CN114779384A - 一种多角度低色差颜色膜及其制备方法 - Google Patents
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Abstract
本发明公开了一种多角度低色差光学颜色膜及其制备方法,该光学颜色膜包括基底、与基底接触的过渡层、中间多层膜、保护膜;所述中间多层膜为氢化非晶硅与高折射率材料和/或低折射率材料分别沉积的单材料层以一定顺序交替堆叠而成。采用本发明制备得到的光学颜色膜用较薄的厚度就可实现在大角度上具有低色差的目标颜色,量产时可以节约大量成本。制备氢化非晶硅使用的能源和材料消耗少,制备工艺简单,可在低温环境沉积,易于在廉价基底上进行大面积生产。
Description
技术领域
本发明属于真空溅射镀膜材料制备领域,具体涉及一种多角度低色差光学颜色膜及其制备方法。
背景技术
目前常见的颜色膜中,一部分是利用材料本身的颜色实现,这种薄膜常使用到一些含贵金属的材料,成本较为高昂,且对环境存在一定的影响;一部分则使用溅射光学薄膜的方法,利用高低折射率材料交替沉积实现目标颜色,这种方法更加绿色环保,成本也更低廉,但是一般的光学薄膜变换角度存在严重的色差,限制了它的应用。
需注意的是,前述背景技术部分公开的信息仅用于加强对本发明的背景理解,因此它可以包括但不构成对本领域普通技术人员已知的现有技术的信息。
发明内容
光学颜色膜的一大优势是,若需求更高的抗损伤性能,则可以优化设计,内层使用与基底结合更好的材料、外层使用高强度的材料或表面特殊处理,在不破坏颜色的情况下实现更高的强度。因此对于光学颜色膜,最需要解决的是大角度的色差问题。
为解决上述技术问题,本发明提供了一种光学颜色膜及其制备方法。
本发明的目的是提供一种光学颜色膜,所述颜色膜包括基底、与基底接触的过渡层、中间多层膜、保护膜;
其中,所述中间多层膜包括氢化非晶硅层。
根据本发明一实施方式,所述中间多层膜为氢化非晶硅与高折射率材料和/或低折射率材料分别沉积的单材料层以一定顺序交替堆叠而成;
,所述高折射率材料为折射率高于标准BK7玻璃折射率的材料,所述高折射率材料包括但不限于TiO2(折射率为2.0)、Nb2O5(折射率为2.3)、ZrO2(折射率为2.0)、Si3N4(折射率为2.0)中的一种或多种;所述低折射率材料为折射率接近或低于相对标准BK7玻璃折射率低或接近的材料,优选地,所述低折射率材料包括但不限于SiO2、MgF2等中的一种或多种。
标准BK7玻璃折射率为1.52。
根据本发明一实施方式,所述中间多层膜的层数为3~13层,优选为7-9层;氢化非晶硅的层数为1~7,优选为3-4层;
每层膜的厚度为10-200nm,优选为10-140nm。
类似于常规的高低折射率材料交替沉积,在此基础上把氢化非晶硅加入或使用其替换高、低折射率材料的一种,包括但不限于以下形式:1、高折射率材料+氢化非晶硅交替沉积;2、低折射率材料+氢化非晶硅交替沉积;3、高折射率材料+低折射率材料+氢化非晶硅交替沉积;4、高折射率材料+氢化非晶硅+低折射率材料交替沉积;5、前述4种方式交替沉积结合。由于镀膜精度和膜层内应力的缘故,每一层的厚度在10-200nm之间为宜。
根据本发明一实施方式,所述颜色膜的总厚度小于1微米,优选地,所述颜色膜的总厚度小于900nm。所述总厚度为过渡层、中间多层膜、保护膜的总厚度,不包括基底的厚度。
根据本发明一实施方式,所述基底为不锈钢、玻璃、陶瓷中的一种或多种。
根据本发明一实施方式,所述过渡层的材料为SiO2、Nb2O5、Si3N4、二氧化钛、二氧化锆中的一种或多种;优选为Nb2O5或SiO2;
