CN115626825B - Alumina/lanthanide perovskite ceramic composite light absorber and preparation method thereof - Google Patents

Alumina/lanthanide perovskite ceramic composite light absorber and preparation method thereof Download PDF

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CN115626825B
CN115626825B CN202211404900.3A CN202211404900A CN115626825B CN 115626825 B CN115626825 B CN 115626825B CN 202211404900 A CN202211404900 A CN 202211404900A CN 115626825 B CN115626825 B CN 115626825B
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light absorber
alumina
lanthanide
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CN115626825A (en
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于刘旭
刘桂武
乔冠军
张相召
侯海港
刘军林
杨建�
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Jiangsu University
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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 wide spectrum and high absorption by solid phase method; (2) Preparing a lanthanide perovskite ceramic substrate with a pore gradient seven-layer structure; (3) Plating compact Al 2 O 3 A membrane; (4) heat treatment in an air furnace. Wherein the surface layer of the lanthanide perovskite ceramic substrate is compact, and distributed in a gradient manner from outside to inside, and a transition layer exists at the interface of the membrane-based structure. The preparation method has simple process and low cost, and the light 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 value, and can be widely applied to components in the high-temperature photo-thermal conversion fields of laser energy meters, laser power meters and the like.

Description

Alumina/lanthanide perovskite ceramic composite light absorber and preparation method thereof
Technical Field
The invention relates to an alumina/lanthanide perovskite ceramic composite light absorber and a preparation method thereof, and 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 photo-thermal 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 testing principle is mainly that a light absorber in a probe is used for absorbing light energy of incident laser to convert the light energy into heat energy, temperature gradient fields are formed at the center and the 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 the laser power meter/energy meter test and the power of the tested laser wavelength, and the probe is a core component of the thermopile type laser power meter/energy meter detector.
Currently, the light absorbing materials (including films and blocks) of thermopile type laser power meter/energy meter probes mainly include metal nanomaterials (such as gold black, silver black, iron black, etc.), carbon materials, sulfides, carbides, nitrides, optical glasses, etc. However, these materials have a narrow absorption wavelength range (mostly in the range of 0.2-2.5 μm) and are prone to failure in high temperature oxygen-rich environments (. Gtoreq.1000 ℃). The light absorbing materials are mostly metal oxides and composite oxide materials thereof under the high-temperature oxygen-enriched environment, for example, document Lu Y, et al high thermal radiation of Ca-doped lanthanum chromite, RSC Advances,2015, 5:3067, the calcium doped lanthanum chromate series ceramics are prepared by a solid phase reaction method, la 0.5 Ca 0.5 CrO 3 Is optimal in light absorption performance, whichThe solar absorptivity reaches 95%. Document He Zhiyong, et al, (Ca, fe) co-doped lanthanum cerium oxide ceramic has near infrared absorption property, silicate theory, 2016, 44:387-391. Compared with the application, the materials and the structures of the documents are significantly different, for example, lanthanum manganate is not adopted as the main material of the light absorber matrix, and the structures of the documents do not show pore gradient characteristics and do not have a film base structure.
Although some people also use LaMnO 3 As light-absorbing materials, there are mentioned, for example, the literature "Zhang PX, et al LaCaMnO 3 thin film laser energy/power meter,Optics&Laser Technology,2004,36:341-343, "La was deposited using pulsed Laser deposition 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 La is prepared on the substrate 1-x Ca x MnO 3 The film acts as a light absorbing layer for the laser power meter and the energy meter. In comparison with the present application, la of 1-x Ca x MnO 3 The porous gradient lanthanide perovskite ceramic is a compact film, and has obviously different existence forms and preparation methods compared with the porous gradient lanthanide perovskite ceramic, and no transition layer is arranged at the interface of a film base structure. Document "Afifah N, et al enhancement of photoresponse to ultraviolet region by coupling perovskite LaMnO 3 with TiO 2 nanomarticles, international Symposium on Current Progress in Functional Materials,2017, 188:01060, "different LaMnOs were prepared by sol-gel method @ 3 /TiO 2 Molar ratio of LaMnO 3 /TiO 2 The nano composite material effectively improves the absorptivity of the material in the ultraviolet light region. Compared with the present application, laMnO thereof 3 Compared with the porous gradient lanthanide perovskite ceramic, the nano powder is a composite material, and has different material composition, structure and preparation method, and no membrane-based structure.
