CN118026273A - High-entropy perovskite infrared radiation material and preparation method thereof - Google Patents
High-entropy perovskite infrared radiation material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a ferrate perovskite infrared radiation material, the chemical formula of which is ABO 3; the A site is any five elements in rare earth elements La, pr, ca, ce, gd, sm, nd, dy, coordinates with 12 oxygen ions and is positioned in a cavity formed by octahedron; b is transition metal element Fe, and the cation and six oxygen ions form octahedral coordination. Meanwhile, the invention also discloses a preparation method of the ferrate perovskite infrared radiation material. The high-entropy ferrite perovskite infrared radiation material has an infrared emissivity of 0.85-0.88 at a wave band of 0.78-16 mu m, has excellent thermal stability at 1300 ℃ for 24 hours, and can be applied to the fields of high-temperature radiation heat transfer and heat protection of power station boilers, aerospace, industrial kilns and the like.
Description
Technical Field
The invention relates to the field of infrared radiation materials, in particular to a high-entropy perovskite infrared radiation material and a preparation method thereof.
Background
Thermal radiation relates to the design of engineered thermal surfaces that can effectively transfer heat from the surface of one thermal object to another without contact, with radiant heat transfer accounting for over 80% of the total heat transfer above 1000 ℃. The technology has the functions of energy conservation, efficiency improvement and heat protection in various fields such as industrial kilns, high-temperature boilers, spacecrafts and the like.
At present, materials such as SiC, siB, cordierite, spinel, perovskite and the like have good infrared radiation performance and thermal stability and have been used as infrared radiation materials. For example, perovskite type LaFeO 3 oxide of ferrite has a melting point of 1900 ℃ and good high-temperature stability. However, the infrared emissivity of the material is quite low in the 3-5 μm band. According to the wien's law of displacement and the planck's law, the radiant energy is mainly concentrated in the wave band of 1-5 um under the high temperature condition. By doping rare earth elements or alkaline earth metal elements (valence may be +1, +2, and +3) at the a site, or doping transition metal ions (valence may be +3, +4, and +5) at the B site, emissivity in the 3-5 μm band can be improved. However, an impurity phase may be introduced in the doping process, so that oxidation resistance at high temperature is reduced to cause reduction of infrared emissivity, and the service period is shortened.
In recent years, high-entropy materials have attracted extensive research interest in the fields of energy storage, conversion, and the like. The high-entropy material has high configuration entropy, can offset the increase of enthalpy, reduces the Gibbs free energy of the system, and forms a single-phase solid solution structure. Furthermore, the multicomponent properties provide a prerequisite for optimizing the functional properties of the material. However, high entropy materials have been reported to be less well in the infrared radiation field. In 2022, china patent No. Zhang Zongtao, which applies for patent CN 114573345A, a preparation method and application of perovskite type high-entropy high-emissivity ceramic coating film plating liquid, a sol-gel method is utilized to prepare the perovskite type high-entropy high-emissivity ceramic coating film plating liquid, but the preparation process is relatively complex, and transition metal is mainly introduced into the B site to increase the emissivity, which is not beneficial to the improvement of the high-temperature thermal stability of the material.
Disclosure of Invention
The invention aims to provide a high-entropy perovskite infrared radiation material for improving high-temperature thermal stability.
The invention aims to provide a preparation method of the ferrate perovskite infrared radiation material.
In order to solve the problems, the invention provides a ferrate perovskite infrared radiation material, which is characterized in that: the chemical formula of the high entropy perovskite ferrite infrared radiation material is ABO 3; the A site is any five elements in rare earth elements La, pr, ca, ce, gd, sm, nd, dy, coordinates with 12 oxygen ions and is positioned in a cavity formed by octahedron; b is transition metal element Fe, and the cation and six oxygen ions form octahedral coordination.
The infrared radiation rate of the high-entropy ferrite perovskite infrared radiation material in a wave band of 0.78-16 mu m is 0.85-0.88.
The preparation method of the ferrate perovskite infrared radiation material is characterized by comprising the following steps of: the method is characterized in that any five of La2O3、Pr6O11、CaO、Ce2O3、Gd2O3、Sm2O3、Nd2O3、Dy2O3 powder and Fe 2O3 are used as raw materials, and the molar ratio of metal atoms is 1:1:1:1:1:5, ball milling and mixing, and drying and grinding to obtain mixture powder; and calcining the mixture powder in a muffle furnace at high temperature, and cooling and grinding to obtain the high-entropy perovskite infrared radiation material.
