CN105399343A - 一种光学玻璃复合膜及镀膜工艺 - Google Patents

一种光学玻璃复合膜及镀膜工艺 Download PDF

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CN105399343A
CN105399343A CN201510804442.6A CN201510804442A CN105399343A CN 105399343 A CN105399343 A CN 105399343A CN 201510804442 A CN201510804442 A CN 201510804442A CN 105399343 A CN105399343 A CN 105399343A
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奚建安
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Changshu Optical Instrument Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/3411Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
    • C03C17/3429Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating
    • C03C17/3447Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating comprising a halide
    • C03C17/3452Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating comprising a halide comprising a fluoride
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/70Properties of coatings
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/70Properties of coatings
    • C03C2217/78Coatings specially designed to be durable, e.g. scratch-resistant
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00Methods for coating glass
    • C03C2218/10Deposition methods
    • C03C2218/15Deposition methods from the vapour phase
    • C03C2218/151Deposition methods from the vapour phase by vacuum evaporation
    • CCHEMISTRY; METALLURGY
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    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00Methods for coating glass
    • C03C2218/10Deposition methods
    • C03C2218/15Deposition methods from the vapour phase
    • C03C2218/154Deposition methods from the vapour phase by sputtering
    • C03C2218/156Deposition methods from the vapour phase by sputtering by magnetron sputtering
    • CCHEMISTRY; METALLURGY
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3225Yttrium oxide or oxide-forming salts thereof

Abstract

本发明公开了一种光学玻璃复合膜,从里至外共3层,第一层为氟化镁膜,第二层为二氧化硅膜,第三层为二氧化锆膜;本发明还公开了该光学玻璃复合膜的镀膜工艺,采用电阻蒸镀法镀氟化镁膜,采用磁控溅射法镀二氧化硅膜,采用电子束热蒸法镀二氧化锆膜。本发明公开的光学玻璃复合膜可较大地提高光学玻璃的透光率和折射率,并且具有较好的防划耐磨性。

Description

一种光学玻璃复合膜及镀膜工艺
技术领域
本发明涉及一种光学玻璃复合膜及镀膜工艺。
背景技术
光学玻璃是用于制造光学仪器或机械系统中的透镜、棱镜、反射镜等的玻璃材料。近年来,随着数码相机、数字摄像机、照相手机等的日益流行,对光学玻璃的需求量也越来越大,并且对光学玻璃的性能也提出了更高的要求。
为了得到理想的光学常数,提高玻璃折射率和透光率,通常会在光学玻璃表面镀膜,镀膜的种类有很多,按材料可分为金属膜、氧化物膜等,按功能可分为增透膜、反射膜、偏振膜等。而目前市场上出现了不少的复合膜,但镀膜的性能方面仍然比较单一。
发明内容
本发明的目的在于克服现有技术中存在的缺陷,提供了一种光学玻璃复合膜,以光学玻璃基体为底,从里至外共3层,第一层为氟化镁膜,直接镀在光学玻璃上,第二层为二氧化硅膜,镀在氟化镁膜上,第三层为二氧化锆膜,镀在二氧化硅膜上;
本发明还提供了上述光学玻璃复合膜的镀膜工艺,包括以下步骤:
1)真空镀膜设备中抽真空,使真空度达到8×10-4~10×10-4Pa;
2)在光学玻璃基体上蒸镀一层氟化镁膜,蒸镀条件为:采用钨或钼作为蒸发源材料,蒸发电流设为100A,时间为15min;
3)在氟化镁膜的基础上磁控溅射一层二氧化硅膜,条件为:采用硅为靶材,在真空镀膜设备中通入氩气作为溅射气体,通入氧气作为反应气体,氩气流量为30sccm,设备内压力0.1~1.0pa,氩气和氧气的比例为1:4;
4)在二氧化硅膜的基础上通过电子束热蒸的方式镀上二氧化锆膜,条件为:烘烤温度设为300℃,时间为1h,电子束流为100mA。
更具体地,氟化镁为晶体状,由水合氟化镁经机械破碎、烘干和低温真空脱水后作为镀膜靶材;晶体氟化镁在蒸镀前进行预熔,预熔电流为60A,预熔时间为10min。
更具体地,二氧化锆采用氧化钇进行稳定后再作为镀膜靶材,稳定包括以下步骤:
1)以二氧化锆和氧化钇粉料为原料,二氧化锆的摩尔百分比为氧化钇的20倍,混合均匀后添加聚乙烯醇结合剂使粉料团聚,造粒成型;
2)对颗粒料进行预烧,预烧温度为1200°C;
3)在真空烧结炉中烧结,然后自然冷却降温至室温。
更具体地,本发明中所使用的靶材纯度均为99.99%以上。
本发明的优点和有益效果在于:
1)提高了光学玻璃的透光性和折射率;
2)由于氟化镁的材质比较软,因此在其基础上镀上二氧化硅可起到增透和保护的作用,而在其上再镀上一层二氧化锆膜可使玻璃表面变得坚硬,可达到防划防磨损的目的。
具体实施方式
下面结合实施例,对本发明的具体实施方式作进一步描述。以下实施例仅用于更加清楚地说明本发明的技术方案,而不能以此来限制本发明的保护范围。
本发明具体实施的技术方案是:
一种光学玻璃复合膜,以光学玻璃基体为底,从里至外共3层,第一层为氟化镁膜,直接镀在光学玻璃上,第二层为二氧化硅膜,镀在氟化镁膜上,第三层为二氧化锆膜,镀在二氧化硅膜上;
上述光学玻璃复合膜的镀膜工艺,包括以下步骤:
1)真空镀膜设备中抽真空,使真空度达到8×10-4~10×10-4Pa;
2)在光学玻璃基体上蒸镀一层氟化镁膜,蒸镀条件为:采用钨或钼作为蒸发源材料,蒸发电流设为100A,时间为15min;
3)在氟化镁膜的基础上磁控溅射一层二氧化硅膜,条件为:采用硅为靶材,在真空镀膜设备中通入氩气作为溅射气体,通入氧气作为反应气体,氩气流量为30sccm,设备内压力0.1~1.0pa,氩气和氧气的比例为1:4;
4)在二氧化硅膜的基础上通过电子束热蒸的方式镀上二氧化锆膜,条件为:烘烤温度设为300℃,时间为1h,电子束流为100mA。
更具体地,氟化镁为晶体状,由水合氟化镁经机械破碎、烘干和低温真空脱水后作为镀膜靶材;晶体氟化镁在蒸镀前进行预熔,预熔电流为60A,预熔时间为10min。
更具体地,二氧化锆采用氧化钇进行稳定后再作为镀膜靶材,稳定包括以下步骤:
1)以二氧化锆和氧化钇粉料为原料,二氧化锆的摩尔百分比为氧化钇的20倍,混合均匀后添加聚乙烯醇结合剂使粉料团聚,造粒成型;
2)对颗粒料进行预烧,预烧温度为1200°C;
3)在真空烧结炉中烧结,然后自然冷却降温至室温。
更具体地,本发明中所使用的靶材纯度均为99.99%以上。
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明技术原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。