The damage of laser to optical thin film element affects the service life of high power laser optical thin film elementFor the main reasons of life, it is important to improve the laser damage resistance of the optical film. Generally, the laser damage resistant material is mainly ceramic, particularly oxide ceramic material, such as document Li Zhaoyan, etc., and the engineering ceramic surface has laser damage resistance, photonics report, 2017, 46:1014003. "study zirconia (ZrO 2 ) Alumina (Al) 2 O 3 ) Silicon nitride ceramics (Si 3 N 4 ) Talc porcelain (MgO/SiO) 2 ) The laser damage resistance of the materials of the stainless steel (Fe/C/Cr) and the aluminum alloy (Al/Mg/Cu) 5052 under nanosecond laser irradiation shows that the laser damage resistance threshold of the alumina ceramic is highest. Therefore, the alumina material is selected as the film with the film base structure resistant to laser damage. At present, al 2 O 3 The thin 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, such as document Liu Zhi superb, ALD alumina single-layer film 1064nm laser damage characteristic research, application optics, 2011, 32:373-376, and 50nm thick Al is plated on fused quartz and BK7 substrates by adopting atomic layer deposition technology 2 O 3 A film. In contrast to the present application, no dense Al was plated on pore gradient lanthanide perovskite ceramic substrates 2 O 3 Ceramic thin films, and the film-based interface also has no transition layer.
In summary, the above-mentioned documents, in comparison with the present application, do not show a uniform gradient porous structure nor use Al plating on the surface of the light absorber, except that the form, material and specific preparation method of the light absorber present in the laser power meter/energy meter are different from those of the film-based structure of the present invention 2 O 3 And (3) a film. The application prepares the alloy containing Al due to design 2 O 3 The film, the porous gradient lanthanide perovskite ceramic body and the film-based structure 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 at solving the problems of narrow absorption range, low absorption rate, no laser damage resistance and poor high-temperature thermal shock resistance of the existing 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 the spectrum range of 0.3-14 mu m, an alumina/lanthanide perovskite ceramic composite light absorber and a preparation method thereof.
The invention is realized by adopting the following specific technical scheme, and is characterized in that the matrix material of the light absorber is lanthanide perovskite ceramic material, and the first and seventh layers are compact LaMnO 3 Ceramic, the second and sixth layers are porous and calcium doped La 1-x Ca x MnO 3 Ceramic, third and fifth layers are porous in network and doped with La 1-y Li y MnO 3 Ceramic, the fourth layer is porous network and doped with La 1- z Ca z CrO 3 Ceramic, wherein the holes are micron-sized macropores; the aperture of the fourth layer is the largest, the aperture of the third and fifth layers is centered, the aperture of the second and sixth layers 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 ceramic, 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 prepared according to LaMnO 3 、La 1-x Ca x MnO 3 、La 1-y Li y MnO 3 La and La 1-z Ca z CrO 3 Mixing materials according to the stoichiometric ratio (x is more than or equal to 0.3 and less than or equal to 0.7,0.3, y is more than or equal to 0.7,0.3 and z is less than or equal to 0.7), performing solid-phase sintering (the sintering temperature is 1000-1200 ℃, the heating speed is 5 ℃/min, the heat preservation time is 2-5 h), performing ball milling at the speed of 300 revolutions per minute and the ball material weight ratio of 3:1 for 24-48 h, and sieving after ball milling to obtain lanthanum manganate, calcium-doped lanthanum manganate, lithium-doped lanthanum manganate and calcium-doped lanthanum chromate powder respectively; the lanthanide perovskite ceramic for the light absorber is innovated in the solid-phase synthesis.
