CN113563769A - Infrared radiation refrigeration optical coating and optical film - Google Patents
Infrared radiation refrigeration optical coating and optical film Download PDFInfo
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- CN113563769A CN113563769A CN202111132388.7A CN202111132388A CN113563769A CN 113563769 A CN113563769 A CN 113563769A CN 202111132388 A CN202111132388 A CN 202111132388A CN 113563769 A CN113563769 A CN 113563769A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C09D127/16—Homopolymers or copolymers of vinylidene fluoride
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/32—Radiation-absorbing paints
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
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Abstract
The invention discloses an infrared radiation refrigeration optical coating and an optical film. Wherein the optical coating comprises a resin and an infrared radiation refrigeration composition dispersed in the resin; the infrared radiation refrigeration composition comprises rare earth silicate particles formed by reacting components including a rare earth source, an Ra ion metal source and an Si source. Compared with the prior art, the invention can realize higher radiation refrigeration performance and can be industrialized more easily.
Description
Technical Field
The invention relates to the technical field of radiation refrigeration, in particular to an infrared radiation refrigeration optical coating and an optical film.
Background
In recent years, a novel cooling method has attracted interest and the technology is expected to be applied to the electroless cooling of buildings. The principle of the refrigeration mode is as follows: according to the Planck black body radiation law, any object with the temperature higher than absolute zero radiates heat energy to the outside in the form of electromagnetic waves, and the temperature of the object is reduced due to the radiation of the energy outwards, namely radiation cooling. Stefan-boltzmann states that the full radiated power of a black body is proportional to its absolute temperature to the power of 4, and it is calculated that a 1 square meter absolute black body radiates 460W of radiant energy in the full band at 300K. A black body will reduce its temperature at a significant rate if it only radiates without absorbing energy from the environment. In theory, radiation cooling can be used to develop refrigeration technology that does not require electrical energy nor rely on external energy sources, which is radiation refrigeration technology. The material used to achieve the radiation refrigeration effect is the radiation refrigeration material.
According to the research on the atmospheric transmittance, the absorption of various gas molecules in the wave band of 8-13 μm is relatively weak, and the infrared rays in the wave band can directly reach the outer space with lower temperature without being absorbed by the atmosphere, and the region is called as an atmospheric window.
In recent years, researchers are constantly researching and developing infrared radiation refrigeration materials, and most of the infrared radiation refrigeration materials adopt silicon dioxide
On the basis of this, as in 2014, the research group of professor Shanhui Fan, university of Stanford, by depositing seven layers alternately
And hafnium oxide form a layered structure. The layered structure can release energy to the outside by radiating infrared rays with the wavelength of 8-13 mu m, and can reflect up to 97% of sunlight, thereby avoiding the temperature rise caused by the sunlight as much as possible. Experiments have shown that such a layered structure is still able to keep the temperature of the object covered under it at 5 degrees celsius below the temperature of the surrounding atmosphere, even during the day and in direct sunlight. The Xiaoobo Yin of Colorado university is incorporated into polymethylpentene (TPX)
The microbead is used to draw the finished product into a sheet with thickness of about 50 μm, then the back surface is coated with silver, 96% of sunlight can be reflected back by the composite material, and at the same time, the material radiates heat energy to space by infrared, especially 8-13 μm atmosphere infrared window.
However, the performance of the infrared radiation refrigeration cannot meet the current requirements in the two modes. Therefore, a material with higher radiation refrigeration performance is urgently needed at present.
Disclosure of Invention
The invention provides an infrared radiation refrigeration optical coating and an optical film, which have higher radiation refrigeration performance compared with the prior art.
The invention provides the following scheme:
in one aspect, an infrared radiation refrigerating optical coating is disclosed, the optical coating comprising a resin and an infrared radiation refrigerating composition dispersed in the resin; the infrared radiation refrigeration composition comprises rare earth silicate particles formed by reacting components including a rare earth source, an Ra ion metal source and an Si source.
In a particular embodiment, the anion of the rare earth source is selected from at least one of rare earth nitrate, rare earth chloride; the source of Ra ion metal is selected from
、
、
、
At least one of (a); the Si source is selected from the group consisting of nano
Wherein x is more than 0 and less than or equal to 2.
In a particular embodiment, the cation of the rare earth source is selected from at least one of La, Sm, Eu, Gd, Tb, Dy, Er, Tm, Yb, Y, Sc.
