CN116332677B - Super-high temperature resistant ceramic metamaterial capable of inhibiting heat radiation and preparation method thereof - Google Patents
Super-high temperature resistant ceramic metamaterial capable of inhibiting heat radiation and preparation method thereof Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 73
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- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims abstract description 16
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- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 8
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- 239000000463 material Substances 0.000 description 14
- 239000011888 foil Substances 0.000 description 12
- 239000000945 filler Substances 0.000 description 7
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 6
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
Abstract
The invention discloses an ultra-high temperature resistant ceramic metamaterial capable of inhibiting heat radiation and a preparation method thereof, wherein the product comprises a first circulating layer and a second circulating layer arranged on the first circulating layer; the first circulation layer is sequentially provided with a first silicon dioxide aerogel heat insulation layer, a first silicon dioxide bonding layer, a second silicon dioxide aerogel heat insulation layer and a first titanium nitride reflecting layer from bottom to top; the second circulation layer is sequentially provided with a third silica aerogel heat insulation layer, a second silica bonding layer, a fourth silica aerogel heat insulation layer, a third silica bonding layer and a second titanium nitride reflecting layer from bottom to top. The preparation method comprises the steps of preparing the heat insulation layer, preparing the bonding layer and preparing the reflecting layer. The ultra-high temperature resistant ceramic metamaterial for inhibiting heat radiation, which is prepared by the invention, has the functions of low emissivity, low heat conductivity, ultra-high temperature stability, large-scale preparation and the like.
Description
Technical Field
The invention relates to an ultra-high temperature resistant ceramic metamaterial and a preparation method thereof.
Background
The suppression of heat radiation from ultra-high temperature heat sources is very important in the fields of aerospace, nuclear power conversion, thermoelectric conversion and the like. For example, in the component parts of the nuclear battery, the heat radiation insulating layer can be designed to reduce the radiation heat loss of a heat source, improve the utilization rate of the radiation heat and further improve the efficiency of the battery. Early researchers coated the emissive surface with a layer of highly reflective material to insulate the radiant heat (int. J. Appl. Ceramic. Technology 2006, 3, 81-93), however, the coating suffers from evaporation and diffusion problems at ultra-high temperatures, resulting in degradation of the coating over time. According to Steven-Boltzmann's law, radiant energy per unit area is proportional to emissivity and fourth power of thermodynamic temperature, and thus, heat radiation of an object can be suppressed by lowering emissivity or lowering thermodynamic temperature. The heat radiation insulating layer commonly used at present is a multi-layer insulating (multi-layer insulations, MLI) structure, which is formed by alternately filling a low-heat-conductivity material in the middle by using a high-reflectivity metal foil as a reflecting layer, can simultaneously reduce the infrared emissivity and the surface thermodynamic temperature, and has extremely low heat conductivity under high vacuum, and is also called as a super heat insulating material. The metallic foil materials commonly used for the MLI structure include molybdenum foil, gold foil, titanium foil, etc., while the low thermal conductivity filler materials commonly used include zirconia, silica, ytterbium powder, etc. Although the MLI structure described above has some adiabatic effect, these materials have some obvious drawbacks, such as that molybdenum foil is relatively brittle, gold foil is not resistant to ultra-high temperature, titanium foil is flammable, and ytterbium powder easily increases the adhesiveness of metal foil, etc. Therefore, the ultra-high temperature stability of the material itself, the compatibility between the reflective layer and the filler layer, and the thermal insulation performance of the MLI structure as a whole are all required to be further improved. Aerogels have been used by researchers as filler layers in MLI structures as ultra low thermal conductivity materials. For example, publication No. CN115257096a reports a novel heat radiation inhibiting laminated structure composed of an upper layer with low infrared emissivity, a phase-change energy storage middle layer and a heat radiation reflecting lower layer based on an aerogel film, which has advantages of high solar reflectance, low average infrared emissivity in the 3-15 μm band, high phase-change enthalpy value, etc., however, phase-change materials in the phase-change energy storage layer include but are not limited to paraffin, polyalcohol, fatty amine, higher fatty alcohol, higher fatty acid, etc., which are easily decomposed at ultra-high temperature and are not suitable for ultra-high temperature systems. In addition, wang et al reported an MLI structure (Heat Mass transfer 2018, 54, 2793-2798) in which an aerogel composite material is used as a filler layer, a copper foil, a stainless steel foil, a molybdenum foil, or the like is used as a reflective layer, which exhibits low thermal conductivity at an ultra-high temperature of 1000 ℃, and although the filler layer uses an aerogel composite material having low thermal conductivity, the reflective layer is still a conventional metal foil material, which is bulky, easily oxidized at an ultra-high temperature, and has poor long-term stability, and the MLI structure is formed by simply sewing with quartz lines, and gaps between the layer structures and between the material and the surface of an actual object must cause loss of radiant Heat, without considering the difficulty of practical use. Therefore, development of an MLI structure ultra-thin metamaterial capable of inhibiting heat radiation of an ultra-high temperature heat source for a long time is needed, and the ultrathin metamaterial has the functions of low emissivity, low heat conductivity, ultra-high temperature stability, large-scale preparation and the like.
