CN101294047B - Radar wave absorbing paint with hollow microsphere as filling material and preparation method thereof - Google Patents

Radar wave absorbing paint with hollow microsphere as filling material and preparation method thereof Download PDF

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Publication number
CN101294047B
CN101294047B CN2008101145553A CN200810114555A CN101294047B CN 101294047 B CN101294047 B CN 101294047B CN 2008101145553 A CN2008101145553 A CN 2008101145553A CN 200810114555 A CN200810114555 A CN 200810114555A CN 101294047 B CN101294047 B CN 101294047B
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condition
product
suction filtration
tiny balloon
behind
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CN101294047A (en
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肇研
段跃新
张桐
梁振方
张润
罗云烽
薛亚娟
袁璐
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Beihang University
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Beihang University
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Abstract

The invention discloses a radar wave absorbing coating with the filler of hollow microsphere, which consists of epoxy-silicone resin 30 to 40wt%, a leveling agent 0.2 to 0.4wt%, a thickening agent 0.2 to 0.4wt%, hollow microsphere plated with metal coating 40 to 55wt%, and solvent being the rest. The radar wave absorbing coating with the hollow microsphere filler has the maximal absorptivity of 20 dB at the electromagnetic wave frequency band of 2 to 18 GHz, and has the frequency width of 5 GHz larger than 10 dB.

Description

A kind of is the radar wave absorbing paint and preparation method thereof of filler with the tiny balloon
Technical field
The present invention relates to a kind of radar wave absorbing paint and preparation method thereof, more particularly say, be meant that a kind of chemical plating technology that adopts is the radar wave absorbing paint of filler at the surface clad coating of functionalization tiny balloon.
Background technology
Tiny balloon is a kind of inorganic powder, compares with metal powder, and less, high temperature resistant, antiacid alkali of density and oxidisability are strong.Handle if modification is carried out on its surface, realize surface metalation, then might solve big, the shortcomings such as high-temperature behavior is poor, anti-oxidant, acid and alkali-resistance ability of density that traditional absorbing material exists.At present, thus adopt suitable technology that the research that tiny balloon carries out surface modification preparation lightweight radar absorbing has been caused scholars' extensive concern.
Because the tiny balloon granularity is little, density is little and characteristics such as physicals excellence, the tiny balloon of surface metalation can replace the preparation that the bigger traditional wave absorbing agent of density is used for microwave absorbing coating, thereby solve that the density that traditional microwave absorbing coating exists is big, high-temperature behavior is poor, anti-oxidant and shortcoming such as acid and alkali-resistance ability, realize the target of absorbing material " thin, light, wide, strong ".
Summary of the invention
It is the radar wave absorbing paint of filler with the tiny balloon that one of purpose of the present invention provides a kind of, and this radar wave absorbing paint is prepared burden by following mass percent:
Epoxy silicone resin 30～40%;
Flow agent 0.2～0.4%;
Thickening material 0.2～0.4%;
The tiny balloon 40～55% of surface clad coating;
The solvent surplus.
The tiny balloon of described surface clad coating is made up of tiny balloon and metal plating, and metal plating is coated on the surface of tiny balloon, and the thickness 50～250nm of metal plating.The composition of described metal plating can be nickel (Ni), iron (Fe) or the cobalt (Co) of simple substance, also can be the iron (Fe) that contains 10～30wt% and cobalt (Co) composite deposite of 70～90wt%, also can be the iron (Fe) that contains 10～30wt% and nickel (Ni) composite deposite of 70～90wt%, also can be the nickel (Ni) that contains 50～70wt% and cobalt (Co) composite deposite of 30～50wt%, also can be the iron (Fe) that contains 5～20wt%, the cobalt (Co) of 20～40wt% and nickel (Ni) composite deposite of surplus.The relative permittivity of the tiny balloon of this surface clad coating is 20～70, and magnetic permeability is 1.5～2.0; Density 2.6～the 3.5g/cm of the tiny balloon of surface clad coating 3
Described is that the radar wave absorbing paint of filler is 20dB in the maximum absorbance of 2～18GHz hertzian wave frequency range with the tiny balloon, is 5GHz greater than the frequency range of 10dB.
Another object of the present invention is that proposing a kind of is the preparation method of the radar wave absorbing paint of filler with the tiny balloon, adopts the plating metal on surface coating of chemical plating technology at tiny balloon in this method.
The present invention adopts the advantage of chemical plating technology preparation process: (1) adds coupling step in the pre-treatment process, improve the quantity of active site in the reactivation process by adding KH550, and the physical bond mode that changes original active site is a Chemical bond, improve the bonding force of active site with this, and then the bonding force of metal plating after the raising electroless plating, make coating have certain wear resistance, be difficult for being peeled off; (2) adopt the single stage method activating process, the stability and the shelf life of having improved plating bath, and can effectively improve the quantity of active site, and can be in reactivation process, by regulating Sn 2+Content, control the quantity of active Pd, thereby be applicable to different chemical plating cladding process; (3) prepare on tiny balloon by chemical plating technology and have nano level metal plating in (metal plating iron+nickel+cobalt layer), can be by adjusting the kind and the amount ratio of chemical plating technology parameter and metal-salt, obtain having the material of different relative permittivitys and relative magnetic permeability, thereby obtain the tiny balloon of surface clad coating of fine quality.
Embodiment
The present invention is described in further detail below in conjunction with embodiment.
The present invention be a kind of be the radar wave absorbing paint of filler with the tiny balloon, this radar wave absorbing paint is prepared burden by following mass percent:
Epoxy silicone resin 30～40%;
Flow agent 0.2～0.4%;
Thickening material 0.2～0.4%;
The tiny balloon 40～55% of surface clad coating;
The solvent surplus.
In the present invention, flow agent can be polyacrylate(s) (CAB-551-0.01, CAB-551-0.2 (Eastman Chemical Company)), polyether-modified polysiloxane-based (BYK333, BYK306, BYK323 (German Bi Ke chemical company));
In the present invention, thickening material can be vinylformic acid and multipolymer (sodium polyacrylate, ACRYLIC EMULSION) thereof, polyurethanes (SN-612 (thinking Nore chemical industry company limited), RM-8W (ROHM AND HAAS chemical industry company limited));
In the present invention, solvent can be dimethylbenzene or propyl carbinol; Can be the mixture of dimethylbenzene and propyl carbinol also, the mass percent of dimethylbenzene be 60～80 in the mixture, and surplus is a propyl carbinol;
Preparation is that the method for the radar wave absorbing paint of filler is that the tiny balloon of (A) epoxy silicone resin and surface clad coating is put into homogenizer with the tiny balloon, under 600～1000r/min condition, take out after stirring 15～30min, make first mixture; (B) first mixture is ground at triple-roller mill make second mixture that particle diameter is 20～40 μ m after grinding 15～30min in the machine; (C) put into homogenizer behind second mixture, flow agent, thickening material and the solvent, under 600～1000r/min condition, behind stirring 15～30min, leave standstill 3～5min, promptly make radar wave absorbing paint.
