CN105176384A - Carbon coated nickel nanoparticle and silicon resin composite microwave absorbing coating and preparation method thereof - Google Patents
Carbon coated nickel nanoparticle and silicon resin composite microwave absorbing coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a carbon coated nickel nanoparticle and silicon resin composite microwave absorbing coating and a preparation method thereof. The composite microwave absorbing coating is composed of 40%-60% by weight of carbon coated nickel nanoparticles and silicon resin. The preparation method comprises the steps that the carbon coated nickel nanoparticles are prepared through an arc discharge method; the carbon coated nickel nanoparticles are filled into the silicon resin to be evenly mixed, and coating slurry is obtained; an adequate amount of xylene is taken to serve as solvent to be added into the slurry, and the viscosity of the slurry is adjusted; a curing agent is added into the slurry, even stirring is conducted, and the coating with certain thickness is prepared. The composite microwave absorbing coating prepared through the method has the advantages of being wide in wave-absorbing band, good in wave-absorbing efficiency, low in reflectivity, high in stability, good in mechanical property and the like, the technology is simple, and the coating is easy to repair.
Description
Technical field
The invention belongs to absorbing material technical field, be specifically related to a kind of carbon nickel coat nano particle/silicone resin composite wave-absorbing coating and preparation method thereof.
Background technology
Since entering 21 century, the widespread use of electronics and development, giving while people's life brings convenience, its electromagnetism good fortune produced is penetrated and is also created very large impact to human health and the environment of depending on for existence.Electromagnetic wave absorbent material not only uses extensively on civilian, and militarily also becomes more and more important, improves military weapon system survivability and defence capability, and stealthy technique becomes the high-new military technique of countries in the world focus development research undoubtedly.Nano composite material microwave absorbing coating by the mode electromagnetic wave absorption of dielectric loss and magnetic loss, can have the advantages such as abundant raw materials, density is little, Technology is relatively simple, can big area suitability for industrialized production.Through time more than ten years, the research of carbon nano-composite material electromagnetic wave absorbing coating is at matrix, and filler, the aspects such as preparation method have made great progress, and also have very large development space in Absorber Bandwidth, absorption intensity, dispersiveness etc. simultaneously.
Traditional absorbing material using ferrite as filler often can not take into account the advantage that strong electromagnetic wave absorbs and broadband absorbs.Dielectric materials and magnetic nanoparticle are combined, can reach and open up wide band object, make electromagnetic parameter convergence optimum matching, reduce reflection, increase and absorb.As patent 200910011350.7 discloses a kind of preparation method of carbon-wrapped iron-cobalt nano wave-absorbing material, carbon shell makes outer shell to have utilized plasma arc legal system standby, and ferrocobalt is as the Nano capsule of kernel, and its absorbing property is better than most ferrites.Patent 201310261578.8 discloses a kind of method using porousness nickel acid lanthanum powder preparation dielectric/ferromagnetic absorption microwave composite material.
Carbon nickel coat nano particle had both had the magnetic loss ability of nickel metal, had again the dielectric loss ability of carbon-coating, can set up good impedance matching, thus showed excellent absorption of electromagnetic wave ability.The nano-carbon layer energy available protecting metallic nickel kernel of carbon nickel coat nano particle is not oxidized, ensure that the stability of microwave absorbing coating, plays again the effect stoping particle agglomeration simultaneously.Silicone resin, as the body material of compound coating, has the advantages such as good chemical stability, thermostability and workability.But, still not prepared by the two compound the bibliographical information of microwave absorbing coating at present.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of carbon nickel coat nano particle/silicone resin composite wave-absorbing coating, this composite wave-absorbing coating has inhales the feature such as ripple bandwidth, wave-absorbing effect is good, reflectivity is low, stability is high, good mechanical property.
Another object of the present invention is to the preparation method that above-mentioned carbon nickel coat nano particle/silicone resin composite wave-absorbing coating is provided.
The present invention is achieved through the following technical solutions:
A kind of carbon nickel coat nano particle/silicone resin composite wave-absorbing coating, described carbon nickel coat nano particle/silicone resin composite wave-absorbing coating is made up of carbon nickel coat nano particle and silicone resin, wherein, the weight percentage of described carbon nickel coat nano particle in composite wave-absorbing coating is 40-60wt%.
Preferably, described carbon nickel coat nano particle has nucleocapsid structure, and nickel core is wrapped up by carbon shell, and carbon nickel coat nano particle is near-spherical, and diameter is 20-35nm.
