CN106810284A - A kind of preparation method of double-deck high temperature resistant heat insulation Wave suction composite material - Google Patents
A kind of preparation method of double-deck high temperature resistant heat insulation Wave suction composite material Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of double-deck high temperature resistant heat insulation Wave suction composite material, belong to absorbing material preparing technical field.The present invention is first by alchlor, the materials such as zirconium carbonate are prepared into ceramic fibre powder, nano titanium oxide is weighed again, coupling agent adds ceramic fibre powder after adding deionized water mixing, heating stirring obtains pulp solution after ultrasonic disperse, moulding by casting after pulp solution and waterglass are mixed, sinter to obtain matrix material, antiradar coatings are prepared using epoxy resin be coated in matrix surface, double-deck high temperature resistant heat insulation Wave suction composite material is can obtain after solidification, basic unit of the present invention is with porous structure ceramic fibrous material, not only resistivity is high, and its thermal conductivity is low, resistance to elevated temperatures is good, can quickly be absorbed and electromagnetic wave of decaying after being combined with outer coating, absorption efficiency is high, and frequency range, light weight, good mechanical performance, coating is firmly combined with by coupling agent and basic unit, it is difficult for drop-off.
Description
Technical field
The present invention relates to a kind of preparation method of double-deck high temperature resistant heat insulation Wave suction composite material, belong to absorbing material and prepare skill
Art field.
Background technology
With the development of modern high technology, the electromagnetic interference and electromagnetic compatibility problem that electromagnetic wave causes are increasingly serious, its
Not only electronic instrument, equipment are interfered and damage, the serious international competitiveness for restricting China's electronic product and equipment, pollution
Environment, endangers human health, and electromagnetic-wave leakage also entail dangers to national information safety and military vital strategic secrets safety.Therefore send out
Exhibition electromagnetic-wave absorbent, the electromagnetic energy between effective attenuation electronic equipment and the external world is propagated, for the peace for improving electronic product
Full reliability, prevents the strike of electromagnetic pulse weapon, it is ensured that information, communication, network, Transmission system it is safe and smooth with important
Meaning.Absorbing material needs the condition for meeting：1. when electromagnetic wave incident is on material, it can not reflect as far as possible and to greatest extent
Ground enters material internal, that is, require that material meets impedance matching；2. into the electromagnetism wave energy in material, promptly almost all declines
Cut, that is, require that material meets decay matching.
Also have that frequency band is narrow, density is big, the low shortcoming of performance in terms of the development of absorbing material both at home and abroad at present, using model
Enclose by a definite limitation, thus the task of top priority is to explore light weight, wideband, pollution-free, environment resistant multifunctional efficient to inhale ripple material
Material.Conduct a research compatible type absorbing material, can compatible metric wave, centimeter wave, millimeter involve the multiwave suction ripple such as infrared laser
Material, widens suction ripple wave band, is one of direction of future development.
Ceramic fibre is that the heat preserving and insulating material being made up of ceramic fibre has that high temperature resistant, heat endurance be good, low thermal conductivity
The advantages of being shaken with mechanical resistant, thus be obtained in the industry such as machinery, metallurgy, petrochemical industry, building materials and electronics and be widely applied, but
It is in the fewer of absorbing material area research.
The content of the invention
The technical problems to be solved by the invention：For traditional absorbing material, with absorbing, frequency range is narrow, density is big lacks
Point, absorption rate are slow, microwave absorbing coating bad adhesion, the drawbacks of easily coming off, there is provided a kind of double-deck high temperature resistant heat insulation is inhaled ripple and answered
The materials such as alchlor, zirconium carbonate are first prepared into ceramic fibre powder by the preparation method of condensation material, the present invention, then weigh nanometer
Titanium dioxide, coupling agent add ceramic fibre powder after adding deionized water mixing, and to obtain slurry molten for heating stirring after ultrasonic disperse
Liquid, moulding by casting after pulp solution and waterglass are mixed, sinters to obtain matrix material, and preparing suction ripple using epoxy resin applies
Material is coated in matrix surface, and double-deck high temperature resistant heat insulation Wave suction composite material is can obtain after solidification, and basic unit of the present invention is with many
Pore structure ceramic fibre material, not only resistivity is high, and its thermal conductivity is low, and resistance to elevated temperatures is good, after being combined with outer coating
Can quickly absorb and electromagnetic wave of decaying, absorption efficiency is high, and frequency range, light weight, good mechanical performance, coating by coupling agent and
Basic unit is firmly combined with, difficult for drop-off.