所述过渡层的作用为用以增加膜层与基底的结合强度,其厚度为10-200nm,优选为20-40nm,具体依据颜色设计目标、结合强度要求和基底材质而定。
根据本发明一实施方式,所述保护膜为二氧化硅、氮化硅、氧化铝或五氧化二铌中的一种,优选为五氧化二铌;保护膜的作用为一方面提升耐磨性,另一方面也防止水汽、氧化剂等侵蚀内层导致变色。所述保护膜的厚度为100-200nm,优选为160-190nm。
本发明的另一目的是提供上述光学颜色膜的制备方法,包括以下步骤:
S1、确定所需材料的工艺参数并设计目标颜色的膜结构;提供一基体,并对基体进行预处理;
S2、提供一磁控溅射镀膜机,并对所述镀膜机进行预处理;
S3、将所述基体装入所述镀膜机,然后对所述基体进行离子源清洗;
S4、采用磁控溅射法,依次制备所述过镀膜、所述多层膜和所述保护膜。
在所述步骤S1中,由于不同设备存在的差异、同一设备在不同时间下的差异,需要对材料的工艺参数提前确定以便于设计。使用本公司制造的KOSS机型磁控溅射镀膜机,靶材直径20cm,长度1.6m,靶基距10-30cm,ICP离子源距基片10-30cm,转架转速80-120rpm。使用硅靶制备SiO2,溅射功率6-12kW,总氩气流量800-1200sccm,总氧气流量800-1200sccm,ICP离子源功率1500-4500W;使用铌靶制备Nb2O5,溅射功率6-12kW,总氩气流量800-1200sccm,总氧气流量800-1200sccm,ICP离子源功率1500-4500W;使用硅靶制备氢化非晶硅,溅射功率6-12kW,总氩气流量800-1200sccm,总氢气流量30-60sccm,ICP离子源功率1500-4500W。在上述参数范围内,依据设备经验参数作为参考,以该材料的标准性质为目标,寻找最佳工艺参数,最后获取最佳工艺参数下对应的材料参数(各波长对应折射率、消光系数等)。
取得所需材料的性质参数后,将其导入膜系设计软件,以需求颜色为目标,设计一个过渡层+氢化非晶硅与高低折材料的交替沉积层+保护层的膜系,过渡层和保护层可能影响最终颜色,设计时应放在一起考虑。
所述预处理为超声波清洗;
在所述步骤S2中,一般来说,氢化非晶硅对颜色的影响要显著高于其他的材料,而镀膜时氢气用量相对氩气、氧气较小,氢气纯度和流量的微小变化都会带来相对更显著的偏差,因此若在镀前较短时间内(2h)未使用过氢气,应通入氩气+氢气一段时间(10-30min),以排除气路、器壁上的杂质气体。
在所述步骤S3中,离子源清洗在氢气循环之后,正式镀膜之前,用以去除表面杂质,增加镀层结合力。
在所述步骤S4中,根据步骤S1确定的参数进行磁控溅射。
有益效果:本发明在使用常用的高低折射率材料的基础上,加入氢化非晶硅这一材料,使膜层更薄的同时在大角度有更低的色差。本发明制备得到的膜系厚度不到1微米,若仅用高低折射率两种材料,难以在这样薄的厚度下实现较低的色差。使用溅射方法用廉价材料制得多角度低色差的光学颜色膜,获得的薄膜对基底适应性强,不同基底上镀膜容易复现设计颜色,对环境适应力强,不易变色、划伤、掉膜。氢化非晶硅是一种新型功能材料,在可见光波段具有优良的光电性质,其透光率较小,可见波段主要表现为吸收与反射,在颜色膜的设计中具有明显的优势。使用氢化非晶硅,使我们在膜系设计时,用较薄的厚度就可实现在大角度上具有低色差的目标颜色,量产时可以节约大量成本。制备氢化非晶硅使用的能源和材料消耗少,制备工艺简单,可在低温环境沉积,易于在廉价基底上进行大面积生产。
附图说明
图1是本申请光学颜色膜的基本构成示意图;
