CN114163142B - 一种磁控溅射单银low-e钢化玻璃及其制造工艺 - Google Patents
一种磁控溅射单银low-e钢化玻璃及其制造工艺 Download PDFInfo
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- 229910052709 silver Inorganic materials 0.000 title claims abstract description 57
- 239000004332 silver Substances 0.000 title claims abstract description 57
- 238000001755 magnetron sputter deposition Methods 0.000 title claims abstract description 40
- 239000005341 toughened glass Substances 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 239000011521 glass Substances 0.000 claims abstract description 86
- 239000000758 substrate Substances 0.000 claims abstract description 35
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000005496 tempering Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000007747 plating Methods 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 49
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 42
- 238000004544 sputter deposition Methods 0.000 claims description 39
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 229910052786 argon Inorganic materials 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 20
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical group [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 claims description 16
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 12
- 238000000576 coating method Methods 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 239000001301 oxygen Substances 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- 229910018487 Ni—Cr Inorganic materials 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 8
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 8
- 239000012495 reaction gas Substances 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims description 3
- 229910001120 nichrome Inorganic materials 0.000 claims 6
- 239000010410 layer Substances 0.000 abstract description 95
- 239000011247 coating layer Substances 0.000 abstract description 7
- 238000009413 insulation Methods 0.000 abstract description 3
- 238000002834 transmittance Methods 0.000 abstract description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical group [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 36
- 239000011787 zinc oxide Substances 0.000 description 18
- 239000011248 coating agent Substances 0.000 description 9
- 230000036760 body temperature Effects 0.000 description 6
- 239000007888 film coating Substances 0.000 description 4
- 238000009501 film coating Methods 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910007667 ZnOx Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000003667 anti-reflective effect Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000007688 edging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000005344 low-emissivity glass Substances 0.000 description 1
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- 238000005457 optimization Methods 0.000 description 1
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- XOFYZVNMUHMLCC-ZPOLXVRWSA-N prednisone Chemical compound O=C1C=C[C@]2(C)[C@H]3C(=O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 XOFYZVNMUHMLCC-ZPOLXVRWSA-N 0.000 description 1
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- 238000001291 vacuum drying Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明属于镀膜钢化玻璃技术领域，具体涉及一种磁控溅射单银LOW‑E钢化玻璃及其制造工艺。本发明提供的磁控溅射单银LOW‑E钢化玻璃的制造工艺，是在玻璃基片上采用磁控溅射法依次镀设SiNx层、ZnOx层、Nicr层、Ag层、Nicr层、ZnOx层、SiNx层，得到单银LOW‑E玻璃；然后对单银LOW‑E玻璃进行物理钢化，得所述的磁控溅射单银LOW‑E钢化玻璃。本发明制得的磁控溅射单银LOW‑E钢化玻璃，具有较好的隔热性能和遮阳性能，透过率偏差小，颜色偏差小，其镀膜层致密均匀且结合力强，质量稳定，综合性能优异。
Description
技术领域
本发明属于镀膜钢化玻璃技术领域，具体涉及一种磁控溅射单银LOW-E钢化玻璃及其制造工艺。
背景技术
Low-E玻璃又称低辐射玻璃，是在玻璃表面镀上多层金属或其他化合物组成的膜系产品。Low-E镀膜玻璃在当代生产和生活中扮演着重要角色，广泛应用于建筑物的门窗、汽车车窗和挡风玻璃等场所。
钢化玻璃是一种预应力玻璃，为提高玻璃的强度，通常使用化学或物理的方法，在玻璃表面形成压应力，玻璃承受外力时首先抵消表层应力，从而提高了承载能力，增强玻璃自身抗风压性，寒暑性，冲击性等。
但是，现有工艺制造Low-E钢化玻璃仍存在一些难以克服的缺陷。玻璃经过升温再降温的钢化工序，很容易导致镀膜层与玻璃基材的结合力减弱、镀膜层疏松不均匀。
