CN109651853A - Stable MoSi in a kind of high temperature air2-SiO2Compound photo-thermal coating and preparation method thereof - Google Patents
Stable MoSi in a kind of high temperature air2-SiO2Compound photo-thermal coating and preparation method thereof Download PDFInfo
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- CN109651853A CN109651853A CN201811472503.3A CN201811472503A CN109651853A CN 109651853 A CN109651853 A CN 109651853A CN 201811472503 A CN201811472503 A CN 201811472503A CN 109651853 A CN109651853 A CN 109651853A
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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Abstract
The invention belongs to technical field of material, and in particular to stable MoSi in a kind of high temperature air2‑SiO2Compound photo-thermal coating and preparation method thereof.The method uses silicon dioxide gel and MoSi2Powder mixing, is spun on carrier after forming black suspension, obtains composite layer after dry, then silicon dioxide gel made from step (2) is spun on composite layer and forms anti-reflection layer, obtains compound photo-thermal coating.Coating proposed by the present invention has high-temperature stability good, and preparation process is easy, low in cost, suitable for scale production to wait many advantages.There are also higher solar absorptances simultaneously.With important practical value.The preparation method of the coating has universality simultaneously, can prepare the functional coating of different packing materials.
Description
Technical field
The invention belongs to technical field of material, and in particular to stable MoSi in a kind of high temperature air2-SiO2It is compound
Object light hot coating and preparation method thereof.
Background technique
Coating for absorbing solar light and heat is a kind of functional coating that can be realized photothermal conversion, can be used for solar heat benefit
With the numerous areas such as heat collection type solar power generation.Solar energy has cleanliness without any pollution, and low in cost, rich reserves etc. are many excellent
Gesture, the alternative energy source as traditional energy is with development potential.The most common solar utilization technique can be roughly divided into photo-thermal and
Two kinds of photovoltaic.Wherein, photothermal technique has many advantages such as energy utilization rate is high, at low cost, equipment is simple.In recent years, low temperature
Photothermal technique it is more universal, such as solar water heater, solar energy housing.And in high temperature Photo-thermal technology application field, there is heat collecting type
Large size optical and thermal-electrotransformation the equipment such as solar power generation is just expanded.Heat collection type solar generating equipment, which has, generates exchange
Electricity is convenient for the advantages such as grid-connected.But because being limited to Carnot efficiency, this kind of equipment must work just at a higher temperature to be had
There is higher energy conversion efficiency.This just proposes the good exclusive requirement of high-temperature stability to its associated components.Photo-thermal, which absorbs, to be applied
Layer is the core component of heat collection type solar generating equipment, and there is also poor high temperature stability, preparations for photo-thermal absorber coatings now
Complex process and many deficiencies such as with high costs.Theoretically, Columnating type solar electricity generation system is 2480K's (~2200 DEG C)
At a temperature of obtain optimal conversion efficiency (85%).But the operating temperature of present photo-thermal absorber coatings is generally 750℃Hereinafter, also
Tomorrow requirement is much not achieved, it is to be developed.
Since the conception of solar energy-thermo-electrically conversion proposes, countries in the world all in the research for carrying out related fields,
And many corresponding achievements come into practical stage.Such as the power station State of Arizona, US Suo Lana, Israel A Shali
Nurse solar power tower etc..In recent years, the similar solar light-heat power-generation facility in China also progresses into the public visual field, such as honest
Bright tower molten salt thermal power station, 10 megawatts of one phase project Dunhuang photo-thermal power station were generated electricity by way of merging two or more grid systems with 2017, every year can be 30,000
The electric power of family family offer absolute cleanliness；The second stage of project has also entered the debugging stage, and total installation of generating capacity is 100 megawatts, it is contemplated that is built
At rear 3.5 hundred million kilowatt hour of annual electricity generating capacity.The photothermal technique of solar energy is not only another Land use systems of heliotechnics, even more
The inherent shortcoming of photovoltaic power generation is compensated for, is suitable for existing energy construction system now, is a kind of effective new energy
Application strategy.
