CN103073961A - Multi-element composite microwave absorbent, microwave absorbing coating, microwave absorbing base material and preparation method - Google Patents

Multi-element composite microwave absorbent, microwave absorbing coating, microwave absorbing base material and preparation method Download PDF

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CN103073961A
CN103073961A CN2013100256884A CN201310025688A CN103073961A CN 103073961 A CN103073961 A CN 103073961A CN 2013100256884 A CN2013100256884 A CN 2013100256884A CN 201310025688 A CN201310025688 A CN 201310025688A CN 103073961 A CN103073961 A CN 103073961A
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polynary compound
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CN103073961B (en
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王磊
金宇龙
顾卫军
朱俊阳
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NANJING LUOPU TECHNOLOGY CO., LTD.
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NANJING LUOPU ELECTRONIC ENGINEERING INSTITUTE
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Abstract

The invention relates to a multi-element composite microwave absorbent, a microwave absorbing coating, a microwave absorbing base material and a preparation method. The multi-element composite microwave absorbent is composed of ACET (acetylene black), alpha-SiC and Ni0.7Zn0.3Fe2O4 based on a weight ratio, wherein the microwave absorbing coating is composed of the microwave absorbent, de-ionized water, a PVA (Polyvinyl Alcohol) solution, a wetting agent, a dispersing agent, a de-foaming agent and a water-based leveling agent based on a weight ratio; and the microwave absorbing base material comprises a plurality of pyramidal substrates of which both sides are coated with the microwave absorbing coating. According to the invention, the microwave absorbing base material has excellent reflection loss performance for 118 GHz microwaves, and can be used for manufacturing an anechoic chamber.

Description

Polynary compound be wave absorbing agent, antiradar coatings, wave absorption base material and preparation method
Technical field
The present invention relates to a kind of polynary compound be wave absorbing agent, adopt the antiradar coatings of this wave absorbing agent, scribble the wave absorption base material of this antiradar coatings, and their preparation method.
Background technology
According to the knowledge of the applicant, microwave unreflected chamber refers to adopt absorbing material (being microwave absorbing material) to lay inwall reducing reflection of electromagnetic wave, thereby forms the finite space near " freeboard " clearing of reflection of electromagnetic wave (namely without).Microwave unreflected chamber can be simulated the work such as measurement, debugging and Comprehensive Experiment that " open area test site " carries out radar, wireless and military-civil electronic electric equipment.The performance of microwave unreflected chamber depends primarily on the performance of absorbing material.Absorbing material is that a class can the attenuation by absorption incident electromagnetic wave, and directric relaxation, eddy current and magnetic loss by absorption agent, electromagnetic energy is changed into heat energy and the material that dissipates.Microwave absorbing material has a wide range of applications at dual-use microwave unreflected chamber and antenna measurement field as the gordian technique means of radar invisible, electromagnetic compatibility and shielding.
Wave absorbing agent is the key component that determines absorbing material performance, and wave absorbing agent can be divided into by the difference of mechanism electrical loss type and magnetic loss type.Wherein, the electrical loss type can be subdivided into: (1) conduction loss type, and such as some non-magnetic metal powder, carbon black, carbon fiber and conducting polymer etc., these materials are mainly by resistance consume, the decay electromagnetic energy of microwave; (2) dielectric loss type such as dielectric ceramic etc., mainly relies on electronic polarization, molecular polarization or the interfacial polarization decay electromagnetic wave absorption of medium.Magnetic loss type wave absorbing agent mainly relies on the Polarization Mechanism decay electromagnetic wave absorption energy such as magnetic hysteresis loss, resonance loss and residual loss.
Traditional wave absorbing agent generally has metal powder, steel fiber, acetylene black (to claim again Shawinigan black, be called for short ACET), carbon fiber, Graphite Powder 99, ceramic fiber and ferrite etc., wherein electromagnetic wave absorbing material mainly comprises ferrite, super-fine metal powder, polycrystalline iron fiber.
