CN109282514A - A kind of high temperature resistant solar selectively absorbing coating and preparation method thereof - Google Patents
A kind of high temperature resistant solar selectively absorbing coating and preparation method thereof Download PDFInfo
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- CN109282514A CN109282514A CN201811089579.8A CN201811089579A CN109282514A CN 109282514 A CN109282514 A CN 109282514A CN 201811089579 A CN201811089579 A CN 201811089579A CN 109282514 A CN109282514 A CN 109282514A
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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
- F24S70/30—Auxiliary coatings, e.g. anti-reflective coatings
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- 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
-
- 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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
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- Life Sciences & Earth Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Spectroscopy & Molecular Physics (AREA)
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- Surface Treatment Of Optical Elements (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The present invention relates to a kind of high temperature resistant solar selectively absorbing coatings and preparation method thereof, the high temperature resistant solar selectively absorbing coating is disposed with infrared reflecting layer, absorbed layer and anti-reflection layer by matrix to coating surface, the absorbed layer includes high metal volume fraction composite layer HMVF and low metal volume fraction composite layer LMVF, and the composite layer is by MoSi2Layer and Si3N4Layer alternating deposit and obtain, the MoSi of the high metal volume fraction composite layer HMVF2Fill factor is 40-60%, the MoSi of the low metal volume fraction composite layer LMVF2Fill factor is 10-20%.Solar selectively absorbing coating provided by the invention is still able to maintain preferable absorptivity and lower emissivity under the harsh environment of high temperature, also has longer service life.
Description
Technical field
The present invention relates to solar selectively absorbing coating fields, and in particular, to a kind of high temperature resistant solar selectively
Absorber coatings and preparation method thereof.
Background technique
Energy industry is to evaluate the important indicator of a national national economy, is mentioned for social, people's living standard
Height has important role.With the rise of energy industry, environmental pollution also occurs therewith.Therefore, it needs to find one kind and meet
The new energy in epoch and environmental requirement.
In current social, people have already sought and the clean energy resource that starts with have wind energy, water energy, geothermal energy, nuclear energy,
Solar energy etc..Due to consideration that the safety of nuclear energy have the defects that it is very big, therefore nuclear energy utilization receive great resistance
Hinder.And although wind energy and water energy be using extensively, it can also be influenced by weather.Solar energy is nexhaustible as one kind, takes it
Inexhaustible epoch new energy has very big application potential, and purposes is suitble to the demand of the common people, for pushing state
People's economy has very big effect.It is analyzed according to data, solar year linchpin in all parts of the country firing association amount is up to 3340~8400MJ/m2,
Although earth surface can receive such objective energy, the mankind are very low to the utilization efficiency of solar energy.Therefore, it improves too
The utilization efficiency of positive energy can improve national economy with indirect.
Solar selectively absorbing coating is the key position of solar thermal collector, and selecting good absorber coatings is to improve
The premise of the efficiency of solar energy utilization, the structure of optimum choice absorber coatings are the key that improve the efficiency of solar energy utilization.According to
Temperature is classified, and solar selectively absorbing coating can be divided into low temperature, medium temperature and high-temperature selective absorber coatings, wherein low temperature
Coating for selective absorption is applied to solar water heater, and medium temperature solar selectively absorbing coating is applied to large-sized solar hot water
Device, high-temperature selective absorber coatings are applied on device of solar generating.
In order to improve the utilization efficiency of solar energy, need to research and develop a kind of high temperature resistant coating for selective absorption and its preparation side
Method.
Summary of the invention
It absorbs and applies it is an object of the invention to overcome the deficiencies of the prior art and provide a kind of high temperature resistant solar selectively
Layer, solar selectively absorbing coating provided by the invention are still able to maintain preferable absorptivity under the harsh environment of high temperature
With lower emissivity, also there is longer service life.
Another object of the present invention is to provide the preparation methods of above-mentioned coating.
