CN109321012A - 陶瓷天线罩防潮用有机-无机涂层及其制备方法 - Google Patents
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Abstract
本发明公开了一种陶瓷天线罩防潮用有机‑无机涂层及其制备方法,所述涂层组分及其质量百分比如下:乙烯基聚二甲基硅氧烷:20~60%;乙烯基八面体低聚倍半硅氧烷:2~30%低聚乙二醇二甲基丙烯酸酯:2~6%;光引发剂:0.01~1%;溶剂:余量。本发明所制备的防潮涂层防潮效果好,不易碳化,涂层成膜性好,介电系数低,耐高温性好,可以实现天线罩在航天领域防潮、抗高温与透波性能;本发明制备工艺简便,材料易得,制备方法简便,反应条件可控。
Description
技术领域
本发明涉及导弹天线罩涂层,具体地指一种陶瓷天线罩防潮用有机-无机涂层及其制备方法。
背景技术
陶瓷材料是用天然或合成化合物经过成型和高温烧结制成的一类无机非金属材料,具有膨胀系数小、介电常数低以及耐高温和耐热冲击等优点。陶瓷材料根据主要成分可以分为氧化物陶瓷、氮化物陶瓷、碳化物陶瓷、金属陶瓷等,其中,氧化物陶瓷常见有主要成分为SiO2石英纤维纱。
导弹天线罩是保护雷达天线系统正常工作的一种设施,它是弹体和雷达系统的组成部分,需要承载导弹气动载荷、气动加热和飞行过程中的恶劣环境,同时,它还需要具备透波性能。
目前,应用于导弹天线罩的涂层主要包括有机涂层体系和无机涂层体系。有机涂层有不错的防潮性能,制备工艺简单,但是碳含量高,高温下会碳化,碳具有较强的无线电波吸收能力,碳化后无线电波透过能力会下降;无机涂层不存在碳化的问题,涂层致密且防潮效果好,但是制备无机涂层需要高温烧结且工艺复杂。因此,寻找一种防潮效果好,不易碳化且制备工艺简单的涂层变成了亟待解决的技术问题。
发明内容
本发明的目的就是要提供一种陶瓷天线罩防潮用有机-无机涂层及其制备方法,该涂层防潮效果好,不易碳化且制备工艺简单。
为实现上述目的,本发明采用的技术方案是:一种陶瓷天线罩防潮用有机-无机涂层,其特征在于:所述涂层组分及其质量百分比如下:
乙烯基聚二甲基硅氧烷:20~60%;
乙烯基八面体低聚倍半硅氧烷:2~30%;
低聚乙二醇二甲基丙烯酸酯:2~6%;
光引发剂:0.01~1%;
溶剂:余量。
进一步地,所述涂层组分及其质量百分比如下:
乙烯基聚二甲基硅氧烷:40~60%;
乙烯基八面体低聚倍半硅氧烷:2~15%;
低聚乙二醇二甲基丙烯酸酯:2~4%;
光引发剂:0.01~0.5%;
溶剂:余量。
进一步地,所述低聚乙二醇二甲基丙烯酸酯的分子量为198~990。
进一步地,所述光引发剂为息香二甲醚、1-羟基环己基苯基甲酮、2-羟基-2-甲基-1-苯基-1-丙酮和2-甲基-1-(4-甲硫基苯基)-2-吗啉基-1-丙酮中的一种。
更进一步地,所述溶剂为四氢呋喃、甲苯、甲醇、乙二醇和三氟乙醇中的一种。
上述陶瓷天线罩防潮用有机-无机涂层的制备方法,包括以下步骤:
