CN109972111A - A kind of highly doped MoOxBase photothermal conversion coating and preparation method thereof - Google Patents
A kind of highly doped MoOxBase photothermal conversion coating and preparation method thereof Download PDFInfo
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- 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
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- 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
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Abstract
A kind of highly doped MoO provided by the inventionxBase photothermal conversion coating and preparation method thereof, including the high-selenium corn layer and antireflection layer set gradually in substrate according to sequence from the bottom to top；High-selenium corn layer is the MoO of high metal Mo nano particle dopingxLaminated film uses the magnetron sputtering technique of single molybdenum target to prepare, and during the preparation process, oxygen sources only react to form molybdenum oxide in remaining air, very limited oxygen atom with a small number of molybdenum atoms, forms a kind of absorber coatings；Antireflection layer is the MoO of medium characterxAnd SiO2Layer；The gradient-structure of this bilayer, due to the interference effect of light, which can effectively absorb sunlight, enhance the efficiency of light absorption of coating；The MoO of this bilayerxThe characteristics of base coating has structure simple, and preparation cost is low, easily extends, simplifies the preparation process of coating, is suitable for low price, large-scale industrial production.
Description
Technical field
The present invention relates to solar energy optical-thermal switch technology fields, and in particular to a kind of highly doped MoOxBase photothermal conversion coating
And preparation method thereof.
Background technique
With the high speed development of global economy, to petroleum, the demand of the fossil fuels such as natural gas and coal is growing, however
The consumption of fossil fuel can cause serious influence to environment, threaten the survival and development of the mankind, and energy environment issues already become
It is extremely urgent to develop alternative new energy for one of major issue of global concern.Solar energy is as a kind of cleanliness without any pollution
Renewable natural energy resources can be considered as the potential solution for solving environmental pollution and energy consumption crisis.In photothermal conversion skill
In art field, in order to capture more energy from solar radiant energy, the scholar of every field, is constantly explored simultaneously in recent years
The optical-thermal conversion material haveing excellent performance is developed, is studied and is applied in different directions, become photothermal conversion utilization
A very active research topic in technical field.Currently, in the structure design of most of photothermal conversion coating, usually all
It is related to a complicated multilayered structure, such as 3 layers " dielectric-metallic-dielectric " stacked structure, 4 layers of bis- " metal potteries
The concatenated optical interference structure of porcelain " base coating structure, multiple dielectric layers and metal layer, the nitride metal of optical property gradual change
Object/nitrogen oxides multilayered structure etc..However, the preparation process of these coating structures mentioned above is extremely complex, need to make
With two targets even more than the co-sputtering technology of target, this makes the preparation cost of coating very high, and labyrinth is set
Meter is also unfavorable for commercially producing for large-scale so that the scalability of coating is poor.Generally speaking, seek a kind of structure process
Simply, solar energy optical-thermal conversion coating low in cost and excellent in optical properties has very important application prospect.
It is well known that Intrinsic Gettering material is mainly the optical absorption characteristic for reflecting material inherence itself, in nature
In besides semiconductor material, some magnesium-yttrium-transition metals and its oxide, carbide and boride etc., also all have it is very good
Intrinsic Gettering characteristic, but photo-thermal efficiency of the Intrinsic Gettering film of single layer in visible wavelength range is unsatisfactory.One
As for, introducing an antireflection layer on the surface of absorbed layer can effectively promote the light absorpting ability of photo-thermal coating, this is
Due to the Destructive Interference Action of film, the reflection loss of entire membrane system is reduced, more sunlights is made to be incident on coating surface,
It is absorbed by photo-thermal coating.In recent years, the Intrinsic Gettering characteristic of metal carbides and boride of some scholars based on single layer, preparation
The simply double-deck photothermal conversion coating of structure, also shows extraordinary optical absorptive character.However, preparing these coatings
The target of carbide and boride is usually all more expensive, the industrialized production at a low price with large area is highly unsuitable to, to honest and clean
The absorbing material of valence haveing excellent performance is still urgent need.