Preferably, in described carbon nickel coat nano particle, carbon shell is made up of the orderly carbon-coating of 5-7 layer, and the interlamellar spacing of carbon-coating is 0.34nm, consistent with the spacing of graphite (002) crystal face, and carbon thickness of the shell is 1.70-2.38nm.
Preferably, the thickness of described carbon nickel coat nano particle/silicone resin composite wave-absorbing coating is 1.5-3mm.
The preparation method of carbon nickel coat nano particle of the present invention/silicone resin composite wave-absorbing coating, comprises the steps:
(1) with powdered graphite and reduced nickel powder for raw material, adopt arc discharge method to prepare carbon nickel coat nano particle;
(2) take silicone resin as matrix, carbon nickel coat nano particle is inserted in silicone resin, mixes, obtain coating paste;
(3) adopt dimethylbenzene to join in coating paste as solvent, regulate slurry viscosity, stir;
(4) in the slurry of step (3), add solidifying agent, stir, be prepared into and there is certain thickness coating.
Preferably, in step (1), the weight ratio of powdered graphite and reduced nickel powder is 2-4:1-3, reaction chamber internal gas pressure is 10-60kPa, volts DS is 20-60V, galvanic current is 100-150A, more preferably the weight ratio of powdered graphite and reduced nickel powder is 4:1, reaction chamber internal gas pressure is 50kPa, operating voltage is 22V, galvanic current is 150A, and the present invention, by controlling these parameters, can improve the output of excellent high quality carbon nickel coat nano particle, effective control granular size, and orderly carbon-coating can be formed outward at nickel core.
Described arc discharge method prepares the preparation of carbon nickel coat nano particle, specifically can adopt following steps:
Arc plasma is used to prepare nano material system, negative electrode is done with graphite rod, powdered graphite (micron order) and reduced nickel powder (micron order) are mixed by weight the ratio for 4:1, be 25mm, be highly the cylinder shape anode of 30mm by being pressed into diameter in metallic phase sample inlaying machine, at a distance of 3-5mm between two electrodes; Reaction chamber is evacuated to 2-3Pa, passes into high-purity argon gas, make chamber internal gas pressure reach 50kPa, control volts DS is 22V, and galvanic current is 150A, makes two interpolars produce stable arc; Anode material is consumed and changes into the internal surface of soot deposits at reaction cavity in electric arc radiative process; After reaction terminates, collect the cigarette ash generated, remove non-magnetic constituents by the method for Magneto separate, then by dilute hydrochloric acid and deionized water wash, after drying, just can obtain the carbon nickel coat nano particle of purifying.
Preferably, in step (2), the mode of described mixing is first after manual preliminary mixing, then adopts three-roll grinder essence mixed.
Preferably, in step (3), the viscosity of the consumption control coating paste of described dimethylbenzene is 800-1000cP, is preferably 900cP.
Preferably, in step (4), described solidifying agent is dibutyl tin dilaurate or ethylenediamine tetraacetic acid (EDTA), and the consumption of solidifying agent is the 2-3wt% of silicone resin consumption.
The present invention compared with prior art, has following beneficial effect:
(1) the present invention is using carbon nickel coat nano particle as filler, makes electromagnetic wave absorbing coating not easily oxidized, ensures the stable of coating absorbing property, combines magnetic loss and dielectric loss two kinds of modes, improve the absorption of electromagnetic wave ability of coating; Using silicone resin as body material, improve the chemical stability of coating, thermostability and mechanical property; The composite wave-absorbing coating of preparation has inhales the advantage such as ripple bandwidth, good absorbing effect, reflectivity is little, stability is high, good mechanical property: reflectivity is less than the widest 8.45GHz that reaches of bandwidth of-5dB, be less than the widest 3.64GHz that reaches of bandwidth of-10dB, the most I of reflectivity reaches-20.54dB;
(2) advantages such as preparation technology of the present invention adopts coating method, and it is simple that opposed configuration type microwave absorbing coating has technique, easy reparation;
(3) the present invention is by adopting manual just mixed, three-roll grinder smart mixed, ensure that filler is dispersed in the base; By controlling the viscosity of slurry, coating protection can be made to maintain an equal level whole, avoid because repeatedly coating causes coating oxygen blast cyanidation, the composite wave-absorbing coatingsurface of preparation is level and smooth, has certain snappiness.
Accompanying drawing explanation
The TEM that in Fig. 1, (a) is carbon nickel coat nano particle schemes, and the high resolution TEM that (b) is carbon nickel coat nano particle schemes.
Fig. 2 is the XRD figure of carbon nickel coat nano particle.
