CN115611526A - 一种可热加工低辐射玻璃及制备方法 - Google Patents
一种可热加工低辐射玻璃及制备方法 Download PDFInfo
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- 239000010410 layer Substances 0.000 claims abstract description 305
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- 229910004205 SiNX Inorganic materials 0.000 claims abstract description 31
- 239000011521 glass Substances 0.000 claims abstract description 28
- 239000000758 substrate Substances 0.000 claims abstract description 16
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- 229910004286 SiNxOy Inorganic materials 0.000 claims abstract description 7
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 28
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 claims description 25
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- 238000013508 migration Methods 0.000 abstract 1
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- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 2
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Abstract
本发明涉及一种可热加工低辐射玻璃及制备方法,玻璃包括玻璃基片和镀膜层,镀膜层自玻璃基片向外依次复合有第一介质层、第一功能层、第二介质层、第一AZO层、第一保护层、第二功能层、第二保护层、第二AZO层、第三介质层;第一介质层、第二介质层、第三介质层为SiNx层、SiOx层、SiNxOy层中的一层或多层;第一功能层为Cu层,第二功能层为Ag层。本发明提供的玻璃,使用成本更低的Cu作为第一功能层,并在第一功能层两侧使用第一介质层和第二介质层保护,减少氧化物使用,从而减少O‑2离子在热加工中迁移对第一功能层的破坏;可在降低贵金属银用量时,保证Cu层在热加工中不被氧化,实现良好的耐加工性和透过色中性。
Description
技术领域
本发明属于镀膜玻璃技术领域,具体涉及一种可热加工低辐射玻璃及制备方法。
背景技术
目前行业通用的办法是使用Ag层作为低辐射玻璃的功能层,但Ag的在地球上的储量有限,是昂贵的不可再生的贵金属。根据公开数据白银每年消费量10亿盎司左右,其中60%为工业需求,约6亿盎司(约1700万千克),每年工业用Ag的消耗量惊人。
因此很早就有专业技术人员尝试将Cu用于低辐射玻璃中代替Ag层作为反射红外热辐射的功能层,但在需要热加工的低辐射玻璃应用中,始终未能找到合适的技术保护Cu在热加工过程中不受损,同时又能保持透过色的中性。
以前的技术应用中通常使用AZO/NiCr+Cu+NiCr/AZO的保护方式,但是热加工过程中AZO内少量的氧离子迁移扩散就能将Cu氧化,造成膜层质量受损,为了保护Cu不被受损,往往使用较厚的NiCr保护Cu,但又会出现另外一个问题:热加工后透过色厚重,严重的影响客户的使用体验。
发明内容
本发明的目的是提供一种可热加工低辐射玻璃及制备方法,减少贵重金属的使用,保护Cu层在热加工过程中不受损,同时又能保持透过色的中性。
为达到上述目的,本发明采用的一种技术方案是:
