CN105111931A - Strong-laser-ablation-resistant protective coating and preparation method thereof - Google Patents
Strong-laser-ablation-resistant protective coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a strong-laser-ablation-resistant protective coating and a preparation method thereof. The protective coating is prepared from flake graphite, a SiC whisker, an epoxy modified organic silicon resin and a phenolic resin. The preparation method comprises the following steps: dissolving the epoxy modified organic silicon resin and phenolic resin, stirring to obtain a mixed adhesive, and mixing the flake graphite and SiC whisker to obtain mixed powder; (2) mixing the mixed adhesive and mixed powder, and carrying out ball milling to obtain a coating slurry; and (3) coating the coating slurry on a base material, and curing by heating to obtain the strong-laser-ablation-resistant protective coating. The strong-laser-ablation-resistant protective coating has the advantages of low density, high strength, low price, stable performance and the like, and can be sprayed. The preparation method has the advantages of simple technique and low cost.
Description
Technical field
The present invention relates to a kind of protective coating and preparation method thereof, protective coating of particularly a kind of anti-light laser ablation and preparation method thereof.
Background technology
Laser weapon have fast (light velocity), accurately, the unrivaled advantage of other weapon such as Anti-amyloid-β antibody, be about to become one of important strike means of war under modern high technology condition.Along with the fast development of laser weapon particularly high energy laser weapon, it is increasing that space vehicle faces the danger that laser weapon hits.The damage mode of laser weapon to target can be divided into soft destruction and hard destruction two classes.Soft destruction makes the optical thin film of aircraft or photo-sensor produce interference, blinding and destruction, and the laser energy density needed for it is lower, only needs 10 ~ 10
2j/cm
2.Hard destruction by the irradiation of light laser (or superlaser), the structural part temperature of aircraft is raised, and causes the reduction of the tension of structured material, ultimate compression strength and Young's modulus and make aircraft produce inefficacy under the effect of self flight load.Laser energy density needed for hard destruction is higher, is about 10
3~ 10
4j/cm
2.
For light laser firmly killing and wounding space vehicle, be effective anti-light laser damaging pathways at space vehicle outer surface anti-light laser ablative coating.Anti-light laser coating can utilize highly reflective material to the reflection characteristic of light; incident laser major part is reflected or scatters out; reduce the deposition of laser energy on material; thus protecting materials; also the high material of effective ablation heat can be utilized under laser irradiation, to produce heat absorption ablation and consume a large amount of laser deposition heats, available protecting structured material.The granulated filler of resistance to laser radiation is coated in transparent radiation protective film by Slemp etc., film bottom deposit has the metal level of specular reflection function, then film stack is added and make the anti-laser structure of multilayer, this structure can reach effect (Slemp.Particulateandsolarradiationstablecoatingforspacec raft [P] .USPat of high reverse--bias and anti-yaw damper simultaneously, 4,008,348.1977.).The processing method that this patent adopts is complicated, is difficult to be generalized in practical engineering application.United States Navy have developed a kind of organic silicon high-temperature coating-TT2P228 containing aluminium pigment, and this coating has higher reflectivity, can play the effect of anti-laser protection under 650 DEG C of hot conditionss.This coating mainly utilize aluminium pigment to laser reflection be used for realize anti-laser protection, the occasion that laser irradiation intensity is lower can only be used for.A kind of anti-laser structure be made up of Multi-layer graphite of American Studies; every layer of graphite is very thin and smooth and bright like a mirror; to laser, there is very high reflectivity; serve anti-laser hardening effect (Guo Yalin, Liang Guozheng, Qiu Zheming etc. the material damage under laser irradiation and Protective Research progress [J]. material protection; 2003;, but the preparation method of this anti-laser structure does not mention 36 (12): 8-10,13.).Chinese Patent Application No. CN200810244070.6 discloses protective coating of a kind of resisting laser ablation and preparation method thereof, the feature of the method first Polycarbosilane and Vinylstyrene is mixed in proportion, heated and stirred forms transparent mixing solutions, then in mixing solutions, add appropriate chopped carbon fiber and Zirconium oxide powder and the obtained coating with certain viscosity that stirs, this paint is put into baking oven and is heating and curing after process to pretreated aluminium alloy base plate surface and obtains compound coating.Containing Zirconium oxide powder in this compound coating, the density of coating is higher.Yu Qingchun etc. adopt brush coating process to prepare flake graphite enhancing ba phenolic resin based composites, and adopt the resistance to laser ablation performance of Repetition Frequency Laser radiation mode to matrix material to be studied.Flake graphite in this matrix material is layered distribution in subparallel mode, plane reflection effect can be played to incident laser in laser irradiation process, thus reduce the energy deposition of laser irradiation, its resistance to laser ablation performance is apparently higher than carbon fiber reinforced ba phenolic resin based composites (Yu Qingchun, Wan Hong. flake graphite strengthens the resistance to laser ablation performance research [J] of polymer matrix composites, Journal of Inorganic Materials, 2012,27 (2): 157-161).Chen Bo etc. have prepared crystalline flake graphite modified epoxy coating, this coated filler volume fraction 85%, solidification value 80 DEG C, and set time, 2h, adopted vacuum molding mode to strengthen the conjugation of asking and the density of resin and filler in solidification process.(Chen Bo, Wan Hong, Bai Shuxin. the anti-laser irradiation performance [J] of graphite modified epoxy resin. light laser and particle beam 2011,23 (10): 2617-2620).Above-mentioned two kinds of coatings have good resisting laser ablation performance, but the intensity of coating is low, is difficult to the requirement meeting engineer applied.