Similarly, magnesium-yttrium-transition metal molybdenum (Mo) has very high fusing point, it is shown that low thermal expansion coefficient and high red
External reflectance characteristic, but photo-thermal efficiency of the Mo film of single layer in visible wavelength range is unsatisfactory, turns at present in photo-thermal
It changes in the design of coating, Mo is mainly used to infrared metallic reflector or is doped in absorbed layer, such as Mo-Al2O3, Mo-
SiO2, NbMoON, MoAlN etc..
Meanwhile single doping MoOxFilm has high absorption characteristic, but its absorption notch length is shorter, visible
The absorption in light region is unsatisfactory, and photothermal conversion efficiency is relatively low.
Summary of the invention
The purpose of the present invention is to provide a kind of highly doped MoOxBase photothermal conversion coating and preparation method thereof solves existing
The photothermal conversion coating of the multilayered structure of some complexity, the preparation process being related to is complicated, and preparation cost is expensive, and is unfavorable for big
The problem of industrialized production of scale.
In order to achieve the above object, the technical solution adopted by the present invention is that:
A kind of highly doped MoO provided by the inventionxBase photothermal conversion coating, including substrate, according under in the substrate
The high-selenium corn layer and antireflection layer that supreme sequence is set gradually, wherein substrate is the substrate with infrared external reflection function, described
High-selenium corn layer is MoOxLayer, antireflection layer MoOxOr SiO2Dielectric layer.
Preferably, the high-selenium corn MoOxLayer with a thickness of 60~80nm.
Preferably, the antireflection layer with a thickness of 80~130nm.
A kind of highly doped MoOxThe preparation method of base photothermal conversion coating, comprising the following steps:
Step 1, substrate is pre-processed；
Step 2, high-selenium corn layer is deposited in substrate；
Step 3, on high-selenium corn layer deposition medium property MoOxOr SiO2Dielectric layer.
Preferably, in step 1, firstly, by substrate respectively in alcohol, acetone and deionized water through ultrasonic cleaning,
It is secondary, the substrate after cleaning is fitted into magnetron sputtering depositing system and carries out plasma cleaning, wherein the condition of plasma cleaning
Be: house vacuum degree is less than 1.0 × 10-3Pa, the argon gas that purity is 99.999%, argon flow 60sccm, Indoor Air are passed through
Pressure is 5Pa, back bias voltage is -350V.
Preferably, in step 2, pretreated substrate is placed on sample carrier, using molybdenum target as sputtering target material, Xiang Zhen
It is passed through the argon gas of purity 99.999% in empty room, regulating valve plate valve controls deposition pressure, opens molybdenum target, using radio-frequency power supply magnetic
It controls sputtering method and bombards molybdenum target, MoO is deposited in substratexHigh-selenium corn layer, wherein argon flow 35sccm, oxygen sources are in true
Remaining air in empty room, air pressure are 0.3~0.4Pa, and sputtering power is 100~110W.
Preferably, in step 3, using molybdenum target as cathode, using argon gas and oxygen as reaction gas, purity is passed through into vacuum chamber
99.999% argon gas and oxygen opens molybdenum target, in MoOxOne layer of MoO is deposited on high-selenium corn layerxAntireflection layer, wherein argon gas stream
Amount is 35sccm, and oxygen flow is 30~50sccm, and air pressure is 0.4~0.5Pa, and sputtering power is 100~110W.
Preferably, in step 3, with SiO2Target is cathode, and using argon gas as sputter gas, purity is passed through into vacuum chamber
99.999% argon gas opens SiO2Target, in MoOxOne layer of SiO is deposited on high-selenium corn layer2Antireflection layer, wherein argon flow is
35sccm, air pressure 2.5Pa, sputtering power are 130~160W.
