CN108841311A - A kind of rare earth mixing with nano alumina powder infrared stealth coating - Google Patents
A kind of rare earth mixing with nano alumina powder infrared stealth coating Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/34—Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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Abstract
The present invention relates to a kind of rare earth mixing with nano alumina powder infrared stealth coatings, using AlCl3·6H2O、ErCl3And Na2CO3With 2.5 ~ 4: 0.025 ~ 0.038: 5 molar ratio, partial size is prepared in the rare earth mixing with nano Al of 20 ~ 50 nm ranges by direct precipitation method2O3Powder;Recycle silane coupling agent KH570 to rare earth mixing with nano Al2O3Powder is modified, and wherein the dosage of KH570 is rare earth mixing with nano Al2O3The 6% ~ 12% of powder quality;By modified RE dopen Nano Al2O3Powder is scattered in dehydrated alcohol in the ratio of 1 g/mL, and is sprayed on aluminium substrate again after mixing with polyurethane, obtains rare earth mixing with nano Al by solidification2O3Powder infrared stealth coating, wherein rare earth mixing with nano Al2O3Mass ratio with polyurethane is 1 ~ 2: 3.Preparation process of the present invention is easy, and infrared stealth coating density is small, infrared reflectivity is low, transparency is high, has good physics, mechanically and chemically performance.
Description
Technical field
A kind of rare earth mixing with nano alumina powder infrared stealth coating of the present invention is related to the shielding and suction of electromagnetic infrared wave
Material is received, Infrared stealthy materials technical field is particularly belonged to.
Background technique
Infrared stealth technology refers to the infrared signature for changing target, reduces target by infrared detector probability of detection
A kind of means.It includes both sides content:First is that weakening the infrared intensity of target, it is allowed to the spirit lower than infrared detector
Sensitivity, it is stealthy to detector to achieve the purpose that;Second is that changing the infra-red radiation frequency range of target, atmosphere infrared window is avoided
Mouthful, or the infrared intensity by controlling target each section, the contrast of target and background is reduced, Infrared image camouflage color is reached
Effect.So Infrared stealthy materials should have following characteristics:(1) satisfactory infrared emittance, (2) good thermostabilization
The associativity of property and base-material, (3) multiband good compatibility, structure is simple, light firm.So red according to nano-metal-oxide
The particle size of outer stealth material is much smaller than the wavelength of infrared waves, more much better than than conventional material to the transmitance of infrared waves, greatly
The big reflectivity for reducing wave;Its specific surface area is more much bigger than blocks of solid simultaneously, and special skin effect and bulk effect is presented,
The electronic state of particle changes, so that the infrared light emission rate of material significantly reduces.When infrared light is incident on nano particle
Surface when, a part it is weak due to molecular energy level transition absorption, another part scattering after again made with other particles
With light generates Multiple Scattering between particle and intensity is weak.Nano-metal-oxide is a kind of polar molecule, dielectric constant simultaneously
It is all relatively large with dielectric loss, there is good absorption to electromagnetic infrared wave, lower infrared emittance can be obtained.Therefore red
Nowadays, the research of nano-metal-oxide Infrared stealthy materials is increasingly taken seriously for the fast development of outer Detection Techniques.
A kind of entitled hollow alumina ceramic microsphere modified polyurethane material of open (bulletin) number CN106634514A and its
Preparation method, through ultrasound, magnetic agitation, hydro-thermal, heat treatment and etc. prepare hollow alumina ceramic microsphere modified polyurethane
Material, though have many advantages, such as high-intensitive, low-heat lead, wearability it is good.Show biggish oxygen from its preparation flow and product property
Change 0.1~5um of aluminium microspherulite diameter, functional filler aluminum oxide micro-sphere is caused to disperse unevenness in polyurethane.Inorganic oxide simultaneously
Aluminium ceramic microsphere do not do it is modified cannot be well compatible with polymer material polyurethane, lead between two substances that there are gap, surfaces
Imperfect bonding causes interfacial failure so as to cause stress concentration, and preparation process is relatively complicated.
