CN118818154A - Method for measuring high-temperature electromagnetic parameters of powdery wave-absorbing material - Google Patents
Method for measuring high-temperature electromagnetic parameters of powdery wave-absorbing material Download PDFInfo
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Abstract
The invention discloses a method for measuring high-temperature electromagnetic parameters of a powdery wave-absorbing material, which comprises the following steps: s1, preparing a powdery wave-absorbing material into a block sample; the method specifically comprises the steps of uniformly mixing and grinding a powdery wave-absorbing material and a high-temperature-resistant wave-transparent material according to a set filler ratio to obtain mixed powder; dripping a preset amount of binder into the mixed powder, and stirring to obtain a mud-like mixed sample; filling the mud-like mixed sample into a mould for compression molding to obtain a blocky sample precursor; naturally drying and solidifying the precursor of the block sample, and then sintering at high temperature under inert atmosphere for further solidification to obtain a block sample; s2, measuring the block sample by adopting a waveguide method to obtain the high-temperature electromagnetic parameters of the powdery wave-absorbing material. The method for measuring the high-temperature electromagnetic parameters of the powdery wave-absorbing material disclosed by the embodiment of the invention is simple to operate, and the prepared block sample has good high-temperature stability and high measurement result accuracy.
Description
Technical Field
The invention belongs to the technical field of measuring electric variables, and particularly relates to a method for measuring high-temperature electromagnetic parameters of a powdery wave-absorbing material.
Background
At present, the high-temperature electromagnetic wave absorption performance of the coated wave absorbing material is mainly tested at high temperature by a waveguide method; however, the waveguide method is used to test a block sample of a certain size, and the coated wave-absorbing material is generally in a powder form. When testing the powdery wave-absorbing material at normal temperature, the powdery wave-absorbing material and paraffin are uniformly mixed according to a certain filler ratio to prepare a block sample with a set size for testing, but when testing the powdery wave-absorbing material in a high-temperature environment, the paraffin is difficult to keep in an original shape, so that the testing is invalid, and corresponding data cannot be obtained.
In order to prepare a block sample for high-temperature test, the existing preparation method is to prepare a sample with a larger than required size from a powdery wave-absorbing material, sinter and deform the sample at a high temperature and then process the sample to the required size, but the method wastes more samples, has low success rate and small application range and has high brittleness requirement on the synthesized sample.
Disclosure of Invention
In view of this, some embodiments disclose a method for measuring a high-temperature electromagnetic parameter of a powdered wave-absorbing material, including:
s1, preparing a powdery wave-absorbing material into a block sample; the method specifically comprises the following steps:
Uniformly mixing and grinding the powdery wave-absorbing material and the high-temperature-resistant wave-transparent material according to a set filler ratio to obtain mixed powder;
dripping a preset amount of binder into the mixed powder, and stirring to obtain a mud-like mixed sample;
Filling the mud-like mixed sample into a mould for compression molding to obtain a blocky sample precursor;
Naturally drying and solidifying the precursor of the block sample, and then sintering at high temperature under inert atmosphere for further solidification to obtain a block sample;
s2, measuring the block sample by adopting a waveguide method to obtain the high-temperature electromagnetic parameters of the powdery wave-absorbing material.
The method for measuring the high-temperature electromagnetic parameters of the powdery wave-absorbing material disclosed by some embodiments has the purity of the high-temperature-resistant wave-transmitting material more than or equal to 99 percent and the granularity less than or equal to 10 mu m.
Some embodiments disclose a method for measuring high-temperature electromagnetic parameters of a powdery wave-absorbing material, wherein the high-temperature-resistant wave-transmitting material is a ceramic wave-transmitting material, an organic resin wave-transmitting material or a phosphate-based wave-transmitting material.
Some embodiments disclose a method for measuring high-temperature electromagnetic parameters of a powdery wave-absorbing material, wherein the ceramic wave-transmitting material is BN, siBNO, siO 2、Si3N4 or Sino.
The embodiment discloses a method for measuring high-temperature electromagnetic parameters of a powdery wave-absorbing material, wherein the organic resin wave-transmitting material is tripropylester cyanuric acid, epoxy resin, polytetrafluoroethylene, phenolic resin, cyanate resin or polyether ether ketone.