Find through retrieval, the Chinese invention patent application of application number 00109462.9 publication number CN1286474A discloses a kind of foam glass type material obsorbing radar waves, mix up in multicellular glass inside mineral material is arranged, chemical materials and electromagnetic consumable material, or at its basal surface coating hertzian wave loss material, make it have sorption to radar wave, the absorption of electromagnetic wave material adopt silicon carbide, graphite, conductive carbon black, ferritic mixture or wherein one or more.The Radar Absorbing Property aspect, in the 2-18GHz range of frequency, this material is 8-25db to the reflection loss amount of radar wave.But for microwave unreflected chamber, the absorptive character of this material are still not ideal enough.
Summary of the invention
Technical problem to be solved by this invention is: for the problem of prior art existence, provide a kind of polynary compound be wave absorbing agent, the antiradar coatings that adopts this wave absorbing agent and the wave absorption base material that scribbles this antiradar coatings, this wave absorption base material has good absorbing property, can be used for making microwave unreflected chamber; The preparation method of above-mentioned wave absorbing agent, antiradar coatings and wave absorption base material also is provided in addition.
Technical conceive of the present invention is as follows: the present patent application people finds in practical studies, ACET(acetylene black) drain performance good, take ACET as main absorption agent, being aided with α-SiC(crystalline structure is six sides or rhombohedral silicon carbide again), Ni 0.7Zn 0.3Fe 2O 4(ferrite) regulates relative permittivity ε and relative magnetic permeability μ, improve wave absorbing agent layer itself to electromagnetic drain performance and with the impedance matching performance of freeboard, thereby realize good absorbing property.
The technical scheme that the present invention solves its technical problem is as follows:
A kind of polynary compound be wave absorbing agent, it is characterized in that, formed by weight by following component:
Figure BDA00002768317600021
Wherein, 0.2≤x＜1.
Preferably, described ACET is cell-grade acetylene black; The granularity of described α-SiC is 1000 orders.
A kind of polynary compound be antiradar coatings, it is characterized in that, formed by weight by following component:
Figure BDA00002768317600031
Wherein, 0.2≤x＜1.
Preferably, the mass concentration of described PVA solution is 4-20%; Described wetting agent is PE100 or BYK-ATU; Described dispersion agent is Tech-5630 or SN5040; Described defoamer is non-silicon defoaming agent Tech-423 or 5060; Described water-based flow agent is Tech-160 or SS-5410.
A kind of polynary compound be wave absorption base material, it is characterized in that, comprise some wedges towards the pyramid substrate of the same side, described substrate is made by fire retardant material, described substrate two sides evenly are coated with aforementioned antiradar coatings.
Preferably, described substrate is positive rectangular pyramid shape; Described fire retardant material is fire retardant nonwoven fabric.
A kind of polynary compound be the wave absorbing agent preparation method, it is characterized in that, may further comprise the steps:
The first step, with raw material ZnO, NiO, Fe 3O 4After adding deionized water, ball milling, drying, grind to get the mixing powder; Described raw material ZnO, NiO, Fe 3O 4Mol ratio be 2.1:0.9:2;
Second step, the first step is obtained powder after pre-burning, ball milling, drying, grind to get Ni 0.7Zn 0.3Fe 2O 4Powder;
The 3rd step, ACET, α-SiC and second step that drying is crossed obtain Ni 0.7Zn 0.3Fe 2O 4Powder is pressed following weight ratio mixing,
Figure BDA00002768317600041
0.2≤x＜1 namely gets wave absorbing agent.
Preferably, in the first step, the second step, rotational speed of ball-mill is at least 200 rev/mins, and Ball-milling Time is at least 24 hours; In the second step, calcined temperature is at least 1200 ℃, and the pre-burning time is at least 3 hours.
Preferably, in the first step, described raw material ZnO, NiO, Fe 3O 4Purity be respectively more than 99%; In the 3rd step, described ACET is cell-grade acetylene black; The granularity of described α-SiC is 1000 orders.
