CN115571916A - Wave absorbing agent and preparation method thereof, wave absorbing material and stealth equipment - Google Patents
Wave absorbing agent and preparation method thereof, wave absorbing material and stealth equipment Download PDFInfo
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Abstract
The application relates to the technical field of wave-absorbing materials, in particular to a wave-absorbing agent, a preparation method thereof, a wave-absorbing material and stealth equipment. The wave absorber has a chemical formula of M 2 XYO 6 Wherein, the M element is selected from Be, mg, ca, sr or Ba, the X element is selected from Ti, zr or Hf, and the Y element is selected from Cr, mo or W. The wave absorbing agent has excellent wave absorbing performance, and the preparation method is simple and low in cost.
Description
Technical Field
The application relates to the technical field of wave-absorbing materials, in particular to a wave-absorbing agent, a preparation method thereof, a wave-absorbing material and stealth equipment.
Background
The radar wave-absorbing material can effectively reduce the radar scattering sectional area of a target object so as to reduce the radar detection precision, thereby improving the survival capability and the penetration resistance of weaponry. Meanwhile, with the rapid development of modern electronic communication technology, electromagnetic pollution becomes the fifth largest pollution source following atmospheric pollution, noise pollution, water pollution and solid waste pollution, and poses serious threat to human life health. The absorption effect of the wave-absorbing material on electromagnetic waves can be utilized to effectively reduce the pollution, and simultaneously, secondary pollution caused by the electromagnetic shielding effect can be prevented.
Absorbing materials can be generally classified into dielectric loss materials and magnetic loss materials. Dielectric loss materials mainly lose incident electromagnetic waves by means of electron polarization, dipole polarization, space charge polarization, leakage conduction loss and the like. Magnetic loss materials mainly lose incident electromagnetic waves by means of hysteresis loss, eddy current loss, ferromagnetic resonance, dimensional resonance, domain wall resonance, natural resonance, and the like. Since the magnetic loss material has the defects of low curie temperature, high density and the like, the practical application thereof is limited. Dielectric materials are popular among researchers because of their wide variety and different properties, and thus have a wide range of selectivity as wave-absorbing materials.
The low-dimensional and structural development of dielectric loss materials and magnetic loss materials is an effective means for improving the wave absorption performance of the materials. Due to the limitation of physical properties, the traditional wave-absorbing material has poor wave-absorbing performance when the thickness of the material is small. In addition, the traditional low-dimensional wave-absorbing material prepared by acid solution etching, chemical vapor deposition and sol-gel method has the defects of complicated preparation process, economy, environmental protection and the like, and is not beneficial to batch production.
Disclosure of Invention
Based on the above, it is necessary to provide a wave absorbing agent, a preparation method thereof, a wave absorbing material and stealth equipment, which can improve the wave absorbing performance and have simple process and low cost.
In one aspect of the present application, a wave absorbing agent is provided, wherein the wave absorbing agent has a chemical formula of M 2 XYO 6 Wherein, M element is selected from Be, mg, ca, sr or Ba, X element is selected from Ti, zr or Hf, and Y element is selected from Cr, mo or W.
In one embodiment, the wave absorbing agent is powder, and the particle size of the wave absorbing agent is 0.01-10 μm.
On one hand, the wave absorbing material comprises a wave transmitting agent and the wave absorbing agent.
In one embodiment, the wave-absorbing material is a wave-absorbing film or a wave-absorbing coating, and the thickness of the wave-absorbing material is 0.5 mm-2 mm.
In one embodiment, the wave-transmitting agent includes one or more of a resin, a paraffin, and an electrically insulating oxide.
In one embodiment, the thickness of the wave-absorbing material is 1 mm-1.5 mm.
In one embodiment, the wave-absorbing material has a wave-absorbing frequency of 1 GHz-18 GHz, and a reflection loss of-1 dB-16 dB.
In one aspect of the present application, there is further provided a method for preparing a wave absorber, comprising the following steps:
mixing M source, X source and Y source in the presence of O 2 Is sintered for one time under the first atmosphere and then contains H 2 Performing secondary sintering in a second atmosphere; the M source, the X source and the Y source are respectively selected from M element-containing carbonate and/or oxide, X element-containing oxide and Y element-containing oxide, wherein the M element is selected from Be, mg, ca, sr or Ba, the X element is selected from Ti, zr or Hf, and the Y element is selected from Cr, mo or W.
