CN113943922B - Preparation method and restoration method of repairable dynamic infrared radiation regulation material - Google Patents
Preparation method and restoration method of repairable dynamic infrared radiation regulation material Download PDFInfo
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- CN113943922B CN113943922B CN202111181913.4A CN202111181913A CN113943922B CN 113943922 B CN113943922 B CN 113943922B CN 202111181913 A CN202111181913 A CN 202111181913A CN 113943922 B CN113943922 B CN 113943922B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/20—Metallic material, boron or silicon on organic substrates
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5886—Mechanical treatment
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B26/00—Optical devices or arrangements for the control of light using movable or deformable optical elements
- G02B26/02—Optical devices or arrangements for the control of light using movable or deformable optical elements for controlling the intensity of light
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Abstract
A preparation method and a restoration method of a repairable dynamic infrared radiation regulation material relate to a preparation method and a restoration method of an infrared radiation regulation material. The invention aims to solve the problems of complex excitation mode and poor stability of the existing dynamic infrared radiation regulation material. The method comprises the following steps: 1. preparing SEBS solution; 2. blade coating SEBS film; 3. stripping the SEBS film; 4. preparing a gold-plated SEBS film; 5. and (3) cracking the gold layer of the gold-plated SEBS film in a mechanical stretching mode to obtain the repairable dynamic infrared radiation regulation material. The repairing method comprises the following steps: and (5) heat treatment. A repairable dynamic infrared radiation regulating material can be used as a new generation dynamic infrared radiation regulating material for repeated use. The invention can obtain a repairable dynamic infrared radiation regulating and controlling material.
Description
Technical Field
The invention relates to a preparation method and a repair method of an infrared radiation regulation material.
Background
The infrared radiation regulating and controlling material plays a role in the fields of energy-saving building, intelligent wearing heat management, infrared thermal imaging, stealth, aerospace heat control and the like. Currently, there are two main infrared radiation regulating materials, a traditional static regulating material and an increasingly rising dynamic regulating material, and the dynamic regulating material is paid attention to because the infrared radiation can be regulated in real time as required. The dynamic infrared control materials are mainly electrochromic materials and thermochromic materials, and the materials need to maintain certain voltage or temperature to stabilize the effect, which is not an ideal control mode in terms of energy saving, so that the realization of infrared radiation control by a simple direct excitation mode is a problem to be solved.
The dynamic infrared regulation and control material prepared by coating a metal layer on an elastic matrix can realize infrared radiation regulation and control in a mechanical stretching mode, and the basic principle is as follows: the elastic substrate has very high infrared transmittance, and the metal layer has very high infrared reflectance, so that when the material is uniaxially stretched, the metal layer can be broken to generate cracks, and at the moment, the elastic substrate is partially exposed. When infrared light irradiates to the surface of the material, the infrared light can permeate at the crack, and reflect at the metal layer, and the width of the crack can be changed by controlling the mechanical stretching degree, so that the infrared transmittance and the reflectivity of the material are changed, and the dynamic and effective infrared radiation regulation and control are realized. Hydrogenated styrene-butadiene block copolymers (SEBS) are linear triblock copolymers with polystyrene as the end block and ethylene-butene copolymers obtained by hydrogenation of polybutadiene as the intermediate elastomeric block. The material does not contain unsaturated double bonds, so that the material has good stability and aging resistance, and more importantly, the material is an elastomer with thermoplastic property, and the transmittance in an infrared band can reach 90%. According to current literature reports, leung et al coated a metallic copper layer on a SEBS substrate to prepare a composite for use in wearable thermostats and achieve different ranges of temperature regulation by varying the degree of stretching (E.M.Leung, M.Colorado Escobar, G.T.Stiubianu, S.R.Jim, A.L.Vyatskikh, Z.Feng, N.Garner, P.Patel, K.L.Naughton, M.Follador, E.Karshalev, M.D.Trexler, A.A.Gorodetsky, A dynamic thermoregulatory material inspired by squid skin, nature Communications,10 (2019) 1947.). However, as the stretching times gradually increase, the width of the crack in the release state is larger and larger, so that the material still generates larger transmittance in the release state, which tends to affect the infrared radiation regulating capability of the material, and the poor stability of the material severely limits the industrialized development of the material.
Disclosure of Invention
The invention aims to solve the problems of complex excitation mode and poor stability of the existing dynamic infrared radiation regulation material, and provides a repairable preparation method and a repairable method of the dynamic infrared radiation regulation material.