In the present invention, the tiny balloon of surface clad coating is made up of tiny balloon and metal plating, and metal plating is coated on the surface of tiny balloon, and the thickness 50～250nm of metal plating.The composition of described metal plating can be nickel (Ni), iron (Fe) or the cobalt (Co) of simple substance, also can be the iron (Fe) that contains 10～30wt% and cobalt (Co) composite deposite of 70～90wt%, also can be the iron (Fe) that contains 10～30wt% and nickel (Ni) composite deposite of 70～90wt%, also can be the nickel (Ni) that contains 50～70wt% and cobalt (Co) composite deposite of 30～50wt%, also can be the iron (Fe) that contains 5～20wt%, the cobalt (Co) of 20～40wt% and nickel (Ni) composite deposite of surplus.
The tiny balloon of the chemical plating technology system of employing surface clad coating of the present invention includes following steps:
The first step: the choosing of body material
Body material is the tiny balloon of particle diameter 1～20 μ m;
In the present invention, to choose the main component that Qinhuangdao glass microballon company limited produces be SiO to tiny balloon 2And Al 2O 3Tiny balloon;
Second step: to the pre-treatment of matrix
(A) preparation alkali cleaning treatment solution
The alkali cleaning treatment solution is made up of sodium hydroxide (NaOH) and deionized water;
The sodium hydroxide (NaOH) that adds 10～20g in the deionized water of consumption: 500ml;
(B) alkali washing process
The tiny balloon that first step is chosen adds in the alkali cleaning treatment solution;
The alkali cleaning condition: 60～80 ℃ alkali cleaning temperature, under the condition of power 500W, magnetic agitation disperses to make first reaction solution behind reaction 60～90min;
First reaction solution is washed acquisition first product;
Washing condition: under room temperature (25 ℃) condition, first reaction solution is diluted (adding 800～1000ml deionized water in every 100ml first reaction solution dilutes) with deionized water, behind sedimentation 60～90min supernatant liquid is removed, repeats 2～3 times after acquisition first product;
In the present invention, adopting washing is with the Na in first reaction solution on the basis that does not influence the tiny balloon dispersiveness +, OH -And the impurities in raw materials removal, thereby obtain first product.
(C) preparation coupling processing liquid
Coupling processing liquid is by silane coupling agent and ethanol (C 2H 5OH) form;
Ethanol (the C of consumption: 500ml 2H 5OH) silane coupling agent that adds 0.5～2g in;
(D) coupling process
First product is added in the coupling processing liquid;
Coupling condition:, under the condition of power 500W, behind ultra-sonic dispersion reaction 6～8h, leave standstill 3～5min and make second reaction solution 35～50 ℃ coupling temperature;
Second reaction solution is carried out suction filtration obtain second product;
The suction filtration condition: under room temperature (25 ℃) condition, the vacuum tightness of regulating suction filtration vacuum instrument is-0.1MPa to obtain second product behind suction filtration time 5～10min;
In the present invention, adopting suction filtration is with the coupling agent in second reaction solution, ethanol (C 2H 5OH) remove, thereby obtain second product.
(E) preparation activation treatment liquid
Activation treatment liquid is by tin protochloride (SnCl 22H 2O), sodium stannate (Na 2SnO 3), Palladous chloride (PdCl 2), hydrochloric acid (HCl) and deionized water form;
Add 1～2g tin protochloride (SnCl in the hydrochloric acid of consumption: 100ml (HCl) 22H 2O) and the Palladous chloride (PdCl of 0.2～0.5g 2), add 12.5～50g tin protochloride (SnCl behind reaction 10～20min 22H 2O), the sodium stannate (Na of 2～4g 2SnO 3) and the deionized water of 400ml;
(F) activating process
Second product is added in the activation treatment liquid;
Activation condition:, under the condition of power 500W, behind ultra-sonic dispersion reaction 30～60min, leave standstill 3～5min and make the 3rd reaction solution 50～70 ℃ activation temperature;
The 3rd reaction solution is carried out suction filtration obtain third product;
The suction filtration condition: under room temperature (25 ℃) condition, the vacuum tightness of regulating suction filtration vacuum instrument is-0.1MPa to obtain third product behind suction filtration time 5～10min;
In the present invention, adopting suction filtration is with the Sn in the 3rd reaction solution 2+, Sn 4+, Pd 2+, Cl -And H +Remove, wherein Sn 4+Be at Sn 2+With Palladous chloride (PdCl 2) chemical reaction takes place obtain.
(G) preparation dispergation treatment solution
The dispergation treatment solution is made up of hydrochloric acid (HCl) and deionized water;
The hydrochloric acid (HCl) that adds 50～100ml in the deionized water of consumption: 500ml;
(H) separate adhesive process
The 3rd reaction product is added in the dispergation treatment solution;
Dispergation condition:, under the condition of power 500W, behind ultra-sonic dispersion reaction 1～3min, leave standstill 3～5min and make the 4th reaction solution 35～50 ℃ dispergation temperature;
The 4th reaction solution is carried out suction filtration obtain the 4th product;
The suction filtration condition: under room temperature (25 ℃) condition, the vacuum tightness of regulating suction filtration vacuum instrument is-0.1MPa to obtain the 4th product behind suction filtration time 5～10min;
In the present invention, adopting suction filtration is with the Sn in the 4th reaction solution 2+And Cl -And H +Remove, thereby obtain the 4th product.Sn wherein 2+Be attached on the tiny balloon of the 4th product;
The 4th product is put into loft drier, behind dry 3～4h under 90～110 ℃ the condition, make the 5th product;
The 3rd step: electroless plating is handled
(A) preparation chemical plating fluid
Chemical plating fluid is by metal-salt, inferior sodium phosphate (NaH 2PO 2), trisodium citrate (Na 3C 6H 5O 7) and the deionized water composition; Described metal-salt is single nickel salt (NiSO 46H 2O), rose vitriol (CoSO 47H 2O) and ferrous sulfate (FeSO 47H 2O) a kind of in or two kinds or three kinds.
