CN113443654A - Rare earth doped spinel material with electromagnetic wave regulation and control function and preparation thereof - Google Patents
Rare earth doped spinel material with electromagnetic wave regulation and control function and preparation thereof Download PDFInfo
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Abstract
The invention relates to a rare earth doped spinel material with an electromagnetic wave regulation function, which has a spinel crystal structure, the particle diameter of the material is 100-700 nm, and the chemical general formula of the material is CuCrMn1‑yREyO4Wherein RE is Ce or La, and y is more than or equal to 0 and less than or equal to 0.20; the solar energy absorptivity at the wave band of 0.3-2.5 μm and the normal infrared emissivity at 2-22 μm are regulated and controlled by electromagnetic waves. Meanwhile, the invention also discloses a preparation method of the material. The rare earth doped spinel material can be regulated and controlled by electromagnetic waves, so that the solar energy absorptivity of the rare earth doped spinel material in a wave band of 0.3-2.5 mu m is more than or equal to 0.87, the normal infrared emissivity of the rare earth doped spinel material in a wave band of 2-22 mu m is more than or equal to 0.92, and the rare earth doped spinel material has good thermal stability in air.
Description
Technical Field
The invention relates to the field of new materials, in particular to a rare earth doped spinel material with an electromagnetic wave regulation function and a preparation method thereof.
Background
With the development of economy and social progress, people put higher and higher requirements on energy, and the search for new energy becomes an urgent subject facing human beings at present. The development and research of novel renewable energy sources become the key point and the trend of the global energy development. The focusing solar thermal power generation system converts solar radiation energy into high-temperature heat energy by utilizing a heat collector through heating water or other working media, and then generates power through a heat circulation process, is a clean and environment-friendly renewable power generation technology, and becomes one of ideal ways for solving energy problems in the future. The solar energy absorbing material is a core material for realizing photothermal conversion, and the light absorption capacity of the solar energy absorbing material in a wave band of 0.3-2.5 mu m plays an important role in photothermal conversion efficiency. Spinel type transition metal oxide is an important solar heat absorbing material, and Chinese invention patent (publication No. CN 102286243B) of Liu just, Gunn Gengfen and the like, a method for preparing solar selective heat absorbing paint by taking spinel type pigment as light absorbing agent, and the like, gel-gel self-propagating combustion method is adopted to prepare fluffy powder, and the spinel type transition oxide powder is obtained through complicated preparation process. However, the spinel-type transition oxide powder prepared by the method has the defects of high cost, complex preparation process, difficulty in control and the like.
The infrared radiation material is characterized in that the energy obtained from the base material is radiated outwards efficiently and quickly in the form of electromagnetic wave radiation, so that the temperature of the base is reduced to achieve the effect of energy conservation; meanwhile, the infrared radiation material can also convert heat energy into infrared radiation energy, and the infrared radiation energy is directly radiated to a heated object in the form of electromagnetic waves to cause molecular resonance and rapidly raise the temperature, so that the heating purpose is achieved. This material has been expanded from the first dry heating to various fields of aerospace, industrial kilns, architectural coatings, health care, medical care, and the like. At present, domestic and overseas research is focused on taking spinel synthesized by transition metal oxide as an infrared radiation material, the spinel type infrared radiation material has high phase stability and infrared emissivity, in the Chinese invention patent (an authorization publication number CN 103771530B) applied by the soldiers and the like, namely, the rare earth element doped spinel structure infrared radiation material and the preparation method, metal nitrate and complexing agent citric acid are adopted, the mixture is stirred in a water bath condition at the temperature of 80-85 ℃ to obtain gel, the obtained gel is placed in an oven at the temperature of 100-120 ℃ to be dried for 3-5 hours to obtain dry gel, then self-propagating combustion is carried out to obtain fluffy powder, the fluffy powder is ground, sieved, sintered for 1-2 hours at the temperature of 600-800 ℃, and cooled to obtain the spinel structure infrared radiation material. However, the spinel-structured infrared radiation material prepared by the method has the characteristics of high raw material cost, multiple preparation steps, complex process, difficulty in control and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a rare earth doped spinel material which has high solar absorptivity and high normal infrared emissivity and has an electromagnetic wave regulation function.
