CN107285641A - 一种超硬防辐射玻璃及其制备方法 - Google Patents

一种超硬防辐射玻璃及其制备方法 Download PDF

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CN107285641A
CN107285641A CN201710429953.3A CN201710429953A CN107285641A CN 107285641 A CN107285641 A CN 107285641A CN 201710429953 A CN201710429953 A CN 201710429953A CN 107285641 A CN107285641 A CN 107285641A
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    • C03C—CHEMICAL 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
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
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    • C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3626—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer one layer at least containing a nitride, oxynitride, boronitride or carbonitride
    • C—CHEMISTRY; METALLURGY
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    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3639—Multilayers containing at least two functional metal layers
    • C—CHEMISTRY; METALLURGY
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    • C03C—CHEMICAL 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
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3644—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the metal being silver
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
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    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3649—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer made of metals other than silver
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL 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
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3657—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the multilayer coating having optical properties
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL 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
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/15—Deposition methods from the vapour phase
    • C03C2218/154—Deposition methods from the vapour phase by sputtering
    • C03C2218/156—Deposition methods from the vapour phase by sputtering by magnetron sputtering

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Abstract

本发明公开了一种超硬防辐射玻璃，包括玻璃基板，玻璃基板上表面开设有若干“S”形孔和“O”形孔，“S”形孔和“O”形孔相邻，胶体填充在“S”形孔和“O”形孔中，胶体的折射率与玻璃基板的折射率相同，玻璃基板从下到上依次设置第一二氧化钛层，厚度为15nm；氧化铝作为纳米缓冲层，厚度为8nm，第二二氧化钛层，厚度66nm；第一Co‑Ni‑Cr‑Al‑Y膜层，厚度4nm；Ag膜层，厚度4.5nm；第二Co‑Ni‑Cr‑Al‑Y膜层，厚度42nm；氧化硅作为过渡层，厚度38nm；氮化硅作为缓冲纳米层，厚度为9nm；氮化碳纳米层，厚度为22nm。本发明还公开了一种超硬防辐射玻璃的制备方法。本发明具有造价低廉、结构简单、具有超强硬度的同时具有防辐射功能。

