CN115626825A - Aluminum oxide/lanthanide perovskite ceramic composite light absorber and preparation method thereof - Google Patents
Aluminum oxide/lanthanide perovskite ceramic composite light absorber and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an alumina/lanthanide perovskite ceramic composite light absorber and a preparation method thereof. The preparation method comprises (1) synthesizing lanthanide perovskite ceramic powder with broad spectrum and high absorption by solid phase method; (2) Preparation of a gradient of poresA structural lanthanide perovskite ceramic substrate; (3) Plating compact Al 2 O 3 A film; and (4) carrying out heat treatment in an air furnace. The surface layer of the lanthanide perovskite ceramic substrate is compact and has gradient pore distribution from outside to inside, and a transition layer exists on the interface of the film-substrate structure. The preparation method has simple and convenient process and low cost, the optical absorber prepared by the method has high absorptivity in the wave band range of 0.3-14 mu m, is high temperature resistant and thermal shock resistant, has high laser damage threshold, and can be widely applied to components in the high-temperature photothermal conversion field such as laser energy meters, laser power meters and the like.
Description
Technical Field
The invention relates to an alumina/lanthanide perovskite ceramic composite light absorber and a preparation method thereof, wherein the film-based structure has the characteristics of laser damage resistance, high-temperature thermal shock resistance and wide-spectrum high absorption, and can be applied to components in the field of photothermal conversion such as laser energy meters, laser power meters, thermal radiation detectors and the like.
Background
For the measurement of high-power laser, a thermopile type laser power meter/energy meter is mainly used, the test principle is that a light absorber in a probe absorbs light energy of incident laser to convert the light energy into heat energy, temperature gradient fields are formed at the center and two ends of the edge of the light absorber, thermoelectric materials in the probe generate thermoelectric electromotive force, and the magnitude of the electromotive force depends on the magnitude of the heat energy converted by the laser. Therefore, the light absorption performance, the laser damage resistance and the thermal shock resistance of the light absorber in the probe directly determine the response strength of a laser power meter/energy meter test and the power of the test laser wavelength, and are core components of the thermopile type laser power meter/energy meter detector.
At present, the light absorption materials (including thin films and blocks) of the thermopile type laser power meter/energy meter probe mainly include metal nano materials (such as gold black, silver black, iron black, and the like), carbon materials, sulfides, carbides, nitrides, optical glass, and the like. However, these materials have a narrow absorption wavelength range (mostly in the range of 0.2 to 2.5 μm) and oxygen-rich rings at high temperaturesEasily lose efficacy in the environment (more than or equal to 1000 ℃). Most of the light absorbing materials in high temperature oxygen-rich environment are metal oxides and composite oxide materials thereof, for example, the documents "Lu Y, et al high thermal radiation of Ca-doped lanthanum chloride, RSC Advances,2015, 30667" are prepared by solid phase reaction method, la-doped lanthanide chromate ceramic, la 30667 0.5 Ca 0.5 CrO 3 The light absorption performance of the solar cell is optimal, and the solar energy absorptivity reaches 95%. In the document He Zhiyong and the like, (Ca, fe) codoped lanthanum ceram has the near infrared absorption performance, reported in silicate science, 2016, 44. These documents are significantly different in both material and structure compared to the present application, e.g., lanthanum manganate is not used as the main material of the light absorber matrix, and the structure does not exhibit the characteristic of pore gradient, much less film-based structure.