Compared with prior art, the beneficial effects of the present invention are:
A kind of highly doped MoO provided by the inventionxBase photothermal conversion coating and preparation method thereof, absorbed layer MoOxMetal
Ceramic membrane, antireflection layer are the MoO of medium characterxOr SiO2Film, due to MoOxFilm has unique multivalent state structure,
The multivalent state structure shows extraordinary optical characteristics and electric property, wherein the MoO of monoclinic system2There are metal-metals
Key, so MoO2Property with metalloid is a kind of opaque conductive film, and pure MoO3The transmitance of film exists
80% or more, it is a kind of transparent medium film；The MoO of this non-stoichiometricxChange between a variety of valence states of film
Change, become a kind of absorbing material haveing excellent performance, has in the design of photothermal conversion coating and potentially apply very much valence
Value；The MoO of complete oxidationxFilm has very high transmitance, and MoOxThe forbidden bandwidth Eg of film is 2.8~3.6eV,
Its cutoff wavelength λcFor 344~442nm, this solar spectrum of explanation greater than 442nm can not be by WOxFilm absorption, so, this
Invention is by the MoO of complete oxidation3Film is used as the antireflection film of photothermal conversion coating；The present invention compares photothermal conversion efficiency
Low doping MoOxFilm is as high-selenium corn layer, in conjunction with MoOxOr SiO2Destructive Interference Action of the film as antireflection layer, preparation
The novel double-deck MoO outxBase solar photothermal conversion coating, the coating are different from traditional complicated assembly of thin films design, this
The characteristics of coating of kind double-layer structure has simple process, and preparation cost is low, and structure extension is good, optical property easy-regulating,
There is boundless application value in solar energy utilization technique.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of photothermal conversion coating of the present invention；
Wherein, 1, substrate 2, high-selenium corn layer 3, antireflection layer.
Specific embodiment
The invention will be described in further detail with reference to the accompanying drawing:
As shown in Figure 1, a kind of highly doped MoO provided by the inventionxBase photothermal conversion coating, including substrate 1, in substrate 1
The high-selenium corn layer 2 and antireflection layer 3 set gradually according to sequence from the bottom to top.
The substrate 1 is the substrate with infrared external reflection function, and the material of substrate 1 is aluminium, copper or stainless steel, specifically,
It can be aluminium flake, copper sheet or stainless steel (316L, 304).
The high-selenium corn layer 2 is MoOxLayer, with a thickness of 60~80nm；This MoOxFilm has very in visible light wave range
Apparent spectral absorption characteristics can be used for absorbed layer in the design of photo-thermal absorbing material, have and potentially answer very much
Use prospect.During the preparation process, oxygen sources remaining air, very limited oxygen atom, so that MoO in depositingxFilm
The laminated film for forming a kind of high metal Mo nano particle doping, has very excellent optical absorption ability.
The antireflection layer 3 is a kind of film of medium character, for reducing the reflection loss of coating surface；Antireflection layer
3 be MoOxOr SiO2Dielectric layer, with a thickness of 80~130nm；The molybdenum oxide of complete oxidation can penetrate the sunlight greater than 344nm
Spectrum, extinction coefficient k < 0.1 is a kind of very valuable antireflection layer material；Traditional SiO2The delustring system of antireflection layer
Number number k=0, has very excellent anti-reflective effect.
The gradient-structure of this bilayer can be effectively absorbed sunlight, be enhanced coating due to the interference effect of film
Efficiency of light absorption.
By highly doped MoO of the inventionxBase photothermal conversion coating is detected according to GB/T25968-2010, survey
MoOx/MoOxFor the solar absorptance of photothermal conversion coating between 0.91~0.92, thermal emissivity is between 0.05~0.06；
MoOx/SiO2The solar absorptance of photothermal conversion coating between 0.89~0.91, thermal emissivity be 0.05~0.06 between,
Illustrate the highly doped MoO of double-layer structurexBase photothermal conversion coating has excellent optical property.
To MoO of the present inventionx/MoOxCoating be heat-treated under vacuum, at 450 DEG C after 200h isothermal holding, according to above-mentioned
Method measures MoO againx/MoOxSolar absorptance~0.913 of coating, emissivity are data between 0.05~0.06
Without large change.To MoO of the present inventionx/SiO2Coating be heat-treated under vacuum, at 450 DEG C after 200h isothermal holding, according to
The above method measures MoO againx/SiO2Solar absorptance~0.899 of coating, emissivity are between 0.05~0.06.
After vacuum annealing, data are without large change, MoO of the inventionxBase photothermal conversion coating is adaptable to high temperature solar energy optical-thermal
Switch technology.