In one embodiment, the temperature of the first sintering and the second sintering is 800-1000 ℃ respectively and independently, the time is 8-12 h respectively and independently, and the heating rate is 3-5 ℃/min respectively and independently.
In one embodiment, the second atmosphere further comprises Ar or N 2 。
In another aspect of the present application, a stealth device is provided, which includes a device body and a wave-absorbing material layer formed on the surface of the device body, wherein the wave-absorbing material layer is made of a material including the wave-absorbing material described above.
The wave absorbing agent has high electromagnetic loss characteristic and can be used in the field of electromagnetic stealth. The wave-absorbing material prepared by the method has wide wave-absorbing bandwidth and low reflection loss, for example, when the thickness of the wave-absorbing material is only 0.8 mm-1.2 mm, the effective wave-absorbing bandwidth with the reflection loss value less than-10 dB at least reaches 3.3GHz, and the wave-absorbing material can cover the whole X wave band.
The wave absorbing agent is simple in preparation method, the material with the wave absorbing performance can be formed only by sintering twice, and processing and design of special shapes are not needed. Compared with the traditional method for preparing the special micro-morphology by an acid solution etching method, chemical vapor deposition or sol-gel method and the like, the method provided by the application does not relate to chemical synthesis and has no pollution reactionThe product is more environment-friendly. In addition, compared with the traditional mode that the wave absorption performance can be better only by preparing special micro-morphology, such as SiC nanowire, magnetic nanoparticle modified multi-wall carbon nanotube and nano hollow structure (Zn) x Fe 3-x O 4 ) And the C-coated ZnO nanowire and the like, the wave absorbing agent provided by the application does not need to have a special shape, and the processing convenience and the economical efficiency are improved.
In addition, the wave-absorbing material provided by the application has the advantages of good wave-absorbing performance, thin thickness, simple process and strong controllability, and is suitable for industrial and large-scale production.
Drawings
In order to more clearly illustrate the detailed description of the present application or the technical solutions in the prior art, the drawings needed to be used in the detailed description of the present application or the prior art description will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 shows Sr obtained in example 1 of the present application 2 TiMoO 6 XRD pattern of (a);
FIG. 2 shows Sr produced in example 1 of the present application 2 TiMoO 6 SEM picture of (g);
FIG. 3 shows Sr obtained in example 1 of the present application 2 TiMoO 6 Distribution diagram of medium Sr element;
FIG. 4 shows Sr obtained in example 1 of the present application 2 TiMoO 6 Distribution diagram of medium Ti element;
FIG. 5 shows Sr obtained in example 1 of the present application 2 TiMoO 6 Distribution diagram of the medium Mo element;
FIG. 6 shows Sr produced in example 1 of the present application 2 TiMoO 6 Distribution diagram of medium O element;
FIG. 7 shows Sr produced in example 1 of the present application 2 TiMoO 6 Reflection loss performance plot in the bandwidth range of 1 GHz-18 GHz.
Detailed Description
To facilitate an understanding of the present application, the present application will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present application are shown in the drawings. This application may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items. In the description herein, "plurality" means at least two, e.g., two, three, etc., unless explicitly specified otherwise. The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
Other than as shown in the operating examples, or where otherwise indicated, all numbers expressing quantities of ingredients, physical and chemical properties, and so forth used in the specification and claims are to be understood as being modified in all instances by the term "about". For example, unless indicated to the contrary, the numerical parameters set forth in the foregoing specification and attached claims are approximations that can be suitably varied by those skilled in the art in seeking to obtain the desired properties utilizing the teachings disclosed herein. The use of numerical ranges by endpoints includes all numbers within that range and any range within that range, for example, 1 to 5 includes 1, 1.1, 1.3, 1.5, 2, 2.75, 3, 3.80, 4, and 5, and the like.
Herein, "preferred" merely describes a more effective embodiment or example, and it should be understood that the scope of the present invention is not limited thereto.
As used herein, "optionally," "optional," and "optional" refer to being optional, i.e., to being selected from either "with" or "without" either of the two side-by-side schemes. If multiple optional parts appear in one technical scheme, if no special description exists, and no contradiction or mutual constraint relation exists, each optional part is independent.