In order to solve the above technical problems, the present invention is using technical scheme as described below：
（1）40~50g alchlors, 1~3g zirconium carbonates, 0.5~0.7g yttrium acetates and 0.1~0.3g lanthanum acetates is weighed respectively to add
Enter in 150~200mL deionized waters, it is 4~5 to adjust pH with the acetic acid solution of mass fraction 10%, and 60~80 are heated to after regulation
DEG C, insulated and stirred adds 1~4g triethyl phosphates after mixing 20~30min, continues to stir 20~30min, after stirring 30~
30~50min of vacuum distillation under 50kPa pressure, obtains concentrate after distillation, concentrate is carried out into spinning, is put after collecting filamentary fibers
Enter in baking oven, 8~10h is dried at a temperature of 100~120 DEG C, dried filamentary fibers are put into tube furnace, in nitrogen atmosphere
700~900 DEG C are warming up under protection, 2~3h is heat-treated, crushed after heat treatment, cross 80~100 mesh sieves, obtain ceramic fibre powder；
（2）Weigh respectively 3~5g nano silicons, 0.3~0.5g3- glycydoxies triethoxysilane and
0.3~0.5g Lauryl Alcohol esters are added in 150~200g deionized waters, add the above-mentioned ceramics of 10~20g fine after stirring mixing
Dimension powder, 10~15min of ultrasonic disperse after addition is heated to 300~400 DEG C after dispersion, slurry is obtained after 1~2h of stirring mixing
Solution；
（3）In mass ratio 5:1 mixes above-mentioned pulp solution and waterglass, is poured into mould after 30~50min of mixing, and
10~12h is dried under the conditions of 130~150 DEG C, the demoulding after drying obtains solid and is put into tube furnace after the demoulding, protected in nitrogen atmosphere
600~700 DEG C are warming up under shield, 1~2h of heat preservation sintering is cooled to room temperature after sintering, obtain matrix material；
（4）180~200g epoxy resin E-51,3~5g nano ferriferrous oxides, 20~30g oleic acid, 5~10g second are weighed respectively
Diamines and 10~15g polyvinylpyrrolidones, are coated uniformly on the surface of above-mentioned matrix material after being uniformly mixed, coating is thick
It is 1~2mm to spend, and the matrix material after coating is put into baking oven, and 8~10h is solidified at a temperature of 60~70 DEG C, is cooled down after solidification
Taken out to room temperature, you can obtain double-deck high temperature resistant heat insulation Wave suction composite material.
Application process of the invention：The double-deck high temperature resistant heat insulation Wave suction composite material that the present invention is prepared can be applicable to be built
Field is built to mitigate electromagnetic radiation to the harm caused by people；During for building, bridge, tower etc., radar can be prevented pseudo-
Picture；In communication base, can be used to improve communication quality;It is tall and big near airport, harbour, navigation mark, TV station and receiving station
It is architectural, can be used to eliminate reflection interference.After tested, being made the standard sample of photo that thickness is 2~4mm carries out electro-magnetic wave absorption survey
Examination, the absorption peak in 8~10GHz is -25~-20dB, there is 4~6 absworption peaks in 10~28GHz frequency ranges, is showed
Excellent broadband absorbing effect, the peak value of its reflection loss is that the wideband width of -10dB is 7.8~8.0GHz, and dielectric constant is
3.4~3.6, relative permeability 0.95~1.02.