(2) Preparation of holesA lanthanide perovskite ceramic substrate with a gap gradient seven-layer structure: uniformly mixing the four powders with a polyvinyl alcohol solution, and sieving the mixture with a 200-mesh sieve to obtain granulated powder; wherein the weight ratio of the polyvinyl alcohol to the polyvinyl alcohol solution in the polyvinyl alcohol solution is 5-10%, and the weight ratio of the polyvinyl alcohol solution to the ceramic powder is 8-10%; then the granulated powder is evenly spread on the surface of the substrate
Figure BDA0003936607000000031
In the hot press mold of (2), 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 pressure is maintained for 5 to 10 minutes under the mould pressing of 10 to 15Mpa to obtain a green body; sintering for 2-4 hours at the high temperature of 1400-1500 ℃ and the pressure of 10-20 kPa in an argon environment to obtain the porous gradient lanthanide perovskite ceramic substrate with compact surface layer and porous middle, 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: adopting vacuum evaporation, pulse laser deposition, atomic layer deposition or magnetron sputtering technology to plate Al with thickness of 50-200nm on the surface of the gradient ceramic 2 O 3 A membrane;
(4) Heat treatment in an air furnace: the membrane base structure is placed in an air furnace, and a transition layer is generated at the interface of the membrane base after heat preservation for 5-30 min at 500-1000 ℃.
Compared with the current laser power meter/energy meter light absorber, the invention has the beneficial effects that (1) as the compact lanthanum manganate ceramic is adopted as the outermost layer of the film-based structure matrix material, compact Al can be realized on the surface of the compact lanthanum manganate ceramic 2 O 3 The film is plated, and simultaneously has excellent broad spectrum light absorption performance and high temperature resistance; (2) As the gradient porous lanthanide perovskite ceramic is adopted as the intermediate layer of the membrane-based structure matrix material, the membrane-based structure has excellent high-temperature thermal shock resistance; the excellent thermal shock resistance is attributed to the network of porous structures formed between the substrates anda gradient transition layer. 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 abrupt change of the thermal expansion coefficient and the thermal conductivity of each layer 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 matrix material.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain 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 LaMnO layers according to the present invention 3 Scanning electron microscope pictures.
FIG. 3 shows a second, six-layer La of the present invention 0.5 Ca 0.5 MnO 3 Scanning electron microscope pictures.
FIG. 4 shows a third and fifth layer La of the present invention 0.5 Li 0.5 MnO 3 Scanning electron microscope pictures.
FIG. 5 shows a fourth layer La of the present invention 0.5 Ca 0.5 CrO 3 Scanning electron microscope pictures.
FIG. 6 shows LaMnO according to the present invention 3 The sample has a light absorptivity in the range of 0.3 to 14. Mu.m.
Detailed Description
In order to further explain the technical scheme and the characteristics of the invention, the following is a film-based structure for a laser power meter/energy meter and a preparation method thereof according to the invention, which are provided by the invention, with reference to figures 1, 2, 3, 4, 5 and typical embodiments, wherein the preparation steps comprise (1) synthesizing lanthanide perovskite ceramic powder with wide spectrum and high absorption by a solid phase method; (2) Preparing a lanthanide perovskite ceramic substrate with a pore gradient seven-layer structure; (3) Plating compact Al 2 O 3 A membrane; (4) heat treatment in an air furnace. Notably, theThe specific embodiments described herein are, however, to be construed as merely illustrative, and not a limitation of the present invention.