发明内容
针对现有技术存在的不足，本发明提供一种磁控溅射单银LOW-E钢化玻璃及其制造工艺。
本发明提供的磁控溅射单银LOW-E钢化玻璃的制造工艺，是在玻璃基片上采用磁控溅射法依次镀设第一膜层、第二膜层、第三膜层、第四膜层、第五膜层、第六膜层和第七膜层，得到单银LOW-E玻璃；然后对单银LOW-E玻璃进行物理钢化，得所述的磁控溅射单银LOW-E钢化玻璃；
第一膜层为SiNx层，SiNx层的厚度为13～17nm；
第二膜层为ZnOx层，ZnOx层的厚度为8～12nm；
第三膜层为Nicr层，Nicr层的厚度为1.5～3nm；
第四膜层为Ag层，Ag层的厚度为8～12nm；
第五膜层为Nicr层，Nicr层的厚度为1.5～3nm；
第六膜层为ZnOx层，ZnOx层的厚度为28～32nm；
第七膜层为SiNx层，SiNx层的厚度为28～32nm。
进一步地，单银LOW-E玻璃的钢化是，先将单银LOW-E玻璃预热至550~580℃，再加热至650~680℃，再冷却至 30~40℃；预热时长为180~200s，加热时长为180~200s，冷却时间为120s。
进一步地，预热单银LOW-E玻璃时，预热炉上炉体的温度依次为535℃、550℃、560℃、550℃、535℃，预热炉下炉体温度依次为545℃、560℃、570℃、560℃和545℃。
进一步地，加热单银LOW-E玻璃时，加热炉上炉体的温度依次为635℃、650℃、660℃、660℃和635℃，下炉体的温度为645℃、660℃、670℃、660℃和645℃。
进一步地，冷却单银LOW-E玻璃时，风量平衡设置码数为130码，风栅开合为26/22码。
进一步地，玻璃基片的镀膜工艺包括以下步骤：
步骤1：采用旋转阴极在玻璃基片上溅射氮化硅；采用气体成分为氩:氮体积比为=15:100，在真空条件下，保持气体压力为2.5bar状态下磁控溅射SiNx层，用交流中频电源、氮气作反应气体溅射SiAl；
步骤2：在完成步骤1的玻璃基片上采用旋转阴极极溅射ZnOx；采用气体成分为氩:氧体积比为=15:100，在真空条件下，保持气体压力为2.5bar状态下磁控溅射ZnOx层，用交流中频电源、氧气作反应气体溅射陶瓷Zn靶；
步骤3：在完成步骤2的玻璃基片上采用平面阴极溅射金属镍铬；采用气体成分为纯氩，在真空条件下，保持气体压力为3.0bar状态下磁控溅射Nicr层，用直流电流电源溅射；
步骤4：在完成步骤3的玻璃基片上，采用平面阴极溅射金属银；采用气体成分为纯氩，在真空条件下，保持气体压力为3.0bar状态下磁控溅射Ag层，用直流电源溅射；
步骤5：在完成步骤4的玻璃基片，采用平面阴极溅射金属镍铬；采用气体成分为纯氩，在真空条件下，保持气体压力为3.0bar状态下磁控溅射Nicr层，用直流电源溅射；
步骤6：在完成步骤5的玻璃基片上采用旋转阴极极溅射ZnOx；采用气体成分为氩:氧体积比为=15:100，在真空条件下，保持气体压力为2.5bar状态下磁控溅射ZnOx层，用交流中频电源、氧气作反应气体溅射ZnOx；
步骤7：在完成步骤6的玻璃基片，采用旋转阴极溅射氮化硅；采用气体成分为氩:氮体积比为=15:100，在真空条件下，保持气体压力为2.5bar状态下磁控溅射SiNx层，用交流中频电源、氮气作反应气体溅射SiAl。
有益效果：
1. 本发明通过对磁控溅射工艺的深度优化将镀膜层溅射在玻璃基材上，在玻璃表面形成致密均匀的镀膜层，并且使镀膜层与玻璃基材之间形成很强的结合力强。
2. 本发明通过镀膜层结构和成分设计，制得的磁控溅射单银LOW-E钢化玻璃具有较好的隔热性能和遮阳性能，能够在保证室内采光充足的条件下，有效地屏蔽进入室内的太阳辐射能，避免室内温度升高，节约室内空调的能源消耗。
3. 本发明提供的磁控溅射单银LOW-E钢化玻璃，钢化前后透过率偏差小于1.5％，偏移小，ΔE＜1.5，颜色偏差小。
4. 本发明钢化阶段采用对流加热方式，显著地改善单银LOW-E玻璃在钢化加热过程中的传热状况，预加热可控制玻璃升温幅度，控制膜层面吸热速度，实现对银层的有效保护。
5. 本发明钢化阶段获得了相互匹配的预热段、加热段的加热时间和加热温度，设计不同对流风机的对流频率，从而生产出高质量的单银LOW-E玻璃。
附图说明
图1为本发明提供的磁控溅射单银LOW-E钢化玻璃的结构示意图。
图中，1第一膜层、2第二膜层、3第三膜层、4第四膜层、5第五膜层、6第六膜层、7第七膜层。
具体实施方式
下面通过具体实施例进一步阐明本发明，这些实施例是示例性的，旨在说明问题和解释本发明，并不是一种限制。
