CN111718584A - Radiation cooling film, preparation method and application thereof - Google Patents
Radiation cooling film, preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a radiation cooling film, which is formed by mixing ceramic particles, organic solution and curing agent to form ceramic particles, mixing the ceramic particles with organic curing precursor solution and curing, wherein a micro-nano photon structure array is formed on the surface of the film and comprises a plurality of micro-nano photon structural elements in an array. Also discloses a preparation method and application of the radiation cooling film. The film has 95% of reflectivity in a sunlight wave band, 96% of radiance in an atmospheric window wave band, 10 ℃ lower than the ambient environment at most under the illumination condition, and has good flexibility, strength and excellent hydrophobicity. The radiation cooling film is prepared by adopting a multi-etching double-spin coating vacuum thermocuring process with low cost and large area. The application of the radiation cooling film in the aspects of human body wearable cooling, temperature-reducing sun-rain umbrella and device heat dissipation realizes the cooling method by removing heat from the surface and the inside of the main body in a heat radiation mode.
Description
Technical Field
The invention belongs to the technical field of functional composite materials, and particularly relates to a radiation cooling film, and a preparation method and application thereof.
Background
With the improvement of living standard and the development of urbanization, great demands are generated on cooling technology and cooling equipment. Commonly used cooling devices rely on vapor compression refrigeration systems to achieve cooling effects, such as refrigerators and air conditioners. However, these cooling devices not only consume a large amount of energy, but also the use of refrigerants (such as hydrofluorocarbons) causes global warming effects, which further poses serious environmental hazards. As refrigeration technology is mostly by consuming non-renewable fossil resources, more heat is actually built up, making the earth more hot. The greenhouse effect and the urban heat island effect are thus exacerbated by the large amount of heat generated by the refrigeration equipment during operation. Studies have shown that cooling systems consume 15% of the electricity worldwide, causing 10% of greenhouse gas emissions. Every 1 deg.C reduction, 3-5% of electric power can be saved. The energy demand for refrigeration and air conditioning has increased dramatically worldwide in the 21 st century due to global warming, population growth, industrial development, and the like. By 2050, the human demand for cooling has grown ten times, and thus, the growing concern over energy situation and environmental issues has created a need for counter-measures to improve the efficiency of existing cooling systems and to seek new alternative cooling technologies as soon as possible. It would therefore be a significant challenge in the new century to develop new refrigeration systems.
Radiation refrigeration utilizes a transparent atmospheric window to radiate heat to the outer space, and under ideal climatic conditions, radiation cooling can realize energy conservation of nearly 70 percent. Compared with the traditional cooling device, the radiation cooling device does not need any external energy supply device, does not need power consumption and energy consumption, and does not have CO2The emission of the isothermal gases and other noxious substances produces a net cooling effect. The energy is saved, no pollution is caused, the trend of sustainable development is met, and the passive refrigeration mode is green and environment-friendly. The radiation cooling effect is realized mainly based on the following two aspects: first, the average tropospheric temperature is typically around 250K, the average temperature in most parts of the year is much lower than this temperature, and the thermal black body of the cosmic microwave background outside the atmosphere radiates around 2.7K, so both can act as a "cooling reservoir" for the radiant cooling devices on earth to dissipate heat. Secondly, the earth's atmosphere has a high transmittance in the mid-infrared band of wavelengths ranging from 8 to 13 μm, and is called a transparent atmospheric window. The transparent atmospheric window allows the object to exchange heat with the "cold reservoir" by thermal radiation in this band. There are a number of literature reports surrounding radiation cooled devices, such as chinese patent CN107923718A entitled "system and method for radiant cooling and heating", the technical features of which are to provide a system and method for radiant cooling and heating, for example, a system for radiant cooling may comprise a top layer comprising one or more polymers, wherein the top layer has a high emissivity in at least a portion of the thermal spectrum and an electromagnetic extinction coefficient of approximately zero, an absorptivity of approximately zero, and a high transmittance in at least a portion of the solar spectrum, and further comprises a reflective layer comprising one or more metals, which have a high emissivity in at least a portion of the solar spectrum, a high absorptivity of approximately zero, and a high transmissivityWherein the reflective layer has a high reflectivity in at least a portion of the solar spectrum. However, the technology is complex to prepare and high in cost, and the radiation cooling effect needs to be further improved. As further shown in chinese patent CN 109070695a entitled "radiation cooling structure and system", the technical feature of this patent is to provide a polymer-based selective radiation cooling structure comprising a selective emission layer of a polymer or polymer-based composite material. Typical selective radiation cooling structures take the form of sheets, films or coatings. However, the technology is difficult to obtain high visible-near infrared reflectivity and high atmospheric window radiance at the same time, and meanwhile, the single-layer material of the method is difficult to simultaneously meet the common improvement of the visible-near infrared reflectivity and the infrared emissivity, so that a ceramic material layer is required to improve the medium infrared radiance, a metal layer is required to increase the reflectivity of a visible near infrared band, and the preparation requirement is complex.