The MLI structure in the radioisotope TPV system developed by the institute of technology in the ma province uses a metallic molybdenum foil as the reflective layer and zirconia powder as the filler layer (PowerMEMS, poland, 2019-12-2 to 2019-12-6). The molybdenum foil has the advantages of low cost and high temperature stability, the zirconia powder has the characteristic of low heat conductivity, and the heat insulating material can reach low heat conductivity of about 0.1W/mK under the vacuum condition of 800 ℃. The molybdenum foil as a reflective layer is relatively brittle and is easily damaged. The large volume and weight of metal foil and powder material can lead to a relatively heavy TPV system, which is not beneficial to the portability of deep space and deep sea exploration equipment on one hand, and the increase of the MLI structure volume can lead to the loss of axial heat radiation on the other hand, and is not suitable for a heat source with high axial-to-radial ratio. In addition, MLI structures can result in loss of radiant heat by simply winding onto the heat source surface by hand.
Disclosure of Invention
The invention aims to provide an ultra-high temperature resistant ceramic metamaterial capable of inhibiting heat radiation and having the functions of low emissivity, low heat conductivity, ultra-high temperature stability, large-scale preparation and the like and a preparation method thereof.
The technical scheme of the invention is as follows:
an ultra-high temperature resistant ceramic metamaterial for inhibiting heat radiation, which is characterized in that: comprises a first circulating layer and a second circulating layer arranged on the first circulating layer; the first circulation layer is sequentially provided with a first silicon dioxide aerogel heat insulation layer, a first silicon dioxide bonding layer, a second silicon dioxide aerogel heat insulation layer and a first titanium nitride reflecting layer from bottom to top; the second circulation layer is sequentially provided with a third silica aerogel heat insulation layer, a second silica bonding layer, a fourth silica aerogel heat insulation layer, a third silica bonding layer and a second titanium nitride reflecting layer from bottom to top.
A preparation method of an ultra-high temperature resistant ceramic metamaterial for inhibiting heat radiation is characterized by comprising the following steps: the preparation method comprises the steps of preparing a heat insulation layer, preparing a bonding layer and preparing a reflecting layer;
the preparation method of the heat insulation layer comprises the following steps: firstly, synthesizing silica sol, sequentially adding 20ml of Tetraethoxysilane (TEOS) and 19.874ml of ethanol (EtOH) 1.775ml of 0.098M hydrochloric acid (HCl) into a beaker, hydrolyzing the mixed solution in a water bath at 60 ℃ for 90min, adding 13.843ml of 0.08M ammonia water and 183.05 ml ethanol for further polycondensation, and slightly stirring and uniformly mixing; aging the obtained silica sol in a constant-temperature water bath box at 50 ℃ for 84 hours, then washing with ethanol for three times in 3 hours, washing with normal hexane for two times in 4 hours, soaking in 0.4M trimethylchlorosilane normal hexane solution for 20 hours, and finally washing with normal hexane for two times in 2 hours; adding a certain amount of ethanol into the obtained silica wet gel, performing ultrasonic breaking to obtain silica sol, and performing centrifugal purification for later use; adopting a 300um thick silicon wafer as a substrate, adopting silicon dioxide sol as impregnating solution, carrying out repeated impregnation and lifting to obtain a 830-920nm thick silicon dioxide aerogel film, and measuring the porosity of the film to be 70% by an ellipsometer;
the preparation method of the bonding layer comprises the following steps: depositing a 160nm thick silicon dioxide film by a plasma enhanced chemical vapor deposition method (Plasma Enhanced Chemical Vapor Deposition, PECVD);
the preparation method of the reflecting layer comprises the following steps: depositing a 160nm thick ceramic titanium nitride film by a magnetron sputtering method, wherein the average reflectivity of the ceramic titanium nitride film is 0.86 at 1000-2500 nm;
and repeatedly preparing each layer of film according to the structural level to obtain the ultra-high temperature resistant ceramic metamaterial for inhibiting heat radiation.