Trisodium citrate (the Na that adds 20～110g in the deionized water of consumption: 500ml 3C 6H 5O 7), the metal-salt of 8～40g and the inferior sodium phosphate (NaH of 8.5～42.5g 2PO 2);
In chemical plating fluid, add ammoniacal liquor (NH 3H 2O) pH=8.5～10 of the described chemical plating fluid of adjusting obtain chemical plating fluid;
(B) chemical plating technology
The 5th product that makes is put into chemical plating fluid;
The electroless plating condition: 70～90 ℃ electroless plating temperature, under the condition of power 500W, react 60～120min under the condition of ultra-sonic dispersion after, leave standstill 3～5min and make the 5th reaction solution;
The 5th reaction solution is carried out suction filtration obtain the 6th product;
The suction filtration condition: under room temperature (25 ℃) condition, the vacuum tightness of regulating suction filtration vacuum instrument is-0.1MPa to obtain the 6th product behind suction filtration time 5～10min;
In the present invention, adopting suction filtration is with the C in the 5th reaction solution 6H 5O 7 3-, H 2PO 3 -, Na +Remove with metal ion, thereby obtain the 6th product.Described metal ion can be Ni 2+, Co 2+Or Fe 2+, also can be Ni 2+With Co 2+Metal ion, also can be Ni 2+With Fe 2+Metal ion, also can be Fe 2+With Co 2+Metal ion, also can be Ni 2+, Co 2+And Fe 2+Metal ion.
The 6th product is put into loft drier, behind dry 3～4h under 90～110 ℃ the condition, make the 7th product, promptly on tiny balloon, be coated with metal plating.
Embodiment 1:
Radar wave absorbing paint is prepared burden by following mass percent:
Epoxy silicone resin 40%;
Flow agent is CAB-551-0.01 0.2%;
Thickening material is a polypropylene sodium 0.2%;
The tiny balloon 40% of surface clad coating;
Solvent is dimethylbenzene (C 8H 10) surplus.
In this example, preparation is that the method for the radar wave absorbing paint of filler is that the tiny balloon of (A) epoxy silicone resin and surface clad coating is put into homogenizer with the tiny balloon, under the 1000r/min condition, take out behind the stirring 15min, make first mixture; (B) first mixture is ground in the machine at triple-roller mill make second mixture that particle diameter is 30 μ m after grinding 15min; (C) put into homogenizer behind second mixture, flow agent, thickening material and the solvent, under the 1000r/min condition, behind the stirring 15min, leave standstill 3min, promptly make radar wave absorbing paint.Adopting radar wave absorbing paint that aforesaid method makes coating thickness 2mm and be 20dB in the maximum absorbance of 2～18GHz hertzian wave frequency range, is 5GHz greater than the frequency range of 10dB.
The tiny balloon of the surface clad coating that this is routine is that (the KW-10 tiny balloon that glass microballon company limited in Qinhuangdao produces, main component is SiO for the tiny balloon of particle diameter 5～10 μ m 2And Al 2O 3), the metal-plated nickel dam forms, the metal-plated nickel dam is coated on the surface of tiny balloon, and the thickness 250nm of metal-plated nickel dam.
Adopt the preparation process of chemical plating technology clad metal nickel layer on tiny balloon as follows:
The first step: the choosing of body material
Body material is the KW-10 tiny balloon of particle diameter 5～10 μ m;
Second step: to the pre-treatment of matrix
(A) preparation alkali cleaning treatment solution
The alkali cleaning treatment solution is made up of sodium hydroxide (NaOH) and deionized water;
The sodium hydroxide (NaOH) that adds 10g in the deionized water of consumption: 500ml;
(B) alkali washing process
The tiny balloon that first step is chosen adds in the alkali cleaning treatment solution;
The alkali cleaning condition: 80 ℃ alkali cleaning temperature, under the condition of power 500W, magnetic agitation disperses to make first reaction solution behind (the high-power magnetic stirring apparatus of 88-1, Changzhou Guohua Electric Appliance Co., Ltd. produces) reaction 90min;
First reaction solution is washed acquisition first product;
The washing condition: under 25 ℃ of conditions, in first reaction solution of 100ml, add the 800ml deionized water and stirring and evenly dilute, behind the sedimentation 60min supernatant liquid is removed, repeats 2 times after acquisition first product;
In the present invention, adopting washing is with the Na in first reaction solution on the basis that does not influence the tiny balloon dispersiveness +, OH -And the impurities in raw materials removal, thereby obtain first product.
(C) preparation coupling processing liquid
Coupling processing liquid is by Y-aminopropyl triethoxysilane (KH550) and ethanol (C 2H 5OH) form;
Ethanol (the C of consumption: 500ml 2H 5OH) the Y-aminopropyl triethoxysilane that adds 0.5g in;
(D) coupling process
First product is added in the coupling processing liquid;
Coupling condition:, under the condition of power 500W, behind ultra-sonic dispersion (KQ-500B type ultrasonic cleaner, Kunshan Ultrasonic Instruments Co., Ltd. produces) the reaction 8h, leave standstill 3min and make second reaction solution 50 ℃ coupling temperature;
Second reaction solution is carried out suction filtration obtain second product;
The suction filtration condition: under 25 ℃ of conditions, the vacuum tightness of regulating suction filtration vacuum instrument (SHZ-III type recirculated water vacuum pump) is-0.1MPa to obtain second product behind the suction filtration time 5min;
In the present invention, adopting suction filtration is to add 40% removal and the adding ethanol (C of the consumption of coupling agent in second reaction solution 2H 5OH) 95% of consumption is removed, thereby obtains second product.
(E) preparation activation treatment liquid
Activation treatment liquid is by tin protochloride (SnCl 22H 2O), sodium stannate (Na 2SnO 3), Palladous chloride (PdCl 2), hydrochloric acid (HCl) and deionized water form;
Add 1g tin protochloride (SnCl in the hydrochloric acid of consumption: 100ml (HCl) 22H 2O) and the Palladous chloride (PdCl of 0.2g 2), add 12.5g tin protochloride (SnCl behind the reaction 20min 22H 2O), the sodium stannate (Na of 2g 2SnO 3) and the deionized water of 400ml;
(F) activating process
Second product is added in the activation treatment liquid;
Activation condition:, under the condition of power 500W, behind ultra-sonic dispersion (KQ-500B type ultrasonic cleaner, Kunshan Ultrasonic Instruments Co., Ltd. produces) the reaction 60min, leave standstill 3min and make the 3rd reaction solution 70 ℃ activation temperature;
The 3rd reaction solution is carried out suction filtration obtain third product;
The suction filtration condition: under 25 ℃ of conditions, the vacuum tightness of regulating suction filtration vacuum instrument (SHZ-III type recirculated water vacuum pump) is-0.1MPa to obtain third product behind the suction filtration time 5min;
In the present invention, adopting suction filtration is with the Sn in the 3rd reaction solution 2+, Sn 4+, Pd 2+, Cl -And H +Remove, wherein Sn 4+Be at Sn 2+With Palladous chloride (PdCl 2) chemical reaction takes place obtain.