Summary of the invention
The technical problem to be solved in the present invention overcomes the deficiencies in the prior art, there is provided that a kind of density is low, intensity is high, cheap, stable performance, the protective coating of anti-light laser ablation that can spray, the preparation method of the protective coating of the anti-light laser ablation also providing a kind of technique simple, with low cost.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of protective coating of anti-light laser ablation, described protective coating is by crystalline flake graphite, SiC whisker, epoxide modified silicone resin and resol preparation form (with SiC whisker for coating enhancer, with epoxide modified silicone resin for caking agent and membrane-forming agent, take resol as solidifying agent), wherein, by massfraction, described crystalline flake graphite is 50% ~ 60%, described SiC whisker is 5% ~ 10%, described epoxide modified silicone resin and resol are 35% ~ 45% altogether, and the mass ratio of described epoxide modified silicone resin and resol is 2 ~ 6: 1.
Above-mentioned protective coating, preferably, the diameter of described crystalline flake graphite is 50 microns ~ 100 microns.
As a total technical conceive, the present invention also provides a kind of preparation method of above-mentioned protective coating, comprises the following steps:
(1) crystalline flake graphite, SiC whisker, epoxide modified silicone resin and resol is taken respectively by described massfraction; Epoxide modified silicone resin and resol are joined in thinner and dissolves, and stir, obtain mixing caking agent; By crystalline flake graphite and the mixing of SiC whisker, after wet ball grinding, obtain mixed powder;
(2) mixing caking agent step (1) obtained and mixed powder mix, and after ball milling, obtain applying slurry;
(3) be coated on body material by step (2) gained coating slurry, be heating and curing, the process repeating described coating and be heating and curing, until reach required coat-thickness, body material obtains the protective coating of anti-light laser ablation.
Above-mentioned preparation method, preferably, in described step (3), the described process be heating and curing for: described in the process that is heating and curing be: be first warming up to 110 DEG C ~ 130 DEG C, insulation 1h ~ 2h, is then warming up to 140 DEG C ~ 160 DEG C, insulation 1h ~ 2h, then be warming up to 180 DEG C ~ 200 DEG C, insulation 2h ~ 4h.
Above-mentioned preparation method, preferably, in described step (3), the mode of described coating is spraying.
Above-mentioned preparation method, preferably, in described step (1), the quality of described thinner is 100% ~ 200% of described epoxide modified silicone resin and resol total mass.
Above-mentioned preparation method, preferably, in described step (1), described thinner is the one in the mixed solvent of dimethylbenzene and propyl carbinol, alcohol or acetone.
Above-mentioned preparation method, preferably, in described step (1), the mixing time of described crystalline flake graphite and SiC whisker is 2h ~ 4h, and the time of described wet ball grinding is 4h ~ 8h.
Above-mentioned preparation method, preferably, in described step (2), the time of described ball milling is 4h ~ 6h.
In the protective coating of anti-light laser ablation of the present invention, the epoxy modified silicone resin that epoxide modified silicone resin preferred Jiangsu Osaka, Jiangyin coating factory produces, commodity are called TR613.