1)天线罩表面改性:将陶瓷基天线罩置于质量分数为1~15%的硅烷偶联剂的正己烷溶液中浸泡1~10h,随后用正己烷、正己烷和乙醇的混合溶剂或乙醇超声处理10~45min,然后在100~150℃温度下干燥处理;
2)紫外光交联固化涂层:将乙烯基聚二甲基硅氧烷、乙烯基八面体低聚倍半硅氧烷、低聚乙二醇二甲基丙烯酸酯、光引发剂、溶剂按照所述质量百分比配成溶液,喷涂在已改性的陶瓷基天线罩基材表面,随后置于紫外光交联仪中交联10~60min成膜,获得所述陶瓷天线罩防潮用有机-无机涂层。
进一步地,所述步骤1)中,硅烷偶联剂为(3-巯基丙基)三甲氧基硅烷或γ-巯丙基三乙氧基硅烷。
更进一步地,所述步骤2)中,在紫外光交联仪中以365nm,30~150W的工作方式交联。
其一,本发明公开的一种含八面体低聚倍半硅氧烷有机-无机陶瓷天线罩防潮涂层,防潮涂层中有机硅材料PDMS(聚二甲基硅氧烷)在不影响主体材料介电常数和力学性能的同时,成膜性能好,制备工艺简便,具有良好的防潮性能。
其二,无机材料占主体的POSS(八面体低聚倍半硅氧烷)体系抗高温能力强,介电常数低,力学性能好,能够赋予涂层良好的耐高温抗氧化和防潮性能。
其三有机-无机材料平衡复合,一方面,无机材料增强有机材料的耐高温性能,另外一方面,有机材料增强无机材料的成膜性。本发明所制备的防潮涂层防潮效果好,不易碳化,涂层成膜性好,介电系数低,耐高温性好,可以实现天线罩在航天领域防潮、抗高温与透波性能。
其四,本发明制备工艺简便,材料易得,制备方法简便,反应条件可控。
具体实施方式
下面结合具体实施例对本发明作进一步的详细说明,便于更清楚地了解本发明,但它们不对本发明构成限定。
实施例1
1)天线罩表面改性:将纤维增强陶瓷基天线罩置于1%的硅烷偶联剂(3-巯基丙基)三甲氧基硅烷的正己烷溶液中浸泡1h,随后用正己烷、正己烷/乙醇(体积比为40%/60%)、乙醇超声处理10min,100℃干燥处理;
2)紫外光交联固化涂层:将乙烯基聚二甲基硅氧烷、乙烯基八面体低聚倍半硅氧烷、低聚乙二醇二甲基丙烯酸酯、光引发剂、溶剂按照质量百分比配成溶液,具体如下:
乙烯基聚二甲基硅氧烷:20%;
乙烯基八面体低聚倍半硅氧烷:30%;
低聚乙二醇二甲基丙烯酸酯6%;
息香二甲醚:1%;
四氢呋喃:余量;
低聚乙二醇二甲基丙烯酸酯分子量为198。
随后将混合溶液喷涂在基材表面,置于紫外光交联仪中以365nm,30W的工作方式交联10min成膜,获得有机-无机防潮涂层。
所得防潮涂层在40℃、95%湿度环境中放置24h,吸潮率为0.52%。
实施例2
1)天线罩表面改性:将纤维增强陶瓷基天线罩置于8%的硅烷偶联剂γ-巯丙基三乙氧基硅烷的正己烷溶液中浸泡5h,随后用正己烷、正己烷/乙醇(体积比为40%/60%)、乙醇超声处理27min,125℃干燥处理;
2)紫外光交联固化涂层:将乙烯基聚二甲基硅氧烷、乙烯基八面体低聚倍半硅氧烷、低聚乙二醇二甲基丙烯酸酯、光引发剂、溶剂按照质量百分比配成溶液,具体如下:
乙烯基聚二甲基硅氧烷:40%;
乙烯基八面体低聚倍半硅氧烷:15%;
低聚乙二醇二甲基丙烯酸酯4%;
1-羟基环己基苯基甲酮:0.5%;
甲苯:余量;
低聚乙二醇二甲基丙烯酸酯分子量为396。