The present invention is with nanometer Al2O3For powder as filler, what polyurethane was prepared as matrix has excellent low infrared hair
Penetrate the camouflage coating of rate.Rare earth mixing with nano Al2O3Powder has good absorption to electromagnetic infrared wave, and compound painting can be effectively reduced
The infrared emittance of layer improves rare earth mixing with nano Al2O3Powder in the base content when, infrared emittance can be significantly reduced.But
It is that ought improve rare earth mixing with nano Al simply2O3When powder content in the base, although infrared emittance reduces, at this time
Coating can become poor to the electromagnetic wave stealth effect of other frequencies, especially the absorption of radar wave;Wherein rare earth element er
Doping so that Al2O3Crystal produces more defects, and part rare earth metal Er atom is instead of Al2O3Aluminium in lattice
Position causes more distortions of lattice, generates smaller crystal grain, mentions high surface energy, improves the interior energy of infrared film, improves
Al2O3The infrared emission performance of coating.Simultaneously be one of the hot physical property of object itself according to emissivity, numerical value change only with object
Type, the related theory of property and surface state of body, the present invention select silane coupling agent KH570 to rare earth mixing with nano Al2O3
Powder is modified, and increases Al2O3Powder and polyurethane interface combination degree, improve Al2O3Powder disperse when uniformity and
Loading improves the surface property and Al of material2O3The compatibility of powder and matrix reduces the polarity of Bulk coat material, favorably
In reduction coating material infrared emittance.
The present invention obtains silane coupling agent KH570 to Al by technological innovation2O3Powder-modified optimum condition, rare earth gold
Belong to the optimum doping content of Er and explores suitable Al2O3The mass ratio of powder and polyurethane, to obtain receiving with rear-earth-doped
Rice Al2O3Powder is the infrared stealth coating material of single inorganic filler, and infrared emittance meets Infrared stealthy materials requirement, and
Coating shows superior mechanical property and heat-proof quality, and corrosion resistance significantly improves, obvious technical effects.It is bis- using IR-2
Wave band emissivity tester measures rare earth mixing with nano Al2O3The infrared emittance of powder infrared stealth coating is in 3~5um wave band
It is 0.47~0.52,8~14um wave band is 0.35~0.42, and performance is than existing Al2O3Infrared stealthy materials are more excellent.
The present invention is solved with rare earth mixing with nano Al2O3Powder is that the infrared of function admirable is prepared in single inorganic filler
Camouflage coating material, while a nanometer Al is improved by KH5702O3Powder disperses unevenness in polyurethane, poor compatibility, and because
The disadvantages of stress is concentrated and causes interfacial failure, improves the performance of Bulk coat material.
Summary of the invention
The present invention is for density is big, infrared emittance is high existing for existing Infrared stealthy materials, wideband absorbs difficulty etc. no
Foot, the invention discloses a kind of rare earth mixing with nano alumina powder infrared stealth coatings.Rare earth mixing with nano oxidation of the present invention
The preparation process of aluminium powder body infrared stealth coating is simple, and infrared emittance is low, good mechanical property.