Another object of the present invention is to provide above-mentioned high temperature resistant solar selectively absorbing coatings in solar water heater
In application.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of high temperature resistant solar selectively absorbing coating, the high temperature resistant solar selectively absorbing coating is by matrix to coating
Surface is disposed with infrared reflecting layer, absorbed layer and anti-reflection layer, and the absorbed layer includes high metal volume fraction composite layer
HMVF and low metal volume fraction composite layer LMVF, the composite layer is by MoSi2Layer and Si3N4Layer alternating deposit and obtain, the height
The MoSi of metal volume score composite layer HMVF2Fill factor is 40 ~ 60%, the low metal volume fraction composite layer LMVF's
MoSi2Fill factor is 10 ~ 20%.
The purpose that absorbed layer is designed as metal gradient type coating is the absorption efficiency for improving it to wavelength by the present invention, from
And improve the utilization efficiency of solar energy.
Preferably, in the high metal volume fraction composite layer HMVF, single layer MoSi2Layer with a thickness of 5 ~ 15nm, single layer
Si3N4Layer with a thickness of 15 ~ 25nm.
Preferably, in the low metal volume fraction composite layer, single layer MoSi2Layer with a thickness of 2-6 nm, single layer Si3N4
Layer with a thickness of 20 ~ 30 nm.
Preferably, the absorbed layer overall thickness is 60 ~ 250 nm.
Preferably, use Ag as infrared reflecting layer；The infrared reflecting layer with a thickness of 80 ~ 120 nm.Matrix due to
It is heated and launches infrared or far infrared wavelength light, distributing for energy can greatly cut down the utilization of solar energy.It selects
Ag is as infrared reflecting layer, and due to the characteristic of metal, Ag infrared reflecting layer has very outside infrared wavelength or far infrared wavelength
High reflectivity, can reduce that matrix is heated and the light of infrared wavelength that emits.This feature is for improving Solar use
Efficiency has extremely important effect.
Preferably, using Si3N4As anti-reflection layer, the anti-reflection layer with a thickness of 40 ~ 60nm.The design of anti-reflection layer for
The absorptivity and service life of coating are improved to a certain extent, Si3N4It is a kind of ceramic material resistant to high temperature, for mentioning
The high-temperature resistance of high coating has significant effect.In addition, Si3N4With biggish forbidden bandwidth, for visible wavelength and
Longer wavelength then can reach absorbed layer through anti-reflection layer.Therefore Si3N4Also there is antireflective work in the coating that the present invention designs
With the utilization efficiency for improving solar energy also has effect of crucial importance.
In the present invention, it is preferred to which the structure of the high temperature resistant solar selectively absorbing coating is Ag/MoSi2-Si3N4
(HMVL)/MoSi2-Si3N4(LMVL)/Si3N4。
The present invention protects the preparation method of above-mentioned high temperature resistant solar selectively absorbing coating simultaneously, and the method is as follows:
Using physical vaporous deposition successively matrix surface deposit infrared reflecting layer, high metal volume fraction composite layer HMVF,
Low metal volume fraction composite layer LMVF and anti-reflection layer.
Preferably, the physical vaporous deposition is magnetron sputtering method.
Application of the above-mentioned high temperature resistant solar selectively absorbing coating in solar water heater is also in protection of the invention
Within the scope of.
The present invention also provides the test methods of the high temperature oxidation resistance of the solar selectively absorbing coating, specifically
Burn-in test condition is as follows: vacuum degree 0.2Pa, and heating rate is 3 DEG C/min, ageing time 10h, 60h, 200h, 300
h。
By long-time burn-in test, the results showed that, high temperature resistant solar selectively absorbing coating provided by the invention
There is no significantly change for absorptivity and emissivity.This bright solar selectively absorbing coating provided by the invention has preferable
High temperature oxidation resistance keeps good stability after long-time high-temperature oxydation.
Compared with prior art, the invention has the following beneficial effects:
High temperature resistant solar selectively absorbing coating provided by the invention is multi-layer nano composite construction, in the harsh ring of high temperature
Good stability, preferable absorptivity and lower emissivity are still able to maintain under border；The solar selectively, which absorbs, to be applied
Layer still keeps good optical property after 700 DEG C of annealing in vacuum high-temperature more than 300 hours, and absorptivity and emissivity respectively reach
0.94 and 0.04；In addition, high temperature resistant solar selectively absorbing coating provided by the invention also has longer service life.