The detailed case is described as follows:
example 1:
(1) Firstly, synthesizing lanthanide perovskite ceramic powder with wide spectrum and high absorption by a solid phase method. Respectively mixing lanthanum oxide, manganese oxide, calcium carbonate, lithium carbonate and chromium oxide powder according to LaMnO 3 、La 0.5 Ca 0.5 MnO 3 、La 0.5 Li 0.5 MnO 3 And La (La) 0.5 Ca 0.5 CrO 3 Mixing materials according to stoichiometric ratio, solid-phase sintering (sintering temperature is 1100 ℃, heating speed is 5 ℃/min, heat preservation time is 3 h), ball milling at 300 rpm for 48h, 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 (La) 0.5 Ca 0.5 CrO 3 Ceramic powder;
(2) Secondly, preparing the lanthanide perovskite ceramic substrate with the pore gradient seven-layer structure. Uniformly mixing the four powders with a polyvinyl alcohol solution, and sieving the mixture with a 200-mesh sieve to obtain granulated powder; wherein the weight ratio of the polyvinyl alcohol to the polyvinyl alcohol solution in the polyvinyl alcohol solution is 6 percent, and the weight ratio of the polyvinyl alcohol solution to the ceramic powder is 9 percent; the granulated powder was then sequentially (LaMnO for the first and seventh layers 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 ) Uniformly spread on
Figure BDA0003936607000000051
Wherein the first and seventh layers of LaMnO 3 0.2g of powder, second and sixth layer La 0.5 Ca 0.5 MnO 3 0.2g of powder, third and fifth layers La 0.5 Li 0.5 MnO 3 0.2g of powder, fourth layer La 0.5 Ca 0.5 CrO 3 0.8g of powder, and maintaining the pressure for 9min under the die pressing of 12MPa to obtain a green body; then in argon ringSintering for 3h at 1450 ℃ and 15kPa to obtain the porous gradient lanthanide perovskite ceramic with compact surface layer and porous middle, wherein the first and seventh layers are LaMnO with thickness of 0.05mm 3 (FIG. 2), the second and sixth layers are La with a thickness of 0.05mm and smaller pores 0.5 Ca 0.5 MnO 3 (FIG. 3), the third and fifth layers are 0.05mm thick, mesoporous La 0.5 Li 0.5 MnO 3 (FIG. 4), the fourth layer is La with a thickness of 0.2mm and larger pores 0.5 Ca 0.5 CrO 3 (as in fig. 5);
(3) Then plating dense Al on the surface of the porous gradient ceramic 2 O 3 And (3) a film. Plating Al with thickness of 200nm on the surface of the pore gradient ceramic by adopting a vacuum evaporation technology 2 O 3 A membrane;
(4) Finally, the film-based structure is heat treated in an air oven. The membrane-based structure is placed in an air furnace, and the temperature is kept at 600 ℃ for 20min, so that the alumina/pore gradient lanthanide perovskite ceramic composite light absorber containing the interface transition layer is obtained, and the schematic diagram is shown in figure 1.
Example 2:
(1) Firstly, synthesizing lanthanide perovskite ceramic powder with wide spectrum and high absorption by a solid phase method. Respectively mixing lanthanum oxide, manganese oxide, calcium carbonate, lithium carbonate and chromium oxide powder according to LaMnO 3 、La 0.6 Ca 0.4 MnO 3 、La 0.6 Li 0.4 MnO 3 And La (La) 0.6 Ca 0.4 CrO 3 Mixing materials according to stoichiometric ratio, solid-phase sintering (sintering temperature is 1100 ℃, heating speed is 5 ℃/min, heat preservation time is 4 h), ball milling at 300 rpm for 24h, 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 (La) 0.6 Ca 0.4 CrO 3 Ceramic powder;
(2) Secondly, preparing the lanthanide perovskite ceramic substrate with the pore gradient seven-layer structure. Uniformly mixing the four powders with a polyvinyl alcohol solution, and sieving the mixture with a 200-mesh sieve to obtain granulated powder; wherein the weight ratio of the polyvinyl alcohol in the polyvinyl alcohol solution to the polyvinyl alcohol solution is 5 percentThe weight ratio of the polyvinyl alcohol solution to the ceramic powder is 8%; the granulated powder was then sequentially (LaMnO for the first and seventh layers 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 ) Uniformly spread on
Figure BDA0003936607000000061
