CN113917755B - 一种智能热控薄膜 - Google Patents
一种智能热控薄膜 Download PDFInfo
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- 230000007704 transition Effects 0.000 claims abstract description 21
- 229910052732 germanium Inorganic materials 0.000 claims abstract description 13
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 10
- 238000013329 compounding Methods 0.000 claims abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 238000000137 annealing Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 5
- 239000010931 gold Substances 0.000 claims description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 5
- 239000005083 Zinc sulfide Substances 0.000 claims description 4
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 4
- 108010025899 gelatin film Proteins 0.000 claims description 3
- 229920001721 polyimide Polymers 0.000 claims description 3
- 239000000741 silica gel Substances 0.000 claims description 3
- 229910002027 silica gel Inorganic materials 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 238000007738 vacuum evaporation Methods 0.000 claims description 2
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims description 2
- 230000007774 longterm Effects 0.000 abstract description 4
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- 239000000523 sample Substances 0.000 abstract description 2
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- 229910052786 argon Inorganic materials 0.000 description 15
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 12
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- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/1514—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material
- G02F1/1523—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material comprising inorganic material
- G02F1/1524—Transition metal compounds
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Abstract
本发明属于功能材料技术领域，具体涉及一种高稳定性红外发射率可随温度变化的智能热控薄膜。该薄膜由基底、金属膜层、过渡层/热致变VO2膜层/过渡层/锗膜层多层结构复合而成；具有无功耗，可自主热控管理，发射率调控范围大的优点，解决了现有热控薄膜热控性能不可调，或调控幅度、调控波段有限、长期使用稳定性差的技术难题。可应用于具有常温热控制需求的航天器舱内仪器设备以及结构外表面，尤其适用于对能源、结构、重量及可靠性有着较高要求的深空探测器和微小型航天器。
Description
技术领域
本发明属于功能材料技术领域，涉及一种智能热控薄膜，具体涉及一种高稳定性红外发射率可随温度变化的智能热控薄膜。
背景技术
航天器在太空轨道运行时面临的外部热环境复杂多变。在太阳光辐射下及深冷背景中，表面温差可能达到几百度，较小的热源波动就足以引起航天器温度的大幅变化。因此航天器需要采用有效的热控技术对热量的吸收、传输、排散等进行调节。