In a specific embodiment, the rare earth silicate particles comprise, by mass fraction, 50-77% of the rare earth source, 20-45% of the Ra ion metal source, and 0.3-10% of the Si source.
In a specific embodiment, the Si source comprises
Particles.
In a particular embodiment, the rare earth silicate particles have a particle size in the range of 50-200nm or 1-10 μm.
In a particular embodiment, the resin is selected from at least one of polyvinyl fluoride PVF, polyvinylidene fluoride PVDF, polychlorotrifluoroethylene PCTFE, polytetrafluoroethylene PTFEDE, polytetrafluoroethylene PTFE, polyvinylidene fluoride hexafluoropropylene (P (VDF-HFP)).
In a specific embodiment, the rare earth silicate particles comprise 5-20% by volume of the optical coating.
The application also discloses an infrared radiation refrigeration optical film, which comprises an infrared radiation refrigeration functional layer formed by the infrared radiation refrigeration optical coating.
In a particular embodiment, the optical film further comprises a metallic reflective layer.
In a particular embodiment, the thickness of the metallic reflective layer is in the range of 0.15-1 μm or 1-150 nm.
In a specific embodiment, the thickness of the infrared radiation refrigeration functional layer is 0.1-5 μm.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
the infrared radiation refrigeration optical coating provided by the invention contains rare earth silicate particles formed by reacting rare earth source, Ra ion metal source and Si source. The rare earth cations are compounded by utilizing the network structure of silicate glass, have octahedral coordination and have strong accumulation capacity on free oxygen. The silicate anion group has various polymerization forms, rare earth cations are doped in the silicate anion group, the structure of the anion group and the cation field where the anion group is located are adjusted, the silica network structure of the silicate is adjusted to have higher symmetry, the rare earth cations have better absorption performance at a near infrared wave band, and the combination of the rare earth cations and the near infrared wave band can realize higher infrared radiation refrigeration performance. Further, in the metal source of Ra ion
The ions have a high valueThe ion activity and the capability of competing for oxygen are stronger, and the silicon-oxygen network structure is damaged strongly. The rare earth ions can more easily occupy the lattice position with higher symmetry in the silicate, and the infrared radiation refrigeration performance of the rare earth silicate particles is further improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments that can be derived by one of ordinary skill in the art from the embodiments given herein are intended to be within the scope of the present invention.
The following describes a specific implementation scheme provided by the embodiment of the present invention in detail.
The invention provides an infrared radiation refrigeration optical coating, which comprises a resin and an infrared radiation refrigeration composition dispersed in the resin; the infrared radiation refrigeration composition comprises rare earth silicate particles formed by reacting components including a rare earth source, an Ra ion metal source and an Si source.
The rare earth ions have better absorption performance at the near infrared position, the rare earth ions are compounded by utilizing the glass silica network structure of the silicate, the rare earth ions have octahedral coordination and have strong accumulation capacity on free oxygen, silicate anion groups have various polymerization forms, the rare earth ions are doped in the silicate anion groups, the anion group structure and the cation field where the anion groups are located are adjusted, the silica network structure of the rare earth silicate is adjusted to have higher symmetry, and better infrared radiation performance can be realized.
And in the Ra ion metal source
The ions have higher ion activity and stronger oxygen competition capability, and have strong destructive effect on the silicon-oxygen network structure. Adding Ra ion metal source during preparing RE silicate particle,
ion pair silica netThe strong destruction and regulation of the complex structure makes the rare earth cation occupy the lattice position with higher symmetry in the silicate more easily, so as to improve the infrared radiation refrigerating capacity of the rare earth silicate particles.
In a particular embodiment of the present application, the anion of the rare earth source is selected from one or both of rare earth nitrate, rare earth chloride. The rare earth source is easy to decompose under the high-temperature reaction condition, and the rare earth compound formed after decomposition has higher activation energy and high reaction activity, thereby being beneficial to the diffusion of rare earth ions and promoting the reaction, and leading the damage of the silica network structure to be more thorough.
The cation of the rare earth source may be at least one selected from La, Sm, Eu, Gd, Tb, Dy, Er, Tm, Yb, Y and Sc.
The Ra ion metal source can be selected from
、
、
、
At least one of (1).
