CN108048227B - 一种光学材料清洗液 - Google Patents

一种光学材料清洗液 Download PDF

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CN108048227B
CN108048227B CN201711361330.3A CN201711361330A CN108048227B CN 108048227 B CN108048227 B CN 108048227B CN 201711361330 A CN201711361330 A CN 201711361330A CN 108048227 B CN108048227 B CN 108048227B
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cleaning solution
potassium
optical material
phosphate
salt
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潘国顺
陈高攀
罗海梅
徐莉
罗桂海
周艳
邹春莉
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Tsinghua University
Shenzhen Research Institute Tsinghua University
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Abstract

本发明涉及一种光学材料清洗液,属于光学材料清洗技术领域。本发明的清洗液包括阴离子表面活性剂、氢键破坏剂、络合剂、醇类、PH调节剂、盐和水,本发明适用于熔石英、K9玻璃及微晶玻璃等光学材料抛光后表面颗粒的清洗。将本发明清洗液稀释1~10倍后,将抛光后的光学材料在清洗液中超声清洗5~10分钟,然后在去离子水中超声清洗1~10分钟去除光学材料表面的清洗液。使用该清洗液可以去除抛光后光学材料表面的污染物,包括有机污染物、颗粒和离子残留等。本发明清洗液中所含有的氢键抑制剂可以克服抛光后光学材料表面容易吸附颗粒的缺点,有效的去其除表面颗粒。

