CN101985551A - Foam glass-based composite radar absorbing material and preparation method thereof - Google Patents
Foam glass-based composite radar absorbing material and preparation method thereof Download PDFInfo
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- CN101985551A CN101985551A CN2010102598191A CN201010259819A CN101985551A CN 101985551 A CN101985551 A CN 101985551A CN 2010102598191 A CN2010102598191 A CN 2010102598191A CN 201010259819 A CN201010259819 A CN 201010259819A CN 101985551 A CN101985551 A CN 101985551A
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Abstract
The invention discloses a foam glass-based composite radar absorbing material and a preparation method thereof. The method comprises the following steps of: adding zinc powder and manganese dioxide into borosilicate foam glass, evaporating the zinc powder at high temperature, and reacting the evaporated zinc powder with oxygen so as to generate zinc oxide in the foam glass in situ. In the method, the needed raw materials are readily available, the cost is lower, the operation process is simple, the material is baked by a powder fusion method, the preparation temperature is low, and the formula is high in stability and reliability. The prepared absorbing material has excellent performance of absorbing electromagnetic waves, is applied to radiation-proof buildings, microwave heating, electromagnetic shielding of electronic equipment and the like, and also can be applied in the fields such as ground fortification anti-radar detection and resistance to electromagnetic interference militarily, microwave unreflected chambers and the like to reduce the electromagnetic radiation pollution.
Description
Technical field
The present invention relates to electromagnetic material of a kind of absorption and preparation method thereof, specifically, relate to a kind of composite radar absorbing material based on multicellular glass and preparation method thereof.
Background technology
Nineteen thirty-five is with glass powder and the fusion of whipping agent mixing post-heating by the multicellular glass that France at first develops, and forms through foaming, annealing again.Multicellular glass is the inorganic materials that a kind of inside is contained a lot of connections or sealed small pore, have lightweight, multi-functional, easily mix and characteristics such as modification.Multicellular glass is divided into two kinds of perforate and closed pores according to the form in hole: open cell type multicellular glass has sound absorption, is used to do sound-absorbing material.Obturator-type multicellular glass has heat-blocking action, is used to do lagging material.
Radar absorbing claims radar invisible or camouflage material again, is the material very little to reflection of radar waves.Dual mode is mainly passed through in the absorption of radar wave: the one, and resonance promptly equals four of radar wave wavelength/for the moment, reduce the radar wave reflection by resonance when the thickness of material.The 2nd, mix, in material, add electrical loss or magnetic loss material, utilize electrical loss material conduction current under electromagnetic field effect to be subjected to the restriction of finite conductivity, make the radar wave that enters material convert heat energy to and lose; Perhaps utilize magnetic loss material internal dipole under electromagnetic field, to move to be subjected to limiting the magnetic permeability restriction and make electromagnetic energy convert heat energy to.
The foam type absorbing material is studied on the basis that concentrates on porous plastics, spongy rubber, foamed ceramics aspect stealthy and the shielding, or adds carbon fiber and ferrite is made absorption agent at Resins, epoxy, is made into coating, paster and laminate.A kind of New Type Radar ripple absorbing coating that Europe GAMMA company releases adopts polycrystalline iron fiber to make absorption agent, and is in light weight, and can realize the efficient absorption radar wave in very wide frequency band range.The invisible coating that the U.S. produces and exports at present can reach 12-25db in 2-18GHz range of frequency internal absorption factor.Japan utilizes ferrite class absorbing material to mix as wallcovering with mortar, is used for shielding electromagnetic waves.(application number is 00109462.9 in Chinese invention patent application " foam glass type material obsorbing radar waves ", the applying date is on June 26th, 2000, being March 7 calendar year 2001 in open day) the employing glass cullet are raw material, utilize silicon carbide, graphite, graphitized carbon black, ferritic mixture to mix, produce according to the ordinary student production art.This design only utilizes the loss material that adds to reach wave-absorbing effect, and adopts glass cullet, though save cost, causes the not high difficulty with technology controlling and process of the purity of product easily.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, providing a kind of is the absorbing material of base material recombination loss material with multicellular glass, adopts pure material to be prepared as raw material simultaneously, thereby makes the preparation of material have the high stability and the reliability of prescription.