Disclosure of Invention
The invention provides a radiation cooling film, which reduces the absorption of sunlight by utilizing the high reflectivity of the film, and simultaneously removes the redundant heat of a main body by carrying out heat radiation to the outside so as to realize the effect of passive cooling;
the invention also provides a preparation method of the radiation cooling film, which is characterized in that the organic-inorganic composite radiation cooling film with the micro-nano photon structure is prepared by utilizing multi-etching micro-nano processing, spin coating and curing, so that the surface micro-nano photon structure is constructed, the composite radiation cooling film with low cost and large area can be prepared, and the universality is strong.
The technical scheme of the invention is as follows:
the utility model provides a radiation cooling film, the raw materials of film include ceramic granule, organic solution, curing agent, ceramic granule, organic solution, curing agent mix and form ceramic granule and mix organic solidification precursor liquid, the film does form after the solidification of ceramic granule mixes organic solidification precursor liquid, the surface of film is formed with micro-nano photon structure array, and micro-nano photon structure array includes that a plurality of is the micro-nano photon's of array structural element, constitutes even array structure on the film surface.
Preferably, the shape of a structural element of the micro-nano photonic structure array is one or more of a pyramid structure, a prismatic structure, a conical structure, an inverted pyramid structure and an inverted cone structure, the characteristic width of the structural element is 0.5-20 μm, and the characteristic height of the structural element is 0.5-20 μm; the film has a thickness of 100 to 2000 μm.
Preferably, the ceramic particles are selected from one or more of alumina, zinc oxide, zirconia, magnesia, boron nitride, yttria, titania.
Preferably, the average particle size of the ceramic particles is 0.2-10 microns, the morphology of the ceramic particles is one or more of angular shape, spheroidal shape and spherical shape, and the mass fraction of the ceramic particles in the ceramic particle mixed organic curing precursor liquid is 5-80%.
Preferably, the organic solution is an organic polymer, and the organic polymer is selected from one of polydimethylsiloxane, polytetrafluoroethylene and polyvinyl chloride; the curing agent enables ceramic particles, organic solution and curing agent to be mixed to form ceramic particles mixed with organic curing precursor solution to be cured under the condition of heating or standing for a long time, and the curing agent comprises resin.
Preferably, the mass ratio of the curing agent to the ceramic particle mixed organic curing precursor liquid is 1: 5 to 1: 20.
the invention also provides a preparation method of the radiation cooling film, and the preparation method of the radiation cooling film comprises the following steps:
step S1, mixing the ceramic particles, the organic solution and the curing agent to prepare a ceramic particle mixed organic curing precursor solution;
step S2: placing the multi-etched micro-nano processed template on a spin coater turntable and communicating a vacuum pump to enable the template to be adsorbed by the spin coater turntable;
step S3: coating the ceramic particle mixed organic curing precursor liquid obtained in the step S1 on a template, and uniformly spin-coating the ceramic particle mixed organic curing precursor liquid on the template through a spin coater;
step S4: placing the template uniformly coated with the ceramic particle mixed organic curing precursor liquid on a heating plate for heating and curing, and then cooling to room temperature;
step S5: and stripping the cured organic-inorganic composite radiation cooling film with the micro-nano photon structure from the template subjected to the micro-nano processing by etching to obtain the radiation cooling film.
Preferably, the method further comprises the following steps:
step S6: repeating the steps S1 to S5, preparing a plurality of organic-inorganic composite radiation cooling films with micro-nano photon structures, and tightly tiling the films on a flat plate by cutting;
step S7: coating the ceramic particle mixed organic curing precursor solution on the tiled film, and performing secondary spin coating;
step S8: placing the plate coated with the ceramic particle mixed organic curing precursor solution on a heating plate for heating and curing, and then cooling to room temperature;
step S9: and stripping the organic-inorganic composite radiation cooling film with the large-area micro-nano photon structure formed after curing from the template to obtain the large-area radiation cooling film.
Preferably, the step S1 of forming the ceramic particle mixed organic solidification precursor liquid includes the following steps:
step S11: putting the ceramic particles into an organic solution, and mixing the ceramic particles and the organic solution uniformly by fully stirring; the ceramic particles are one or more selected from alumina, zinc oxide, zirconia, magnesia, boron nitride, yttria and titanium oxide white powder, the organic solution is an organic polymer, and the organic polymer is one selected from polydimethylsiloxane, polytetrafluoroethylene and polyvinyl chloride transparent solution;
step S12: adding a curing agent into the solution obtained in the step S11, and stirring to uniformly mix the curing agent and the solution;
step S13: putting the solution obtained in the step S12 into a vacuum drying oven, vacuumizing to discharge air in the solution, so that no bubbles are emitted in the solution finally;
step S14: and opening a vent valve of the vacuum box, and slowly returning the air pressure in the vacuum box to the initial state which is the same as the external air pressure after 5 to 10 minutes, thus obtaining the ceramic particle mixed organic curing precursor liquid.
Preferably, the step S13 is performed in the vacuum drying oven for 5-120 minutes.
