CN106868451B - 一种具有vo2镀膜的智能节能玻璃的镀膜工艺 - Google Patents

一种具有vo2镀膜的智能节能玻璃的镀膜工艺 Download PDF

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CN106868451B
CN106868451B CN201710193452.XA CN201710193452A CN106868451B CN 106868451 B CN106868451 B CN 106868451B CN 201710193452 A CN201710193452 A CN 201710193452A CN 106868451 B CN106868451 B CN 106868451B
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洪铮铮
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Abstract

本发明公开了一种具有VO2镀膜的智能节能玻璃的镀膜工艺,包括玻璃基底、VO2镀层和增透层,镀膜工艺为:将玻璃基底超声清洗,烘干备用;将玻璃基底和钨掺杂纳米VO2放入真空室内,抽真空,加热玻璃基底,充入氩气,施加负偏压,辉光放电清洗,充入氮气,施加负偏压,调解多弧电流,进行多弧离子镀,得具有VO2镀层的玻璃基底;将Nd2O5和B2O3混合,放入坩埚中,将具有VO2镀层的玻璃基底放入真空室中,抽真空,采用电子束蒸发源加热镀膜,镀膜完成后,即得具有VO2镀膜的智能节能玻璃。本发明制备的智能节能玻璃具有低发射率,高可见光透过率等优点,同时能够对不同季节的阳光热调控,实现了冬暖夏凉的智能节能模式。