随后将混合溶液喷涂在基材表面,置于紫外光交联仪中以365nm,90W的工作方式交联35min成膜,获得有机-无机防潮涂层。
所得防潮涂层在40℃、95%湿度环境中放置24h,吸潮率为0.71%。
实施例3
1)天线罩表面改性:将纤维增强陶瓷基天线罩置于15%的硅烷偶联剂γ-巯丙基三乙氧基硅烷的正己烷溶液中浸泡10h,随后用正己烷、正己烷/乙醇(体积比为40%/60%)、乙醇超声处理45min,150℃干燥处理;
2)紫外光交联固化涂层:将乙烯基聚二甲基硅氧烷、乙烯基八面体低聚倍半硅氧烷、低聚乙二醇二甲基丙烯酸酯、光引发剂、溶剂按照质量百分比配成溶液,具体如下:
乙烯基聚二甲基硅氧烷:60%;
乙烯基八面体低聚倍半硅氧烷:2%;
低聚乙二醇二甲基丙烯酸酯2%;
2-羟基-2-甲基-1-苯基-1-丙酮:0.01%;
甲醇:余量;
低聚乙二醇二甲基丙烯酸酯分子量为594。
随后将混合溶液喷涂在基材表面,置于紫外光交联仪中以365nm,150W的工作方式交联60min成膜,获得有机-无机防潮涂层。
所得防潮涂层在40℃、95%湿度环境中放置24h,吸潮率为0.82%。
实施例4
1)天线罩表面改性:将纤维增强陶瓷基天线罩置于5%的硅烷偶联剂γ-巯丙基三乙氧基硅烷的正己烷溶液中浸泡4h,随后用正己烷、正己烷/乙醇(体积比为40%/60%)、乙醇超声处理30min,110℃干燥处理;
2)紫外光交联固化涂层:将乙烯基聚二甲基硅氧烷、乙烯基八面体低聚倍半硅氧烷、低聚乙二醇二甲基丙烯酸酯、光引发剂、溶剂按照质量百分比配成溶液,具体如下:
乙烯基聚二甲基硅氧烷:60%;
乙烯基八面体低聚倍半硅氧烷:2%;
低聚乙二醇二甲基丙烯酸酯2%;
2-甲基-1-(4-甲硫基苯基)-2-吗啉基-1-丙酮:0.01%;
乙二醇:余量;
低聚乙二醇二甲基丙烯酸酯分子量为792。
随后将混合溶液喷涂在基材表面,置于紫外光交联仪中以365nm,100W的工作方式交联40min成膜,获得有机-无机防潮涂层。
所得防潮涂层在40℃、95%湿度环境中放置24h,吸潮率为0.44%。
实施例5
1)天线罩表面改性:将纤维增强陶瓷基天线罩置于2%的硅烷偶联剂(3-巯基丙基)三甲氧基硅烷的正己烷溶液中浸泡8h,随后用正己烷、正己烷/乙醇(体积比为40%/60%)、乙醇超声处理40min,130℃干燥处理;
2)紫外光交联固化涂层:将乙烯基聚二甲基硅氧烷、乙烯基八面体低聚倍半硅氧烷、低聚乙二醇二甲基丙烯酸酯、光引发剂、溶剂按照质量百分比配成溶液,具体如下:
乙烯基聚二甲基硅氧烷:25%;
乙烯基八面体低聚倍半硅氧烷:30%;
低聚乙二醇二甲基丙烯酸酯:5%;
1-羟基环己基苯基甲酮:0.01%;
三氟乙醇:余量;
低聚乙二醇二甲基丙烯酸酯分子量为990。
随后将混合溶液喷涂在基材表面,置于紫外光交联仪中以365nm,135W的工作方式交联30min成膜,获得有机-无机防潮涂层。
所得防潮涂层在40℃、95%湿度环境中放置24h,吸潮率为0.21%。
实施例6
1)天线罩表面改性:将纤维增强陶瓷基天线罩置于10%的硅烷偶联剂(3-巯基丙基)三甲氧基硅烷的正己烷溶液中浸泡4h,随后用正己烷、正己烷/乙醇(体积比为40%/60%)、乙醇超声处理25min,145℃干燥处理;