一种可热加工低辐射玻璃,其包括玻璃基片和镀膜层,所述的镀膜层自所述的玻璃基片向外依次复合有第一介质层、第一功能层、第二介质层、第一AZO层、第一保护层、第二功能层、第二保护层、第二AZO层、第三介质层;所述的第一介质层、第二介质层、第三介质层为SiNx层、SiOx层、SiNxOy层中的一层或多层的组合;所述的第一功能层为Cu层,所述的第二功能层为Ag层。
优选地,所述的第一保护层、第二保护层的材质均为NiCr或Ti、Cr、Ni。
优选地,所述的第一功能层、第二功能层的厚度均为7-20nm。
优选地,所述的第一功能层的厚度为7~16nm;所述的第二功能层的厚度均为9~20nm。
优选地,所述的第一介质层、第二介质层、第三介质层的厚度均为25-80nm;所述的第一AZO层与所述的第二AZO层的厚度均为8-10nm。
优选地,所述的可热加工低辐射玻璃还包括依次设置的第三AZO层、第三保护层、第三功能层、第四保护层、第四AZO层、第四介质层,所述的第三AZO层设置在所述的第三介质层远离所述的第二AZO层一侧;所述的第三保护层、第四保护层均为NiCr层或Ti、Cr、Ni,所述的第三功能层为Ag层;所述的第四介质层为SiNx层、SiOx层、SiNxOy层中的一层或多层的组合。
优选地,所述的第三功能层的厚度为9~20nm。
优选地,所述的第三保护层、第四保护层的厚度均为0~4nm。
优选地,所述的第三AZO层、第四AZO层的厚度均为8-10nm;所述的第四介质层的厚度为30~50nm。
本发明采用的另一种技术方案是:
一种可热加工低辐射玻璃的制备方法,包括如下步骤:采用磁控溅射镀膜方式,在玻璃基板的一侧表面依次镀设所述的第一介质层、第一功能层、第二介质层、第一AZO层、第一保护层、第二功能层、第二保护层、第二AZO层、第三介质层。
由于上述技术方案运用,本发明与现有技术相比具有下列优点:
本发明提供的可热加工低辐射玻璃,使用金属成本更低的Cu作为低辐射玻璃的第一功能层,通过在第一功能层两侧使用第一介质层和第二介质层保护Cu层,减少氧化物的使用,从而减少了O-2离子在热加工过程中迁移对第一功能层Cu的破坏;第一介质层、第二介质层和第一功能层具有良好的膜层结合力,确保了保护层在使用较薄的厚度时仍可具有良好的耐加工性,最大限度的保证热加工后透过色的中性;可以实现在降低贵金属Ag层用量的同时,保证Cu层在热加工过程中不被氧化的目的,最终实现良好的耐加工性和透过色中性;Cu替代部分或者全部Ag,可以尽可能地减少贵重金属的使用,在降低生产成本的同时减少对稀有资源的耗用。
具体实施方式
下面结合所示的实施例对本发明作进一步描述。
实施例1
一种可热加工低辐射玻璃,其包括玻璃基片和镀膜层,镀膜层自玻璃基片向外依次复合有第一介质层、第一功能层、第二介质层、第一AZO层、第一保护层、第二功能层、第二保护层、第二AZO层、第三介质层。
其中,第一介质层、第二介质层、第三介质层为SiNx层、SiOx层、SiNxOy层中的一层或多层的组合;第一功能层为Cu层,第二功能层为Ag层;第一保护层、第二保护层均为NiCr层或Ti、Cr、Ni。
本例中,第一功能层、第二功能层的厚度均为7-20nm,其中,第一功能层的厚度为7~16nm;第二功能层的厚度均为9~20nm;第一介质层、第二介质层、第三介质层的厚度均为25-80nm;第一AZO层与第二AZO层的厚度均为8-10nm。
在本例的一个优选的实施方式中,第一介质层为SiNx层,膜层厚度是46.8nm;第一功能层为Cu层,膜层厚度是10.4nm;第二介质层SiNx层,膜层厚度是69.5nm;第一AZO层,膜层厚度是9nm;第一保护层为NiCr层,膜层厚度是1.1nm;第二功能层为Ag层,膜层厚度是11.9nm;第二保护层为NiCr层,膜层厚度是1.2nm;第二AZO层,膜层厚度是9.0nm;第三介质层为SiNx层,膜层厚度是43.1nm。
本实施例热加工前和热加工后的透过色数据如下:
表1实施例1的可热加工低辐射玻璃的透过色数据
透过色a* | 透过色b* | |
热加工前 | 1.86 | 1.81 |
热加工后 | -0.52 | -0.69 |
由上表可知,本实施例所示的可热加工低辐射玻璃产品热加工后透过颜色呈中性色,其颜色接近自然色。
实施例2
一种可热加工低辐射玻璃,其包括玻璃基片和镀膜层,镀膜层自玻璃基片向外依次复合有第一介质层、第一功能层、第二介质层、第一AZO层、第一保护层、第二功能层、第二保护层、第二AZO层、第三介质层、第三AZO层、第三保护层、第三功能层、第四保护层、第四AZO层、第四介质层。
