CN105111931B - Protective coating of anti-light laser ablation and preparation method thereof - Google Patents
Protective coating of anti-light laser ablation and preparation method thereof Download PDFInfo
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- CN105111931B CN105111931B CN201510547116.1A CN201510547116A CN105111931B CN 105111931 B CN105111931 B CN 105111931B CN 201510547116 A CN201510547116 A CN 201510547116A CN 105111931 B CN105111931 B CN 105111931B
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Abstract
The invention discloses a kind of protective coating of anti-light laser ablation and preparation method thereof.The protective coating is to be prepared to form by crystalline flake graphite, SiC whiskers, epoxide modified organic siliconresin and phenolic resin.Preparation method includes（1）Bonding agent must be mixed by being stirred after epoxide modified organic siliconresin and phenolic resin dissolving, mixed powder is obtained after crystalline flake graphite and SiC whiskers are mixed；（2）Ball milling obtains coating slurry after mixing bonding agent and mixed powder are mixed；（3）It is heating and curing after coating slurry is coated on matrix material, obtains the protective coating of anti-light laser ablation.The protective coating of the anti-light laser ablation of the present invention has the advantages that density is low, intensity is high, cheap, performance is stable, sprayable, and preparation method technique is easy, with low cost.
Description
Technical field
The present invention relates to a kind of protective coating and preparation method thereof, more particularly to a kind of protective coating of anti-light laser ablation
And preparation method thereof.
Background technology
Laser weapon has quick（The light velocity）, the unrivaled advantage of other weapons, Ji Jiangcheng such as accurate, Anti-amyloid-β antibody
One of important strike means for war under the conditions of modern high technology.It is quick with laser weapon particularly high energy laser weapon
Development, spacecraft faces the dangerous increasing of laser weapon strike.Laser weapon can be divided into the damage mode of target
Two classes of soft destruction and hard destruction.Soft destruction is that the optical thin film or photoelectric sensor for making aircraft produce interference, blinding and destruction,
Laser energy density needed for it is relatively low, it is only necessary to 10~102 J/cm2.Hard destruction is by light laser（Or superlaser）Spoke
According to the structural member temperature of aircraft is raised, cause the reduction of the tension, compression strength and modulus of elasticity of structural material and make to fly
Row device produces failure in the presence of itself flight load.Laser energy density needed for hard destruction is higher, and about 103~104
J/cm2。
Hard killing for light laser to spacecraft, anti-light laser ablative coating is coated in spacecraft outer surface
It is effective anti-light laser damaging pathways.Anti- light laser coating be able to will enter using highly reflective material to the reflection characteristic of light
Penetrate laser largely to reflect or scatter out, deposition of the laser energy on material is reduced, so that protection materials, can also be used
The high material of the effect heat of ablation produces heat absorption ablation under laser irradiation and consumes substantial amounts of laser deposition heat, effective protection structure
Material.The granulated filler of resistance to laser emission is coated in transparent radiation protective film by Slemp etc., on film bottom deposit
There is the metal level of mirror-reflection function, film stack is then added into the anti-laser structure of multilayer, the structure can reach high anti-simultaneously
Penetrate the effect with anti-yaw damper（Slemp. Particulate and solar radiation stable coating for
spacecraft[P]. US Pat, 4, 008, 348. 1977.）.The process that the patent is used is complicated, it is difficult to promote
Into practical engineering application.USN have developed a kind of organic silicon high-temperature coating-TT2P228 containing aluminium pigment, the coating
With higher reflectivity, anti-laser protection can be played a part of under 650 DEG C of hot conditions.The coating mainly utilizes aluminium pigment
Anti-laser protection is realized to the effect of laser reflection, the relatively low occasion of laser irradiation intensity is only used for.American Studies one
The anti-laser structure being made up of Multi-layer graphite is planted, the very thin and smooth such as mirror of every layer of graphite has very high reflectivity to laser, risen
The effect of anti-laser hardening is arrived（Material damage and Protective Research under the irradiation of the such as Guo Yalin, Liang Guozheng, Qiu Zheming laser
Be in progress [J] material protections, 2003,36 (12): 8-10, 13.）, but the preparation method of the anti-laser structure do not refer to.