Description

一种具有VO2镀膜的智能节能玻璃的镀膜工艺
技术领域
本发明涉及特殊性能的玻璃领域,具体涉及一种具有VO2镀膜的智能节能玻璃的镀膜工艺。
背景技术
为实现玻璃的节能功能,一般在玻璃表面镀制具备某种特殊性能的薄膜,此种玻璃称为镀膜玻璃。目前,按照对太阳辐射热量调控类型和建筑物周围环境辐射热量的不同,可分为两大类:基于太阳得热隔热技术和调控技术的节能玻璃。
其中,基于隔热技术的节能玻璃,一般采用中空、夹层玻璃等方式仅对热传导和热对流进行了控制,这种双层或者多层结构的节能玻璃虽然较好地抑制了由传导和对流导致的热量损失,但是并未考虑热辐射造成的损失。
基于得热调控技术的节能玻璃中一类为:通过对太阳热的吸收或反射来减少进入室内的太阳热量,因此一般情况下适用于夏热冬暖地区,可以减少制冷能耗;另一类为:通过在玻璃上镀制具有可响应外界激励动态调控光通断的功能性薄膜进而实现对太阳能摄入量调控的节能玻璃。这种节能玻璃克服了太阳得热静态调控节能玻璃只能适合于夏热冬暖地区的缺点,其可以通过相应环境条件的改变,进而实现冷热双向的智能调节,达到适用于更加广泛地区的目的。
中国专利CN201610123717.4公开了一种环保智能玻璃,为两层透明玻璃,在两层透明玻璃之间设有液晶膜层,交流供电电源通过控制装置与液晶膜层两侧接线端连接。但是该专利由于热辐射造成能量损失,同时由于多层玻璃降低了其透光率。
因此,为解决上述问题,需要一种有低发射率,高可见光透过率,同时能够对不同季节的阳光热调控,实现了冬暖夏凉的智能节能模式的智能节能玻璃。
发明内容
本发明针对上述问题,提供一种具有VO2镀膜的智能节能玻璃的镀膜工艺。
本发明解决上述问题所采用的技术方案是:一种具有VO2镀膜的智能节能玻璃,包括玻璃基底、VO2镀层和增透层,具有VO2镀膜的智能节能玻璃的镀膜工艺,包括以下步骤:
步骤S1,玻璃前处理:将玻璃基底放入体积分数为50%~70%的乙醇溶液中,进行超声清洗5min~8min,清洗2次~3次,然后烘干备用;
步骤S2,VO2镀层:将步骤S1处理后的玻璃基底作为衬底放入真空室中的阴极位置上,将钨掺杂纳米VO2作为镀层材料放入真空室内,抽真空至真空度为10-4Pa~10-6Pa,加热玻璃基底,然后充入氩气使真空度为10-1Pa~10-2Pa,开启电源,对玻璃基底施加负偏压500V~800V,进行辉光放电清洗 6min~10min,然后在真空室内充入氮气至真空度为10-1Pa~10-2Pa,对玻璃基底施加负偏压为160V~200V,调解多弧电流至250A~300A,进行多弧离子镀VO2镀层,即得具有VO2镀层的玻璃基底;
步骤S3,增透层:将Nd2O5和B2O3混合作为镀层材料,放入真空室的坩埚中,将步骤S2得到的具有VO2镀层的玻璃基底作为衬底放入真空室中,抽真空至真空度为10-2Pa~10- 4Pa,然后开启电源,采用电子束蒸发源加热镀膜,镀膜完成后,即得具有VO2镀膜的智能节能玻璃;
其中,钨掺杂纳米VO2具有金属-绝缘体相互转变的特性,由于其具有在相变前后较大差值的电阻率和其相转变温度接近室温,作为玻璃变色系统,镀制在玻璃的表面,使其对太阳热的通透性能够随着外界环境温度的变化而变化;掺杂B2O3的Nd2O5在中远红外区具有高反射率,降低了VO2智能节能薄膜的发射率,同时提高智能节能玻璃的透光率。
进一步地,VO2镀层的厚度为:20nm~30nm。
进一步地,增透层的厚度为:30nm~50nm。
进一步地,步骤S2中,钨掺杂纳米VO2的粒径为:30nm~50nm。
进一步地,步骤S2中,玻璃基底加热后的温度为:200℃~300℃。
进一步地,步骤S2中,充入氮气的体积为:氩气体积的10%~20%。
进一步地,步骤S2中,多弧离子镀VO2镀层的镀膜时间为:30min~40min。
进一步地,步骤S3中,Nd2O5和B2O3的质量比为:1:0.05~0.1。
进一步地,步骤S3中,电子束蒸发源加热的温度为:1000℃~1200℃。
进一步地,步骤S3中,镀膜的时间为:40min~50min。
本发明的优点是:
1.本发明制备的智能节能玻璃具有低发射率,高可见光透过率等优点,同时能够对不同季节的阳光热调控,实现了冬暖夏凉的智能节能模式;其中,钨掺杂纳米VO2具有金属-绝缘体相互转变的特性,由于其具有在相变前后较大差值的电阻率和其相转变温度接近室温,作为玻璃变色系统,镀制在玻璃的表面,使其对太阳热的通透性能够随着外界环境温度的变化而变化;掺杂B2O3的Nd2O5在中远红外区具有高反射率,降低了VO2智能节能薄膜的发射率,同时提高智能节能玻璃的透光率;
2.本发明镀膜工艺简单,镀膜结构均匀,缺陷少,性能好;其中镀VO2镀层时,充入氮气,防止VO2的氧化。
具体实施方式
以下对本发明的实施例进行详细说明,但是本发明可以由权利要求限定和覆盖的多种不同方式实施。
实施例1
一种具有VO2镀膜的智能节能玻璃,包括玻璃基底、VO2镀层和增透层;其中,VO2镀层的厚度为:20nm;增透层的厚度为:30nm;具有VO2镀膜的智能节能玻璃的镀膜工艺,包括以下步骤:
步骤S1,玻璃前处理:将玻璃基底放入体积分数为50%的乙醇溶液中,进行超声清洗5min,清洗2次,然后烘干备用;
步骤S2,VO2镀层:将步骤S1处理后的玻璃基底作为衬底放入真空室中的阴极位置上,将钨掺杂纳米VO2作为镀层材料放入真空室内,抽真空至真空度为10-4Pa,加热玻璃基底,然后充入氩气使真空度为10-1Pa,开启电源,对玻璃基底施加负偏压500V,进行辉光放电清洗6min,然后在真空室内充入氮气至真空度为10-1Pa,对玻璃基底施加负偏压为160V,调解多弧电流至250A,进行多弧离子镀VO2镀层,即得具有VO2镀层的玻璃基底;其中,钨掺杂纳米VO2的粒径为:30nm;玻璃基底加热后的温度为:200℃;充入氮气的体积为:氩气体积的10%;多弧离子镀VO2镀层的镀膜时间为:30min;