According to the invention, the silicon dioxide aerogel with low thermal conductivity is adopted as the thermal insulation filling layer, so that the room temperature thermal conductivity of the metamaterial is only 0.34W/mK (70% porosity), and the ceramic titanium nitride with high reflectivity is adopted as the reflecting layer, so that the metamaterial has lower emissivity in a wave band of 1.5-10 mu m, and the multilayer structure has no obvious collapse or cracking after the ultrahigh temperature test at 1050 ℃, has ultrahigh temperature stability, and can be applied to long-time heat radiation inhibition of an ultrahigh temperature object. The ceramic metamaterial can be prepared on the surface of the substrate in situ in a large scale with controllable film thickness by adopting mature dipping and pulling, PECVD and magnetron sputtering coating processes. In addition, the thickness of the metamaterial is only 4.4 mu m, the axial radiation heat loss is small, the metamaterial has the advantage of light weight and thinness, and the metamaterial can be better applied to a small heat source of deep space and deep sea exploration equipment.
Drawings
The invention is further described below with reference to the drawings and examples.
FIG. 1 is a schematic structural view of a ceramic metamaterial according to the present invention.
FIG. 2 is a reflection spectrum of a titanium nitride film.
FIG. 3 is a scanning electron microscope image of a ceramic metamaterial according to the present invention.
FIG. 4 is a graph of the emission spectra of the ceramic metamaterials of the present invention at different temperatures.
FIG. 5 is a scanning electron microscope image of a ceramic metamaterial according to the present invention after testing at 1050 ℃.
Description of the embodiments
An ultra-high temperature resistant ceramic metamaterial for inhibiting heat radiation comprises a first circulating layer 1 and a second circulating layer 2 arranged on the first circulating layer; the first circulation layer is sequentially provided with a first silica aerogel heat insulation layer 11, a first silica bonding layer 12, a second silica aerogel heat insulation layer 13 and a first titanium nitride reflecting layer 14 from bottom to top; the second circulation layer is provided with a third silica aerogel heat insulation layer 21, a second silica bonding layer 22, a fourth silica aerogel heat insulation layer 23, a third silica bonding layer 24 and a second titanium nitride reflecting layer 25 in sequence from bottom to top.
The preparation method comprises the steps of preparing a heat insulation layer, preparing a bonding layer and preparing a reflecting layer;
the preparation method of the heat insulation layer comprises the following steps: firstly, synthesizing silica sol, sequentially adding 20ml of Tetraethoxysilane (TEOS) and 19.874ml of ethanol (EtOH) 1.775ml of 0.098M hydrochloric acid (HCl) into a beaker, hydrolyzing the mixed solution in a water bath at 60 ℃ for 90min, adding 13.843ml of 0.08M ammonia water and 183.05 ml of ethanol for further polycondensation, and slightly stirring and uniformly mixing. The silica sol obtained was aged in a 50 ℃ thermostat water bath for 84 hours, then washed three times with ethanol in 3 hours, then washed twice with n-hexane in 4 hours, then soaked in 0.4M trimethylchlorosilane in n-hexane for 20 hours, and finally washed twice with n-hexane in 2 hours. Adding a certain amount of ethanol into the obtained silica wet gel, performing ultrasonic breaking to obtain silica sol, and performing centrifugal purification for later use. Silica aerogel is selected as the low thermal conductivity filler material because the material has a relatively low thermal conductivity and is suitable for ultra-high temperature conditions. The method is characterized in that a large amount of ethanol and n-hexane are used for cleaning in the synthesis process, so that water in a gel porous structure is replaced, the capillary force of solvent volatilization in the drying process is reduced, thus the collapse of holes is reduced, and the subsequent trimethylchlorosilane soaking is used for carrying out alkylation modification, so that the gel is hydrophobic, the capillary action caused by hydroxyl reaction is reduced, and the shrinkage and cracking of the film during normal-pressure drying are reduced. The silicon dioxide aerogel film with the thickness of 830-920nm is obtained by adopting a silicon wafer with the thickness of 300um as a substrate and silicon dioxide sol as impregnating solution and carrying out repeated impregnation and lifting, and the porosity is 70 percent measured by an ellipsometer. The dip-coating process can control the thickness of the film well by changing the dip-coating time, the drawing speed and the drawing times, and can prepare the film in situ on any flat substrate. The porosity of the film can be further improved by optimizing the preparation parameters, so that the heat insulation effect of the material is improved.