A kind of polynary compound be the antiradar coatings preparation method, it is characterized in that, may further comprise the steps:
The first step, adopt aforementioned polynary compound be the wave absorbing agent preparation method, make wave absorbing agent;
Second step, in wave absorbing agent, add deionized water, PVA solution, wetting agent, dispersion agent, defoamer, water-based flow agent by following weight ratio,
Figure BDA00002768317600042
0.2≤x＜1；
Namely get antiradar coatings behind the 3rd step, the ball milling.
Preferably, in the second step, the mass concentration of described PVA solution is 4-20%; Described wetting agent is PE100 or BYK-ATU; Described dispersion agent is Tech-5630 or SN5040; Described defoamer is non-silicon defoaming agent Tech-423 or 5060; Described water-based flow agent is Tech-160 or SS-5410.
Preferably, in the 3rd step, rotational speed of ball-mill is at least 200 rev/mins, and Ball-milling Time is at least 2 hours.
A kind of polynary compound be the wave absorption base material preparation method, it is characterized in that, may further comprise the steps:
The first step, adopt aforementioned polynary compound be the antiradar coatings preparation method, make antiradar coatings;
Second step, described antiradar coatings evenly is coated in the two sides of some substrates, described substrate is made by fire retardant material;
The 3rd step, with each substrate cut out, fold, gluing, make substrate be pyramid; Each substrate bottom is mutually bonding, obtain each substrate wedge towards the wave absorption base material of the same side.
Preferably, in the second step, described fire retardant material is fire retardant nonwoven fabric; In the 3rd step, described substrate is positive rectangular pyramid shape.
Compared with prior art, beneficial effect of the present invention is as follows:
(1) wave absorbing agent of the present invention is take ACET(acetylene black) be main absorption agent, being aided with α-SiC(crystalline structure is six sides or rhombohedral silicon carbide again), Ni 0.7Zn 0.3Fe 2O 4(ferrite) regulates relative permittivity ε and relative magnetic permeability μ, reduced specific conductivity, can improve wave absorbing agent layer itself to electromagnetic drain performance on the one hand, make on the other hand the impedance mismatching of wave absorbing agent layer and freeboard reduce (namely improving impedance matching performance), thereby reduce hertzian wave at the interface reflection, make most of electromagnetic wave energy can enter the wave absorbing agent coating inner and be dissipated, and then realize good absorbing property.
(2) wave absorption base material resistivity of the present invention reduces with the increase of x, and ρ is changed to 120 Ω cm from 12500 Ω cm, can be used as the rapid detection index.
(3) wave absorption base material of the present invention has good reflection loss performance to the 1-18GHz microwave, and performance is best when x=0.5.
(4) preparation method of the present invention only needs conventional equipment, utilizes cheap raw material can make wave absorbing agent, antiradar coatings, wave absorption base material by easy steps, is suitable for commercial scale production.
Description of drawings
Fig. 1 is the schematic diagram of the embodiment of the invention 1 single substrate.
Fig. 2 is the schematic diagram that the some substrates of Fig. 1 embodiment are bonded together.
Fig. 3 is the change in resistance figure of the embodiment of the invention 2.
Fig. 4 is the reflection loss results of property schematic diagram of 3 couples of 1GHz of the embodiment of the invention, 15GHz microwave.
Fig. 5 is that Fig. 4 embodiment is to the reflection loss results of property schematic diagram of 1-18GHz microwave.
Embodiment
With reference to the accompanying drawings and in conjunction with the embodiments the present invention is described in further detail.But the invention is not restricted to given example.