Compared with other method, Advantageous Effects are the present invention：
（1）The characteristics of preferable electromagnetic-wave absorbent should have absorption band wide, light weight, thickness of thin, good physical and mechanical properties；
（2）Meet absorbing material well has matching properties to electromagnetic wave, incoming electromagnetic wave energy is entered material to greatest extent
Material is internal without reflecting on its front surface, and the electromagnetism wave energy into material internal is promptly by rapidly absorption, decay；
（3）The Wave suction composite material that the present invention is prepared can be in metric wave, centimeter wave, millimeter wave and the ultratvide frequency band such as infrared
Work, and with preferable environment and Acclimation temperature performance.
Specific embodiment
40~50g alchlors, 1~3g zirconium carbonates, 0.5~0.7g yttrium acetates and 0.1~0.3g lanthanum acetates are weighed respectively
It is added in 150~200mL deionized waters, it is 4~5 to adjust pH with the acetic acid solution of mass fraction 10%, it is heated to 60 after regulation~
80 DEG C, insulated and stirred adds 1~4g triethyl phosphates after mixing 20~30min, continues to stir 20~30min, 30 after stirring
30~50min of vacuum distillation under~50kPa pressure, obtains concentrate after distillation, concentrate is carried out into spinning, after collecting filamentary fibers
It is put into baking oven, 8~10h is dried at a temperature of 100~120 DEG C, dried filamentary fibers is put into tube furnace, in nitrogen gas
700~900 DEG C are warming up under atmosphere protection, 2~3h is heat-treated, crushed after heat treatment, cross 80~100 mesh sieves, obtain ceramic fibre powder
End；Weigh respectively 3~5g nano silicons, 0.3~0.5g3- glycydoxies triethoxysilane and 0.3~
0.5g Lauryl Alcohol esters are added in 150~200g deionized waters, and the above-mentioned ceramic fibre powder of 10~20g is added after stirring mixing
End, 10~15min of ultrasonic disperse after addition is heated to 300~400 DEG C after dispersion, it is molten to obtain slurry after 1~2h of stirring mixing
Liquid；In mass ratio 5:1 mixes above-mentioned pulp solution and waterglass, is poured into mould after 30~50min of mixing, and 130
10~12h is dried under the conditions of~150 DEG C, the demoulding after drying obtains solid and is put into tube furnace, under nitrogen atmosphere protection after the demoulding
600~700 DEG C are warming up to, 1~2h of heat preservation sintering is cooled to room temperature after sintering, obtain matrix material；180~200g is weighed respectively
Epoxy resin E-51,3~5g nano ferriferrous oxides, 20~30g oleic acid, 5~10g ethylenediamines and 10~15g polyvinyl pyrroles
Alkanone, is coated uniformly on the surface of above-mentioned matrix material after being uniformly mixed, coating thickness is 1~2mm, by the base after coating
Body material is put into baking oven, and 8~10h is solidified at a temperature of 60~70 DEG C, room temperature taking-up is cooled to after solidification, you can obtain bilayer
High temperature resistant heat insulation Wave suction composite material.
Example 1
40g alchlors, 1g zirconium carbonates, 0.5g yttrium acetates and 0.1g lanthanum acetates is weighed respectively to be added in 150mL deionized waters,
It is 4 to adjust pH with the acetic acid solution of mass fraction 10%, and 60 DEG C are heated to after regulation, and 1g phosphoric acid is added after insulated and stirred mixing 20min
Triethyl, continue stir 20min, after stirring under 30kPa pressure vacuum distillation 30min, after distillation concentrate, by concentrate
Spinning is carried out, is put into baking oven after collecting filamentary fibers, 8h is dried at a temperature of 100 DEG C, dried filamentary fibers are put into pipe
In formula stove, 700 DEG C are warming up under nitrogen atmosphere protection, are heat-treated 2h, crushed after heat treatment, cross 80 mesh sieves, obtain ceramic fibre
Powder；3g nano silicons, 0.3g3- glycydoxies triethoxysilane and the carbon of 0.3g 12 are weighed respectively
Alcohol ester is added in 150g deionized waters, and the above-mentioned ceramic fibre powder of 10g, ultrasonic disperse after addition are added after stirring mixing
10min, is heated to 300 DEG C after dispersion, pulp solution is obtained after stirring mixing 1h；In mass ratio 5:1 by above-mentioned pulp solution and
Waterglass mixes, and is poured into mould after mixing 30min, and 10h is dried under the conditions of 130 DEG C, the demoulding after drying, after the demoulding
Solid is put into tube furnace, and 600 DEG C are warming up under nitrogen atmosphere protection, and heat preservation sintering 1h is cooled to room temperature after sintering, obtain base
Body material；180g epoxy resin E-51,3g nano ferriferrous oxide, 20g oleic acid, 5g ethylenediamines and 10g polyethylene are weighed respectively
Pyrrolidones, is coated uniformly on the surface of above-mentioned matrix material after being uniformly mixed, coating thickness is 1mm, after coating
Matrix material is put into baking oven, and 8h is solidified at a temperature of 60 DEG C, room temperature taking-up is cooled to after solidification, you can obtain double-deck high temperature resistant
Heat-insulated Wave suction composite material.