Fig. 3 is the carbon nickel coat nano particle loading level of the embodiment of the present invention 1 is 40wt%, and coat-thickness is respectively 1.5mm, the reflection of electromagnetic wave rate curve figure of the composite wave-absorbing coating of 2mm, 2.5mm, 3mm.
Fig. 4 is the carbon nickel coat nano particle loading level of the embodiment of the present invention 2 is 50wt%, and coat-thickness is respectively 1.5mm, the reflection of electromagnetic wave rate curve figure of the composite wave-absorbing coating of 2mm, 2.5mm, 3mm.
Fig. 5 is the carbon nickel coat nano particle loading level of the embodiment of the present invention 3 is 60wt%, and coat-thickness is respectively 1.5mm, the reflection of electromagnetic wave rate curve figure of the composite wave-absorbing coating of 2mm, 2.5mm, 3mm.
Embodiment
Further illustrate the present invention below by embodiment, following examples are the concrete embodiment of the present invention, but embodiments of the present invention are by the restriction of following embodiment.
The material used in embodiment is as follows:
Silicone resin: rise and annotate electronic material (Shenzhen) company limited, model is SC-8-268.
Solidifying agent: commercial, model is CA250, CA126.
embodiment 1:
A preparation method for carbon nickel coat nano particle/silicone resin composite wave-absorbing coating, comprises the steps:
(1) preparation of carbon nickel coat nano particle:
Arc plasma is used to prepare nano material system, negative electrode is done with graphite rod, powdered graphite (micron order) and reduced nickel powder (micron order) are mixed by weight the ratio for 4:1, be 25mm, be highly the cylinder shape anode of 30mm by being pressed into diameter in metallic phase sample inlaying machine, at a distance of 3-5mm between two electrodes; Reaction chamber is evacuated to 2-3Pa, passes into high-purity argon gas, make chamber internal gas pressure reach 50kPa, control volts DS is 22V, and galvanic current is 150A, makes two interpolars produce stable arc; Anode material is consumed and changes into the internal surface of soot deposits at reaction cavity in electric arc radiative process; After reaction terminates, collect the cigarette ash generated, remove non-magnetic constituents by the method for Magneto separate, then by dilute hydrochloric acid and deionized water wash, after drying, just can obtain the carbon nickel coat nano particle of purifying.Fig. 1 is the TEM figure of carbon nickel coat nano particle, and as can be seen from Fig. 1 (a), all nano particles all have obvious nucleocapsid structure, and nickel core is wrapped by very thin carbon shell, and carbon nickel coat nano particle is near-spherical, and diameter is 20-35nm, distribute comparatively even; And Fig. 1 (b) can find out more significantly, the carbon shell of nickel core outside is orderly carbon-coating, and carbon shell is made up of the orderly carbon-coating of 5-7 layer, and thickness is approximately 2.2nm, and the interlamellar spacing of carbon-coating is consistent with the spacing (about 0.34nm) of graphite (002) crystal face.Fig. 2 is the XRD figure spectrum of carbon nickel coat nano particle, as can be observed from Figure, in 2 θ=44.51 °, 51.85 °, and the diffraction peak that 76.37 ° of place's appearance three are sharp-pointed, respectively (111), (200), (220) crystal face of corresponding nickel, which illustrate nickel crystalline nucleation degree high, the diffracted signal of nickel oxide do not detected, show that carbon shell can available protecting nickel kernel, prevent oxidized;
(2) the carbon nickel coat nano particle of 180g is mixed with the silicone resin of 120g, after manual preliminary mixing, place it in three-roll grinder and repeatedly roll 4 times, filler and matrix are fully mixed, obtains coating paste;
(3) get appropriate dimethylbenzene to add in above-mentioned slurry as solvent, and the consumption of dimethylbenzene controls the viscosity of slurry within the scope of 900cP, stirs 30 minutes, makes it mix;
(4) then add the solidifying agent dibutyl tin dilaurate of 2.4g respectively, then stir 5 minutes, slurry is poured in automatic spray dryer and be prepared into the coating that thickness is respectively 1.5mm, 2mm, 2.5mm, 3mm.
