CN102493204B - Preparation method of hanging wave absorbing composite material - Google Patents
Preparation method of hanging wave absorbing composite material Download PDFInfo
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- CN102493204B CN102493204B CN201110402503.8A CN201110402503A CN102493204B CN 102493204 B CN102493204 B CN 102493204B CN 201110402503 A CN201110402503 A CN 201110402503A CN 102493204 B CN102493204 B CN 102493204B
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Abstract
The invention discloses a preparation method of a hanging wave absorbing composite material for improving absorbing property, which relates to the preparation method of the wave absorbing composite material, and aims to solve the technical problems that the existing wave absorbing fabric which is produced from wave absorbing fibers has a complicated production technology, is higher in cost and has bad wave absorbing performance of the wave absorbing fabric which utilizes electromagnetic power to fill textile gaps. The method comprises the steps that: a wave absorbing body and a liquid organic polymer are mixed to obtain a sizing agent, the surface modification fabric is soaked in the sizing agent to be spread with the sizing agent, after frictioning, rolling or extruding operation, the hanging wave absorbing composite material can be obtained after solidifying and drying. The lowest reflectivity of the hanging wave absorbing composite material is in a range of -10 dB to -80dB, the absorbing bandwidth which is less than -10dB is in a range of 1-10GH, and the preparation technology is simple. The material can be used for military aircrafts, ships, missiles and other hiding military fields.
Description
Technical field
The present invention relates to the preparation method of Wave suction composite material.
Background technology
In modern war, the technical development of radar absorbing is to improve one of key technology of stealth technology.The principle of work and power of absorbing material is the electromagnetic energy of incident to be changed into heat energy loss fall, thereby avoids electromagnetic reflection.If realize, this electromagnetic high efficiency is absorbed and must meet two conditions: first electromagnetic wave can enter into absorbing material inside and can strong reflection not occur at incidence surface; Next electromagnetic wave that enters into material internal is changed into heat energy expeditiously.Common wave-absorbing and camouflage material is for to be dispersed in wave-absorber in resin, and brushing, at aircraft surface, realizes electromagnetic absorption.Compare with being coated with brush wave-absorbing and camouflage material, inhale ripple fabric and have easy to usely, can be used repeatedly and the feature such as excellent performance.Existing suction ripple fabric has two kinds: the one, by the fiber process with suction wave energy, become textiles, as metal fibre, carbon fiber and metallized fibre etc.The material of the method manufacture has good absorbing property, but complicated process of preparation, and cost is higher.The 2nd, on fabric, apply the functional material with absorbing property.With the space with the electromagnetic powder filling fabric of inhaling wave energy, form the suction ripple fabric with certain bearing capacity.But in current research, because used filler is dusty raw materials, this powder is filled in the space of fabric, and is isolated by textile fabric between powder, does not constitute continuous electromagnetic powder passage, is difficult to obtain good absorbing property.
Due to, " absorbing property of non-woven fabrics fabric figure layer ", Zhu Liqun etc., " aeronautical material journal ", in the 28th disclosed document of the 4th phase of volume, disclosed employing wave absorbing agent is " carbonyl iron dust and acetylene carbon black ";
" carbon fiber/carbonyl iron dust meets figure layer wave-absorbing effect and Analysis on Mechanism ", Meng Hui etc., " material protection ", on January 15th, 2006 disclosed document, disclosed employing wave absorbing agent is " with the carbon fiber after nickel plating and carbonyl iron dust ";
" progress of carbon nano-tube magnetic nanometer particle complex technique ", Su Xiuzhi etc., " material Leader ", the 23rd the 4th phase of volume, on November 15th, 2009 disclosed document, disclosed employing wave absorbing agent is " in CNT, filling magnetic metal particle ";
There is following problem in above-mentioned disclosed wave absorbing agent: the wave absorbing agent of employing is CNT, poor to electromagnetic absorption and dissipative effect, poor with the suction ripple fabric absorbing property in electromagnetic powder filling fabric space; In preparation, in absorbing material, need catalyst, complex process, cost are high.
