CN103866231A - Method for preparing solar selective absorbing coating - Google Patents
Method for preparing solar selective absorbing coating Download PDFInfo
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- CN103866231A CN103866231A CN201210554621.5A CN201210554621A CN103866231A CN 103866231 A CN103866231 A CN 103866231A CN 201210554621 A CN201210554621 A CN 201210554621A CN 103866231 A CN103866231 A CN 103866231A
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24S—SOLAR HEAT COLLECTORS; SOLAR HEAT SYSTEMS
- F24S70/00—Details of absorbing elements
- F24S70/20—Details of absorbing elements characterised by absorbing coatings; characterised by surface treatment for increasing absorption
- F24S70/225—Details of absorbing elements characterised by absorbing coatings; characterised by surface treatment for increasing absorption for spectrally selective absorption
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/40—Solar thermal energy, e.g. solar towers
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Abstract
The invention discloses a method for preparing a solar selective absorbing coating. According to the method, quartz glass is adopted as a substrate, and a groove which is 500-600nm wide and 100-150nm deep is etched on the substrate by using the etching technology; six layers of metal/ceramic multi-layer gradient films with different components are deposited on the substrate provided with the groove by adopting a vacuum coating method; finally, a layer of Al2O3 antireflection layer is deposited on each metal/ceramic multi-layer gradient film by using a vacuum evaporation plating method. By adopting the substrate provided with the groove, light trap action can be generated on the sunlight, so that the solar absorptance of the film is greatly improved; meanwhile, a gradient coating is formed by heat-resisting metal W, Mo and the like, so that the heat resistance of the coating is greatly improved, and the requirements of a high-temperature coating can be met.
Description
Technical field
The invention belongs to solar energy film field, relate to a kind of new coating structure for the preparation of solar selectively absorbing coating, prepared plough groove type metal/ceramic multilayer gradual change solar selectively absorbing coating, has good resistance to elevated temperatures, can be used for solar-energy water heater vacuum endothermic tube.
Background technology
Solar selectively absorbing coating, its basic object is in visible ray and near infrared spectrum district, coating has very high specific absorption (reaching more than 90%), and the infrared emittance of self very low (lower than 5%) can become solar energy converting lower energy density the heat energy of high-energy-density.Therefore, preparing efficient solar selectively absorbing coating is the gordian technique in solar thermal utilization, most important to improving collector efficiency.Since the fifties in last century, solar selectively absorbing coating is a very active research topic in solar energy utilization technique field always.Solar selectively absorbing coating is divided into high temperature coating (400 DEG C of T >) according to the temperature range difference of its work, middle temperature coating (100 DEG C < T < 400 DEG C), low temperature coating (100 DEG C of T <).China, in the sun power coating research and utilization in nearly twenty or thirty year, only limits to lower temperature application, as solar water heater, solar energy dryer, solar energy housing etc. more.But from more long-range viewpoint, middle high-temperature selective coating has better utilization prospect and demand.
Desirable solar selectively absorbing coating be except possessing good optical selective, also should meet optical property long-term stability, weathering resistance strong, cheap, form that coating process is simple, materials supply are sufficient and the condition such as environmentally safe.Conventional selective coating can not all meet these conditions.Problem mainly concentrates on optical property, cost and reparation technology.Along with the development of new material technology, new selective coating has obtained application, and the development of coating type coating is towards the future development of environment-friendly type.With regard to domestic, the preparation of the solar selectively absorbing coating under middle hot conditions is still a difficult point so far at present.
Summary of the invention
1. a preparation method for solar selectively absorbing coating, is characterized in that: adopting quartz glass, as substrate, utilizes lithographic technique, and in substrate, carving width is the groove that 500nm-600nm, the degree of depth are 100-150nmnm, and groove is regular square dentation.
2. according to the substrate fabrication method described in summary of the invention 1, in plough groove type substrate, adopt the method for vacuum plating, metal/ceramic multilayer film with gradually variable in deposition.Rete has six layers, from bottom, by controlling the sputter rate of target, realizes metal concentration and reduces gradually, and concentration of ceramic increases gradually.
3. according to the method for manufacturing thin film described in summary of the invention 2, on metal/ceramic multilayer film with gradually variable, use vacuum evaporation coating method, deposition one deck Al2O3 antireflection layer.