The invention aims to solve another technical problem of providing the preparation of the rare earth doped spinel material with the electromagnetic wave regulation function.
In order to solve the above problems, the rare earth doped spinel material with electromagnetic wave regulation function of the present invention is characterized in that: the material has a spinel crystal structure, the particle diameter of the material is 100-700 nm, and the chemical general formula of the material is CuCrMn1-yREyO4Wherein RE is Ce or La, and y is more than or equal to 0 and less than or equal to 0.20; the solar energy absorptivity at the wave band of 0.3-2.5 μm and the normal infrared emissivity at 2-22 μm are regulated and controlled by electromagnetic waves.
The preparation method of the rare earth doped spinel material with the electromagnetic wave regulation function is characterized by comprising the following steps: firstly, CuO and Cr are added2O3、MnO2、REOxThe powder is prepared by the following steps of 1: 1: 1-y: weighing the molar ratio of the metal elements of y, and then performing ball milling, mixing, drying and grinding to obtain mixture powder; calcining the mixture powder at high temperature in an air atmosphere, cooling and grinding the mixture powder until the particle diameter is 100-700 nm to obtain the powder; the REOxRefers to CeO2Or La2O3(ii) a The value range of y is 0-0.20.
The ball milling conditions are that a planetary ball mill is adopted, the ball milling rotating speed is 300-500 r/min, the ball milling time is 5-12 hours, and the mass ratio of ball material to water is 2-5: 1: 3.
the drying condition is that the temperature is 75-85 ℃ and the time is 10-14 h.
The high-temperature calcination condition is that the calcination temperature is 600-900 ℃, the heating rate is 10-15 ℃/min, and the calcination time is 2-6 hours.
The cooling mode is one of furnace cooling, air quenching cooling and liquid nitrogen quenching cooling.
Compared with the prior art, the invention has the following advantages:
1. the invention uses rare earth element Ce4+Or La3+The doping of the alloy changes the original CuCrMnO4The crystal crystallization condition and the lattice distortion are caused, the original lattice vibration period is destroyed, and the lattice vibration is increased, so that the light absorption performance of the material is improved, and the segregation of the traditional spinel is avoided.
2. The method for preparing the rare earth doped spinel material by combining the mechanical wet grinding method mixing with the solid phase synthesis method has the advantages of simple operation, high production efficiency, no need of complex post-treatment, realization of industrial production and the like.
3. The rare earth doped spinel material prepared by the invention can be regulated and controlled by electromagnetic waves, so that the solar energy absorptivity of the rare earth doped spinel material in a wave band of 0.3-2.5 mu m is more than or equal to 0.87, the normal infrared emissivity of 2-22 mu m is more than or equal to 0.92, and a thermal stability experiment is carried out in 1000 ℃ air for 100h, and the result shows that the crystal structure is stable, which indicates that the material has good thermal stability.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 shows CuCrMn prepared in example 2 of the present invention0.99Ce0.01O4XRD pattern of (a).
FIG. 2 shows CuCrMn prepared in example 3 of the present invention0.99La0.01O4XRD pattern of (a).
FIG. 3 shows CuCrMn prepared in example 3 of the present invention0.99La0.01O4SEM image of (d).
Detailed Description
Electromagnetic wave modulatorThe rare earth doped spinel material with the controlled function has a spinel crystal structure, the particle diameter of the material is 100-700 nm, and the chemical general formula of the material is CuCrMn1-yREyO4Wherein RE is Ce or La, and y is more than or equal to 0 and less than or equal to 0.20; the solar energy absorptivity at the wave band of 0.3-2.5 μm and the normal infrared emissivity at 2-22 μm are regulated and controlled by electromagnetic waves.
The preparation method comprises the following steps: firstly, CuO and Cr are added2O3、MnO2、REOxThe powder is prepared by the following steps of 1: 1: 1-y: weighing the molar ratio of the metal elements of y, and then performing ball milling, mixing, drying and grinding to obtain mixture powder; the mixture powder is calcined at high temperature in the air atmosphere, cooled and ground until the particle diameter is 100-700 nm.