第一阶段为镀膜阶段，如图1所示，在玻璃基片上采用磁控溅射的方式依次镀设七层镀膜。
第一膜层1为SiNx层，即氮化硅层，SiNx是一种非常坚硬的材料，它确保了整个镀层具有良好的机械耐久性，设置在最内层作为保护玻璃的最后一道屏障，SiNx层的厚度为13～17nm。
第二膜层2为ZnOx层，即氧化锌层，是减反射的金属氧化物层，提高银膜的导电率，ZnOx的厚度为8～12nm。
第三膜层3为Nicr层，即金属镍铬层，金属镍铬层提高膜层耐磨性，提高钢化时抗高温氧化性，Nicr的厚度为1.5～3nm。
第四膜层4为Ag层，即金属银层，金属银层提供了较低的辐射率，起环保节能的作用，Ag层的厚度为8～12nm。
第五膜层5为Nicr层，即金属镍铬层，金属镍铬层提高膜层耐磨性，提高钢化时抗高温氧化性，Nicr的厚度为1.5～3nm。
第六膜层6为ZnOx层，即氧化锌层，是减反射的金属氧化物层，同时进一步提高银膜的导电率。氧化锌ZnO可用作助熔剂，降低玻璃的烧结温度，用作玻璃涂料，让可见光通过的同时反射红外线，以达到保温或隔热的效果，ZnOx的厚度为28～32nm。
第七膜层7为SiNx层，即氮化硅层，氮化硅层提高钢化时抗高温氧化性，SiNx厚度为28～32nm。
镀膜工艺步骤如下。
预处理步骤：将玻璃基片裁切成所需尺寸，放置在输送带上，随着输送带的运转，玻璃基片进入清洗室，然后用去离子水将玻璃基片清洗干净。清洗干净的玻璃基片随着输送带的运送，进入真空干燥箱中进行干燥。
步骤1：干燥后的玻璃，随着输送带的输送进行1#镀膜室，采用旋转阴极在玻璃基片上溅射第一层的氮化硅。1#镀膜室内，采用气体成分为氩:氮体积比为=15:100，在真空条件下，保持气体压力为2.5bar状态下磁控溅射SiNx层，用交流中频电源、氮气作反应气体溅射SiAl。
步骤2：在1#镀膜室内，完成步骤1的玻璃基片，采用旋转阴极极溅射第二层的ZnOx。1#镀膜室内，采用气体成分为氩:氧体积比为=15:100，在真空条件下，保持气体压力为2.5bar状态下磁控溅射ZnOx层，用交流中频电源、氧气作反应气体溅射陶瓷Zn靶。
步骤3：将完成步骤2的玻璃基片输送至2#镀膜室，采用平面阴极溅射第三层的金属镍铬。2#镀膜室内，采用气体成分为纯氩，在真空条件下，保持气体压力为3.0bar状态下磁控溅射Nicr层，用直流电流电源溅射。
步骤4：在2#镀膜室内，完成步骤3的玻璃基片，采用平面阴极溅射第四层的金属银。2#镀膜室内，采用气体成分为纯氩，在真空条件下，保持气体压力为3.0bar状态下磁控溅射Ag层，用直流电源溅射。
步骤5：在2#镀膜室内，完成步骤4的玻璃基片，采用平面阴极溅射第五层的金属镍铬。2#镀膜室内，采用气体成分为纯氩，在真空条件下，保持气体压力为3.0bar状态下磁控溅射Nicr层，用直流电源溅射。
步骤6：将完成步骤5的玻璃基片输送至3#镀膜室，采用旋转阴极极溅射第六层的ZnOx。3#镀膜室内，采用气体成分为氩:氧体积比为=15:100，在真空条件下，保持气体压力为2.5bar状态下磁控溅射ZnOx层，用交流中频电源、氧气作反应气体溅射ZnOx。
步骤7：完成步骤6的玻璃基片，采用旋转阴极溅射第七层的氮化硅。3#镀膜室内，采用气体成分为氩：氮体积比为=15:100，在真空条件下，保持气体压力为2.5bar状态下磁控溅射SiNx层，用交流中频电源、氮气作反应气体溅射SiAl。
后处理步骤：将完成步骤7的玻璃输送至检测室，进行低辐射镀膜玻璃的合格检测，检测合格的玻璃即为单银LOW-E玻璃，输送至下一工序，将不合格的玻璃做捡废处理，并放置在捡废专用架上。
第二阶段为钢化阶段，该阶段的工艺步骤如下。
步骤1：对单银LOW-E玻璃进行切割、磨边、清洗处理。
步骤2：将处理后的单银LOW-E玻璃通过辊道送入对流钢化炉，预热段和加热段上方分别对应设有对流风机，单银LOW-E玻璃先在对流钢化炉预热段进行预加热，预热炉加热时长为180~200s，预热段温度为550~580℃，预热时，单银LOW-E玻璃靠对流风机所产生的对流进行加热，对流风机对流频率为70Hz。
步骤3：预热处理后的单银LOW-E玻璃进入对流钢化炉加热段，加热炉加热时长为180~200s，加热段温度为650~680℃，初段对流风机对流频率为70Hz、时长20s；中段对流风机对流频率为40~50Hz、时长110s；末段对流段对流风机对流频率为30Hz、时长60s。