步骤S3,增透层:将Nd2O5和B2O3混合作为镀层材料,放入真空室的坩埚中,将步骤S2得到的具有VO2镀层的玻璃基底作为衬底放入真空室中,抽真空至真空度为10-2Pa,然后开启电源,采用电子束蒸发源加热镀膜,镀膜完成后,即得具有VO2镀膜的智能节能玻璃;其中,Nd2O5和B2O3的质量比为: 1:0.05;电子束蒸发源加热的温度为:1000℃;镀膜的时间为:40min。
实施例2
一种具有VO2镀膜的智能节能玻璃,包括玻璃基底、VO2镀层和增透层;其中,VO2镀层的厚度为:22nm;增透层的厚度为:35nm;具有VO2镀膜的智能节能玻璃的镀膜工艺,包括以下步骤:
步骤S1,玻璃前处理:将玻璃基底放入体积分数为55%的乙醇溶液中,进行超声清洗6min,清洗2次,然后烘干备用;
步骤S2,VO2镀层:将步骤S1处理后的玻璃基底作为衬底放入真空室中的阴极位置上,将钨掺杂纳米VO2作为镀层材料放入真空室内,抽真空至真空度为5×10-5Pa,加热玻璃基底,然后充入氩气使真空度为2×10-2Pa,开启电源,对玻璃基底施加负偏压600V,进行辉光放电清洗7min,然后在真空室内充入氮气至真空度为2×10-2Pa,对玻璃基底施加负偏压为180V,调解多弧电流至 270A,进行多弧离子镀VO2镀层,即得具有VO2镀层的玻璃基底;其中,钨掺杂纳米VO2的粒径为:35nm;玻璃基底加热后的温度为:220℃;充入氮气的体积为:氩气体积的12%;多弧离子镀VO2镀层的镀膜时间为:34min;
步骤S3,增透层:将Nd2O5和B2O3混合作为镀层材料,放入真空室的坩埚中,将步骤S2得到的具有VO2镀层的玻璃基底作为衬底放入真空室中,抽真空至真空度为5×10-3Pa,然后开启电源,采用电子束蒸发源加热镀膜,镀膜完成后,即得具有VO2镀膜的智能节能玻璃;其中,Nd2O5和B2O3的质量比为:1:0.07;电子束蒸发源加热的温度为:1050℃;镀膜的时间为:42min。
实施例3
一种具有VO2镀膜的智能节能玻璃,包括玻璃基底、VO2镀层和增透层;其中,VO2镀层的厚度为:28nm;增透层的厚度为:40nm;具有VO2镀膜的智能节能玻璃的镀膜工艺,包括以下步骤:
步骤S1,玻璃前处理:将玻璃基底放入体积分数为60%的乙醇溶液中,进行超声清洗7min,清洗3次,然后烘干备用;
步骤S2,VO2镀层:将步骤S1处理后的玻璃基底作为衬底放入真空室中的阴极位置上,将钨掺杂纳米VO2作为镀层材料放入真空室内,抽真空至真空度为10-5Pa,加热玻璃基底,然后充入氩气使真空度为8×10-2Pa,开启电源,对玻璃基底施加负偏压700V,进行辉光放电清洗8min,然后在真空室内充入氮气至真空度为8×10-2Pa,对玻璃基底施加负偏压为190V,调解多弧电流至 280A,进行多弧离子镀VO2镀层,即得具有VO2镀层的玻璃基底;其中,钨掺杂纳米VO2的粒径为:45nm;玻璃基底加热后的温度为:280℃;充入氮气的体积为:氩气体积的18%;多弧离子镀VO2镀层的镀膜时间为:38min;
步骤S3,增透层:将Nd2O5和B2O3混合作为镀层材料,放入真空室的坩埚中,将步骤S2得到的具有VO2镀层的玻璃基底作为衬底放入真空室中,抽真空至真空度为8×10-3PaPa,然后开启电源,采用电子束蒸发源加热镀膜,镀膜完成后,即得具有VO2镀膜的智能节能玻璃;其中,Nd2O5和B2O3的质量比为:1:0.08;电子束蒸发源加热的温度为:1150℃;镀膜的时间为:48min。
实施例4
一种具有VO2镀膜的智能节能玻璃,包括玻璃基底、VO2镀层和增透层;其中,VO2镀层的厚度为:30nm;增透层的厚度为:50nm;具有VO2镀膜的智能节能玻璃的镀膜工艺,包括以下步骤:
步骤S1,玻璃前处理:将玻璃基底放入体积分数为70%的乙醇溶液中,进行超声清洗8min,清洗3次,然后烘干备用;
步骤S2,VO2镀层:将步骤S1处理后的玻璃基底作为衬底放入真空室中的阴极位置上,将钨掺杂纳米VO2作为镀层材料放入真空室内,抽真空至真空度为10-6Pa,加热玻璃基底,然后充入氩气使真空度为10-2Pa,开启电源,对玻璃基底施加负偏压800V,进行辉光放电清洗10min,然后在真空室内充入氮气至真空度为10-2Pa,对玻璃基底施加负偏压为200V,调解多弧电流至 300A,进行多弧离子镀VO2镀层,即得具有VO2镀层的玻璃基底;其中,钨掺杂纳米VO2的粒径为:50nm;玻璃基底加热后的温度为:300℃;充入氮气的体积为:氩气体积的20%;多弧离子镀VO2镀层的镀膜时间为:40min;
步骤S3,增透层:将Nd2O5和B2O3混合作为镀层材料,放入真空室的坩埚中,将步骤S2得到的具有VO2镀层的玻璃基底作为衬底放入真空室中,抽真空至真空度为10-4Pa,然后开启电源,采用电子束蒸发源加热镀膜,镀膜完成后,即得具有VO2镀膜的智能节能玻璃;其中,Nd2O5和B2O3的质量比为: 1:0.1;电子束蒸发源加热的温度为:1200℃;镀膜的时间为:50min。
实验例1
对实施例1~4制备的具有VO2镀膜的智能节能玻璃作为1号~4号样品,进行光透过率和发射率性能测试,测试结果如表1所示。
光透过率测试:采用紫外-可见-近红外分光光度计测试,波长范围为 300nm~2600nm,扫描速度为600nm/min,取波长为1500nm时的值。
发射率测试:采用手持式非制冷焦平面热像仪测试,测试波长范围为 8μm~12μm。
表1具有VO2镀膜的智能节能玻璃的性能测试结果
结果:实施例1~4制备的具有VO2镀膜的智能节能玻璃的可见光透过率为 74%~78%,金属相发射率为:0.24~0.28,半导体相发射率为0.14~0.17。
结论:本发明制备的智能节能玻璃具有低发射率,高可见光透过率等优点,同时能够对不同季节的阳光热调控,实现了冬暖夏凉的智能节能模式。
以上仅为本发明的优选实施例而已,并不用于限制本发明,对于本领域的技术人员来说,本发明可以有各种更改和变化。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。