Although some also employ LaMnO 3 As light-absorbing materials, there are described in the literature "Zhang PX, et al 3 thin film laser energy/power meter,Optics&Laser Technology,2004,36 1-x Ca x MnO 3 (x is more than or equal to 0.05 and less than or equal to 0.33) is deposited on LaAlO 3 Preparing La on the substrate 1-x Ca x MnO 3 The film acts as a light absorbing layer for the laser power meter and energy meter. Compared with the present application, la thereof 1-x Ca x MnO 3 Compared with the pore gradient lanthanide perovskite ceramic, the pore gradient lanthanide perovskite ceramic is a compact thin film, the existing form and the preparation method are obviously different, and no transition layer exists at the interface of a film-based structure. The document "Afifah N, et al, enhancement of phosphor to ultraviolet region by coupling Perovskite LaMnO 3 with TiO 2 nanoparticles, international Symposium on Current Progress in Functional Materials,2017,188 3 /TiO 2 LaMnO of mole ratio 3 /TiO 2 Nanocomposite material of effectively improvedThe material has absorptivity in ultraviolet region. Compared with the application, the LaMnO thereof 3 The ceramic is nano powder and a composite material, and compared with the pore gradient lanthanide perovskite ceramic, the ceramic has different material compositions, structures and preparation methods and does not have a film-based structure.
The damage of the laser to the optical thin film element is a main cause affecting the service life of the high-power laser optical thin film element, so that it is important to improve the laser damage resistance of the optical thin film. Generally speaking, the laser damage resistant material is mainly ceramic, especially oxide ceramic material, such as document "Li Zhaoyan, etc., the laser damage resistant capability research of the surface of engineering ceramic, the photonics report, 2017, 46. "research on zirconia (ZrO) 2 ) Alumina (Al) 2 O 3 ) Silicon nitride ceramics (Si) 3 N 4 ) Steatite porcelain (MgO/SiO) 2 ) The laser damage resistance of the 304 stainless steel (Fe/C/Cr) and 5052 aluminum alloy (Al/Mg/Cu) materials under nanosecond laser irradiation shows that the laser damage resistance threshold of the alumina ceramic is the highest. Therefore, an alumina material is selected as a thin film with a film-based structure resistant to laser damage. At present, al 2 O 3 The film preparation technology comprises physical vapor deposition, thermal evaporation deposition, magnetron sputtering, ion beam assisted deposition, pulse laser deposition, plasma arc plating, chemical vapor deposition, sol-gel, anodic oxidation and the like, for example, in the document' Liu Zhi super and the like, research on 1064nm laser damage characteristics of an ALD alumina single-layer film, optics is applied, 2011, 32 2 O 3 A film. Compared with the application, compact Al is not plated on the pore gradient lanthanide series perovskite ceramic substrate 2 O 3 The ceramic film has no transition layer at the film-substrate interface.
In summary, the above documents are compared with the present application, and besides the forms, materials and specific preparation methods existing in the light absorber for laser power meter/energy meter are different from those of the film-based structure of the present invention, the light absorber in the above documents does not exhibit a uniform gradient porous structure, nor is Al plating applied to the surface of the light absorber 2 O 3 And (3) a membrane. The application is due toIs designed and prepared to contain Al 2 O 3 The film, the pore gradient lanthanide perovskite ceramic body and the film-based structured light absorber of the intermediate transition layer have the comprehensive advantages of laser damage resistance, wide spectrum high absorption and high temperature thermal shock resistance.
Disclosure of Invention
The invention aims to solve the problems of narrow absorption range, low absorption rate, no laser damage resistance and poor high-temperature thermal shock resistance of the conventional laser power meter/energy meter light absorber, and aims to provide a film-based structure with high absorption, laser damage resistance and high-temperature thermal shock resistance in a spectral range of 0.3-14 mu m, an alumina/lanthanide perovskite ceramic composite light absorber and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following specific technical scheme that the aluminum oxide/lanthanide perovskite ceramic composite light absorber is characterized in that the base material of the light absorber is lanthanide perovskite ceramic material, and the first layer and the seventh layer are compact LaMnO 3 The second and sixth layers are network porous calcium-doped La 1-x Ca x MnO 3 Ceramic, third and fifth layers being network porous lithium doped La 1-y Li y MnO 3 The fourth layer is network porous calcium-doped La 1- z Ca z CrO 3 Ceramic with micron-sized macropores; the aperture of the fourth layer is the largest, the aperture of the third layer is centered with that of the fifth layer, the aperture of the second layer is the smallest, the thickness of each layer is 0.05-0.2mm, and the total thickness is 0.5-1mm; the film material of the light absorber is alumina ceramics, and the thickness is 50-200nm.