Summary of the invention
The present invention will solve that the existing suction ripple preparation process of textile prepared with wave-absorption fibre is complicated and cost is higher, the poor technical problem of suction ripple fabric absorbing property in use electromagnetic powder filling fabric space, and a kind of preparation method who improves the put on a suit of armour formula Wave suction composite material of absorbing property is provided.
A kind of preparation method who puts on a suit of armour formula Wave suction composite material of the present invention carries out according to the following steps:
One, wave-absorber and liquid organic polymer are mixed, then add the curing agent of organic polymer, then mix, obtain having the slurry of mobility; Wave-absorber in step 1 is hollow carbon fiber and ferritic mixture, or the mixture of hollow carbon fiber and metallic magnetic powder, or the mixture of hollow carbon fiber and carbon-based powder;
Two, textiles is immersed after surface modification in slurry prepared by step 1 and flood 0.5h～5h, obtain hanging textiles; Wherein textiles has 10 μ m～1mm holes;
Three, hanging textile surface step 3 being obtained after frictioning, roll extrusion or extrusion operation, dry, obtain putting on a suit of armour formula Wave suction composite material.
The present invention first mainly soaks the surface modification of textiles by bases (NaOH etc.), remove surperficial greasy dirt, the surface of alligatoring textiles, the good combination of assurance textiles and wave absorbing agent.Then use the further textiless that soak such as surface modifier (stearic acid, butyl titanate and Span80 etc.), change the polarity of textile surface, realize good combination with inhaling ripple substrate macromolecule material, thereby realize effective dispersion of wave-absorber.
Utilize liquid organic polymer matrix and wave-absorbing powder, first mix, then add the curing agent of matrix material to be mixed into slurry, by putting into slurry as the textiles of carrier, flood again, finally by frictioning, roll extrusion or extruding, on the one hand slurry is clamp-oned to fibre bundle inside, another side is removed unnecessary slurry, then drying reacts matrix material and its curing agent, and wave-absorbing powder and textiles are combined with each other, and obtains putting on a suit of armour formula Wave suction composite material; By method of the present invention, after liquid organic polymer solidifies, for having elasticity and good flexible material, and wave-absorbing powder can be punished cloth with the fold of textile surface uniformly in the aperture of hollow carbon fiber.This distribution mode can make composite magnetic powder in compound with fabric, still keeps continuous passage, realizes good absorbing property.The formula Wave suction composite material performance of putting on a suit of armour of the present invention is as follows: a, wave-absorber are dispersed in wave transparent matrix; B, prepared microstructure of composite even structure; The minimum reflectivity (dB) of c, Wave suction composite material is at-10～-80dB, and the absorption frequency range of be less than-10dB is at 1-10GH.Preparation technology of the present invention is simple simultaneously.
Put on a suit of armour formula Wave suction composite material prepared by the present invention can carry out cutting by the profile of aircraft, makes, and the invisible clothes that can be used as aircraft is reused.For military fields such as military spacecraft, naval vessel, guided missiles.
The specific embodiment
The specific embodiment one: a kind of preparation method who puts on a suit of armour formula Wave suction composite material of present embodiment carries out according to the following steps:
One, wave-absorber and liquid organic polymer are mixed, then add the curing agent of organic polymer, then mix, obtain having the slurry of mobility; Wave-absorber in step 1 is hollow carbon fiber and ferritic mixture, or the mixture of hollow carbon fiber and metallic magnetic powder, or the mixture of hollow carbon fiber and carbon-based powder;
Two, textiles is immersed after surface modification in slurry prepared by step 1 and flood 0.5h～5h, obtain hanging textiles; Wherein textiles has 10 μ m～1mm holes;
Three, hanging textile surface step 3 being obtained after frictioning, roll extrusion or extrusion operation, dry, obtain putting on a suit of armour formula Wave suction composite material.
The liquid organic polymer of step 1 in present embodiment, after adding curing agent to solidify, at room temperature has pliability and elasticity.