Embodiment 1 preparation polynary compound be wave absorbing agent, antiradar coatings, wave absorption base material
One, the preparation polynary compound be wave absorbing agent
The first step, with raw material ZnO, NiO, Fe 3O 4After adding deionized water, ball milling, drying, grind to get the mixing powder; Raw material ZnO, NiO, Fe 3O 4Mol ratio be 2.1:0.9:2;
Wherein, raw material ZnO, NiO, Fe 3O 4Purity be respectively more than 99%; Rotational speed of ball-mill is at least 200 rev/mins, and Ball-milling Time is at least 24 hours;
Second step, the first step is obtained powder after pre-burning, ball milling, drying, grind to get Ni 0.7Zn 0.3Fe 2O 4Powder;
Wherein, calcined temperature is at least 1200 ℃, and the pre-burning time is at least 3 hours; Rotational speed of ball-mill is at least 200 rev/mins, and Ball-milling Time is at least 24 hours;
The 3rd step, ACET, α-SiC and second step that drying is crossed obtain Ni 0.7Zn 0.3Fe 2O 4Powder is pressed following weight ratio mixing,
Figure BDA00002768317600061
0.2≤x＜1 namely gets wave absorbing agent;
Wherein, ACET is cell-grade acetylene black; The granularity of α-SiC is 1000 orders.
Two, the preparation polynary compound be antiradar coatings
The first step, adopt aforementioned polynary compound be the wave absorbing agent preparation method, make wave absorbing agent;
Second step, in wave absorbing agent, add deionized water, PVA solution, wetting agent, dispersion agent, defoamer, water-based flow agent by following weight ratio,
Figure BDA00002768317600071
0.2≤x＜1；
Wherein, the mass concentration of described PVA solution is 4-20%(preferred 5%); Described wetting agent is PE100 or BYK-ATU; Described dispersion agent is that Tech-5630 or SN5040(main component are sodium polyacrylate); Described defoamer is that non-silicon defoaming agent Tech-423 or 5060(main component are mineral oil and polyether ester); Described water-based flow agent is that Tech-160 or SS-5410(main component are silicone-polyether copolymer).
The manufacturer of wetting agent PE100 such as Shanghai red brightness chemical industry company limited; The manufacturer of wetting agent BYK-ATU, dispersion agent Tech-5630, non-silicon defoaming agent Tech-423, water-based flow agent Tech-160 such as Shanghai Tag Polymer Sciences Ltd.; The manufacturer of dispersion agent SN5040 such as Nippon Nopco Assistant Co., Ltd.; The magnificent chemical industry of the manufacturer of defoamer 5060 such as the Dongguan City rising sun hundred million company limited; The three liters of trade Co., Ltds in the manufacturer of water-based flow agent SS-5410 such as Shunde District, Foshan City.
Namely get antiradar coatings behind the 3rd step, the ball milling; Rotational speed of ball-mill is at least 200 rev/mins, and Ball-milling Time is at least 2 hours.
Three, the preparation polynary compound be wave absorption base material
The first step, adopt aforementioned polynary compound be the antiradar coatings preparation method, make antiradar coatings;
Second step, in the two sides of some substrates, described substrate is made by fire retardant material described antiradar coatings evenly to be applied (preferably with hairbrush brush); Described fire retardant material is fire retardant nonwoven fabric (namely passing through the non-woven fabrics of fire-retardant finish);
The 3rd step, with each substrate cut out, fold, gluing, make substrate be pyramid (preferably being positive rectangular pyramid shape), as shown in Figure 1; As shown in Figure 2, each substrate bottom is mutually bonding, obtain each substrate wedge towards the wave absorption base material of the same side.
Embodiment 2 wave absorption base material resistivity detect
Press embodiment 1 method, in x value 0.2,0.3,0.4,0.5,0.6,0.7,0.8,0.9 and make wave absorption base material during ultimate value 1.0, detect its resistivity, the result as shown in Figure 3, as seen with the increase of x value, wave absorption base material resistivity constantly reduces.
Because resistivity can characterize the basic electrical parameter that makes product, so when actual production, can judge fast whether the fundamental property of product meets the requirements by check resistivity.