Wherein: REOxRefers to CeO2Or La2O3(ii) a The value range of y is 0-0.20.
The ball milling conditions are that a planetary ball mill is adopted, the ball milling rotating speed is 300-500 r/min, the ball milling time is 5-12 hours, and the mass ratio of ball material to water is 2-5: 1: 3.
the drying condition is that the temperature is 75-85 ℃ and the time is 10-14 h.
The high-temperature calcination condition is that the calcination temperature is 600-900 ℃, the heating rate is 10-15 ℃/min, and the calcination time is 2-6 hours.
The cooling mode is one of furnace cooling, air quenching cooling and liquid nitrogen quenching cooling.
Embodiment 1A rare earth doped spinel material with electromagnetic wave control function has a chemical composition formula of CuCrMnO4. The preparation process comprises the following steps:
according to the molar ratio of metal elements of 1: 1: 1 weighing CuO (15.910 g) and Cr respectively2O3（15.199g）、MnO2(17.388 g) powder; pressing a ball: material preparation: the mass ratio of water is 2: 1: 3, respectively pouring the ball milling beads, the raw materials and ultrapure water into a ball milling tank; placing the ball milling tank on a ball milling machine station, firstly performing ball milling for 1 hour at the rotating speed of 300r/min, then pausing for 10 minutes, taking the ball milling period as one ball milling period, performing ball milling for 1 hour after 10 minutes, wherein the rotating speed is 300r/min, and performing ball milling for 5 hours in total to obtain the ball milling productMixing the powder; then drying and grinding the mixture powder obtained after ball milling; then the ground mixture powder is heated to 600 ℃ in the air atmosphere of a box-type resistance furnace for calcination, the heating rate is 10 ℃/min, the calcination time is 2 hours, and the mixture powder is cooled to room temperature along with the furnace after calcination to obtain the CuCrMnO4A spinel material.
0.2g of the CuCrMnO was taken4The spinel material is evaluated for solar absorptivity by a Lambda 950 type ultraviolet/visible/near infrared spectrophotometer (equipped with a 150mm integrating sphere) manufactured by PerkinElmer company in America, and then the solar absorptivity is calculated according to a calculation formula in international standard ISO 9845-1 (1992), and the solar absorptivity of the spinel material in a wave band of 0.3-2.5 mu m is measured to be 0.87. The infrared emissivity of the rare earth doped spinel material is evaluated by adopting a TSS-5X-2 infrared emissivity detector manufactured by the Japan Senor company, and the normal infrared emissivity of the rare earth doped spinel material in a 2-22 mu m wave band is measured to be 0.91.
Embodiment 2A rare earth doped spinel material with electromagnetic wave control function has a chemical composition formula of CuCrMn0.99Ce0.01O4. The preparation process comprises the following steps:
according to the molar ratio of metal elements of 1: 1: 0.99: 0.01 separately weighed CuO (15.910 g) and Cr2O3（15.199g）、MnO2（17.214g）、CeO2(0.344 g) powder; pressing a ball: material preparation: the mass ratio of water is 4: 1: 3, respectively pouring the ball milling beads, the raw materials and ultrapure water into a ball milling tank; placing a ball milling tank on a ball milling machine station, firstly carrying out ball milling for 1 hour at the rotation speed of 450r/min, then pausing for 10 minutes, taking the ball milling period as one ball milling period, carrying out ball milling for 1 hour after 10 minutes, and carrying out ball milling at the rotation speed of 450r/min for 8 hours in total to obtain mixed powder; then drying and grinding the mixture powder obtained after ball milling; then heating the ground mixture powder to 900 ℃ in the air atmosphere of a box-type resistance furnace for calcination, wherein the heating rate is 12 ℃/min, the calcination time is 3 hours, and air quenching and cooling are carried out after calcination to room temperature, thus obtaining the CuCrMn0.99Ce0.01O4A spinel material.
