CN108715996B - 一种高透防刮伤防蓝光纳米薄膜材料及其制备方法 - Google Patents
一种高透防刮伤防蓝光纳米薄膜材料及其制备方法 Download PDFInfo
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Abstract
本发明提供了一种高透防刮伤防蓝光纳米薄膜材料以及其制备方法,该材料包括氢化非晶碳化硅薄膜层(a‑SiCx:H)、氢化非晶碳薄膜层(a‑C:H)和位于两层薄膜中间的过渡层。该材料的制备方法是利用等离子增强化学气相沉积技术,设置一定的沉积参数,首先在基板上沉积硅原子含量为20%~60%的氢化非晶碳化硅薄膜。然后通过不断的改变沉积参数,沉积硅含量逐渐变化的过渡层(硅含量变化:x→0)。最后设置一定的参数,在过渡层上沉积一层氢化非晶碳薄膜。最后经过200~300℃在真空炉中退火。经过此方法制备的纳米薄膜具有高透防刮伤和防蓝光作用,可以应用在眼镜和显示屏中。
Description
技术领域
本发明属于材料制备技术领域,具体涉及一种高透防刮伤防蓝光纳米薄膜材料的制备方法。
背景技术
随着大数据时代的到来,人们每天上网的时长不断增加。尤其是那些上班族和学生党,长期面对电脑、手机等各种显示屏,容易造成眼睛疲劳、干涩,甚至产生各种眼科疾病。这些问题多是由于我们所使用的各种显示仪器所产生的辐射造成的。目前常见的电子显示屏,多采用蓝色LED混合黄色荧光粉实现的WLED背光。由于电子显示屏的背光利用蓝色LED混合黄色荧光粉实现的白色效果,所以蓝光成分较多,而蓝光在可见光谱中能量相对高,能够穿透角膜、晶状体,到达视网膜,视网膜一旦受损,将造成不可逆的伤害。
而目前存在的一些高透防刮伤防蓝光材料分为单层膜结构的防蓝光材料和多层膜结构的防防蓝光材料。单层膜结构的防蓝光材料的制造工艺简单但是其高透射、防刮伤和防蓝光的优点很难同时保证。多层膜结构的高透防刮伤防蓝光材料是目前兼顾高透射、防刮伤和防蓝光性能较好的材料,但其复杂的制造工艺大大降低了其在产品中的应用。
发明内容
为克服上述现有技术中的不足,本发明提供了一种高透防刮伤防蓝光纳米薄膜材料及其制备方法。该高透防刮伤防蓝光纳米薄膜材料包括内层的氢化非晶碳化硅薄膜层、过渡层和外层的氢化非晶碳薄膜层。
本发明所提供的高透防刮伤防蓝光纳米薄膜材料的制备方法包括一下步骤:
(1)清洗并干燥基板。先将玻璃/聚碳酸酯片置于无水乙醇中超声清洗5~10分钟,然后利用去离子水对玻璃片再次超声冲洗4~6分钟,最后用氮气吹干;
(2)反应室预抽真空。利用机械泵、罗茨泵、分子泵等真空设备在50~300℃条件下对反应室预抽真空,至压强低于10-4 Pa;
(3)氢化非晶碳化硅层的制备。首先以甲烷和硅烷为工作气体,采用等离子体增强化学气相沉积技术在步骤(2)中的反应室内于玻璃/聚碳酸酯基板上制备氢化非晶碳化硅薄膜。氢化非晶碳化硅薄膜具体制备工艺参数:射频功率:200~500 W,沉积温度:50~300℃,沉积压强:30~200 Pa,甲烷流量:20~50 sccm,开始硅烷流量:20~40 sccm,氢化非晶碳化硅薄膜层沉积厚度:0.5µm~1µm;
(4)过渡层的制备,以甲烷和硅烷为工作气体,采用等离子体增强化学气相沉积技术在步骤(2)中的反应室内于步骤(3)沉积的氢化非晶碳化硅层上制备过渡层;为保证过渡层中硅含量逐渐减小至零,在过渡层制备过程中,硅烷流量从起始设定值(40~20sccm)每分钟减少0.5~1sccm,当硅烷流量减小到零时过渡层沉积完成。过渡层具体制备工艺参数:射频功率:200~500 W,沉积温度:50~300℃,沉积压强:30~200 Pa,甲烷流量:20~50sccm,起始硅烷流量:20~40 sccm,过渡层薄膜沉积厚度:0.5µm;