Embodiment 3 wave absorption base material reflection loss Performance Detection
Press embodiment 1 method, in x value 0.2,0.3,0.4,0.5,0.6,0.7,0.8,0.9 and make wave absorption base material during ultimate value 1.0, detect it to the reflection loss performance of 1-18GHz microwave, main result has:
1. to the reflection loss performance of 1GHz, 3GHz, 6GHz, 10GHz, 15GHz, 18GHz microwave:
? 1GHz 3GHz 6GHz 10GHz 15GHz 18GHz
x=0.2 -33dB -42dB -51dB -50dB -37dB -28dB
x=0.3 -33dB -43dB -53dB -52dB -44dB -40dB
x=0.4 -35dB -47dB -60dB -62dB -55dB -55dB
x=0.5 -44dB -58dB -63dB -67dB -60dB -60dB
x=0.6 -36dB -45dB -61dB -65dB -58dB -57dB
x=0.7 -35dB -45dB -58dB -60dB -54dB -50dB
x=0.8 -36dB -47dB -58dB -57dB -50dB -45dB
x=0.9 -32dB -45dB -54dB -56dB -45dB -38dB
X is ultimate value 1.0 -30dB -42dB -51dB -50dB -35dB -31dB
2.x=0.2,0.3,0.4,0.5,0.6,0.7,0.8,0.9 and during ultimate value 1.0, to the reflection loss results of property of 1GHz, 15GHz microwave as shown in Figure 4.By this result as can be known, when x=0.5, wave absorption base material has best absorbing property: the reflection loss to the 1GHz microwave can reach-44dB, can reach-60dB the reflection loss of 15GHz microwave.
3.x=0.2,0.4,0.5,0.6 and during ultimate value 1.0, to the reflection loss results of property of 1-18GHz microwave as shown in Figure 5.By this result as can be known, no matter what value x gets, and the reflection loss performance of wave absorption base material has to a certain degree decline at L-band (1-2GHz) and Ku wave band (12.5-18GHz); When x=0.5, it is best that the reflection loss performance of wave absorption base material reaches, and especially the performance at L-band and Ku wave band has obvious lifting.
The safety test of embodiment 4 wave absorption base materials
As shown in the table, embodiment 1 makes wave absorption base material and has passed through every safety test project, shows that its safety performance can not descend because adopting wave absorbing agent of the present invention or antiradar coatings.
Figure BDA00002768317600091
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of requirement of the present invention.

Claims (10)

  1. One kind polynary compound be wave absorbing agent, it is characterized in that, formed by weight by following component:
    Figure FDA00002768317500011
    Wherein, 0.2≤x＜1.
  2. One kind polynary compound be antiradar coatings, it is characterized in that, formed by weight by following component:
    Wherein, 0.2≤x＜1.
  3. According to claim 2 described polynary compound be antiradar coatings, it is characterized in that, the mass concentration of described PVA solution is 4-20%; Described wetting agent is PE100 or BYK-ATU; Described dispersion agent is Tech-5630 or SN5040; Described defoamer is non-silicon defoaming agent Tech-423 or 5060; Described water-based flow agent is Tech-160 or SS-5410.
  4. One kind polynary compound be wave absorption base material, it is characterized in that, comprise some wedges towards the pyramid substrate of the same side, described substrate is made by fire retardant material, described substrate two sides evenly be coated with claim 2 described polynary compound be antiradar coatings.
  5. One kind polynary compound be the wave absorbing agent preparation method, it is characterized in that, may further comprise the steps:
    The first step, with raw material ZnO, NiO, Fe 3O 4After adding deionized water, ball milling, drying, grind to get the mixing powder; Described raw material ZnO, NiO, Fe 3O 4Mol ratio be 2.1:0.9:2;
    Second step, the first step is obtained powder after pre-burning, ball milling, drying, grind to get Ni 0.7Zn 0.3Fe 2O 4Powder;
    The 3rd step, ACET, α-SiC and second step that drying is crossed obtain Ni 0.7Zn 0.3Fe 2O 4Powder is pressed following weight ratio mixing,
    Figure FDA00002768317500021
    0.2≤x＜1 namely gets wave absorbing agent.