Now, photothermal technique is used in low temperature field (< 200 DEG C) popularity, such as solar water heater, solar energy housing
Deng.And high temperature photothermal technique is there is also high-temperature stability is good enough, the excessively high many defects of production cost.Traditional solar energy
Heat absorption coating usually has complicated structure, multi-layer absorber layer, infrared reflecting layer, barrier layer including different packing ratios and
Anti-reflection layer etc..All these designs require accurate composition proportion and thickness control, therefore the preparation of existing coating is most
Expensive vacuum deposition device is relied on, such as magnetron sputtering and heat are steamed.This has not only resulted in production cost raising, and produces
Inefficiency is unfavorable for large-scale production.Simultaneously as the number of plies is more and structure is complicated, similar sunlight heat coating is in height
Interface element diffusion, and internal malformation can occur under the conditions of temperature.It has been reported that this kind of photo-thermal coating gone out has MoSi2–
Si3N4Compound absorbed layer, Al/NbMoN/NbMoON/SiO2Multi-layer film structure absorbed layer, self assembly Al-AlN absorbed layer etc., he
Highest work temperature be lower than 750 DEG C mostly, and be confined to use under vacuum conditions.
It has also widely been ground using the spectrum selective paint of the more economical technology preparation such as sol-gel method
Study carefully, such as copper galaxite structure light heat absorption coating and Ni-Al2O3Cermet photo-thermal absorber coatings etc..But use this kind of side
The coating for absorbing solar light and heat of method preparation cannot have sufficiently high thermal stability, be difficult to meet large-scale heat collecting type generating equipment
Technical need.
Recently about black cobalt/cobalt oxide coating and Ni-SiO1.5The report of coating, this type coating is because a kind of from termination oxygen
Change process occurs, and stablizes in 750 DEG C of air.But Columnating type solar electricity generation system is in the temperature of 2480K (~2200 DEG C)
Lower acquisition optimal conversion efficiency (85%), therefore there are also very big rooms for promotion for the thermostabilization of photo-thermal coating.In addition, cost is the sun
How the factor that energy absorber coatings large-scale production must be taken into consideration, further increase thermal stability and reduce cost, be still me
The problem that primarily solves.
For example, prior art CN201810545478.0 is related to a kind of MoSi2-SiO2Borosilicate high temperature resistant high emissivity
Coating and the preparation method and application thereof, the raw material composition of coating and the mass percent of each ingredient are as follows: MoSi2-SiO2Composite granule
20~70%, borosilicate glass powder 25~80%, SiB6 0~6%.First with MoO2It is raw material with Si, prepares by a certain percentage
MoSi2-SiO2Composite granule is high-temperature agglomerant as high emissivity phase, borosilicate glass powder, and SiB6 is additive, poly- second
Alkene pyrrolidone PVP is dispersing agent, and ethyl alcohol is solvent, evenly dispersed slurry is made, using spray coating method in aluminium oxide ceramic substrate
On prepare coating with thermostability and high emissivity.
There are following technical problems for the existing prior art: (1) high-temperature stability has to be hoisted.(2) material complicated composition have
Higher production cost, the device is complicated needed for production, is unfavorable for being mass produced.(3) vacuum environment is required, it is unsuitable steady in a long-term
It uses.
Summary of the invention
In view of technical problem of the existing technology, the present invention provides MoSi stable in a kind of high temperature air2-SiO2
Compound photo-thermal coating and preparation method thereof, is achieved through the following technical solutions:
Stable MoSi in a kind of high temperature air2-SiO2The preparation method of compound photo-thermal coating, comprising:
(1) a certain amount of silicon powder and molybdenum powder are subjected to high-energy ball milling reaction, MoSi is made2Powder；
(2) preparation of silicon dioxide gel, by tetraethyl orthosilicate (TEOS) methyltriethoxysilane (MTES), ethyl alcohol,
Deionized water and acetic acid are put into the method preparation of hydrolysis in container, polycondensation；
(3) by silicon dioxide gel and MoSi made from step (2)2Powder mixing, is spun on after forming black suspension
On carrier, composite layer is obtained after dry, then silicon dioxide gel made from step (2) is spun on composite layer and forms anti-reflection
Layer, obtains MoSi2-SiO2Compound photo-thermal coating.