(5)氢化非晶碳层的制备。以氩气稀释的甲烷为工作气体,采用等离子体增强化学气相沉积技术在步骤(2)中的反应室内于步骤(3)沉积的氢化非晶碳化硅层上制备氢化非晶碳薄膜。氢化非晶碳薄膜具体制备工艺参数:射频功率:200~500 W,沉积温度:50~300℃,沉积压强:30~200 Pa,甲烷流量:40~70 sccm,氩气流量:280 sccm,氢化非晶碳薄膜沉积厚度:0.5 µm~1 µm;
(6)退火过程。把经过以上步骤沉积的多层膜放置于真空炉中加热到 100~500℃,保持10~30 min,并在真空环境中冷却到室温。
经过以上步骤,化学惰性良好、绿色环保的高透防刮伤防蓝光纳米薄膜材料便制备完成。
进一步优选为,沉积在聚碳酸酯基板上,制备氢化非晶碳化硅薄膜的工艺参数最是:射频功率500W,沉积温度50℃,腔体压强30Pa,甲烷流量30sccm,硅烷流量30sccm,薄膜厚度为1µm;制备过渡层的工艺参数是:射频功率500W,沉积温度50℃,腔体压强30Pa,甲烷流量30sccm,起始硅烷流量30sccm,薄膜厚度为0.5µm;制备氢化非晶碳薄膜的工艺参数是:射频功率500W,沉积温度50℃,腔体压强30Pa,甲烷流量40sccm,氩气流量280 sccm,薄膜厚度为0.5µm;退火工艺参数是:退火温度100℃,保持30min。
进一步优选为,沉积在玻璃基板上,制备氢化非晶碳化硅薄膜的工艺参数是:射频功率200W,沉积温度300℃,腔体压强200Pa,甲烷流量30sccm,硅烷流量30sccm,薄膜厚度为0.5µm;制备过渡层的工艺参数是:射频功率200W,沉积温度300℃,腔体压强200Pa,甲烷流量30sccm,起始硅烷流量30sccm,薄膜厚度为0.5µm; 制备氢化非晶碳薄膜的工艺参数是:射频功率200W,沉积温度300℃,腔体压强200Pa,甲烷流量70sccm,氩气流量280 sccm,薄膜厚度为1µm;退火工艺参数是:退火温度500℃,保持10min。
由于上述技术方案运用,本发明与现有技术相比具有的优点是: 1、本发明的高透防刮伤防蓝光纳米薄膜材料依次设置的氢化非晶碳化硅薄膜层可以有效阻隔了短波蓝光射线、紫光射线、紫外光射线的刺激,大大减轻光对眼睛的伤害;过渡层起到了从氢化非晶碳化硅薄膜层到氢化非晶碳薄膜层的柔性过渡,此设计代替两层不同折射率薄膜的直接接触,有效减弱了由于光线穿过折射率不同的薄膜时所带来的界面反射,从而提高材料的透光性;退火后的氢化非晶碳薄膜层具有较高的硬度,可以有效防止尖锐物体对表面的刮伤。另一方面,过渡层的设计大大降低了材料的内应力,提高氢化非晶碳化硅薄膜层和非晶碳薄膜层的结合强度,保持产品使用性能的持久性。 2、本发明高透防刮伤防蓝光纳米薄膜材料的制作工艺简单便捷,氢化非晶碳化硅薄膜层、过渡层和氢化非晶碳薄膜层在一个仪器中完成,中间只需要调整沉积参数即可。3、利用本工艺所制备的高透防刮伤防蓝光纳米薄膜材料的透过率大于92%,防蓝光阻隔率在70%以上,20次摩擦试验后的透射率和防蓝光阻隔率分别在90%和70%以上。
附图说明
图1为实施例所制备的高透防刮伤防蓝光纳米薄膜材料结构图。
图2为玻璃片、目前市场上的防蓝光膜和实施例2制备的薄膜材料的透射图谱。
具体实施方式
实施例1
(1)清洗并干燥基板。先将聚碳酸酯片置于无水乙醇中超声清洗5~10分钟,然后利用去离子水对玻璃片再次超声冲洗4~6分钟,最后用氮气吹干;
(2)反应室预抽真空。利用机械泵、罗茨泵、分子泵等真空设备在50℃条件下对反应室预抽真空,至压强低于10-4 Pa;
(3)氢化非晶碳化硅层的制备。首先以甲烷和硅烷为工作气体,采用等离子体增强化学气相沉积技术在步骤(2)中的反应室内于玻璃/聚碳酸酯基板上制备氢化非晶碳化硅薄膜。氢化非晶碳化硅薄膜具体制备工艺参数:射频功率:500W,沉积温度:50℃,沉积压强:30Pa,甲烷流量:20 sccm,硅烷流量:40 sccm,氢化非晶碳化硅薄膜沉积厚度:1µm;