Prepared carbon nickel coat nano particle loading level is the reflection of electromagnetic wave rate curve of composite wave-absorbing coating in 2-18GHz frequency range of 60wt%, as shown in Figure 5.When thickness is 2.5mm, frequency reaches-20.54dB at 9.08GHz place reflectivity; When thickness is 2mm, the bandwidth that reflectivity is less than-5dB reaches 8.45GHz; When thickness is 1.5mm, the bandwidth that reflectivity is less than-10dB reaches 3.64GHz.
embodiment 2:
A preparation method for carbon nickel coat nano particle/silicone resin composite wave-absorbing coating, comprises the steps:
(1) preparation of carbon nickel coat nano particle:
Arc plasma is used to prepare nano material system, negative electrode is done with graphite rod, powdered graphite (micron order) and reduced nickel powder (micron order) are mixed by weight the ratio for 2:3, be 25mm, be highly the cylinder shape anode of 30mm by being pressed into diameter in metallic phase sample inlaying machine, at a distance of 3-5mm between two electrodes; Reaction chamber is evacuated to 2-3Pa, passes into high-purity argon gas, make chamber internal gas pressure reach 45kPa, control volts DS is 30V, and galvanic current is 130A, makes two interpolars produce stable arc; Anode material is consumed and changes into the internal surface of soot deposits at reaction cavity in electric arc radiative process; After reaction terminates, collect the cigarette ash generated, remove non-magnetic constituents by the method for Magneto separate, then by dilute hydrochloric acid and deionized water wash, after drying, just can obtain the carbon nickel coat nano particle of purifying.
(2) the carbon nickel coat nano particle of 150g is mixed with the silicone resin of 150g, after manual preliminary mixing, place it in three-roll grinder and repeatedly roll 3 times, filler and matrix are fully mixed, obtains coating paste;
(3) get appropriate dimethylbenzene to add in above-mentioned slurry as solvent, and the viscosity that the consumption of dimethylbenzene controls slurry is 800cP, stirs 25 minutes, makes it mix;
(4) then add the curing agent ethylene diamine tetraacethyl of 4.5g respectively, then stir 5 minutes, slurry is poured in automatic spray dryer and be prepared into the coating that thickness is respectively 1.5mm, 2mm, 2.5mm, 3mm.
Prepared carbon nickel coat nano particle loading level is the reflection of electromagnetic wave rate curve of composite wave-absorbing coating in 2-18GHz frequency range of 50wt%, as shown in Figure 4.When thickness is 3mm, frequency reaches-13.80dB at 8.89GHz place reflectivity, and the bandwidth that reflectivity is less than-10dB reaches 1.94GHz; When thickness is 2mm, the bandwidth that reflectivity is less than-5dB reaches 6.1GHz.
embodiment 3:
A preparation method for carbon nickel coat nano particle/silicone resin composite wave-absorbing coating, comprises the steps:
(1) preparation of carbon nickel coat nano particle:
Arc plasma is used to prepare nano material system, negative electrode is done with graphite rod, powdered graphite (micron order) and reduced nickel powder (micron order) are mixed by weight the ratio for 3:2, be 25mm, be highly the cylinder shape anode of 30mm by being pressed into diameter in metallic phase sample inlaying machine, at a distance of 3-5mm between two electrodes; Reaction chamber is evacuated to 2-3Pa, passes into high-purity argon gas, make chamber internal gas pressure reach 30kPa, control volts DS is 20V, and galvanic current is 120A, makes two interpolars produce stable arc; Anode material is consumed and changes into the internal surface of soot deposits at reaction cavity in electric arc radiative process; After reaction terminates, collect the cigarette ash generated, remove non-magnetic constituents by the method for Magneto separate, then by dilute hydrochloric acid and deionized water wash, after drying, just can obtain the carbon nickel coat nano particle of purifying.
(2) the carbon nickel coat nano particle of 120g is mixed with the silicone resin of 180g, after manual preliminary mixing, place it in three-roll grinder and repeatedly roll 4 times, filler and matrix are fully mixed, obtains coating paste;
(3) get appropriate dimethylbenzene to add in above-mentioned slurry as solvent, and the viscosity that the consumption of dimethylbenzene controls slurry is 1000cP, stirs 20 minutes, makes it mix;
(4) in slurry, then add the solidifying agent dibutyl tin dilaurate of 4.5g, then stir 5 minutes, slurry is poured in automatic spray dryer and be prepared into the coating that thickness is respectively 1.5mm, 2mm, 2.5mm, 3mm.
Prepared carbon nickel coat nano particle loading level is the reflection of electromagnetic wave rate curve of composite wave-absorbing coating in 2-18GHz frequency range of 40wt%, as shown in Figure 3.When thickness is 3mm, frequency reaches-10.06dB at 10.24GHz place reflectivity; When thickness is 2.5mm, the bandwidth that reflectivity is less than-5dB reaches 5.32GHz.