Chinese Patent Application No. CN200810244070.6 discloses a kind of protective coating of resisting laser ablation and preparation method thereof, the party
The characteristics of method is first to mix Polycarbosilane in proportion with divinylbenzene, and heating stirring forms transparent mixed solution, then
Appropriate chopped carbon fiber and Zirconium oxide powder and the coating for being made and there is certain viscosity that stirs is added in mixed solution,
The coating is coated to pretreated aluminium alloy base plate surface and is put into baking oven to be heating and curing after processing and obtains composite coating.
Contain Zirconium oxide powder in the composite coating, the density of coating is higher.Yu Qingchun etc. is prepared for flake graphite using brush coating process
Strengthen ba phenolic resin based composites, and the resistance to laser ablation performance of composite is carried out using Repetition Frequency Laser radiation mode
Research.Flake graphite in the composite is in layered distribution in subparallel mode, can be to entering in laser irradiation process
Penetrate laser and play plane reflection effect, so as to reduce the energy deposition of laser irradiation, its resistance to laser ablation performance is apparently higher than carbon
Fibre-reinforced ba phenolic resin based composites（Yu Qingchun, the resistance to of ten thousand red flake graphites reinforced resin based composites swashs
Light ablation property research [J], Journal of Inorganic Materials, 2012,27 (2): 157-161）.Chen Bo etc. is prepared for crystalline flake graphite modification
Using true in epoxy coating, the coated filler volume fraction 85%, 80 DEG C of solidification temperature, the h of hardening time 2, solidification process
The conjugation asked and consistency of empty press moulding mode reinforced resin and filler.（The graphite modified epoxies of Chen Bo, Wan Hong, Bai Shuxin
Anti- laser irradiation behaviour [J] the light lasers of resin and the particle beams 2011,23 (10)：2617-2620）.Above two coating has
There are good resisting laser ablation performance, but the low intensity of coating, it is difficult to meet the requirement of engineer applied.
The content of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art there is provided a kind of density is low, intensity is high, price
The protective coating of stable, the sprayable anti-light laser ablation of cheap, performance, also provides a kind of technique simple, with low cost anti-
The preparation method of the protective coating of light laser ablation.
In order to solve the above technical problems, the present invention is adopted the following technical scheme that：
A kind of protective coating of anti-light laser ablation, the protective coating is by crystalline flake graphite, SiC whiskers, epoxide modified
Organic siliconresin and phenolic resin prepare form（Using SiC whiskers as coating enhancer, using epoxide modified organic siliconresin as
Bonding agent and film forming agent, using phenolic resin as curing agent）, wherein, as mass fraction, the crystalline flake graphite is 50%~60%,
The SiC whiskers are 5%~10%, and the epoxide modified organic siliconresin and phenolic resin are 35%~45% altogether, and the ring
The organic siliconresin and the mass ratio of phenolic resin that oxygen is modified are 2~6: 1.
Above-mentioned protective coating, it is preferred that a diameter of 50 microns~100 microns of the crystalline flake graphite.
As a total technical concept, the present invention also provides a kind of preparation method of above-mentioned protective coating, including following
Step：
（1）Crystalline flake graphite, SiC whiskers, epoxide modified organic siliconresin and phenolic aldehyde are weighed respectively by the mass fraction
Resin；Epoxide modified organic siliconresin and phenolic resin are added in diluent and dissolved, and is stirred, mixing is obtained viscous
Connect agent；Crystalline flake graphite and SiC whiskers are mixed, after wet ball grinding, mixed powder is obtained；
（2）By step（1）Obtained mixing bonding agent and mixed powder is mixed, and after ball milling, obtains coating slurry；
（3）By step（2）Gained coating slurry is coated on matrix material, is heating and curing, repeat it is described coating and
The process being heating and curing, until reaching required coating layer thickness, obtains the protective coating of anti-light laser ablation on matrix material.
Above-mentioned preparation method, it is preferred that the step（3）In, the process that is heating and curing is：It is described to be heating and curing
Process is：110 DEG C~130 DEG C are first warming up to, 1h~2h is incubated, 140 DEG C~160 DEG C are then heated to, 1h~2h is incubated, then rise
Temperature is incubated 2h~4h to 180 DEG C~200 DEG C.
Above-mentioned preparation method, it is preferred that the step（3）In, the mode of the coating is spraying.
Above-mentioned preparation method, it is preferred that the step（1）In, the quality of the diluent has to be described epoxide modified
The 100%~200% of machine silicones and phenolic resin gross mass.
Above-mentioned preparation method, it is preferred that the step（1）In, the diluent is molten for the mixing of dimethylbenzene and n-butanol
One kind in agent, alcohol or acetone.