(4)过渡层的制备。以甲烷和硅烷为工作气体,采用等离子体增强化学气相沉积技术在步骤(2)中的反应室内于步骤(3)沉积的氢化非晶碳化硅层上制备过渡层;为保证过渡层中硅含量逐渐减小至零,在过渡层制备过程中,硅烷流量从起始设定值40sccm,每分钟减少1sccm,当硅烷流量减小到零时过渡层沉积完成。过渡层具体制备工艺参数:射频功率:500 W,沉积温度:50℃,沉积压强:30 Pa,甲烷流量:20sccm,起始硅烷流量:40sccm,过渡层薄膜沉积厚度:0.5µm;
(5)氢化非晶碳层的制备。以氩气稀释的甲烷为工作气体,采用等离子体增强化学气相沉积技术在步骤(2)中的反应室内于步骤(3)沉积的氢化非晶碳化硅层上制备氢化非晶碳薄膜。氢化非晶碳薄膜具体制备工艺参数:射频功率:500W,沉积温度:50℃,沉积压强:30 Pa,甲烷流量:40 sccm,氩气流量:280 sccm,氢化非晶碳薄膜沉积厚度:0.5µm;
(6)退火过程。把经过以上步骤沉积的多层膜放置于真空炉中加热到 100℃,保持30min,并在真空环境中冷却到室温。
本实施例所制备的高透防刮伤防蓝光纳米薄膜材料的透过率大于93%,防蓝光阻隔率大于70%,20次摩擦试验后的透射率和防蓝光阻隔率分别在90%和70%以上。
实施例2
(1)清洗并干燥基板。先将玻璃片置于无水乙醇中超声清洗5~10分钟,然后利用去离子水对玻璃片再次超声冲洗4~6分钟,最后用氮气吹干;
(2)反应室预抽真空。利用机械泵、罗茨泵、分子泵等真空设备在300℃条件下对反应室预抽真空,至压强低于10-4 Pa;
(3)氢化非晶碳化硅层的制备。首先以甲烷和硅烷为工作气体,采用等离子体增强化学气相沉积技术在步骤(2)中的反应室内于玻璃/聚碳酸酯基板上制备氢化非晶碳化硅薄膜。氢化非晶碳化硅薄膜具体制备工艺参数:射频功率:200W,沉积温度:300℃,沉积压强:200 Pa,甲烷流量:50 sccm,硅烷流量:20 sccm,氢化非晶碳化硅薄膜沉积厚度:0.5µm;
(4)过渡层的制备。以甲烷和硅烷为工作气体,采用等离子体增强化学气相沉积技术在步骤(2)中的反应室内于步骤(3)沉积的氢化非晶碳化硅层上制备过渡层;为保证过渡层中硅含量的逐渐减小(t→0),在过渡层制备过程中,硅烷流量从起始设定值(20sccm)每分钟减少0.5sccm,当硅烷流量减小到零时过渡层沉积完成。过渡层具体制备工艺参数:射频功率:200 W,沉积温度:300℃,沉积压强:200 Pa,甲烷流量:50sccm,起始硅烷流量:20sccm,过渡层薄膜沉积厚度:0.5µm;
(5)氢化非晶碳层的制备。以氩气稀释的甲烷为工作气体,采用等离子体增强化学气相沉积技术在步骤(2)中的反应室内于步骤(3)沉积的氢化非晶碳化硅层上制备氢化非晶碳薄膜。氢化非晶碳薄膜具体制备工艺参数:射频功率:200 W,沉积温度:300 ℃,沉积压强:200 Pa,甲烷流量:70 sccm,氩气流量:280 sccm,氢化非晶碳薄膜沉积厚度:1 µm;
(6)退火过程。把经过以上步骤沉积的多层膜放置于真空炉中加热到 500 ℃,保持10 min,并在真空环境中冷却到室温。
本实施例所制备的高透防刮伤防蓝光纳米薄膜材料的透过率大于94%,防蓝光阻隔率大于80%,20次摩擦试验后的透射率和防蓝光阻隔率分别在92%和78%以上。
实施例3
与实施例1相比除了步骤(3)、步骤(4)和步骤(5)的沉积温度(100℃)不同,其余和实施例1相同。
本实施例所制备的高透防刮伤防蓝光纳米薄膜材料的透过率大于91%,防蓝光阻隔率大于60%,20次摩擦试验后的透射率和防蓝光阻隔率分别在90%和60%以上。
