CN103996456B - A highly abrasive resistant nano-metal transparent conductive film production method - Google Patents

A highly abrasive resistant nano-metal transparent conductive film production method Download PDF

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CN103996456B
CN103996456B CN 201410188864 CN201410188864A CN103996456B CN 103996456 B CN103996456 B CN 103996456B CN 201410188864 CN201410188864 CN 201410188864 CN 201410188864 A CN201410188864 A CN 201410188864A CN 103996456 B CN103996456 B CN 103996456B
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魏寅
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天津宝兴威科技股份有限公司
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Abstract

本发明涉及一种高耐磨纳米金属透明导电膜的制造方法,其特征在于:制造步骤如下:(1)将纳米金属制成初始悬浊液;(2)制备添加剂;(3)将添加剂加入纳米金属初始悬浮液中,配成涂布纳米金属墨水;(4)将配好的纳米金属墨水以旋涂、狭缝式涂布、微凹板式涂布或喷涂方式涂布至基板上,然后在烘箱中100度预烘烤5分钟~20分钟后,再放进烘箱中140度烘烤5分钟~20分钟,此时得到高硬度、致密性好的导电层;(5)最后将带有导电层的基板经过轧光机,得到雾度较低的导电层。 The present invention relates to a method for producing a nano-metal high wear resistance of the transparent conductive film, wherein: the manufacturing steps are as follows: (1) the initial suspension formed nano metal; Preparation of (2) an additive; (3) adding an additive the initial suspension of the nano metal, nano-metal ink formulated coating; (4) nano-metal ink with a good spin coating, slit coating, micro gravure coating or spraying the plate coated onto a substrate, then in an oven to 100 degrees prebaking 5 to 20 minutes, and then placed in an oven to 140 degrees bake 5 to 20 minutes, this time to obtain a high hardness, good compactness conductive layer; (5) Finally, with the conductive layer through the substrate calender, to give a conductive layer low haze. 采用一步法涂布工艺提高薄膜的硬度、环境耐受性以及降低薄膜雾度。 One-step coating process increases the hardness, environmental resistance and reduced film haze of the film.

Description

一种高耐磨纳米金属透明导电膜的制造方法 A highly abrasive resistant nano-metal transparent conductive film production method

技术领域 FIELD

[0001] 本发明涉及改进纳米金属涂布液配方,特别涉及改进涂布液配方后,使用一步涂布法制造高耐磨纳米金属导电膜。 [0001] The present invention relates to an improved metal coated nano-fluid formulation, particularly to the improved liquid coating formulation, the coating method used for producing high wear-step nano metal conductive film.

背景技术 Background technique

[0002] 目前,透明导电薄基板主要有金属氧化物基板、碳纳米管或者石墨烯基板。 [0002] Currently, the transparent conductive metal oxide thin substrate main substrate, the substrate graphene or carbon nanotubes. 纳米金属基板、导电聚合物基板,其中铟锡氧化物(ITO)基板最为广泛应用。 Nano-metal substrate, a conductive polymer substrate, wherein the indium tin oxide (ITO) substrates most widely used. 透明导电基板的主要性能指标有导电性和可见光透明度,大部分导电基板需要平衡两者之间的性能,往往高导电性基板的透过率较低,高透过率的基板导电性较低,金属氧化物基板、碳纳米管或者石墨烯基板、导电聚合物基板往往不能同时满足这两者的高要求,如ITO导电膜在方阻50 Ω/口的条件下,其透过率低于80%,而后三者的方阻很少能做到150 Ω /口。 The main performance indexes of the transparent conductive substrate and a conductive visible light transparency, the majority of the conductive substrate to balance between the two properties, tend to have lower transmittance highly conductive substrate, a conductive substrate low high transmittance, a metal oxide substrate, the substrate graphene or carbon nanotubes, electrically conductive polymer substrate often can not meet the high demands of both, such as ITO conductive film side under the condition of 50 Ω / barrier ports, which transmittance is lower than 80 %, then the three parties to provide minimal resistance 150 Ω / port.