The preparation method of the light absorber comprises the following steps:
(1) Synthesizing lanthanide perovskite ceramic powder with wide spectrum and high absorption by a solid phase method: lanthanum oxide, manganese oxide, calcium carbonate, lithium carbonate and chromium oxide are respectively added according to LaMnO 3 、La 1-x Ca x MnO 3 、La 1-y Li y MnO 3 And La 1-z Ca z CrO 3 The stoichiometric ratio (x is more than or equal to 0.3 and less than or equal to 0.7,0.3 and less than or equal to y is more than or equal to 0.7,0.3 and less than or equal to z is less than or equal to 0.7) is mixed and then solid phase sintering is carried out (sintering temperatureThe temperature is 1000-1200 ℃, the heating rate is 5 ℃/min, the heat preservation time is 2-5 h), ball milling is carried out for 24-48 h at the speed of 300 r/min and the ball material weight ratio of 3:1, and lanthanum manganate, calcium-doped lanthanum manganate, lithium-doped lanthanum manganate and calcium-doped lanthanum chromate powder are respectively obtained after ball milling and sieving; the lanthanide perovskite ceramic used for the light absorber is prepared in the solid-phase synthesis process.
(2) Preparing a pore gradient seven-layer structure lanthanide perovskite ceramic substrate: uniformly mixing the four kinds of powder with a polyvinyl alcohol solution, and sieving the mixture through a 200-mesh sieve to obtain granulated powder; wherein the weight ratio of polyvinyl alcohol to polyvinyl alcohol solution in the polyvinyl alcohol solution is 5-10%, and the weight ratio of polyvinyl alcohol solution to ceramic powder is 8-10%; then evenly spreading the granulated powder on the surface of the substrateIn the hot press mold of (1), the first and seventh layers are LaMnO 3 The second and sixth layers are La 1-x Ca x MnO 3 The third and fifth layers are La 1-y Li y MnO 3 The fourth layer is La 1-z Ca z CrO 3 Wherein the weight of the powder of each layer is between 0.2 and 0.8g, and the green body is obtained by keeping the pressure for 5 to 10min under the mould pressing of 10 to 15 Mpa; sintering at 1400-1500 ℃ and 10-20 kPa for 2-4 h under the argon environment to obtain a pore gradient lanthanide perovskite ceramic substrate with a compact surface layer and a porous middle layer, wherein the thickness of each layer is 0.05-0.2mm, and the total thickness is 0.5-1mm;
(3) Plating compact Al 2 O 3 Film formation: plating Al with the thickness of 50-200nm on the surface of the gradient ceramic by adopting the vacuum evaporation, pulsed laser deposition, atomic layer deposition or magnetron sputtering technology 2 O 3 A film;
(4) Heat treatment in an air furnace: and (3) placing the film-substrate structure in an air furnace, and preserving the heat for 5-30 min at 500-1000 ℃ to generate a transition layer at the interface of the film substrate.
Compared with the current laser power meter/energy meter light absorber, the invention has the advantages that (1) the compact lanthanum manganate ceramic is adopted as the substrate with the film-based structureThe outermost layer of the material can realize compact Al on the surface 2 O 3 The film is plated, and simultaneously has excellent broad-spectrum light absorption performance and high temperature resistance; (2) Because the gradient porous lanthanide perovskite ceramic is used as the middle layer of the substrate material of the membrane-based structure, the membrane-based structure has excellent high-temperature thermal shock resistance; the excellent thermal shock resistance is attributed to the network porous structure and the gradient transition layer formed between the substrates. The increase of the porosity can reduce the elastic modulus of the material, and meanwhile, the thermal residual stress can be released through the holes in the cooling process; on the other hand, the gradient transition layer can eliminate the mutation of the thermal expansion coefficient and the thermal conductivity of each interface of the base material, thereby improving the high-temperature thermal shock resistance; (3) Because the surface of the film-based structure is plated with compact Al with the thickness of 50-200nm 2 O 3 The film can obviously improve the laser damage resistance of the base material.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention.