For the CuCrMn0.99Ce0.01O4X-ray diffraction test of spinel material shows that the obtained material has CuCrMnO4Spinel structure, and good crystal structure and growth state (as shown in figure 1).
0.2g of the CuCrMn is taken0.99Ce0.01O4The spinel material is respectively subjected to solar absorptivity and infrared emissivity tests, the test method is the same as that of the spinel material in example 1, and the result shows that the normal infrared emissivity of the spinel material in a 2-22 mu m wave band is 0.94, and the solar absorptivity of the spinel material in a 0.3-2.5 mu m wave band is 0.92.
Embodiment 3A rare earth doped spinel material with electromagnetic wave control function has a chemical composition formula of CuCrMn0.99La0.01O4. The preparation process comprises the following steps:
according to the molar ratio of metal elements of 1: 1: 0.99: 0.01 separately weighed CuO (15.910 g) and Cr2O3（15.199g）、MnO2（17.214g）、La2O3(0.326 g) powder; pressing a ball: material preparation: the mass ratio of water is 4: 1: 3, respectively pouring the ball milling beads, the raw materials and ultrapure water into a ball milling tank; placing a ball milling tank on a ball milling machine station, performing ball milling for 1 hour at the rotation speed of 400r/min, then pausing for 10 minutes, taking the ball milling period as one ball milling period, performing ball milling for 1 hour after 10 minutes, and performing ball milling for 9 hours at the rotation speed of 400r/min to obtain mixed powder; then drying and grinding the mixture powder obtained after ball milling; then heating the ground mixture powder to 875 ℃ in the air atmosphere of a box-type resistance furnace for calcination at the heating rate of 11 ℃/min for 4.5 hours, and cooling the calcined mixture powder to room temperature along with the furnace to obtain the CuCrMn0.99La0.01O4A spinel material.
For the CuCrMn0.99La0.01O4X-ray diffraction test of spinel material shows that the obtained material has CuCrMnO4Spinel structure, and good crystal structure and growth state (as shown in figure 2).
0.2g of the CuCrMn is taken0.99La0.01O4The spinel material is respectively subjected to solar energy absorptivity and infrared emissivity tests, and the test method is the same as the test methodThe result of example 1 shows that the normal infrared emissivity of the material in a 2-22 mu m wave band is 0.94, and the solar energy absorptivity of the material in a 0.3-2.5 mu m wave band is 0.91.
For the CuCrMn0.99La0.01O4Scanning the spinel material by an electron microscope, wherein the particle diameter is 100-700 nm (shown in figure 3).
Embodiment 4A rare earth doped spinel material with electromagnetic wave control function has a chemical composition formula of CuCrMn0.8Ce0.2O4. The preparation process comprises the following steps:
according to the molar ratio of metal elements of 1: 1: 0.8: 0.2 weighing CuO (15.910 g) and Cr respectively2O3（15.199g）、MnO2（13.910g）、CeO2(6.884 g) powder; pressing a ball: material preparation: the mass ratio of water is 5: 1: 3, respectively pouring the ball milling beads, the raw materials and ultrapure water into a ball milling tank; placing a ball milling tank on a ball milling machine station, firstly carrying out ball milling for 1 hour at the rotation speed of 500r/min, then pausing for 10 minutes, taking the ball milling period as one ball milling period, carrying out ball milling for 1 hour after 10 minutes, and carrying out ball milling at the rotation speed of 500r/min for 12 hours in total to obtain mixed powder; then drying and grinding the mixture powder obtained after ball milling; then heating the ground mixture powder to 900 ℃ in the air atmosphere of a box-type resistance furnace for calcination, wherein the heating rate is 13 ℃/min, the calcination time is 7 hours, and air quenching and cooling are carried out after calcination to room temperature, thus obtaining the CuCrMn0.8Ce0.2O4A spinel material.
0.2g of the CuCrMn is taken0.8Ce0.2O4The spinel material is respectively subjected to solar absorptivity and infrared emissivity tests, the test method is the same as that of the spinel material in example 1, and the result shows that the normal infrared emissivity of the spinel material in a 2-22 mu m wave band is 0.90, and the solar absorptivity of the spinel material in a 0.3-2.5 mu m wave band is 0.91.