图2是实施例1制备得到的颜色膜在小角度下样品的外观图;
图3是实施例1制备得到的颜色膜在大角度下样品的外观图;
图4是软件模拟的由实施例1制备得到的颜色膜在各角度下颜色值及色彩变化;
图5是实施例2制备得到的颜色膜在小角度下样品的外观图;
图6是实施例2制备得到的颜色膜在大角度下样品的外观图;
图7是软件模拟的由实施例2制备得到的颜色膜在各角度下颜色值及色彩变化;
具体实施方式
下面结合具体实施例对本发明做进一步详细说明,所述方法如无特别说明均为常规方法,本发明采用的试剂或材料等均可从市售购得。
实施例1、一种大角度低色差的中国红颜色膜
步骤1、以“中国红”颜色为目标,设计制备一个颜色膜:首先确定本次设计使用的材料为Nb2O5、SiO2以及氢化非晶硅;通过对比和优化,确定采用表1的工艺参数制备以上材料。
表1
Nb2O5和SiO2为常见材料,确定工艺参数的方法无需赘述。a-Si:H即氢化非晶硅,镀膜前进行氢气循环10-30min,然后采用多组参数镀单层100-200nm的氢化非晶硅,使用椭偏偏振仪进行测量,获得镀层性质参数(折射率n、消光系数k等),上表工艺制得的氢化非晶硅的性质参数为:在波长850nm处,n=3.5,k=0.04。将各材料及其性质参数带入膜系设计软件中,以颜色为目标进行设计,如表所示为一个设计好的膜层堆叠顺序与对应厚度。具体结构及参数如表2所示:
表2
层数 | 材料 | 厚度 |
11 | Nb<sub>2</sub>O<sub>5</sub> | 185nm |
10 | a-Si:H | 12nm |
9 | Nb<sub>2</sub>O<sub>5</sub> | 62nm |
8 | a-Si:H | 132nm |
7 | SiO<sub>2</sub> | 64nm |
6 | Nb<sub>2</sub>O<sub>5</sub> | 118nm |
5 | SiO<sub>2</sub> | 91nm |
4 | a-Si:H | 48nm |
3 | Nb<sub>2</sub>O<sub>5</sub> | 84nm |
2 | a-Si:H | 40nm |
1 | Nb<sub>2</sub>O<sub>5</sub> | 40nm |
基底 | Glass | 0 |
表2中,最底层为待镀基底,表格向上层数1为过渡层,层数2-10为含氢化非晶硅的交替堆叠层,层数11为最外保护层。
步骤2、对基底进行酒精和丙酮超声清洗后装入机器,
步骤3、氢气循环20min
步骤4、再用离子源(功率2500W,氩气流量1000sccm,氧气流量1000sccm,转速120rpm)离子轰击1min。
步骤5、使用确定的工艺参数,按照膜系设定的堆叠顺序、厚度进行沉积。
实施例1膜系总厚度仅为876nm。
上述膜系所镀制的薄膜,垂直于镀膜表面正视观察可见清晰的红色反射光,此角度下L值为43.1,a值为66.4,b值为39.2,与中国红Lab值(43,66,38)相吻合,不同的基底会有一定的差异但可调可控。
在30度及以下范围内,由膜系设计软件计算出L值43-49,a值65-67,b值37-42.5,在此角度范围内观察,颜色值变化较小,几乎无肉眼可辩的色差;在45度范围内,L值43-54,a值60-67,b值37-44,整体颜色依旧显示较强的红色。
小角度下样品的外观见附图2,大角度下样品的外观见附图3,由软件模拟的在各角度下颜色值及色彩变化见图4。。
该膜系厚度不到1微米,若仅用高低折射率两种材料,难以在这样薄的厚度下实现较低的色差。
实施例2一种大角度低色差的蓝绿颜色膜