The preparation method of the bonding layer comprises the following steps: a 160nm thick silicon dioxide film was deposited by plasma enhanced chemical vapor deposition (Plasma Enhanced Chemical Vapor Deposition, PECVD). The film impregnated with the lifting aerogel is easy to crack when reaching the thickness of a micron level, and the thickness of the silica aerogel film is further increased by taking the silica film as a bonding layer by utilizing the similarity of physical and chemical properties of the silica film and the silica aerogel, so that the radiation heat insulation capability is improved. In addition, the silica film can cover porous rough sites of the silica aerogel film, so that the surface is smoother, and the deposition of the ceramic reflecting layer is facilitated.
The preparation method of the reflecting layer comprises the following steps: a160 nm thick ceramic titanium nitride film was deposited by magnetron sputtering with an average reflectance of 0.86 at 1000-2500nm, as shown in FIG. 2. Titanium nitride is a ceramic material, has ultrahigh temperature resistance, is not easy to oxidize, has high reflectivity, can well reflect heat radiation, and reduces radiation leakage.
And repeatedly preparing each layer of film according to the structure diagram to obtain the MLI structure multilayer ceramic metamaterial (see figure 3). The adiabatic effect of the MLI structure increases with increasing number of layers. The room temperature thermal conductivity of the obtained metamaterial is 0.34W/mK (70% porosity), the average emissivity of the bands of 1.5-10 mu m is respectively 0.21, 0.25 and 0.31 under the vacuum condition of 450 ℃, 850 ℃ and 1050 ℃, the emission spectrum is shown in figure 4, and the material has no obvious cracking and collapse after the superhigh temperature test (see figure 5).
Claims (1)
1. A preparation method of an ultra-high temperature resistant ceramic metamaterial for inhibiting heat radiation is characterized by comprising the following steps: the ultra-high temperature resistant ceramic metamaterial comprises a first circulating layer and a second circulating layer arranged on the first circulating layer; the first circulation layer is sequentially provided with a first silicon dioxide aerogel heat insulation layer, a first silicon dioxide bonding layer, a second silicon dioxide aerogel heat insulation layer and a first titanium nitride reflecting layer from bottom to top; the second circulation layer is sequentially provided with a third silica aerogel heat insulation layer, a second silica bonding layer, a fourth silica aerogel heat insulation layer, a third silica bonding layer and a second titanium nitride reflecting layer from bottom to top; the room temperature thermal conductivity of the ultra-high temperature resistant ceramic metamaterial is 0.34W/mK, the porosity is 70%, and the average emissivity of the wave bands of 1.5-10 mu m is respectively 0.21, 0.25 and 0.31 under the vacuum condition of 450 ℃ and 850 ℃ and 1050 ℃;
the preparation method comprises the steps of preparing a heat insulation layer, preparing a bonding layer and preparing a reflecting layer;
the preparation method of the heat insulation layer comprises the following steps: firstly, synthesizing silica sol, sequentially adding 20ml of ethyl orthosilicate and 19.874ml of ethanol 1.775ml of 0.098M hydrochloric acid into a beaker, hydrolyzing the mixed solution in a water bath at 60 ℃ for 90min, adding 13.843ml of 0.08M ammonia water and 183.05 ml ethanol for further polycondensation, slightly stirring and uniformly mixing; aging the obtained silica sol in a constant-temperature water bath box at 50 ℃ for 84 hours, then washing with ethanol for three times in 3 hours, washing with normal hexane for two times in 4 hours, soaking in 0.4M trimethylchlorosilane normal hexane solution for 20 hours, and finally washing with normal hexane for two times in 2 hours; adding a certain amount of ethanol into the obtained silica wet gel, performing ultrasonic breaking to obtain silica sol, and performing centrifugal purification for later use; adopting a 300 mu m thick silicon wafer as a substrate, adopting silicon dioxide sol as impregnating solution, and carrying out repeated impregnation and lifting to obtain a silicon dioxide aerogel film with the thickness of 830-920 nm;
the preparation method of the bonding layer comprises the following steps: depositing a 160nm thick silicon dioxide film by a plasma enhanced chemical vapor deposition method;
the preparation method of the reflecting layer comprises the following steps: depositing a 160nm thick ceramic titanium nitride film by a magnetron sputtering method, wherein the average reflectivity of the ceramic titanium nitride film is 0.86 at 1000-2500 nm;
and repeatedly preparing each layer of film according to the structural level to obtain the ultra-high temperature resistant ceramic metamaterial for inhibiting heat radiation.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1544324A (en) * | 2003-11-20 | 2004-11-10 | 中国科学院上海技术物理研究所 | Silica dioxide aerogel membrane material preparation method |
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