2)紫外光交联固化涂层:将乙烯基聚二甲基硅氧烷、乙烯基八面体低聚倍半硅氧烷、低聚乙二醇二甲基丙烯酸酯、光引发剂、溶剂按照质量百分比配成溶液,具体如下:
乙烯基聚二甲基硅氧烷:35%;
乙烯基八面体低聚倍半硅氧烷:25%;
低聚乙二醇二甲基丙烯酸酯:6%;
息香二甲醚:0.6%;
甲苯:余量;
低聚乙二醇二甲基丙烯酸酯分子量为792。
随后将混合溶液喷涂在基材表面,置于紫外光交联仪中以365nm,80W的工作方式交联50min成膜,获得有机-无机防潮涂层。
所得防潮涂层在40℃、95%湿度环境中放置24h,吸潮率为0.39%。
Claims (8)
1.一种陶瓷天线罩防潮用有机-无机涂层,其特征在于:所述涂层组分及其质量百分比如下:
乙烯基聚二甲基硅氧烷:20~60%;
乙烯基八面体低聚倍半硅氧烷:2~30%;
低聚乙二醇二甲基丙烯酸酯:2~6%;
光引发剂:0.01~1%;
溶剂:余量。
2.根据权利要求1所述的陶瓷天线罩防潮用有机-无机涂层,其特征在于:所述涂层组分及其质量百分比如下:
乙烯基聚二甲基硅氧烷:40~60%;
乙烯基八面体低聚倍半硅氧烷:2~15%;
低聚乙二醇二甲基丙烯酸酯:2~4%;
光引发剂:0.01~0.5%;
溶剂:余量。
3.根据权利要求1或2所述的陶瓷天线罩防潮用有机-无机涂层,其特征在于:所述低聚乙二醇二甲基丙烯酸酯的分子量为198~990。
4.根据权利要求1或2所述的陶瓷天线罩防潮用有机-无机涂层,其特征在于:所述光引发剂为息香二甲醚、1-羟基环己基苯基甲酮、2-羟基-2-甲基-1-苯基-1-丙酮和2-甲基-1-(4-甲硫基苯基)-2-吗啉基-1-丙酮中的一种。
5.根据权利要求1或2所述的陶瓷天线罩防潮用有机-无机涂层,其特征在于:所述溶剂为四氢呋喃、甲苯、甲醇、乙二醇和三氟乙醇中的一种。
6.根据权利要求1所述陶瓷天线罩防潮用有机-无机涂层的制备方法,其特征在于:包括以下步骤:
1)天线罩表面改性:将陶瓷基天线罩置于质量分数为1~15%的硅烷偶联剂的正己烷溶液中浸泡1~10h,随后用正己烷、正己烷和乙醇的混合溶剂或乙醇超声处理10~45min,然后在100~150℃温度下干燥处理;
2)紫外光交联固化涂层:将乙烯基聚二甲基硅氧烷、乙烯基八面体低聚倍半硅氧烷、低聚乙二醇二甲基丙烯酸酯、光引发剂、溶剂按照所述质量百分比配成溶液,喷涂在已改性的陶瓷基天线罩基材表面,随后置于紫外光交联仪中交联10~60min成膜,获得所述陶瓷天线罩防潮用有机-无机涂层。
7.根据权利要求6所述陶瓷天线罩防潮用有机-无机涂层的制备方法,其特征在于:所述步骤1)中,硅烷偶联剂为(3-巯基丙基)三甲氧基硅烷或γ-巯丙基三乙氧基硅烷。
8.根据权利要求6或7所述陶瓷天线罩防潮用有机-无机涂层的制备方法,其特征在于:所述步骤2)中,在紫外光交联仪中以365nm,30~150W的工作方式交联。
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