Description

一种光学材料清洗液
技术领域
本发明涉及一种光学材料清洗液,属于光学材料清洗技术领域,特别涉及一种用于熔石英、K9玻璃及微晶玻璃抛光后表面颗粒清洗的技术领域。
背景技术
随着光学系统性能的不断提升,近年来光学元、部件的精度指标,表面质量等要求也越来越高。化学机械抛光过程作为光学元件的重要的加工工序,能够消除光学材料表面机械损伤、残留的亚表面裂纹及残余应力等缺陷,但是抛光后材料表面不可避免的会出现有机物、颗粒及金属离子等残留。尤其是作为典型光学材料的熔石英、K9玻璃及微晶玻璃等材料,抛光后表面存在大量活性羟基,极易与抛光液中的颗粒羟基形成氢键,使得材料表面吸附大量颗粒,很难清洗,从而降低光学元件激光损伤阈值。
涉及玻璃的清洗液的专利,目前报道较多如:CN 102504978 A,CN 102994254 A,CN101434891A,CN101580773A,CN102504980A等,但他们都是关于普通玻璃,如汽车玻璃表面污渍的清洗。专利CN105251745A公开了古典法抛光拼盘加工K9玻璃和熔石英元件的清洗方法,对精密抛光后的元件表面有机污染物和抛物粉残留颗粒有较高清洗效率。但是该专利中使用毒性较大的四氯化碳溶液作为清洗液,且步骤复杂,不适于大规模使用。
发明内容
本发明的目的在于克服现有技术中的不足,提出了一种光学材料清洗液,使用该清洗液可以破坏抛光后光学材料表面羟基与颗粒间形成的氢键,并通过其它化学试剂将颗粒带离材料表面,可以有效的避免颗粒的吸附。同时清洗液中的其它化学试剂可以去除光学材料表面的有机物及金属离子残留,避免了光学材料化学机械抛光后表面污染问题。
一种光学材料清洗液,其特征在于,该清洗液包括阴离子表面活性剂、氢键破坏剂、络合剂、醇类、PH调节剂、盐和水;该清洗液的组分重量配比为:
阴离子表面活性剂:0.01~10wt%;
氢键破坏剂:0.1~1wt%;
络合剂:0.1~5wt%;
醇类:1~10wt%;
PH调节剂:0.1~10wt%;
盐:0.1~2wt%;
去离子水:余量。
所述阴离子表面活性剂5-10wt%,氢键抑制剂0.1-0.3wt%,络合剂2-5wt%,醇类7-10wt%、PH调节剂0.1-2wt%,盐0.5-0.6wt%,去离子水余量。
所述阴离子表面活性剂为磷酸酯系列表面活性剂,包括:脂肪醇醚磷酸酯(MOA-3P)、脂肪醇醚磷酸酯(MOA-9P)、酚醚磷酸酯(TXP-4)、酚醚磷酸酯(TXP-10)、脂肪醇醚磷酸酯钾盐(MOA-3PK-40)、脂肪醇醚磷酸酯钾盐(MOA-3PK-70)、酚醚磷酸酯钾盐(NP-4PK)、酚醚磷酸酯钾盐(NP-10PK-40)、酚醚磷酸酯钾盐(NP-10PK-80)、异十三醇磷酸酯(ITAP)、异十三醇醚(6)磷酸酯钾盐(IT6APK)、月桂基磷酸酯(MA24P)、月桂基磷酸酯钾盐(MA24PK-30)、月桂基磷酸酯或钾盐(MA24PK-50)中的一种或几种。
所述氢键破坏剂通式为:H2N-(C=R1)-R2的化合物中的一种或几种,其中R1为O或N元素,R2为C或H元素。
所述氢键破坏剂包括尿素、甲酰胺、哌啶甲酰胺、吡啶甲酰胺、氨基苯甲酰胺、硝基苯甲酰胺、苯甲酰胺、盐酸胍、氨基胍中的一种或几种。
所述络合剂为次氮基三乙酸三钠(NTA)、羟乙基二胺四乙酸(HEDTA)、二乙烯三胺五乙酸(DTPA)、乙二胺四乙酸(EDTA)中的一种或几种。
所述醇类包括甲醇、乙醇、异丙醇、乙二醇、丙二醇、丙三醇中的一种或几种。
所述PH调节剂选用甲酸、乙酸、盐酸、硝酸、硫酸、磷酸、氢氧化钾、氢氧化钠、氨、四甲基氢氧化铵、乙醇胺、二乙醇胺、三乙醇胺中的一种或几种。
所述盐包括氯化钠、硫酸钠、硝酸钠、亚硝酸钠、磷酸钠、碳酸钠、氯化钾、硫酸钾、硫酸氢钾、硝酸钾、亚硝酸钾、磷酸钾、碳酸钾中的一种或几种。
本发明清洗液PH值在4~10之间
本发明与现有技术相比具有如下优点:
1.加入磷酸酯系列表面活性剂,对残留在光学材料表面有机物和游离的颗粒具有吸附作用,将它们带离材料表面;
2.氢键破坏剂破坏颗粒与光学材料表面形成的氢键,减弱它们之间的作用,有利于其他化学试剂将颗粒带离材料表面;
3.抛光液中的金属离子会吸附在抛光后光学材料表面,造成金属离子污染,络合剂对金属离子有很强的螯合能力,能把这些金属离子封闭起来,以减少金属离子对材料表面的影响;
4.醇类物质有较小的表面张力,容易吸附在光学材料表面,形成一层膜,降低污染物与材料表面的接触几率;
5.PH调节剂可以调节清洗液的PH值来获得最佳的清洗效果;
6.盐可以调节清洗液的流变,增加清洗效果;
7.本发明清洗液可以稀释1~10倍后使用,成本低,清洗效果好。
附图说明
图1是本发明实施例三清洗后光学材料表面原子力显微镜图。
图2是对比例一清洗后光学材料表面原子力显微镜图。
具体实施方式
首先将本发明清洗液稀释1~10倍,将抛光后的光学材料在清洗液中超声清洗5~10分钟,然后在去离子水中超声清洗1~10分钟去除光学材料表面的清洗液,干燥后待检测。清洗过程中的温度保持在40~50摄氏度之间。然后,利用原子力显微镜(布鲁克)测量清洗之后的光学材料表面颗粒情况。
以下结合具体实施例对本发明进行详细说明。
实施例一
清洗液的制备:在不断的搅拌情况下,向去离子水中加入磷酸酯系列表面活性剂至其完全溶解,然后依次加入氢键破坏剂,络合剂,醇类和盐,最后加入PH调节剂,清洗液的PH=8.6。使各组分含量分别为:阴离子表面活性剂(MOA-3P)10wt%,氢键破坏剂(尿素)0.1wt%,络合剂(NTA)5wt%,醇类(乙醇)10wt%,PH调节剂润湿剂(盐酸)0.1wt%,盐(硝酸钾)0.5wt%。原子力显微镜检测清洗后表面残留效果,表面颗粒无、其他残留无。
实施例二
清洗液的制备:在不断的搅拌情况下,向去离子水中加入磷酸酯系列表面活性剂至其完全溶解,然后依次加入氢键破坏剂,络合剂,醇类和盐,最后加入PH调节剂,清洗液的PH=5.2。使各组分含量分别为:阴离子表面活性剂(TXP-10)4wt%,氢键破坏剂(甲酰胺)0.5wt%,络合剂(EDTA)1wt%,醇类(乙二醇)5wt%,PH调节剂润湿剂(乙酸)1wt%,盐(磷酸钠)0.1wt%。原子力显微镜检测清洗后表面残留效果,表面颗粒少量、其他残留无。
实施例三
清洗液的制备:在不断的搅拌情况下,向去离子水中加入磷酸酯系列表面活性剂至其完全溶解,然后依次加入氢键破坏剂,络合剂,醇类和盐,最后加入PH调节剂,清洗液的PH=9.1。使各组分含量分别为:阴离子表面活性剂(NP-10PK-80)5wt%,氢键破坏剂(盐酸胍)0.3wt%,络合剂(EDTA)2wt%,醇类(丙三醇)7wt%,PH调节剂润湿剂(氢氧化钾)2wt%,盐(硫酸钠)0.6wt%。原子力显微镜检测清洗后表面残留效果,表面颗粒无、其他残留无。
实施例四
清洗液的制备:在不断的搅拌情况下,向去离子水中加入磷酸酯系列表面活性剂至其完全溶解,然后依次加入氢键破坏剂,络合剂,醇类和盐,最后加入PH调节剂,清洗液的PH=10。使各组分含量分别为:阴离子表面活性剂(MA24P)0.01wt%,氢键破坏剂(苯甲酰胺)1wt%,络合剂(HEDTA)0.5wt%,醇类(甲醇)1wt%,PH调节剂润湿剂(氨)10wt%,盐(碳酸钾)2wt%。原子力显微镜检测清洗后表面残留效果,表面颗粒少量、其他残留中等。
实施例五
清洗液的制备:在不断的搅拌情况下,向去离子水中加入磷酸酯系列表面活性剂至其完全溶解,然后依次加入氢键破坏剂,络合剂,醇类和盐,最后加入PH调节剂,清洗液的PH=9.7。使各组分含量分别为:阴离子表面活性剂(MOA-9P)1wt%,氢键破坏剂(氨基胍)0.2wt%,络合剂(DTPA)0.1wt%,醇类(丙二醇)4wt%,PH调节剂润湿剂(三乙醇胺)0.3wt%,盐(亚硝酸钠)1wt%。原子力显微镜检测清洗后表面残留效果,表面颗粒少量、其他残留少量。对比例一
清洗液的制备:在不断的搅拌情况下,向去离子水中加入磷酸酯系列表面活性剂至其完全溶解,然后依次加入络合剂,醇类和盐,最后加入PH调节剂,清洗液的PH=8.5。使各组分含量分别为:阴离子表面活性剂(NP-10PK-80)5wt%,络合剂(EDTA)2wt%,醇类(丙三醇)7wt%,PH调节剂润湿剂(氢氧化钾)2wt%,盐(硫酸钠)0.6wt%。原子力显微镜检测清洗后表面残留效果,表面残留大量颗粒、其他残留无。
对比例二
清洗液的制备:在不断的搅拌情况下,向去离子水中加入磷酸酯系列表面活性剂至其完全溶解,然后依次加入氢键破坏剂,络合剂和盐,最后加入PH调节剂,清洗液的PH=9.1。使各组分含量分别为:阴离子表面活性剂(NP-10PK-80)5wt%,氢键破坏剂(盐酸胍)0.3wt%,络合剂(EDTA)2wt%,PH调节剂润湿剂(氢氧化钾)2wt%,盐(硫酸钠)0.6wt%。原子力显微镜检测清洗后表面残留效果,表面颗粒少量、其他残留中等。
抛光后光学材料表面颗粒及其它残留情况分为四个等级:大量,中等,少量,无。