实施例4
与实施例1相比除了步骤(3)、步骤(4)和步骤(5)的沉积压强(200Pa)不同,其余和实施例1相同。
本实施例所制备的高透防刮伤防蓝光纳米薄膜材料的透过率大于85%,防蓝光阻隔率大于60%,20次摩擦试验后的透射率和防蓝光阻隔率分别在82%和60%以上。
实施例5
与实施例1相比除了步骤(3)、步骤(4)和步骤(5)的射频功率(200W)不同,其余和实施例1相同。
本实施例所制备的高透防刮伤防蓝光纳米薄膜材料的透过率大于91%,防蓝光阻隔率大于75%,20次摩擦试验后的透射率和防蓝光阻隔率分别在90%和75%以上。
实施例6
与实施例1相比除了步骤(3)中甲烷流量(30sccm)和硅烷流量(30sccm)以及步骤(4)中的甲烷流量(30sccm)、起始硅烷流量(30sccm)和硅烷流量减少速度(0.75sccm/min)不同,其余和实施例1相同。
本实施例所制备的高透防刮伤防蓝光纳米薄膜材料的透过率大于94%,防蓝光阻隔率大于90%,20次摩擦试验后的透射率和防蓝光阻隔率分别在91%和90%以上。
实施例7
与实施例1相比除了步骤(3)中甲烷流量(50sccm)和硅烷流量(20sccm)以及步骤(4)中的甲烷流量(50sccm)、起始硅烷流量(20sccm)和硅烷流量减少速度(0.5sccm/min)不同,其余和实施例1相同。
本实施例所制备的高透防刮伤防蓝光纳米薄膜材料的透过率大于92%,防蓝光阻隔率大于60%,20次摩擦试验后的透射率和防蓝光阻隔率分别在91% 和60%以上。
实施例8
与实施例1相比除了步骤(5)中甲烷流量(70sccm)不同,其余和实施例1相同。
本实施例所制备的高透防刮伤防蓝光纳米薄膜材料的透过率大于94%,防蓝光阻隔率大于60%,20次摩擦试验后的透射率和防蓝光阻隔率分别在92%和60%以上。
实施例9
与实施例1相比除了氢化非晶碳化硅薄膜沉积厚度(0.5µm)和氢化非晶碳薄膜沉积厚度(1µm)不同,其余和实施例1相同。
本实施例所制备的高透防刮伤防蓝光纳米薄膜材料的透过率大于92%,防蓝光阻隔率大于70%,20次摩擦试验后的透射率和防蓝光阻隔率分别在90%和70%以上。
实施例10
与实施例2相比除了步骤(3)、步骤(4)和步骤(5)的沉积温度(100℃)不同,其余和实施例2相同。
本实施例所制备的高透防刮伤防蓝光纳米薄膜材料的透过率大于93%,防蓝光阻隔率大于70%,20次摩擦试验后的透射率和防蓝光阻隔率分别在90%和68%以上。
实施例11
与实施例2相比除了步骤(3)、步骤(4)和步骤(5)的沉积压强(30Pa)不同,其余和实施例2相同。
本实施例所制备的高透防刮伤防蓝光纳米薄膜材料的透过率大于94%,防蓝光阻隔率大于74%,20次摩擦试验后的透射率和防蓝光阻隔率分别在93%和74%以上。
实施例12
与实施例2相比除了步骤(3)、步骤(4)和步骤(5)的射频功率(500W)不同,其余和实施例2相同。
本实施例所制备的高透防刮伤防蓝光纳米薄膜材料的透过率大于95%,防蓝光阻隔率大于80%,20次摩擦试验后的透射率和防蓝光阻隔率分别在92%和80%以上。
实施例13
与实施例2相比除了步骤(3)中甲烷流量(30sccm)和硅烷流量(30sccm)以及步骤(4)中的甲烷流量(30sccm)、起始硅烷流量(30sccm)和硅烷流量减少速度(0.75sccm/min)不同,其余和实施例2相同。
本实施例所制备的高透防刮伤防蓝光纳米薄膜材料的透过率大于95%,防蓝光阻隔率大于82%,20次摩擦试验后的透射率和防蓝光阻隔率分别在93%和82%以上。
实施例14
与实施例2相比除了步骤(3)中甲烷流量(20sccm)和硅烷流量(40sccm)以及步骤(4)中的甲烷流量(20sccm)、起始硅烷流量(40sccm)和硅烷流量减少速度(1sccm/min)不同,其余和实施例2相同。