Wherein the first and seventh layers of LaMnO 3 0.2g of powder, second and sixth layer La 0.5 Ca 0.5 MnO 3 0.4g of powder, third and fifth layers La 0.5 Li 0.5 MnO 3 0.4g of powder, fourth layer La 0.5 Ca 0.5 CrO 3 0.8g of powder, and maintaining the pressure for 10min under the die pressing of 10MPa to obtain a green body; sintering for 4 hours at 1400 ℃ and 20kPa under argon environment to obtain the porous gradient perovskite ceramic body with compact surface layer and porous middle, wherein the first and seventh layers are thick and compact LaMnO with the thickness of 0.05mm 3 The second and sixth layers were La with a thickness of 0.1mm and smaller pores 0.6 Ca 0.4 MnO 3 The third and fifth layers are La with thickness of 0.1mm and mesopores 0.6 Li 0.4 MnO 3 The fourth layer is La with thickness of 0.2mm and larger hole 0.6 Ca 0.4 CrO 3 ；
(3) Then plating dense Al on the surface of the porous gradient ceramic 2 O 3 And (3) a film. Al with the thickness of 50nm is plated on the surface of the pore gradient ceramic by adopting a pulse laser deposition technology 2 O 3 A membrane;
(4) Finally, the film-based structure is heat treated in an air oven. The membrane-based structure is placed in an air furnace, and is kept at 500 ℃ for 30min to obtain the alumina/pore gradient lanthanide perovskite ceramic composite light absorber containing the interface transition layer, and the schematic diagram is shown in figure 1.
Example 3:
(1) Firstly, 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 powderAccording to LaMnO respectively 3 、La 0.7 Ca 0.3 MnO 3 、La 0.7 Li 0.3 MnO 3 And La (La) 0.7 Ca 0.3 CrO 3 Mixing the materials according to the stoichiometric ratio, performing solid-phase sintering (the sintering temperature is 1000 ℃, the heating speed is 5 ℃/min, the heat preservation time is 5 h), performing ball milling at the speed of 300 rpm 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 (La) 0.7 Ca 0.3 CrO 3 Ceramic powder;
(2) Secondly, preparing the lanthanide perovskite ceramic substrate with the pore gradient seven-layer structure. Uniformly mixing the four powders with a polyvinyl alcohol solution, and sieving the mixture with a 200-mesh sieve to obtain granulated powder; wherein the weight ratio of the polyvinyl alcohol to the polyvinyl alcohol solution in the polyvinyl alcohol solution is 7 percent, and the weight ratio of the polyvinyl alcohol solution to the ceramic powder is 9 percent; the granulated powder was then sequentially (LaMnO for the first and seventh layers 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 ) Uniformly spread on
Figure BDA0003936607000000071
Wherein the first and seventh layers of LaMnO 3 0.4g of powder, second and sixth layer La 0.5 Ca 0.5 MnO 3 0.4g of powder, third and fifth layers La 0.5 Li 0.5 MnO 3 0.4g of powder, fourth layer La 0.5 Ca 0.5 CrO 3 0.8g of powder, and maintaining the pressure for 7min under the die pressing of 13MPa to obtain a green body; sintering for 2h at 1500 ℃ and 10kPa under argon environment to obtain the porous gradient perovskite ceramic body with compact surface layer and porous middle, wherein the first and seventh layers are thick and compact LaMnO with the thickness of 0.1mm 3 The second and sixth layers were La with a thickness of 0.1mm and smaller pores 0.7 Ca 0.3 MnO 3 The third and fifth layers are La with thickness of 0.1mm and mesopores 0.7 Li 0.3 MnO 3 Fourth layerLa with thickness of 0.2mm and larger hole 0.7 Ca 0.3 CrO 3 ；
(3) Then plating dense Al on the surface of the porous gradient ceramic 2 O 3 And (3) a film. Plating 150nm thick Al on the surface of the pore gradient ceramic by adopting an atomic layer deposition technology 2 O 3 A membrane;
(4) Finally, the film-based structure is heat treated in an air oven. Placing the membrane-based structure in an air furnace, and preserving heat at 700 ℃ for 10min to obtain the alumina/pore gradient lanthanide perovskite ceramic composite light absorber containing the interface transition layer, wherein each LaMnO 3 The thickness of the base ceramic layers was 0.12mm, and the schematic diagram is shown in FIG. 1.