A kind of composite radar absorbing material based on multicellular glass of the present invention is a base material with multicellular glass, and original position generates zinc oxide on multicellular glass, prepares according to following method steps:
(1) take by weighing multicellular glass raw material, zinc powder and Manganse Dioxide according to following ratio, wherein said multicellular glass raw material is made up of 58-62% silicon-dioxide, 3-6% aluminium sesquioxide, 3-6% potassium hydroxide, 13-16% sodium hydroxide, 14-20% boric acid and 0.5-1.5% graphite according to mass percent; The adding quality of described zinc powder is 5.5-17% of a described multicellular glass raw materials quality; The adding quality of described Manganse Dioxide is 2-6% of zinc powder and a multicellular glass raw material total mass;
(2) multicellular glass raw material, zinc powder and the Manganse Dioxide after will taking by weighing mixes and is levigate, obtains material to be burnt;
(3) will wait to burn material burns till according to following technology, promptly obtain composite radar absorbing material: be warming up to 380-450 ℃ and be incubated 20-40 minutes earlier based on multicellular glass, be warming up to 700-800 ℃ and be incubated 20-40 minutes then, be cooled to 600-650 ℃ and annealed 20-40 minutes again, naturally cool to room temperature at last.
The multicellular glass raw material of described step (1) is made up of 58-60% silicon-dioxide, 4-6% aluminium sesquioxide, 3-6% potassium hydroxide, 14-16% sodium hydroxide, 16-20% boric acid and 1-1.5% graphite according to mass percent.
The adding quality of the zinc powder of described step (1) is 8-17% of a described multicellular glass raw materials quality.
The adding quality of the Manganse Dioxide of described step (1) is 4-6% of zinc powder and a multicellular glass raw material total mass.
Described step (2) adopts wet-milling or dry grind process that multicellular glass raw material, zinc powder and Manganse Dioxide are mixed and is levigate.
The firing process of described step (3) is for being warming up to 400 ℃ and be incubated 30 minutes earlier, is warming up to 750 ℃ and be incubated 30 minutes then, is cooled to 600 ℃ and annealed 30 minutes again, naturally cools to room temperature at last.
The temperature rise rate that is warming up to 380-450 ℃ in the firing process of described step (3) is 3 ℃/min, and the temperature rise rate that is warming up to 700-800 ℃ is 5 ℃/min, and the cooling rate that is cooled to 600-650 ℃ is 3 ℃/min.
A kind of preparation of the present invention is carried out according to following step based on the method for the composite radar absorbing material of multicellular glass:
(1) take by weighing multicellular glass raw material, zinc powder and Manganse Dioxide according to following ratio, wherein said multicellular glass raw material is made up of 58-62% silicon-dioxide, 3-6% aluminium sesquioxide, 3-6% potassium hydroxide, 13-16% sodium hydroxide, 14-20% boric acid and 0.5-1.5% graphite according to mass percent; The adding quality of described zinc powder is 5.5-17% of a described multicellular glass raw materials quality; The adding quality of described Manganse Dioxide is 2-6% of zinc powder and a multicellular glass raw material total mass;
(2) multicellular glass raw material, zinc powder and the Manganse Dioxide after will taking by weighing mixes and is levigate, obtains material to be burnt;
(3) will wait to burn material burns till according to following technology, promptly obtain composite radar absorbing material: be warming up to 380-450 ℃ and be incubated 20-40 minutes earlier based on multicellular glass, be warming up to 700-800 ℃ and be incubated 20-40 minutes then, be cooled to 600-650 ℃ and annealed 20-40 minutes again, naturally cool to room temperature at last.
The multicellular glass raw material of described step (1) is made up of 58-60% silicon-dioxide, 4-6% aluminium sesquioxide, 3-6% potassium hydroxide, 14-16% sodium hydroxide, 16-20% boric acid and 1-1.5% graphite according to mass percent.
The adding quality of the zinc powder of described step (1) is 8-17% of a described multicellular glass raw materials quality.