Brief description of the drawings
Fig. 1 film layer structure schematic diagram
Fig. 2 plough groove type structure vertical view
A: substrate width 30mm; B: groove width: 500nm-600nm; C: gash depth: 100nm-150nm; D: metal/ceramic graded bedding thickness: 200nm-250nm; E: anti-reflection layer thickness: 1 μ m
Embodiment
By specific examples, technical scheme of the present invention is further described.
Embodiment 1:
After 3mm*3mm substrate is cleaned, carry out front baking, coating photoresist material, by exposing substrate, soaks and develops, and carries out etching and obtains the wide square roller seating space of designed 500nn-600nm groove (figure bis-), except after glue after rear baking.Substrate is placed in to 100ml dehydrated alcohol ultrasonic oscillation 20min, takes out dry.Gained gash depth 100nm-150nm.
Embodiment 2:
In the substrate of preparing at embodiment 1, adopt magnetic control sputtering device, target is that W target, Al2O3 control condition are: vacuum tightness: 10
-3pa, encourage=2.13A of I, encourage=13V of U, direct supply I
max=1A, the first layer oxygen flow is 5.0cc/s, the time is 20 minutes, W: Al2O3=95: 5; Second layer oxygen flow is 7.0cc/s, W: Al2O3=80: 20, and the time is 20 minutes; The 3rd layer of oxygen flow is 9.0cc/s,, W: Al2O3=60: 40, the time is 20 minutes; The 4th layer of oxygen flow is 11.0cc/s, W: Al2O3=40: 60, and the time is 20 minutes; Layer 5 oxygen flow is 13.0cc/s,, W: Al2O3=20: 80, the time is 20 minutes; Layer 6 oxygen flow is 15.0cc/s,, W: Al2O3=0: 100, the time is 20 minutes.The every layer thickness of six layer films is about 200nm-250nm.To plate metal/sull vacuum evaporation coating last layer Al2O3 antireflective film, condition control is: vacuum tightness: 10
-4pa, electric current: 15A, time 5min, thicknesses of layers is about 1 μ m.
Embodiment 2:
In the substrate of preparing at embodiment 1, adopt magnetic control sputtering device, target is that W target, Al2O3 control condition are: vacuum tightness: 10
-3pa, encourage=2.13A of I, encourage=13V of U, direct supply I
max=1A, the first layer oxygen flow is 1.0cc/s, the time is 20 minutes, W: Al2O3=100: 0; Second layer oxygen flow is 4.0cc/s, W: Al2O3=80: 20, and the time is 20 minutes; The 3rd layer of oxygen flow is 7.0cc/s,, W: Al2O3=60: 40, the time is 20 minutes; The 4th layer of oxygen flow is 10.0cc/s, W: Al2O3=40: 60, and the time is 20 minutes; Layer 5 oxygen flow is 13.0cc/s,, W: Al2O3=20: 80, the time is 20 minutes; Layer 6 oxygen flow is 16.0cc/s,, W: Al2O3=0: 100, the time is 20 minutes.The every layer thickness of six layer films is about 200nm-250nm.To plate metal/sull vacuum evaporation coating last layer Al2O3 antireflective film, condition control is: vacuum tightness: 10
-4pa, electric current: 15A, time 5min, thicknesses of layers is about 1 μ m.
Embodiment 4
In the substrate of preparing at embodiment 1, adopt magnetic control sputtering device, target is that W target, SiO2 control condition are: vacuum tightness: 10-3Pa, encourage=2.13A of I, encourage=13V of U, direct supply Imax=1A.The first layer oxygen flow is 5.0cc/s, and the time is 20 minutes, W: SiO2=100: 0; Second layer oxygen flow is 7.0cc/s, W: SiO2=80: 20, and the time is 20 minutes; The 3rd layer of oxygen flow is 9.0cc/s,, W: SiO2=60: 40, the time is 20 minutes; The 4th layer of oxygen flow is 11.0cc/s, W: SiO2=40: 60, and the time is 20 minutes; Layer 5 oxygen flow is 13.0cc/s,, W: SiO2=20: 80, the time is 20 minutes; Layer 6 oxygen flow is 15.0cc/s,, W: SiO2=0: 100, the time is 20 minutes.The every layer thickness of six layer films is about 200nm-250nm.To plate metal/sull vacuum evaporation coating last layer Al2O3 antireflective film, condition control is: vacuum tightness: 10
-4pa, electric current: 15A, time 5min, thicknesses of layers is about 1 μ m.