[0003] 将纳米导电金属线与水性粘合剂配制成涂布墨水,经过高精密涂布机将纳米导电金属线涂布于柔性基板上,烘烤后形成纳米级厚的纳米导电金属线薄膜,纳米金属线之间互相搭接,形成导电路径,而空隙处可见光完全透过,形成高透明导电膜。 [0003] The conductive nano metal wires coated with the aqueous binder formulation as ink, through high-precision coater conductive nano metal wires coated onto a flexible substrate, forming nanometer thick film conductive nano metal wires after baking , overlap each other between the nano-metal wires to form a conductive path, and the gap at the visible light completely transparent, a transparent conductive film is formed high. 导电金属选择具有最佳的导电率以及柔韧性,所以涂布成的透明导电薄膜具有很低的方阻和耐弯折性,同时兼有极高的透过率,如当方阻为50 Ω/□时,其可见光透过率为90%。 Conductive metal selected having the best electrical conductivity and flexibility, the transparent conductive film in a square having a low resistance, and excellent bending resistance, with both a high transmittance, such as when the sheet resistance of 50 Ω / when □, the visible light transmittance thereof was 90%.

[0004] 将纳米导电金属线与水性粘合剂配制成涂布墨水,涂布于透明基板,烘烤后将溶剂蒸发,留下粘合剂将纳米金属线嵌入其中,形成导电薄膜,由于目前所使用的粘合剂形成薄膜后,表面硬度低,而透明导电薄膜的膜表面硬度会影响其应用于产品的良率,比如应用于制造触摸屏,不良率重要因素之一就是制造过程中膜硬度不足造成的划伤或凹陷;另外薄膜的环境耐受性也比较差,易受潮气及氧化性气体的浸润,产生霉斑及纳米金属被氧化,无法应用于电子产品的制造;还有一个缺陷是由于水性粘合剂烘烤后不是完全平整的,具有高低起伏的平面,所以光入射自后,产生较大的雾度,目前的解决办法是在导电层上面再涂布一层保护层,这样薄膜的表面电阻就会增加很多,至少两倍以上,不符合于电子产品低电阻的要求。 [0004] The conductive nano metal wires coated with the aqueous binder formulation as ink, applied to a transparent substrate, baked The solvent was evaporated, leaving a pressure-sensitive adhesive nano metal wires embedded therein, the conductive thin film is formed, due to the current after forming a thin film of adhesive used, a low surface hardness, and the transparent conductive thin film surface hardness can affect product yield applied, such as a touch screen applied to the manufacturing, the defect rate is an important factor in the manufacturing process of the film hardness scratches caused by insufficient or recesses; additional environmental resistance film is also relatively poor, and is susceptible to moisture infiltration oxidizing gas generating and mildew nano metal is oxidized, can not be applied to the manufacture of electronic products; there is a defect Since the adhesive is an aqueous baking is not perfectly flat, the plane having ups and downs, so that the light incident from the rear, the greater the haze, the current solution is then coated with a protective layer above the conductive layer, Thus the surface resistance of the film will increase a lot, at least twice, electronic products do not meet the requirements of low resistance.

发明内容 SUMMARY

[0005] 本发明可以解决以上问题,通过优化纳米金属悬浮液的配方,将水性蜡及硅氧化物添加至纳米导电金属线与水性粘合剂配制成涂布墨水中,可以使涂布的导电膜具有极低的摩擦系数,产生极佳的滑度和抗划伤效果,并改进涂布工艺条件,采用一步法涂布工艺提高薄膜的硬度、环境耐受性以及降低薄膜雾度。 [0005] The present invention can solve the above problems, by optimizing the metal nano-suspension formulation, adding to the aqueous wax and a silicon oxide nano-conductor wires coated with the aqueous binder formulation as ink, a conductive coating can be made film having a low coefficient of friction, produce excellent smoothness and scratch effect, and to improve the coating process conditions, the one-step process to improve the coating hardness, environmental resistance and reduced film haze of the film. 一种高耐磨纳米金属透明导电膜的制造方法,制造步骤如下: A method for producing a nano-metal high wear resistance of the transparent conductive film, the manufacturing steps are as follows:

[0006] (1)将纳米金属制成初始悬浊液;纳米金属可以是纳米金线、铜线或银线或者是三者任意组合,纳米金属线含量0.1〜1 %,优选0.1 %〜0.6%,线长应在0.1〜ΐοομπι,优选20um〜40μηι,线径应在IOnm〜100nm,优选10〜20nm;纳米金属的初始悬浮液的溶剂由水、乙醇、丙酮、乙二醇、丙二醇、丙三醇和异丙醇组成; [0006] (1) made of metal nano initial suspension; nano nano metal may be gold, silver or copper or any combination of the three, the content of the nano metal wires 0.1~1%, preferably 0.1% ~0.6 %, the line length should 0.1~ΐοομπι, preferably 20um~40μηι, diameter should IOnm~100nm, preferably 10~20nm; nano metal initial solvent suspension of water, ethanol, acetone, ethylene glycol, propylene glycol, triols and isopropyl alcohol;