Highly doped MoO of the inventionxPhotothermal conversion coating the preparation method is as follows:
1. being pre-processed to substrate 1
The substrate 1 of polishing is packed into magnetron sputtering depositing system through ultrasonic cleaning in alcohol, acetone and deionized water
In (Shenyang distance of travel of roc vacuum technique Co., Ltd 560C type magnetron sputtering apparatus), by the vacuum degree of the vacuum chamber of magnetic control sputtering system
It is evacuated to less than 1.0 × 10-3Pa；Then the argon gas of purity 99.999% is passed through into vacuum chamber, adjustment air pressure is 5Pa, is opened negative
Bias -350V carries out ion sputtering cleaning to substrate 1, the pollutant and oxide skin on 1 surface of substrate is removed, to improve 1 He of substrate
The binding force of coating.
2. depositing high-selenium corn layer 2 on the base 1
By step, 1. pretreated substrate 1 is placed on sample carrier, and molybdenum target (purity 99.95%) is used as sputtering target
Material is passed through the argon gas of purity 99.999% into vacuum chamber, adjusts deposition pressure, opens molybdenum target, is splashed using radio-frequency power supply magnetic control
Method bombardment tungsten target is penetrated, deposits MoO on the base 1xLayer, as high-selenium corn layer 2.
Parameter setting is as follows: argon flow 60sccm, and air pressure is 0.4~0.5Pa, and sputtering power is 100~110W, splashes
Penetrating the time is 20~30 minutes, controls MoO by control sputtering timexThe thickness of layer regulates and controls MoOxThe optical absorption of layer.
3. depositing MoO on high-selenium corn layer 2xAntireflection layer 3
Using tungsten as cathode, using argon gas and oxygen as reaction gas, be passed through into vacuum chamber purity 99.999% argon gas and
Oxygen opens molybdenum target, and the MoO of one layer of medium character is deposited on high-selenium corn layerxAntireflection layer 3.
Parameter setting is as follows: argon flow 60sccm, and oxygen flow is 30~50sccm, and air pressure is 0.4~0.5Pa,
Sputtering power is 100~110W, and sputtering time is 25~40 minutes, controls MoO by control sputtering timexAntireflection layer 3
Thickness.
4. depositing SiO on high-selenium corn layer 22Antireflection layer 3
Step 2. on the basis of, keep argon flow it is constant, with SiO2Target is cathode, using argon gas as sputter gas, to
It is passed through the argon gas of purity 99.999% in vacuum chamber, opens SiO2Target, in MoOxOne layer of SiO is deposited on absorbed layer2Antireflection layer 3.
Parameter setting is as follows: argon flow 60sccm, air pressure 2.5Pa, and sputtering power is 130~160W, when sputtering
Between be 120~180 minutes, SiO is controlled by control sputtering time2The thickness of antireflection layer 3.
The present invention has the effect of positive:
(1) MoO of the inventionxBase photothermal conversion coating is by substrate, high-selenium corn layer and anti-reflection with infrared external reflection function
Penetrate layer composition.
Wherein, high-selenium corn layer is MoOxFilm, this MoOxFilm is inhaled in visible light wave range with obviously spectrum
Absorbed layer can be used in the design of photo-thermal absorbing material by receiving characteristic, have very potential application prospect.It is making
During standby, oxygen sources remaining air, considerably less oxygen atom, so that MoO in depositingxFilm forms a kind of high metal
The laminated film of Mo nano particle doping, has very high optical absorption ability.
Composite absorption layer is double-deck gradient-structure, and due to the interference effect of light, which can effectively absorb the sun
Light enhances the efficiency of light absorption of coating.
Antireflection layer is MoOxOr SiO2Dielectric layer；The tungsten oxide of complete oxidation can penetrate the sunlight greater than 344nm
Spectrum, extinction coefficient k < 0.1 is a kind of very valuable antireflection layer material；Traditional SiO2The delustring system of antireflection layer
Number number k=0, has very excellent anti-reflective effect.