Herein, the terms "first," "second," "third," "fourth," and the like, in the context of "first purpose," "second purpose," "third purpose," "fourth purpose," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or quantity, nor is it to be construed as implicitly indicating the importance or quantity of the technical feature being indicated. Also, "first," "second," "third," "fourth," etc. are used for non-exhaustive enumeration of description purposes only and should not be construed as a closed limitation to the number.
The temperature parameter herein is not particularly limited, and is allowed to be constant temperature treatment or to vary within a certain temperature range. It will be appreciated that the described thermostatic process allows the temperature to fluctuate within the accuracy of the instrument control. For example, fluctuations in the range of, for example,. + -. 5 ℃,. + -. 4 ℃,. + -. 3 ℃,. + -. 2 ℃,. + -. 1 ℃ are allowed.
Aiming at the defects that the preparation method of the high-performance radar wave-absorbing material in the prior art is complex, high in cost, not suitable for batch production and large-scale application and the like, the application provides the wave-absorbing agent which is simple in preparation method, low in cost, strong in synthesis controllability, good in powder wave-absorbing performance and suitable for batch production and large-scale application. The composite material has conductivity and excellent wave-absorbing performance, and can be used in the field of electromagnetic stealth. The wave-absorbing material has wide wave-absorbing bandwidth and low reflection loss, for example, when the thickness of the wave-absorbing material is only 0.8 mm-1.2 mm, the effective wave-absorbing bandwidth with the reflection loss value less than-10 dB at least reaches 3.3GHz, and the wave-absorbing material can cover the whole X wave band (8.2 GHz-12.4 GHz).
The first objective of the present application is to provide a wave absorber with a chemical formula of M 2 XYO 6 Wherein, M element is selected from beryllium (Be), magnesium (Mg), calcium (Ca), strontium (Sr) or barium (Ba), X element is selected from titanium (Ti), zirconium (Zr) or hafnium (Hf), and Y element is selected from chromium (Cr), molybdenum (Mo) or tungsten (W).
In some embodiments, the wave absorber may have the formula Sr 2 TiMoO 6 、Sr 2 ZrMoO 6 、Sr 2 TiCrO 6 、Ba 2 HfCrO 6 、Mg 2 TiCrO 6 、Ca 2 ZrMoO 6 、Be 2 HfWO 6 、Sr 2 TiWO 6 And so on. Preferably, the wave absorber has the chemical formula of Sr 2 TiMoO 6 。
In some embodiments, the wave absorbing agent is a powder, and the particle size of the wave absorbing agent may be any value between 0.01 μm and 10 μm, for example, 0.05 μm, 0.08 μm, 0.1 μm, 0.5 μm, 0.2 μm, 0.5 μm, 1 μm, 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm.
The second purpose of the present application also provides a wave-absorbing material, which comprises a wave-transmitting agent and the wave-absorbing agent.
The wave-absorbing material provided by the application has the advantages of good wave-absorbing performance, thin thickness, simple process and strong controllability, and is suitable for industrial and large-scale production. When the thickness of the wave-absorbing material is only 0.8 mm-1.2 mm, the effective wave-absorbing bandwidth with the reflection loss value less than-10 dB at least reaches 3.3GHz, and the wave-absorbing material can cover the whole X wave band.
It can be understood that the wave-absorbing material may be a wave-absorbing film or a wave-absorbing coating. Further, the thickness of the wave-absorbing material can be any value between 0.5mm and 2mm, for example, 1mm, 1.2mm, 1.5mm, 1.8mm. Preferably, the thickness of the wave-absorbing material can be any value between 1mm and 1.5mm.
In some embodiments, the wave-transmitting agent may be any known wave-transmitting agent commonly used in the art, for example, the wave-transmitting agent may be a resin, a paraffin, an electrically insulating oxide, or the like. Wherein the resin can be phenolic resin, polystyrene, polytetrafluoroethylene, etc., and the electrically insulating oxide can be Al 2 O 3 、SiO 2 Mullite, cordierite, etc.
In some embodiments, the weight ratio of the wave transmitting agent to the wave absorbing agent can be 1:1 to 1:4.
In some embodiments, the wave-absorbing material can have a wave-absorbing frequency in any interval between 1GHz and 18GHz, for example, 2GHz-4 GHz, 4GHz-8 GHz, 8GHz-12 GHz, 12 GHz-18 GHz, and a reflection loss in any value between-1 dB and-16 dB.