A kind of preparation step of rare earth mixing with nano alumina powder infrared stealth coating of the present invention is as follows:
Step 1:Prepare rare earth mixing with nano Al2O3Powder
Control AlCl3·6H2O、ErCl3With Na2CO3Molar ratio be 2.5~4: 0.025~0.038: 5, Na2CO3It is molten
Liquid is added drop-wise to AlCl with the speed of 1-2mL/min3·6H2O and ErCl3Solution in, mechanical stirring generates heavy under 40 DEG C of water-baths
It forms sediment, after reacting 30min, stops 20 min of stirring ageing;Product is filtered by vacuum, then is washed with deionized water laggard to no chloride ion
Row microwave drying, obtained presoma is polished, then 1.5~2h is calcined at 500-700 DEG C, obtains rare earth mixing with nano
Al2O3Powder;
Step 2:Prepare modified RE dopen Nano Al2O3Powder
In the ratio of 1g/4mL, by rare earth mixing with nano Al2O3Powder is added to absolute ethanol, and is uniformly dispersed with ultrasonic wave
Afterwards, rare earth mixing with nano Al is added2O3The silane coupling agent KH570 of powder quality 6%~12%, and in 50 DEG C of water bath with thermostatic control
Lower stirring 1h;Thereafter it is modified mixed liquor to filter through sand core funnel, is ground again after microwave drying 3-6min, obtain modified RE
Dopen Nano Al2O3Powder;
Step 3:The preparation of coating
Control modified RE dopen Nano Al2O3The quality of powder and polyurethane is 1~2: 3;Using ultrasonic dispersion,
By modified RE dopen Nano Al2O3Powder is scattered in dehydrated alcohol according to the ratio of 1g/mL, and poly- ammonia is added after stirring 5min
After ester, then high-speed stirred dispersion 1h, modified RE dopen Nano Al is obtained2O3Polyurethane coating;Aluminium substrate is cleaned with ethyl alcohol
Completely, it and is fixed on spray coating plate, then by modified RE dopen Nano Al2O3Polyurethane coating be sprayed on aluminium substrate, after
It is cured to obtain rare earth mixing with nano alumina powder infrared stealth coating.
The rare earth mixing with nano alumina powder infrared stealth coating with a thickness of 20~50 μm.
3~5um of infrared emittance of the rare earth mixing with nano alumina powder infrared stealth coating:0.47~
0.52,8~14um:0.35~0.42.
Beneficial effects of the present invention:Nanometer Al of the present invention2O3Powder average grain diameter is in 20~50nm, while Al2O3Metal oxygen
Compound is a kind of polar molecule, and dielectric constant and dielectric loss are all relatively large, and rare earth mixing with nano shape Al2O3Metal oxidation
The dielectric constant of object is more several times greater than the dielectric constant of bulk, thus rare earth mixing with nano Al2O3Powder has electromagnetic infrared wave good
Good absorption, can be effectively reduced the infrared emittance of composite material.The doping of rare earth metal Er is so that Al2O3Crystal produces
More defects cause more distortions of lattice, improve a nanometer Al2O3Energy in powder.Recycle silane coupling agent KH570
To the rear-earth-doped Al of preparation2O3Powder is modified, in Al2O3Powder surface introduces lipophilic group, so that Al2O3Powder turns
For oil wet grain, to increase Al2O3Powder and polyurethane interface combination degree, increase Al2O3Uniformity when powder disperses
And loading, so that Al2O3Powder is preferably compatible with matrix, improves the performance of integral composite.It is with polyurethane simultaneously
Adhesive, can make coating show superior mechanical property, and corrosion resistance significantly improves.It is surveyed using IR-2 two waveband emissivity
Examination instrument measures rare earth mixing with nano Al2O3Powder infrared stealth coating infrared emittance is 0.47~0.52,8 in 3~5um wave band
~14um wave band is 0.35~0.42, and performance is than existing Al2O3Infrared stealthy materials are more excellent.Manufacture craft letter of the present invention
Just, infrared stealth coating has many advantages, such as low infrared emittance, good mechanical property, corrosion-resistant, has in terms of Infrared stealthy materials
There is very strong practical value, there is the advantages that spraying is uniform, high-quality, defect is few, and thickness is controllable.
Specific embodiment
Embodiment 1
(1) 1mmol/mLAlCl is configured3·6H2O solution, 0.1mmol/mLErCl3Solution and 1mmol/mLNa2CO3Solution.
(2) AlCl of 25mL is measured3Solution and 2.5mLErCl3Solution is put into a beaker, is placed in 40 DEG C of heating water baths.
(3) Na of 50mL is measured2CO3Solution is equally placed in 40 DEG C of heating water baths in another beaker.
