CN113149088A - High-emissivity infrared energy-saving high-entropy material with perovskite structure and preparation method thereof - Google Patents
High-emissivity infrared energy-saving high-entropy material with perovskite structure and preparation method thereof Download PDFInfo
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Abstract
The invention provides a method for preparing a high-emissivity infrared energy-saving high-entropy material with a perovskite structure, and belongs to the technical field of infrared energy saving. The prepared high-emissivity infrared energy-saving high-entropy material with the perovskite structure is in the perovskite structure (ABO)3Structure) as main phase, La element as A site, and three to five metal elements of Co, Cr, Fe, Mn, Ni and Al as B site. The emissivity of the material is 0.85-0.95. The preparation method is a high-temperature solid-phase synthesis method. The high-emissivity infrared energy-saving high-entropy material with the perovskite structure has the beneficial effects that: the emissivity can reach as high as 0.95, the heat conductivity is low, the high-temperature stability is good, and the heat-conducting material has great potential in the field of energy conservation of heat engineering kilns.
Description
Technical Field
The invention belongs to the technical field of infrared energy conservation, and particularly relates to a high-emissivity infrared energy-saving high-entropy material with a perovskite structure and a preparation method thereof.
Background
In recent years, various high entropy ceramics and their structures and properties, such as oxides, carbides, borides, nitrides, and silicides, etc., have been studied. Among these crystalline high-entropy ceramics, high-entropy oxides have attracted great research interest due to their potential for use, such as rock salt, spinel, perovskite, and fluorite. Perovskite type (ABO)3Structure) the crystal structure of the oxide generally consists of a 12 coordinated a-site atom and a 6 coordinated B-site atom, as well as oxygen octahedra. Because the A, B bit coordination number is large, different combinations of cations are increased, A, B bit cation radiuses with different sizes exist in different permutation and combination, so that the tolerance factor t is changed, lattice distortion is generated, the symmetry of the perovskite structure is reduced, the perovskite structure shows rich physicochemical properties, and the perovskite structure has wide application prospects in solar cells, photocatalysis, proton conductors, dielectrics, ferroelectrics, multiferroics and the like. Although some progress has been made on oxide high-entropy ceramics with perovskite structure at present, the research on the radiation performance has not been reported yet.
From the perspective of thermal technology, the theoretical percentage of radiation heat transfer in three heat transfer modes (radiation, convection and conduction) to a workpiece exceeds 80% in a high-temperature environment of more than 800 ℃, and the radiation heat transfer mode is a leading factor for determining the thermal efficiency of a high-temperature furnace. Therefore, the enhancement of radiation heat transfer is a necessary way for realizing energy conservation of the thermal kiln. The mutual doping of elements with different atomic masses and atomic radii in the high-entropy material crystal lattice enhances the nonlinear vibration of the crystal lattice, thereby reducing the mean free path of phonons, further intensifying the scattering effect among the phonons and leading to lower thermal conductivity. The near-infrared high-emissivity material is mainly characterized in that ions with different valence states and valence bond structures are doped to form an impurity energy level locally, so that the aim of improving the emissivity is fulfilled. Therefore, the preparation of the high-entropy material with high emissivity and low thermal conductivity is a key problem in the field of kiln energy conservation.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a high-emissivity infrared energy-saving high-entropy material with a perovskite structure and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme:
according to the semiconductor energy band theory, the absorption mechanism which plays a leading role in the near infrared band is photo-electric transition absorption, and ions with different valence states and valence bond structures are doped to form impurity energy levels locally, so that the possibility of free carriers to transition from the valence band to the conduction band is enhanced, the increase of the concentration of the free carriers (electrons, holes and the like) in the valence band and the transition between band gaps are promoted, and the near infrared emissivity is improved. Because Cr, Mn, Fe, Co and Ni are all multi-valence atoms, the doping conditions for preparing the near-infrared high-emissivity material are matched.
The high-emissivity infrared energy-saving high-entropy material with the perovskite structure comprises the raw materials of lanthanum oxide, cobalt oxide, chromium oxide, iron oxide, manganese oxide, nickel oxide and aluminum oxide; the A site of the perovskite structure is La element, and the B site is three to five metal elements of Co, Cr, Fe, Mn, Ni and Al.