以某蓝绿色样板为目标,设计一个光学颜色膜,该样板色彩Lab值(83,-32,-3.5)。本例仍旧使用实施例1中的材料及其工艺参数,在膜系设计软件中进行设计,下表为设计好的膜层堆叠顺序及对应厚度:
表3
层数 | 材料 | 厚度(nm) | 层数 | 材料 | 厚度(nm) |
0 | 基底 | / | 5 | a-SiH | 78.7 |
1 | SiO<sub>2</sub> | 22.7 | 6 | SiO<sub>2</sub> | 165 |
2 | Nb<sub>2</sub>O<sub>5</sub> | 27.4 | 7 | a-SiH | 33.8 |
3 | a-SiH | 36.5 | 8 | SiO<sub>2</sub> | 49.3 |
4 | Nb<sub>2</sub>O<sub>5</sub> | 54 | 9 | Nb<sub>2</sub>O<sub>5</sub> | 165.2 |
层数1为过渡层,层数2-8为含氢化非晶硅的交替堆叠层,层数9为最外保护层。使用玻璃作为基底,酒精、丙酮超声清洗后装入镀膜机内,进行20min氩气+氢气循环,再用离子源(功率2500W,氩气流量1000sccm,氧气流量1000sccm,转速120rpm)离子轰击1min。依照设计的堆叠顺序,使用之前确定的工艺参数进行镀膜。
该膜系所制得的薄膜,目视可见明亮的蓝绿色,垂直表面测试其Lab值为(83.8,-32.1,-3.5)。在30度及以下角度范围内,由膜系设计软件计算出L值82—84,a值-32—-38.7,b值-3.5—-4,在此角度范围内观察,颜色值变化较小,几乎无肉眼可辩的色差;在45度角度范围内,L值79.5—84,a值-32—-39.5,b值-3.5—-5,颜色值无太大变化,目视仍为明亮的蓝绿色;在65度角度范围内,L值78—84,a值-22—-39.5,b值-3.5—-6.5,负b值变大显示的是绿色变淡的趋势,目视观察颜色虽变淡,但仍显示很强的蓝绿色,与小角度下的差异不大。该膜系总厚682.6nm,在较薄的情况下实现了大角度下较低的色差。
小角度下样品的外观见附图5,大角度下样品的外观见附图6,由软件模拟的在各角度下颜色值及色彩变化见图7。
对比例:一种光学红色膜。
使用实施例一提供的Nb2O5、SiO2两种材料交替沉积一种光学膜,颜色目标为红色。膜层堆叠顺序及厚度如下表4:
表4
层数 | 材料 | 厚度(nm) | 层数 | 材料 | 厚度(nm) |
0 | 基底 | / | 7 | SiO<sub>2</sub> | 116 |
1 | SiO<sub>2</sub> | 165 | 8 | Nb<sub>2</sub>O<sub>5</sub> | 78 |
2 | Nb<sub>2</sub>O<sub>5</sub> | 10 | 9 | SiO<sub>2</sub> | 100 |
3 | SiO<sub>2</sub> | 178 | 10 | Nb<sub>2</sub>O<sub>5</sub> | 92 |
4 | Nb<sub>2</sub>O<sub>5</sub> | 82 | 11 | SiO<sub>2</sub> | 81 |
5 | SiO<sub>2</sub> | 125.5 | 12 | Nb<sub>2</sub>O<sub>5</sub> | 98 |
6 | Nb<sub>2</sub>O<sub>5</sub> | 74.5 |