热控薄膜具有重量轻、体积小、能耗少、调控灵活等优点，是航天器表面的第一道防护屏障。热控薄膜的热发射率是重要的热辐射性能参数，决定了暴露于空间环境中航天器表面的温度水平。目前绝大多数热控薄膜的热控性能不可调，无法使航天器在难以预知的外部环境下具有自主调节温度的能力。智能型热控薄膜以热致变色材料或电致变色材料为主设计制备，其中以热致变折射率材料VO2为基础的热控薄膜是一大研究方向，可以根据温度变化进行薄膜发射率调节。但仍然存在热控性能不理想、调控波段不够宽、使用寿命有限等问题。
A.Hendaoui等(VO2-based smart coatings with improved emittance-switching properties for an energy-efficient near room-temperature thermalcontrol of spacecrafts,Solar Energy Materials&Solar Cells,2013,117,494–498)通过磁控溅射工艺在石英衬底上制备了Au/SiO2/VO2三层膜结构薄膜，保持Au膜(350nm)和VO2膜(30nm)厚度不变，研究了不同SiO2厚度(460nm、720nm、1030nm、1360nm、1570nm)下膜系的发射率变化。通过测试25℃及100℃的红外反射光谱并计算得出，在SiO2厚度为1030nm时可达到最大红外发射率变化量(2.5μm～25μm)0.46，宽波段红外发射率变化量无法进一步提升。当SiO2厚度为460nm时，3μm～5μm的发射率变化量可达0.85，但该红外波段范围过窄，且该波段不属于黑体辐射强度及热控温度变化的主要波长范围。
兰州空间技术物理研究所(航天器热控薄膜技术，国防工业出版社，2016，91)采用磁控溅射方法在柔性基底上制备了VO2/Ge薄膜，常温下2.5μm～25μm红外发射率为0.06，80℃时2.5μm～25μm红外发射率为0.49，变化量0.43。但VO2膜和Ge膜之间易发生化学反应，导致热循环一定次数后膜层折射率不匹配，红外发射率变化量大大降低，不能长期使用。
发明内容
针对现有技术存在的诸多不足之处，本发明提出一种高稳定性红外发射率可随温度变化的智能热控薄膜，解决了现有热控薄膜热控性能不可调，或调控幅度、调控波段有限、长期使用稳定性差的技术难题。
本发明的目的是这样实现的：以玻璃、硅片或柔性薄膜作为基底，在基底表面依次沉积金属层和过渡层/热致变VO2膜层/过渡层/锗膜层复合结构。金属层能够改变单层热致变VO2膜室温下高发射率高温下低发射率的本征性能，使智能热控薄膜在相变温度以下为高反射率低发射率，在相变温度以上为低反射率高发射率；采用过渡层/热致变VO2膜层/过渡层/锗膜层复合结构，以增加相变前后智能热控薄膜红外发射率的变化量；过渡层位于热致变VO2膜和金属膜、热致变VO2膜和锗膜之间，以防止热致变VO2膜与金属膜、热致变VO2膜与锗膜之间发生化学反应，提高热控薄膜的长期稳定性和循环次数，避免红外发射率变化量减小。
本申请采用的技术方案如下：
一种智能热控薄膜，其特征在于：由基底、金属膜层、组合膜层复合而成；所述组合膜层由至少2个单元结构复合而成，所述单元结构为多层结构，自下而上依次为过渡层、热致变VO2膜层、过渡层和锗膜层。
一种智能热控薄膜，其特征在于：所述基底为石英玻璃、硅片、聚酰亚胺薄膜、硅胶膜中的一种；所述金属膜层为银(Ag)膜、金(Au)膜、铝(Al)膜、铂(Pt)膜或镍(Ni)膜中的一种，厚度为30nm～200nm；所述热致变VO2膜厚度为50nm～300nm；所述过渡层为二氧化硅(SiO2)膜、硫化锌(ZnS)膜、硅(Si)膜中的一种，厚度为30nm～150nm；所述锗(Ge)膜厚度为300nm～650nm。
一种智能热控薄膜，其特征在于：所述组合膜层由2～4个单元结构复合而成。
一种智能热控薄膜，其特征在于：所述单元结构(3)中各膜层的厚度彼此独立。
一种智能热控薄膜，其特征在于：所述组合膜层中各单元结构的厚度彼此独立。
一种智能热控薄膜，其特征在于：所述热致变VO2膜层采用磁控溅射和真空煺火工艺制备而成，其他膜层采用磁控溅射或真空蒸镀工艺制备而成。
本发明的有益技术效果：
本发明涉及的智能热控薄膜，利用相变功能材料VO2膜可通过温度改变引起材料折射率改变，使智能热控薄膜具有随环境温度变化改变红外发射率的特性，进而来控制薄膜的表面温度。智能热控薄膜的相变温度≥68℃，在温度高于相变温度时表现为红外低反射率、高发射率特性，使辐射出去的能量增加；温度低于相变温度时表现为红外高反射率、低发射率特性，辐射出去的能量变少，从而维持温度不再降低。
采用过渡层/热致变VO2膜层/过渡层/锗膜层复合叠加，以增加相变前后智能热控薄膜红外发射率的变化量；过渡层位于热致变VO2膜和金属膜、热致变VO2膜和锗膜之间，以防止热致变VO2膜与金属膜、热致变VO2膜与锗膜之间发生化学反应，提高热控薄膜的长期稳定性和循环次数，避免红外发射率变化量减小。
该智能热控薄膜具有无功耗，可自主热控管理，发射率调控范围大的优点，可应用于具有常温热控制需求的航天器舱内仪器设备以及结构外表面，尤其适用于对能源、结构、重量及可靠性有着较高要求的深空探测器和微小型航天器。
附图说明
图1为本发明涉及的智能热控薄膜结构示意图
其中：1-基底，2-金属层，3-单元结构，3-1-过渡层，3-2-热致变VO2膜层，3-3-锗膜层
具体实施方式
为使本发明的目的、内容和优点更加清楚，下面结合实施例，对本发明的具体实施方式作进一步详细描述。
实施例一
以石英玻璃作为基底材料，采用磁控溅射工艺依次沉积100nmAl膜/45nmSiO2膜/65nmVO2膜/45nmSiO2膜/300nmGe膜/45nmSiO2膜/65nmVO2膜/45nmSiO2膜/300nmGe膜，其中VO2膜直流溅射功率200W，溅射气压0.6Pa，氧气占氧气和氩气总流量的5％；溅射后对VO2膜进行真空煺火处理，450℃褪火3h。Ag膜直流溅射功率50W，氩气气压0.67Pa；SiO2膜射频溅射功率120W，氩气气压0.67Pa；Ge膜直流溅射功率40W，氩气气压0.67Pa。