The method of present embodiment, wave-absorbing powder can be punished cloth with the fold of textile surface uniformly in the aperture of hollow carbon fiber.This distribution mode can make composite magnetic powder in compound with fabric, still keeps continuous passage, realizes good absorbing property.The formula Wave suction composite material performance of putting on a suit of armour of the present invention is as follows: a, wave-absorber are dispersed in wave transparent matrix; B, prepared microstructure of composite even structure; The minimum reflectivity (dB) of c, Wave suction composite material is at-10～-80dB, and the absorption frequency range of be less than-10dB is at 1-10GH.The preparation technology of present embodiment is simple simultaneously.
The specific embodiment two: present embodiment is different from the specific embodiment one is that organic polymer in step 1 is liquid rubber, liquid-state silicon gel or liquid polyurethane.Other is identical with the specific embodiment one.
In present embodiment, liquid rubber, liquid-state silicon gel or liquid polyurethane are the liquid with mobility, are commercially available prod.
The specific embodiment three: present embodiment is different from the specific embodiment one or two is that in hollow carbon fiber in step 1 and ferritic mixture, hollow carbon fiber and ferritic mass ratio are 1:1～10.Other is identical with the specific embodiment one or two.
The specific embodiment four: present embodiment is different from the specific embodiment one or two is that in the mixture of hollow carbon fiber in step 1 and metallic magnetic powder, the mass ratio of hollow carbon fiber and metallic magnetic powder is 1:1～10.Other is identical with the specific embodiment one or two.
The specific embodiment five: what present embodiment was different from the specific embodiment one or two is in step 1; In step 1, in the mixture of hollow carbon fiber and carbon-based powder, the mass ratio of hollow carbon fiber and carbon-based powder is 1:1～10.Other is identical with the specific embodiment one or two.
The specific embodiment six: present embodiment is different from one of specific embodiment one to five is that textiles in step 2 is linen, cotton or chemical fiber cloth etc.Other is identical with one of specific embodiment one to five.
The specific embodiment seven: present embodiment is different from one of specific embodiment one to six is that textile surface modification method in step 2 is: first textiles is immersed in to aqueous slkali 0.5h～10h, and then be immersed in surface modification agent solution and soak 0.5h～10h, complete the surface modification of textiles.Other is identical with one of specific embodiment one to six.
The specific embodiment eight: present embodiment is different from the specific embodiment seven is that alkali in the textile surface modification method in step 2 refers to NaOH, potassium hydroxide or ammoniacal liquor etc.Other is identical with one of specific embodiment seven.
The specific embodiment nine: present embodiment is different from the specific embodiment eight is that surface modifier in the textile surface modification method in step 2 refers to stearic acid, butyl titanate or Span80 etc.Other is identical with one of specific embodiment eight.
The specific embodiment ten: what present embodiment was different from one of specific embodiment one to nine is that in step 1, wave-absorber is 0.5～20:100 with the mass ratio with flexible organic polymer.Other is identical with one of specific embodiment one to nine.
The specific embodiment 11: present embodiment is different from one of specific embodiment one to ten is the hollow carbon fiber described in step 1 by the patent No.: described in ZL201010152182.6 prepared by method, concrete preparation method carries out according to the following steps: one, carbon source material is put into graphite crucible, and graphite crucible is placed in to atmosphere sintering furnace, then by atmosphere sintering stove evacuation, make pressure in stove reach 0.1Pa～1Pa; Two, in atmosphere sintering furnace, be filled with high pure nitrogen or argon gas, make gas pressure intensity in atmosphere sintering furnace reach 0.2MPa～2.5MPa; Three, be incubated 1h～4h after making temperature in atmosphere sintering furnace rise to 900 ℃～1500 ℃ with the speed of 5 ℃/min～30 ℃/min, then, with stove cool to room temperature, obtain hollow carbon fiber; Wherein the carbon source described in step 1 is urea or is the mixture of polyvinyl alcohol and urea, wherein polyvinyl alcohol: the mass ratio of urea is 1:50～100; In step 2, the purity of high pure nitrogen is >=99.999%(quality); The purity of argon gas is >=99.999%(quality).Other is identical with the specific embodiment one.
The hollow carbon fiber of preparing in present embodiment is that caliber is 0.2 μ m～1 μ m, and length reaches the hollow carbon fiber of Centimeter Level.