The double-deck high temperature resistant heat insulation Wave suction composite material that the present invention is prepared can be applicable to building field to mitigate electromagnetism
Harm caused by Radiation On Humans；During for building, bridge, tower etc., radar pseudomorphism can be prevented；In communication base, can
For improving communication quality;On pile near airport, harbour, navigation mark, TV station and receiving station, can be used to disappear
Except reflection interference.After tested, being made the standard sample of photo that thickness is 2mm carries out electro-magnetic wave absorption test, the absworption peak in 8GHz
It is -20dB to be worth, and has 4 absworption peaks in 10GHz frequency ranges, shows excellent broadband absorbing effect, the peak value of its reflection loss
For the wideband width of -10dB is 7.8GHz, dielectric constant is 3.4, relative permeability 0.95.
Example 2
45g alchlors, 2g zirconium carbonates, 0.6g yttrium acetates and 0.2g lanthanum acetates is weighed respectively to be added in 175mL deionized waters,
It is 4.5 to adjust pH with the acetic acid solution of mass fraction 10%, and 70 DEG C are heated to after regulation, and 2.5g is added after insulated and stirred mixing 25min
Triethyl phosphate, continue stir 25min, after stirring under 40kPa pressure vacuum distillation 40min, after distillation concentrate, will be dense
Contracting liquid carries out spinning, is put into baking oven after collecting filamentary fibers, and 9h is dried at a temperature of 110 DEG C, and dried filamentary fibers are put
Enter in tube furnace, 800 DEG C are warming up under nitrogen atmosphere protection, be heat-treated 2.5h, crushed after heat treatment, cross 90 mesh sieves, must make pottery
Porcelain fiber dust；4g nano silicons, 0.4g3- glycydoxies triethoxysilane and 0.4g are weighed respectively
Lauryl Alcohol ester is added in 175g deionized waters, and the above-mentioned ceramic fibre powder of 15g is added after stirring mixing, ultrasound point after addition
13min is dissipated, 350 DEG C are heated to after dispersion, pulp solution is obtained after stirring mixing 1.5h；In mass ratio 5:1 is molten by above-mentioned slurry
Liquid and waterglass mix, and are poured into mould after mixing 40min, and 11h is dried under the conditions of 140 DEG C, the demoulding, the demoulding after drying
Solid being obtained afterwards to be put into tube furnace, 650 DEG C being warming up under nitrogen atmosphere protection, heat preservation sintering 1.5h is cooled to room after sintering
Temperature, obtains matrix material；190g epoxy resin E-51,4g nano ferriferrous oxide, 25g oleic acid, 8g ethylenediamines and 13g are weighed respectively
Polyvinylpyrrolidone, is coated uniformly on the surface of above-mentioned matrix material after being uniformly mixed, coating thickness is 1.5mm, will
Matrix material after coating is put into baking oven, and 9h is solidified at a temperature of 65 DEG C, and room temperature taking-up is cooled to after solidification, you can obtain double
Layer high temperature resistant heat insulation Wave suction composite material.