FIG. 1 is a schematic cross-sectional view of a film-based structured light absorber according to the present invention.
FIG. 2 shows a first and a seventh layer LaMnO according to the present invention 3 Scanning electron micrographs.
FIG. 3 shows a second and sixth layer La according to the present invention 0.5 Ca 0.5 MnO 3 Scanning electron micrographs.
FIG. 4 shows a third and a fifth layer La according to the present invention 0.5 Li 0.5 MnO 3 Scanning electron micrographs.
FIG. 5 shows a fourth layer La according to the present invention 0.5 Ca 0.5 CrO 3 Scanning electron micrographs.
FIG. 6 shows LaMnO according to the present invention 3 The light absorption of the sample is in the range of 0.3 to 14 μm.
Detailed Description
To further illustrate the technical solution and the features of the present invention, the following figures 1, 2, 3, 4, 5 and typical figures are combinedThe invention provides a film-based structure for a laser power meter/energy meter and a preparation method thereof, which comprises the following steps of (1) synthesizing lanthanide perovskite ceramic powder with broad spectrum and high absorption by a solid phase method; (2) Preparing a pore gradient seven-layer structure lanthanide perovskite ceramic substrate; (3) Plating compact Al 2 O 3 A film; and (4) carrying out heat treatment in an air furnace. It should be noted that the specific embodiments described herein are only for explaining the present invention and are not used for limiting the present invention.
The detailed case is described as follows:
example 1:
(1) Firstly, lanthanide perovskite ceramic powder with wide spectrum and high absorption is synthesized by a solid phase method. Lanthanum oxide, manganese oxide, calcium carbonate, lithium carbonate and chromium oxide powder are respectively mixed according to LaMnO 3 、La 0.5 Ca 0.5 MnO 3 、La 0.5 Li 0.5 MnO 3 And La 0.5 Ca 0.5 CrO 3 Mixing the materials according to the stoichiometric ratio, performing solid phase sintering (the sintering temperature is 1100 ℃, the heating rate is 5 ℃/min, the heat preservation time is 3 h), performing ball milling for 48h at the speed of 300 r/min, and sieving to obtain lanthanum manganate and La respectively 0.5 Ca 0.5 MnO 3 、La 0.5 Li 0.5 MnO 3 And La 0.5 Ca 0.5 CrO 3 A ceramic powder;
(2) Secondly, preparing the lanthanide perovskite ceramic substrate with the pore gradient seven-layer structure. Uniformly mixing the four kinds of powder with a polyvinyl alcohol solution, and sieving the mixture through a 200-mesh sieve to obtain granulated powder; wherein the weight ratio of polyvinyl alcohol to polyvinyl alcohol solution in the polyvinyl alcohol solution is 6%, and the weight ratio of polyvinyl alcohol solution to ceramic powder is 9%; then the granulated powder is put in turn (first and seventh layers are LaMnO) 3 The second and sixth layers are La 0.5 Ca 0.5 MnO 3 The third and fifth layers are La 0.5 Li 0.5 MnO 3 The fourth layer is La 0.5 Ca 0.5 CrO 3 ) Is evenly spread onIn the hot press mold of (1), wherein the first and seventh layers of LaMnO 3 Powder 0.2g, second and sixth layer La 0.5 Ca 0.5 MnO 3 Powder 0.2g, third and fifth layer La 0.5 Li 0.5 MnO 3 Powder 0.2g, fourth layer La 0.5 Ca 0.5 CrO 3 0.8g of powder, and keeping the pressure for 9min under the mould pressing of 12MPa to obtain a green body; sintering at 1450 deg.C and 15kPa for 3h in argon atmosphere to obtain dense-surface-layer and porous-middle-layer gradient La-series perovskite ceramic with first and seventh layers of 0.05mm thick and dense LaMnO 3 (see FIG. 2), the second and sixth layers were 0.05mm thick, smaller pore La 0.5 Ca 0.5 MnO 3 (see FIG. 3), the third and fifth layers were 0.05mm thick mesoporous La 0.5 Li 0.5 MnO 3 (see FIG. 4), the fourth layer is 0.2mm thick, larger pore La 0.5 Ca 0.5 CrO 3 (see FIG. 5);
(3) Then, plating compact Al on the surface of the pore gradient ceramic 2 O 3 And (3) a membrane. Plating Al with thickness of 200nm on the surface of the pore gradient ceramic by adopting a vacuum evaporation technology 2 O 3 A film;
(4) Finally, the film-based structure is heat-treated in an air furnace. And (3) placing the membrane-based structure in an air furnace, and preserving the heat for 20min at 600 ℃ to obtain the alumina/pore gradient lanthanide perovskite ceramic composite light absorber containing the interface transition layer, wherein the schematic diagram is shown in figure 1.