Detailed description of the invention
Fig. 1 is the high temperature resistant solar selectively absorbing coating structural schematic diagram that the embodiment of the present invention 1 provides, wherein (1)
For Ag infrared reflecting layer；It (2) is MoSi2-Si3N4High metal filled layer；It (3) is MoSi2-Si3N4Low metal filled layer；(4) it is
Si3N4Anti-reflection layer；
Fig. 2 high temperature resistant solar selectively absorbing coating provided in this embodiment passes through 700oAfter C vacuum high-temperature aging 300 hours
Reflectance spectrum figure.
Specific embodiment
Further illustrate the present invention below in conjunction with specific embodiments and the drawings, but embodiment the present invention is not done it is any
The restriction of form.Unless stated otherwise, the present invention uses reagent, method and apparatus is the art conventional reagents, method
And equipment.
Unless stated otherwise, agents useful for same and material of the present invention are commercially available.
Embodiment 1
A kind of high temperature resistant solar selectively absorbing coating, preparation method are as follows:
(1) it uses acetone and dehydrated alcohol in each ultrasonic 10 min of ultrasonic cleaner stainless steel base, then uses dried and clean
Compressed air drying.
(2) pretreated matrix is uniformly fixed on bracket, 20 mm of spacing, is packed into vacuum chamber, work support turns
Speed is 5 rpm.
(3) base vacuum is taken out to 5 × 10-3Pa is simultaneously heated to 500 DEG C, is passed through Ar gas and chamber pressure is made to be 1.0 Pa, adjust
Whole bias is that 800 V carry out 5 min of sputter clean, is then cooled to 300 DEG C.
(4) it is then turned on Ag magnetic control target, adjustment Ar air pressure is maintained at 0.9 Pa, opens DC power supply and adjusts sputtering function
Rate is 20W, deposition rate 5nm/min, deposits the Ag infrared reflecting layer that a layer thickness is 100nm on stainless steel base surface.
(5) Ag target, alternating deposit MoSi are closed2And Si3N4Three period of layer.Wherein MoSi2In Ar gas, pressure is layer
It is obtained under 0.9Pa by Mo magnetic target material and Si magnetic control target as sputter.Mo target uses DC power supply, sputtering power 30w；Si target
Using radio-frequency power supply, sputtering power 90W, the MoSi2Thickness in monolayer is 12nm.Si3N4Layer is in N2Air pressure is 0.9Pa by force
Lower deposition, Si rf sputtering power are 90W, the Si3N4Thickness in monolayer is 15 nm.
(6) in the nano combined layer surface of high metal volume fraction, alternating deposit MoSi2And Si3N4Two period of layer.Wherein
MoSi2For layer in Ar gas, pressure is to be obtained under 0.9Pa by Mo magnetic target material and Si magnetic control target as sputter.Mo target uses DC power supply,
Sputtering power is 30w；Si target uses radio-frequency power supply, sputtering power 90W, the MoSi2Thickness in monolayer is 3 nm.Si3N4
Layer is in N2Air pressure is to deposit under 0.9Pa by force, and Si rf sputtering power is 90W, the Si3N4Thickness in monolayer is 25 nm.
(7) Mo target and DC power supply are closed, N is adjusted2Air pressure is 0.9Pa, and radio-frequency power supply power is 89 W, in absorbed layer
Surface deposits the Si that a layer thickness is 50 nm3N4Anti-reflection layer.
(8) Si target and radio-frequency power supply are closed, room temperature is down to temperature and takes out sample.
Fig. 1 is high temperature resistant solar selectively absorbing coating structural schematic diagram provided in this embodiment, wherein (1) is that Ag is red
Outer reflective layer；It (2) is MoSi2-Si3N4High metal filled layer；It (3) is MoSi2-Si3N4Low metal filled layer；It (4) is Si3N4Subtract
Anti- layer.
Fig. 2 is that high temperature resistant solar selectively absorbing coating provided in this embodiment passes through 700 DEG C of vacuum high-temperature agings 300
Reflectance spectrum figure after hour has by theoretical calculation it can be found that absorptivity and emissivity respectively reach 0.94 and 0.04
Good selective absorbing characteristic.
The present invention has also carried out high temperature ageing test to above-mentioned solar selectively absorbing coating, specific as follows:
I carries out 10h, 700 DEG C of high annealing under vacuum conditions
(1) by sample acetone and ethyl alcohol on supersonic wave cleaning machine each ultrasound 10min, dried up with clean compressed air.