Some embodiments disclose a method for measuring high-temperature electromagnetic parameters of a powdery wave-absorbing material, wherein the phosphate-based wave-transmitting material is chromium phosphate, aluminum phosphate or chromium aluminum phosphate.
Some embodiments disclose a method for measuring high-temperature electromagnetic parameters of a powdery wave-absorbing material, wherein the adhesive is an inorganic silicon adhesive, an epoxy resin adhesive, a polyimide adhesive or a pressure-sensitive adhesive.
The embodiment discloses a method for measuring high-temperature electromagnetic parameters of a powdery wave-absorbing material, wherein the pressure intensity of the pressing forming of a mud-like mixed sample is 120-530 kPa.
Some embodiments disclose a method for measuring high-temperature electromagnetic parameters of a powdery wave-absorbing material, wherein the high-temperature sintering temperature of a precursor of a block sample is 300-1000 ℃, the time is 0-10 h, and the heating rate is 1-20 ℃/min.
The embodiment discloses a method for measuring high-temperature electromagnetic parameters of a powdery wave-absorbing material, wherein the inert atmosphere is argon or nitrogen, and the flow rate of the inert atmosphere is 30-70 ml/min.
According to the method for measuring the high-temperature electromagnetic parameters of the powdery wave-absorbing material, disclosed by the embodiment of the invention, the high-temperature-resistant wave-transmitting material and the adhesive are sequentially and uniformly mixed with the powdery wave-absorbing material and then are subjected to compression molding and high-temperature sintering to prepare the block-shaped sample, so that the powdery wave-absorbing material and the high-temperature-resistant wave-transmitting material are tightly combined, the mechanical strength of the block-shaped sample can be enhanced, the integral wave-absorbing performance of the block-shaped sample is kept, the prepared block-shaped sample has good high-temperature stability, abnormal measurement results caused by severe deformation in the high-temperature test process of a waveguide method can be avoided, and the accuracy of the high-temperature test of the waveguide method can be ensured. The method for measuring the high-temperature electromagnetic parameters of the powdery wave-absorbing material disclosed by the embodiment of the invention is simple to operate, and the prepared block sample has good high-temperature stability and high measurement result accuracy.
Drawings
FIG. 1 is a schematic diagram of a bulk sample of example 1;
FIG. 2 example 1 dimensional measurement of a bulk sample;
FIG. 3 is a second plot of the dimensional measurements of the bulk sample of example 1;
FIG. 4 is a graph of test performance for example 1 block samples;
FIG. 5 is a graph of test performance for example 1 block samples;
FIG. 6 is a plot of the intensity of absorption versus frequency for a block sample of example 1.
Detailed Description
The word "embodiment" as used herein does not necessarily mean that any embodiment described as "exemplary" is preferred or advantageous over other embodiments. Performance index testing in the examples of the present application, unless otherwise specified, was performed using conventional testing methods in the art. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the disclosure.
Unless otherwise defined, 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; other test methods and techniques not specifically mentioned in the present application are those commonly used by those skilled in the art.
The terms "substantially" and "about" are used herein to describe small fluctuations. For example, they may refer to less than or equal to ±5%, such as less than or equal to ±2%, such as less than or equal to ±1%, such as less than or equal to ±0.5%, such as less than or equal to ±0.2%, such as less than or equal to ±0.1%, such as less than or equal to ±0.05%. Numerical data presented or represented herein in a range format is used only for convenience and brevity and should therefore be interpreted flexibly to include not only the numerical values explicitly recited as the limits of the range, but also to include all the individual numerical values or sub-ranges encompassed within that range. For example, a numerical range of "1 to 5%" should be interpreted to include not only the explicitly recited values of 1% to 5%, but also include individual values and sub-ranges within the indicated range. Thus, individual values, such as 2%, 3.5% and 4%, and subranges, such as 1% to 3%, 2% to 4% and 3% to 5%, etc., are included in this numerical range. The same principle applies to ranges reciting only one numerical value. Moreover, such an interpretation applies regardless of the breadth of the range or the characteristics being described.