The third objective of the present application also provides a preparation method of the wave absorbing agent, which comprises the following steps:
mixing M source, X source and Y source in the presence of O 2 Is sintered for one time under the first atmosphere and then contains H 2 Performing secondary sintering in the second atmosphere; the M source, the X source and the Y source are respectively selected from carbonate and/or oxide containing M element, oxide containing X element and oxide containing Y element, wherein the M element is selected from Be, mg, ca, sr or Ba, the X element is selected from Ti, zr or Hf, and the Y element is selected from Cr, mo or W.
The wave absorbing agent provided by the application is simple in preparation method, the material with the wave absorbing performance can be formed only by sintering twice, and processing and design of special shapes are not needed. Compared with the traditional method for preparing the special micro-morphology by an acid solution etching method, chemical vapor deposition or sol-gel method and the like, the method provided by the application does not relate to chemical synthesis, does not have pollution reaction products, and is more environment-friendly. In addition, compared with the traditional mode that the special micro-morphology is required to be prepared to have better wave absorption performance, such as SiC nanowire, magnetic nanoparticle modified multi-walled carbon nanotube and nano hollow structure (Zn) x Fe 3-x O 4 ) And the C-coated ZnO nanowire and the like, the wave absorbing agent provided by the application does not need to have a special shape, and the processing convenience and the economical efficiency are improved.
In some embodiments, the M source may be selected from M-containing carbonates and/or oxides. Wherein the carbonate containing M includes but is not limited to strontium carbonate (SrCO) 3 ) Barium carbonate (BaCO) 3 ) Calcium carbonate (CaCO) 3 ) Magnesium carbonate (MgCO) 3 ) And beryllium carbonate (BeCO) 3 ) One or more of; containing M elementIncluding, but not limited to, one or more of strontium oxide (SrO), barium oxide (BaO), calcium oxide (CaO), magnesium oxide (MgO), and beryllium oxide (BeO).
In some embodiments, the X source may be selected from oxides containing the element X. Wherein the oxide containing X may be titanium oxide (TiO) 2 ) Zirconium oxide (ZrO) 2 ) And hafnium oxide (HfO) 2 ) One or more of (a).
In some embodiments, the Y source may be selected from oxides containing Y elements. The Y-containing oxide specifically includes, but is not limited to, chromium oxide (Cr) 2 O 3 ) Molybdenum oxide (MoO) 3 ) And tungsten oxide (WO) 3 ) One or more of (a).
In some embodiments, the process parameters of the first sintering and the second sintering are not limited, and the process parameters commonly used in the art may be selected. As an illustration, the temperature of the primary sintering can be 800-1000 ℃, the time can be 8-12 h, and the heating rate can be 3-5 ℃/min. The temperature of the secondary sintering can be 800-1000 ℃, the time can be 8-12 h, and the heating rate can be 3-5 ℃/min. It is understood that the process parameters of the primary sintering and the secondary sintering may be the same or different.
In some embodiments, containing O 2 The first atmosphere of (2) may specifically be an air atmosphere and/or an oxygen atmosphere, containing H 2 May be H 2 And a mixed gas atmosphere of Ar, or H 2 And N 2 The mixed gas atmosphere of (4).
In some embodiments, the method for preparing the wave absorber may specifically comprise the following steps:
step S1: according to the formula M 2 XYO 6 And respectively weighing an M source, an X source and a Y source, mixing and preparing mixed powder.
It is understood that the specific manner of mixing is not limited, and the mixing process and parameters commonly used in the art are selected, so as to achieve uniform mixing. For example, the mixing may be performed using a planetary ball milling process.
Step S2: mixing the mixed powder prepared in the step S1Containing O 2 Is performed under the first atmosphere.
And step S3: the product obtained in step S2 is added with H 2 Is subjected to secondary sintering in a second atmosphere.
The fourth purpose of the application is to provide stealthy equipment, which comprises an equipment body and a wave-absorbing material layer formed on the surface of the equipment body, wherein the wave-absorbing material layer is made of the wave-absorbing material.
In some embodiments, the cloaking device may specifically be a device utilizing magnetic cloaking technology, for example, may be an airplane, a wearable device, or the like.
The present application will be described in further detail with reference to specific examples.