Example 2:
(1) Firstly, lanthanide perovskite ceramic powder with wide spectrum and high absorption is synthesized by a solid phase method. Lanthanum oxide, manganese oxide, calcium carbonate, lithium carbonate and chromium oxide powder are respectively mixed according to LaMnO 3 、La 0.6 Ca 0.4 MnO 3 、La 0.6 Li 0.4 MnO 3 And La 0.6 Ca 0.4 CrO 3 Mixing the materials according to the stoichiometric ratio, performing solid phase sintering (the sintering temperature is 1100 ℃, the heating speed is 5 ℃/min, the heat preservation time is 4 h), performing ball milling for 24h at the speed of 300 r/min, and sieving to obtain lanthanum manganate and La respectively 0.6 Ca 0.4 MnO 3 、La 0.6 Li 0.4 MnO 3 And La 0.6 Ca 0.4 CrO 3 A ceramic powder;
(2) Secondly, preparing the pore gradient seven-layer structure lanthanide perovskite ceramic substrate. Uniformly mixing the four kinds of powder with a polyvinyl alcohol solution, and sieving the mixture through a 200-mesh sieve to obtain granulated powder; wherein the weight ratio of polyvinyl alcohol to polyvinyl alcohol solution in the polyvinyl alcohol solution is 5%, and the weight ratio of polyvinyl alcohol solution to ceramic powder is 8%; then the granulated powder is put in turn (first and seventh layers are LaMnO) 3 The second and sixth layers are La 0.6 Ca 0.4 MnO 3 The third and fifth layers are La 0.6 Li 0.4 MnO 3 The fourth layer is La 0.6 Ca 0.4 CrO 3 ) Is evenly spread onIn the hot press mold of (1), wherein the first and seventh layers of LaMnO 3 Powder 0.2g, second and sixth layer La 0.5 Ca 0.5 MnO 3 Powder 0.4g, third and fifth layer La 0.5 Li 0.5 MnO 3 Powder 0.4g, fourth layer La 0.5 Ca 0.5 CrO 3 0.8g of powder, and keeping the pressure for 10min under the mould pressing of 10MPa to obtain a green body; sintering at 1400 deg.C under argon atmosphere and 20kPa for 4h to obtain a porous gradient perovskite ceramic body with a compact surface layer and a porous middle layer, wherein the first and seventh layers are compact LaMnO layers with a thickness of 0.05mm 3 The second and sixth layers were 0.1mm thick, smaller pore La 0.6 Ca 0.4 MnO 3 The third and fifth layers are 0.1mm thick mesoporous La 0.6 Li 0.4 MnO 3 The fourth layer is La with the thickness of 0.2mm and larger holes 0.6 Ca 0.4 CrO 3 ;
(3) Then, plating compact Al on the surface of the pore gradient ceramic 2 O 3 And (3) a membrane. Plating 50nm thick Al on the surface of the pore gradient ceramic by adopting a pulse laser deposition technology 2 O 3 A film;
(4) Finally, the film-based structure is heat-treated in an air furnace. And (3) placing the membrane-based structure in an air furnace, and preserving the heat for 30min at 500 ℃ to obtain the alumina/pore gradient lanthanide perovskite ceramic composite light absorber containing the interface transition layer, wherein the schematic diagram is shown in figure 1.