In this document, including the claims, conjunctions such as "comprising," including, "" carrying, "" having, "" containing, "" involving, "" containing, "and the like are to be construed as open-ended, i.e., to mean" including, but not limited to. Only the conjunctions "consisting of … …" and "consisting of … …" are closed conjunctions.
Numerous specific details are set forth in the following examples in order to provide a better understanding of the present application. It will be understood by those skilled in the art that the present application may be practiced without some of these specific details. In the examples, some methods, means, instruments, devices, etc. well known to those skilled in the art are not described in detail in order to highlight the gist of the present application.
On the premise of no conflict, the technical features disclosed by the embodiment of the application can be combined at will, and the obtained technical scheme belongs to the disclosure of the embodiment of the application. It should be noted that the terms "center", "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like refer to the directions or positional relationships based on the directions or positional relationships shown in the drawings, and are merely for convenience of description and to simplify description, and do not indicate or imply that the apparatus or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present application unless otherwise in conflict with the context. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying relative importance unless otherwise conflicting with context.
In some embodiments, the method for measuring the high-temperature electromagnetic parameter of the powdery wave-absorbing material comprises the following steps:
s1, preparing a powdery wave-absorbing material into a block sample; the method specifically comprises the following steps:
Uniformly mixing and grinding the powdery wave-absorbing material and the high-temperature-resistant wave-transparent material according to a set filler ratio to obtain mixed powder; typically, the powdered wave-absorbing material is a high temperature resistant material having a particle size of less than 100 μm, such as nanospheres, nanorods, nanoplatelets of silicon carbide based materials or microparticles of carbon based materials; generally, the selection of the high-temperature-resistant wave-transmitting material is mainly determined according to the system of the powdery wave-absorbing material, and the high-temperature-resistant wave-transmitting material has the characteristic of complete wave transmission, is used for adjusting the proportion of the powdery wave-absorbing material in a block sample, does not react with the powdery wave-absorbing material, does not influence the wave-absorbing performance of the powdery wave-absorbing material, can be well combined with the powdery wave-absorbing material, and does not deform; in some embodiments, the high temperature resistant wave-transparent material is a ceramic wave-transparent material, an organic resin wave-transparent material or a phosphate-based wave-transparent material, the selection of the three wave-transparent materials is mainly determined according to the test temperature of a waveguide method and the high temperature performance of a powdery wave-absorbing material, and when the test temperature is 800 ℃, the high temperature resistant wave-transparent material matched with the silicon carbide wave-absorbing material can be selected from silicon oxide, silicon nitride, and both the silicon oxide and the silicon nitride can not deform and can not chemically react with the silicon carbide at 800 ℃; high temperature resistant wave-transparent material the purity of (2) is more than or equal to 99 percent, the granularity is less than or equal to 10 mu m; in general, the packing ratio of the powdery wave-absorbing material to the high-temperature-resistant wave-transparent material is the same as that of the existing powdery wave-absorbing material to paraffin;
Dripping a preset amount of binder into the mixed powder, and stirring to obtain a mud-like mixed sample; generally, the selection of the binder is determined according to the type of the powdery wave-absorbing material, the type of the high-temperature-resistant wave-transmitting material and the testing temperature; generally, the amount of binder added is proportional to the size of the bulk sample to be prepared, and in some embodiments, the amount of binder added is from 0.2 to 1.5ml; the adhesive is inorganic silicon adhesive, epoxy resin adhesive, polyimide adhesive or pressure sensitive adhesive; the inorganic silicon adhesive can keep better mechanical strength at high temperature, is mainly used for being mixed with the powdery wave-absorbing material containing the silicon element, and can effectively avoid influencing the wave-absorbing performance of the powdery wave-absorbing material containing the silicon element; the epoxy resin adhesive has good corrosion resistance and high forming precision, is mainly used for preparing block samples with small powdery wave-absorbing materials and high size requirements when testing high frequency, but can deform after the temperature of the adhesive is higher than 500 ℃, and needs to be selected according to the testing temperature; polyimide adhesive has good oxidation resistance, when the powdery wave-absorbing material is of an easily oxidized type, the adhesive can be selected to prevent the powdery wave-absorbing material from being oxidized, but the adhesive can only be used at 350 ℃; the pressure sensitive adhesive has better plasticity, is suitable for a low-temperature bonding scene, and the dripping amount of the adhesive is determined by the quality of the powdery wave-absorbing material, so that the obtained mud-like mixed sample cannot be too diluted or too dried so as not to influence the next step of compression molding;