Example 4:
(1) Firstly, synthesizing lanthanide perovskite ceramic powder with wide spectrum and high absorption by a solid phase method. Respectively mixing lanthanum oxide, manganese oxide, calcium carbonate, lithium carbonate and chromium oxide powder according to LaMnO 3 、La 0.3 Ca 0.7 MnO 3 、La 0.3 Li 0.7 MnO 3 And La (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 speed is 5 ℃/min, the heat preservation time is 2 h), performing ball milling at the speed of 300 rpm for 36h, and sieving to obtain lanthanum manganate and La respectively 0.3 Ca 0.7 MnO 3 、La 0.3 Li 0.7 MnO 3 And La (La) 0.3 Ca 0.7 CrO 3 Ceramic powder;
(2) Secondly, preparing the lanthanide perovskite ceramic substrate with the pore gradient seven-layer structure. Uniformly mixing the four powders with a polyvinyl alcohol solution, and sieving the mixture with a 200-mesh sieve to obtain granulated powder; wherein the weight ratio of the polyvinyl alcohol to the polyvinyl alcohol solution in the polyvinyl alcohol solution is 10 percent, and the weight ratio of the polyvinyl alcohol solution to the ceramic powder is 10 percent; the granulated powder was then sequentially (LaMnO for the first and seventh layers 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 ) Uniformly spread on
Figure BDA0003936607000000081
Wherein the first and seventh layers of LaMnO 3 0.4g of powder, second and sixth layer La 0.5 Ca 0.5 MnO 3 0.4g of powder, third and fifth layers La 0.5 Li 0.5 MnO 3 0.8g of powder, fourth layer La 0.5 Ca 0.5 CrO 3 0.8g of powder, and maintaining the pressure for 5min under the die pressing of 15MPa to obtain a green body; sintering for 2h at 1500 ℃ and 15kPa under argon environment to obtain the light absorber with compact/middle porous alumina/lanthanum manganate film base structure, wherein the first and seventh layers are compact LaMnO with the thickness of 0.1mm 3 The second and sixth layers were La with a thickness of 0.1mm and smaller pores 0.3 Ca 0.7 MnO 3 The third and fifth layers are La with thickness of 0.2mm and mesopores 0.3 Li 0.7 MnO 3 The fourth layer is La with thickness of 0.2mm and larger hole 0.3 Ca 0.7 CrO 3 The method comprises the steps of carrying out a first treatment on the surface of the LaMnO thereof 3 The light absorptivity of the ceramic in the range of 0.3-14 μm is shown in FIG. 6;
(3) Then plating dense Al on the surface of the porous gradient ceramic 2 O 3 And (3) a film. Plating Al with thickness of 200nm on the surface of the pore gradient ceramic by adopting a magnetron sputtering technology 2 O 3 A membrane;
(4) Finally, the film-based structure is heat treated in an air oven. The membrane-based structure is placed in an air furnace, and the temperature is kept at 1000 ℃ for 5min, so that the alumina/pore gradient lanthanide perovskite ceramic composite light absorber containing the interface transition layer is obtained, and the schematic diagram is shown in figure 1.
The above description is only a partial typical case of the present invention, and the present invention is not limited thereto, and any modification, variation and equivalent element transformation made on the above embodiments according to the process substance of the present invention still falls within the protection scope of the technical solution of the present invention.