(G) preparation dispergation treatment solution
The dispergation treatment solution is made up of hydrochloric acid (HCl) and deionized water;
The hydrochloric acid (HCl) that adds 50ml in the deionized water of consumption: 500ml;
(H) separate adhesive process
The 3rd reaction product is added in the dispergation treatment solution;
Dispergation condition:, under the condition of power 500W, behind ultra-sonic dispersion (KQ-500B type ultrasonic cleaner, Kunshan Ultrasonic Instruments Co., Ltd. produces) the reaction 3min, leave standstill 3min and make the 4th reaction solution 35 ℃ dispergation temperature;
The 4th reaction solution is carried out suction filtration obtain the 4th product;
The suction filtration condition: under 25 ℃ of conditions, the vacuum tightness of regulating suction filtration vacuum instrument (SHZ-III type recirculated water vacuum pump) is-0.1MPa to obtain the 4th product behind the suction filtration time 5min;
In the present invention, adopting suction filtration is with the Sn in the 4th reaction solution 2+And Cl -And H +Remove, thereby obtain the 4th product.Sn wherein 2+Be attached on the tiny balloon of the 4th product;
The 4th product is put into loft drier, behind dry 4h under 90 ℃ the condition, make the 5th product;
The 3rd step: electroless plating is handled
(A) preparation chemical plating fluid
Chemical plating fluid is by single nickel salt (NiSO 46H 2O), inferior sodium phosphate (NaH 2PO 2), trisodium citrate (Na 3C 6H 5O 7) and the deionized water composition;
Trisodium citrate (the Na that adds 20g in the deionized water of consumption: 500ml 3C 6H 5O 7), the single nickel salt (NiSO of 8g 46H 2O) and the inferior sodium phosphate (NaH of 8.5g 2PO 2);
In chemical plating fluid, add ammoniacal liquor (NH 3H 2O) pH=8.5 of the described chemical plating fluid of adjusting obtains chemical plating fluid;
(B) chemical plating technology
The 5th product that makes is put into chemical plating fluid;
Electroless plating condition:, under the condition of power 500W, behind the reaction 60min, leave standstill 3min and make the 5th reaction solution under the condition of ultra-sonic dispersion (KQ-500B type ultrasonic cleaner, Kunshan Ultrasonic Instruments Co., Ltd. produces) 70 ℃ electroless plating temperature;
The 5th reaction solution is carried out suction filtration obtain the 6th product;
The suction filtration condition: under 25 ℃ of conditions, the vacuum tightness of regulating suction filtration vacuum instrument (SHZ-III type recirculated water vacuum pump) is-0.1MPa to obtain the 6th product behind the suction filtration time 5min;
In the present invention, adopting suction filtration is with the C in the 5th reaction solution 6H 5O 7 3-, H 2PO 3 -, Na +, Ni 2+Remove, obtain the 6th product from face.
The 6th product is put into loft drier, behind dry 4h under 90 ℃ the condition, make the 7th product, promptly on tiny balloon, be coated with the metal-plated nickel dam.
Adopt the tiny balloon (KW-10 tiny balloon+metal nickel dam) of the surface clad coating that above-mentioned technology makes, relative permittivity when coating thickness is 250nm is 50, relative magnetic permeability is 1.5, and the density of the tiny balloon of surface clad coating is 3.5g/cm 3The relative permittivity of KW-10 tiny balloon is 4, and relative magnetic permeability is 1.The tiny balloon of the surface clad coating of KW-10 tiny balloon+metal nickel dam is 20dB in the maximum absorbance of 2～18GHz hertzian wave frequency range, is 5GHz greater than the frequency range of 10dB.
Adopt above-mentioned same process chemical plating metal cobalt (Co) layer on the KW-10 tiny balloon, the relative permittivity when coating thickness is 250nm is 40, and relative magnetic permeability is 1.4, and the density of the tiny balloon of surface clad coating is 3.5g/cm 3The tiny balloon of the surface clad coating of KW-10 tiny balloon+layer of metal cobalt is 20dB in the maximum absorbance of 2～18GHz hertzian wave frequency range, is 5GHz greater than the frequency range of 10dB.
Adopt above-mentioned same process chemical plating metal iron (Fe) layer on the KW-10 tiny balloon, the relative permittivity when coating thickness is 250nm is 60, and relative magnetic permeability is 2.0, and the density of the tiny balloon of surface clad coating is 3.4g/cm 3The tiny balloon of the surface clad coating of KW-10 tiny balloon+metallic iron layer is 20dB in the maximum absorbance of 2～18GHz hertzian wave frequency range, is 6GHz greater than the frequency range of 10dB.
Embodiment 2:
Radar wave absorbing paint is prepared burden by following mass percent:
Epoxy silicone resin 30%;
Flow agent is CAB-551-0.2 0.3%;
Thickening material is a polyurethanes 0.3%;
The tiny balloon 50% of surface clad coating;
Solvent is the mixture of dimethylbenzene and propyl carbinol, the mixture surplus.
Middle dimethylbenzene is 60wt%, and propyl carbinol is 40wt%
Preparation is that the method for the radar wave absorbing paint of filler is that the tiny balloon of (A) epoxy silicone resin and surface clad coating is put into homogenizer with the tiny balloon, under the 800r/min condition, takes out behind the stirring 20min, makes first mixture; (B) first mixture is ground in the machine at triple-roller mill make second mixture that particle diameter is 40 μ m after grinding 15min; (C) put into homogenizer behind second mixture, flow agent, thickening material and the solvent, under the 800r/min condition, behind the stirring 20min, leave standstill 5min, promptly make radar wave absorbing paint.Adopting radar wave absorbing paint that aforesaid method makes coating thickness 2mm and be 20dB in the maximum absorbance of 2～18GHz hertzian wave frequency range, is 8GHz greater than the frequency range of 10dB.