Embodiment 5
In the substrate of preparing at embodiment 1, adopt magnetic control sputtering device, target is that W target, SiO2 control condition are: vacuum tightness: 10-3Pa, encourage=2.13A of I, encourage=13V of U, direct supply Imax=1A.The first layer oxygen flow is 1.0cc/s, and the time is 20 minutes, W: SiO2=100: 0; Second layer oxygen flow is 4.0cc/s, W: SiO2=80: 20, and the time is 20 minutes; The 3rd layer of oxygen flow is 7.0cc/s,, W: SiO2=60: 40, the time is 20 minutes; The 4th layer of oxygen flow is 10.0cc/s, W: SiO2=40: 60, and the time is 20 minutes; Layer 5 oxygen flow is 13.0cc/s,, W: SiO2=20: 80, the time is 20 minutes; Layer 6 oxygen flow is 16.0cc/s,, W: SiO2=0: 100, the time is 20 minutes.The every layer thickness of six layer films is about 200nm-250nm.To plate metal/sull vacuum evaporation coating last layer Al2O3 antireflective film, condition control is: vacuum tightness: 10
-4pa, electric current: 15A, time 5min, thicknesses of layers is about 1 μ m.
Embodiment 6
In the substrate of preparing at embodiment 1, adopt magnetic control sputtering device, target is that Mo target, SiO2 control condition are: vacuum tightness: 10-3Pa, encourage=2.13A of I, encourage=13V of U, direct supply Imax=1A.The first layer oxygen flow is 1.0cc/s, and the time is 20 minutes, Mo: SiO2=100: 0; Second layer oxygen flow is 4.0cc/s, Mo: SiO2=80: 20, and the time is 20 minutes; The 3rd layer of oxygen flow is 7.0cc/s,, Mo: SiO2=60: 40, the time is 20 minutes; The 4th layer of oxygen flow is 100cc/s, Mo: SiO2=40: 60, and the time is 20 minutes; Layer 5 oxygen flow is 13.0cc/s,, Mo: SiO2=20: 80, the time is 20 minutes; Layer 6 oxygen flow is 16.0cc/s,, Mo: SiO2=0: 100, the time is 20 minutes.The every layer thickness of six layer films is about 200nm-250nm.To plate metal/sull vacuum evaporation coating last layer Al2O3 antireflective film, condition control is: vacuum tightness: 10
-4pa, electric current: 15A, time 5min, thicknesses of layers is about 1 μ m.
Embodiment 7
In the substrate of preparing at embodiment 1, adopt magnetic control sputtering device, target is that Mo target, SiO2 control condition are: vacuum tightness: 10-3Pa, encourage=2.13A of I, encourage=13V of U, direct supply Imax=1A.The first layer oxygen flow is 5.0cc/s, and the time is 20 minutes, Mo: SiO2=100: 0; Second layer oxygen flow is 7.0cc/s, Mo: SiO2=80: 20, and the time is 20 minutes; The 3rd layer of oxygen flow is 9.0cc/s,, Mo: SiO2=60: 40, the time is 20 minutes; The 4th layer of oxygen flow is 11.0cc/s, Mo: SiO2=40: 60, and the time is 20 minutes; Layer 5 oxygen flow is 13.0cc/s,, Mo: SiO2=20: 80, the time is 20 minutes; Layer 6 oxygen flow is 15.0cc/s,, Mo: SiO2=0: 100, the time is 20 minutes.The every layer thickness of six layer films is about 200nm-250nm.To plate metal/sull vacuum evaporation coating last layer Al2O3 antireflective film, condition control is: vacuum tightness: 10
-4pa, electric current: 15A, time 5min, thicknesses of layers is about 1 μ m.
Embodiment 8
In the substrate of preparing at embodiment 1, adopt magnetic control sputtering device, target is that Mo target, Al2O3 control condition are: vacuum tightness: 10-3Pa, encourage=2.13A of I, encourage=13V of U, direct supply Imax=1A.The first layer oxygen flow is 1.0cc/s, and the time is 20 minutes, Mo: Al2O3=100: 0; Second layer oxygen flow is 4.0cc/s, Mo: Al2O3=80: 20, and the time is 20 minutes; The 3rd layer of oxygen flow is 7.0cc/s,, Mo: Al2O3=60: 40, the time is 20 minutes; The 4th layer of oxygen flow is 10.0cc/s, Mo: Al2O3=40: 60, and the time is 20 minutes; Layer 5 oxygen flow is 13.0cc/s,, Mo: Al2O3=20: 80, the time is 20 minutes; Layer 6 oxygen flow is 16.0cc/s,, Mo: Al2O3=0: 100, the time is 20 minutes.The every layer thickness of six layer films is about 200nm-250nm.To plate metal/sull vacuum evaporation coating last layer Al2O3 antireflective film, condition control is: vacuum tightness: 10
-4pa, electric current: 15A, time 5min, thicknesses of layers is about 1 μ m.