Preferably, the processing method of the multi-etching micro-nano processing template comprises one or more of ultraviolet lithography, wet chemical etching, dry etching, nano imprinting, ultra-precision processing and laser processing; the surface of the template is provided with a nano or micron scale ordered structure array; the template is made of one of a silicon wafer, a silicon wafer with a silicon dioxide plated surface, a silicon wafer with a silicon nitride plated surface, stainless steel and iron-nickel alloy; the surface structure array of the template is in one or more of a pyramid structure, a prismatic structure, a conical structure, an inverted pyramid structure and an inverted conical structure; the surface structure array has structural elements with a characteristic width of 0.5-20 μm and a characteristic height of 0.5-20 μm.
Preferably, in step S3, the ceramic particle mixed organic curing precursor solution in step S1 is coated on the template, and after standing for 1-20 minutes, the ceramic particle mixed organic curing precursor solution is uniformly spin-coated on the template by a spin coater.
Preferably, the rotation speed of the spin coater is set to be a single rotation speed or a multiple rotation speed of 100 to 3000 revolutions per minute, and the running time is 10 to 200 seconds.
Preferably, the curing temperature is set to a single temperature or multiple temperature gradients between 50 ℃ and 120 ℃ and the curing time is 10 minutes to 10 hours.
Preferably, in step S6, the surface with the micro-nano photonic structure peeled off faces a plate, and the plate is selected from one of a polycarbonate plate, a glass plate, and a metal plate.
The film has high reflectivity in a sunlight wave band (0.3-2 microns), has high radiance in an atmospheric window wave band (8-13 microns), can reduce the ambient temperature under the direct sunlight condition, and has high average cooling power. In addition, the film has better flexibility and strength and excellent hydrophobic property, and has good effects in the aspects of building roof cooling, human body wearable cooling, temperature-reducing sun-rain umbrella, device heat dissipation and the like.
The invention is based on the following principle: in the visible-near infrared band, two action mechanisms for enhancing reflectivity are mainly included, firstly, the phenomenon of total internal reflection is generated when light irradiates organic polymer with a specific photon structure, and on the other hand, the phenomenon of mie scattering is generated when the light irradiates the particles because the size of the doped ceramic particles is matched with that of the light. In the middle infrared band, two theoretical mechanisms for enhancing the infrared radiance are mainly included, firstly, the polymer film with a specific photon structure can generate gradient refractive index on the surface of the polymer film, and the polymer film has the effect of enhancing the radiance, and secondly, the ceramic particles have the phonon polarization resonance effect in the middle infrared band, so that the ceramic particles can strongly absorb infrared light and enhance the radiance. The coupling effect through the several mechanisms enables the composite film material with the specific photon structure to theoretically realize the feasibility of realizing the radiation cooling effect.
Compared with the prior art, the invention has the following beneficial effects:
firstly, a micro-nano photonic structure array is formed on the surface of the film, the reflectivity of the film can be increased by the micro-nano photonic structure in a visible near-infrared band, the infrared emissivity can be enhanced by the change of the gradient refractive index in a middle-infrared band, so that the purpose of radiation cooling is achieved, the components in the film are uniformly mixed, the preparation difficulty is reduced, and the effect which can be achieved only by compounding a multilayer structure can be realized;
secondly, the micro-nano structure arrays with different anisotropic morphologies are obtained through the preparation process of multi-etching micro-nano processing, and the micro-nano structure arrays on the surface play an important role in enhancing the visible near-infrared reflectivity and the radiance of the intermediate infrared band; according to the film with the micro-nano photonic structure array on the surface, which is prepared by direct mixing, the effect of multiple layers can be realized by utilizing the surface structure of the film and the performance of a particle-doped material, namely the reflectivity is improved by a visible near-infrared band, and the radiance is improved by a middle-infrared band; the method is simple, low in cost and strong in universality;
thirdly, the method uses a general production process and adopts a multi-etching double-spin coating vacuum thermosetting process to prepare the organic-inorganic composite radiation cooling film with the micro-nano photon structure in large area for the first time at low cost, and solves the problems of insufficient strength of splicing parts and reduced optical effect caused by bonding the splicing parts
Fourthly, the radiation cooling efficiency of the organic-inorganic composite film with the micro-nano photon structure is obviously improved, and meanwhile, the film has good flexibility and tensile strength, and can be used for refrigeration of small electronic devices and wearable cooling clothes;
fifthly, the micro-nano photon structure on the surface of the film can enable the film to have very good hydrophobic performance, the hydrophobic angle is between 100 and 160 degrees, and the film can be made into a weather umbrella cover; in addition, the film can also be used for cooling devices such as mobile phones and the like, and the cooling effect is excellent, so that the devices such as the mobile phones and the like can be ensured to run quickly and durably.
Sixth, the organic-inorganic composite radiation cooling film with the micro-nano photon structure prepared by the invention is bright white in appearance, has a reflectivity of 95% in a sunlight wave band (0.3-2 micrometers), has a radiance of 96% in an atmospheric window wave band (8-13 micrometers), is 10 ℃ lower than the ambient environment at most under an illumination condition, and has a good radiation cooling and heat dissipation effect.
Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.
Drawings
Fig. 1-3 are schematic surface microtopography diagrams of an organic-inorganic composite radiation cooling film with a micro-nano photon structure according to the invention;
FIG. 4 is an optical photograph of an organic-inorganic composite radiation cooling film having a micro-nano photonic structure according to example 1 of the present invention;
FIG. 5 is an optical photograph of an organic-inorganic composite radiation cooling film having a micro-nano photonic structure according to examples 2 to 5 of the present invention;
FIG. 6 is a graph showing a visible NIR reflectance spectrum of an organic-inorganic composite radiation-cooled monolithic film with a micro-nano photonic structure in example 5 of the present invention;
FIG. 7 is a spectrum diagram of the mid-infrared emissivity of an organic-inorganic composite radiation cooling monolithic thin film with a micro-nano photonic structure in example 5 of the present invention;
FIG. 8 is a scanning electron microscope photograph of an organic-inorganic composite radiation cooling film with a micro-nano photonic structure in example 6 of the present invention;
FIG. 9 is an infrared spectrum of an organic-inorganic composite radiation cooling film of a micro-nano photonic structure in example 7 of the present invention;
FIG. 10 is a graph showing a visible-near infrared reflectance spectrum of an organic-inorganic composite radiation cooling film of a micro-nano photonic structure in example 8 of the present invention;
fig. 11 is a mid-infrared radiance spectrogram of the organic-inorganic composite radiation cooling film with the micro-nano photonic structure in embodiment 8 of the present invention.
Detailed Description
The invention is further illustrated with reference to the following specific figures. It should be understood that these examples are only for illustrating the present invention and are not intended to limit the scope of the present invention. In practice, the invention will be understood to cover all modifications and variations of this invention provided they come within the scope of the appended claims.
The utility model provides a radiation cooling film, the raw materials of film include ceramic granule, organic solution, curing agent, ceramic granule, organic solution, curing agent mix and form ceramic granule and mix organic solidification precursor liquid, the film does form after the solidification of ceramic granule mixes organic solidification precursor liquid, the surface of film is formed with micro-nano photon structure array, and micro-nano photon structure array includes that a plurality of is the micro-nano photon's of array structural element, constitutes even array structure on the film surface.
The micro-nano photonic structure array can be a conical structure as shown in fig. 1, or a prismatic structure as shown in fig. 2, or a pyramidal structure as shown in fig. 3. Or the surface structure array of the template has one or more of a pyramid structure, a prismatic structure, a conical structure, an inverted pyramid structure and an inverted cone structure according to the requirement.
The following further describes the present invention with reference to specific examples.
Example 1
Stirring and mixing 200g of spherical alumina powder particles with the particle size (mean particle size, the same below) of 2 microns with 220g of PDMS solution uniformly, adding 22g of tetraethoxysilane curing agent into the curing precursor solution, and fully stirring to mix uniformly; and putting the mixed solution into a vacuum drying oven, vacuumizing, keeping for 30min, slowly introducing the atmosphere until the pressure is equal to the external air pressure, and taking out the mixed solution.
Placing a multi-etching silicon wafer template for photoetching, dry etching and wet etching on a spin coater, wherein the surface appearance of the template is composed of pyramid groove arrays with the width of 8 microns, the depth of 6 microns and the interval of 2 microns, and the pyramid groove arrays can be shown in figure 1; the mixed solution was slowly poured onto the template and left to stand for 20 minutes, after which the rotation speed of the spin coater was adjusted from 0 to 700RPM for 100 seconds, kept at 500RPM for 30 seconds, and then stopped.
Taking down the template, placing the template on a hot plate, adjusting the temperature of the hot plate to 80 ℃, keeping the temperature for 2 hours, and then cooling to room temperature; in order to obtain a radiation-cooled thin film of large area, a secondary spin-coating operation is required for the thin film. The film previously spin-coated multiple times was cut into squares and placed neatly on a flat plastic sheet with the structured side facing down to prevent contamination or masking of the structure, and then spin-coating was performed again to join the films. And then the plate is transferred to a hot table for heating and curing for two hours, wherein the heating temperature is 100 ℃. And after cooling to room temperature, stripping the film on the template to obtain the organic-inorganic composite radiation cooling film with the micro-nano prismatic structure array. The 670 μm thick radiative cooling film has 95% reflectivity in the solar band, 96% emissivity in the atmospheric window band, and 8 ℃ lower than ambient under light conditions. In addition, the film has good flexibility and tensile strength, undergoes several hundred twists and can withstand a stress of 4 mpa.
An optical photograph of the organic-inorganic composite radiation cooling film with the micro-nano photonic structure in the embodiment is shown in fig. 4, and the film is white and has certain flexibility.