The tiny balloon of the surface clad coating that this is routine is that KW-10 tiny balloon, the metal nickel plating+iron+cobalt layer of particle diameter 10～20 μ m formed, and metal nickel plating+iron+cobalt layer is coated on the surface of tiny balloon, and the thickness 150nm of metal-plated nickel dam.The mass percent of iron is 15 in metal nickel plating+iron+cobalt layer, and the mass percent of cobalt is 40, and surplus is a nickel.
The employing chemical plating technology is that the preparation process of the thick metal nickel plating+iron+cobalt layer of the KW-10 tiny balloon surface coating 150nm of particle diameter 10～20 μ m is as follows:
The first step: the choosing of body material
Body material is the KW-10 tiny balloon of particle diameter 10～20 μ m;
Second step: to the pre-treatment of matrix
(A) preparation alkali cleaning treatment solution
The alkali cleaning treatment solution is made up of sodium hydroxide (NaOH) and deionized water;
The sodium hydroxide (NaOH) that adds 15g in the deionized water of consumption: 500ml;
(B) alkali washing process
The tiny balloon that first step is chosen adds in the alkali cleaning treatment solution;
The alkali cleaning condition: 70 ℃ alkali cleaning temperature, under the condition of power 500W, magnetic agitation disperses to make first reaction solution behind (the high-power magnetic stirring apparatus of 88-1, Changzhou Guohua Electric Appliance Co., Ltd. produces) reaction 75min;
First reaction solution is repeatedly washed acquisition first product;
The washing condition: under 25 ℃ of conditions, in first reaction solution of 100ml, add the 1000ml deionized water and stirring and evenly dilute, behind the sedimentation 75min supernatant liquid is removed, repeats 3 times after acquisition first product;
In the present invention, adopting washing is with the Na in first reaction solution on the basis that does not influence the tiny balloon dispersiveness +, OH -And the impurities in raw materials removal, thereby obtain first product.
(C) preparation coupling processing liquid
Coupling processing liquid is by Y-aminopropyl triethoxysilane (KH550) and ethanol (C 2H 5OH) form;
Ethanol (the C of consumption: 500ml 2H 5OH) KH550 that adds 1g in;
(D) coupling process
First product is added in the coupling processing liquid;
Coupling condition:, under the condition of power 500W, behind ultra-sonic dispersion (KQ-500B type ultrasonic cleaner, Kunshan Ultrasonic Instruments Co., Ltd. produces) the reaction 7h, leave standstill 4min and make second reaction solution 40 ℃ coupling temperature;
Second reaction solution is carried out suction filtration obtain second product;
The suction filtration condition: under 25 ℃ of conditions, the vacuum tightness of regulating suction filtration vacuum instrument (SHZ-III type recirculated water vacuum pump) is-0.1MPa to obtain second product behind the suction filtration time 8min;
In the present invention, adopting suction filtration is to add 45% removal and the adding ethanol (C of the consumption of coupling agent in second reaction solution 2H 5OH) 98% of consumption is removed, thereby obtains second product.
(E) preparation activation treatment liquid
Activation treatment liquid is by tin protochloride (SnCl 22H 2O), sodium stannate (Na 2SnO 3), Palladous chloride (PdCl 2), hydrochloric acid (HCl) and deionized water form;
Add 1.5g tin protochloride (SnCl in the hydrochloric acid of consumption: 100ml (HCl) 22H 2O) and the Palladous chloride (PdCl of 0.4g 2), add 37.5g tin protochloride (SnCl behind the reaction 15min 22H 2O), the sodium stannate (Na of 3g 2SnO 3) and the deionized water of 400ml;
(F) activating process
Second product is added in the activation treatment liquid;
Activation condition:, under the condition of power 500W, behind ultra-sonic dispersion (KQ-500B type ultrasonic cleaner, Kunshan Ultrasonic Instruments Co., Ltd. produces) the reaction 45min, leave standstill 4min and make the 3rd reaction solution 60 ℃ activation temperature;
The 3rd reaction solution is carried out suction filtration obtain third product;
The suction filtration condition: under 25 ℃ of conditions, the vacuum tightness of regulating suction filtration vacuum instrument (SHZ-III type recirculated water vacuum pump) is-0.1MPa to obtain third product behind the suction filtration time 8min;
In the present invention, adopting suction filtration is with the Sn in the 3rd reaction solution 2+, Sn 4+, Pd 2+, Cl -And H +Remove, wherein Sn 4+Be at Sn 2+With Palladous chloride (PdCl 2) chemical reaction takes place obtain.
(G) preparation dispergation treatment solution
The dispergation treatment solution is made up of hydrochloric acid (HCl) and deionized water;
The hydrochloric acid (HCl) that adds 75ml in the deionized water of consumption: 500ml;
(H) separate adhesive process
The 3rd reaction product is added in the dispergation treatment solution;
Dispergation condition:, under the condition of power 500W, behind ultra-sonic dispersion (KQ-500B type ultrasonic cleaner, Kunshan Ultrasonic Instruments Co., Ltd. produces) the reaction 2min, leave standstill 4min and make the 4th reaction solution at 40 ℃ sensitizing temperature;
The 4th reaction solution is carried out suction filtration obtain the 4th product;
The suction filtration condition: under 25 ℃ of conditions, the vacuum tightness of regulating suction filtration vacuum instrument (SHZ-III type recirculated water vacuum pump) is-0.1MPa to obtain the 4th product behind the suction filtration time 8min;
In the present invention, adopting suction filtration is with the Sn in the 4th reaction solution 2+And Cl -And H +Remove, thereby obtain the 4th product.Sn wherein 2+Be attached on the tiny balloon of the 4th product;
The 4th product is put into loft drier, behind dry 3.5h under 100 ℃ the condition, make the 5th product;
The 3rd step: electroless plating is handled
(A) preparation chemical plating fluid
Chemical plating fluid is by single nickel salt (NiSO 46H 2O), rose vitriol (CoSO 47H 2O), ferrous sulfate (FeSO 47H 2O), inferior sodium phosphate (NaH 2PO 2), trisodium citrate (Na 3C 6H 5O 7) and the deionized water composition;
Trisodium citrate (the NaXC that adds 51.5g in the deionized water of consumption: 500ml 6H 5O 7), the single nickel salt (NiSO of 8g 46H 2O), the rose vitriol (CoSO of 8g 47H 2O), the ferrous sulfate (FeSO of 16g 47H 2O) and the inferior sodium phosphate (NaH of 21.5g 2PO 2);
In chemical plating fluid, add ammoniacal liquor (NH 3H 2O) pH=9 of the described chemical plating fluid of adjusting obtains chemical plating fluid;
(B) chemical plating technology
The 5th product that makes is put into chemical plating fluid;
Electroless plating condition:, under the condition of power 500W, behind the reaction 90min, leave standstill 4min and make the 5th reaction solution under the condition of ultra-sonic dispersion (KQ-500B type ultrasonic cleaner, Kunshan Ultrasonic Instruments Co., Ltd. produces) 80 ℃ electroless plating temperature;
The 5th reaction solution is carried out suction filtration obtain the 6th product;
The suction filtration condition: under 25 ℃ of conditions, the vacuum tightness of regulating suction filtration vacuum instrument (SHZ-III type recirculated water vacuum pump) is-0.1MPa to obtain the 6th product behind the suction filtration time 8min;
In the present invention, adopting suction filtration is with the C in the 5th reaction solution 6H 5O 7 3-, H 2PO 3 -, Na +And Ni 2+Remove, thereby obtain the 6th product.