Following verification experimental verification beneficial effect of the present invention for the present invention:
Test one: a kind of preparation method who puts on a suit of armour formula Wave suction composite material of this test carries out according to the following steps:
One, taking 5g hollow carbon fiber and 5g particle diameter is the Fe of 10nm～10 μ m
3o
4powder, 100g mould silica gel and 3g silica gel solid agent, first by hollow carbon fiber and Fe
3o
4powder is put into ultrasonic dispersion 10min in ultrasonic disperser, and then mixed powder is joined in neoprene after mixing, more ultrasonic dispersion 10min, finally adds curing agent, then mixes, and obtains having the slurry of mobility;
Two, linen being immersed in to mass concentration is to soak 5 hours in 10% sodium hydroxide solution, and then to be immersed in mass concentration be to soak 5 hours in 10% butyl titanate solution, in temperature, be after drying under the condition of 100 ℃, immerse again in slurry prepared by step 1 and flood 3h, obtain hanging textiles; Wherein linen has the hole that aperture is 0.5mm;
Three, hanging textile surface step 3 being obtained after frictioning, be placed on temperature and be in the baking oven of 100 ℃ and dry 50min, obtain putting on a suit of armour formula Wave suction composite material.
In this test one, the hollow carbon fiber described in step 1 is by the patent No.: described in ZL201010152182.6 prepared by method, concrete preparation method carries out according to the following steps: one, carbon source material is put into graphite crucible, and graphite crucible is placed in to atmosphere sintering furnace, then by atmosphere sintering stove evacuation, make pressure in stove reach 0.1Pa; Two, in atmosphere sintering furnace, be filled with high pure nitrogen, make gas pressure intensity in atmosphere sintering furnace reach 0.2MPa; Three, be incubated 2h after making temperature in atmosphere sintering furnace rise to 1200 ℃ with the speed of 5 ℃/min, then, with stove cool to room temperature, obtain hollow carbon fiber; Wherein the carbon source described in step 1 is the mixture of polyvinyl alcohol and urea, wherein polyvinyl alcohol: the mass ratio of urea is 1:80; In step 2, the purity of high pure nitrogen is >=99.999%(quality).
The put on a suit of armour formula Wave suction composite material of this test one preparation is cut to three samples, be designated as 1#, 2# and 3#, carry out performance test, occurrence is as table 1:
The put on a suit of armour formula Wave suction composite material of table 1 test one preparation carries out performance
| Sample | Maximum reflection decay (dB) | The highest absorption band width (< 10dB) |
| 1# | 25.403 | 5.88 |
| 2# | 51.777 | 4.77 |
| 3# | 37.324 | 7.28 |
Claims (8)
1. improve a preparation method for the put on a suit of armour formula Wave suction composite material of absorbing property, the preparation method who it is characterized in that improving the put on a suit of armour formula Wave suction composite material of absorbing property carries out according to the following steps:
One, wave-absorber and liquid organic polymer are mixed, then add the curing agent of organic polymer, then mix, obtain having the slurry of mobility; Wave-absorber in step 1 is hollow carbon fiber and ferritic mixture, or the mixture of hollow carbon fiber and metallic magnetic powder, or the mixture of hollow carbon fiber and carbon-based powder;
Two, textiles is immersed after surface modification in slurry prepared by step 1 and flood 0.5h～10h, obtain hanging textiles; Wherein textiles has 10 μ m～1mm holes;
Three, hanging textile surface step 2 being obtained, after frictioning, roll extrusion or extrusion operation, is dried, and obtains putting on a suit of armour formula Wave suction composite material;
Hollow carbon fiber in step 1 is that caliber is 0.2 μ m～1 μ m, and length reaches the hollow carbon fiber of Centimeter Level;
Hollow carbon fiber preparation method carries out according to the following steps: (one) puts into graphite crucible by carbon source material, and graphite crucible is placed in to atmosphere sintering furnace, then by atmosphere sintering stove evacuation, makes pressure in stove reach 0.1Pa～1Pa; (2) in atmosphere sintering furnace, be filled with high pure nitrogen or argon gas, make gas pressure intensity in atmosphere sintering furnace reach 0.2MPa～2.5MPa; (3) be incubated 1h～4h after making temperature in atmosphere sintering furnace rise to 900 ℃～1500 ℃ with the speed of 5 ℃/min～30 ℃/min, then, with stove cool to room temperature, obtain hollow carbon fiber; Wherein the carbon source described in step () is urea or is the mixture of polyvinyl alcohol and urea, wherein polyvinyl alcohol: the mass ratio of urea is 1:50～100; In step (two), the purity of high pure nitrogen is >=99.999%(quality); The purity of argon gas is >=99.999%(quality); Liquid organic polymer described in step 1 is liquid-state silicon gel or liquid polyurethane.