The preparation method of the repairable dynamic infrared radiation regulation material is completed according to the following steps:
1. preparing SEBS solution:
adding SEBS powder into tetrahydrofuran, and completely dissolving the SEBS powder into the tetrahydrofuran under the conditions of magnetic stirring and heating to obtain SEBS solution;
2. blade coating SEBS film:
pouring the SEBS solution on the clean glass surface, and then carrying out blade coating film formation by using a manual blade coater;
3. stripping SEBS film:
drying the SEBS film scraped on the glass at room temperature, soaking in ethanol solution after drying, stripping the SEBS film from the glass in the ethanol solution, transferring the SEBS film to the surface of filter paper, and drying in an oven to obtain an unsupported SEBS film;
4. preparing a gold-plated SEBS film:
performing thermal evaporation of gold particles on the SEBS film by adopting a vacuum thermal evaporation method to obtain a gold-plated SEBS film;
5. and (3) cracking the gold layer of the gold-plated SEBS film in a mechanical stretching mode to obtain the repairable dynamic infrared radiation regulation material.
The repairing method of the repairable dynamic infrared radiation regulating material is completed according to the following steps:
and repeatedly flushing the repairable dynamic infrared radiation regulating material by using absolute ethyl alcohol, and then putting the repairable dynamic infrared radiation regulating material into an oven for heat treatment to finish the repairable dynamic infrared radiation regulating material.
The principle and the advantages of the invention are that:
1. according to the invention, the repairable dynamic infrared radiation regulation material is prepared by combining the infrared high-transmittance elastic matrix with the infrared high-reflectance metal coating, and a simple and direct mechanical stretching mode is utilized to enable the metal layer to generate cracks, so that when infrared light irradiates to the surface of the material, the infrared transmittance and the reflectivity of the material are changed, and the effective dynamic infrared radiation regulation is realized; when the length of the gold-plated SEBS film is stretched from the original length to three times of the original length under the action of mechanical stretching, the regulating and controlling range of the transmittance of the gold-plated SEBS film is increased from 0% to 51%, and the regulating and controlling range of the reflectance is reduced from 100% to 37%;
2. the repairable dynamic infrared radiation regulating material prepared by the invention can repair cracks in a heating mode after being subjected to multiple mechanical stretching, the transmittance of the material can be recovered to 0% after heating, and the reflectivity of the material can be recovered to 100%, so that the material can be repeatedly used as a new generation of dynamic infrared radiation regulating material for multiple times.
The invention can obtain a repairable dynamic infrared radiation regulating and controlling material.
Drawings
FIG. 1 is an SEM image of a gold-plated SEBS film obtained in the step four of the example;
FIG. 2 is an SEM image of the gold-plated SEBS film obtained in the fourth step of the example when the length of the film is stretched to three times the original length;
FIG. 3 is an SEM image showing the recovery of the gold-plated SEBS film from three times the original length to the original length in the fourth step of the example;
FIG. 4 is an SEM image of a multi-mechanically stretched gold-plated SEBS film after repair.
Detailed Description
The following examples further illustrate the invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, procedures, or conditions of the present invention without departing from the spirit of the invention are intended to be within the scope of the present invention.
The first embodiment is as follows: the preparation method of the repairable dynamic infrared radiation regulation material is completed according to the following steps:
1. preparing SEBS solution:
adding SEBS powder into tetrahydrofuran, and completely dissolving the SEBS powder into the tetrahydrofuran under the conditions of magnetic stirring and heating to obtain SEBS solution;
2. blade coating SEBS film:
pouring the SEBS solution on the clean glass surface, and then carrying out blade coating film formation by using a manual blade coater;
3. stripping SEBS film:
drying the SEBS film scraped on the glass at room temperature, soaking in ethanol solution after drying, stripping the SEBS film from the glass in the ethanol solution, transferring the SEBS film to the surface of filter paper, and drying in an oven to obtain an unsupported SEBS film;
4. preparing a gold-plated SEBS film:
performing thermal evaporation of gold particles on the SEBS film by adopting a vacuum thermal evaporation method to obtain a gold-plated SEBS film;
5. and (3) cracking the gold layer of the gold-plated SEBS film in a mechanical stretching mode to obtain the repairable dynamic infrared radiation regulation material.
The second embodiment is as follows: the present embodiment differs from the specific embodiment in that: the mass fraction of the SEBS solution in the first step is 6% -12%. The other steps are the same as in the first embodiment.
And a third specific embodiment: this embodiment differs from the first or second embodiment in that: the speed of the magnetic stirring in the first step is 100 r/min-1000 r/min. The other steps are the same as those of the first or second embodiment.