The 6th product is put into loft drier, behind dry 3.5h under 100 ℃ the condition, make the 7th product, promptly on tiny balloon, be coated with metal plating.
Adopt the tiny balloon (KW-10 tiny balloon+metallic nickel+cobalt+iron layer) of the surface clad coating that above-mentioned technology makes, relative permittivity when coating thickness is 150nm is 70, relative magnetic permeability is 2.0, and the density of the tiny balloon of surface clad coating is 3.0g/cm 3The relative permittivity of KW-10 tiny balloon is 4, and relative magnetic permeability is 1.The tiny balloon of the surface clad coating of KW-10 tiny balloon+metallic nickel+cobalt+iron layer is 15dB in the maximum absorbance of 2～18GHz hertzian wave frequency range, is 3GHz greater than the frequency range of 10dB.
Embodiment 3:
Radar wave absorbing paint is prepared burden by following mass percent:
Epoxy silicone resin 35%;
Flow agent is BYK333 0.2%;
Thickening material is RM-8W 0.2%;
The tiny balloon 45% of surface clad coating;
Solvent is the propyl carbinol surplus.
Preparation is that the method for the radar wave absorbing paint of filler is that the tiny balloon of (A) epoxy silicone resin and surface clad coating is put into homogenizer with the tiny balloon, under the 600r/min condition, takes out behind the stirring 30min, makes first mixture; (B) first mixture is ground in the machine at triple-roller mill make second mixture that particle diameter is 40 μ m after grinding 20min; (C) put into homogenizer behind second mixture, flow agent, thickening material and the solvent, under the 600r/min condition, behind the stirring 30min, leave standstill 3min, promptly make radar wave absorbing paint.Adopting radar wave absorbing paint that aforesaid method makes coating thickness 2mm and be 22dB in the maximum absorbance of 2～18GHz hertzian wave frequency range, is 5GHz greater than the frequency range of 10dB.
The tiny balloon of the surface clad coating that this is routine is that KW-10 tiny balloon, the metal cobalt plating+iron layer of particle diameter 1～20 μ m formed, and metal cobalt plating+iron layer is coated on the surface of tiny balloon, and the thickness 50nm of metal-plated nickel dam.
Adopt chemical plating technology at tiny balloon surface clad cobalt plating+iron layer, its preparation process is as follows:
The first step: the choosing of body material
Body material is the KW-10 tiny balloon of particle diameter 1～20 μ m;
Second step: to the pre-treatment of matrix
(A) preparation alkali cleaning treatment solution
The alkali cleaning treatment solution is made up of sodium hydroxide (NaOH) and deionized water;
The sodium hydroxide (NaOH) that adds 20g in the deionized water of consumption: 500ml;
(B) alkali washing process
The tiny balloon that first step is chosen adds in the alkali cleaning treatment solution;
The alkali cleaning condition: 60 ℃ alkali cleaning temperature, under the condition of power 500W, magnetic agitation disperses to make first reaction solution behind (the high-power magnetic stirring apparatus of 88-1, Changzhou Guohua Electric Appliance Co., Ltd. produces) reaction 60min; First reaction solution is repeatedly washed acquisition first product;
The washing condition: under 25 ℃ of conditions, in first reaction solution of 100ml, add the 900ml deionized water and stirring and evenly dilute, behind the sedimentation 60min supernatant liquid is removed, repeats 3 times after acquisition first product;
In the present invention, adopting washing is with the Na in first reaction solution on the basis that does not influence the tiny balloon dispersiveness +, OH -And the impurities in raw materials removal, thereby obtain first product.
(C) preparation coupling processing liquid
Coupling processing liquid is by Y-aminopropyl triethoxysilane (KH550) and ethanol (C 2H 5OH) form;
Ethanol (the C of consumption: 500ml 2H 5OH) KH550 that adds 2g in;
(D) coupling process
First product is added in the coupling processing liquid;
Coupling condition:, under the condition of power 500W, behind ultra-sonic dispersion (KQ-500B type ultrasonic cleaner, Kunshan Ultrasonic Instruments Co., Ltd. produces) the reaction 6h, leave standstill 5min and make second reaction solution 35 ℃ coupling temperature;
Second reaction solution is carried out suction filtration obtain second product;
The suction filtration condition: under 25 ℃ of conditions, the vacuum tightness of regulating suction filtration vacuum instrument (SHZ-III type recirculated water vacuum pump) is-0.1MPa to obtain second product behind the suction filtration time 10min;
In the present invention, adopting suction filtration is to add 50% removal and the adding ethanol (C of the consumption of coupling agent in second reaction solution 2H 5OH) 95% of consumption is removed, thereby obtains second product.
(E) preparation activation treatment liquid
Activation treatment liquid is by tin protochloride (SnCl 22H 2O), sodium stannate (Na 2SnO 3), Palladous chloride (PdCl 2), hydrochloric acid (HCl) and deionized water form;
Add 2g tin protochloride (SnCl in the hydrochloric acid of consumption: 100ml (HCl) 22H 2O) and the Palladous chloride (PdCl of 0.5g 2), add 50g tin protochloride (SnCl behind the reaction 10min 22H 2O), the sodium stannate (Na of 4g 2SnO 3) and the deionized water of 400ml;
(F) activating process
Second product is added in the activation treatment liquid;
Activation condition:, under the condition of power 500W, behind ultra-sonic dispersion (KQ-500B type ultrasonic cleaner, Kunshan Ultrasonic Instruments Co., Ltd. produces) the reaction 30min, leave standstill 5min and make the 3rd reaction solution 50 ℃ activation temperature;
The 3rd reaction solution is carried out suction filtration obtain third product;
The suction filtration condition: under room temperature (25 ℃) condition, the vacuum tightness of regulating suction filtration vacuum instrument (SHZ-III type recirculated water vacuum pump) is-0.1MPa to obtain third product behind the suction filtration time 10min;
In the present invention, adopting suction filtration is with the Sn in the 3rd reaction solution 2+, Sn 4+, Pd 2+, Cl -And H +Remove, wherein Sn 4+Be at Sn 2+With Palladous chloride (PdCl 2) chemical reaction takes place obtain.
