CN115433906B - 硒化锌基底8-12um波段高耐久性增透膜的制备方法 - Google Patents
硒化锌基底8-12um波段高耐久性增透膜的制备方法 Download PDFInfo
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- PFNQVRZLDWYSCW-UHFFFAOYSA-N (fluoren-9-ylideneamino) n-naphthalen-1-ylcarbamate Chemical compound C12=CC=CC=C2C2=CC=CC=C2C1=NOC(=O)NC1=CC=CC2=CC=CC=C12 PFNQVRZLDWYSCW-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 239000000758 substrate Substances 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims description 20
- 238000007747 plating Methods 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 238000006386 neutralization reaction Methods 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 12
- 238000000576 coating method Methods 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 9
- 230000008020 evaporation Effects 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000010894 electron beam technology Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims 3
- 239000010410 layer Substances 0.000 description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- IQAKAOAPBMJSGJ-UHFFFAOYSA-N [Cu].[Y].[Ba] Chemical compound [Cu].[Y].[Ba] IQAKAOAPBMJSGJ-UHFFFAOYSA-N 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000001771 vacuum deposition Methods 0.000 description 2
- 229910052984 zinc sulfide Inorganic materials 0.000 description 2
- 229910016036 BaF 2 Inorganic materials 0.000 description 1
- 229910004261 CaF 2 Inorganic materials 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- -1 YBF 3 Inorganic materials 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/26—Vacuum evaporation by resistance or inductive heating of the source
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
本公开提供了一种硒化锌基底8‑12um波段高耐久性增透膜的制备方法，其膜系结构为：SUB/YBF3/ZNS/GE/ZNS/YBF3/ZNS/LAF3/SI/AF/AIR，其中SUB为基底材料硒化锌，AIR为空气。本公开的工艺方案可有效解决红外长波段增透膜耐摩擦的问题。
Description
技术领域
本发明涉及红外镀膜领域，具体涉及一种硒化锌基底8-12um波段高耐久性增透膜的制备方法。
背景技术
在红外长波段常用的减反射膜料，如ZnS、YBF3、BaF2、CaF2等，这些材料一般比较松软且容易吸潮。作为减反射层使用膜强度差非常不耐摩擦，又因硒化锌材料本身硬度差，在镀制完增透膜后镜片无法抵御中度摩擦要求。因此需要提供一种工艺方案解决红外长波段增透膜耐摩擦的问题。
发明内容
鉴于现有技术中存在的问题，本公开的目的在于提供一种硒化锌基底8-12um波段高耐久性增透膜的制备方法。
为了实现上述目的，本公开提供了一种硒化锌基底8-12um波段高耐久性增透膜的制备方法，其膜系结构为：SUB/YBF3/ZNS/GE/ZNS/YBF3/ZNS/LAF3/SI/AF/AIR，其中SUB为基底材料硒化锌，AIR为空气。
在一些实施例中，所述的基底材料为硒化锌。
在一些实施例中，所述硒化锌镜片镀膜前需将设备真空抽至1.5×10-3pa以下，腔体加热至150℃，镀前使用离子清洗。
在一些实施例中，所述镀膜材料GE、YBF3、SI为电子束加热蒸发，ZNS、LAF3、AF为电阻加热蒸发。
在一些实施例中，镀制LAF3时加热温度为180℃，镀制AF不加热温度要小于100℃。
在一些实施例中，硒化锌镜片镀膜前需要超声波清洗，或人工擦拭保证镜片表面洁净无污染。