采用与实施例1同样的工艺参数及流程,按上表膜系的堆叠顺序与厚度进行镀膜,得到外观红色的镀膜样品。垂直于镀膜表面正视观察可见清晰的红色反射光,此角度下测得L值为53,a值为62.3,b值为31.9。在0-30度的角度范围内,L值53-64,a值60-64,b值31-50,正b值上升显示的是色彩变黄的趋势,通过观察已经能明显看出较大的色差,对比实施例1,其在此角度范围内的b值为37-42.5,变化较小。在0-45度范围内,L值53-75,a值40-64,b值31-64,正a值下降显示的是红色变弱的趋势,此时观察到膜层已由红色变为橙色,对比实施例1,其在此角度范围内的a值为60-67,变化较小。此红色膜系总厚度1200nm,镀膜样品在不同角度下观察有明显的色差,而实施例1膜系总厚度仅为876nm,在较大的角度范围内仍可保持相近的色彩,原因就在于氢化非晶硅在可见光波段的优良光学性能。
Claims (10)
1.一种光学颜色膜,其特征在于,包括:所述颜色膜包括基底、与基底接触的过渡层、中间多层膜、保护膜;
所述中间多层膜为氢化非晶硅与高折射率材料和/或低折射率材料分别沉积的单材料层以一定顺序交替堆叠而成;所述中间多层膜包括氢化非晶硅层。
2.根据权利要求1所述的颜色膜,其特征在于,所述高折射率材料为折射率高于标准BK7玻璃折射率的材料,优选地,所述高折射率材料选自TiO2、Nb2O5、ZrO2、Si3N4中的一种或多种;所述低折射率材料为折射率接近或低于相对标准BK7玻璃折射率低或接近的材料,优选地,所述低折射率材料选自SiO2、MgF2等中的一种或多种。
3.根据权利要求2所述的颜色膜,其特征在于,所述中间多层膜的层数为3~13层,优选为7-9层;氢化非晶硅的层数为1~7,优选为3-4层;
每层膜的厚度为10-200nm,优选为10-140nm。
4.根据权利要求1-3任一项所述的颜色膜,其特征在于,所述颜色膜的总厚度小于1微米,优选地,所述颜色膜的总厚度小于900nm。
5.根据权利要求1-4任一项所述的颜色膜,其特征在于,所述基底为不锈钢、玻璃、陶瓷中的一种或多种。
6.根据权利要求1-5任一项所述的颜色膜,其特征在于,所述过渡层的材料为SiO2、Nb2O5、Si3N4、二氧化钛、二氧化锆中的一种或多种,优选为Nb2O5或SiO2;
所述过渡层的厚度为10-200nm,优选为20-40nm。
7.根据权利要求1-6任一项所述的颜色膜,其特征在于,所述保护膜为二氧化硅、氮化硅、氧化铝或五氧化二铌中的一种或多种,优选为五氧化二铌;所述保护膜的厚度为100-200nm,优选为160-190nm。
8.权利要求1-7任一项所述颜色膜的制备方法,其特征在于,包括以下步骤:
S1、提供一基体,并对基体进行预处理;
S2、提供一磁控溅射镀膜机,并对所述镀膜机进行预处理;
S3、将所述基体装入所述镀膜机,然后对所述基体进行离子源清洗;
S4、采用磁控溅射法,依次制备所述过镀膜、所述多层膜和所述保护膜;
优选地,在所述步骤S1中,所述预处理为超声波清洗;在所述步骤S2中,所述预处理为循环氢气处理,其中所述处理步骤通入的气体为氢气和氩气的混合气。
9.根据权利要求8所述的制备方法,其特征在于,所述磁控溅射法选自直流磁控溅射法、高功率脉冲磁控溅射法、中频磁控溅射法、射频磁控溅射法和反应磁控溅射法中的一种或多种。
10.根据权利要求8所述的制备方法,其特征在于,在所述步骤S4中,采用用硅靶制备所述氢化非晶硅,溅射功率6-12kW,总氩气流量800-1200sccm,总氢气流量30-60sccm,ICP离子源功率1500-4500W。
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