Example 3:
(1) Firstly, lanthanide perovskite ceramic powder with wide spectrum and high absorption is synthesized by a solid phase method. Lanthanum oxide, manganese oxide, calcium carbonate, lithium carbonate and chromium oxide powder are respectively mixed according to LaMnO 3 、La 0.7 Ca 0.3 MnO 3 、La 0.7 Li 0.3 MnO 3 And La 0.7 Ca 0.3 CrO 3 Mixing the materials according to the stoichiometric ratio, performing solid phase sintering (sintering temperature is 1000 ℃, heating rate is 5 ℃/min, heat preservation time is 5 h), performing ball milling at the speed of 300 r/min for 36h, and sieving to obtain lanthanum manganate and La respectively 0.7 Ca 0.3 MnO 3 、La 0.7 Li 0.3 MnO 3 And La 0.7 Ca 0.3 CrO 3 A ceramic powder;
(2) Secondly, preparing the pore gradient seven-layer structure lanthanide perovskite ceramic substrate. Uniformly mixing the four kinds of powder with a polyvinyl alcohol solution, and sieving the mixture through a 200-mesh sieve to obtain granulated powder; wherein the weight ratio of polyvinyl alcohol to polyvinyl alcohol solution in the polyvinyl alcohol solution is 7%, and the weight ratio of polyvinyl alcohol solution to ceramic powder is 9%; then the granulated powder is put in turn (the first and seventh layers are LaMnO) 3 The second and sixth layers are La 0.7 Ca 0.3 MnO 3 The third and fifth layers are La 0.7 Li 0.3 MnO 3 The fourth layer is La 0.7 Ca 0.3 CrO 3 ) Is uniformly laid onIn the hot press mold of (1), wherein the first and seventh layers of LaMnO 3 Powder 0.4g, second and sixth layer La 0.5 Ca 0.5 MnO 3 Powder 0.4g, third and fifth layer La 0.5 Li 0.5 MnO 3 Powder 0.4g, fourth layer La 0.5 Ca 0.5 CrO 3 0.8g of powder, and keeping the pressure for 7min under the mould pressing of 13MPa to obtain a green body; then in an argon environmentSintering at 1500 deg.C under 10kPa for 2h to obtain a porous gradient perovskite ceramic body with compact surface layer and porous middle layer, wherein the first and seventh layers are compact LaMnO layer with thickness of 0.1mm 3 The second and sixth layers were 0.1mm thick, smaller pore La 0.7 Ca 0.3 MnO 3 The third and fifth layers are 0.1mm thick mesoporous La 0.7 Li 0.3 MnO 3 The fourth layer is 0.2mm thick, and the larger hole is La 0.7 Ca 0.3 CrO 3 ;
(3) Then, plating compact Al on the surface of the pore gradient ceramic 2 O 3 And (3) a film. Plating Al with the thickness of 150nm on the surface of the pore gradient ceramic by adopting an atomic layer deposition technology 2 O 3 A film;
(4) Finally, the film-based structure is heat-treated in an air furnace. Placing the membrane substrate structure in an air furnace, and preserving heat at 700 ℃ for 10min to obtain the alumina/pore gradient lanthanide series perovskite ceramic composite light absorber containing the interface transition layer, wherein each LaMnO is 3 The thickness of the base ceramic layer was 0.12mm, as schematically shown in FIG. 1.