Example 2
Stirring and mixing 30g of zinc oxide powder particles with the particle size of 5 microns and 30g of PTFE solution uniformly, adding 3g of dicumyl peroxide curing agent into the curing precursor solution, and stirring fully to mix uniformly; and putting the mixed solution into a vacuum drying oven, vacuumizing, keeping for 30min, slowly introducing the atmosphere until the pressure is equal to the external air pressure, and taking out the mixed solution.
Placing the nickel-plated stainless steel template after ultraprecise processing on a spin coater, wherein the surface appearance of the template is composed of a pyramid groove array with the width of 2 microns, the depth of 6 microns and the interval of 3 microns; the mixed solution was slowly poured onto the template and left to stand for 5 minutes, after which the rotation speed of the spin coater was adjusted from 0 liter to 500RPM for 10 seconds, kept at 500RPM for 30 seconds, and then stopped.
Taking down the template, placing the template on a hot plate, adjusting the temperature of the hot plate to 100 ℃, keeping the temperature for 1 hour, and then cooling to room temperature; and after cooling to room temperature, stripping the film on the template to obtain the organic-inorganic composite radiation cooling film with the micro-nano prismatic structure array. The 1090 μm thick radiative cooling film has a reflectivity of 94% in the solar band and an emissivity of 97% in the atmospheric window band, which can be 7.2 ℃ lower than ambient conditions under light conditions. In addition, the film has good flexibility and tensile strength, is not broken after being twisted for hundreds of times, and can bear the stress of 6 MPa.
Example 3
Adding 8g of spherical magnesium oxide particles with the particle size of 0.5 micron and 16g of angular zirconia powder particles with the particle size of 2 microns into 30g of PDMS liquid, and stirring and mixing uniformly; 2g of dicumyl peroxide curing agent is added and stirred continuously; and putting the mixed solution into a vacuum drying oven for vacuumizing, keeping the vacuum drying oven for 60min, then slowly introducing the atmosphere until the pressure is equal to the external air pressure, and taking out the mixed solution.
Placing the IPS template subjected to nanoimprint on a spin coater, wherein the surface appearance of the template consists of an elliptic cylindrical groove array with the width of 15 micrometers, the depth of 10 micrometers and the interval of 5 micrometers; the mixed solution was slowly poured onto the template and allowed to stand for 5 minutes, after which the rotation speed of the spin coater was adjusted to rise from 0 to 750RPM for 10 seconds, kept at the rotation speed of 750RPM for 15 seconds, and then stopped.
Taking down the template, placing the template on a hot plate, adjusting the temperature of the hot plate to 80 ℃, keeping the temperature for 2 hours, and then cooling to room temperature; after cooling to room temperature, the film on the template is stripped off to obtain the ceramic particle-organic polymer based radiation cooling film. The 480 μm thick radiative cooling film has a reflectivity of 93% in the solar band and a emissivity of 93% in the atmospheric window band, which is 5.1 ℃ lower than the ambient temperature under light conditions. In addition, the film has good flexibility and tensile strength, is not broken after being twisted for hundreds of times, and can bear the stress of 4 MPa.
Example 4
Stirring and mixing 20g of titanium oxide powder particles with the particle size of 2 microns and 20g of PTFE solution uniformly, adding 4g of polyamide curing agent into the curing precursor solution, and stirring fully to mix uniformly; and putting the mixed solution into a vacuum drying oven for vacuumizing, keeping the vacuum drying oven for 60min, then slowly introducing the atmosphere until the pressure is equal to the external air pressure, and taking out the mixed solution.
Placing the stainless steel template subjected to laser etching on a spin coater, wherein the surface appearance of the template is composed of reverse cone arrays with the width of 10 microns, the depth of 6 microns and the interval of 4 microns; the mixed solution was slowly poured onto the template and left to stand for 10 minutes, after which the rotation speed of the spin coater was adjusted from 0 to 2000RPM for 5 seconds, kept at 500RPM for 60 seconds, and then stopped.
Taking down the template, placing the template on a hot plate, adjusting the temperature of the hot plate to 70 ℃, keeping the temperature for 5 hours, and then cooling to room temperature; and after cooling to room temperature, stripping the film on the template to obtain the organic-inorganic composite radiation cooling film with the micro-nano photon structure. The radiation cooling film with the thickness of 360 mu m has the reflectivity of 90 percent in the sunlight wave band and the radiance of 86 percent in the atmospheric window wave band, and the temperature is 2.3 ℃ lower than that of the ambient environment under the illumination condition. In addition, the film has good flexibility and tensile strength, is not broken after being twisted for hundreds of times, and can bear the stress of 8 MPa.
Example 5
Adding 10g of spherical yttrium oxide particles with the particle size of 6 microns into 10g of PVC liquid, and uniformly stirring and mixing; adding 1g of polyamide curing agent and continuing stirring; and putting the mixed solution into a vacuum drying oven for vacuumizing, keeping the vacuum drying oven for 10min, then slowly introducing the atmosphere until the pressure is equal to the external air pressure, and taking out the mixed solution.