Example 1
1. Preparation of wave absorber
This example uses SrCO 3 、TiO 2 And MoO 3 As raw material, the chemical formula of the wave absorbing agent is Sr 2 TiMoO 6 . The steps for preparing the wave absorbing agent are as follows:
(1) Weighing 14.763g SrCO 3 、3.993g TiO 2 And 7.197g MoO 3 And uniformly mixing by adopting a planetary ball milling process to prepare mixed slurry. Wherein the solvent adopted by ball milling is absolute ethyl alcohol, and the ball milling medium is ZrO 2 The ball milling speed is 500rpm, the ball milling time is 10h, and the material-liquid ratio is 1:4;
(2) Placing the mixed slurry prepared in the step (1) into a constant-temperature drying oven at 70 ℃ and preserving heat for 10 hours to remove absolute ethyl alcohol to obtain mixed powder, and sieving the mixed powder with a 200-mesh sieve;
(3) And (3) sintering the mixed powder obtained in the step (2) for 10 hours at 900 ℃ in an air atmosphere to finish primary sintering, so as to obtain a sintered material. Wherein the heating rate and the cooling rate are both 5 ℃/min;
(4) Sintering the sintering material obtained in the step (3) in a tubular furnace at 1000 ℃ for 10 hours in a weak reducing atmosphere to finish secondary sintering, thus obtaining Sr 2 TiMoO 6 A wave absorbing agent. Wherein the weak reducing atmosphere is composed of 5% by weight of hydrogen and 95% by weight of hydrogenThe argon gas is mixed, the tube furnace is always kept in a positive pressure state in the reaction, the gas flow is more than 0.1mL/min, and the heating and cooling speeds are both 5 ℃/min.
Sr produced in this example 2 TiMoO 6 The XRD pattern of the crystal is shown in FIG. 1, the morphology is shown in FIG. 2, and the distributions of Sr element, ti element, mo element and O element in the wave absorber are shown in FIGS. 3 to 6, respectively. As can be seen, this example produced Sr, a chemical formula 2 TiMoO 6 The wave absorber of (1).
2. Preparation of wave-absorbing material and wave-absorbing performance test
The wave absorber Sr 2 TiMoO 6 The mixture is uniformly mixed with paraffin according to the mass ratio of 4:1, and is subjected to uniaxial compression to prepare a coaxial ring with the hollow diameter of 3.04mm, the outer ring diameter of 7mm and the section thickness of 2mm. And carrying out electromagnetic parameter test on the coaxial ring by adopting a vector network analyzer so as to obtain the reflection loss performance of the wave-absorbing material. The uniaxial compression pressure is 2MPa, the electromagnetic parameter test adopts a frequency sweep model, the test wavelength range is 1 GHz-18 GHz, and the step length is 0.01GHz.
The radar reflection loss performance of the coaxial ring in the range of 1 GHz-18 GHz is measured and is shown in FIG. 7. As can be seen from FIG. 7, the effective wave-absorbing bandwidth covers the whole X-band (8.2 GHz-12.4 GHz), and the bandwidth with the reflection loss value less than-5 dB is 6GHz, which indicates that the wave-absorbing agent has excellent wave-absorbing performance.
Example 2
The method of preparing the wave absorber of example 2 is substantially the same as the method of preparing example 1 except that: replacement of SrO for SrCO 3 (ii) a The method comprises the following specific steps:
in this example, srO and TiO are used 2 And MoO 3 As raw material, the chemical formula of the wave absorbing agent is Sr 2 TiMoO 6 . The steps for preparing the wave absorbing agent are as follows:
(1) 10.362g SrO, 3.993g TiO are weighed 2 And 7.197g MoO 3 And uniformly mixing by adopting a planetary ball milling process to prepare mixed slurry. Wherein the solvent adopted by ball milling is absolute ethyl alcohol, and the ball milling medium is ZrO 2 The ball milling speed is 500rpm,the ball milling time is 10h, and the material-liquid ratio is 1:4;
(2) Placing the mixed slurry prepared in the step (1) into a constant-temperature drying oven at 70 ℃ and preserving heat for 10 hours to remove absolute ethyl alcohol to obtain mixed powder, and sieving the mixed powder with a 200-mesh sieve;
(3) And (3) sintering the mixed powder obtained in the step (2) for 10 hours at 900 ℃ in an air atmosphere to finish primary sintering, so as to obtain a sintered material. Wherein the heating rate and the cooling rate are both 5 ℃/min;
(4) Sintering the sintering material obtained in the step (3) in a tubular furnace at 1000 ℃ for 10 hours in a weak reducing atmosphere to finish secondary sintering, thus obtaining Sr 2 TiMoO 6 A wave absorbing agent. Wherein the weak reducing atmosphere is formed by mixing 5 mass percent of hydrogen and 95 mass percent of argon, the tubular furnace is always kept in a positive pressure state in the reaction, the gas flow is more than 0.1mL/min, and the heating and cooling speeds are both 5 ℃/min.
