,添加含氧化鎢粉體,可進一步提升光波長選擇性遮蔽膜的拉伸強度。 (2) Analysis of tensile properties of optical wavelength selective masking film: Tested according to the standard of ASTM D638, the test specification is tensile test of Type V, and the tensile rate is 100±25% mm/min. The test results are listed in Table III. As can be seen from Table 3, when M is titanium, the addition of the tungsten oxide-containing powder further enhances the tensile strength of the optical wavelength selective masking film.
(三)光波長選擇性遮蔽膜的熱影像溫差分析:熱影像溫差量測方式係以FTTS中FTTS-FA-010規範為標準並加以改良,將實施例1、4、7、10與12的光波長選擇性遮蔽膜裁切成面積約100cm2的圓形試樣,記錄各試樣的初始溫度為T0,架設500W鹵素燈,鹵素燈照射距離試樣高度約300mm,照射角度為90度,照射600秒,記錄其溫度為T10,記錄其溫度為T10,關閉鹵素燈冷卻10分鐘,記錄其溫度為T20,將量測結果列於表四。由表四可知,實施例1、4、7、10與12的光波長選擇性遮蔽膜經過10分鐘的照射與經過10分鐘的冷卻後,其溫度均 高於初始溫度3℃以上,顯示實施例1、4、7、10與12的光波長選擇性遮蔽膜具有蓄熱保溫的功效。換言之,當M為鈦時,添加含氧化鎢粉體,可進一步提升光波長選擇性遮蔽膜的蓄熱保溫功效。 (III) Thermal image temperature difference analysis of optical wavelength selective masking film: The thermal image temperature difference measuring method is based on the FTTS-FA-010 specification in FTTS and improved, and the examples 1, 4, 7, 10 and 12 are The light wavelength selective shielding film is cut into a circular sample with an area of about 100 cm 2 , and the initial temperature of each sample is recorded as T0, and a 500 W halogen lamp is mounted. The height of the halogen lamp is about 300 mm, and the irradiation angle is 90 degrees. For 600 seconds, record the temperature as T10, record the temperature as T10, turn off the halogen lamp for 10 minutes, record the temperature as T20, and list the measurement results in Table 4. As can be seen from Table 4, the optical wavelength selective masking films of Examples 1, 4, 7, 10 and 12 were irradiated for 10 minutes and cooled for 10 minutes. Above the initial temperature of 3 ° C or more, the optical wavelength selective masking films of Examples 1, 4, 7, 10 and 12 were shown to have the effect of heat storage and heat retention. In other words, when M is titanium, the addition of the tungsten oxide-containing powder further enhances the heat storage and heat retention effect of the optical wavelength selective masking film.
雖然本發明已以實施方式揭露如上,然其並非用以限定本發明,任何熟習此技藝者,在不脫離本發明之精神和範圍內,當可作各種之更動與潤飾,因此本發明之保護範圍當視後附之申請專利範圍所界定者為準。 Although the present invention has been disclosed in the above embodiments, it is not intended to limit the present invention, and the present invention can be modified and modified without departing from the spirit and scope of the present invention. The scope is subject to the definition of the scope of the patent application attached.
300‧‧‧光波長選擇性遮蔽膜 300‧‧‧Light wavelength selective masking film
310‧‧‧高分子塑料 310‧‧‧Polymer plastic
320‧‧‧含氧化鎢粉體 320‧‧‧Tungsten oxide powder
d‧‧‧厚度 D‧‧‧thickness
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