(2) pretreated sample is put into vacuum tube furnace, and is evacuated to vacuum 10-2Pa。
(3) it is passed through Ar gas, adjustment air pressure is 0.2Pa, and is heated after through-flow 10min.
(4) adjustment heating rate is 3 DEG C/min, is heated to 700 DEG C and keeps 10h.
(5) it is taken out after temperature drops to room temperature.
According to above annealing burn-in test, optic test the result shows that, absorptivity 0.96, emissivity 0.03.With
Absorptivity and emissivity before annealing do not change significantly, illustrate that coating provided by the invention can keep good at 700 DEG C
Stability.
II carries out 60h, 700 DEG C of high annealing under vacuum conditions
(1) by sample acetone and ethyl alcohol on supersonic wave cleaning machine each ultrasound 10min, dried up with clean compressed air.
(2) pretreated sample is put into vacuum tube furnace, and is evacuated to vacuum 10-2Pa。
(3) it is passed through Ar gas, adjustment air pressure is 0.2Pa, and is heated after through-flow 10min.
(4) adjustment heating rate is 3 DEG C/min, is heated to 700 DEG C and keeps 60h.
(5) it is taken out after temperature drops to room temperature.
According to above annealing burn-in test, optic test the result shows that, absorptivity 0.96, emissivity 0.04.With
Absorptivity and emissivity before annealing also do not change significantly, and illustrate that coating provided by the invention has extraordinary stabilization
Property.
III carries out 200h, 700 DEG C of high annealing under vacuum conditions
(1) by sample acetone and ethyl alcohol on supersonic wave cleaning machine each ultrasound 10min, dried up with clean compressed air.
(2) pretreated sample is put into vacuum tube furnace, and is evacuated to vacuum 10-2Pa。
(3) it is passed through Ar gas, adjustment air pressure is 0.2Pa, and is heated after through-flow 10min.
(4) adjustment heating rate is 3 DEG C/min, is heated to 600 DEG C and keeps 200h.
(5) it is taken out after temperature drops to room temperature.
According to above annealing burn-in test, optic test the result shows that, absorptivity 0.95, emissivity 0.04.With
Absorptivity and emissivity before annealing also do not change significantly, and illustrate that coating provided by the invention has and preferably use the longevity
Life.
IV carries out 300h, 700 DEG C of high annealing under vacuum conditions
(1) by sample acetone and ethyl alcohol on supersonic wave cleaning machine each ultrasound 10min, dried up with clean compressed air.
(2) pretreated sample is put into vacuum tube furnace, and is evacuated to vacuum 10-2Pa。
(3) it is passed through Ar gas, adjustment air pressure is 0.2Pa, and is heated after through-flow 10min.
(4) adjustment heating rate is 3 DEG C/min, is heated to 600 DEG C and keeps 300h.
(5) it is taken out after temperature drops to room temperature.
According to above annealing burn-in test, optic test the result shows that, absorptivity 0.94, emissivity 0.04.With
Absorptivity and emissivity before annealing also do not change significantly, and illustrate that coating provided by the invention has extraordinary stability
And longer service life, it can be applied in real life.
To sum up, solar selectively absorbing coating provided by the invention is still kept good under 700 DEG C of hot environment
Stability.It is tested by long-time high temperature ageing, absorptivity and emissivity change there is no apparent.This shows the present invention
The solar selectively absorbing coating of offer has very big application potential, is expected to realize the application on water heater.
Above-described specific embodiment has carried out further the purpose of the present invention, technical scheme and beneficial effects
It is described in detail, it should be understood that being not intended to limit the present invention the foregoing is merely a specific embodiment of the invention
Protection scope, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should all include
Within protection scope of the present invention.
Claims (10)
1. a kind of high temperature resistant solar selectively absorbing coating, which is characterized in that the high temperature resistant solar selectively, which absorbs, to be applied
Layer is disposed with infrared reflecting layer, absorbed layer and anti-reflection layer by matrix to coating surface, and the absorbed layer includes high metal body
Fraction composite layer HMVF and low metal volume fraction composite layer LMVF, the composite layer is by MoSi2Layer and Si3N4Layer alternating is heavy
It accumulates and obtains, the MoSi of the high metal volume fraction composite layer HMVF2Fill factor is 40 ~ 60%, the low metal volume fraction
The MoSi of composite layer LMVF2Fill factor is 10 ~ 20%.