The adding quality of the Manganse Dioxide of described step (1) is 4-6% of zinc powder and a multicellular glass raw material total mass.
Described step (2) adopts wet-milling or dry grind process that multicellular glass raw material, zinc powder and Manganse Dioxide are mixed and is levigate.
The firing process of described step (3) is for being warming up to 400 ℃ and be incubated 30 minutes earlier, is warming up to 750 ℃ and be incubated 30 minutes then, is cooled to 600 ℃ and annealed 30 minutes again, naturally cools to room temperature at last.
The temperature rise rate that is warming up to 380-450 ℃ in the sintering process of described step (3) is 3 ℃/min, and the temperature rise rate that is warming up to 700-800 ℃ is 5 ℃/min, and the cooling rate that is cooled to 600-650 ℃ is 3 ℃/min.
Compared with prior art, the Borosilicate Foam Glass that the distinctive feature of technical solution of the present invention is made feedstock production with pure material has the stability and the high reliability of prescription, in Borosilicate Foam Glass, add zinc powder and Manganse Dioxide, generate material zinc oxide with oxygen reaction original position in multicellular glass behind the zinc powder high temperature evaporation with absorption of electromagnetic wave drain performance, and the synthetic of this original position can obtain ZnOw (shown in attached Fig. 1 and 2, in the XRD figure of accompanying drawing 2, measure the diffraction peak height, and the peak height of establishing 43.2 ° is 100%, obtaining at 31.3 ° of corresponding peak heights of zinc oxide is 47.1%), add reactivity and the form of regulation and control generation zinc oxide and the size and the homogeneity of abscess that Manganse Dioxide improves zinc powder and oxygen simultaneously.Method desired raw material of the present invention is easy to get, cost is lower, operating process is simply easy, adopts the powder melts method to fire, and preparation temperature is low, the absorbing material of preparation has the electromagnetic premium properties (as shown in Figure 3) of absorption, be applicable to anti-radiation building, the electromagnetic shielding of microwave heating, electronics etc. can also be applied in the anti-radar detection of military ground fortification and prevent electromagnetic interference, fields such as microwave unreflected chamber reduce electromagenetic wave radiation and pollute.
Description of drawings
Fig. 1 is the electron scanning micrograph of absorbing material of the present invention.
Fig. 2 is the X-ray diffractogram of absorbing material of the present invention.
Fig. 3 is the reflectance test figure as a result of absorbing material of the present invention.
Embodiment
Further specify technical scheme of the present invention below in conjunction with specific embodiment.
The foregoing description adopts preparation method of the present invention to be prepared, and earlier takes by weighing corresponding raw material according to formula rate, mixes then and levigate, obtains material to be burnt.Can adopt dry grind process, also can adopt wet milling process, with water is ball-milling medium wet-milling compound, abundant mixing compound, waiting to burn the material amount of water as every 50g is 40ml, the abrading-ball that uses is the corundum abrading-ball, the add-on of abrading-ball is according to material to be burnt: the mass ratio of abrading-ball is that 1:2 adds, with 600r/min rotating speed ball milling 3h, the slip that obtains during the air blast heat drying, prevent the formation of slip caking in loft drier, should stir frequently, smash compound to pieces, cross 140 mesh sieves at last, get the undersized material that mixes, add jolt ramming in the plumbago crucible to, in order to reduce the oxidation of plumbago crucible, crucible should be placed in the airtight alumina crucible, and then be put into the sintering kiln roasting.
Firing temperature system of the present invention is: earlier be warming up to 380-450 ℃ and be incubated 20-40 minutes from room temperature, so that get rid of the moisture in the multicellular glass; Be warming up to 700-800 ℃ and be incubated 20-40 minutes then, if too high or too low for temperature, can cause abscess excessively to grow up or do not foam; Be cooled to 600-650 ℃ and annealed 20-40 minutes again, naturally cool to room temperature at last, promptly make composite radar absorbing material based on multicellular glass.