The MoSi that the present invention selects2It is the material with preferable high-temperature stability, in the high temperature environment, MoSi2Surface can be with
Oxygen in air, which combines, generates SiO2Barrier layer ensure that its high-temperature stability, if do not used this to prevent further oxidation
Class material, coating will not have so good thermal stability.The present invention uses sol gel method, and principle is that the presoma of liquid is molten
Glue forms gel after evaporating wherein completely, i.e. will after spin coating is uniform on substrate by silicon dioxide gel in this case
Wherein form a film after liquid drying.The advantage of this scheme be it is easy to operate, do not depend on vacuum equipment, it is low in cost, convenient for extensive
Production.Anti-reflection layer is the absorption for increasing the sunlight of coating by the principle of film interference cancellation, does not use anti-reflection layer such as, is applied
The reflection of layer can increase, and absorb decline.
As a preferred technical solution of the present invention, in the step (1), carried out according to the molar ratio of Mo:Si=1:3
High-energy ball milling reaction, the process carry out 10 hours, and MoSi is made2Powder.
Through a large number of experiments the study found that this method, which can synthesize, forms purer MoSi2Powder ensure that coating
High-temperature stability.In addition, the MoSi of this method synthesis2Powder particle is small, disperse it can in silicon dioxide gel more
It is even.
As a preferred technical solution of the present invention, in the step (2), by quality be respectively 12.93g, 7.65g,
The tetraethyl orthosilicate (TEOS) of 18.25g, 6.83g and 0.50g, methyltriethoxysilane (MTES), ethyl alcohol, deionized water and
Acetic acid is separately added into 100ml round-bottomed flask, at room temperature magnetic agitation for 24 hours to get arrive transparent silicon dioxide gel.
Through a large number of experiments the study found that it is liquid that silicon dioxide gel, which is not powder, using the molten of the method preparation
Gumminess is suitable, and good film-forming property.Not using this proportion will lead to, colloidal sol viscosity is too small or film forming is bad.Such as ethanol consumption mistake
Greatly, colloidal sol is diluter, MoSi2Powder can settle rapidly wherein, be unfavorable for spin coating.Ethanol consumption is excessive, and colloidal sol viscosity is excessive, dries
Gel meeting fragmentation, is not easy to form stable coatings after dry.
As a preferred technical solution of the present invention, in the step (3), silicon dioxide gel and MoSi2Powder is mixed
The proportion of conjunction is that 1ml silicon dioxide gel matches 0.1g MoSi2Powder；In the step (3), then by dioxy made from step (2)
SiClx colloidal sol, which is spun on composite layer, forms anti-reflection layer, and the overall thickness for obtaining coating is~6.62 μm.
Through a large number of experiments the study found that proportion is that 1ml silicon dioxide gel matches 0.1g MoSi2Powder, this proportion can
To obtain to the maximum absorptivity of sunlight.
As a preferred technical solution of the present invention, in the step (3), the carrier is stainless steel (SUS-304)
On, dry half an hour is put into 80 DEG C of baking ovens；The step is repeated twice altogether.Then transparent silicon dioxide colloidal sol is spun on compound
Anti-reflection layer is formed on layer, is put into 80 DEG C of baking ovens dry half an hour, which is equally repeated twice.
Through a large number of experiments the study found that thicker coating can be obtained by being repeated twice, and make filler more complete
Covering substrate surface, number of repetition is excessively unnecessary waste, and not exclusively, absorb reduces the covering of very few substrate.It is warm herein
The lower drying of degree, can make to evaporate in colloidal sol completely, form stable gel coat.