The ball milling and mixing conditions are that a planetary ball mill is adopted for wet ball milling, the ball milling rotating speed is 300-500 r/min, the ball milling time is 12-24 hours, and the mass ratio of ball materials to absolute ethyl alcohol is 2-5: 1:3.
The high-temperature calcination condition means that the calcination temperature is 1000-1500 ℃, the heating rate is 3-5 ℃/min, and the calcination time is 4-10 hours.
The cooling mode is one of furnace-following cooling, air quenching cooling and liquid nitrogen quenching cooling.
Compared with the prior art, the invention has the following advantages:
1. The chemical formula of the high-entropy ferrite perovskite infrared radiation material is ABO 3; the A-site multi-element rare earth is doped, coordinated with 12 oxygen ions and positioned in a cavity formed by an octahedron; b is transition metal element Fe, and the cation and six oxygen ions form octahedral coordination. The structure can accommodate a plurality of cations, has rich optimization space for infrared radiation performance, has excellent structural stability, and can be suitable for high-temperature and corrosive environments.
2. The invention synthesizes the high entropy ferrite material with a single perovskite structure by adopting an entropy-driven high entropy stabilization strategy, and the material has the characteristics of single phase, high purity, small particle size, uniform element distribution and the like.
3. The ferrate perovskite infrared radiation material has the advantages of high entropy effect and delayed diffusion effect, good high-temperature stability in air, no impurity peak on an XRD spectrum after long-time thermal stability experiment is carried out at 1300 ℃ for 24 hours, and the change range of the infrared emissivity is only 0.01, thus the ferrate perovskite infrared radiation material has excellent thermal stability. In addition, the material has good acid-base corrosion resistance.
4. The plurality of rare earth elements in the ferrate perovskite infrared radiation material form a plurality of impure f-electron intermediate energy levels, which is beneficial to reducing the band gap. The band gap of the material is 1.25eV, which is beneficial to improving the infrared radiation performance of the material in the near infrared region. Meanwhile, due to the size difference of doping elements, lattice distortion effect is caused, and lattice vibration absorption is increased, so that the infrared radiation efficiency in the middle infrared region is higher, and the infrared heat transfer efficiency under the high-temperature condition can be improved. The infrared emissivity of the infrared radiation material in the wave band of 0.78-16 μm is 0.85-0.88. Therefore, the high-entropy ferrite perovskite infrared radiation material can be applied to the fields of high-temperature radiation heat transfer and heat protection of power station boilers, aerospace, industrial kilns and the like.
5. The invention adopts a simple mechanical wet ball milling and solid phase synthesis calcining method to prepare the high entropy perovskite infrared radiation material, which is suitable for industrial mass production.
Drawings
The following describes the embodiments of the present invention in further detail with reference to the drawings.
FIG. 1 is an XRD pattern for example 1 (La 0.2Ca0.2Pr0.2Ce0.2Sm0.2)FeO3) of the present invention.
Fig. 2 is an XRD pattern of inventive example 2 (La 0.2Ca0.2Pr0.2Ce0.2Nd0.2)FeO3).
FIG. 3 is an infrared spectrum of embodiment 2 (La 0.2Ca0.2Pr0.2Ce0.2Nd0.2)FeO3 in the 0.78-16 μm band) of the present invention.
Fig. 4 is an XRD pattern of example 3 (La 0.2Ca0.2Pr0.2Ce0.2Gd0.2)FeO3) of the present invention.
Fig. 5 is an XRD pattern of example 4 (La 0.2Ca0.2Pr0.2Ce0.2Dy0.2)FeO3) of the present invention.
Detailed Description
A perovskite ferrate infrared radiation material, the chemical formula of which is ABO 3; the A site is any five elements in rare earth elements La, pr, ca, ce, gd, sm, nd, dy, coordinates with 12 oxygen ions and is positioned in a cavity formed by octahedron; b is transition metal element Fe, and the cation and six oxygen ions form octahedral coordination.
The infrared radiation rate of the high-entropy ferrite perovskite infrared radiation material in a wave band of 0.78-16 mu m is 0.85-0.88.