In a preferred embodiment of the present application, the Si source is selected from the group consisting of nano-sized Si
Wherein x is more than 0 and less than or equal to 2. Preferably of nanometer
Has smaller grain diameter, better size distribution, larger specific surface area and specific surface energy and relatively higher reaction activity.
Preferably, the rare earth silicate particles comprise 50-77% of the rare earth source, 20-45% of the Ra ion metal source and 0.3-10% of the Si source in mass fraction. The ratio ofThe range of more rare earth ions entering into a silicon-oxygen network structure is beneficial to the mass generation of non-bridging oxygen bonds Si-O if
When the ions are excessive, the rare earth ions are converted into network forming ions from the network exo-ions, so that the fractured silicon-oxygen network structure starts to polymerize again.
In one embodiment, the rare earth silicate particles have a particle size in the range of 50-200 nm. In this particle size range, the visible light transmittance can be improved.
In another embodiment, the rare earth silicate particles have a particle size in the range of 1-10 μm. The particle microspheres have different resonance forms excited by the interaction with incident wavelength, and when the rare earth silicate particles are in the particle size range, the rare earth silicate particles can be excited by 8-13 mu m magnetic waves to form high-order resonance forms, so that the rare earth silicate particles have high emissivity in the wavelength range of 8-13 mu m. The particles having a particle diameter within the above range have excellent forward scattering ability, so that the heat radiating property thereof can be improved.
In another embodiment of the present application, the Si source in the optical coating is nano
Particles.
The resin in the coating can be at least one selected from polyvinyl fluoride PVF, polyvinylidene fluoride PVDF, polychlorotrifluoroethylene PCTFE, polytetrafluoroethylene PTFEDE, polytetrafluoroethylene PTFE and polyvinylidene fluoride-hexafluoropropylene (P (VDF-HFP)). The materials have good weather resistance and good anti-fouling effect.
The application also discloses an infrared radiation refrigeration optical film in another aspect, and the optical film comprises an infrared radiation refrigeration functional layer formed by the infrared radiation refrigeration optical coating mentioned in the embodiment.
In order to realize the reflection of light under sunlight and further improve the refrigeration performance, the optical film also comprises a metal reflecting layer. The metal in the metal reflective layer is selected from: aluminum, silver alloys.
In a specific embodiment, the thickness of the metal reflective layer is set to be in the range of 0.15 to 1 μm in order to improve the reflectivity. When the metal reflecting layer is too thin, the reflectivity of the visible light wave band is low because most visible light directly penetrates through the composite film. When the metal reflecting layer is larger than 1 μm, the reflectivity of the metal reflecting layer achieves the ideal effect, and when the thickness exceeds a certain value, the sunlight reflectivity is kept unchanged.
If there is a high demand for visible light transmittance of the entire film in some cases, the thickness of the metal reflective layer may be set to be in the range of 1 to 150 nm.
The thickness range of the infrared radiation refrigeration functional layer is selected from 0.1-5 mu m, and when the thickness range is within the range, multiple scattering and absorption can be generated when light waves pass through the infrared radiation refrigeration functional layer, so that the refrigeration effect is better.
The rare earth silicate particles in the infrared radiation refrigeration functional layer account for 5-20% of the volume fraction range of the infrared functional layer, the infrared emissivity is gradually increased along with the increase of the filling volume fraction, but the transmittance of a film material is influenced when the filling volume fraction is increased to a certain degree, and meanwhile, the infrared radiation refrigeration functional layer is not beneficial to industrial processing.
The present application also provides a method for preparing an infrared radiation refrigeration composition in an optical coating, comprising:
taking alcohol as a ball milling medium, and performing ball milling on a rare earth source, an Ra ion metal source and an Si source at a rotating speed of 100-200 r/min. And (5) after ball milling for a preset time, putting into an oven for drying. Finally placing the mixture in a high-temperature furnace for reaction to obtain the infrared radiation refrigeration composition.
In a preferred embodiment, the temperature of the high temperature furnace is set to 700-900 ℃ and the reaction time is 12-16 hours. Exceeding this temperature range leads to the onset of melting of the rare earth silicate and the tendency of the silicon tetrahedron to re-associate into aggregates. The appropriate time is favorable for further diffusion among reactants in the solid-phase reaction, so that the reaction is more thorough, and the rare earth ions enter a silicon-oxygen network structure, so that silicon-oxygen tetrahedrons in the product are regularly arranged and bond angles are close.