[0007] (2)制备添加剂,添加剂包括水性粘合剂、硅氧化物水溶胶、水性蜡、表面活性剂和热固化透明树脂;水性粘合剂包括羧甲基纤维素钠、羧丙基甲基纤维素、羧乙基纤维素、聚乙烯醇和羟丙基甲基纤维素;硅氧化物包括二氧化硅、硅酸盐和水性硅油;水性蜡包括改性聚乙烯蜡、聚四氟乙烯蜡和改性聚酰胺蜡;表面活性剂包括十二烷基硫酸钠、聚乙二醇、烷基糖苷、椰油酸二乙醇酰胺和聚乙二醇辛基苯基醚;; [0007] Preparation of (2) an additive comprising an aqueous binder, the silicon oxide hydrosol, aqueous wax, a surfactant, and a transparent thermosetting resin; aqueous binder comprises sodium carboxymethyl cellulose, carboxypropyl A cellulose, carboxyethyl cellulose, polyvinyl alcohol, and hydroxypropylmethylcellulose; silicon oxides include silica, silicates, and aqueous silicone oils; aqueous wax comprises a modified polyethylene wax, polytetrafluoroethylene wax and modified polyamide waxes; surfactants include sodium lauryl sulfate, polyethylene glycol, alkyl glucoside, coconut diethanolamide and polyethylene glycol octylphenyl ether ;;

[0008] (3)将添加剂加入纳米金属初始悬浮液中,配成涂布纳米金属墨水,粘度20cP〜IOOcP,其中纳米金属的含量为0.05〜0.6%,水性粘合剂的含量为0.1〜1 %,硅氧化物含量为0.2〜2 %,水性蜡粉含量0.2〜2 %,表面活性剂含量0.01〜0.1 %。 [0008] (3) The nano-sized metal additives to the initial suspension, nano-metal ink formulated coating viscosity 20cP~IOOcP, wherein the content of the nano metal is 0.05~0.6%, content of the aqueous binder is 0.1~1 %, a silicon oxide content of 0.2~2% 0.2~2% aqueous wax content, surfactant content 0.01~0.1%. ;

[0009] ⑷将配好的纳米金属墨水以旋涂、狭缝式涂布、微凹板式涂布或喷涂方式涂布至基板上,然后在烘箱中100度预烘烤5分钟〜20分钟后,再放进烘箱中140度烘烤5分钟〜20分钟,此时得到高硬度、致密性好的导电层; After [0009] ⑷ nano metal ink with a good spin coating, slit coating, micro gravure coating or spraying the plate coated onto the substrate, and then pre-baked in an oven at 100 degrees for 5 minutes ~ 20 minutes , and then into the 140 degree oven baked 5 minutes ~ 20 minutes at which time high hardness, good compactness conductive layer;

[0010] (5)最后将带有导电层的基板经过乳光机,得到雾度较低的导电层。 [0010] (5) Finally, the substrate with conductive layers through the opalescent machine to obtain a conductive layer low haze.

[0011] 步骤⑷所述基板是刚性或柔性的,刚性的基板可以是玻璃或加硬的聚碳酸酯;柔性基板可以是聚酯、聚烯烃或聚乙烯。 [0011] Step ⑷ the substrate is rigid or flexible, a rigid substrate may be a glass or hardened polycarbonate; flexible substrate may be a polyester, polyolefin or polyethylene.

[0012] 本发明的有益效果是:可通过优化纳米金属悬浮液的配方,将水性蜡及硅氧化物添加至纳米导电金属线与水性粘合剂配制成涂布墨水中,可以使其具有极低的摩擦系数,使得涂料和印刷油墨里有极佳的滑度和抗划伤效果,并改进涂布工艺条件,采用一步法涂布工艺提高薄膜的硬度、环境耐受性以及降低薄膜雾度。 [0012] Advantageous effects of the invention are: by optimizing the suspension of metal nano-formulations, adding to the aqueous wax and a silicon oxide nano wire and a conductive metal coating formulated as an aqueous ink binder, it can have a very low coefficient of friction, such coatings and printing inks, there are excellent effects of slip and scratch resistance, and to improve the conditions of the coating process, one-step coating process increases the hardness, environmental resistance and reduced film haze of the film .