Compared with prior art, the invention has the advantages that:
1, the protective coating of anti-light laser ablation of the present invention, take crystalline flake graphite as function of tonic chord phase, and SiC whisker is reinforcement, and epoxide modified silicone resin is matrix resin, and resol is solidifying agent.Wherein flaky graphite has natural laminate structure, have good reflecting properties, low longitudinal thermal conductivity and high transverse thermal conductivity, also there is higher vaporization temperature, the latent heat of vaporization and radiant ratio, there is high resistance to laser ablation performance, and density is low, cheap.But, due to crystalline flake graphite because interfacial bonding strength is very low, the tensile strength of the ablative cork coatings taking crystalline flake graphite as function of tonic chord phase can be caused low, the present invention adopts SiC whisker to improve strength of coating, adopts epoxide modified silicone resin as matrix resin, has both had good manufacturability and temperature tolerance, play again the effect of coating membrane-forming agent and caking agent, adopt resol to serve as resin curing agent, realize high charring rate and higher solidification intensity, improve thermotolerance and the flintiness of coating.
2, preparation method's simple process of the protective coating of anti-light laser ablation of the present invention, with low cost, wherein applies slurry and can directly adopt the method for spraying to be applied to protected substrate material surface, as aluminium alloy, steel and polymer matrix composites surface.
Accompanying drawing explanation
Fig. 1 is the microscopic appearance figure of crystalline flake graphite used in the embodiment of the present invention 1.
Fig. 2 is the microscopic appearance figure of the protective coating of anti-light laser ablation in the embodiment of the present invention 1.
Fig. 3 is the pictorial diagram of the protective coating of anti-light laser ablation in the embodiment of the present invention 1.
Fig. 4 is the ablation shape appearance figure of the protective coating of anti-light laser ablation in the embodiment of the present invention 1.
Fig. 5 is the back side temperature rise curve of the protective coating of anti-light laser ablation in the embodiment of the present invention 1.
Embodiment
Below in conjunction with Figure of description and concrete preferred embodiment, the invention will be further described, but protection domain not thereby limiting the invention.
The material adopted in following examples and instrument are commercially available.
embodiment 1:
A kind of protective coating of anti-light laser ablation of the present invention, this protective coating is prepared by crystalline flake graphite, SiC whisker, epoxide modified silicone resin and resol to form, wherein, by massfraction, crystalline flake graphite is 50%, SiC whisker is 10%, and epoxide modified silicone resin is 32%, resol is 8%, and epoxide modified silicone resin and the mass ratio of resol are 4: 1.
In the present embodiment, the diameter of crystalline flake graphite is 80 microns ~ 100 microns.
In the present embodiment, epoxide modified silicone resin is from epoxide modified silicone resin solution, and the concrete epoxy modified silicone resin solution adopting Osaka, Jiangyin, Jiangsu coating company limited to produce, trade names are TR613, and its solid content is 50%.That is, epoxide modified silicone resin quality contained in epoxide modified silicone resin solution accounts for 32% of above-mentioned four kinds of coating material total masses.
A preparation method for the protective coating of the anti-light laser ablation of above-mentioned the present embodiment, comprises the following steps:
(1) the epoxide modified silicone resin solution (wherein epoxide modified silicone resin mass content is 50%, and solvent quality content is 50%) of 50g crystalline graphite powder, 10gSiC whisker, 64g and 8g resol is taken respectively by above-mentioned massfraction.Epoxide modified silicone resin solution and resol mixed and adds 60g thinner (alcohol), being placed in agitator stir about 1 hour, after stirring, obtaining mixing caking agent.Crystalline graphite powder and SiC whisker are placed in V-type mixer mixing 2 hours, and wet ball grinding is after 4 hours, obtains mixed powder;
(2) mixed powder step (1) obtained and mixing caking agent mix, and are placed in planetary ball mill ball milling 4h, obtain applying slurry;
(3) step (2) gained coating slurry is loaded in conventional hand-held spray guns, and be sprayed on the aluminium alloy plate of polishing and cleaning up, in spraying process, thinner contained in coating volatilizees in atmosphere, be positioned in a conventional oven by the aluminium alloy plate being coated with coating slurry, be heating and curing, the concrete steps be heating and curing are as follows: first by after baking oven for heating to 120 DEG C of insulation 1h, continue to improve oven temperature to 150 DEG C of insulation 1h, and then baking oven is brought up to 180 DEG C of insulation 2h.After baking oven cooling, take out sample, namely obtain completely crued coating sample.Coat-thickness prepared by 1 spraying is about 0.5mm, and repetitive coatings and the process be heating and curing, until reach required coat-thickness, body material obtains the protective coating of anti-light laser ablation.In the present embodiment, adopt and spray curing process six times, obtain the coating sample that thickness is about 3mm.
The microscopic appearance figure of the present embodiment crystalline flake graphite used as shown in Figure 1.