Absorbing material to preparation carries out performance test, and before the test, block will be made the standard test specimen that is of a size of 22.74mm * 10.02mm * 2.20mm(± 0.10mm).Test result shows, the minimum reflectance of absorbing material of the present invention is-12dB, maximum reflectivity is-7dB, in full test frequency range (8-13GHz), present-7----12 higher and stable reflection (as shown in Figure 3), be applicable to anti-radiation building, the electromagnetic shielding of microwave heating, electronics etc. can also be applied in the anti-radar detection of military ground fortification and prevent electromagnetic interference, fields such as microwave unreflected chamber reduce electromagenetic wave radiation and pollute.
More than the present invention has been done exemplary description; should be noted that; under the situation that does not break away from core of the present invention, the replacement that is equal to that any simple distortion, modification or other those skilled in the art can not spend creative work all falls into protection scope of the present invention.
Claims (10)
1. the composite radar absorbing material based on multicellular glass is a base material with multicellular glass, it is characterized in that, original position generates zinc oxide on multicellular glass, prepares according to following step:
(1) take by weighing multicellular glass raw material, zinc powder and Manganse Dioxide according to following ratio, wherein said multicellular glass raw material is made up of 58-62% silicon-dioxide, 3-6% aluminium sesquioxide, 3-6% potassium hydroxide, 13-16% sodium hydroxide, 14-20% boric acid and 0.5-1.5% graphite according to mass percent; The adding quality of described zinc powder is 5.5-17% of a described multicellular glass raw materials quality; The adding quality of described Manganse Dioxide is 2-6% of zinc powder and a multicellular glass raw material total mass;
(2) multicellular glass raw material, zinc powder and the Manganse Dioxide after will taking by weighing mixes and is levigate, obtains material to be burnt;
(3) will wait to burn material burns till according to following technology, promptly obtain composite radar absorbing material: be warming up to 380-450 ℃ and be incubated 20-40 minutes earlier based on multicellular glass, be warming up to 700-800 ℃ and be incubated 20-40 minutes then, be cooled to 600-650 ℃ and annealed 20-40 minutes again, naturally cool to room temperature at last.
2. a kind of composite radar absorbing material according to claim 1 based on multicellular glass, it is characterized in that the multicellular glass raw material of described step (1) is made up of 58-60% silicon-dioxide, 4-6% aluminium sesquioxide, 3-6% potassium hydroxide, 14-16% sodium hydroxide, 16-20% boric acid and 1-1.5% graphite according to mass percent; The adding quality of the zinc powder of described step (1) is 8-17% of a described multicellular glass raw materials quality; The adding quality of the Manganse Dioxide of described step (1) is 4-6% of zinc powder and a multicellular glass raw material total mass.
3. a kind of composite radar absorbing material based on multicellular glass according to claim 1 is characterized in that, described step (2) adopts wet-milling or dry grind process that multicellular glass raw material, zinc powder and Manganse Dioxide are mixed and be levigate.
4. a kind of composite radar absorbing material according to claim 1 based on multicellular glass, it is characterized in that, the temperature rise rate that is warming up to 380-450 ℃ in the firing process of described step (3) is 3 ℃/min, the temperature rise rate that is warming up to 700-800 ℃ is 5 ℃/min, and the cooling rate that is cooled to 600-650 ℃ is 3 ℃/min.
5. according to claim 1 or 4 described a kind of composite radar absorbing material based on multicellular glass, it is characterized in that, the firing process of described step (3) is for being warming up to 400 ℃ and be incubated 30 minutes earlier, be warming up to 750 ℃ and be incubated 30 minutes then, be cooled to 600 ℃ and annealed 30 minutes again, naturally cool to room temperature at last.