The specific embodiment IV is as follows: one difference between this embodiment and the first to third embodiments is that: the heating temperature in the first step is 60-90 ℃. The other steps are the same as those of the first to third embodiments.
Fifth embodiment: one to four differences between the present embodiment and the specific embodiment are: the manual blade coater in the second step had a specification of 100. Mu.m. Other steps are the same as those of the first to fourth embodiments.
Specific embodiment six: the present embodiment differs from the first to fifth embodiments in that: the mass fraction of the ethanol solution in the third step is 99%. Other steps are the same as those of the first to fifth embodiments.
Seventh embodiment: one difference between the present embodiment and the first to sixth embodiments is that: the temperature of the oven in the third step is 60-80 ℃; the drying time is 10-12 h. Other steps are the same as those of embodiments one to six.
Eighth embodiment: one difference between the present embodiment and the first to seventh embodiments is that: and step four, the thickness of the gold film on the gold-plated SEBS film is 100 nm-300 nm. The other steps are the same as those of embodiments one to seven.
Detailed description nine: the repairing method of the repairable dynamic infrared radiation regulating material in the embodiment is completed according to the following steps:
and repeatedly flushing the repairable dynamic infrared radiation regulating material by using absolute ethyl alcohol, and then putting the repairable dynamic infrared radiation regulating material into an oven for heat treatment to finish the repairable dynamic infrared radiation regulating material. Other steps are the same as those of embodiments one to eight.
Detailed description ten: the present embodiment differs from the first to ninth embodiments in that: the flushing times are 2-3 times, the temperature of the heat treatment is 80-120 ℃, and the heat treatment time is 10-12 hours. The other steps are the same as those of embodiments one to nine.
The present invention will be described in detail with reference to the accompanying drawings and examples.
Embodiment one: the preparation method of the repairable dynamic infrared radiation regulation material is completed according to the following steps:
1. preparing SEBS solution:
adding SEBS powder into tetrahydrofuran, and completely dissolving the SEBS powder into the tetrahydrofuran under the conditions of magnetic stirring speed of 500r/min and heating temperature of 80 ℃ to obtain SEBS solution with mass fraction of 10%;
2. blade coating SEBS film:
pouring the SEBS solution on the clean glass surface, and then carrying out blade coating film formation by using a manual blade coater;
the specification of the manual knife coater in the second step is 100 mu m;
3. stripping SEBS film:
drying the SEBS film scraped on the glass at room temperature, soaking the SEBS film in ethanol solution after drying, stripping the SEBS film from the glass in the ethanol solution, transferring the SEBS film to the surface of filter paper, and drying the SEBS film in an oven at 80 ℃ for 12 hours to obtain an unsupported SEBS film;
the mass fraction of the ethanol solution in the third step is 99%;
4. preparing a gold-plated SEBS film:
performing thermal evaporation of gold particles on the SEBS film by adopting a vacuum thermal evaporation method to obtain a gold-plated SEBS film;
the thickness of the gold film on the gold-plated SEBS film in the fourth step is 200nm;
5. and (3) cracking the gold layer of the gold-plated SEBS film in a multiple mechanical stretching mode to obtain the repairable dynamic infrared radiation regulation material.
When the length of the gold-plated SEBS film obtained in the step four in the embodiment is stretched from the original length to three times of the original length under the action of mechanical stretching, the regulating and controlling range of the transmittance is increased from 0% to 51%, and the regulating and controlling range of the reflectance is reduced from 100% to 37%.
FIG. 1 is an SEM image of a gold-plated SEBS film obtained in the step four of the example;
FIG. 2 is an SEM image of the gold-plated SEBS film obtained in the fourth step of the example when the length of the film is stretched to three times the original length;
fig. 3 is an SEM image of the gold-plated SEBS film obtained in the step four of the example from three times the original length to the original length.
As can be seen from fig. 1 to 3: the original state of the gold-plated SEBS film is a dense structure, cracks appear when it is stretched from the original length to three times the length, and the width of the cracks is reduced but still present when it is restored to the original state.
The repairing method of the repairable dynamic infrared radiation regulating material (the gold-plated SEBS film subjected to multiple mechanical stretching) obtained in the step four is completed according to the following steps:
and repeatedly flushing the repairable dynamic infrared radiation regulation material for 3 times by using absolute ethyl alcohol, and then placing the repairable dynamic infrared radiation regulation material into an oven with the temperature of 100 ℃ for heat treatment for 12 hours to finish the repairable dynamic infrared radiation regulation material.