Example 4:
(1) Firstly, lanthanide perovskite ceramic powder with wide spectrum and high absorption is synthesized by a solid phase method. Lanthanum oxide, manganese oxide, calcium carbonate, lithium carbonate and chromium oxide powder are respectively mixed according to LaMnO 3 、La 0.3 Ca 0.7 MnO 3 、La 0.3 Li 0.7 MnO 3 And La 0.3 Ca 0.7 CrO 3 Mixing the materials according to the stoichiometric ratio, performing solid phase sintering (the sintering temperature is 1200 ℃, the heating rate is 5 ℃/min, the heat preservation time is 2 h), performing ball milling at the speed of 300 r/min for 36h, and sieving to respectively obtain lanthanum manganate and La 0.3 Ca 0.7 MnO 3 、La 0.3 Li 0.7 MnO 3 And La 0.3 Ca 0.7 CrO 3 A ceramic powder;
(2) Secondly, preparing the pore gradient seven-layer structure lanthanide perovskite ceramic substrate. Uniformly mixing the four kinds of powder with a polyvinyl alcohol solution, and sieving the mixture through a 200-mesh sieve to obtain granulated powder; wherein the weight of the polyvinyl alcohol and the polyvinyl alcohol solution in the polyvinyl alcohol solutionThe weight ratio of the polyvinyl alcohol solution to the ceramic powder is 10 percent; then the granulated powder is put in turn (first and seventh layers are LaMnO) 3 The second and sixth layers are La 0.3 Ca 0.7 MnO 3 The third and fifth layers are La 0.3 Li 0.7 MnO 3 The fourth layer is La 0.3 Ca 0.7 CrO 3 ) Is evenly spread onIn the hot press mold of (1), wherein the first and seventh layers of LaMnO 3 Powder 0.4g, second and sixth layer La 0.5 Ca 0.5 MnO 3 Powder 0.4g, third and fifth layer La 0.5 Li 0.5 MnO 3 Powder 0.8g, fourth layer La 0.5 Ca 0.5 CrO 3 0.8g of powder, and keeping the pressure for 5min under the mould pressing of 15MPa to obtain a green body; sintering at 1500 deg.C under argon atmosphere and 15kPa for 2h to obtain compact/porous alumina/lanthanum manganate film-based light absorber with surface layer, wherein the first and seventh layers are compact LaMnO layer with thickness of 0.1mm 3 The second and sixth layers were 0.1mm thick, smaller pore La 0.3 Ca 0.7 MnO 3 The third and fifth layers are 0.2mm thick mesoporous La 0.3 Li 0.7 MnO 3 The fourth layer is La with the thickness of 0.2mm and larger holes 0.3 Ca 0.7 CrO 3 (ii) a Its LaMnO 3 The optical absorption of the ceramic in the range of 0.3 to 14 μm is shown in FIG. 6;
(3) Then, plating compact Al on the surface of the pore gradient ceramic 2 O 3 And (3) a membrane. Plating Al with the thickness of 200nm on the surface of the pore gradient ceramic by adopting a magnetron sputtering technology 2 O 3 A film;
(4) Finally, the film-based structure is heat-treated in an air furnace. And (3) placing the membrane-based structure in an air furnace, and preserving the heat for 5min at 1000 ℃ to obtain the alumina/pore gradient lanthanide perovskite ceramic composite light absorber containing the interface transition layer, wherein the schematic diagram is shown in figure 1.
The above description is only a part of exemplary embodiments of the present invention, and not intended to limit the present invention, and any modifications, variations and equivalent element changes made on the above embodiments according to the process substance of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (8)
1. The aluminum oxide/lanthanide perovskite ceramic composite light absorber is characterized in that the base material of the light absorber is lanthanide perovskite ceramic material, and the first layer and the seventh layer are compact LaMnO 3 The second and sixth layers are network porous calcium-doped La 1-x Ca x MnO 3 Ceramic, third and fifth layers being network porous lithium doped La 1-y Li y MnO 3 The fourth layer is network porous calcium-doped La 1-z Ca z CrO 3 Ceramic with micron-sized macropores; the aperture of the fourth layer is the largest, the aperture of the third layer is in the middle, the aperture of the sixth layer is the smallest, the thickness of each layer is 0.05-0.2mm, and the total thickness is 0.5-1mm; the film material of the light absorber is alumina ceramics, and the thickness is 50-200nm.