步骤4：将加热处理后的单银LOW-E玻璃从对流钢化炉取出，送至风栅来回往复冷却，冷却至 30~40℃，冷却时间为120s，风栅吹风时间120s，上风栅风压为 3800Pa，下风栅风压为3300Pa，通过编码器，控制风量平衡设置码数为130码，控制风栅开合为26/22码，然后冷却至常温，即得钢化的单银LOW-E玻璃。
在步骤2中，预热炉上炉体的温度依次为535℃、550℃、560℃、550℃、535℃，预热炉下炉体温度依次为545℃、560℃、570℃、560℃和545℃。
步骤3中，加热炉上炉体的温度依次为635℃、650℃、660℃、660℃和635℃，下炉体的温度为645℃、660℃、670℃、660℃和645℃。
在步骤4中，风量平衡设置码数为130码，即为上风栅静压箱出风口87%敞开，下风栅静压箱出风口开度为13%敞开。风栅开合为26/22码，即上风栅出风口距单银LOW-E玻璃上表面距离为17mm，下风栅出风口距离单银LOW-E玻璃下表面距离为14mm。
以上实施方式是示例性的，其目的是说明本发明的技术构思及特点，以便熟悉此领域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 (3)
1.一种磁控溅射单银LOW-E钢化玻璃的制造工艺，其特征在于：在玻璃基片上采用磁控溅射法依次镀第一膜层、第二膜层、第三膜层、第四膜层、第五膜层、第六膜层和第七膜层，得到单银LOW-E玻璃；然后对单银LOW-E玻璃进行物理钢化，得所述的磁控溅射单银LOW-E钢化玻璃；
第一膜层为SiNx层，SiNx层的厚度为13～17nm；
第二膜层为ZnOx层，ZnOx层的厚度为8～12nm；
第三膜层为NiCr层，NiCr层的厚度为1.5～3nm；
第四膜层为Ag层，Ag层的厚度为8～12nm；
第五膜层为NiCr层，NiCr层的厚度为1.5～3nm；
第六膜层为ZnOx层，ZnOx层的厚度为28～32nm；
第七膜层为SiNx层，SiNx层的厚度为28～32nm；
单银LOW-E玻璃的钢化是，先将单银LOW-E玻璃预热至550~580℃，再加热至650~680℃，再冷却至 30~40℃；预热时长为180~200s，加热时长为180~200s，冷却时间为120s；
预热单银LOW-E玻璃时，预热炉上炉体的温度依次为535℃、550℃、560℃、550℃、535℃，预热炉下炉体温度依次为545℃、560℃、570℃、560℃和545℃；
加热单银LOW-E玻璃时，加热炉上炉体的温度依次为635℃、650℃、660℃、660℃和635℃，下炉体的温度为645℃、660℃、670℃、660℃和645℃；
玻璃基片的镀膜工艺包括以下步骤：
步骤1：采用旋转阴极在玻璃基片上溅射氮化硅；采用气体成分为氩:氮体积比为=15:100，在真空条件下，保持气体压力为2.5bar状态下磁控溅射SiNx层，用交流中频电源、氮气作反应气体溅射SiAl；
步骤2：在完成步骤1的玻璃基片上采用旋转阴极极溅射ZnOx；采用气体成分为氩:氧体积比为=15:100，在真空条件下，保持气体压力为2.5bar状态下磁控溅射ZnOx层，用交流中频电源、氧气作反应气体溅射陶瓷Zn靶；
步骤3：在完成步骤2的玻璃基片上采用平面阴极溅射金属镍铬；采用气体成分为纯氩，在真空条件下，保持气体压力为3.0bar状态下磁控溅射NiCr层，用直流电源溅射；
步骤4：在完成步骤3的玻璃基片上，采用平面阴极溅射金属银；采用气体成分为纯氩，在真空条件下，保持气体压力为3.0bar状态下磁控溅射Ag层，用直流电源溅射；
步骤5：在完成步骤4的玻璃基片，采用平面阴极溅射金属镍铬；采用气体成分为纯氩，在真空条件下，保持气体压力为3.0bar状态下磁控溅射NiCr层，用直流电源溅射；
步骤6：在完成步骤5的玻璃基片上采用旋转阴极极溅射ZnOx；采用气体成分为氩:氧体积比为=15:100，在真空条件下，保持气体压力为2.5bar状态下磁控溅射ZnOx层，用交流中频电源、氧气作反应气体溅射ZnOx；
步骤7：在完成步骤6的玻璃基片，采用旋转阴极溅射氮化硅；采用气体成分为氩:氮体积比为=15:100，在真空条件下，保持气体压力为2.5bar状态下磁控溅射SiNx层，用交流中频电源、氮气作反应气体溅射SiAl。
2.根据权利要求1所述的磁控溅射单银LOW-E钢化玻璃的制造工艺，其特征在于：冷却单银LOW-E玻璃时，风量平衡设置码数为130码，风栅开合为26/22码。
3.一种磁控溅射单银LOW-E钢化玻璃，其特征在于：根据权利要求1或2所述的制造工艺制得。
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