The following effects are illustrated by experimental data of examples and comparative examples:
comparative example 1
Blank test thermocouple was placed directly in the incubator and is designated as R11.
Comparative example 2
Weighing 80 g
Is a rare earth source, 5 g
Is a source of Si. Taking ethanol as a ball milling medium, performing ball milling for 10 hours at the rotating speed of 90 r/min, putting the ball milled mixture into a 60 ℃ oven for drying, and finally reacting for 15 hours at the temperature of 600 ℃ in a high-temperature furnace to obtain the rare earth silicate. The particle size of the prepared rare earth silicate is 300 nm. Preparing the infrared radiation refrigeration coating by the prepared rare earth silicate and polyvinylidene fluoride, wherein the rare earth silicate accounts for 10% of the volume fraction of the infrared radiation refrigeration coating, and then coating the coating on a silver alloy reflecting layer far away from a base material layer prepared from the polyvinylidene fluoride. The thickness of the substrate layer is 50 μm, the thickness of the silver alloy reflective layer is 0.5 μm, and the thickness of the functional layer formed by the coating is 5 μm. The resulting film was designated R12.
Example 1
The difference from comparative example 2 is that 15 g is added
Is a source of Ra ion metal to prepare the rare earth silicate. The prepared rare earth silicate and polyvinylidene fluoride are prepared into infrared radiation refrigeration coating, and the infrared radiation refrigeration coating is coated on the silver alloy reflecting layer far away from the base material layer. The resulting film was designated R21.
Example 2
The difference from the embodiment 1 is that,
the mass of (a) is 45 g,
the weight of the mixture is 50 g,
is 5 g. The prepared rare earth silicate and polyvinylidene fluoride are prepared into infrared radiation refrigeration coating, and the infrared radiation refrigeration coating is coated on the silver alloy reflecting layer far away from the base material layer. The resulting film was designated R22.
Example 3
The difference from the embodiment 1 is that,
the mass of (a) is 75 g,
the mass of (a) is 20 g,
the mass of the rare earth silicate is 5 g, and the rare earth silicate is prepared. The prepared rare earth silicate and polyvinylidene fluoride are prepared into infrared radiation refrigeration coating, and the infrared radiation refrigeration coating is coated on the silver alloy reflecting layer far away from the base material layer. The resulting film was designated R23.
Example 4
The difference from the embodiment 1 is that,
the mass of (a) is 50 g,
the mass of (a) is 45 g,
the mass of the rare earth silicate is 5 g, and the rare earth silicate is prepared. The prepared rare earth silicate and polyvinylidene fluoride are prepared into infrared radiation refrigeration coating, and the infrared radiation refrigeration coating is coated on the silver alloy reflecting layer far away from the base material layer. The resulting film was designated R24.
Example 5
The difference from the embodiment 1 is that,
the mass of (a) is 65 g,
the mass of (a) is 30 g,
the mass of (2) is 5 g, and the prepared rare earth silicate. The prepared rare earth silicate and polyvinylidene fluoride are prepared into infrared radiation refrigeration coating, and the infrared radiation refrigeration coating is coated on the silver alloy reflecting layer far away from the base material layer. The resulting film was designated R25.
Example 6
The difference from example 5 is that the reaction was carried out at 700 ℃ in a high temperature furnace. The resulting film was designated R26.
Example 7
The difference from example 5 is that the reaction was carried out at 900 ℃ in a high temperature furnace. The resulting film was designated R27.
Example 8
The difference from example 7 is that the reaction was carried out in a high temperature furnace for 13 hours. The resulting film was designated R28.
Example 9
The difference from example 8 is that the rotation speed is 100 r/min. The resulting film was designated R29.
Example 10
The difference from example 8 is that the rotation speed is 200 r/min. The resulting film was designated R210.
Example 11
The difference from example 10 is that the particle size of the obtained rare earth silicate is 4 μm. The resulting film was designated as R211.
Example 12
The difference from example 11 is that the particle size of the obtained rare earth silicate is 100 nm. The resulting film was designated R212.