Filling the mud-like mixed sample into a mould for compression molding to obtain a blocky sample precursor; in some embodiments, the pressure of the press forming of the mud-like mixed sample is 120 to 530kPa; in general, a full-automatic tablet press is used for pressing and forming a mud-shaped mixed sample to obtain a blocky sample precursor, the difference value between the upper pressurizing limit and the lower pressurizing limit of the full-automatic tablet press is set to be 0.3 ton, the pressurizing time is 1-5 min, the excessive pressurizing time can cause the sample to stick to a die, and the sample is difficult to take out; the mould pressure is set according to the size of the block sample to be prepared, the size of the block sample is set according to the test frequency of the waveguide method, the test frequency of the waveguide method is different, the size of the prepared block sample is different, and the mould pressure is different; for example, when the test frequency band is 2.17-3.3 GHz, the size of the block sample is recommended to be 86.19mm multiplied by 43.01mm, the tolerance is-0.2 mm, and the pressure is recommended to be 330-530 kPa; when the test frequency band is 3.22-4.9 GHz, the size of the block sample is recommended to be 58.05mm multiplied by 28.96mm, the tolerance is-0.15 mm, and the pressure is recommended to be 240-420 kPa; when the test frequency band is 4.64-7.05 GHz, the size of the block sample is recommended to be 40.305mm multiplied by 20.112mm, the tolerance is-0.1 mm, and the pressure is recommended to be 120-250 kPa; the highest test frequency of the waveguide method is 40GHz, the size of the block sample is reduced along with the increase of the frequency, and the pressure recommended value is correspondingly reduced according to the area equal proportion of the block sample; generally, the pressure intensity of the die is also adjusted according to different powdery wave-absorbing materials so as to enable the obtained massive sample to be compact and complete; the thickness of the block sample is generally 2-4 mm;
Naturally drying and curing the block sample precursor, namely naturally drying the block sample precursor for 2-8 hours in an air environment after demolding, completely drying the block sample precursor, and then sintering at high temperature in an inert atmosphere for further curing to obtain a block sample; the obtained block sample cannot deform in the high-temperature test process, so that the distortion of a measurement result can be avoided;
generally, the sintering parameters are adjusted according to the change of the powdery wave absorbing material and the high temperature resistant wave transmitting material, the sintering temperature is not higher than the testing temperature of the waveguide method, the sintering time is adjusted according to the size of the block sample, the temperature rising rate of the sintering is not too fast, and the complete solidification of the inside of the block sample is required to be ensured; in some embodiments, the bulk sample precursor is sintered at a high temperature of 300-1000 ℃ for 0-10 hours at a rate of 1-20 ℃/min; generally, when the sintering temperature is below 500 ℃, the heating rate is set to be 1-5 ℃/min, and when the sintering temperature is above 500 ℃, the heating rate is set to be 1-20 ℃/min;
generally, setting a block sample precursor in a crucible of a tube furnace for high-temperature sintering, laying graphite sheets or corundum fine particles at the bottom of the crucible for preventing the obtained block sample precursor from adhering to the bottom of the crucible, and polishing the block sample obtained by sintering by using superfine sand paper with the mesh number of 800-1500 after the sintering is finished;
Generally, the inert atmosphere is selected according to the properties of the powdery wave-absorbing material, and the oxidation performance of the powdery wave-absorbing material is not affected; in some embodiments, the inert atmosphere is argon or nitrogen, and the flow rate of the inert atmosphere is set to 30-70 ml/min according to the furnace chamber area of the tube furnace;
S2, measuring a block sample by adopting a waveguide method, generally, measuring the block sample by adopting the existing waveguide method, loading the block sample into a carbon fiber mould, placing the carbon fiber mould on a measuring table, insulating the carbon fiber mould by using a refractory felt, protecting a testing unit by water cooling, and generally testing a group of data at intervals of 100 ℃, wherein in the testing process, the high-temperature electromagnetic parameters of the powdery wave-absorbing material are obtained after the temperature rises to the testing temperature and the temperature is kept for 15 min.