Claims (9)

1.一种具有VO2镀膜的智能节能玻璃,包括玻璃基底、VO2镀层和增透层,其特征在于,所述具有VO2镀膜的智能节能玻璃的镀膜工艺,包括以下步骤:
步骤S1,玻璃前处理:将所述玻璃基底放入体积分数为50%~70%的乙醇溶液中,进行超声清洗5min~8min,清洗2次~3次,然后烘干备用;
步骤S2,VO2镀层:将步骤S1处理后的玻璃基底作为衬底放入真空室中的阴极位置上,将钨掺杂纳米VO2作为镀层材料放入真空室内,抽真空至真空度为10-4Pa~10-6Pa,加热玻璃基底,然后充入氩气使真空度为10-1Pa~10-2Pa,开启电源,对玻璃基底施加负偏压500V~800V,进行辉光放电清洗6min~10min,然后在真空室内充入氮气至真空度为10-1Pa~10- 2Pa,对玻璃基底施加负偏压为160V~200V,调解多弧电流至250A~300A,进行多弧离子镀VO2镀层,即得具有VO2镀层的玻璃基底;
步骤S3,增透层:将Nd2O5和B2O3混合作为镀层材料,所述Nd2O5和B2O3的质量比为:1:0.05~0.1,放入真空室的坩埚中,将步骤S2得到的具有VO2镀层的玻璃基底作为衬底放入真空室中,抽真空至真空度为10-2Pa~10-4Pa,然后开启电源,采用电子束蒸发源加热镀膜,镀膜完成后,即得所述具有VO2镀膜的智能节能玻璃。
2.根据权利要求1所述的具有VO2镀膜的智能节能玻璃,其特征在于,所述VO2镀层的厚度为:20nm~30nm。
3.根据权利要求1所述的具有VO2镀膜的智能节能玻璃,其特征在于,所述增透层的厚度为:30nm~50nm。
4.根据权利要求1所述的具有VO2镀膜的智能节能玻璃,其特征在于,步骤S2中,所述钨掺杂纳米VO2的粒径为:30nm~50nm。
5.根据权利要求1所述的具有VO2镀膜的智能节能玻璃,其特征在于,步骤S2中,所述玻璃基底加热后的温度为:200℃~300℃。
6.根据权利要求1所述的具有VO2镀膜的智能节能玻璃,其特征在于,步骤S2中,所述充入氮气的体积为:氩气体积的10%~20%。
7.根据权利要求1所述的具有VO2镀膜的智能节能玻璃,其特征在于,步骤S2中,所述多弧离子镀VO2镀层的镀膜时间为:30min~40min。
8.根据权利要求1所述的具有VO2镀膜的智能节能玻璃,其特征在于,步骤S3中,所述电子束蒸发源加热的温度为:1000℃~1200℃。
9.根据权利要求1所述的具有VO2镀膜的智能节能玻璃,其特征在于,步骤S3中,所述镀膜的时间为:40min~50min。
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