The preparation method of the high-emissivity infrared energy-saving high-entropy material with the perovskite structure comprises the following steps:
(1) preparing materials: the method comprises the following steps of proportioning raw materials of the high-emissivity infrared energy-saving high-entropy material with the perovskite structure, and weighing 3 to five kinds of metal oxide powder according to the molar ratio of A: B =1:1 and the molar ratio of B-site metal atoms being 1:1:1 or 1:1:1:1, wherein the raw materials of the high-emissivity infrared energy-saving high-entropy material with the perovskite structure consist of lanthanum oxide, cobalt oxide, chromium oxide, iron oxide, manganese oxide, nickel oxide and aluminum oxide;
(2) ball-milling the powder weighed in the step (1);
(3) and (3) calcining: calcining the ball-milled raw materials in an air atmosphere at 1200-1600 ℃ for 120-360 min to enable the raw materials to generate a high-temperature solid-phase reaction, and finally preparing the powder of the high-emissivity infrared energy-saving high-entropy material with the perovskite structure.
The emissivity of the high-emissivity infrared energy-saving high-entropy material with the perovskite structure is 0.85-0.95.
The invention provides a high-emissivity infrared energy-saving high-entropy material with a perovskite structure; when the high-emissivity infrared energy-saving high-entropy material with the perovskite structure is prepared, because Cr, Mn, Fe, Co and Ni are multi-valence atoms, partial oxygen atoms overflow to form oxygen vacancies in a high-temperature solid-phase reaction, and partial ions are subjected to valence change in order to keep charge balance, so that impurity energy levels are formed locally, impurity absorption and free carrier absorption are enhanced, and the emissivity of the material is improved.
The high-emissivity infrared energy-saving high-entropy material with the perovskite structure has the beneficial effects that:
(1) the emissivity of the high-emissivity infrared energy-saving high-entropy material with the perovskite structure prepared by the invention can reach 0.95 at most, and is higher than that of the existing high-temperature oxide system infrared energy-saving material.
(2) The high-emissivity infrared energy-saving high-entropy material with the perovskite structure prepared by the invention belongs to a high-temperature oxide system, and the maximum use temperature can reach 1800 ℃.
(3) The mutual doping of elements with different atomic masses and atomic radii in the crystal lattice enhances the nonlinear vibration of the crystal lattice, thereby reducing the mean free path of phonons, further intensifying the scattering effect among the phonons and leading to lower thermal conductivity.
(4) The high-emissivity infrared energy-saving high-entropy material with the perovskite structure prepared by the invention has the advantages of easily available raw materials, simple preparation process, low production cost and easy industrial production.
Drawings
FIG. 1 shows La (Co) in example 10.2Cr0.2Fe0.2Mn0.2Ni0.2)O3X-ray diffraction pattern of high entropy oxide.
FIG. 2 shows La (Co) in example 10.2Cr0.2Fe0.2Mn0.2Ni0.2)O3The emissivity spectrum of the high-entropy oxide in a near-red (0.76-2.5 mu m) wave band.
Detailed Description
The present invention is further illustrated by the following specific examples, which should not be construed as limiting the scope of the invention.
The invention is described in connection with the accompanying drawings and the specific embodiments:
example 1: lanthanum oxide, cobalt oxide, chromium oxide, iron oxide, manganese oxide and nickel oxide are mixed according to the molar ratio of La, Cr, Mn, Fe, Co, Ni =1:0.2:0.2:0.2:0.2:0.2, ball-milled for 6 hours, dried and calcined for 300 minutes in air atmosphere at 1200 ℃, so that high-temperature solid-phase reaction occurs, and finally the high-emissivity, energy-saving and high-entropy infrared material with the perovskite structure is prepared, wherein the emissivity of the high-emissivity, energy-saving and high-entropy infrared material is 0.95.
As can be seen from fig. 1: the diffraction peak of the high-emissivity infrared energy-saving high-entropy material synthesized in the embodiment is positioned between five single components and almost completely coincides with the diffraction peak of LaMnO3, and the diffraction peak is broadened at the same time, so that the five elements are well dissolved in the crystal lattice, the high configuration entropy formed by the equal molar ratio promotes the compatibility among the elements and the formation of solid solution, no other impurity peak and a second phase are generated, the crystal structure is a perovskite structure, and the successful synthesis of the high-entropy material La (Co) with a single phase is shown0.2Cr0.2Fe0.2Mn0.2Ni0.2)O3。
As can be seen from fig. 2: in the embodiment, the emissivity of the high-emissivity infrared energy-saving high-entropy material in a near infrared (0.76-2.5 mu m) wave band reaches 0.95, which is one of the highest-emissivity oxide materials found at present.
Example 2: lanthanum oxide, cobalt oxide, chromium oxide, iron oxide, manganese oxide and nickel oxide are mixed according to the molar ratio of La, Cr, Mn, Fe, Co, Ni =1:0.2:0.2:0.2:0.2:0.2, ball-milled for 24 hours, dried and calcined for 360 minutes in 1400 ℃ air atmosphere to generate high-temperature solid-phase reaction, and finally the high-emissivity, energy-saving and high-entropy infrared material with the perovskite structure is prepared, wherein the emissivity of the high-emissivity, energy-saving and high-entropy infrared material is 0.91.