In some embodiments, the ceramic-based wave-transparent material is BN, siBNO, siO 2、Si3N4 or SiNO; the ceramic wave-transmitting material mainly comprises Si, B, N, O elements and the like, and thermodynamic calculation is carried out on the ceramic wave-transmitting material and the powdery wave-absorbing material before use, so that the wave-transmitting material is ensured not to chemically react with the powdery wave-absorbing material in a test temperature range, and the measurement result of the powdery wave-absorbing material is influenced.
In some embodiments, the organic resin-based wave-transparent material is tripropylester isocyanate, epoxy resin, polytetrafluoroethylene, phenolic resin, cyanate resin, or polyetheretherketone; the organic resin wave-transmitting material has the characteristic of high molding precision, and the wave-transmitting material is mainly applied to the test temperature of not more than 500 ℃.
In some embodiments, the phosphate-based wave-transparent material is chromium phosphate, aluminum phosphate, or chromium aluminum phosphate; the wave-transmitting material can resist high temperature of 1500 ℃.
Further exemplary details are described below in connection with the embodiments.
Example 1
FIG. 1 is a schematic illustration of a bulk sample as disclosed in example 1; FIG. 2 is a plot of the dimensional measurements of the bulk sample disclosed in example 1; FIG. 3 is a second plot of the dimensional measurements of the bulk sample disclosed in example 1; FIG. 4 is a graph of test performance of the bulk sample disclosed in example 1; FIG. 5 is a graph of the test performance of the bulk sample disclosed in example 1; fig. 6 is a graph showing the change in the absorption intensity with frequency of the bulk sample disclosed in example 1.
The embodiment discloses a method for measuring high-temperature electromagnetic parameters of a powdery wave-absorbing material, which comprises the following steps:
s1, preparing a powdery wave-absorbing material into a block sample; the method specifically comprises the following steps:
Silicon carbide and silicon oxide were mixed at a ratio of 1:1, uniformly mixing and grinding the filler ratio to obtain mixed powder;
dripping 0.2-1.5 ml of binder into the mixed powder, and stirring to obtain a mud-like mixed sample;
Filling the mud-like mixed sample into a mould for compression molding to obtain a blocky sample precursor;
Naturally drying and solidifying the block sample precursor for 2-8 h in an air environment, and then sintering at a high temperature under an inert atmosphere with a flow rate of 30ml/min for further solidification, wherein the high temperature sintering temperature is 500 ℃, the time is 2h, and the heating rate is 5 ℃/min;
Obtaining a block sample with a length of 22.78mm and a width of 10.34mm as shown in FIGS. 1 to 3;
S2, measuring the block sample by adopting a waveguide method, wherein the test frequency is 8.4-12.4 GHz, and the test temperature is 25 ℃,100 ℃,200 ℃, 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃ and 800 ℃ respectively, so as to obtain the high-temperature electromagnetic parameters of the powdery wave-absorbing material. FIG. 4 is a graph showing the real part of the permittivity of a bulk sample, as shown in FIG. 4, and it can be seen that the permittivity of the bulk sample increases with increasing temperature, without distortion occurring in the entire test frequency range; FIG. 5 is an imaginary part of the dielectric constant of a bulk sample, as shown in FIG. 5, and it can be seen that the dielectric constant of the bulk sample increases with increasing temperature, without distortion over the entire test frequency range; fig. 6 is a graph showing the variation of electromagnetic wave absorption intensity with frequency of a bulk sample, and as shown in fig. 6, the absorption intensity of the bulk sample reaches an optimum of-26.29 dB at 9.6GHz, and the frequency width of less than-10 dB reaches 2.11GHz throughout the entire test frequency band, and no distortion occurs throughout the entire test frequency range.