Embodiment 5A rare earth-doped spinel material with electromagnetic wave control function has a chemical composition formula of CuCrMn0.8La0.2O4. The preparation process comprises the following steps:
according to the molar ratio of metal elements of 1: 1: 0.8: 0.2 weighing CuO (15.910 g) and Cr respectively2O3（15.199g）、MnO2（13.910g）、La2O3(6.517 g) powder; pressing a ball: material preparation: the mass ratio of water is 5: 1: 3, respectively pouring the ball milling beads, the raw materials and ultrapure water into a ball milling tank; placing a ball milling tank on a ball milling machine station, firstly carrying out ball milling for 1 hour at the rotation speed of 500r/min, then pausing for 10 minutes, taking the ball milling period as one ball milling period, carrying out ball milling for 1 hour after 10 minutes, and carrying out ball milling at the rotation speed of 500r/min for 12 hours in total to obtain mixed powder; then drying and grinding the mixture powder obtained after ball milling; heating the ground mixture powder to 900 ℃ in the air atmosphere of a box-type resistance furnace for calcination at the heating rate of 15 ℃/min for 7 hours, and cooling the calcined mixture powder to room temperature along with the furnace to obtain the CuCrMn0.8La0.2O4A spinel material.
0.2g of the CuCrMn is taken0.8La0.2O4The spinel material is respectively subjected to solar absorptivity and infrared emissivity tests, and the test method is the same as that of the spinel material in example 1, and the result shows that the normal infrared emissivity of the spinel material in a 2-22 mu m wave band is 0.92, and the solar absorptivity of the spinel material in a 0.3-2.5 mu m wave band is 0.89.
Claims (6)
1. A rare earth doped spinel material with an electromagnetic wave regulation function is characterized in that: the material has a spinel crystal structure, the particle diameter of the material is 100-700 nm, and the chemical general formula of the material is CuCrMn1-yREyO4Wherein RE is Ce or La, and y is more than or equal to 0 and less than or equal to 0.20; the solar energy absorptivity at the wave band of 0.3-2.5 μm and the normal infrared emissivity at 2-22 μm are regulated and controlled by electromagnetic waves.
2. The method for preparing a rare earth doped spinel material with electromagnetic wave regulation function of claim 1, wherein: firstly, CuO and Cr are added2O3、MnO2、REOxThe powder is prepared by the following steps of 1: 1: 1-y: weighing the molar ratio of the metal elements of y, and then performing ball milling, mixing, drying and grinding to obtain mixture powder; calcining the mixture powder at high temperature in an air atmosphere, cooling and grinding the mixture powder until the particle diameter is 100-700 nm to obtain the powder; the REOxRefers to CeO2Or La2O3(ii) a The value range of y is 0-0.20.
3. The method for preparing a rare earth doped spinel material with electromagnetic wave regulation function of claim 2, wherein: the ball milling conditions are that a planetary ball mill is adopted, the ball milling rotating speed is 300-500 r/min, the ball milling time is 5-12 hours, and the mass ratio of ball material to water is 2-5: 1: 3.
4. the method for preparing a rare earth doped spinel material with electromagnetic wave regulation function of claim 2, wherein: the drying condition is that the temperature is 75-85 ℃ and the time is 10-14 h.
5. The method for preparing a rare earth doped spinel material with electromagnetic wave regulation function of claim 2, wherein: the high-temperature calcination condition is that the calcination temperature is 600-900 ℃, the heating rate is 10-15 ℃/min, and the calcination time is 2-6 hours.
6. The method for preparing a rare earth doped spinel material with electromagnetic wave regulation function of claim 2, wherein: the cooling mode is one of furnace cooling, air quenching cooling and liquid nitrogen quenching cooling.
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| CN115724658B (en) * | 2022-12-02 | 2024-03-01 | 中国科学院兰州化学物理研究所 | High-temperature high-emissivity protective coating for coal-fired boiler and preparation method thereof |
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