Another object of the present invention is to provide MoSi stable in a kind of high temperature air2-SiO2Compound photo-thermal coating, institute
Coating is stated to be prepared by aforementioned preparation process.
Compared with the prior art, the beneficial effects of the invention include:
Coating proposed by the present invention has high-temperature stability good, and preparation process is easy, low in cost, suitable for scale production
Equal many advantages.There are also higher solar absorptances simultaneously.With important practical value.The preparation method of the coating simultaneously
With universality, the functional coating of different packing materials can be prepared.
Detailed description of the invention
Fig. 1, MoSi of the present invention2-SiO2Composite coating preparation process schematic diagram.
Fig. 2, the MoSi of the embodiment of the present invention 12-SiO2The reflectance spectrum schematic diagram of composite coating annealing front and back, wherein
Reflectance spectrum in 0.2~25 μ m wavelength range is as shown in Figure 2 a.Reflectance spectrum such as Fig. 2 b of the coating after 850 DEG C of annealing
Shown in, wherein " --- " curve indicates the reflectivity curve after annealing 10 hours in air, the expression of " ... " curve is moved back in air
Reflectivity curve of the fire after 100 hours.
Fig. 3, the MoSi of the embodiment of the present invention 12-SiO2Composite coating surface topography and cross-sectional scans electron microscope, Fig. 3 a)
MoSi after annealing 100 hours in 850 DEG C of air2-SiO2Composite coating surface topography, wherein interior figure is macro morphology
Photo, outer figure are microscopic appearance figure.The cross-sectional scans electron microscope of coating after 3b) annealing 100 hours in 850 DEG C of air.
Wherein top gray layer is stainless steel lining bottom, and centre is MoSi2-SiO2Composite coating.
Fig. 4, the reflection-absorption curve synoptic diagram of the embodiment of the present invention 1,2 and 3.
Fig. 5 compares NiSi2-SiO2And MoSi2-SiO2The reflection contrast schematic diagram of two systems.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is described in further detail, but the embodiment invented is not limited to
This.
Embodiment 1
MoSi shown in referring to Fig.12-SiO2Composite coating preparation process schematic diagram,
A certain amount of molybdenum powder and silicon powder are subjected to high-energy ball milling reaction according to the molar ratio of Mo:Si=1:3, which carries out
10 hours, MoSi is made2Powder.
Silicon dioxide gel is using tetraethyl orthosilicate (TEOS) hydrolysis, the method preparation of polycondensation.It is respectively by quality
The tetraethyl orthosilicate (TEOS) of 12.93g, 7.65g, 18.25g, 6.83g and 0.50g, methyltriethoxysilane (MTES), second
Alcohol, deionized water and acetic acid are separately added into 100ml round-bottomed flask.At room temperature magnetic agitation for 24 hours to get arrive transparent titanium dioxide
Silica solution.
By silicon dioxide gel obtained and MoSi2(1ml silicon dioxide gel matches 0.1g MoSi for powder mixing2Powder),
It is spun on stainless steel (SUS-304) after forming black suspension, is put into 80 DEG C of baking ovens dry half an hour.The step repeats altogether
Twice.Then transparent silicon dioxide colloidal sol (volume 1ml) is spun on composite layer and forms anti-reflection layer, be put into 80 DEG C of baking ovens and do
Dry half an hour, the step are equally repeated twice.
Reflectance spectrum before the coating annealing of acquisition in 0.2~25 μ m wavelength range is as shown in Figure 2 a.It anneals at 850 DEG C
Afterwards the reflectance spectrum of the coating as shown in figure 2b, wherein " --- " curve indicate air in anneal 10 hours after reflectivity curve,
" ... " curve indicates the reflectivity curve after annealing 100 hours in air.
Embodiment 2
0.1g MoSi2 powder matches 2ml silicon dioxide gel, is absorbed using the coating that the identical method of embodiment 1 obtains
Lower, reflectance spectrum is shown in Fig. 4 " --- " curve.