Claims (8)

1. An alumina/lanthanide perovskite ceramic composite light absorber is characterized in that the matrix material of the light absorber is lanthanide perovskiteThe first and seventh layers are compact LaMnO 3 Ceramic, the second and sixth layers are porous and calcium doped La 1-x Ca x MnO 3 Ceramic, third and fifth layers are porous in network and doped with La 1-y Li y MnO 3 Ceramic, the fourth layer is porous network and doped with La 1-z Ca z CrO 3 Ceramic, wherein the holes are micron-sized macropores; the aperture of the fourth layer is the largest, the aperture of the third and fifth layers is centered, the aperture of the second and sixth layers 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 ceramic, and the thickness is 50-200nm.
2. An alumina/lanthanide perovskite ceramic composite light absorber as recited in claim 1, wherein La is calcium doped 1-x Ca x MnO 3 The Ca doping amount x in the ceramic is 0.3-0.7, and the La is doped with lithium 1-y Li y MnO 3 The Li doping amount y in the ceramic is 0.3-0.7, and La is doped with calcium 1-z Ca z CrO 3 The doping amount z of Ca in the ceramic is 0.3-0.7.
3. An alumina/lanthanide perovskite ceramic composite light absorber as recited in claim 1, wherein a nano-transition layer is disposed between said alumina film layer and said lanthanide perovskite ceramic interface of said light absorber.
4. The method for preparing the alumina/lanthanide perovskite ceramic composite light absorber as defined in claim 1, which comprises the following specific steps:
(1) Synthesizing lanthanide perovskite ceramic powder with wide spectrum and high absorption by a solid phase method: mixing lanthanum oxide, manganese oxide, calcium carbonate, lithium carbonate and chromium oxide powder according to stoichiometric ratio, solid-phase sintering, ball milling, 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 Calcium-doped lanthanum chromate La 1-z Ca z CrO 3 Powder；
(2) Preparing a pore gradient seven-layer structure lanthanide perovskite ceramic substrate: mixing the powder with polyvinyl alcohol solution uniformly, sieving to obtain granulated powder; uniformly spreading the granulated powder in a hot-pressing die according to the proportion, and obtaining a green body under a certain die pressing condition; sintering at high temperature in argon environment to obtain porous gradient lanthanide perovskite ceramic body with compact surface layer and porous middle;
(3) Plating compact Al 2 O 3 Film: plating Al on the surface of the pore gradient ceramic by adopting a plating technology 2 O 3 A membrane;
(4) Heat treatment in an air oven produces a transition layer at the membrane-based interface.
5. The method for producing an alumina/lanthanoid perovskite ceramic composite light absorber according to claim 4, wherein in the step (1), the solid phase sintering process is as follows: the sintering temperature is 1000-1200 ℃, the heating speed 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 materials is 3:1.
6. The method for producing an alumina/lanthanoid perovskite ceramic composite light absorber according to claim 4, wherein in the step (2), sieving means sieving with a 200 mesh sieve, wherein the weight ratio of polyvinyl alcohol to polyvinyl alcohol solution in the polyvinyl alcohol solution is 5 to 10%, and the weight ratio of polyvinyl alcohol solution to ceramic powder is 8 to 10%; the diameter of the hot pressing die is
Figure QLYQS_1
The molding conditions are as follows: the pressure is 10-15 MPa, and the pressure maintaining time is 5-10 min; sintering for 2-4 h at 1400-1500 ℃ and 10-20 kPa under argon environment.
7. The method for producing an alumina/lanthanoid perovskite ceramic composite optical absorber according to claim 4, wherein in the step (3), al 2 O 3 The thickness of the film is 50-200nm, and the film plating technology is vacuumOne of evaporation, pulsed laser deposition, atomic layer deposition and magnetron sputtering techniques.
8. The method for preparing an alumina/lanthanide perovskite ceramic composite light absorber as defined in claim 4, wherein the heat treatment process parameters are as follows: preserving heat for 5-30 min at 500-1000 ℃.
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