其中,第一介质层、第二介质层、第三介质层、第四介质层均为SiNx层、SiOx层、SiNxOy层中的一层或多层的组合;第一保护层、第二保护层、第三保护层、第四保护层均为NiCr层或Ti、Cr、Ni;第一功能层为Cu层,第二功能层为Ag层,第三功能层为Ag层。
本例中,第一功能层、第二功能层、第三功能层的厚度均为9~20nm;第一AZO层、第二AZO层、第三AZO层、第四AZO层的厚度均为8-10nm;第一保护层、第二保护层、第三保护层、第四保护层的厚度均为0~4nm;第一功能层、第二功能层、第三功能层的厚度均为9~20nm。
在本例的一个优选的实施方式中,第一介质层为SiNx层,膜层厚度是28.3nm;第一功能层为Cu层,膜层厚度是8.5nm;第二介质层为SiNx层,膜层厚度是73nm;第一AZO层,膜层厚度是9nm;第一保护层为NiCr层,膜层厚度是0.8nm;第二功能层为Ag层,膜层厚度为12.64nm;第二保护层为NiCr层,膜层厚度0.9nm;第二AZO层,膜层厚度为9.0nm;第三介质层为SiNx层,膜层厚度为49.3nm;第三AZO层,膜层厚度为9nm;第三保护层为NiCr层,膜层厚度为0.6nm;第三功能层为Ag层,膜层厚度为8.1nm;第四保护层为NiCr层,膜层厚度为0.7nm;第四AZO层,膜层厚度为9.0nm;第四介质层为SiNx层,膜层厚度为31.5nm。
本实施例热加工前和热加工后的透过色数据如下:
表2实施例2的可热加工低辐射玻璃的透过色数据
透过色a* | 透过色b* | |
热加工前 | -1.1 | 2.9 |
热加工后 | -1.2 | -0.4 |
由上表可知,本实施例所示的可热加工低辐射玻璃产品热加工后透过颜色呈中性色,其颜色接近自然色。
在实施例1和实施例2中,第一介质层、第二介质层、第三介质层、第四介质层材质均以SiNx层为最优,SiNx是一种化学稳定性极好的超强度、超硬度材料,SiNx与玻璃具有良好的结合性能,且具有很强的抗腐蚀、抗机械划伤、抗高温氧化的性能;可以起到提高功能银层对玻璃表面附着力、保护功能银层、调节颜色、提高膜系的硬度的作用。使整个膜系在进行热加工时耐热性更好,机械加工性能更好,以此来改善传统low-E玻璃膜层结合力不足、易划伤的问题。
因SiNx具有较低的扩散系数,在热加工过程中可以非常好的阻挡外界及玻璃内部的O-2和玻璃内部的Na+扩散破坏第一功能层的Cu层。同时Cu和SiNx具有良好的附着力,不管是在热加工前后均能保持膜层附着牢固,确保了膜层具有良好耐加工性。该种膜层设计相比原有技术更好地减少了起膜层过渡、增加附着力的保护层的使用,确保了热加工后具有良好的透过色。
通过在第一功能层两侧使用第一介质层SiNx和第二介质层SiNx保护Cu层,减少氧化物的使用,从而减少了O-2离子在热加工过程中迁移对第一功能层Cu的破坏;第一介质层SiNx、第二介质层SiNx和第一功能层Cu具有良好的膜层结合力,使用SiNx作为功能层Cu的打底膜层和保护层,确保了保护层在使用较薄的厚度(可以尽可能地减少保护层的使用量)时仍可具有良好的耐加工性,最大限度的保证热加工后透过色的中性;可以实现在降低贵金属Ag层用量的同时,保证Cu层在热加工过程中不被氧化的目的,最终实现良好的耐加工性和透过色中性;Cu替代部分或者全部Ag,可以尽可能地减少贵重金属的使用,在降低生产成本的同时减少对稀有资源的耗用。
第一功能层Cu层、第二功能层Ag层、第三功能层Ag层是Low-E玻璃低辐射性能的核心功能层,金属Ag具有非常好的导电性,可以使整个膜层的面电阻和辐射率降低,同时也起着调节膜层颜色和性能的作用。
第一AZO层、第二AZO层、第三AZO层均使用氧化锌铝陶瓷靶材在纯氩气氛围中进行溅射制备而来,溅射速率较高,使用过程不会产生掉渣,膜层表面光滑致密,能够防止前面保护层及功能层被后续溅射过程氧化,起到极好的保护作用,同时,还可以减少low-E玻璃热加工后的光散射,使玻璃颜色更加清晰透彻。
保护层作为Ag层的保护层及平整层,能够保护Ag层不被后续的溅射过程及加工过程氧化,提高Ag层的耐氧化性能;同时保护层与氧化物和氮化物的结合力比Ag与他们的结合力强,保护层的存在使Ag层在膜层中的附着力更加牢靠,提高Ag层的抗常温氧化和抗高温氧化性能;保护层NiCr也是光的强吸收层材料,可以起到调节膜层透光率的作用。其中保护层以NiCr层为最优。