The double-deck high temperature resistant heat insulation Wave suction composite material that the present invention is prepared can be applicable to building field to mitigate electromagnetism
Harm caused by Radiation On Humans；During for building, bridge, tower etc., radar pseudomorphism can be prevented；In communication base, can
For improving communication quality;On pile near airport, harbour, navigation mark, TV station and receiving station, can be used to disappear
Except reflection interference.After tested, being made the standard sample of photo that thickness is 3mm carries out electro-magnetic wave absorption test, the absworption peak in 9GHz
It is -23dB to be worth, and has 5 absworption peaks in 20GHz frequency ranges, shows excellent broadband absorbing effect, the peak value of its reflection loss
For the wideband width of -10dB is 7.9GHz, dielectric constant is 3.5, relative permeability 1.00.
Example 3
50g alchlors, 3g zirconium carbonates, 0.7g yttrium acetates and 0.3g lanthanum acetates is weighed respectively to be added in 200mL deionized waters,
It is 5 to adjust pH with the acetic acid solution of mass fraction 10%, and 80 DEG C are heated to after regulation, and 4g phosphoric acid is added after insulated and stirred mixing 30min
Triethyl, continue stir 30min, after stirring under 50kPa pressure vacuum distillation 50min, after distillation concentrate, by concentrate
Spinning is carried out, is put into baking oven after collecting filamentary fibers, 10h is dried at a temperature of 120 DEG C, dried filamentary fibers are put into pipe
In formula stove, 900 DEG C are warming up under nitrogen atmosphere protection, are heat-treated 3h, crushed after heat treatment, cross 100 mesh sieves, obtain ceramic fibre
Powder；5g nano silicons, 0.5g3- glycydoxies triethoxysilane and the carbon of 0.5g 12 are weighed respectively
Alcohol ester is added in 200g deionized waters, and the above-mentioned ceramic fibre powder of 20g, ultrasonic disperse after addition are added after stirring mixing
15min, is heated to 400 DEG C after dispersion, pulp solution is obtained after stirring mixing 2h；In mass ratio 5:1 by above-mentioned pulp solution and
Waterglass mixes, and is poured into mould after mixing 50min, and 12h is dried under the conditions of 150 DEG C, the demoulding after drying, after the demoulding
Solid is put into tube furnace, and 700 DEG C are warming up under nitrogen atmosphere protection, and heat preservation sintering 2h is cooled to room temperature after sintering, obtain base
Body material；200g epoxy resin E-51,5g nano ferriferrous oxide, 30g oleic acid, 10g ethylenediamines and 15g polyethylene are weighed respectively
Pyrrolidones, is coated uniformly on the surface of above-mentioned matrix material after being uniformly mixed, coating thickness is 2mm, after coating
Matrix material is put into baking oven, and 10h is solidified at a temperature of 70 DEG C, room temperature taking-up is cooled to after solidification, you can obtain double-deck resistance to height
The heat-insulated Wave suction composite material of temperature.
The double-deck high temperature resistant heat insulation Wave suction composite material that the present invention is prepared can be applicable to building field to mitigate electromagnetism
Harm caused by Radiation On Humans；During for building, bridge, tower etc., radar pseudomorphism can be prevented；In communication base, can
For improving communication quality;On pile near airport, harbour, navigation mark, TV station and receiving station, can be used to disappear
Except reflection interference.After tested, being made the standard sample of photo that thickness is 4mm carries out electro-magnetic wave absorption test, the absworption peak in 10GHz
It is -20dB to be worth, and has 6 absworption peaks in 28GHz frequency ranges, shows excellent broadband absorbing effect, the peak value of its reflection loss
For the wideband width of -10dB is 8.0GHz, dielectric constant is 3.6, relative permeability 1.02.