Above-mentioned preparation method, it is preferred that the step（1）In, the incorporation time of crystalline flake graphite and the SiC whisker is 2h
~4h, the time of the wet ball grinding is 4h~8h.
Above-mentioned preparation method, it is preferred that the step（2）In, the time of the ball milling is 4h~6h.
In the protective coating of the anti-light laser ablation of the present invention, epoxide modified organic siliconresin preferred Jiangsu Jiangyin Osaka
The epoxy modified silicone resin of coating factory production, trade name TR613.
Compared with prior art, the advantage of the invention is that：
1st, the protective coating of anti-light laser ablation of the invention, using crystalline flake graphite as main function phase, SiC whiskers are enhancing
Body, epoxide modified organic siliconresin is matrix resin, and phenolic resin is curing agent.Wherein flaky graphite has natural layer
Shape structure, possesses good reflecting properties, low longitudinal thermal conductivity and high transverse thermal conductivity, also with higher vapourizing temperature, vapour
Change latent heat and radiance, with high resistance to laser ablation performance, and density is low, cheap.But, because crystalline flake graphite is because of layer
Between bond strength it is very low, can cause it is low using the tensile strength of crystalline flake graphite as the ablative cork coatings of main function phase, the present invention use
SiC whiskers improve strength of coating, using epoxide modified organic siliconresin as matrix resin, both with good manufacturability
And temperature tolerance, play a part of coating film forming agent and bonding agent again, resin curing agent is served as using phenolic resin, realize high into charcoal
Rate and higher solidification intensity, improve the heat resistance and flintiness of coating.
2nd, the preparation method technique of the protective coating of anti-light laser ablation of the invention is easy, with low cost, wherein coating
Slurry directly can be applied to protected substrate material surface, such as aluminium alloy, steel and polymer matrix composites using the method for spraying
Surface.
Brief description of the drawings
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 the moderate resistance light laser ablation of the embodiment of the present invention 1.
Fig. 3 is the pictorial diagram of the protective coating of the moderate resistance light laser ablation of the embodiment of the present invention 1.
Fig. 4 is the ablation shape appearance figure of the protective coating of the moderate resistance light laser ablation of the embodiment of the present invention 1.
Fig. 5 is the back side temperature rise curve of the protective coating of the moderate resistance light laser ablation of the embodiment of the present invention 1.
Embodiment
Below in conjunction with Figure of description and specific preferred embodiment, the invention will be further described, but not therefore and
Limit the scope of the invention.
Material and instrument employed in following examples are commercially available.
Embodiment 1：
A kind of protective coating of anti-light laser ablation of the invention, the protective coating is by crystalline flake graphite, SiC whiskers, ring
Prepared by the organic siliconresin and phenolic resin that oxygen is modified forms, wherein, as mass fraction, crystalline flake graphite is 50%, SiC whiskers
For 10%, epoxide modified organic siliconresin is 32%, and phenolic resin is 8%, epoxide modified organic siliconresin and phenolic resin
Mass ratio is 4: 1.
In the present embodiment, a diameter of 80 microns~100 microns of crystalline flake graphite.
In the present embodiment, epoxide modified organic siliconresin is specific to use from epoxide modified organic siliconresin solution
The epoxy modified silicone resin solution of Jiangsu Jiangyin Osaka coating Co., Ltd production, product designation TR613, its solid content
For 50%.That is, epoxide modified organic siliconresin quality contained in epoxide modified organic siliconresin solution accounts for above-mentioned
The 32% of four kinds of coating material gross masses.