Embodiment 3
0.2g MoSi2Powder matches 1ml silicon dioxide gel, is absorbed using the coating that the identical method of embodiment 1 obtains
Lower, reflectance spectrum is shown in Fig. 4 " ... " curve.
Comparative example 1
Using NiSi2-SiO2System, other are the same as 1 method of embodiment.Compare NiSi2-SiO2And MoSi2-SiO2Two systems are real
It tests, finds MoSi2-SiO2System solar spectrum range internal reflection rate is low, and sunshine absorptivity is high, and concrete outcome is shown in Fig. 5.
4 performance detection of embodiment
Under conditions of only considering normal incidence, the calculation formula of absorptivity be can simplify are as follows:
Wherein, λ is wavelength, and S is standard sunlight spoke gross energy (AM 1.5), SλFor the standard sunlight spoke of corresponding wavelength
Penetrate energy.It is the emissivity of coating under corresponding wavelength.According to different wave-length coverages, light can be divided by ultraviolet-visible-near-infrared
Degree meter and Fourier Transform Infrared Spectrometer measurement gained.Equally, under conditions of only considering normal incidence, thermal emissivity be can simplify
For following formula:
Wherein, I is total blackbody radiation intensity, IλIt is the blackbody radiation intensity under corresponding wavelength.
Then we calculate the photothermal conversion of coating for selective absorption of sunlight spectrum according to absorptivity α and thermal emissivity ε
Efficiency is come since the not single sunlight of existing frequently-used sunlight collecting apparatus is incident often through optical focus
Biggish sunlight amount of incident is obtained, so the photothermal conversion efficiency of coating is also related with the focusing multiple of sunlight.Photo-thermal turns
Change efficiency etaPhoto-thermalDefer to following equation:
Wherein, σ is this special fence-Boltzmann constant；TEnvironmentAnd THigh temperatureIt is the temperature of environment and coating surface respectively；ηIt focusesIt is
Optical focusing efficiency, if not considering the optical loss in focusing, it is believed that ηIt focusesEqual to 1.C is to focus multiple, meaning
Justice is to focus the ratio between front and back sunlight institute swept area.It can thus be concluded that photothermal conversion efficiency, but as it was noted above, photothermal conversion
Efficiency is only measured by sunlight to the index of heat-convertibility energy superiority and inferiority, if it is considered that being turned heat-energy secondary using Carnot Engine
Change, the whole efficiency of system defers to following formula:
That is product of the gross efficiency equal to photothermal conversion efficiency and Carnot efficiency.
The results are shown in Table 1 for embodiment 1,2 and the calculating of 3 gained coating absorptivities:
| Embodiment | Absorptivity (%) |
| 1 | 95.0 |
| 2 | 88.1 |
| 3 | 93.7 |
The specific performance parameter calculated result of 1 gained coating of embodiment is as shown in table 2:
Table 2, the absorptivity under coating difference annealing case, thermal emissivity, photothermal conversion efficiency and system total efficiency
After coating is annealed 10 hours in 850 DEG C of air, MoSi2-SiO2Composite coating surface topography and cross-sectional scans electricity
Mirror figure, Fig. 3 a) anneal 100 hours in 850 DEG C of air after MoSi2-SiO2Composite coating surface topography, wherein interior figure
For macro morphology photo, outer figure is microscopic appearance figure.It sweeps in the section of coating after 3b) annealing 100 hours in 850 DEG C of air
Retouch electron microscope.Wherein top gray layer is stainless steel lining bottom, and centre is MoSi2-SiO2Composite coating.Illustrate preparation of the present invention
Obtained coating has high-temperature stability good, the advantages such as higher solar absorptance.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (8)
1. stable MoSi in a kind of high temperature air2-SiO2The preparation method of compound photo-thermal coating, comprising:
(1) a certain amount of silicon powder and molybdenum powder are subjected to high-energy ball milling reaction, MoSi is made2Powder；
(2) preparation of silicon dioxide gel, by tetraethyl orthosilicate (TEOS) methyltriethoxysilane (MTES), ethyl alcohol, go from
Sub- water and acetic acid are put into the method preparation of hydrolysis in container, polycondensation；
(3) by silicon dioxide gel and MoSi made from step (2)2Powder mixing, is spun on carrier after forming black suspension
On, composite layer is obtained after dry, then silicon dioxide gel made from step (2) is spun on composite layer and forms anti-reflection layer, obtained
To MoSi2-SiO2Compound photo-thermal coating.