Example 3
The method of preparing the wave absorber of example 3 is substantially the same as the method of preparing example 1, except that: zrO 2 is mixed with 2 Replacement of TiO 2 (ii) a The method comprises the following specific steps:
this example uses SrCO 3 、ZrO 2 And MoO 3 As raw material, the chemical formula of the wave absorbing agent is Sr 2 ZrMoO 6 . The steps for preparing the wave absorbing agent are as follows:
(1) 14.763g SrCO is weighed 3 、6.161g ZrO 2 And 7.197g MoO 3 And uniformly mixing by adopting a planetary ball milling process to prepare mixed slurry. Wherein the solvent adopted by ball milling is absolute ethyl alcohol, and the ball milling medium is ZrO 2 The ball milling speed is 500rpm, the ball milling time is 10h, and the material-liquid ratio is 1:4;
(2) Placing the mixed slurry prepared in the step (1) into a constant-temperature drying oven at 70 ℃ and preserving heat for 10 hours to remove absolute ethyl alcohol to obtain mixed powder, and sieving the mixed powder with a 200-mesh sieve;
(3) And (3) sintering the mixed powder obtained in the step (2) for 10 hours at 900 ℃ in an air atmosphere to finish primary sintering to obtain a sintered material. Wherein the heating rate and the cooling rate are both 5 ℃/min;
(4) Sintering the sintering material obtained in the step (3) in a tubular furnace at 1000 ℃ for 10 hours in a weak reducing atmosphere to finish secondary sintering to obtain Sr 2 ZrMoO 6 A wave absorbing agent. Wherein the weak reducing atmosphere is formed by mixing 5 mass percent of hydrogen and 95 mass percent of argon, the tubular furnace is always kept in a positive pressure state in the reaction, the gas flow is more than 0.1mL/min, and the heating and cooling speeds are both 5 ℃/min.
Example 4
The method of preparing the wave absorber of example 4 is substantially the same as the method of preparing example 1, except that: mixing Cr 2 O 3 Replacement of MoO 3 (ii) a The method comprises the following specific steps:
this example uses SrCO 3 、TiO 2 And Cr 2 O 3 As raw material, the wave absorbing agent has a chemical formula of Sr 2 TiCrO 6 . The steps for preparing the wave absorbing agent are as follows:
(1) 14.763g SrCO is weighed 3 、3.993g TiO 2 And 3.8g Cr 2 O 3 And uniformly mixing by adopting a planetary ball milling process to prepare mixed slurry. Wherein the solvent adopted by the ball milling is absolute ethyl alcohol, and the ball milling medium is ZrO 2 The ball milling speed is 500rpm, the ball milling time is 10h, and the material-liquid ratio is 1:4;
(2) Placing the mixed slurry prepared in the step (1) into a constant-temperature drying oven at 70 ℃ and preserving heat for 10 hours to remove absolute ethyl alcohol to obtain mixed powder, and sieving the mixed powder with a 200-mesh sieve;
(3) And (3) sintering the mixed powder obtained in the step (2) for 10 hours at 900 ℃ in an air atmosphere to finish primary sintering, so as to obtain a sintered material. Wherein the heating rate and the cooling rate are both 5 ℃/min;
(4) Sintering the sintering material obtained in the step (3) in a tubular furnace at 1000 ℃ for 10 hours in a weak reducing atmosphere to finish secondary sintering to obtain Sr 2 TiCrO 6 A wave absorbing agent. Wherein the weak reducing atmosphere is formed by mixing 5 mass percent of hydrogen and 95 mass percent of argon, and the reaction is carried outThe tube furnace is kept in a positive pressure state all the time, the gas flow is more than 0.1mL/min, and the heating and cooling speeds are both 5 ℃/min.