Description

一种超硬防辐射玻璃及其制备方法
技术领域
本发明属于玻璃技术领域，本发明涉及一种超硬防辐射玻璃及其制备方法。
背景技术
为了增强玻璃的表面强度，比如通过镀层等形成复合层方式来实现，现有技术中通过氮化硅镀层来改性玻璃的强度，但是在特殊的应用领域依然不能满足要求，研究出表面强度更高的玻璃成为一种需求，其中材料的选择和应用一直制约这技术的进一步发展的瓶颈。
中国专利，专利号：201410310367.3，公开一种防刮伤超硬玻璃及其制备方法，包括玻璃基板，玻璃基板上设置缓冲纳米层，纳米缓冲层上设置有纳米过渡层，纳米过渡层上设置氮化碳纳米层；所述纳米过渡层与氮化碳纳米层之间增设纳米缓冲层；缓冲纳米层为氧化铝或氮化硅纳米层，所述纳米过渡层为二氧化硅纳米层，上述各层通过设置条形阳极层离子源的磁控反应溅射镀层工艺连接。
此种方法和现有技术中的技术会存在硬度和防辐射不能有效的结合，适用范围较小。
发明内容
为克服上述现有技术的缺点和不足，本发明的首要目的在于提供一种造价低廉、结构简单、具有超强硬度的同时具有防辐射功能的超硬防辐射玻璃。
本发明的另一目的在于提供一种超硬防辐射玻璃的其制备方法。
本发明的目的通过下述的方法实现：一种超硬防辐射玻璃，包括玻璃基板，玻璃基板上表面开设有若干“S”形孔和“O”形孔，“S”形孔和“O”形孔相邻，胶体填充在“S”形孔和“O”形孔中，胶体的折射率与玻璃基板的折射率相同，玻璃基板从下到上依次设置第一二氧化钛层，厚度为15nm；氧化铝作为纳米缓冲层，厚度为8nm，第二二氧化钛层，厚度66nm；第一Co-Ni-Cr-Al-Y膜层，厚度4nm；Ag膜层，厚度4.5nm；第二Co-Ni-Cr-Al-Y膜层，厚度42nm；氧化硅作为过渡层，厚度38nm；氮化硅作为缓冲纳米层，厚度为9nm；氮化碳纳米层，厚度为22nm。
所述“S”形孔和“O”形孔的孔径为98nm。
所述“O”形孔整个孔径为550nm。
所述胶体为聚甲基丙烯酸甲酯或者环氧基树脂。
所述胶体与玻璃基板相平齐。
上述超硬防辐射玻璃的制备方法，包括以下步骤：
(1)、取一玻璃基板，玻璃基板上开设有若干“S”形孔和“O”形孔；
(2)、向“S”形孔和“O”形孔内填充胶体，胶体的折射率与所述玻璃基板的折射率相同或相近；
(3)、对胶体进行整平和固化处理；
(4)、在步骤(3)的基体上通过设置条形阳极层离子源的磁控反应溅射镀层工艺镀制第一二氧化钛层、纳米缓冲层及第二二氧化钛层；
(5)、充入Ar，靶材为第一Co-Ni-Cr-Al-Y膜层靶，沉积厚度4nm；
(6)、充入Ar，靶材为Ag靶，在第一Co-Ni-Cr-Al-Y膜上沉积Ag膜，厚度4.5nm；
(7)、充入Ar，靶材为第二Co-Ni-Cr-Al-Y膜层靶，在Ag膜上沉积第二Co-Ni-Cr-Al-Y膜层，厚度42nm；
(8)、通过设置条形阳极层离子源的磁控反应溅射镀层工艺镀制过渡层，厚度38nm；氮化硅作为缓冲纳米层，厚度为9nm；氮化碳纳米层，厚度为22nm。
所述条形阳极层离子源的磁控反应溅射镀层工艺，条形阳极层离子源，长度为1500mm，大于溅射靶材的长度，该离子源的基本参数设定为：放电电压200～500V、束流平均能量大约为放电电压的55％、放电电流为≤9A、供气量为160scmm氩气。
所述镀制氮化碳镀层环节中用分子泵优化排列和靶位隔离形成井喷，从而阻断氧气与氮气互窜，保证氮化物纯度，获得稳定的氮化碳纳米层。
所述步骤(7)中加入1％体积的醋酸。
还包括清洗步骤，采用超声波振荡清洗，之后在温度115℃下进行干燥，获得成品。
本发明与现有的技术相比具有如下的优点：
1)本发明中玻璃基板上表面开设有若干“S”形孔和“O”形孔，“S”形孔和“O”形孔相邻，胶体填充在“S”形孔和“O”形孔中，胶体的折射率与玻璃基板的折射率相同，能有效的对防辐射层进行复合，另外特殊的孔状结构和胶体配合，对于整体硬度无不良影响，同时能够保证超强硬度和防辐射的使用寿命。