(4) Na2CO3AlCl is added with 1mL/min speed in solution3·6H2O solution, mechanical stirring generate precipitating, reaction
After 30min, stop stirring, it is made to be aged 20min.
(5) after reaction, it is filtered through vacuum filtration machine, the mode being washed with deionized water, washing to no chloride ion.
(6) sediment is dried with optimized microwave drying process.Presoma after drying is polished, is put into
Crucible is placed in Muffle furnace, is calcined 1.5h at 500 DEG C, obtains rare earth Er doping Al2O3Powder.
(7) 5g rare earth mixing with nano Al is weighed2O3Powder adds 20mL dehydrated alcohol in wherein in beaker.
(8) it is uniformly dispersed with supersonic generator, addition rare earth Er adulterates Al2O310% silane of powder quality
Coupling agent KH570, is transferred in conical flask, is placed in 50 DEG C of water bath with thermostatic control, and 1h is stirred.
(9) reaction solution is taken out, is filtered with sand core funnel, microwave drying 5min, products obtained therefrom grinds to obtain modified RE slightly
Dopen Nano alumina powder.
(10) the anhydrous of 3ml is first dispersed for the modified RE dopen Nano alumina powder of 3g using ultrasonic dispersion
In ethyl alcohol, stirs 5 minutes, 6g polyurethane is then added, then disperse 1h through high-speed stirred, finally carries out spraying operation.
(11) first by 45 × 45mm before spraying2Specification aluminium substrate is cleaned up with ethyl alcohol to be fixed on spray coating plate, then will
Coating is sprayed on aluminium substrate, cured to obtain rare earth mixing with nano alumina powder polyurethane coating.Utilize IR-2 two waveband
Emissivity tester measures infrared emittance:3~5 μm of wave bands are 0.49, are 0.40 in 8~14 mu m wavebands.
Embodiment 2
(1) 1mmol/mLAlCl is configured3·6H2O solution, 0.1mmol/mLErCl3Solution and 1mmol/mLNa2CO3Solution.
(2) AlCl of 30mL is measured3Solution and 2.8mLErCl3Solution is put into a beaker, is placed in 40 DEG C of heating water baths.
(3) Na of 50mL is measured2CO3Solution is equally placed in 40 DEG C of heating water baths in another beaker.
(4) Na2CO3AlCl is added with 2mL/min speed in solution3·6H2O solution, mechanical stirring generate precipitating, reaction
After 30min, stop stirring, it is made to be aged 20min.
(5) after reaction, it is filtered through vacuum filtration machine, the mode being washed with deionized water, washing to no chloride ion.
(6) sediment is dried with optimized microwave drying process.Presoma after drying is polished, is put into
Crucible is placed in Muffle furnace, is calcined 1.5h at 700 DEG C, obtains rare earth Er doping Al2O3Powder.
(7) 5g rare earth Er dopen Nano Al is weighed2O3Powder adds 20mL dehydrated alcohol in wherein in beaker.
(8) it is uniformly dispersed with supersonic generator, addition rare earth Er adulterates Al2O38% silane of powder quality is even
Even agent KH570, is transferred in conical flask, is placed in 50 DEG C of water bath with thermostatic control, and 1h is stirred.
(9) reaction solution is taken out, is filtered with sand core funnel, microwave drying 5min, products obtained therefrom grinds to obtain modified RE slightly
Dopen Nano alumina powder.
(10) the anhydrous of 4ml is first dispersed for the modified RE dopen Nano alumina powder of 4g using ultrasonic dispersion
In ethyl alcohol, stirs 5 minutes, 6g polyurethane is then added, then disperse 1h through high-speed stirred, finally carries out spraying operation.
(11) first by 45 × 45mm before spraying2Specification aluminium substrate is cleaned up with ethyl alcohol to be fixed on spray coating plate, then will
Coating is sprayed on aluminium substrate, cured to obtain rare earth mixing with nano alumina powder polyurethane coating.
Infrared emittance is measured using IR-2 two waveband emissivity tester:3~5 mu m wavebands are 0.47, in 8~14 μm of waves
Section is 0.35.