The microscopic appearance of the protective coating of the anti-light laser ablation prepared by the present embodiment as shown in Figure 2, can be observed silicon carbide whisker and is distributed in wherein.
The pictorial diagram of the protective coating of the anti-light laser ablation prepared by the present embodiment as shown in Figure 3.
The ablation shape appearance figure of protective coating after CW Laser 5s of the anti-light laser ablation of Fig. 4 prepared by the present embodiment, laser apparatus used is myriawatt level semiconductor laser apparatus, adopt 10 high power laser diodes to fold battle array as groundwork device, target surface forms square focus spot.Laser apparatus institute Emission Lasers wavelength is 976nm, total light power 10874W of laser apparatus, facula area 2.1cm × 2.5cm.According to calculating, the laser average lamp power density that coating is born is 2071W/cm
2, mean energy density is 10.355kJ/cm
2, but coating only has slight ablation, and do not come off from body material, this illustrates that this layer has good resisting laser ablation performance.
The back side temperature rise curve of protective coating in laser irradiation process of the anti-light laser ablation of Fig. 5 prepared by the present embodiment.Can be observed, in laser irradiation process, the back temperature of protective coating is not higher than 170 DEG C.
embodiment 2:
A kind of protective coating of anti-light laser ablation of the present invention, this protective coating is prepared by crystalline flake graphite, SiC whisker, epoxide modified silicone resin and resol to form, wherein, by massfraction, crystalline flake graphite is 60%, SiC whisker is 5%, and epoxide modified silicone resin is 25%, resol is 10%, and epoxide modified silicone resin and the mass ratio of resol are 2.5: 1.
In the present embodiment, the diameter of crystalline flake graphite is 50 microns ~ 80 microns.
In the present embodiment, epoxide modified silicone resin is from epoxide modified silicone resin solution, and the concrete epoxy modified silicone resin solution adopting Osaka, Jiangyin, Jiangsu coating company limited to produce, trade names are TR613, and its solid content is 50%.That is, epoxide modified silicone resin quality contained in epoxide modified silicone resin solution accounts for 25% of above-mentioned four kinds of coating material total masses.
A preparation method for the protective coating of the anti-light laser ablation of above-mentioned the present embodiment, concrete operation step and processing parameter substantially the same manner as Example 1, difference is:
Step (1) takes 60g crystalline graphite powder, 5gSiC whisker, the resol of the silicone resin solution (the silicone resin mass content of this solution in ethylene modification is 50%, and solvent quality content is 50%) that 50g is epoxide modified and 10g;
The thinner added after step (1) is 70g, and the thinner in the present embodiment is the mixed solvent of dimethylbenzene and propyl carbinol, and wherein the volume ratio of dimethylbenzene and propyl carbinol is 7: 3.
embodiment 3:
A kind of protective coating of anti-light laser ablation of the present invention, this protective coating is prepared by crystalline flake graphite, SiC whisker, epoxide modified silicone resin and resol to form, wherein, by massfraction, crystalline flake graphite is 50%, SiC whisker is 5%, and epoxide modified silicone resin is 38%, resol is 7%, and epoxide modified silicone resin and the mass ratio of resol are about 5.5: 1.
In the present embodiment, the diameter of crystalline flake graphite is 60 microns ~ 90 microns.
In the present embodiment, epoxide modified silicone resin is from epoxide modified silicone resin solution, and the concrete epoxy modified silicone resin solution adopting Osaka, Jiangyin, Jiangsu coating company limited to produce, trade names are TR613, and its solid content is 50%.That is, epoxide modified silicone resin quality contained in epoxide modified silicone resin solution accounts for 38% of above-mentioned four kinds of coating material total masses.
A preparation method for the protective coating of the anti-light laser ablation of above-mentioned the present embodiment, concrete operation step and processing parameter substantially the same manner as Example 1, difference is:
Step (1) takes 50g crystalline graphite powder, 5gSiC whisker, 76g epoxy modified silicone resin solution (the silicone resin mass content of this solution in ethylene modification is 50%, and solvent quality content is 50%), and the resol of 7g.
The thinner added after step (1) is 60g, and the thinner adopted in the present embodiment is acetone.
The above is only the preferred embodiment of the present invention, and protection scope of the present invention is not limited to above-described embodiment.All technical schemes belonged under thinking of the present invention all belong to protection scope of the present invention.It is noted that for those skilled in the art, modification under the premise without departing from the principles of the invention and retouching, also should be considered as protection scope of the present invention.