According to the method for measuring the high-temperature electromagnetic parameters of the powdery wave-absorbing material, disclosed by the embodiment of the invention, the high-temperature-resistant wave-transmitting material and the adhesive are sequentially and uniformly mixed with the powdery wave-absorbing material and then are subjected to compression molding and high-temperature sintering to prepare the block-shaped sample, so that the powdery wave-absorbing material and the high-temperature-resistant wave-transmitting material are tightly combined, the mechanical strength of the block-shaped sample can be enhanced, the integral wave-absorbing performance of the block-shaped sample is kept, the prepared block-shaped sample has good high-temperature stability, abnormal measurement results caused by severe deformation in the high-temperature test process of a waveguide method can be avoided, and the accuracy of the high-temperature test of the waveguide method can be ensured. The method for measuring the high-temperature electromagnetic parameters of the powdery wave-absorbing material disclosed by the embodiment of the invention is simple to operate, and the prepared block sample has good high-temperature stability and high measurement result accuracy.
The technical details disclosed in the technical scheme and the embodiment of the invention are only illustrative of the inventive concept of the invention and are not limiting to the technical scheme of the invention, and all conventional changes, substitutions or combinations of the technical details disclosed in the embodiment of the invention have the same inventive concept as the invention and are within the scope of the claims of the invention.
Claims (10)
1. The method for measuring the high-temperature electromagnetic parameters of the powdery wave-absorbing material is characterized by comprising the following steps of:
s1, preparing a powdery wave-absorbing material into a block sample; the method specifically comprises the following steps:
Uniformly mixing and grinding the powdery wave-absorbing material and the high-temperature-resistant wave-transparent material according to a set filler ratio to obtain mixed powder;
dripping a preset amount of binder into the mixed powder, and stirring to obtain a mud-like mixed sample;
Filling the mud-like mixed sample into a mould for compression molding to obtain a blocky sample precursor;
Naturally drying and solidifying the precursor of the block sample, and then sintering at high temperature under inert atmosphere for further solidification to obtain a block sample;
s2, measuring the block sample by adopting a waveguide method to obtain the high-temperature electromagnetic parameters of the powdery wave-absorbing material.
2. The method for measuring the high-temperature electromagnetic parameters of the powdery wave-absorbing material according to claim 1, wherein the purity of the high-temperature-resistant wave-transmitting material is more than or equal to 99 percent, and the granularity is less than or equal to 10 mu m.
3. The method for measuring high-temperature electromagnetic parameters of a powdery wave-absorbing material according to claim 1, wherein the high-temperature-resistant wave-transmitting material is a ceramic wave-transmitting material, an organic resin wave-transmitting material or a phosphate-based wave-transmitting material.
4. The method for measuring high-temperature electromagnetic parameters of a powdery wave-absorbing material according to claim 3, wherein the ceramic wave-transparent material is BN, siBNO, siO 2、Si3N4 or Sino.
5. The method for measuring high-temperature electromagnetic parameters of a powdery wave-absorbing material according to claim 3, wherein the organic resin wave-transmitting material is tripropylester isocyanate, epoxy resin, polytetrafluoroethylene, phenolic resin, cyanate resin or polyether ether ketone.
6. The method for measuring high-temperature electromagnetic parameters of a powdery wave-absorbing material according to claim 3, wherein the phosphate-based wave-transmitting material is chromium phosphate, aluminum phosphate or chromium aluminum phosphate.
7. The method for measuring high-temperature electromagnetic parameters of a powdery wave-absorbing material according to claim 1, wherein the adhesive is an inorganic silicon-based adhesive, an epoxy resin-based adhesive, a polyimide-based adhesive or a pressure-sensitive adhesive.
8. The method for measuring the high-temperature electromagnetic parameters of the powdery wave-absorbing material according to claim 1, wherein the pressure of the pressing forming of the mud-like mixed sample is 120-530 kPa.
9. The method for measuring the high-temperature electromagnetic parameters of the powdery wave-absorbing material according to claim 1, wherein the high-temperature sintering temperature of the massive sample precursor is 300-1000 ℃, the time is 0-10 h, and the heating rate is 1-20 ℃/min.
10. The method for measuring the high-temperature electromagnetic parameters of the powdery wave-absorbing material according to claim 1, wherein the inert atmosphere is argon or nitrogen, and the flow rate of the inert atmosphere is 30-70 ml/min.
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