本实施例所制备的高透防刮伤防蓝光纳米薄膜材料的透过率大于90%,防蓝光阻隔率大于55%,20次摩擦试验后的透射率和防蓝光阻隔率分别在89%和55%以上。
实施例15
与实施例2相比除了步骤(5)中甲烷流量(40sccm)不同,其余和实施例2相同。
本实施例所制备的高透防刮伤防蓝光纳米薄膜材料的透过率大于92%,防蓝光阻隔率大于60%,20次摩擦试验后的透射率和防蓝光阻隔率分别在90%和60%以上。
实施例16
与实施例2相比除了氢化非晶碳化硅薄膜沉积厚度(1µm)和氢化非晶碳薄膜沉积厚度(0.5µm)不同,其余和实施例2相同。
本实施例所制备的高透防刮伤防蓝光纳米薄膜材料的透过率大于92%,防蓝光阻隔率大于65%,20次摩擦试验后的透射率和防蓝光阻隔率分别在90%和65%以上。
上述的实施例仅为本发明的优选技术方案,而不应视为对于本发明的限制,本申请中的实施例及实施例中的特征在不冲突的情况下,可以相互任意组合。本发明的保护范围应以权利要求记载的技术方案,包括权利要求记载的技术方案中技术特征的等同替换方案为保护范围。即在此范围内的等同替换改进,也在本发明的保护范围之内。
Claims (2)
1.一种高透防刮伤防蓝光纳米薄膜材料的制备方法,其特征在于,该材料包括内层的氢化非晶碳化硅薄膜层、过渡层和外层的氢化非晶碳薄膜层,包括以下步骤:
(1)清洗并干燥基板,先将玻璃/聚碳酸酯片置于无水乙醇中超声清洗,然后利用去离子水对玻璃片再次超声冲洗,最后用氮气吹干;
(2)反应室预抽真空,在50~300℃条件下对反应室预抽真空,至压强低于10-4 Pa;
(3)氢化非晶碳化硅层的制备,以甲烷和硅烷为工作气体,采用等离子体增强化学气相沉积技术在步骤(2)中的反应室内于玻璃/聚碳酸酯基板上制备氢化非晶碳化硅薄膜层,所述的氢化非晶碳化硅薄膜具体制备工艺参数:射频功率:200~500 W,沉积温度:50~300℃,沉积压强:30~200 Pa,甲烷流量:20~50 sccm,硅烷流量:20~40 sccm;
(4)过渡层的制备,以甲烷和硅烷为工作气体,采用等离子体增强化学气相沉积技术在步骤(2)中的反应室内于步骤(3)沉积的氢化非晶碳化硅层上制备过渡层,所述的过渡层具体制备工艺参数:射频功率:200~500 W,沉积温度:50~300℃,沉积压强:30~200 Pa,甲烷流量:20~50 sccm,硅烷流量从起始设定值20~40sccm每分钟减少0.5~1sccm,当硅烷流量减小到零时过渡层沉积完成;
(5)氢化非晶碳层的制备,以氩气稀释的甲烷为工作气体,体积稀释倍数:4~7倍,采用等离子体增强化学气相沉积技术在步骤(2)中的反应室内于步骤(4)沉积的过渡层上制备氢化非晶碳薄膜层,氢化非晶碳薄膜具体制备工艺参数:射频功率:200~500 W,沉积温度:50~300 ℃,沉积压强:30~200 Pa,甲烷流量:40~70 sccm,氩气流量:280 sccm;
(6)退火过程,将步骤(5)中沉积的多层膜放置于真空炉中加热到100~500 ℃,保持10~30 min,并在真空环境中冷却到室温,即可制备得到高透防刮伤防蓝光纳米薄膜材料。
2.根据权利要求1所述的高透防刮伤防蓝光纳米薄膜材料的制备方法,其特征在于,所述的氢化非晶碳化硅薄膜层中,硅原子百分含量为20%~60%;所述的过渡层中,硅原子百分含量从20%~60%均匀减小至零;所述的氢化非晶碳化硅薄膜层沉积厚度:0.5µm~1µm;所述的过渡层沉积厚度为0.5µm;所述的氢化非晶碳薄膜层沉积厚度:0.5µm~1µm。
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