The transmittance of the repairable dynamic infrared radiation regulating material can be recovered to 0% after heating, and the reflectivity of the repairable dynamic infrared radiation regulating material can be recovered to 100%.
FIG. 4 is an SEM image of a multi-mechanically stretched gold-plated SEBS film after repair.
As can be seen from fig. 4, after thermal repair, the cracks of the gold-plated SEBS film disappeared.
Claims (9)
1. A repairable dynamic infrared radiation regulation material repairing method is characterized in that the repairable dynamic infrared radiation regulation material repairing method is completed according to the following steps:
repeatedly washing the repairable dynamic infrared radiation regulation material by using absolute ethyl alcohol, and then putting the repairable dynamic infrared radiation regulation material into an oven for heat treatment to finish the repairable dynamic infrared radiation regulation material repairing method;
the preparation method of the repairable dynamic infrared radiation regulation material is completed according to the following steps:
1. preparing SEBS solution:
adding SEBS powder into tetrahydrofuran, and completely dissolving the SEBS powder into the tetrahydrofuran under the conditions of magnetic stirring and heating to obtain SEBS solution;
2. blade coating SEBS film:
pouring the SEBS solution on the clean glass surface, and then carrying out blade coating film formation by using a manual blade coater;
3. stripping SEBS film:
drying the SEBS film scraped on the glass at room temperature, soaking in ethanol solution after drying, stripping the SEBS film from the glass in the ethanol solution, transferring the SEBS film to the surface of filter paper, and drying in an oven to obtain an unsupported SEBS film;
4. preparing a gold-plated SEBS film:
performing thermal evaporation of gold particles on the SEBS film by adopting a vacuum thermal evaporation method to obtain a gold-plated SEBS film;
5. and (3) cracking the gold layer of the gold-plated SEBS film in a mechanical stretching mode to obtain the repairable dynamic infrared radiation regulation material.
2. The method for repairing the repairable dynamic infrared radiation regulation material according to claim 1, wherein the flushing times are 2-3 times, the heat treatment temperature is 80-120 ℃, and the heat treatment time is 10-12 hours.
3. The method for repairing a repairable dynamic infrared radiation regulating material according to claim 1, wherein the mass fraction of the SEBS solution in the step one is 6% -12%.
4. The method for repairing a repairable dynamic infrared radiation regulating material according to claim 1, wherein the magnetic stirring speed in the first step is 100 r/min-1000 r/min.
5. The method for repairing a repairable dynamic infrared radiation regulating material according to claim 1, wherein the heating temperature in the first step is 60-90 ℃.
6. The method for repairing a repairable dynamic infrared radiation modulation material according to claim 1, wherein the manual blade coater in the second step has a specification of 100 μm.
7. The method for repairing a repairable dynamic infrared radiation modulation material according to claim 1, wherein the mass fraction of the ethanol solution in the third step is 99%.
8. The method for repairing a repairable dynamic infrared radiation regulation material according to claim 1, wherein the temperature of the oven in the third step is 60-80 ℃; the drying time is 10-12 hours.
9. The method for repairing a repairable dynamic infrared radiation regulating material according to claim 1, wherein the thickness of the gold film on the gold-plated SEBS film in the fourth step is 100 nm-300 nm.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111077603A (en) * | 2019-12-30 | 2020-04-28 | 哈尔滨工业大学 | Flexible film with adjustable infrared emissivity and preparation method thereof |
| CN112647107A (en) * | 2020-11-30 | 2021-04-13 | 哈尔滨工业大学 | Preparation method of polyaniline/gold particle composite film with high infrared radiation regulation and control capability |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111077603A (en) * | 2019-12-30 | 2020-04-28 | 哈尔滨工业大学 | Flexible film with adjustable infrared emissivity and preparation method thereof |
| CN112647107A (en) * | 2020-11-30 | 2021-04-13 | 哈尔滨工业大学 | Preparation method of polyaniline/gold particle composite film with high infrared radiation regulation and control capability |
Non-Patent Citations (2)
| Title |
|---|
| A dynamic thermoregulatory material inspired by squid skin;Erica M. Leung et.al.;《NATURE COMMUNICATIONS》;第1-10页 * |
| Highly adhesive, washable and stretchable on-skin electrodes based on polydopamine and silk fibroin for ambulatory electrocardiography sensing;Xiaohui Du et.al.;《Journal of Materials Chemistry C》;12257-12264页 * |
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