Claims (4)

1.一种光学玻璃复合膜,其特征在于,从里至外共3层,第一层为氟化镁膜,第二层为二氧化硅膜,第三层为二氧化锆膜。
2.一种光学玻璃复合膜镀膜工艺,其特征在于,包括如下步骤:
1)将真空镀膜设备中进行抽真空,使真空度达到8×10-4~10×10-4Pa;
2)在光学玻璃基体上蒸镀一层氟化镁膜,蒸镀条件为:采用钨或钼作为蒸发源材料,蒸发电流设为100A,时间为15min;
3)在氟化镁膜的基础上磁控溅射一层二氧化硅膜,条件为:采用硅为靶材,在真空镀膜设备中通入氩气作为溅射气体,通入氧气作为反应气体,所述的氩气流量为30sccm,设备内压力0.1~1.0pa,氩气和氧气的比例为1:4;
4)在二氧化硅膜的基础上通过电子束热蒸的方式镀上二氧化锆膜,条件为:烘烤温度设为300℃,时间为1h,电子束流为100mA。
3.根据权利要求2中所述的光学玻璃复合膜镀膜工艺,其特征在于,所述的氟化镁为晶体状,由水合氟化镁经机械破碎、烘干和低温真空脱水后作为镀膜靶材;所述的晶体氟化镁在蒸镀前进行预熔,预熔电流为60A,预熔时间为10min。
4.根据权利要求2中所述的光学玻璃复合镀膜工艺,其特征在于,所述的二氧化锆采用氧化钇进行稳定后再作为镀膜靶材。
CN201510804442.6A 2015-11-20 2015-11-20 一种光学玻璃复合膜及镀膜工艺 Withdrawn CN105399343A (zh)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107283955A (zh) * 2016-03-30 2017-10-24 新科实业有限公司 一种屏幕保护膜及其制作方法
CN108675788A (zh) * 2018-06-20 2018-10-19 江苏瑞尔光学有限公司 一种稳定氧化锆镀膜靶材及其制备方法
CN109851231A (zh) * 2019-01-24 2019-06-07 福建工程学院 一种减反射、抗激光损伤玻璃及其制备方法
CN111045268A (zh) * 2019-12-31 2020-04-21 哈尔滨工业大学 一种以氟化物为电解质层的全固态电致变色器件及其制备方法
CN113562986A (zh) * 2021-07-06 2021-10-29 苏州光大光电科技有限公司 一种光学玻璃镀膜和强化方法

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107283955A (zh) * 2016-03-30 2017-10-24 新科实业有限公司 一种屏幕保护膜及其制作方法
CN108675788A (zh) * 2018-06-20 2018-10-19 江苏瑞尔光学有限公司 一种稳定氧化锆镀膜靶材及其制备方法
CN109851231A (zh) * 2019-01-24 2019-06-07 福建工程学院 一种减反射、抗激光损伤玻璃及其制备方法
CN111045268A (zh) * 2019-12-31 2020-04-21 哈尔滨工业大学 一种以氟化物为电解质层的全固态电致变色器件及其制备方法
CN113562986A (zh) * 2021-07-06 2021-10-29 苏州光大光电科技有限公司 一种光学玻璃镀膜和强化方法

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