实施例3
实施例1的可热加工低辐射玻璃的制备方法如下:
1、将待镀膜的玻璃基板进行清洗干燥;
2、真空过渡;
3、自玻璃基板向外依次真空磁控溅射形成以下各溅射层,具体溅射方法为:
S1、第一介质层为SiNx层,采用磁控溅射工艺溅射镀膜,膜层厚度范围是25~50nm;
S2、第一功能层为Cu层,采用磁控溅射工艺溅射镀膜,膜层厚度总范围是7~16nm;
S3、第二介质层为SiNx层,采用磁控溅射工艺溅射镀膜,膜层厚度范围是60~80nm;
S4、第一AZO层,采用磁控溅射工艺溅射镀膜,膜层厚度范围是8~10nm;
S5、第一保护层为NiCr层,采用磁控溅射工艺溅射镀膜,膜层厚度范围是0~4nm;
S6、第二功能层为Ag层,采用磁控溅射工艺溅射镀膜,膜层厚度范围是9~20nm;
S7、第二保护层为NiCr层,采用磁控溅射工艺溅射镀膜,膜层厚度范围是0~4nm;
S8、第二AZO层,采用磁控溅射工艺溅射镀膜,膜层厚度范围是8~10nm;
S9、第三介质层为SiNx层,采用磁控溅射工艺溅射镀膜,膜层厚度范围是30~50nm。
其中,步骤S1、S3、S9中第一介质层、第二介质层、第三介质层的溅射方法为:采用交流中频电源,使用靶材为SiAl靶或者纯Si靶,靶材纯度大于99.7%(如果采用SiAl靶,SiAl靶中中Al含量为8~15wt%,SiAl材料中掺杂的Al主要作用是增加膜层材料的导电性,下同),在氩气、氮气混合气体中溅射而成。
步骤S2、S6中第一功能层、第二功能层的溅射方法为:采用直流电源,使用靶材为Cu靶和Ag靶,靶材纯度大于99.99%,在纯氩气工作气体中进行溅射。
步骤S5、S7中第一保护层和第二保护层的溅射方法为:采用直流电源,使用靶材为NiCr靶,靶材纯度大于99.9%,在纯氩气工作气体中进行溅射。
步骤S4、S8中第一AZO层、第二AZO层的溅射方法为:采用交流电源,使用靶材为AZO靶(AZO靶为氧化物陶瓷掺铝氧化锌靶,靶材中Al2O3含量范围是2~3wt%)靶材纯度大于99.8%,在纯氩气工作气体中进行溅射。
实施例4
实施例2的可热加工低辐射玻璃的制备方法如下:
1、将待镀膜的玻璃基板进行清洗干燥;
2、真空过渡;
3、自玻璃基板向外依次真空磁控溅射形成以下各溅射层,具体溅射方法为:
S1、第一介质层为SiNx层,采用磁控溅射工艺溅射镀膜,膜层厚度范围是25~50nm;
S2、第一功能层为功能层Cu,采用磁控溅射工艺溅射镀膜,膜层厚度总范围是7~16nm;
S3、第二介质层为SiNx层,采用磁控溅射工艺溅射镀膜,膜层厚度范围是60~80nm;
S4、第一AZO层,采用磁控溅射工艺溅射镀膜,膜层厚度范围是8~10nm;
S5、第一保护层为NiCr层,采用磁控溅射工艺溅射镀膜,膜层厚度范围是0~4nm;
S6、第二功能层为Ag层,采用磁控溅射工艺溅射镀膜,膜层厚度范围是9~20nm;
S7、第二保护层为NiCr层,采用磁控溅射工艺溅射镀膜,膜层厚度范围是0~4nm;
S8、第二AZO层,采用磁控溅射工艺溅射镀膜,膜层厚度范围是8~10nm;
S9、第三介质层为SiNx层,采用磁控溅射工艺溅射镀膜,膜层厚度范围是30~50nm;
S10、第三AZO层,采用磁控溅射工艺溅射镀膜,膜层厚度范围是8~10nm;
S11、第三保护层为NiCr层,采用磁控溅射工艺溅射镀膜,膜层厚度范围是0~4nm;
S12、第三功能层为Ag层,采用磁控溅射工艺溅射镀膜,膜层厚度范围是9~20nm;
S13、第四保护层为NiCr层,采用磁控溅射工艺溅射镀膜,膜层厚度范围是0~4nm;
S14、第四AZO层,采用磁控溅射工艺溅射镀膜,膜层厚度是8~10nm;
S15、第四介质层为SiNx层,采用磁控溅射工艺溅射镀膜,膜层厚度范围是30~50nm。
其中,步骤S1、S3、S9、S15中第一介质层、第二介质层、第三介质层的溅射方法为:采用交流中频电源,使用靶材为SiAl靶或者纯Si靶,靶材纯度大于99.7%(如果采用SiAl靶,SiAl靶中中Al含量为8~15wt%,SiAl材料中掺杂的Al主要作用是增加膜层材料的导电性,下同),在氩气、氮气混合气体中溅射而成。
步骤S2、S6、S12中第一功能层、第二功能层的溅射方法为:采用直流电源,使用靶材为Cu靶和Ag靶,靶材纯度大于99.99%,在纯氩气工作气体中进行溅射。