2. preparation method according to claim 1, which is characterized in that in the step (1), according to rubbing for Mo:Si=1:3
You carry out 10 hours than carrying out high-energy ball milling reaction, the process, and MoSi is made2Powder.
3. preparation method according to claim 1, which is characterized in that in the step (2), be respectively by quality
The tetraethyl orthosilicate (TEOS) of 12.93g, 7.65g, 18.25g, 6.83g and 0.50g, methyltriethoxysilane (MTES), second
Alcohol, deionized water and acetic acid are separately added into 100ml round-bottomed flask, at room temperature magnetic agitation for 24 hours to get arrive transparent titanium dioxide
Silica solution.
4. preparation method according to claim 1, which is characterized in that in the step (3), silicon dioxide gel and MoSi2
The proportion of powder is that 1ml silicon dioxide gel matches 0.1g MoSi2Powder, i.e. coating precursor concentration are 0.1g/ml.
5. preparation method according to claim 1, which is characterized in that in the step (3), then step (2) is obtained
Silicon dioxide gel, which is spun on composite layer, forms anti-reflection layer, and the overall thickness for obtaining coating is~6.62 μm.
6. preparation method according to claim 1, which is characterized in that in the step (3), the carrier is stainless steel
(SUS-304) on, dry half an hour is put into 80 DEG C of baking ovens；The step is repeated twice altogether, obtains composite layer after dry.
7. preparation method according to claim 1, which is characterized in that in the step (3), then by transparent silicon dioxide
Colloidal sol, which is spun on composite layer, forms anti-reflection layer, is put into 80 DEG C of baking ovens dry half an hour, which is equally repeated twice, obtains
Compound photo-thermal coating.
8. stable MoSi in a kind of high temperature air2-SiO2Compound photo-thermal coating, which is characterized in that the coating passes through aforementioned
The described in any item preparation methods of claim 1-7 are prepared.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114958041A (en) * | 2021-12-30 | 2022-08-30 | 江南大学 | Preparation method and application of high-temperature solar energy absorption coating with antireflection function |
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| EP2243860A3 (en) * | 2009-04-24 | 2011-11-23 | ZYRUS Beteiligungsgesellschaft mbH & Co. Patente I KG | Method for manufacturing a solar absorber coating |
| CN103302917A (en) * | 2013-05-27 | 2013-09-18 | 欧阳俊 | Dual-absorption-layer TiON weather-resistant photothermal coating and preparation method thereof |
| CN107541106A (en) * | 2017-09-01 | 2018-01-05 | 西藏自治区能源研究示范中心 | A kind of solar energy hot coating and preparation method thereof and the Solar wall based on coating |
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| EP2243860A3 (en) * | 2009-04-24 | 2011-11-23 | ZYRUS Beteiligungsgesellschaft mbH & Co. Patente I KG | Method for manufacturing a solar absorber coating |
| CN101737982A (en) * | 2009-11-25 | 2010-06-16 | 北京航空航天大学 | Solar selectively absorbing coating and preparation method thereof |
| CN103302917A (en) * | 2013-05-27 | 2013-09-18 | 欧阳俊 | Dual-absorption-layer TiON weather-resistant photothermal coating and preparation method thereof |
| CN107541106A (en) * | 2017-09-01 | 2018-01-05 | 西藏自治区能源研究示范中心 | A kind of solar energy hot coating and preparation method thereof and the Solar wall based on coating |
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| CN114958041A (en) * | 2021-12-30 | 2022-08-30 | 江南大学 | Preparation method and application of high-temperature solar energy absorption coating with antireflection function |
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