该智能热控薄膜在2.5μm～25μm波段室温时的发射率为0.13，80℃时的发射率为0.60，发射率变化量达到0.47。循环20000次后，发射率变化量为0.45。
实施例二
以聚酰亚胺薄膜作为基底材料，采用磁控溅射工艺依次沉积80nmAu膜/100nmSiO2膜/150nmVO2膜/80nmSiO2膜/550nmGe膜/50nmSiO2膜/150nmVO2膜/30nmSiO2膜/550nmGe膜/50nmSiO2膜/70nmVO2膜/50nmSiO2膜/550nmGe膜，其中VO2膜直流溅射功率200W，溅射气压0.6Pa，氧气占氧气和氩气总流量的5％；溅射后对VO2膜进行真空煺火处理，450℃褪火3h。Ag膜直流溅射功率50W，氩气气压0.67Pa；SiO2膜射频溅射功率120W，氩气气压0.67Pa；Ge膜直流溅射功率40W，氩气气压0.67Pa。
该智能热控薄膜在2.5μm～25μm波段室温时的发射率为0.12，80℃时的发射率为0.72，发射率变化量达到0.60。循环20000次后，发射率变化量为0.57。
实施例三
以石英玻璃作为基底材料，采用磁控溅射工艺依次沉积30nmAg膜/70nmSiO2膜/300nmVO2膜/50nmSiO2膜/650nmGe膜/50nmSiO2膜/210nmVO2膜/50nmSiO2膜/650nmGe膜/50nmSiO2膜/100nmVO2膜/50nmSiO2膜/650nmGe膜/50nmSiO2膜/50nmVO2膜/60nmSiO2膜/600nmGe膜，其中VO2膜直流溅射功率200W，溅射气压0.6Pa，氧气占氧气和氩气总流量的5％；溅射后对VO2膜进行真空煺火处理，450℃褪火3h。Ag膜直流溅射功率50W，氩气气压0.67Pa；SiO2膜射频溅射功率120W，氩气气压0.67Pa；Ge膜直流溅射功率40W，氩气气压0.67Pa。
该智能热控薄膜在2.5μm～25μm波段室温时的发射率为0.17，80℃时的发射率为0.70，发射率变化量达到0.53。循环20000次后，发射率变化量为0.49。
实施例四
以硅片作为基底材料，依次沉积200nmNi膜/70nmZnS膜/160nmVO2膜/50nmZnS膜/400nmGe膜/100nmZnS膜/50nmVO2膜/50nmZnS膜/400nmGe膜，其中VO2膜通过磁控溅射和真空煺火的方法制备，其他膜层通过真空蒸镀的方法制备。VO2膜直流溅射功率200W，溅射气压0.6Pa，氧气占氧气和氩气总流量的5％；溅射后将VO2膜450℃真空褪火3h。Ag膜蒸镀速率2A/s，最大功率14W，腔室温度35℃；ZnS膜蒸镀速率8A/s，最大功率25W，腔室温度100℃；Ge膜蒸镀速率5A/s，最大功率37W，腔室温度90℃。
该智能热控薄膜在2.5μm～25μm波段室温时的发射率为0.12，80℃时的发射率为0.75，发射率变化量达到0.63。循环20000次后，发射率变化量为0.57。
实施例五
以硅胶膜作为基底材料，依次沉积130nmPt膜/150nmSi膜/210nmVO2膜/60nmSi膜/550nmGe膜/50nmSi膜/140nmVO2膜/50nmSi膜/500nmGe膜/40nmSi膜/60nmVO2膜/50nmSi膜/500nmGe膜，其中VO2膜通过磁控溅射和真空煺火的方法制备，其他膜层通过真空蒸镀的方法制备。VO2膜直流溅射功率200W，溅射气压0.6Pa，氧气占氧气和氩气总流量的5％；溅射后将VO2膜450℃真空褪火3h。VO2膜直流溅射功率200W，溅射气压0.6Pa，氧气占氧气和氩气总流量的5％；溅射后将VO2膜450℃真空褪火3h。Ag膜蒸镀速率2A/s，最大功率14W，腔室温度35℃；Si膜蒸镀速率3.5A/s，最大功率35W，腔室温度120℃；Ge膜蒸镀速率5A/s，最大功率37W，腔室温度90℃。
该智能热控薄膜在2.5μm～25μm波段室温时的发射率为0.11，80℃时的发射率为0.72，发射率变化量达到0.61。循环20000次后，发射率变化量为0.55。
Claims (6)
1.一种智能热控薄膜，其特征在于：由基底(1)、金属膜层(2)、组合膜层复合而成；所述组合膜层由至少2个单元结构(3)复合而成，所述单元结构(3)为多层结构，自下而上依次为过渡层(3-1)、热致变VO2膜层(3-2)、过渡层(3-1)和锗膜层(3-3)；所述过渡层(3-1)为二氧化硅膜、硫化锌膜、硅膜中的一种，厚度为30nm～150nm。
2.根据权利要求1所述的智能热控薄膜，其特征在于：所述基底(1)为石英玻璃、硅片、聚酰亚胺薄膜、硅胶膜中的一种；所述金属膜层(2)为银膜、金膜、铝膜、铂膜或镍膜中的一种，厚度为30nm～200nm；所述热致变VO2膜(3-2)厚度为50nm～300nm；所述锗膜(3-3)厚度为300nm～650nm。
3.根据权利要求1或2所述的智能热控薄膜，其特征在于：所述组合膜层由2～4个单元结构(3)复合而成。
4.根据权利要求1或2所述的智能热控薄膜，其特征在于：所述单元结构(3)中各膜层的厚度彼此独立。
5.根据权利要求1或2所述的智能热控薄膜，其特征在于：所述组合膜层中各单元结构(3)的厚度彼此独立。
6.根据权利要求1或2所述的智能热控薄膜，其特征在于：所述热致变VO2膜层(3-2)采用磁控溅射和真空煺火工艺制备而成，其它膜层采用磁控溅射或真空蒸镀工艺制备而成。
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