(G) preparation dispergation treatment solution
The dispergation treatment solution is made up of hydrochloric acid (HCl) and deionized water;
The hydrochloric acid (HCl) that adds 100ml in the deionized water of consumption: 500ml;
(H) separate adhesive process
The 3rd reaction product is added in the dispergation treatment solution;
Dispergation condition:, under the condition of power 500W, behind ultra-sonic dispersion (KQ-500B type ultrasonic cleaner, Kunshan Ultrasonic Instruments Co., Ltd. produces) the reaction 1min, leave standstill 5min and make the 4th reaction solution 50 ℃ dispergation temperature;
The 4th reaction solution is carried out suction filtration obtain the 4th product;
The suction filtration condition: under 25 ℃ of conditions, the vacuum tightness of regulating suction filtration vacuum instrument (SHZ-III type recirculated water vacuum pump) is-0.1MPa to obtain the 4th product behind the suction filtration time 10min;
In the present invention, adopting suction filtration is with the Sn in the 4th reaction solution 2+And Cl -And H +Remove, thereby obtain the 4th product.Sn wherein 2+Be attached on the tiny balloon of the 4th product;
The 4th product is put into loft drier, behind dry 3h under 110 ℃ the condition, make the 5th product;
The 3rd step: electroless plating is handled
(A) preparation chemical plating fluid
Chemical plating fluid is by rose vitriol (CoSO 47H 2O), ferrous sulfate (FeSO 47H 2O), inferior sodium phosphate (NaH 2PO 2), trisodium citrate (Na 3C 6H 5O 7) and the deionized water composition;
Trisodium citrate (the Na that adds 110g in the deionized water of consumption: 500ml 3C 6H 5O 7), the single nickel salt (CoSO of 20g 47H 2O), 20g ferrous sulfate (FeSO 47H 2O) and the inferior sodium phosphate (NaH of 42.5g 2PO 2);
In chemical plating fluid, add ammoniacal liquor (NH 3H 2O) pH=10 of the described chemical plating fluid of adjusting obtains chemical plating fluid;
(B) chemical plating technology
The 5th product that makes is put into chemical plating fluid;
Electroless plating condition:, under the condition of power 500W, behind the reaction 120min, leave standstill 5min and make the 5th reaction solution under the condition of ultra-sonic dispersion (KQ-500B type ultrasonic cleaner, Kunshan Ultrasonic Instruments Co., Ltd. produces) 90 ℃ electroless plating temperature;
The 5th reaction solution is carried out suction filtration obtain the 5th product;
The suction filtration condition: under 25 ℃ of conditions, the vacuum tightness of regulating suction filtration vacuum instrument (SHZ-III type recirculated water vacuum pump) is-0.1MPa to obtain the 5th product behind the suction filtration time 10min;
In the present invention, adopting suction filtration is with the C in the 5th reaction solution 6H 5O 7 3-, H 2PO 3 -, Na +, Co 2+And Fe 2+Remove, thereby obtain the 5th product.
The 5th product is put into loft drier, behind dry 4h under 110 ℃ the condition, make the 6th product, promptly on tiny balloon, be coated with metal plating.
Adopt the tiny balloon (KW-10 tiny balloon+cobalt metal+iron layer) of the surface clad coating that above-mentioned technology makes, relative permittivity when coating thickness is 50nm is 60, relative magnetic permeability is 1.4, and the density of the tiny balloon of surface clad coating is 2.65g/cm 3The relative permittivity of KW-10 tiny balloon is 4, and relative magnetic permeability is 1.The tiny balloon of the surface clad coating of KW-10 tiny balloon+cobalt metal+iron layer is 10dB in the maximum absorbance of 2～18GHz hertzian wave frequency range, is 3GHz greater than the frequency range of 8dB.
Adopt above-mentioned same process chemical plating metal cobalt+nickel dam on the KW-10 tiny balloon, the relative permittivity when coating thickness is 50nm is 50, and relative magnetic permeability is 1.5, and the density of the tiny balloon of surface clad coating is 2.60g/cm 3The tiny balloon of the surface clad coating of KW-10 tiny balloon+metallic nickel+cobalt layer is 10dB in the maximum absorbance of 2～18GHz hertzian wave frequency range, is 3GHz greater than the frequency range of 8dB.
Adopt above-mentioned same process chemical plating metal iron+nickel dam on the KW-10 tiny balloon, the relative permittivity when coating thickness is 50nm is 70, and relative magnetic permeability is 1.8, and the density of the tiny balloon of surface clad coating is 2.71g/cm 3The tiny balloon of the surface clad coating of KW-10 tiny balloon+metallic nickel+iron layer is 10dB in the maximum absorbance of 2～18GHz hertzian wave frequency range, is 4GHz greater than the frequency range of 8dB.

Claims (4)

1. one kind is the radar wave absorbing paint of filler with the tiny balloon, and it is characterized in that: this radar wave absorbing paint is prepared burden by following mass percent:
Epoxy silicone resin 30～40%;
Flow agent 0.2～0.4%;
Thickening material 0.2～0.4%;
The tiny balloon 40～55% of surface clad coating;
The solvent surplus;
Flow agent is a polyacrylate(s), polyether-modified polysiloxane-based;
Thickening material is sodium polyacrylate, ACRYLIC EMULSION, polyurethanes;
Solvent is dimethylbenzene or propyl carbinol; Or the mixture of dimethylbenzene and propyl carbinol, the mass percent of dimethylbenzene is 60～80 in the mixture, surplus is a propyl carbinol;
Described radar wave absorbing paint is 20dB in the maximum absorbance of 2～18GHz hertzian wave frequency range, is 5GHz greater than the frequency range of 10dB.