2. The alumina/lanthanide perovskite ceramic composite light absorber of claim 1, wherein the calcium is doped with La 1-x Ca x MnO 3 The doping amount x of Ca in the ceramic is 0.3-0.7, and the Li is doped with La 1-y Li y MnO 3 The Li doping amount y in the ceramic is 0.3-0.7, and the calcium is doped with La 1-z Ca z CrO 3 The doping amount z of Ca in the ceramic is 0.3-0.7.
3. The alumina/lanthanide perovskite ceramic composite light absorber as claimed in claim 1, wherein a nano-transition layer is formed between the alumina film layer of the light absorber and the lanthanide perovskite ceramic interface.
4. The preparation method of the alumina/lanthanide perovskite ceramic composite light absorber as claimed in claim 1, which is characterized by comprising the following steps:
(1) Solid phase method for synthesizing lanthanide perovskite ceramic with wide spectrum and high absorptionCeramic powder: mixing lanthanum oxide, manganese oxide, calcium carbonate, lithium carbonate and chromium oxide powder according to a stoichiometric ratio respectively, performing solid-phase sintering, ball-milling and sieving to obtain lanthanum manganate and calcium-doped lanthanum manganate La 1-x Ca x MnO 3 Lithium-doped lanthanum manganate La 1-y Li y MnO 3 And calcium-doped lanthanum chromate La 1-z Ca z CrO 3 Powder;
(2) Preparing a pore gradient seven-layer structure lanthanide perovskite ceramic substrate: uniformly mixing the powder with a polyvinyl alcohol solution respectively, and screening the mixture by using a screen to obtain granulated powder; then evenly paving the granulated powder in a hot-pressing mould according to the above steps, and obtaining a green body under a certain mould pressing condition; sintering at high temperature in an argon environment to obtain a pore gradient lanthanide perovskite ceramic body with a compact surface layer and a porous middle part;
(3) Plating compact Al 2 O 3 Film preparation: plating Al on the surface of the pore gradient ceramic by adopting a film plating technology 2 O 3 A film;
(4) Heat treatment in an air furnace produces a transition layer at the film-substrate interface.
5. The method for preparing the alumina/lanthanide perovskite ceramic composite light absorber as claimed in claim 4, wherein in the step (1), the solid phase sintering process comprises: the sintering temperature is 1000-1200 ℃, the heating rate is 5 ℃/min, and the heat preservation time is 2-5 h; ball milling is carried out for 24-48 h at the speed of 300 r/min, and the weight ratio of the ball material is 3:1.
6. The method for preparing the alumina/lanthanide perovskite ceramic composite light absorber as claimed in claim 4, wherein in the step (2), the sieving refers to 200 mesh sieving, the weight ratio of polyvinyl alcohol to polyvinyl alcohol solution in the polyvinyl alcohol solution is 5-10%, and the weight ratio of polyvinyl alcohol solution to ceramic powder is 8-10%; the diameter of the hot pressing die isThe molding conditions were: pressure of 10-15 MPa, keeping the pressure for 5-10 min; sintering for 2-4 h at 1400-1500 ℃ and 10-20 kPa under argon atmosphere.
7. The method for preparing the alumina/lanthanide perovskite ceramic composite light absorber as claimed in claim 4, wherein in the step (3), al is added 2 O 3 The thickness of the film is 50-200nm, and the coating technology is one of vacuum evaporation, pulsed laser deposition, atomic layer deposition and magnetron sputtering technology.
8. The method for preparing the alumina/lanthanide perovskite ceramic composite light absorber as claimed in claim 4, wherein the heat treatment process parameters are as follows: keeping the temperature for 5-30 min at 500-1000 ℃.
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