2)本发明中玻璃基板从下到上依次设置第一二氧化钛层，厚度为15nm；氧化铝作为纳米缓冲层，厚度为8nm，第二二氧化钛层，厚度66nm；第一Co-Ni-Cr-Al-Y膜层，厚度4nm；Ag膜层，厚度4.5nm；第二Co-Ni-Cr-Al-Y膜层，厚度42nm；氧化硅作为过渡层，厚度38nm；氮化硅作为缓冲纳米层，厚度为9nm；氮化碳纳米层，厚度为22nm，经过整体设计，有效保证使用效果和使用寿命。
3)本发明中的“S”形孔和“O”形孔的孔径为98nm，经实验证明，这样的尺寸在使用时，防辐射效果会大大增强，玻璃硬度，孔洞尺寸过大或过小时，硬度会大大减小，从而影响使用寿命，如果单用一种孔洞，将也会影响硬度，得不到想到保护的玻璃产品。
4)本发明中的工艺步骤，与现有技术中大大的不同，需要很高的创造性劳动，各个步骤相辅相成，从而达到想要的设计效果，步骤(7)中加入1％体积的醋酸，经实验证明，玻璃品质会产生质变，防辐射层不容易刮花，硬度也大大加强。
具体实施方式
下面结合实施例对本发明作进一步详细的描述，但本发明的实施方式不限于此。
实施例1：
一种超硬防辐射玻璃，包括玻璃基板，玻璃基板上表面开设有若干“S”形孔和“O”形孔，“S”形孔和“O”形孔相邻，胶体填充在“S”形孔和“O”形孔中，胶体的折射率与玻璃基板的折射率相同，玻璃基板从下到上依次设置第一二氧化钛层，厚度为15nm；氧化铝作为纳米缓冲层，厚度为8nm，第二二氧化钛层，厚度66nm；第一Co-Ni-Cr-Al-Y膜层，厚度4nm；Ag膜层，厚度4.5nm；第二Co-Ni-Cr-Al-Y膜层，厚度42nm；氧化硅作为过渡层，厚度38nm；氮化硅作为缓冲纳米层，厚度为9nm；氮化碳纳米层，厚度为22nm。
本实施例中的“S”形孔和“O”形孔的孔径为98nm；“O”形孔整个孔径为550nm。
本实施例中的胶体为聚甲基丙烯酸甲酯；胶体与玻璃基板相平齐。
上述超硬防辐射玻璃的制备方法，包括以下步骤：
(1)、取一玻璃基板，玻璃基板上开设有若干“S”形孔和“O”形孔；
(2)、向“S”形孔和“O”形孔内填充胶体，胶体的折射率与所述玻璃基板的折射率相同或相近；
(3)、对胶体进行整平和固化处理；
(4)、在步骤(3)的基体上通过设置条形阳极层离子源的磁控反应溅射镀层工艺镀制第一二氧化钛层、纳米缓冲层及第二二氧化钛层；
(5)、充入Ar，靶材为第一Co-Ni-Cr-Al-Y膜层靶，沉积厚度4nm；
(6)、充入Ar，靶材为Ag靶，在第一Co-Ni-Cr-Al-Y膜上沉积Ag膜，厚度4.5nm；
(7)、充入Ar，靶材为第二Co-Ni-Cr-Al-Y膜层靶，在Ag膜上沉积第二Co-Ni-Cr-Al-Y膜层，厚度42nm；
(8)、通过设置条形阳极层离子源的磁控反应溅射镀层工艺镀制过渡层，厚度38nm；氮化硅作为缓冲纳米层，厚度为9nm；氮化碳纳米层，厚度为22nm。
所述条形阳极层离子源的磁控反应溅射镀层工艺，条形阳极层离子源，长度为1500mm，大于溅射靶材的长度，该离子源的基本参数设定为：放电电压200～500V、束流平均能量大约为放电电压的55％、放电电流为≤9A、供气量为160scmm氩气。经实验证明，这样的工艺数据，可以提升产品的品质。
上述镀制氮化碳镀层环节中用分子泵优化排列和靶位隔离形成井喷，从而阻断氧气与氮气互窜，保证氮化物纯度，获得稳定的氮化碳纳米层。
还包括清洗步骤，采用超声波振荡清洗，之后在温度115℃下进行干燥，获得成品。
采用上述结构和方法，硬度超强，防辐射性能好，成本低廉，深受消费者的喜爱，外观美观大方，并不会影响具体的使用。
实施例2：
本实施例与实施例1不同之处在于：本实施例中的胶体为环氧基树脂。骤(7)中加入1％体积的醋酸，经实验证明，玻璃品质会产生质变，防辐射层不容易刮花，硬度也大大加强。与实施例1相比，本实施例中的防辐射层，在同等实验条件下，硬度增加50～63％，防辐射层使用寿命增加1倍以上。
对比实施例：
采用中国专利，专利号：201410310367.3的制造而成的玻璃，在同等测试条件下，对比实施例1产生的硬度高出55％，且具有防辐射效果，防辐射效果比起一般的防辐射膜，高出性能9％左右。足以能够证明其性能的优越性。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (10)