One kind to prepare as claimed in claim 1 be the method for the radar wave absorbing paint of filler with the tiny balloon, it is characterized in that the following step is arranged: preparation is that the method for the radar wave absorbing paint of filler is that the tiny balloon of (A) epoxy silicone resin and surface clad coating is put into homogenizer with the tiny balloon, under 600～1000r/min condition, take out after stirring 15～30min, make first mixture; (B) first mixture is ground at triple-roller mill make second mixture that particle diameter is 20～40 μ m after grinding 15～30min in the machine; (C) put into homogenizer behind second mixture, flow agent, thickening material and the solvent, under 600～1000r/min condition, behind stirring 15～30min, leave standstill 3～5min, promptly make radar wave absorbing paint.
3. preparation according to claim 2 is the method for the radar wave absorbing paint of filler with the tiny balloon, it is characterized in that: the tiny balloon of surface clad coating is made up of tiny balloon and metal plating, metal plating is coated on the surface of tiny balloon, and the thickness 50～250nm of metal plating; The composition of described metal plating is nickel, iron or the cobalt of simple substance, or contain the iron of 10～30wt% and the compound Sn-Co coating of 70～90wt%, or contain the iron of 10～30wt% and the nickel composite deposite of 70～90wt%, or contain the nickel of 50～70wt% and the compound Sn-Co coating of 30～50wt%, or contain the iron of 5～20wt%, the cobalt of 20～40wt% and the nickel composite deposite of surplus.
4. preparation according to claim 2 is the method for the radar wave absorbing paint of filler with the tiny balloon, it is characterized in that being prepared as of tiny balloon of described surface clad coating:
The first step: the choosing of body material
Body material is the tiny balloon of particle diameter 1～20 μ m;
Second step: to the pre-treatment of matrix
(A) preparation alkali cleaning treatment solution
The alkali cleaning treatment solution is made up of sodium hydroxide and deionized water;
The sodium hydroxide that adds 10～20g in the deionized water of consumption: 500ml;
(B) alkali washing process
The tiny balloon that first step is chosen adds in the alkali cleaning treatment solution;
The alkali cleaning condition: 60～80 ℃ alkali cleaning temperature, under the condition of power 500W, magnetic agitation disperses to make first reaction solution behind reaction 60～90min;
First reaction solution is washed acquisition first product;
The washing condition: under 25 ℃ of conditions, first reaction solution is diluted with deionized water, behind sedimentation 60～90min supernatant liquid is removed, repeats 2～3 times after acquisition first product;
Adding 800～1000ml deionized water in every 100ml first reaction solution dilutes;
(C) preparation coupling processing liquid
Coupling processing liquid is made up of silane coupling agent and ethanol;
The silane coupling agent that adds 0.5～2g in the ethanol of consumption: 500ml;
(D) coupling process
First product is added in the coupling processing liquid;
Coupling condition:, under the condition of power 500W, behind ultra-sonic dispersion reaction 6～8h, leave standstill 3～5min and make second reaction solution 35～50 ℃ coupling temperature;
Second reaction solution is carried out suction filtration obtain second product;
The suction filtration condition: under 25 ℃ of conditions, the vacuum tightness of regulating suction filtration vacuum instrument is-0.1MPa to obtain second product behind suction filtration time 5～10min;
Adopting suction filtration is that the coupling agent in second reaction solution, ethanol are removed, thereby obtained second product;
(E) preparation activation treatment liquid
Activation treatment liquid is made up of tin protochloride, sodium stannate, Palladous chloride, hydrochloric acid and deionized water;
The Palladous chloride that adds 1～2g tin protochloride and 0.2～0.5g in the hydrochloric acid of consumption: 100ml adds the sodium stannate of 12.5～50g tin protochloride, 2～4g and the deionized water of 400ml behind reaction 10～20min;
(F) activating process
Second product is added in the activation treatment liquid;
Activation condition:, under the condition of power 500W, behind ultra-sonic dispersion reaction 30～60min, leave standstill 3～5min and make the 3rd reaction solution 50～70 ℃ activation temperature;
The 3rd reaction solution is carried out suction filtration obtain third product;
The suction filtration condition: under 25 ℃ of conditions, the vacuum tightness of regulating suction filtration vacuum instrument is-0.1MPa to obtain third product behind suction filtration time 5～10min;
(G) preparation dispergation treatment solution
The dispergation treatment solution is made up of hydrochloric acid and deionized water;
The hydrochloric acid that adds 50～100ml in the deionized water of consumption: 500ml;
(H) separate adhesive process
The 3rd reaction product is added in the dispergation treatment solution;
Dispergation condition:, under the condition of power 500W, behind ultra-sonic dispersion reaction 1～3min, leave standstill 3～5min and make the 4th reaction solution 35～50 ℃ dispergation temperature;
The 4th reaction solution is carried out suction filtration obtain the 4th product;
The suction filtration condition: under 25 ℃ of conditions, the vacuum tightness of regulating suction filtration vacuum instrument is-0.1MPa to obtain the 4th product behind suction filtration time 5～10min;
The 4th product is put into loft drier, behind dry 3～4h under 90～110 ℃ the condition, make the 5th product;
The 3rd step: electroless plating is handled
(A) preparation chemical plating fluid
Chemical plating fluid is made up of metal-salt, inferior sodium phosphate, trisodium citrate and deionized water; Described metal-salt is a kind of in single nickel salt, rose vitriol and the ferrous sulfate or two kinds or three kinds;
Add the trisodium citrate of 20～110g, the metal-salt of 8～40g and the inferior sodium phosphate of 8.5～42.5g in the deionized water of consumption: 500ml;
In chemical plating fluid, add pH=8.5～10 that ammoniacal liquor is regulated described chemical plating fluid, obtain chemical plating fluid;
(B) chemical plating technology
The 5th product that makes is put into chemical plating fluid;
The electroless plating condition: 70～90 ℃ electroless plating temperature, under the condition of power 500W, react 60～120min under the condition of ultra-sonic dispersion after, leave standstill 3～5min and make the 5th reaction solution;
The 5th reaction solution is carried out suction filtration obtain the 6th product;
The suction filtration condition: under 25 ℃ of conditions, the vacuum tightness of regulating suction filtration vacuum instrument is-0.1MPa to obtain the 6th product behind suction filtration time 5～10min;
The 6th product is put into loft drier, behind dry 3～4h under 90～110 ℃ the condition, make the 7th product, i.e. the radar wave absorbing agent of clad metal coating on tiny balloon.
CN2008101145553A 2008-06-04 2008-06-04 Radar wave absorbing paint with hollow microsphere as filling material and preparation method thereof Expired - Fee Related CN101294047B (en)

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