Claims (3)
1. a kind of rare earth mixing with nano alumina powder infrared stealth coating, it is characterised in that:The infrared stealth coating
Preparation step is as follows:
Step 1:Prepare rare earth mixing with nano Al2O3Powder
Control AlCl3·6H2O、ErCl3With Na2CO3Molar ratio be 2.5 ~ 4: 0.025 ~ 0.038: 5, Na2CO3Solution is with 1-2
The speed of mL/min is added drop-wise to AlCl3·6H2O and ErCl3Solution in, under 40 DEG C of water-baths mechanical stirring generate precipitating, reaction
After 30 min, stop stirring ageing 20min;Product is filtered by vacuum, then carries out microwave after being washed with deionized water to no chloride ion
Dry, obtained presoma is polished, then 1.5 ~ 2 h are calcined at 500-700 DEG C, obtains rare earth mixing with nano Al2O3Powder
Body;
Step 2:Prepare modified RE dopen Nano Al2O3Powder
In the ratio of 1g/4mL, by rare earth mixing with nano Al2O3Powder is added to absolute ethanol, and after being uniformly dispersed with ultrasonic wave, is added
Add rare earth mixing with nano Al2O3The silane coupling agent KH570 of powder quality 6% ~ 12%, and 1h is stirred under 50 DEG C of waters bath with thermostatic control;Its
It is modified mixed liquor afterwards to filter through sand core funnel, is ground again after microwave drying 3-6 min, obtains modified RE dopen Nano
Al2O3Powder;
Step 3:The preparation of coating
Control modified RE dopen Nano Al2O3The quality of powder and polyurethane is 1 ~ 2: 3;Using ultrasonic dispersion, will be modified
Rare earth mixing with nano Al2O3Powder is scattered in dehydrated alcohol according to the ratio of 1g/mL, polyurethane is added after stirring 5min, then high
After speed is dispersed with stirring 1h, modified RE dopen Nano Al is obtained2O3Polyurethane coating;Aluminium substrate is cleaned up with ethyl alcohol,
And be fixed on spray coating plate, then by modified RE dopen Nano Al2O3Polyurethane coating be sprayed on aluminium substrate, by solid
Change obtains rare earth mixing with nano alumina powder infrared stealth coating.
2. a kind of rare earth mixing with nano alumina powder infrared stealth coating according to claim 1, it is characterised in that:Institute
The rare earth mixing with nano alumina powder infrared stealth coating stated with a thickness of 20 ~ 50 μm.
3. a kind of rare earth mixing with nano alumina powder infrared stealth coating according to claim 1, it is characterised in that:Institute
3 ~ the 5um of infrared emittance for the rare earth mixing with nano alumina powder infrared stealth coating stated:0.47 ~ 0.52,8 ~ 14 um:
0.35~0.42。
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CN115228434A (en) * | 2022-07-21 | 2022-10-25 | 南京信息工程大学 | Surface-wrapped gamma-Al 2 O 3 : carbon nanotube adsorbent with Dy & lt 3+ & gt particles and preparation method thereof |
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CN114623728A (en) * | 2022-03-22 | 2022-06-14 | 湖南中泰特种装备有限责任公司 | Preparation method of bulletproof plate with infrared stealth function and bulletproof plate |
CN114623728B (en) * | 2022-03-22 | 2024-03-26 | 湖南中泰特种装备有限责任公司 | Preparation method of bulletproof plate with infrared stealth function and bulletproof plate |
CN115228434A (en) * | 2022-07-21 | 2022-10-25 | 南京信息工程大学 | Surface-wrapped gamma-Al 2 O 3 : carbon nanotube adsorbent with Dy & lt 3+ & gt particles and preparation method thereof |
CN115228434B (en) * | 2022-07-21 | 2023-09-01 | 南京信息工程大学 | gamma-Al coated on surface 2 O 3 : dy3+ particle carbon nanotube adsorbent and preparation method thereof |
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