Claims (4)

1.一种光学材料清洗液,其特征在于,该清洗液包括阴离子表面活性剂、氢键破坏剂、络合剂、醇类、pH调节剂、盐和水;该清洗液的组分重量配比为:
所述的阴离子表面活性剂5-10wt%,氢键抑制剂0.1-0.3wt%,络合剂2-5wt%,醇类7-10wt%、pH调节剂0.1-2wt%,盐0.5-0.6wt%,去离子水余量;
所述氢键破坏剂为尿素、甲酰胺、哌啶甲酰胺、吡啶甲酰胺、氨基苯甲酰胺、硝基苯甲酰胺、苯甲酰胺、盐酸胍、氨基胍中的一种或几种;
所述络合剂为次氮基三乙酸三钠、羟乙基二胺四乙酸、二乙烯三胺五乙酸、乙二胺四乙酸中的一种或几种;
所述阴离子表面活性剂为磷酸酯系列表面活性剂,包括:脂肪醇醚磷酸酯、酚醚磷酸酯、脂肪醇醚磷酸酯钾盐、酚醚磷酸酯钾盐、异十三醇磷酸酯、异十三醇醚(6)磷酸酯钾盐、月桂基磷酸酯或钾盐中的一种或几种。
2.根据权利要求1所述的光学材料清洗液,其特征在于,所述醇类包括甲醇、乙醇、异丙醇、乙二醇、丙二醇、丙三醇中的一种或几种。
3.根据权利要求1所述的光学材料清洗液,其特征在于,所述pH调节剂选用甲酸、乙酸、盐酸、硝酸、硫酸、磷酸、氢氧化钾、氢氧化钠、氨、四甲基氢氧化铵、乙醇胺、二乙醇胺、三乙醇胺中的一种或几种。
4.根据权利要求1所述的光学材料清洗液,其特征在于,所述盐包括氯化钠、硫酸钠、硝酸钠、亚硝酸钠、磷酸钠、碳酸钠、氯化钾、硫酸钾、硫酸氢钾、硝酸钾、亚硝酸钾、磷酸钾、碳酸钾中的一种或几种。
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