1.一种超硬防辐射玻璃，其特征在于：包括玻璃基板，玻璃基板上表面开设有若干“S”形孔和“O”形孔，“S”形孔和“O”形孔相邻，胶体填充在“S”形孔和“O”形孔中，胶体的折射率与玻璃基板的折射率相同，玻璃基板从下到上依次设置第一二氧化钛层，厚度为15nm；氧化铝作为纳米缓冲层，厚度为8nm，第二二氧化钛层，厚度66nm；第一Co-Ni-Cr-Al-Y膜层，厚度4nm；Ag膜层，厚度4.5nm；第二Co-Ni-Cr-Al-Y膜层，厚度42nm；氧化硅作为过渡层，厚度38nm；氮化硅作为缓冲纳米层，厚度为9nm；氮化碳纳米层，厚度为22nm。
2.根据权利要求1所述的超硬防辐射玻璃，其特征在于：所述“S”形孔和“O”形孔的孔径为98nm。
3.根据权利要求1所述的超硬防辐射玻璃，其特征在于：所述“O”形孔整个孔径为550nm。
4.根据权利要求1所述的超硬防辐射玻璃，其特征在于：所述胶体为聚甲基丙烯酸甲酯或者环氧基树脂。
5.根据权利要求1所述的超硬防辐射玻璃，其特征在于：所述胶体与玻璃基板相平齐。
6.根据权利要求1～6任一项所述的超硬防辐射玻璃的制备方法，其特征在于，包括以下步骤：
(1)、取一玻璃基板，玻璃基板上开设有若干“S”形孔和“O”形孔；
(2)、向“S”形孔和“O”形孔内填充胶体，胶体的折射率与所述玻璃基板的折射率相同或相近；
(3)、对胶体进行整平和固化处理；
(4)、在步骤(3)的基体上通过设置条形阳极层离子源的磁控反应溅射镀层工艺镀制第一二氧化钛层、纳米缓冲层及第二二氧化钛层；
(5)、充入Ar，靶材为第一Co-Ni-Cr-Al-Y膜层靶，沉积厚度4nm；
(6)、充入Ar，靶材为Ag靶，在第一Co-Ni-Cr-Al-Y膜上沉积Ag膜，厚度4.5nm；
(7)、充入Ar，靶材为第二Co-Ni-Cr-Al-Y膜层靶，在Ag膜上沉积第二Co-Ni-Cr-Al-Y膜层，厚度42nm；
(8)、通过设置条形阳极层离子源的磁控反应溅射镀层工艺镀制过渡层，厚度38nm；氮化硅作为缓冲纳米层，厚度为9nm；氮化碳纳米层，厚度为22nm。
7.根据权利要求6所述的超硬防辐射玻璃的制备方法，其特征在于：所述条形阳极层离子源的磁控反应溅射镀层工艺，条形阳极层离子源，长度为1500mm，大于溅射靶材的长度，该离子源的基本参数设定为：放电电压200～500V、束流平均能量大约为放电电压的55％、放电电流为≤9A、供气量为160scmm氩气。
8.根据权利要求7所述的超硬防辐射玻璃的制备方法，其特征在于：所述镀制氮化碳镀层环节中用分子泵优化排列和靶位隔离形成井喷，从而阻断氧气与氮气互窜，保证氮化物纯度，获得稳定的氮化碳纳米层。
9.根据权利要求8所述的超硬防辐射玻璃的制备方法，其特征在于：所述步骤(7)中加入1％体积的醋酸。
10.根据权利要求9所述的超硬防辐射玻璃的制备方法，其特征在于：还包括清洗步骤，采用超声波振荡清洗，之后在温度115℃下进行干燥，获得成品。
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