  6. According to claim 5 polynary compound be the wave absorbing agent preparation method, it is characterized in that, in the first step, the second step, rotational speed of ball-mill is at least 200 rev/mins, Ball-milling Time is at least 24 hours; In the second step, calcined temperature is at least 1200 ℃, and the pre-burning time is at least 3 hours; In the first step, described raw material ZnO, NiO, Fe 3O 4Purity be respectively more than 99%; In the 3rd step, described ACET is cell-grade acetylene black; The granularity of described α-SiC is 1000 orders.
  7. One kind polynary compound be the antiradar coatings preparation method, it is characterized in that, may further comprise the steps:
    The first step, adopt claim 5 described polynary compound be the wave absorbing agent preparation method, make wave absorbing agent;
    Second step, in wave absorbing agent, add deionized water, PVA solution, wetting agent, dispersion agent, defoamer, water-based flow agent by following weight ratio,
    Figure FDA00002768317500031
    0.2≤x＜1；
    Namely get antiradar coatings behind the 3rd step, the ball milling.
  8. According to claim 7 polynary compound be the antiradar coatings preparation method, it is characterized in that, in the second step, the mass concentration of described PVA solution is 4-20%; Described wetting agent is PE100 or BYK-ATU; Described dispersion agent is Tech-5630 or SN5040; Described defoamer is non-silicon defoaming agent Tech-423 or 5060; Described water-based flow agent is Tech-160 or SS-5410; In the 3rd step, rotational speed of ball-mill is at least 200 rev/mins, and Ball-milling Time is at least 2 hours.
  9. One kind polynary compound be the wave absorption base material preparation method, it is characterized in that, may further comprise the steps:
    The first step, adopt claim 7 described polynary compound be the antiradar coatings preparation method, make antiradar coatings;
    Second step, described antiradar coatings evenly is coated in the two sides of some substrates, described substrate is made by fire retardant material;
    The 3rd step, with each substrate cut out, fold, gluing, make substrate be pyramid; Each substrate bottom is mutually bonding, obtain each substrate wedge towards the wave absorption base material of the same side.
  10. According to claim 9 polynary compound be the wave absorption base material preparation method, it is characterized in that, in the second step, described fire retardant material is fire retardant nonwoven fabric; In the 3rd step, described substrate is positive rectangular pyramid shape.
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CN103289641A (en) * 2013-06-08 2013-09-11 南京洛普电子工程研究所 Multi-layer polyurethane flexible foam composite wave-absorbing material and preparation method thereof
CN104130458A (en) * 2014-07-24 2014-11-05 中国热带农业科学院农产品加工研究所 Absorbing material and preparation method
CN105714553A (en) * 2015-09-18 2016-06-29 安徽义林塑业有限公司 Preparation method of wave-absorbing non-woven fabrics
CN108795168A (en) * 2018-07-17 2018-11-13 合肥雅克丽新型建材有限公司 A kind of radiation protection inner wall decorative coating of high stability
CN111270529A (en) * 2018-12-05 2020-06-12 洛阳尖端技术研究院 Light high-elasticity wave-absorbing material and preparation method thereof
CN111876046A (en) * 2019-12-12 2020-11-03 温州市鹿城印染厂 Visible light-near infrared-thermal infrared-millimeter wave-centimeter wave multi-spectrum stealth integrated composite coating

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CN103289641A (en) * 2013-06-08 2013-09-11 南京洛普电子工程研究所 Multi-layer polyurethane flexible foam composite wave-absorbing material and preparation method thereof
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CN108795168A (en) * 2018-07-17 2018-11-13 合肥雅克丽新型建材有限公司 A kind of radiation protection inner wall decorative coating of high stability
CN111270529A (en) * 2018-12-05 2020-06-12 洛阳尖端技术研究院 Light high-elasticity wave-absorbing material and preparation method thereof
CN111876046A (en) * 2019-12-12 2020-11-03 温州市鹿城印染厂 Visible light-near infrared-thermal infrared-millimeter wave-centimeter wave multi-spectrum stealth integrated composite coating

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