The preparation method comprises the following steps: the method is characterized in that any five of La2O3、Pr6O11、CaO、Ce2O3、Gd2O3、Sm2O3、Nd2O3、Dy2O3 powder and Fe 2O3 are used as raw materials, and the molar ratio of metal atoms is 1:1:1:1:1:5, carrying out wet ball milling by adopting a planetary ball mill, wherein the ball milling rotating speed is 300-500 r/min, the ball milling time is 12-24 hours, and the mass ratio (g/g) of ball materials to absolute ethyl alcohol is 2-5: 1:3. ball milling and mixing, drying at 80-100 ℃, and grinding to obtain mixture powder; and (3) calcining the mixture powder in a muffle furnace at a high temperature, wherein the calcining temperature is 1000-1500 ℃, the heating rate is 3-5 ℃/min, and the calcining time is 4-10 hours. And cooling to room temperature by one of furnace cooling, air quenching cooling and liquid nitrogen quenching cooling after calcining, and finally grinding to obtain the high-entropy perovskite infrared radiation material.
Example 1a method for preparing a perovskite ferrate infrared radiation material:
According to the metal atom mole ratio of 1:1:1:1:1: respectively weighing CaO（1mol）、Pr6O11（1mol）、La2O3（1mol）、Ce2O3（1mol）、Sm2O3（1mol）、Fe2O3（5mol） powder as a raw material; the mass ratio (g/g) of the ball material to the absolute ethyl alcohol is 2:1: and 3, respectively pouring the zirconia balls, the raw materials and the absolute ethyl alcohol into a planetary ball mill, performing ball milling for 1 hour at the rotating speed of 300 r/min, and then suspending for 10min, wherein the ball milling period is one ball milling period, performing ball milling for 1 hour after 10min, and performing ball milling for 24 hours at the rotating speed of 300 r/min. Ball milling and mixing, drying at 80-100 ℃, and grinding to obtain mixture powder; the mixture powder is calcined in a muffle furnace at a high temperature, the calcining temperature is 1000 ℃, the heating rate is 3 ℃/min, and the calcining time is 8 hours. And (3) quenching and cooling the calcined material to room temperature by liquid nitrogen, and finally grinding the calcined material to obtain the single-phase (La 0.2Ca0.2Pr0.2Ce0.2Sm0.2)FeO3 high entropy perovskite ferrite infrared radiation material).
FIG. 1 is an XRD pattern of the (La 0.2Ca0.2Pr0.2Ce0.2Sm0.2)FeO3 ferrate perovskite infrared radiation material) described in example 1, which is very coincident with the LaFeO 3 line (PDF # 75-0439) with perovskite structure in the ICDD database, showing that the ferrate perovskite infrared radiation material prepared in this example is perovskite structure.
The obtained (La 0.2Ca0.2Pr0.2Ce0.2Sm0.2)FeO3 ferrate perovskite infrared radiation material is subjected to infrared radiation performance and thermal stability assessment:
The testing method comprises the following steps: reflectance spectra were measured at bands of 0.78 to 2.5 μm and 2.5 to 16 μm using a U.S. Lambda950 UV-visible near infrared spectrophotometer (containing 150mm integrating sphere) and a German Bruker Tensor 27 IR spectrometer (containing integrating sphere), respectively.
The high entropy perovskite ferrite infrared radiation material is placed in the air atmosphere of a box-type furnace, and a long-time thermal stability experiment is carried out at 1300 ℃ for 24 hours.
The amount of the test sample was 0.2g.
The results show that: the infrared radiation rate of the high-entropy ferrite perovskite infrared radiation material in a wave band of 0.78-16 mu m is 0.856; after a thermal stabilization experiment, the infrared emissivity of the material is measured to be 0.849 at 0.78-16 mu m.