After tested, MoOx/MoOxBetween 0.90~0.92, thermal emissivity is the solar absorptance of photothermal conversion coating
Between 0.05~0.06；MoOx/SiO2Between 0.89~0.91, thermal emissivity is the solar absorptance of photothermal conversion coating
Between 0.05~0.06, illustrate the MoO of double-layer structurexBase photothermal conversion coating has excellent optical property.
(2) photothermal conversion coating of the invention is only 2 layers of structure, is set different from the multilayered structure of reported complexity
Meter, the MoO of this bilayerxThe characteristics of base coating has structure simple, and preparation cost is low, easily extends has very extensive answer
Use prospect.
Claims (8)
1. a kind of highly doped MoOxBase photothermal conversion coating, which is characterized in that including substrate (1), on the substrate (1) according to by
Under supreme sequence the high-selenium corn layer (2) and antireflection layer (3) that set gradually, wherein substrate (1) is to have the function of infrared external reflection
Substrate, the high-selenium corn layer (2) be MoOxLayer, antireflection layer (3) are MoOxOr SiO2Dielectric layer.
2. a kind of highly doped MoO according to claim 1xBase photothermal conversion coating, which is characterized in that the high-selenium corn layer
(2) with a thickness of 60~80nm.
3. a kind of highly doped MoO according to claim 1xPhotothermal conversion coating, which is characterized in that the antireflection layer (3)
With a thickness of 80~130nm.
4. a kind of highly doped MoOxThe preparation method of photothermal conversion coating, which comprises the following steps:
Step 1, substrate (1) is pre-processed；
Step 2, high-selenium corn layer (2) are deposited on substrate (1)；
Step 3, MoO is deposited on high-selenium corn layer (3)xOr SiO2Dielectric layer.
5. a kind of highly doped MoO according to claim 4xThe preparation method of photothermal conversion coating, which is characterized in that step 1
In, firstly, by substrate through ultrasonic cleaning in alcohol, acetone and deionized water, secondly, the substrate after cleaning is packed into magnetic
Sputter clean is carried out in control sputtering depositing system, wherein the condition of sputter clean is: house vacuum degree is less than 1.0 × 10-3Pa、
Being passed through the argon gas, room pressure 5Pa, back bias voltage that purity is 99.999% is -350V.
6. a kind of highly doped MoO according to claim 4xThe preparation method of photothermal conversion coating, which is characterized in that step 2
In, pretreated substrate is placed on sample carrier, using molybdenum target as sputtering target material, purity is passed through into vacuum chamber
99.999% argon gas adjusts deposition pressure, opens molybdenum target, molybdenum target is bombarded using radio-frequency power supply magnetron sputtering method, in substrate
Deposit MoOxLayer, wherein argon flow 35sccm, for oxygen sources in remaining air, air pressure is 0.3~0.4Pa, sputters function
Rate is 100~110W.
7. a kind of highly doped MoO according to claim 4xThe preparation method of photothermal conversion coating, which is characterized in that step 3
In, using molybdenum target as cathode, using argon gas and oxygen as reaction gas, the argon gas and oxygen of purity 99.999% are passed through into vacuum chamber
Gas opens molybdenum target, in MoOxOne layer of MoO is deposited on absorbed layerxAntireflection layer, wherein argon flow 35sccm, oxygen flow
For 30~50sccm, air pressure is 0.4~0.5Pa, and sputtering power is 100~110W.
8. a kind of highly doped MoO according to claim 4xThe preparation method of photothermal conversion coating, which is characterized in that step 3
In, with SiO2Target is cathode, and using argon gas as sputter gas, the argon gas of purity 99.999% is passed through into vacuum chamber, opens SiO2
Target, in MoOxOne layer of SiO is deposited on absorbed layer2Antireflection layer, wherein argon flow 60sccm, air pressure 2.5Pa sputter function
Rate is 130~160W.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111690904A (en) * | 2020-06-11 | 2020-09-22 | 国家纳米科学中心 | High-temperature-resistant anti-reflection optical film and preparation method and application thereof |
| CN114054318A (en) * | 2021-11-11 | 2022-02-18 | 陕西科技大学 | Carbon-based micro-nano photo-thermal coating and preparation method thereof |
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