Placing the IPS template subjected to nanoimprint on a spin coater, wherein the surface appearance of the template is composed of elliptic cylindrical groove arrays with the width of 6 micrometers, the depth of 2 micrometers and the interval of 10 micrometers; the mixed solution was slowly poured onto the template and left to stand for 15 minutes, after which the rotation speed of the homogenizer was adjusted from 0 to 1050RPM for 60 seconds, the rotation speed of 1050RPM was maintained for 100 seconds, and then stopped.
Taking down the template, placing the template on a hot plate, adjusting the temperature of the hot plate to 120 ℃, keeping the temperature for 10 minutes, and then cooling the template to room temperature; after cooling to room temperature, the film on the template is stripped off to obtain the ceramic particle-organic polymer based radiation cooling film. The radiation cooling film with the thickness of 1020 mu m has the reflectivity of 95 percent in the solar wave band, the radiance of 95 percent in the atmospheric window wave band and the temperature of 7.7 ℃ lower than the ambient environment under the illumination condition. In addition, the film has good flexibility and tensile strength, is not broken after being twisted for hundreds of times, and can bear the stress of 4 MPa.
Optical photographs of the organic-inorganic composite radiation cooling film with the micro-nano photonic structure in the examples 2-5 are shown in fig. 5, wherein the examples 2-5 are sequentially arranged from left to right and from top to bottom, and fig. 5 shows that the film material prepared by the examples is white in appearance and has certain flexibility.
The visible-near infrared reflectance spectrogram of the organic-inorganic composite radiation cooling monolithic film with the micro-nano photonic structure in the example 5 is shown in fig. 6, which shows that the monolithic film has higher reflectance in the visible near infrared band.
The spectrum of the mid-infrared radiance of the organic-inorganic composite radiation cooling monolithic thin film with the micro-nano photonic structure in the example 5 is shown in fig. 7, which shows that the emissivity of the monolithic thin film in the mid-infrared band is at a higher level.
Example 6
5g of alumina powder particles with the particle size of 0.5 micron and 10g of PTFE solution are stirred and mixed uniformly, 2g of polyamide curing agent is added into the curing precursor solution, and the mixture is stirred fully to be mixed uniformly; and putting the mixed solution into a vacuum drying oven, vacuumizing, keeping for 20min, slowly introducing the atmosphere until the pressure is equal to the external air pressure, and taking out the mixed solution.
Placing the stainless steel template subjected to laser etching on a spin coater, wherein the surface appearance of the template is composed of groove arrays with the width of 20 microns, the depth of 2 microns and the interval of 1 micron; the mixed solution was slowly poured onto the template and left to stand for 10 minutes, after which the rotation speed of the spin coater was adjusted from 0 to 1000RPM for 15 seconds, held at 1500RPM for 30 seconds, and then stopped.
Taking down the template, placing the template on a hot plate, adjusting the temperature of the hot plate to 100 ℃, keeping the temperature for 2 hours, and then cooling to room temperature; in order to obtain a radiation-cooled thin film of large area, a secondary spin-coating operation is required for the thin film. The film previously spin-coated multiple times was cut into squares and placed neatly on a flat plastic sheet with the structured side facing down to prevent contamination or masking of the structure, and then spin-coating was performed again to join the films. And then the plate is transferred to a hot table to be heated and cured for one hour, wherein the heating temperature is 95 ℃. And after cooling to room temperature, stripping the film on the template to obtain the organic-inorganic composite radiation cooling film with the micro-nano photon structure. The 740 μm thick radiative cooling film has a reflectivity of 94% in the solar band and a emissivity of 96% in the atmospheric window band, and is 7.1 ℃ lower than the ambient temperature under the illumination condition. In addition, the film has good flexibility and tensile strength, is not broken after being twisted for hundreds of times, and can bear the stress of 4 MPa.
Fig. 8 shows a scanning electron micrograph of the organic-inorganic composite radiation cooling film with the micro-nano photonic structure in example 6, which shows that the surface of the film has a micro-nano structure array arranged in order.
Example 7
Adding 15g of spherical yttrium oxide particles with the particle size of 2 microns and 15g of spherical titanium oxide powder particles with the particle size of 2 microns into 30g of PTFE liquid, and stirring and mixing uniformly; adding 3g of epoxy resin curing agent and continuing stirring; and putting the mixed solution into a vacuum drying oven, vacuumizing, keeping for 20min, slowly introducing the atmosphere until the pressure is equal to the external air pressure, and taking out the mixed solution.
Placing the silicon wafer template after multiple etching on a spin coater, wherein the surface appearance of the template is composed of an elliptic cylindrical groove array with the width of 10 microns, the depth of 2 microns and the interval of 10 microns; the mixed solution was slowly poured onto the template and left to stand for 10 minutes, after which the rotation speed of the spin coater was adjusted from 0 to 1550RPM for 5 seconds, kept at the rotation speed of 750RPM for 100 seconds, and then stopped.