Prepared by embodiment 1,2,3, the absorption of electromagnetic wave performance related data of carbon nickel coat nano particle/silicone resin composite wave-absorbing coating is out as shown in table 1 below:
The absorption of electromagnetic wave performance related data synopsis of table 1 carbon nickel coat nano particle/silicone resin composite wave-absorbing coating
As can be seen from the above results, carbon nickel coat nano particle prepared by the present invention/silicone resin composite wave-absorbing coating reflectivity is less than the widest 8.45GHz that reaches of bandwidth of-5dB, is less than the widest 3.64GHz that reaches of bandwidth of-10dB, and the most I of reflectivity reaches-20.54dB.
Claims (10)
1. carbon nickel coat nano particle/silicone resin composite wave-absorbing coating, it is characterized in that, described carbon nickel coat nano particle/silicone resin composite wave-absorbing coating is made up of carbon nickel coat nano particle and silicone resin, wherein, the weight percentage of described carbon nickel coat nano particle in composite wave-absorbing coating is 40-60wt%.
2. carbon nickel coat nano particle according to claim 1/silicone resin composite wave-absorbing coating, is characterized in that, described carbon nickel coat nano particle has nucleocapsid structure, and nickel core is wrapped up by carbon shell, and carbon nickel coat nano particle is near-spherical, and diameter is 20-35nm.
3. carbon nickel coat nano particle according to claim 2/silicone resin composite wave-absorbing coating, it is characterized in that, in described carbon nickel coat nano particle, carbon shell is made up of the orderly carbon-coating of 5-7 layer, the interlamellar spacing of carbon-coating is 0.34nm, consistent with the spacing of graphite 002 crystal face, carbon thickness of the shell is 1.70-2.38nm.
4. carbon nickel coat nano particle according to claim 1/silicone resin composite wave-absorbing coating, is characterized in that, the thickness of described carbon nickel coat nano particle/silicone resin composite wave-absorbing coating is 1.5-3mm.
5. the preparation method of the carbon nickel coat nano particle according to any one of claim 1-4/silicone resin composite wave-absorbing coating, is characterized in that, comprise the steps:
(1) with powdered graphite and reduced nickel powder for raw material, adopt arc discharge method to prepare carbon nickel coat nano particle;
(2) take silicone resin as matrix, carbon nickel coat nano particle is inserted in silicone resin, mixes, obtain coating paste;
(3) adopt dimethylbenzene to join in coating paste as solvent, regulate slurry viscosity, stir;
(4) in the slurry of step (3), add solidifying agent, stir, be prepared into and there is certain thickness coating.
6. the preparation method of carbon nickel coat nano particle according to claim 5/silicone resin composite wave-absorbing coating, it is characterized in that, in step (1), the weight ratio of powdered graphite and reduced nickel powder is 2-4:1-3, reaction chamber internal gas pressure is 10-60kPa, volts DS is 20-60V, and galvanic current is 100-150A.
7. the preparation method of carbon nickel coat nano particle according to claim 6/silicone resin composite wave-absorbing coating, is characterized in that, in step (1), the weight ratio of powdered graphite and reduced nickel powder is 4:1, reaction chamber internal gas pressure is 50kPa, and operating voltage is 22V, and galvanic current is 150A.
8. the preparation method of carbon nickel coat nano particle according to claim 5/silicone resin composite wave-absorbing coating, is characterized in that, in step (2), the mode of described mixing is first after manual preliminary mixing, then adopts three-roll grinder essence mixed.
9. the preparation method of carbon nickel coat nano particle according to claim 5/silicone resin composite wave-absorbing coating, is characterized in that, in step (3), the viscosity of the consumption control coating paste of described dimethylbenzene is 800-1000cP, is preferably 900cP.
10. the preparation method of carbon nickel coat nano particle according to claim 5/silicone resin composite wave-absorbing coating, it is characterized in that, in step (4), described solidifying agent is dibutyl tin dilaurate or ethylenediamine tetraacetic acid (EDTA), and the consumption of solidifying agent is the 2-3wt% of silicone resin consumption.
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| CN106001551A (en) * | 2016-05-31 | 2016-10-12 | 安徽工业大学 | Ni@C@g-C3N4 nanocomposite and preparation method and application thereof |
| CN107459927A (en) * | 2017-09-25 | 2017-12-12 | 广东工业大学 | One kind inhales ripple slurry, absorbing material and preparation method thereof |
| CN115787291A (en) * | 2022-12-28 | 2023-03-14 | 艾利特控股集团有限公司 | Electromagnetic wave absorption finishing liquid and application thereof in preparation of electromagnetic radiation protection textile fabric |
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