Example 2a method for preparing a perovskite ferrate infrared radiation material:
According to the metal atom mole ratio of 1:1:1:1:1: respectively weighing CaO（1mol）、Pr6O11（1mol）、La2O3（1mol）、Ce2O3（1mol）、Nd2O3（1mol）、Fe2O3（5mol） powder as a raw material; the mass ratio (g/g) of the ball material to the absolute ethyl alcohol is 3:1: and 3, respectively pouring the zirconia balls, the raw materials and the absolute ethyl alcohol into a planetary ball mill, performing ball milling for 1 hour at the rotating speed of 500r/min, and then suspending for 10min, wherein the ball milling period is one ball milling period, performing ball milling for 1 hour after 10min, and performing ball milling for 12 hours at the rotating speed of 500 r/min. Ball milling and mixing, drying at 80-100 ℃, and grinding to obtain mixture powder; the mixture powder is calcined in a muffle furnace at a high temperature of 1300 ℃, the temperature rising rate is 3 ℃/min, and the calcination time is 6 hours. And (3) quenching and cooling the calcined material to room temperature by air, and finally grinding the calcined material to obtain the single-phase (La 0.2Ca0.2Pr0.2Ce0.2Nd0.2)FeO3 high-entropy perovskite ferrite infrared radiation material).
FIG. 2 is an XRD pattern of the (La 0.2Ca0.2Pr0.2Ce0.2Nd0.2)FeO3 ferrate perovskite infrared radiation material) described in example 2, which is very coincident with the LaFeO 3 line (PDF # 75-0439) with perovskite structure in the ICDD database, showing that the ferrate perovskite infrared radiation material prepared in this example is a single phase solid solution with perovskite structure.
The obtained (La 0.2Ca0.2Pr0.2Ce0.2Nd0.2)FeO3 ferrate perovskite infrared radiation material is subjected to infrared radiation performance and thermal stability assessment:
The test method and the test sample amounts were the same as in example 1.
The result shows that the infrared radiation rate of the ferrate perovskite infrared radiation material in the wave band of 0.78-16 mu m is 0.88. As shown in fig. 3, it is shown that it has a high infrared emissivity in this band.
After a thermal stabilization experiment, the infrared emissivity of the material is measured to be 0.872 at 0.78-16 mu m.
Example 3a method for preparing a perovskite ferrate infrared radiation material:
According to the metal atom mole ratio of 1:1:1:1:1: respectively weighing CaO（1mol）、Pr6O11（1mol）、La2O3（1mol）、Ce2O3（1mol）、Gd2O3（1mol）、Fe2O3（5mol） powder as a raw material; the mass ratio (g/g) of the ball material to the absolute ethyl alcohol is 4:1: and 3, respectively pouring the zirconia balls, the raw materials and the absolute ethyl alcohol into a planetary ball mill, performing ball milling for 1 hour at the rotating speed of 300 r/min, and then suspending for 10min, wherein the ball milling period is one ball milling period, performing ball milling for 1 hour after 10min, and performing ball milling for 12 hours at the rotating speed of 300 r/min. Ball milling and mixing, drying at 80-100 ℃, and grinding to obtain mixture powder; the mixture powder is calcined in a muffle furnace at a high temperature of 1200 ℃, the temperature rising rate is 4 ℃/min, and the calcination time is 10 hours. And cooling to room temperature along with the furnace after calcining, and finally grinding to obtain the single-phase (La 0.2Ca0.2Pr0.2Ce0.2Gd0.2)FeO3 high entropy perovskite ferrite infrared radiation material).
FIG. 4 is an XRD pattern of the (La 0.2Ca0.2Pr0.2Ce0.2Gd0.2)FeO3 ferrate perovskite infrared radiation material) described in example 3, which is very coincident with the LaFeO 3 line (PDF # 75-0439) with perovskite structure in the ICDD database, showing that the ferrate perovskite infrared radiation material prepared in this example is a single phase solid solution with perovskite structure.
The obtained (La 0.2Ca0.2Pr0.2Ce0.2Gd0.2)FeO3 ferrate perovskite infrared radiation material is subjected to infrared radiation performance and thermal stability assessment:
The test method and the test sample amounts were the same as in example 1.
The result shows that the infrared radiation rate of the ferrate perovskite infrared radiation material in the wave band of 0.78-16 mu m is 0.855. After a thermal stabilization experiment, the infrared emissivity of the material is measured to be 0.848 at 0.78-16 mu m.