Taking down the template, placing the template on a hot plate, adjusting the temperature of the hot plate to 95 ℃, keeping the temperature for 1 hour, and then cooling to room temperature; in order to obtain a radiation-cooled thin film of large area, a secondary spin-coating operation is required for the thin film. The film previously spin-coated multiple times was cut into squares and placed neatly on a flat plastic sheet with the structured side facing down to prevent contamination or masking of the structure, and then spin-coating was performed again to join the films. And then the plate is transferred to a hot table for heating and curing for two hours, wherein the heating temperature is 80 ℃. After cooling to room temperature, the film on the template is stripped off to obtain the ceramic particle-organic polymer based radiation cooling film. The 270 μm thick radiative cooling film has 88% reflectivity in the solar band and 82% emissivity in the atmospheric window band, which is 1.7 ℃ lower than ambient under light conditions. In addition, the film has good flexibility and tensile strength, is not broken after being twisted for hundreds of times, and can bear the stress of 6 MPa.
The infrared spectrogram of the organic-inorganic composite radiation cooling film with the micro-nano photonic structure in the example 7 is shown in fig. 9, which shows that the reflectivity of the film in the mid-infrared band is low, and therefore the mid-infrared radiance of the film is correspondingly high.
Example 8
Adding 15g of spherical alumina particles with the particle size of 6 microns into 30g of PDMS liquid, and stirring and mixing uniformly; adding 5g of dicumyl peroxide curing agent and continuing stirring; and putting the mixed solution into a vacuum drying oven for vacuumizing, keeping the vacuum drying oven for 40min, then slowly introducing the atmosphere until the pressure is equal to the external air pressure, and taking out the mixed solution.
Placing the IPS template subjected to nanoimprint on a spin coater, wherein the surface appearance of the template is formed by an elliptic cylindrical groove array with the width of 16 micrometers, the depth of 8 micrometers and the interval of 6 micrometers; the mixed solution was slowly poured onto the template and left to stand for 40 minutes, after which the rotation speed of the spin coater was adjusted from 0 to 1250RPM for 40 seconds, kept at a rotation speed of 350RPM for 70 seconds, and then stopped.
Taking down the template, placing the template on a hot plate, adjusting the temperature of the hot plate to 80 ℃, keeping the temperature for 60 minutes, and then cooling the template to room temperature; in order to obtain a radiation-cooled thin film of large area, a secondary spin-coating operation is required for the thin film. The film previously spin-coated multiple times was cut into squares and placed neatly on a flat plastic sheet with the structured side facing down to prevent contamination or masking of the structure, and then spin-coating was performed again to join the films. And then the plate is transferred to a hot table for heating and curing for two hours, wherein the heating temperature is 80 ℃. After cooling to room temperature, the film on the template is stripped off to obtain the ceramic particle-organic polymer based radiation cooling film. The 860 μm thick radiative cooling film has 95% reflectivity in the solar band and 95% emissivity in the atmospheric window band, which is 7.8 ℃ lower than ambient conditions under light conditions. In addition, the film has good flexibility and tensile strength, is not broken after being twisted and bent for hundreds of times, and can bear the stress of 7 MPa.
The visible-near infrared reflectance spectrogram of the organic-inorganic composite radiation cooling film with the micro-nano photonic structure in the example 8 is shown in fig. 10, which shows that the film has higher reflectance in the visible near infrared band.
The mid-infrared radiance spectrogram of the organic-inorganic composite radiation cooling film with the micro-nano photonic structure in the example 8 is shown in fig. 11, which shows that the emissivity of the film in the mid-infrared band is at a higher level.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (16)
1. The utility model provides a radiation cooling film, its characterized in that, the raw materials of film include ceramic granule, organic solution, curing agent, ceramic granule, organic solution, curing agent mix and form ceramic granule and mix organic solidification precursor liquid, the film does form after the solidification of ceramic granule mixes organic solidification precursor liquid, the surface of film is formed with micro-nano photon structure array, and micro-nano photon structure array includes that a plurality of is the micro-nano photon's of array structural element.
2. The film according to claim 1, wherein the micro-nano photonic structure array has a structural element shape of one of a pyramid structure, a prismatic structure, a cone structure, an inverted pyramid structure and an inverted cone structure, the structural element has a characteristic width of 0.5 μm to 20 μm and a characteristic height of 0.5 μm to 20 μm; the film has a thickness of 100 to 2000 μm.
3. The radiant cooling film of claim 1, wherein the ceramic particles are selected from one or more of alumina, zinc oxide, zirconia, magnesia, boron nitride, yttria, titania.
4. The radiation cooling film as claimed in claim 1, wherein the average particle size of the ceramic particles is 0.2-10 μm, the morphology of the ceramic particles is one or more of angular, spheroidal and spherical, and the mass fraction of the ceramic particles in the organic curing precursor liquid mixed with the ceramic particles is 5-80%.
5. The film of claim 1, wherein the organic solution is an organic polymer, and the organic polymer is selected from one of polydimethylsiloxane, polytetrafluoroethylene and polyvinyl chloride; the curing agent enables ceramic particles, organic solution and curing agent to be mixed to form ceramic particles mixed with organic curing precursor solution to be cured under the condition of heating or standing for a long time, and the curing agent comprises resin.