在一些实施例中，所述镀制YBF3、ZNS、LAF3、SI、GE均使用离子辅助，离子源参数为：中和电流0.3-1A、中和气流量6-8sccm、阳极电压100-280V、阳极电流0.5-4A、氩气体流量100％。
本公开的有益效果如下：
本公开的工艺方案可有效解决红外长波段增透膜耐摩擦的问题。
具体实施方式
下面详细说明本申请的硒化锌基底8-12um波段高耐久性增透膜的制备方法。
本申请公开一种硒化锌基底8-12um波段高耐久性增透膜的制备方法，其膜系结构为：SUB/YBF3/ZNS/GE/ZNS/YBF3/ZNS/LAF3/SI/AF/AIR，其中SUB为基底材料硒化锌，AIR为空气。
本公开中具有1至8层增透膜系，其中LAF3作为低折射率材料透明波段截止到12um，在加热至180度以上条件下可以形成有效硬质保护层，AF作为防水层其本身具有一定润滑效果，但AF与LAF3的结合力很差，SI可以有效链接2种材料，增加结合力，最终膜层以一定硬度加润滑的条件即可抵御中度摩擦。
在一些实施例中，所述的基底材料为硒化锌。
在一些实施例中，所述硒化锌镜片镀膜前需将设备真空抽至1.5×10-3pa以下，腔体加热至150℃，镀前使用离子清洗。
在一些实施例中，所述镀膜材料GE、YBF3、SI为电子束加热蒸发，ZNS、LAF3、AF为电阻加热蒸发。GE不适合电阻加热蒸发，它的蒸发温度太高用电子束加热的方式可以快速升温至蒸发温度，硫化锌如用电子束蒸发的话也是可以的但容易产生膜料点。
在一些实施例中，镀制LAF3时加热温度为180℃，镀制AF不加热，温度要小于100℃。
在一些实施例中，硒化锌镜片镀膜前需要超声波清洗，或人工擦拭保证镜片表面洁净无污染。
在一些实施例中，所述镀制YBF3、ZNS、LAF3、SI、GE均使用离子辅助，离子源参数为：中和电流0.3-1A、中和气流量6-8sccm、阳极电压100-280V、阳极电流0.5-4A、氩气体流量100％。这样的离子源参数可以提高膜层质量。
[测试]
实施例1
将规格D25*2的硒化锌圆片经过超声波清洗干净，置于真空镀膜机内。
设备抽真空至2.0×10-3Pa抽真空的同时开启加热温度设定150℃，真空度达到后开启霍尔离子源，设置中和电流0.6A、中和气流量8sccm、阳极电压240伏、阳极电流4安、氩气流量比例100％，以此参数离子清洗300秒；
完成后开始镀膜，根据膜系结构设计具体膜层厚度为；YBF3(146nm)/ZNS(193nm)/GE(70nm)/ZNS(300nm)/YBF3(1150nm)/ZNS(101nm)/LAF3(150nm)/SI(10nm)/AF(10nm)，镀膜过程中从第一层YBF3开始至第八层SI使用的离子源参数均为中和电流0.36A、中和气流量6sccm、阳极电压180V、阳极电流2A、氩气流量比例100％；
镀第九层AF时不使用离子源，镀膜过程中从第一层YBF3开始至第6层ZNS均使用150℃加热，镀第7层LAF3和第八层SI时温度升至180℃，镀完降温；
镀第九层AF时温度需要降低至100℃以下，镀完后自然冷却5分钟后取片。膜层可抗中度摩擦。
实施例2
将规格D20*1的硒化锌圆片经过脱脂棉加酒精丙酮混合液擦拭干净，置于真空镀膜机内。
设备抽真空至1.5×10-3Pa抽真空的同时开启加热温度设定150℃，真空度达到后开启霍尔离子源，设置中和电流0.5A、中和气流量6sccm、阳极电压220V、阳极电流2A、氩气流量比例100％，以此参数离子清洗300秒。
完成后开始镀膜，根据膜系结构设计具体膜层厚度为；YBF3(141nm)/ZNS(226nm)/GE(70nm)/ZNS(300nm)/YBF3(1150nm)/ZNS(80nm)/LAF3(140nm)/SI(15nm)/AF(15nm)，镀膜过程中从第一层YBF3开始至第八层SI使用的离子源参数均为中和电流0.3A、中和气流量6sccm、阳极电压160V、阳极电流1.5A、氩气流量比例100％；
镀第九层AF时不使用离子源，镀膜过程中从第一层YBF3开始至第6层ZNS均使用140℃加热，镀第7层LAF3和第八层SI时温度升至180℃，镀完降温，镀第九层AF时温度需要降低至100℃以下，
镀完后自然冷却5分钟后取片。膜层可抗中度摩擦。
以上对本申请做了详尽的描述，其目的在于让熟悉此领域技术的人士能够了解本申请的内容并加以实施，并不能以此限制本申请的保护范围，凡根据本申请的精神实质所作的等效变化或修饰，都应涵盖在本申请的包括范围内。
Claims (2)
1.一种硒化锌基底8-12um波段高耐久性增透膜的制备方法，其膜系结构为：SUB/YBF3/ZNS/GE/ZNS/YBF3/ZNS/LAF3/SI/AF/AIR，其中SUB为基底材料硒化锌，AIR为空气；
所述硒化锌镜片镀膜前需将设备真空抽至1.5×10-3Pa以下，腔体加热至150℃，镀前使用离子清洗；
所述镀膜材料GE、YBF3、SI为电子束加热蒸发，ZNS、LAF3、AF为电阻加热蒸发；
镀制LAF3时加热温度为180℃，镀制AF不加热温度要小于100℃；
所述镀制YBF3、ZNS、LAF3、SI、GE均使用离子辅助，离子源参数为：中和电流0.3-1A、中和气流量6-8sccm、阳极电压100-280V、阳极电流0.5-4A、氩气体流量100％。
2.根据权利要求1所述的硒化锌基底8-12um波段高耐久性增透膜的制备方法，其特征在于，
硒化锌镜片镀膜前需要超声波清洗，或人工擦拭保证镜片表面洁净无污染。
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