Example 5
The method of preparing the wave absorber of example 5 is substantially the same as the method of preparing example 1, except that: mixing BaCO 3 Replacement of SrCO 3 ，HfO 2 Replacement of TiO 2 ，Cr 2 O 3 Replacement of MoO 3 (ii) a The method comprises the following specific steps:
this example uses BaCO 3 、HfO 2 And Cr 2 O 3 As raw material, the chemical formula of the wave absorbing agent is Ba 2 HfCrO 6 . The steps for preparing the wave absorbing agent are as follows:
(1) 19.73g of BaCO were weighed 3 、10.525g HfO 2 And 3.8g Cr 2 O 3 And uniformly mixing by adopting a planetary ball milling process to prepare mixed slurry. Wherein the solvent adopted by ball milling is absolute ethyl alcohol, and the ball milling medium is ZrO 2 The ball milling speed is 500rpm, the ball milling time is 10h, and the material-liquid ratio is 1:4;
(2) Placing the mixed slurry prepared in the step (1) into a constant-temperature drying oven at 70 ℃ and preserving heat for 10 hours to remove absolute ethyl alcohol to obtain mixed powder, and sieving the mixed powder with a 200-mesh sieve;
(3) And (3) sintering the mixed powder obtained in the step (2) for 10 hours at 900 ℃ in an air atmosphere to finish primary sintering, so as to obtain a sintered material. Wherein the heating rate and the cooling rate are both 5 ℃/min;
(4) Sintering the sintering material obtained in the step (3) in a tubular furnace at 1000 ℃ for 10 hours in a weak reducing atmosphere to finish secondary sintering to obtain Ba 2 HfCrO 6 A wave absorbing agent. Wherein the weak reducing atmosphere is argon, the tube furnace is always kept in a positive pressure state in the reaction, the gas flow is more than 0.1mL/min, and the heating and cooling speeds are both 5 ℃/min.
The following table 1 shows the raw materials in the method for preparing the wave absorber of examples 1 to 5:
TABLE 1
| Group of | M source (g) | X source (g) | Y source (g) | Chemical formula of wave absorber |
| Example 1 | 14.763g SrCO 3 | 3.993g TiO 2 | 7.197g MoO 3 | Sr 2 TiMoO 6 |
| Example 2 | 10.362g SrO | 3.9935g TiO 2 | 7.197g MoO 3 | Sr 2 TiMoO 6 |
| Example 3 | 14.763g SrCO 3 | 6.161g g ZrO 2 | 7.197g MoO 3 | Sr 2 ZrMoO 6 |
| Example 4 | 14.763g SrCO 3 | 3.993g TiO 2 | 3.8g Cr 2 O 3 | Sr 2 TiCrO 6 |
| Example 5 | 19.73g BaCO 3 | 10.525g HfO 2 | 3.8g Cr 2 O 3 | Ba 2 HfCrO 6 |
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present application, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the concept of the present application, which falls within the scope of protection of the present application. Therefore, the scope of the claims should be determined from the appended claims, and the description and drawings should be used for interpreting the scope of the claims.
Claims (10)
1. The wave absorbing agent is characterized in that the chemical formula of the wave absorbing agent is M 2 XYO 6 Wherein, the M element is selected from Be, mg, ca, sr or Ba, the X element is selected from Ti, zr or Hf, and the Y element is selected from Cr, mo or W.
2. The wave absorber according to claim 1, wherein the wave absorber is a powder, and the particle size of the wave absorber is 0.01 μm to 10 μm.
3. A wave-absorbing material comprising a wave-transmitting agent and the wave-absorbing agent of claim 1 or 2.
4. A wave-absorbing material according to claim 3 having at least one of the following characteristics:
(1) The wave-absorbing material is a wave-absorbing film or a wave-absorbing coating, and the thickness of the wave-absorbing material is 0.5 mm-2 mm;
(2) The wave-transmitting agent comprises one or more of resin, paraffin and electrically insulating oxide.
5. The wave-absorbing material of claim 4, wherein the thickness of the wave-absorbing material is 1mm to 1.5mm.
6. The wave-absorbing material of claim 4, wherein the wave-absorbing frequency of the wave-absorbing material is 1 GHz-18 GHz, and the reflection loss is-1 dB-16 dB.