6. a method for preparing based on the composite radar absorbing material of multicellular glass is characterized in that, carries out according to following step:
(1) take by weighing multicellular glass raw material, zinc powder and Manganse Dioxide according to following ratio, wherein said multicellular glass raw material is made up of 58-62% silicon-dioxide, 3-6% aluminium sesquioxide, 3-6% potassium hydroxide, 13-16% sodium hydroxide, 14-20% boric acid and 0.5-1.5% graphite according to mass percent; The adding quality of described zinc powder is 5.5-17% of a described multicellular glass raw materials quality; The adding quality of described Manganse Dioxide is 2-6% of zinc powder and a multicellular glass raw material total mass;
(2) multicellular glass raw material, zinc powder and the Manganse Dioxide after will taking by weighing mixes and is levigate, obtains material to be burnt;
(3) will wait to burn material burns till according to following technology, promptly obtain composite radar absorbing material: be warming up to 380-450 ℃ and be incubated 20-40 minutes earlier based on multicellular glass, be warming up to 700-800 ℃ and be incubated 20-40 minutes then, be cooled to 600-650 ℃ and annealed 20-40 minutes again, naturally cool to room temperature at last.
7. a kind of preparation according to claim 6 is based on the method for the composite radar absorbing material of multicellular glass, it is characterized in that the multicellular glass raw material of described step (1) is made up of 58-60% silicon-dioxide, 4-6% aluminium sesquioxide, 3-6% potassium hydroxide, 14-16% sodium hydroxide, 16-20% boric acid and 1-1.5% graphite according to mass percent; The adding quality of the zinc powder of described step (1) is 8-17% of a described multicellular glass raw materials quality; The adding quality of the Manganse Dioxide of described step (1) is 4-6% of zinc powder and a multicellular glass raw material total mass.
8. a kind of preparation according to claim 6 is characterized in that based on the method for the composite radar absorbing material of multicellular glass described step (2) adopts wet-milling or dry grind process that multicellular glass raw material, zinc powder and Manganse Dioxide are mixed and be levigate.
9. a kind of preparation according to claim 6 is based on the method for the composite radar absorbing material of multicellular glass, it is characterized in that, the temperature rise rate that is warming up to 380-450 ℃ in the sintering process of described step (3) is 3 ℃/min, the temperature rise rate that is warming up to 700-800 ℃ is 5 ℃/min, and the cooling rate that is cooled to 600-650 ℃ is 3 ℃/min.
10. according to claim 6 or 9 described a kind of methods that prepare based on the composite radar absorbing material of multicellular glass, it is characterized in that, the firing process of described step (3) is for being warming up to 400 ℃ and be incubated 30 minutes earlier, be warming up to 750 ℃ and be incubated 30 minutes then, be cooled to 600 ℃ and annealed 30 minutes again, naturally cool to room temperature at last.
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Cited By (4)
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CN102516934A (en) * | 2011-11-09 | 2012-06-27 | 天津大学 | Foam glass-based microwave absorbing material added with metal powder |
CN103601477A (en) * | 2013-11-19 | 2014-02-26 | 宜宾红星电子有限公司 | Preparation process of absorber with low voltage standing-wave ratio |
CN104445934A (en) * | 2014-11-11 | 2015-03-25 | 中国人民解放军国防科学技术大学 | High-temperature-resistant wedge-shaped microwave absorbing material and preparation method thereof |
CN105502951A (en) * | 2016-01-09 | 2016-04-20 | 北京工业大学 | Porous glass ceramic capable of absorbing electromagnetic waves and preparation method thereof |
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RU2657018C1 (en) * | 2017-07-26 | 2018-06-08 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Томский государственный университет" (ТГУ, НИ ТГУ) | Absorber electromagnetic waves of the gigahertz range |
RU2707656C1 (en) * | 2019-04-17 | 2019-11-28 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Томский политехнический университет" | Composition and method of producing material which absorbs electromagnetic radiation |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102516934A (en) * | 2011-11-09 | 2012-06-27 | 天津大学 | Foam glass-based microwave absorbing material added with metal powder |
CN103601477A (en) * | 2013-11-19 | 2014-02-26 | 宜宾红星电子有限公司 | Preparation process of absorber with low voltage standing-wave ratio |
CN104445934A (en) * | 2014-11-11 | 2015-03-25 | 中国人民解放军国防科学技术大学 | High-temperature-resistant wedge-shaped microwave absorbing material and preparation method thereof |
CN105502951A (en) * | 2016-01-09 | 2016-04-20 | 北京工业大学 | Porous glass ceramic capable of absorbing electromagnetic waves and preparation method thereof |
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