[0013] [0013]

Figure CN103996456BD00041

具体实施例[0014] 实施例一: Specific Example [0014] Example a:

[0015] 柔性基板选择聚对苯二甲酸乙二醇酯(Polyethylene terephthalate,PET) [0015] The flexible substrate is polyethylene terephthalate (Polyethylene terephthalate, PET)

[0016] 导电层涂布液的配方是:纳米金属线选择纳米银线,平均线长应在20μπι,平均线径应在35nm,纳米银线含量0.1%,0.34%聚乙烯醇,0.2%二氧化硅,0.5%的氧化聚乙烯蜡、0.01 %聚乙二醇辛基苯基醚。 [0016] The conductive layer coating fluid formulation is: selected nano metal wires silver nanowires average length should be in the 20μπι, 35nm average diameter should, silver nanowires content of 0.1%, 0.34% polyvinyl alcohol, 0.2% silica, oxidized polyethylene wax 0.5%, 0.01% polyethylene glycol octylphenyl ether. 具体配制方法是取250g的0.2%纳米银线初始悬浮液,此悬浮液的溶剂是纯水,边搅拌边向其中加入215g的0.8 %的聚乙烯醇水溶液,最后分别加入IOg的10 %二氧化硅水溶胶、25g的10 %氧化聚乙烯蜡水溶胶、0.05g的聚乙二醇辛基苯基醚充分搅拌后配制完成。 Methods of formulation are specifically taken 250g of 0.2% silver nanowire initial suspension, this suspension is a solvent of pure water, was added thereto with stirring 215g of a 0.8% aqueous solution of polyvinyl alcohol, and finally were added 10% of IOg dioxide aqueous silica sol, after 25g of a 10% aqueous oxidized polyethylene wax sol, 0.05 g of polyethylene glycol octylphenyl ether thoroughly stirred to complete the formulation.

[0017] 将配好的涂布墨水以旋涂方式涂布至基板上,然后在烘箱中100度预烘烤5分钟在放进烘箱中140度烘烤20分钟,此时得到高硬度、致密性好的导电层,最后将带有导电层的基板经过乳光机,得到雾度较低的导电层。 [0017] In the ink coating with a good spin coating applied onto a substrate and then in an oven at 100 degrees for 5 minutes pre-baked into 140 degree oven for 20 minutes to obtain a high hardness at this time, densified good conductive layer, the substrate with the conductive layer and finally through opalescent machine to obtain a conductive layer low haze.

[0018] 实施例二: [0018] Example II:

[0019] 柔性基板选择聚对苯二甲酸乙二醇酯(Polyethylene terephthalate,PET) [0019] The flexible substrate is polyethylene terephthalate (Polyethylene terephthalate, PET)

[0020] 涂布液的配方是:纳米金属线选择纳米银线,平均线长应在20μπι,平均线径应在35nm,纳米银线含量0.1 %,0.34%羧丙基甲基纤维素,0.2%二氧化硅,0.3%的氧化聚乙烯蜡、0.2%的聚四氟乙烯蜡、0.01 %聚乙二醇辛基苯基醚。 [0020] Formulation of the coating solution is: selected nano metal wires silver nanowires average length should be in the 20μπι, 35nm average diameter should, silver nanowires content of 0.1%, 0.34% hydroxypropylmethylcellulose, 0.2 % silica, 0.3% of oxidized polyethylene wax, polytetrafluoroethylene wax, 0.2%, 0.01% polyethylene glycol octylphenyl ether. 具体配制方法是取250g的0.2%纳米银线初始悬浮液,此悬浮液的溶剂是纯水,边搅拌边向其中加入215g的0.8 %的羧丙基甲基纤维素水溶液,最后分别加入IOg的10 %二氧化硅水溶胶、25g的6 %氧化聚乙烯蜡和4 %聚四氟乙烯蜡混合水溶胶、0.05g的聚乙二醇辛基苯基醚充分搅拌后配制完成。 Methods of formulation are specifically taken 250g of 0.2% silver nanowire initial suspension, this suspension is a solvent of pure water, was added thereto with stirring 215g of a 0.8% aqueous solution of hydroxypropylmethyl cellulose, were added and finally the IOg 10% silica hydrosol, 25g of 6% and 4% wax, oxidized polyethylene wax, polytetrafluoroethylene hydrosol mixture, prepared after the completion of 0.05g polyethylene glycol octylphenyl ether thoroughly stirred.