7. The preparation method of the wave absorbing agent is characterized by comprising the following steps:
mixing M source, X source and Y source in the presence of O 2 Is sintered for one time under the first atmosphere and then contains H 2 Performing secondary sintering in the second atmosphere; the M source, the X source and the Y source are respectively selected from M element-containing carbonate and/or oxide, X element-containing oxide and Y element-containing oxide, wherein the M element is selected from Be, mg, ca, sr or Ba, the X element is selected from Ti, zr or Hf, and the Y element is selected from Cr, mo or W.
8. The method for preparing a wave absorbing agent according to claim 7, wherein the temperatures of the primary sintering and the secondary sintering are 800 ℃ to 1000 ℃ respectively and independently, the time is 8h to 12h respectively and independently, and the heating rates are 3 ℃/min to 5 ℃/min respectively and independently.
9. The method according to any one of claims 6 to 8, wherein the second atmosphere further comprises Ar or N 2 。
10. A stealth device is characterized by comprising a device body and a wave-absorbing material layer formed on the surface of the device body, wherein the wave-absorbing material layer comprises the wave-absorbing material in any one of claims 3 to 6.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102044319A (en) * | 2009-10-23 | 2011-05-04 | 中国科学院物理研究所 | Composite wave absorbing material and preparation method thereof |
| CN104157881A (en) * | 2014-07-31 | 2014-11-19 | 北京科技大学 | Double-perovskite-type anode material and preparation method thereof |
| CN106190119A (en) * | 2016-07-20 | 2016-12-07 | 上海应用技术学院 | A kind of white light LEDs Eu3+the preparation method of doping molybdenum hydrochlorate Hydrargyri Oxydum Rubrum |
| US20180019478A1 (en) * | 2016-07-14 | 2018-01-18 | Institute of Nuclear Energy Research, Atomic Energy Council, Executive Yuan, R.O.C. | Strontium magnesium molybdenum oxide material having double perovskite structure and method for preparing the same |
| CN112275291A (en) * | 2020-09-15 | 2021-01-29 | 上海理工大学 | Iron-doped perovskite intercalated montmorillonite composite catalyst and preparation method and application thereof |
| CN112350075A (en) * | 2020-10-19 | 2021-02-09 | 内蒙古大学 | Multilayer composite material with strong microwave absorption in GHz interval and preparation method thereof |
-
2022
- 2022-10-10 CN CN202311167643.0A patent/CN117228720A/en active Pending
- 2022-10-10 CN CN202211235625.7A patent/CN115571916B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102044319A (en) * | 2009-10-23 | 2011-05-04 | 中国科学院物理研究所 | Composite wave absorbing material and preparation method thereof |
| CN104157881A (en) * | 2014-07-31 | 2014-11-19 | 北京科技大学 | Double-perovskite-type anode material and preparation method thereof |
| US20180019478A1 (en) * | 2016-07-14 | 2018-01-18 | Institute of Nuclear Energy Research, Atomic Energy Council, Executive Yuan, R.O.C. | Strontium magnesium molybdenum oxide material having double perovskite structure and method for preparing the same |
| CN106190119A (en) * | 2016-07-20 | 2016-12-07 | 上海应用技术学院 | A kind of white light LEDs Eu3+the preparation method of doping molybdenum hydrochlorate Hydrargyri Oxydum Rubrum |
| CN112275291A (en) * | 2020-09-15 | 2021-01-29 | 上海理工大学 | Iron-doped perovskite intercalated montmorillonite composite catalyst and preparation method and application thereof |
| CN112350075A (en) * | 2020-10-19 | 2021-02-09 | 内蒙古大学 | Multilayer composite material with strong microwave absorption in GHz interval and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| MANDVI SAXENA ET AL.: ""Environmental friendly Sr2TiMoO6 double perovskite for high temperature thermoelectric applications"", 《SCRIPTA MATERIALIA》, vol. 130, pages 205 - 209, XP029898699, DOI: 10.1016/j.scriptamat.2016.11.033 * |
| TAHER GHRIB ET AL.: ""Structural, Optical and Photocatalytic Activity of The Cerium Doped Ba2TiMoO6 Double Perovskite"", 《RESEARCH SQUARE》, vol. 649, pages 1 - 23 * |
| Y.P. LIU ET AL.: ""Investigation of possible half-metalmaterial on double perovskites Sr2BBO6 (B, B¼3d transition metal)using first-principle calculations"", 《SOLID STATE COMMUNICATIONS》, vol. 152, pages 968 - 973 * |
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