Embodiment 9
In the substrate of preparing at embodiment 1, adopt magnetic control sputtering device, target is that Mo target, Al2O3 control condition are: vacuum tightness: 10-3Pa, encourage=2.13A of I, encourage=13V of U, direct supply Imax=1A.The first layer oxygen flow is 5.0cc/s, and the time is 20 minutes, Mo: Al2O3=100: 0; Second layer oxygen flow is 7.0cc/s, Mo: Al2O3=80: 20, and the time is 20 minutes; The 3rd layer of oxygen flow is 9.0cc/s,, Mo: Al2O3=60: 40, the time is 20 minutes; The 4th layer of oxygen flow is 11.0cc/s, Mo: Al2O3=40: 60, and the time is 20 minutes; Layer 5 oxygen flow is 13.0cc/s,, Mo: Al2O3=20: 80, the time is 20 minutes; Layer 6 oxygen flow is 15.0cc/s,, Mo: Al2O3=0: 100, the time is 20 minutes.The every layer thickness of six layer films is about 200nm-250nm.To plate metal/sull vacuum evaporation coating last layer Al2O3 antireflective film, condition control is: vacuum tightness: 10
-4pa, electric current: 15A, time 5min, thicknesses of layers is about 1 μ m.
Claims (4)
1. the preparation method of a solar selectively absorbing coating.Use lithographic technique, in substrate, carving width is the groove that 500nm-600nm, the degree of depth are 100nm-150nm, and groove is regular square dentation.
2. rete adopts metal/ceramic multilayer gradual manner, uses magnetron sputtering method depositional coating.Rete has six layers, from bottom, by controlling the sputter rate of target, realizes metal concentration and reduces gradually, and concentration of ceramic increases gradually.Every layer thickness is about 200nm-250nm.
3. film is selected refractory metal W, Mo, as the main component of metal level, uses Al2O3, the SiO2 main component as ceramic layer, makes rete have very outstanding performance aspect high temperature resistant.Adopt the rete of this membranous layer ingredient, can be at 600 DEG C steady operation.
4. in the outside of gradual change rete, use vacuum evaporation coating method, deposition one deck Al2O3 antireflection layer.Thicknesses of layers is about 1 μ m, and this rete can reduce the emittance of film with gradually variable, play a protective role simultaneously, and the oxidation of minimizing film and aging.The specific absorption of current thin film can reach 93.8%, and emittance is only 5.1%.
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CN104730603A (en) * | 2015-04-01 | 2015-06-24 | 京东方科技集团股份有限公司 | Anti-reflection stacked structure and manufacture method, substrate and display device thereof |
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CN102203024A (en) * | 2008-10-20 | 2011-09-28 | 阿文戈亚太阳能新技术公司 | Selective solar absorbent coating and manufacturing method |
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CN102203024A (en) * | 2008-10-20 | 2011-09-28 | 阿文戈亚太阳能新技术公司 | Selective solar absorbent coating and manufacturing method |
Non-Patent Citations (2)
Title |
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HITOSHI 等: "Solar selective absorbers based on two-dimensional W surface gratings with submicron periods for high-temperature photothermal conversion", 《SOLAR ENERGY MATERIALS & SOLAR CELLS》 * |
HITOSHI 等: "Solar selective absorbers based on two-dimensional W surface gratings with submicron periods for high-temperature photothermal conversion", 《SOLAR ENERGY MATERIALS & SOLAR CELLS》, vol. 79, no. 1, 31 December 2003 (2003-12-31), pages 35 - 49, XP004446735, DOI: doi:10.1016/S0927-0248(02)00364-1 * |
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CN104730603A (en) * | 2015-04-01 | 2015-06-24 | 京东方科技集团股份有限公司 | Anti-reflection stacked structure and manufacture method, substrate and display device thereof |
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Application publication date: 20140618 |