2. a kind of preparation method who improves the put on a suit of armour formula Wave suction composite material of absorbing property according to claim 1, is characterized in that in hollow carbon fiber in step 1 and ferritic mixture that hollow carbon fiber and ferritic mass ratio are 1:1～10.
3. a kind of preparation method who improves the put on a suit of armour formula Wave suction composite material of absorbing property according to claim 1, is characterized in that in the mixture of hollow carbon fiber in step 1 and metallic magnetic powder, the mass ratio of hollow carbon fiber and metallic magnetic powder is 1:1～10.
4. a kind of preparation method who improves the put on a suit of armour formula Wave suction composite material of absorbing property according to claim 1, is characterized in that in the mixture of hollow carbon fiber and carbon-based powder in step 1, the mass ratio of hollow carbon fiber and carbon-based powder is 1:1～10.
5. a kind of preparation method who improves the put on a suit of armour formula Wave suction composite material of absorbing property according to claim 1, is characterized in that the textiles in step 2 is linen, cotton or chemical fiber cloth.
6. a kind of preparation method who improves the put on a suit of armour formula Wave suction composite material of absorbing property according to claim 1, it is characterized in that the textile surface modification method in step 2 is: first textiles is immersed in to 0.5h～10h in aqueous slkali, and then be immersed in surface modification agent solution and soak 0.5h～10h, complete the surface modification of textiles.
7. a kind of preparation method who improves the put on a suit of armour formula Wave suction composite material of absorbing property according to claim 6, is characterized in that the alkali of the textile surface modification method in step 2 refers to NaOH, potassium hydroxide or ammoniacal liquor.
8. a kind of preparation method who improves the put on a suit of armour formula Wave suction composite material of absorbing property according to claim 7, is characterized in that the surface modifier of the textile surface modification method in step 2 refers to stearic acid, butyl titanate or Span80.
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| CN201110402503.8A CN102493204B (en) | 2011-12-07 | 2011-12-07 | Preparation method of hanging wave absorbing composite material |
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| CN201110402503.8A CN102493204B (en) | 2011-12-07 | 2011-12-07 | Preparation method of hanging wave absorbing composite material |
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| 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 |
| CN105568664B (en) * | 2015-12-30 | 2017-08-01 | 浙江博尼锦纶科技有限公司 | A kind of preparation method of the polyamide-based textile material with good electro-magnetic wave absorption ability in ultra-wide spectral range |
| CN107123500A (en) * | 2017-06-13 | 2017-09-01 | 安徽中研辐射防护有限公司 | A kind of composite wave-suction material |
| CN107118559A (en) * | 2017-06-13 | 2017-09-01 | 安徽中研辐射防护有限公司 | A kind of enhanced Wave suction composite material and preparation method thereof |
| CN107365135A (en) * | 2017-07-21 | 2017-11-21 | 无锡博轩电磁材料科技有限公司 | W types barium ferrite/carbonyl iron composite wave-absorbing silica gel piece and preparation method thereof |
| CN112941905A (en) * | 2021-02-22 | 2021-06-11 | 南通纺织丝绸产业技术研究院 | Carbon fiber radar wave-absorbing material |
| CN114481635A (en) * | 2022-02-10 | 2022-05-13 | 安徽隆润高分子材料有限公司 | Production method, device and application of equipment invisible cloth |
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