Example 3: lanthanum oxide, cobalt oxide, chromium oxide, iron oxide, manganese oxide and nickel oxide are mixed according to the molar ratio of La, Cr, Mn, Fe, Co, Ni =1:0.2:0.2:0.2:0.2:0.2, ball-milled for 24 hours, dried and calcined in 1500 ℃ air atmosphere for 120 minutes to generate high-temperature solid-phase reaction, and finally the high-emissivity, energy-saving and high-entropy infrared material with the perovskite structure is prepared, wherein the emissivity of the high-emissivity, energy-saving and high-entropy infrared material is 0.89.
Example 4: lanthanum oxide, cobalt oxide, chromium oxide, iron oxide, manganese oxide and nickel oxide are mixed according to the molar ratio of La, Cr, Mn, Fe, Co, Ni =1:0.2:0.2:0.2:0.2:0.2, ball-milled for 10 hours, dried and calcined in air atmosphere at 1200 ℃ for 120 minutes to generate high-temperature solid-phase reaction, and finally the high-emissivity, energy-saving and high-entropy infrared material with the perovskite structure is prepared, wherein the emissivity of the high-emissivity, energy-saving and high-entropy infrared material is 0.91.
Example 5: lanthanum oxide, cobalt oxide, chromium oxide, iron oxide, aluminum oxide and nickel oxide are mixed according to the molar ratio of La, Cr, Al, Fe, Co, Ni =1:0.2:0.2:0.2:0.2:0.2, ball-milled for 12 hours, dried and calcined in an air atmosphere at 1600 ℃ for 120 minutes to generate high-temperature solid-phase reaction, and finally the high-emissivity, energy-saving and high-entropy infrared material with the perovskite structure is prepared, wherein the emissivity of the high-emissivity, energy-saving and high-entropy infrared material is 0.90.
Example 6: lanthanum oxide, cobalt oxide, chromium oxide, iron oxide and manganese oxide are mixed according to the molar ratio of La, Cr, Mn, Fe, Co =1:0.25:0.25:0.25:0.25, ball-milled for 10 hours, dried and calcined for 180 minutes in air atmosphere at 1200 ℃, so that the materials are subjected to high-temperature solid-phase reaction, and finally the high-emissivity infrared energy-saving high-entropy material with the perovskite structure is prepared, wherein the emissivity of the high-emissivity infrared energy-saving high-entropy material is 0.92.
Example 7: lanthanum oxide, manganese oxide, chromium oxide, iron oxide and nickel oxide are mixed according to the molar ratio of La, Cr, Mn, Fe, Ni =1:0.25:0.25:0.25:0.25, ball-milled for 20 hours, dried and calcined for 300 minutes in 1300 ℃ air atmosphere to carry out high-temperature solid-phase reaction, and finally the high-emissivity infrared energy-saving high-entropy material with the perovskite structure is prepared, wherein the emissivity of the high-emissivity infrared energy-saving high-entropy material is 0.92.
Example 8: lanthanum oxide, cobalt oxide, chromium oxide, manganese oxide and nickel oxide are mixed according to the molar ratio of La, Cr, Mn, Co, Ni =1:0.25:0.25:0.25:0.25, ball-milled for 8 hours, dried and calcined in air atmosphere at 1400 ℃ for 120 minutes to perform high-temperature solid-phase reaction, and finally the high-emissivity infrared energy-saving high-entropy material with the perovskite structure is prepared, wherein the emissivity of the high-emissivity infrared energy-saving high-entropy material is 0.91.
Example 9: lanthanum oxide, cobalt oxide, iron oxide, chromium oxide and nickel oxide are mixed according to the molar ratio of La, Cr, Fe, Co, Ni =1:0.25:0.25:0.25:0.25, ball-milled for 8 hours, dried and calcined in 1500 ℃ air atmosphere for 240 minutes to perform high-temperature solid-phase reaction, and finally the high-emissivity infrared energy-saving high-entropy material with the perovskite structure is prepared, wherein the emissivity of the high-emissivity infrared energy-saving high-entropy material is 0.90.
Example 10: lanthanum oxide, cobalt oxide, iron oxide, manganese oxide and nickel oxide are mixed according to the molar ratio of La, Mn, Fe, Co, Ni =1:0.25:0.25:0.25:0.25, ball-milled for 8 hours, dried and calcined in 1500 ℃ air atmosphere for 120 minutes to perform high-temperature solid-phase reaction, and finally the high-emissivity infrared energy-saving high-entropy material with the perovskite structure is prepared, wherein the emissivity of the high-emissivity infrared energy-saving high-entropy material is 0.93.