步骤S5、S7、S11、S13中第一保护层和第二保护层的溅射方法为:采用直流电源,使用靶材为NiCr靶,靶材纯度大于99.9%,在纯氩气工作气体中进行溅射。
步骤S4、S8、S10中第一AZO层、第二AZO层的溅射方法为:采用交流电源,使用靶材为AZO靶(AZO靶为氧化物陶瓷掺铝氧化锌靶,靶材中Al2O3含量范围是2~3wt%)靶材纯度大于99.8%,在纯氩气工作气体中进行溅射。
本发明的可热加工节能LOW-E产品机械加工性能好,满足异地加工要求,可进行后续切、磨、钢、夹层等工艺加工,便于实现大面积生产且可以保证长期运输、储存过程中不易划伤、氧化等问题;可提高生产效率,减少成本,提高成品率。
本发明提供的可热加工低辐射玻璃,可热加工低辐射薄膜镀在6毫米普通浮法玻璃上经热加工后透过颜色中性,透过色为中性灰,其中透过色a*值的范围是[-3.5,1],b*值的范围是[-2,1];(备注1:目前市场上的可热加工的双银产品透过色a*值一般在[-9,-5]范围内,b*值的范围是[-6,-4]。
上述中,为了能定量的说明和衡量颜色,在国际上一般采用CIE1976L*a*b*色度空间来测量颜色:一般用L或者R来表示亮度,两者有一定的换算关系,数值在0-100范围内,数值越大表示亮度越高;用a*表示红绿度,a*为负表示绿,a*为正表示红,绝对值越大表示绿或者红的程度越大;用b*表示黄蓝度,b*为负表示蓝,b*为正表示黄,绝对值越大表示黄或者蓝的程度越大;a*和b*越接近于零表示透过色越中性)。
该镀膜层设计不局限于可钢化双银产品,非可钢化双银产品、可钢化与非可钢化三银产品亦可通过本发明提出的方法获得良好的透过色。
上述实施例只为说明本发明的技术构思及特点,其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施,并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰,都应涵盖在本发明的保护范围之内。
Claims (10)
1.一种可热加工低辐射玻璃,其特征在于,包括玻璃基片和镀膜层,所述的镀膜层自所述的玻璃基片向外依次复合有第一介质层、第一功能层、第二介质层、第一AZO层、第一保护层、第二功能层、第二保护层、第二AZO层、第三介质层;
所述的第一介质层、第二介质层、第三介质层为SiNx层、SiOx层、SiNxOy层中的一层或多层的组合;
所述的第一功能层为Cu层,所述的第二功能层为Ag层。
2.根据权利要求1所述的可热加工低辐射玻璃,其特征在于,所述的第一保护层、第二保护层的材质均为NiCr或Ti、Cr、Ni。
3.根据权利要求2所述的可热加工低辐射玻璃,其特征在于,所述的第一功能层、第二功能层的厚度均为7-20nm。
4.根据权利要求3所述的可热加工低辐射玻璃,其特征在于,所述的第一功能层的厚度为7~16nm;所述的第二功能层的厚度均为9~20nm。
5.根据权利要求1所述的可热加工低辐射玻璃,其特征在于,所述的第一介质层、第二介质层、第三介质层的厚度均为25-80nm;所述的第一AZO层与所述的第二AZO层的厚度均为8-10nm。
6.根据权利要求1-5任意一项所述的可热加工低辐射玻璃,其特征在于,所述的可热加工低辐射玻璃还包括依次设置的第三AZO层、第三保护层、第三功能层、第四保护层、第四AZO层、第四介质层,所述的第三AZO层设置在所述的第三介质层远离所述的第二AZO层一侧;所述的第三保护层、第四保护层均为NiCr层或Ti、Cr、Ni,所述的第三功能层为Ag层;所述的第四介质层为SiNx层、SiOx层、SiNxOy层中的一层或多层的组合。
7.根据权利要求6所述的可热加工低辐射玻璃,其特征在于,所述的第三功能层的厚度为9~20nm。
8.根据权利要求6所述的可热加工低辐射玻璃,其特征在于,所述的第三保护层、第四保护层的厚度均为0~4nm。
9.根据权利要求6所述的可热加工低辐射玻璃,其特征在于,所述的第三AZO层、第四AZO层的厚度均为8-10nm;所述的第四介质层的厚度为30~50nm。
10.一种制备权利要求1-9任一项所述的可热加工低辐射玻璃的方法,其特征在于,包括如下步骤:采用磁控溅射镀膜方式,在玻璃基板的一侧表面依次镀设所述的第一介质层、第一功能层、第二介质层、第一AZO层、第一保护层、第二功能层、第二保护层、第二AZO层、第三介质层。
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