2. high temperature resistant solar selectively absorbing coating according to claim 1, which is characterized in that the high metal volume point
In number composite layer HMVF, single layer MoSi2Layer with a thickness of 5 ~ 15nm, single layer Si3N4Layer with a thickness of 15 ~ 25 nm.
3. high temperature resistant solar selectively absorbing coating according to claim 1, which is characterized in that the low metal volume point
In number composite layer, single layer MoSi2Layer with a thickness of 2 ~ 6 nm, single layer Si3N4Layer with a thickness of 20 ~ 30 nm.
4. high temperature resistant solar selectively absorbing coating according to claim 1, which is characterized in that the absorbed layer overall thickness
For 60 ~ 250 nm.
5. high temperature resistant solar selectively absorbing coating according to claim 1, which is characterized in that use Ag as infrared anti-
Penetrate layer；The infrared reflecting layer with a thickness of 80 ~ 120nm.
6. high temperature resistant solar selectively absorbing coating according to claim 1, which is characterized in that use Si3N4As anti-reflection
Layer, the anti-reflection layer with a thickness of 40 ~ 60 nm.
7. high temperature resistant solar selectively absorbing coating according to claim 1, which is characterized in that the high temperature resistant solar energy
The structure of coating for selective absorption is Ag/MoSi2-Si3N4(HMVL)/MoSi2-Si3N4(LMVL)/Si3N4。
8. the preparation method of any high temperature resistant solar selectively absorbing coating of claim 1~7, which is characterized in that institute
It is as follows to state method:
Using physical vaporous deposition successively matrix surface deposit infrared reflecting layer, high metal volume fraction composite layer HMVF,
Low metal volume fraction composite layer LMVF and anti-reflection layer.
9. preparation method according to claim 8, which is characterized in that the physical vaporous deposition is magnetron sputtering method.
10. application of any high temperature resistant solar selectively absorbing coating of claim 1~7 in solar water heater.
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| CN201811089579.8A CN109282514B (en) | 2018-09-18 | 2018-09-18 | High-temperature-resistant solar selective absorption coating and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102653151A (en) * | 2012-05-23 | 2012-09-05 | 皇明太阳能股份有限公司 | Solar selective absorption coating |
| CN103625032A (en) * | 2012-08-27 | 2014-03-12 | 中国科学院大连化学物理研究所 | Medium-high temperature solar photothermal selective-absorbing coat |
| CN104949362A (en) * | 2014-03-28 | 2015-09-30 | 北京桑达太阳能技术有限公司 | Solar spectrum selective absorbing coating |
| CN105444443A (en) * | 2014-08-14 | 2016-03-30 | 北京桑达太阳能技术有限公司 | Solar selective absorbing coating and preparation method thereof |
| CN106958005A (en) * | 2017-03-31 | 2017-07-18 | 中国科学院宁波材料技术与工程研究所 | A kind of refractory metal ceramic solar spectral selective absorbing coating and preparation method |
-
2018
- 2018-09-18 CN CN201811089579.8A patent/CN109282514B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102653151A (en) * | 2012-05-23 | 2012-09-05 | 皇明太阳能股份有限公司 | Solar selective absorption coating |
| CN103625032A (en) * | 2012-08-27 | 2014-03-12 | 中国科学院大连化学物理研究所 | Medium-high temperature solar photothermal selective-absorbing coat |
| CN104949362A (en) * | 2014-03-28 | 2015-09-30 | 北京桑达太阳能技术有限公司 | Solar spectrum selective absorbing coating |
| CN105444443A (en) * | 2014-08-14 | 2016-03-30 | 北京桑达太阳能技术有限公司 | Solar selective absorbing coating and preparation method thereof |
| CN106958005A (en) * | 2017-03-31 | 2017-07-18 | 中国科学院宁波材料技术与工程研究所 | A kind of refractory metal ceramic solar spectral selective absorbing coating and preparation method |
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