6. The radiation cooling film as claimed in claim 1, wherein the mass ratio of the curing agent to the ceramic particle mixed organic curing precursor liquid is 1: 5 to 1: 20.
7. the preparation method of the radiation cooling film is characterized by comprising the following steps:
step S1, mixing the ceramic particles, the organic solution and the curing agent to prepare a ceramic particle mixed organic curing precursor solution;
step S2: placing the multi-etched micro-nano processed template on a spin coater turntable and communicating a vacuum pump to enable the template to be adsorbed by the spin coater turntable;
step S3: coating the ceramic particle mixed organic curing precursor liquid obtained in the step S1 on a template, and uniformly spin-coating the ceramic particle mixed organic curing precursor liquid on the template through a spin coater;
step S4: placing the template uniformly coated with the ceramic particle mixed organic curing precursor liquid on a heating plate for heating and curing, and then cooling to room temperature;
step S5: and stripping the cured organic-inorganic composite radiation cooling film with the micro-nano photon structure from the template subjected to the micro-nano processing by etching to obtain the radiation cooling film.
8. The method for preparing the radiation cooling film according to claim 7, further comprising the following steps:
step S6: repeating the steps S1 to S5, preparing a plurality of organic-inorganic composite radiation cooling films with micro-nano photon structures, and tightly tiling the films on a flat plate by cutting;
step S7: coating the ceramic particle mixed organic curing precursor solution on the tiled film, and performing secondary spin coating;
step S8: placing the plate coated with the ceramic particle mixed organic curing precursor solution on a heating plate for heating and curing, and then cooling to room temperature;
step S9: and stripping the organic-inorganic composite radiation cooling film with the large-area micro-nano photon structure formed after curing from the template to obtain the large-area radiation cooling film.
9. The method for preparing the radiation cooling film according to claim 7 or 8, wherein the step S1 of forming the ceramic particle mixed organic curing precursor solution comprises the following steps:
step S11: putting the ceramic particles into an organic solution, and mixing the ceramic particles and the organic solution uniformly by fully stirring; the ceramic particles are one or more selected from alumina, zinc oxide, zirconia, magnesia, boron nitride, yttria and titanium oxide white powder, the organic solution is an organic polymer, and the organic polymer is one selected from polydimethylsiloxane, polytetrafluoroethylene and polyvinyl chloride transparent solution;
step S12: adding a curing agent into the solution obtained in the step S11, and stirring to uniformly mix the curing agent and the solution;
step S13: putting the solution obtained in the step S12 into a vacuum drying oven, vacuumizing to discharge air in the solution, so that no bubbles are emitted in the solution finally;
step S14: and opening a vent valve of the vacuum box, and slowly returning the air pressure in the vacuum box to the initial state which is the same as the external air pressure after 5 to 10 minutes, thus obtaining the ceramic particle mixed organic curing precursor liquid.
10. The method for preparing the radiation cooling film according to claim 9, wherein the time for vacuumizing in the vacuum drying oven of step S13 is 5-120 minutes.
11. The preparation method of the radiation cooling film according to claim 7, wherein the processing method of the multi-etching micro-nano processing template comprises one or more of ultraviolet lithography, wet chemical etching, dry etching, nano imprinting, ultra-precision processing and laser processing; the surface of the template is provided with a nano or micron scale ordered structure array; the template is made of one of a silicon wafer, a silicon wafer with a silicon dioxide plated surface, a silicon wafer with a silicon nitride plated surface, stainless steel and iron-nickel alloy; the surface structure array of the template is in one or more of a pyramid structure, a prismatic structure, a conical structure, an inverted pyramid structure and an inverted conical structure; the surface structure array has structural elements with a characteristic width of 0.5-20 μm and a characteristic height of 0.5-20 μm.
12. The method for preparing a radiation cooling film according to claim 7, wherein in step S3, the ceramic particle mixed organic curing precursor solution of step S1 is coated on the template, and after standing for 1-20 minutes, the ceramic particle mixed organic curing precursor solution is uniformly spin-coated on the template through a spin coater.
13. The method for preparing a radiation cooling film according to claim 7, wherein the rotation speed of the spin coater is set to be a single rotation speed or multiple rotation speeds of 100 to 3000 rpm, and the operation time is 10 to 200 s.
14. The method for preparing a radiation cooling film according to claim 7, wherein the curing temperature is set to a single temperature or multiple temperature gradients between 50 ℃ and 120 ℃ and the curing time is 10 minutes to 10 hours.
15. The method for preparing the radiation cooling film according to claim 8, wherein in the step S6, the surface with the micro-nano photonic structure peeled off faces a plate, and the plate is selected from one of a polycarbonate plate, a glass plate and a metal plate.
16. The radiant cooling film prepared by the method for preparing the radiant cooling film according to any one of claims 1 to 6 or the radiant cooling film according to any one of claims 7 to 15, and the application of the radiant cooling film in building roof cooling, human body wearable cooling, temperature-reducing sun-rain umbrella or device heat dissipation.
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