And (3) respectively putting the prepared films into a heat preservation box, covering the heat preservation box with a transparent cover plate, arranging a thermocouple temperature measuring point at the lower part of the film material, and testing for 3 hours. The R11 blank test was performed by placing a thermocouple directly into the incubator for 3 hours. And recording the temperature value of the temperature measuring point of the thermocouple after 3 hours. The results are given in table 1 below:
table 1 optical film temperature testing
As can be seen from the table above, the addition of the Ra ion metal source improves the infrared radiation refrigeration effect. And the Ra ion metal source has better effect at 20-45%. And when the particle size of the rare earth silicate is in the micron level, the infrared radiation refrigeration effect is better. Meanwhile, the temperature, the grinding speed and the reaction time of the high-temperature furnace have certain influence on the infrared radiation refrigeration effect.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. An infrared radiation refrigerating optical coating, characterized in that the optical coating comprises a resin and an infrared radiation refrigerating composition dispersed in the resin; the infrared radiation refrigeration composition comprises rare earth silicate particles formed by reacting components including a rare earth source, an Ra ion metal source and an Si source.
2. An infrared radiation refrigeration optical coating as recited in claim 1, wherein the anion of said rare earth source is selected from at least one of rare earth nitrate, rare earth chloride;
and/or the presence of a gas in the gas,
the source of Ra ion metal is selected from
、
、
、
At least one of (a);
and/or the presence of a gas in the gas,
the Si source is selected from the group consisting of nano
Wherein x is more than 0 and less than or equal to 2;
and/or the presence of a gas in the gas,
the resin is at least one selected from polyvinyl fluoride, polyvinylidene fluoride, polychlorotrifluoroethylene, polytetrafluoroethylene and polyvinylidene fluoride-hexafluoropropylene.
3. An infrared radiation refrigerating optical coating as recited in claim 1, wherein the cation of said rare earth source is selected from at least one of La, Sm, Eu, Gd, Tb, Dy, Er, Tm, Yb, Y, Sc.
4. An infrared radiation refrigeration optical coating as recited in claim 1, wherein said rare earth silicate particles comprise, in mass fraction, 50-77% of said rare earth source, 20-45% of said Ra ion metal source, and 0.3-10% of said Si source.
5. The infrared radiation refrigeration optical coating of claim 1 wherein the Si source is
Particles; the particle size range of the rare earth silicate particles is 50-200nm or 1-10 mu m.
6. An infrared radiation refrigerating optical coating as claimed in claim 5 wherein said rare earth silicate particles occupy 5-20% by volume of said optical coating.
7. An infrared radiation refrigerating optical film, characterized in that the optical film comprises an infrared radiation refrigerating functional layer formed by the infrared radiation refrigerating optical coating material according to any one of claims 1 to 6.
8. The infrared radiation refrigerating optical film of claim 7 wherein the optical film further comprises a metal reflective layer.
9. An infrared radiation refrigerating optical film as recited in claim 8, wherein the thickness of the metal reflective layer is 0.15-1 μm or 1-150 nm.
10. The infrared radiation refrigeration optical film of claim 8 wherein the infrared radiation refrigeration functional layer has a thickness of 0.1 to 5 μm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115353779A (en) * | 2022-08-18 | 2022-11-18 | 江苏博云塑业股份有限公司 | Radiation refrigeration coating, preparation method thereof and radiation refrigeration film |
| CN115537056A (en) * | 2022-08-18 | 2022-12-30 | 江苏博云塑业股份有限公司 | Rare earth silicate, radiation refrigeration composition, radiation refrigeration coating and preparation method |
| CN117567894A (en) * | 2024-01-11 | 2024-02-20 | 中稀易涂科技发展有限公司 | High-emission rare earth-based radiation refrigeration coating |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115353779A (en) * | 2022-08-18 | 2022-11-18 | 江苏博云塑业股份有限公司 | Radiation refrigeration coating, preparation method thereof and radiation refrigeration film |
| CN115537056A (en) * | 2022-08-18 | 2022-12-30 | 江苏博云塑业股份有限公司 | Rare earth silicate, radiation refrigeration composition, radiation refrigeration coating and preparation method |
| CN117567894A (en) * | 2024-01-11 | 2024-02-20 | 中稀易涂科技发展有限公司 | High-emission rare earth-based radiation refrigeration coating |
| CN117567894B (en) * | 2024-01-11 | 2024-04-05 | 中稀易涂科技发展有限公司 | High-emission rare earth-based radiation refrigeration coating |
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