Claims (1)
1. a kind of preparation method of double-deck high temperature resistant heat insulation Wave suction composite material, it is characterised in that specific preparation process is：
（1）40~50g alchlors, 1~3g zirconium carbonates, 0.5~0.7g yttrium acetates and 0.1~0.3g lanthanum acetates is weighed respectively to add
Enter in 150~200mL deionized waters, it is 4~5 to adjust pH with the acetic acid solution of mass fraction 10%, and 60~80 are heated to after regulation
DEG C, insulated and stirred adds 1~4g triethyl phosphates after mixing 20~30min, continues to stir 20~30min, after stirring 30~
30~50min of vacuum distillation under 50kPa pressure, obtains concentrate after distillation, concentrate is carried out into spinning, is put after collecting filamentary fibers
Enter in baking oven, 8~10h is dried at a temperature of 100~120 DEG C, dried filamentary fibers are put into tube furnace, in nitrogen atmosphere
700~900 DEG C are warming up under protection, 2~3h is heat-treated, crushed after heat treatment, cross 80~100 mesh sieves, obtain ceramic fibre powder；
（2）Weigh respectively 3~5g nano silicons, 0.3~0.5g3- glycydoxies triethoxysilane and
0.3~0.5g Lauryl Alcohol esters are added in 150~200g deionized waters, add the above-mentioned ceramics of 10~20g fine after stirring mixing
Dimension powder, 10~15min of ultrasonic disperse after addition is heated to 300~400 DEG C after dispersion, slurry is obtained after 1~2h of stirring mixing
Solution；
In mass ratio 5:1 mixes above-mentioned pulp solution and waterglass, is poured into mould after 30~50min of mixing, and 130
10~12h is dried under the conditions of~150 DEG C, the demoulding after drying obtains solid and is put into tube furnace, under nitrogen atmosphere protection after the demoulding
600~700 DEG C are warming up to, 1~2h of heat preservation sintering is cooled to room temperature after sintering, obtain matrix material；
（3）180~200g epoxy resin E-51,3~5g nano ferriferrous oxides, 20~30g oleic acid, 5~10g second are weighed respectively
Diamines and 10~15g polyvinylpyrrolidones, are coated uniformly on the surface of above-mentioned matrix material after being uniformly mixed, coating is thick
It is 1~2mm to spend, and the matrix material after coating is put into baking oven, and 8~10h is solidified at a temperature of 60~70 DEG C, is cooled down after solidification
Taken out to room temperature, you can obtain double-deck high temperature resistant heat insulation Wave suction composite material.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107840643A (en) * | 2017-11-23 | 2018-03-27 | 济南大学 | One kind inhales wave mode ceramic base composite insulation boards and preparation method thereof |
| CN109534779A (en) * | 2018-12-27 | 2019-03-29 | 中国建筑材料科学研究总院有限公司 | A kind of high-strength ceramic fibrous insulating material and preparation method thereof |
| WO2020114090A1 (en) * | 2018-12-05 | 2020-06-11 | 洛阳尖端技术研究院 | Lightweight and highly elastic wave-absorbing material and preparation method therefor |
| CN112830771A (en) * | 2021-01-19 | 2021-05-25 | 中国科学院福建物质结构研究所 | Alumina-titanium oxide double-layer composite ceramic and preparation method and application thereof |
| CN114801363A (en) * | 2022-06-27 | 2022-07-29 | 中国航发四川燃气涡轮研究院 | Aeroengine outfield test background comprehensive suppression structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107840643A (en) * | 2017-11-23 | 2018-03-27 | 济南大学 | One kind inhales wave mode ceramic base composite insulation boards and preparation method thereof |
| WO2020114090A1 (en) * | 2018-12-05 | 2020-06-11 | 洛阳尖端技术研究院 | Lightweight and highly elastic wave-absorbing material and preparation method therefor |
| CN109534779A (en) * | 2018-12-27 | 2019-03-29 | 中国建筑材料科学研究总院有限公司 | A kind of high-strength ceramic fibrous insulating material and preparation method thereof |
| CN112830771A (en) * | 2021-01-19 | 2021-05-25 | 中国科学院福建物质结构研究所 | Alumina-titanium oxide double-layer composite ceramic and preparation method and application thereof |
| CN112830771B (en) * | 2021-01-19 | 2022-06-10 | 中国科学院福建物质结构研究所 | Alumina-titanium oxide double-layer composite ceramic and preparation method and application thereof |
| CN114801363A (en) * | 2022-06-27 | 2022-07-29 | 中国航发四川燃气涡轮研究院 | Aeroengine outfield test background comprehensive suppression structure |
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Application publication date: 20170609 |