Example 4a method for preparing a perovskite ferrate infrared radiation material:
According to the metal atom mole ratio of 1:1:1:1:1: respectively weighing CaO（1mol）、Pr6O11（1mol）、La2O3（1mol）、Ce2O3（1mol）、Dy2O3（1mol）、Fe2O3（5mol） powder as a raw material; the mass ratio (g/g) of the ball material to the absolute ethyl alcohol is 5:1: and 3, respectively pouring the zirconia balls, the raw materials and the absolute ethyl alcohol into a planetary ball mill, performing ball milling for 1 hour at the rotating speed of 400 r/min, and then suspending for 10min, wherein the ball milling period is one ball milling period, performing ball milling for 1 hour after 10min, and performing ball milling for 10 hours at the rotating speed of 400 r/min. Ball milling and mixing, drying at 80-100 ℃, and grinding to obtain mixture powder; the mixture powder is calcined in a muffle furnace at a high temperature, the calcining temperature is 1500 ℃, the heating rate is 5 ℃/min, and the calcining time is 4 hours. And (3) quenching and cooling the calcined material to room temperature by air, and finally grinding the calcined material to obtain the single-phase (La 0.2Ca0.2Pr0.2Ce0.2Dy0.2)FeO3 high-entropy perovskite ferrite infrared radiation material).
FIG. 5 is an XRD pattern of the (La 0.2Ca0.2Pr0.2Ce0.2Dy0.2)FeO3 ferrate perovskite infrared radiation material) described in example 4, which is very coincident with the LaFeO 3 line (PDF # 75-0439) with perovskite structure in the ICDD database, showing that the ferrate perovskite infrared radiation material prepared in this example is a single phase solid solution with perovskite structure.
The obtained (La 0.2Ca0.2Pr0.2Ce0.2Dy0.2)FeO3 ferrate perovskite infrared radiation material is subjected to infrared radiation performance and thermal stability assessment:
The test method and the test sample amounts were the same as in example 1.
The result shows that the infrared radiation rate of the ferrate perovskite infrared radiation material in the wave band of 0.78-16 μm is 0.858. After a thermal stability experiment, the infrared emissivity of the material is measured to be 0.850 at 0.78-16 mu m.
The foregoing is illustrative of the preferred embodiments of the present invention and is not to be construed as limiting the claims. The present invention is not limited to the above embodiments, and the specific structure thereof is allowed to vary. All changes which come within the meaning and range of equivalency of the claims are to be embraced within their scope.
Claims (6)
1. A high entropy perovskite ferrate infrared radiation material, characterized by: the chemical formula of the high entropy perovskite ferrite infrared radiation material is ABO 3; the A site is any five elements in rare earth elements La, pr, ca, ce, gd, sm, nd, dy, coordinates with 12 oxygen ions and is positioned in a cavity formed by octahedron; b is transition metal element Fe, and the cation and six oxygen ions form octahedral coordination.
2. A ferrate perovskite infrared radiation material as recited in claim 1, wherein: the infrared radiation rate of the high-entropy ferrite perovskite infrared radiation material in a wave band of 0.78-16 mu m is 0.85-0.88.
3. A method for preparing a ferrate perovskite infrared radiation material according to claim 1 or 2, wherein: the method is characterized in that any five of La2O3、Pr6O11、CaO、Ce2O3、Gd2O3、Sm2O3、Nd2O3、Dy2O3 powder and Fe 2O3 are used as raw materials, and the molar ratio of metal atoms is 1:1:1:1:1:5, ball milling and mixing, and drying and grinding to obtain mixture powder; and calcining the mixture powder in a muffle furnace at high temperature, and cooling and grinding to obtain the high-entropy perovskite infrared radiation material.
4. A method for producing a ferrate perovskite infrared radiation material as claimed in claim 3, wherein: the ball milling and mixing conditions are that a planetary ball mill is adopted for wet ball milling, the ball milling rotating speed is 300-500 r/min, the ball milling time is 12-24 hours, and the mass ratio of ball materials to absolute ethyl alcohol is 2-5: 1:3.
5. A method for producing a ferrate perovskite infrared radiation material as claimed in claim 3, wherein: the high-temperature calcination condition means that the calcination temperature is 1000-1500 ℃, the heating rate is 3-5 ℃/min, and the calcination time is 4-10 hours.
6. A method for producing a ferrate perovskite infrared radiation material as claimed in claim 3, wherein: the cooling mode is one of furnace-following cooling, air quenching cooling and liquid nitrogen quenching cooling.
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