Example 11: lanthanum oxide, chromium oxide, iron oxide and manganese oxide are mixed according to the molar ratio of La to Cr to Mn to Fe =3 to 1, ball-milled for 16 h, dried and calcined for 180 min in air atmosphere at 1200 ℃ to generate high-temperature solid-phase reaction, and finally the high-emissivity infrared energy-saving high-entropy material with the perovskite structure is prepared, wherein the emissivity of the high-emissivity infrared energy-saving high-entropy material is 0.91.
Example 12: lanthanum oxide, cobalt oxide, iron oxide and nickel oxide are mixed according to the molar ratio of La to Fe to Co to Ni =3 to 1, ball-milled for 12 hours, dried and calcined in air atmosphere at 1400 ℃ for 300 minutes to generate high-temperature solid-phase reaction, and finally the high-emissivity infrared energy-saving high-entropy material with the perovskite structure is prepared, wherein the emissivity of the high-emissivity infrared energy-saving high-entropy material is 0.87.
Example 13: lanthanum oxide, cobalt oxide, manganese oxide and nickel oxide are mixed according to the molar ratio of La to Mn to Co to Ni =3 to 1, ball-milled for 24 hours, dried and calcined in air atmosphere at 1300 ℃ for 120 minutes to generate high-temperature solid-phase reaction, and finally the high-emissivity infrared energy-saving high-entropy material with the perovskite structure is prepared, wherein the emissivity of the high-emissivity infrared energy-saving high-entropy material is 0.88.
Example 14: lanthanum oxide, cobalt oxide, chromium oxide, iron oxide, manganese oxide and nickel oxide are mixed according to the molar ratio of La to Cr to Fe to Al =1:0.2:0.2:0.2:0.2:0.2, ball-milled for 6 hours, dried and calcined in an air atmosphere at 1400 ℃ for 120 minutes to perform high-temperature solid-phase reaction, and finally the high-emissivity infrared energy-saving high-entropy material with the perovskite structure is prepared, wherein the emissivity of the high-emissivity infrared energy-saving high-entropy material is 0.85.
Example 15: lanthanum oxide, cobalt oxide, chromium oxide, iron oxide, manganese oxide and nickel oxide are mixed according to the molar ratio of La to Cr to Fe to Ni =1:0.2:0.2:0.2:0.2:0.2, ball-milled for 6 hours, dried and calcined in 1500 ℃ air atmosphere for 120 minutes to generate high-temperature solid-phase reaction, and finally the high-emissivity infrared energy-saving high-entropy material with the perovskite structure is prepared, wherein the emissivity of the high-emissivity infrared energy-saving high-entropy material is 0.88.
Claims (4)
1. A high-emissivity infrared energy-saving high-entropy material with a perovskite structure is characterized in that: the raw materials of the high-emissivity infrared energy-saving high-entropy material with the perovskite structure comprise lanthanum oxide, cobalt oxide, chromium oxide, iron oxide, manganese oxide, nickel oxide and aluminum oxide; the A site of the perovskite structure is La element, and the B site is three to five metal elements of Co, Cr, Fe, Mn, Ni and Al.
2. The preparation method of the high-emissivity infrared energy-saving high-entropy material with the perovskite structure as claimed in claim 1 is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing materials: preparing raw materials of the high-emissivity infrared energy-saving high-entropy material with the perovskite structure according to a molar ratio of A: B =1: 1; 3 to five kinds of metal oxide powder are respectively weighed according to the molar ratio of B-site metal atoms of 1:1:1 or 1:1:1:1, and the raw material of the high-emissivity infrared energy-saving high-entropy material with the perovskite structure consists of lanthanum oxide, cobalt oxide, chromium oxide, iron oxide, manganese oxide, nickel oxide and aluminum oxide;
(2) ball-milling the powder weighed in the step (1);
(3) and (3) calcining: calcining the ball-milled raw materials in an air atmosphere at 1200-1600 ℃ for 120-360 min to enable the raw materials to generate a high-temperature solid-phase reaction, and finally preparing the powder of the high-emissivity infrared energy-saving high-entropy material with the perovskite structure.
The emissivity of the high-emissivity infrared energy-saving high-entropy material with the perovskite structure is 0.85-0.95.
3. The preparation method of the high-emissivity infrared energy-saving high-entropy material with the perovskite structure as claimed in claim 2, wherein ball milling in the step 2 is planetary ball milling for 6-24 h.
4. The preparation method of the high-emissivity infrared energy-saving high-entropy material with the perovskite structure according to claim 2, is characterized in that: the emissivity of the high-emissivity infrared energy-saving high-entropy material with the perovskite structure is 0.85-0.95.
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| CN114573345A (en) * | 2022-03-24 | 2022-06-03 | 郑州大学 | Preparation method and application of perovskite type high-entropy high-emissivity ceramic coating film coating liquid |
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