Claims (9)
1. the protective coating of an anti-light laser ablation, it is characterized in that, described protective coating is prepared by crystalline flake graphite, SiC whisker, epoxide modified silicone resin and resol to form, wherein, by massfraction, described crystalline flake graphite is 50% ~ 60%, and described SiC whisker is 5% ~ 10%, described epoxide modified silicone resin and resol are 35% ~ 45% altogether, and the mass ratio of described epoxide modified silicone resin and resol is 2 ~ 6: 1.
2. the protective coating of anti-light laser ablation according to claim 1, is characterized in that, the diameter of described crystalline flake graphite is 50 microns ~ 100 microns.
3. a preparation method for the protective coating of anti-light laser ablation as claimed in claim 1 or 2, comprises the following steps:
(1) crystalline flake graphite, SiC whisker, epoxide modified silicone resin and resol is taken respectively by described massfraction; Epoxide modified silicone resin and resol are joined in thinner and dissolves, and stir, obtain mixing caking agent; By crystalline flake graphite and the mixing of SiC whisker, after wet ball grinding, obtain mixed powder;
(2) mixing caking agent step (1) obtained and mixed powder mix, and after ball milling, obtain applying slurry;
(3) be coated on body material by step (2) gained coating slurry, be heating and curing, the process repeating described coating and be heating and curing, until reach required coat-thickness, body material obtains the protective coating of anti-light laser ablation.
4. preparation method according to claim 3, is characterized in that, in described step (3), the described process be heating and curing is: be first warming up to 110 DEG C ~ 130 DEG C, and insulation 1h ~ 2h, is then warming up to 140 DEG C ~ 160 DEG C, insulation 1h ~ 2h, then be warming up to 180 DEG C ~ 200 DEG C, insulation 2h ~ 4h.
5. preparation method according to claim 3, is characterized in that, in described step (3), the mode of described coating is spraying.
6. the preparation method according to any one of claim 3 ~ 5, is characterized in that, in described step (1), the quality of described thinner is 100% ~ 200% of described epoxide modified silicone resin and resol total mass.
7. the preparation method according to any one of claim 3 ~ 5, is characterized in that, in described step (1), described thinner is the one in the mixed solvent of dimethylbenzene and propyl carbinol, alcohol or acetone.
8. the preparation method according to any one of claim 3 ~ 5, is characterized in that, in described step (1), the mixing time of described crystalline flake graphite and SiC whisker is 2h ~ 4h, and the time of described wet ball grinding is 4h ~ 8h.
9. the preparation method according to any one of claim 3 ~ 5, is characterized in that, in described step (2), the time of described ball milling is 4h ~ 6h.
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| CN107083183A (en) * | 2017-05-24 | 2017-08-22 | 中南大学 | A kind of boron bakelite resin/epoxy modified silicone resin self-lubricating coat in use of resistance to ablation and preparation method thereof |
| CN107177307A (en) * | 2017-05-24 | 2017-09-19 | 中南大学 | A kind of acetylene benzeneazo xenol urea formaldehyde/epoxy modified silicone resin coating of resistance to ablation protection and preparation method thereof |
| CN107201171A (en) * | 2017-05-24 | 2017-09-26 | 中南大学 | A kind of boron bakelite resin/epoxy modified silicone resin coating of resistance to ablation protection and preparation method thereof |
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| CN107083183A (en) * | 2017-05-24 | 2017-08-22 | 中南大学 | A kind of boron bakelite resin/epoxy modified silicone resin self-lubricating coat in use of resistance to ablation and preparation method thereof |
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| CN107201171A (en) * | 2017-05-24 | 2017-09-26 | 中南大学 | A kind of boron bakelite resin/epoxy modified silicone resin coating of resistance to ablation protection and preparation method thereof |
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| CN107083183B (en) * | 2017-05-24 | 2019-09-03 | 中南大学 | A kind of boron bakelite resin/epoxy modified silicone resin self-lubricating coat in use of resistance to ablation and preparation method thereof |
| CN111500146A (en) * | 2020-03-11 | 2020-08-07 | 中国船舶重工集团公司第七二五研究所 | Composite laser ablation resistant coating, preparation method and use method thereof |
| CN111500146B (en) * | 2020-03-11 | 2021-11-30 | 中国船舶重工集团公司第七二五研究所 | Composite laser ablation resistant coating, preparation method and use method thereof |
| CN113549862A (en) * | 2020-04-08 | 2021-10-26 | 北京理工大学 | High-energy laser protection multilayer composite material coating structure and manufacturing method thereof |
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