[0021] 将配好的涂布墨水以旋涂方式涂布至基板上,然后在烘箱中100度预烘烤5分钟在放进烘箱中140度烘烤20分钟,此时得到高硬度、致密性好的导电层,最后将带有导电层的基板经过乳光机,得到雾度较低的导电层。 [0021] In the ink coating with a good spin coating applied onto a substrate and then in an oven at 100 degrees for 5 minutes pre-baked into 140 degree oven for 20 minutes to obtain a high hardness at this time, densified good conductive layer, the substrate with the conductive layer and finally through opalescent machine to obtain a conductive layer low haze.

[0022] 以上所述,仅为本发明的具体实施方式和优选实施例,熟悉本领域的技术人员在本发明揭露的范围内,可轻易想到的变化,都应涵盖在发明的保护范围之内。 [0022] The above are only specific embodiments of the present invention and preferred embodiments, those skilled in the art within the scope of the present invention is disclosed, variations easily occur, should fall within the scope of the claimed invention .

Claims (2)

  1. 1. 一种高耐磨纳米金属透明导电膜的制造方法,其特征在于:制造步骤如下, (1) 将纳米金属制成初始悬池液;纳米金属是纳米金线或铜线或银线,纳米金属线含量0· 1〜1%,线长是在0· 1〜ΙΟΟμπι,线径是在IOnm〜IOOnm;纳米金属的初始悬池液的溶剂由水、乙醇、丙酮、乙二醇、丙二醇、丙三醇和异丙醇组成; (2) 制备添加剂,添加剂包括水性粘合剂、硅氧化物水溶胶、水性蜡、表面活性剂和热固化透明树脂;水性粘合剂为聚乙烯醇;硅氧化物是二氧化硅;水性蜡为改性聚乙烯蜡;表面活性剂为聚乙二醇辛基苯基醚; (3) 将添加剂加入纳米金属初始悬池液中,配成涂布纳米金属墨水,粘度20cP〜100cP, 其中纳米金属的含量为0.05〜0.6 %,水性粘合剂的含量为0.1〜1 %,硅氧化物含量为0.2 〜2 %,水性蜡粉含量0.2〜2 %,表面活性剂含量0.01〜0.1 % ; ⑷将配好的纳米金属墨 A method for producing a highly abrasive resistant nano-metal transparent conductive film, wherein: the manufacturing steps, (1) the metal nano initial cell suspension liquid; nano metal nano gold or silver or copper, the content of the nano metal wires 1~1 0.5%, the line length is at 0 · 1~ΙΟΟμπι, in diameter IOnm~IOOnm; initial cell suspension solution of metal nano solvent consisting of water, ethanol, acetone, ethylene glycol, propylene glycol , glycerol, and isopropanol; preparation of (2) an additive comprising an aqueous binder, the silicon oxide hydrosol, aqueous wax, a surfactant, and a transparent thermosetting resin; aqueous binder is a polyvinyl alcohol; silicon oxide is silica; aqueous wax is a modified polyethylene wax; the surfactant is a polyethylene glycol octylphenyl ether; (3) adding the additive metal nano initial cell suspension solution, dubbed nano metal coating ink viscosity 20cP~100cP, wherein the content of the nano metal is 0.05~0.6%, content of the aqueous binder is 0.1~1%, a silicon oxide content of 0.2 ~ 2%, 0.2~2% aqueous wax content, surface surfactant content 0.01~0.1%; ⑷ nano metal ink with a good 以旋涂、狭缝式涂布、微凹板式涂布或喷涂方式涂布至基板上,然后在烘箱中100度预烘烤5分钟〜20分钟后,再放进烘箱中140度烘烤5分钟〜20分钟, 此时得到高硬度、致密性好的导电层; ⑸最后将带有导电层的基板经过乳光机,得到雾度较低的导电层。 Spin coating, slit coating, micro gravure coating or spraying the plate coated onto a substrate, and then in an oven at 100 degrees prebaking 5 minutes ~ 20 minutes, and then placed in an oven bake 140 degree 5 minutes ~ 20 minutes, at high hardness, good compactness conductive layer; ⑸ Finally, the substrate with conductive layers through the opalescent machine to obtain a conductive layer low haze.
  2. 2. 根据权利要求1所述的一种高耐磨纳米金属透明导电膜的制造方法,其特征在于: 步骤⑷所述基板是刚性或柔性的,刚性的基板是玻璃或加硬的聚碳酸酯;柔性基板是聚酯或聚烯烃。 The method according to claim 1 for producing a high wear-resistant nano-metal transparent conductive film as claimed in claim, wherein: said step of ⑷ rigid or flexible substrate is a rigid substrate is a glass or hardened polycarbonate ; flexible substrate is a polyolefin or a polyester.
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