A kind of preparation method of the protective coating of the anti-light laser ablation of above-mentioned the present embodiment, comprises the following steps：
（1）Epoxide modified organic of 50g crystalline graphite powders, 10g SiC whiskers, 64g is weighed respectively by above-mentioned mass fraction
Silicon resin solution（Wherein epoxide modified organic siliconresin mass content is 50%, and solvent quality content is 50%）With 8g phenolic aldehyde
Resin.Epoxide modified organic siliconresin solution and phenolic resin are mixed and added into 60g diluents（Alcohol）, it is placed in agitator
Middle stir about 1 hour, after stirring, obtains mixing bonding agent.Crystalline graphite powder and SiC whiskers are placed in V-type batch mixer
Mixing 2 hours, and wet ball grinding obtains mixed powder after 4 hours；
（2）By step（1）Obtained mixed powder and mixing bonding agent is mixed, and is placed in ball milling in planetary ball mill
4h, obtains coating slurry；
（3）By step（2）Gained coating slurry is fitted into the hand-held spray guns of routine, and is sprayed to have polished and cleans up
Aluminium alloy plate on, in spraying process, contained diluent is volatilized in atmosphere in coating, and the aluminium for being coated with coating slurry is closed
Golden plate is positioned in a conventional oven, is heating and curing, and what is be heating and curing comprises the following steps that：Baking oven is first heated to 120 DEG C
It is incubated after 1h, continues to improve oven temperature to 150 DEG C of insulation 1h, baking oven is then brought up into 180 DEG C of insulation 2h again.Treat that baking oven is cold
But sample is taken out afterwards, that is, the coating sample being fully cured.Because the coating layer thickness prepared by 1 spraying is about 0.5mm, weight
The process that overcoating is covered and is heating and curing, until reaching required coating layer thickness, obtains anti-light laser ablation on matrix material
Protective coating.In the present embodiment, using six spraying curing process, thickness about 3mm coating sample is obtained.
The microscopic appearance figure of crystalline flake graphite used in the present embodiment is as shown in Figure 1.
The microscopic appearance of the protective coating of anti-light laser ablation prepared by the present embodiment is as shown in Fig. 2 can be observed carbon
SiClx whisker is distributed in wherein.
The pictorial diagram of the protective coating of anti-light laser ablation prepared by the present embodiment is as shown in Figure 3.
Fig. 4 is ablation shape of the protective coating of the anti-light laser ablation prepared by the present embodiment after CW Laser 5s
Looks figure, laser used is myriawatt level semiconductor laser, and folding battle array using 10 high power laser diodes is used as groundwork
Device, forms square focus spot on target surface.Laser launches optical maser wavelength for 976nm, total light power of laser
The cm of 10874W, the cm of facula area 2.1 × 2.5.According to calculating, the laser average lamp power density that coating is born is 2071
W/cm2, mean energy density is 10.355 kJ/cm2, but coating only has slight ablation, and do not come off from matrix material, this
Illustrate that the figure layer has good resisting laser ablation performance.
Fig. 5 is back side temperature rise of the protective coating of the anti-light laser ablation prepared by the present embodiment in laser irradiation process
Curve.It 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 invention, the protective coating is by crystalline flake graphite, SiC whiskers, ring
Prepared by the organic siliconresin and phenolic resin that oxygen is modified forms, wherein, as mass fraction, crystalline flake graphite is 60%, SiC whiskers
For 5%, epoxide modified organic siliconresin is 25%, and phenolic resin is 10%, epoxide modified organic siliconresin and phenolic resin
Mass ratio is 2.5: 1.
In the present embodiment, a diameter of 50 microns~80 microns of crystalline flake graphite.
In the present embodiment, epoxide modified organic siliconresin is specific to use from epoxide modified organic siliconresin solution
The epoxy modified silicone resin solution of Jiangsu Jiangyin Osaka coating Co., Ltd production, product designation TR613, its solid content
For 50%.That is, epoxide modified organic siliconresin quality contained in epoxide modified organic siliconresin solution accounts for above-mentioned
The 25% of four kinds of coating material gross masses.
A kind of preparation method of the protective coating of the anti-light laser ablation of above-mentioned the present embodiment, concrete operation step and technique
Parameter is substantially the same manner as Example 1, and difference is：
Step（1）Weigh 60g crystalline graphite powders, 5g SiC whiskers, organic siliconresin solution epoxide modified 50g（This is molten
Epoxide modified organic siliconresin mass content is 50% in liquid, and solvent quality content is phenolic resin 50%) with 10g；
Step（1）The diluent added afterwards is that the diluent in 70g, the present embodiment is molten for the mixing of dimethylbenzene and n-butanol
The volume ratio of agent, wherein dimethylbenzene and n-butanol is 7: 3.
Embodiment 3：
A kind of protective coating of anti-light laser ablation of the invention, the protective coating is by crystalline flake graphite, SiC whiskers, ring
Prepared by the organic siliconresin and phenolic resin that oxygen is modified forms, wherein, as mass fraction, crystalline flake graphite is 50%, SiC whiskers
For 5%, epoxide modified organic siliconresin is 38%, and phenolic resin is 7%, epoxide modified organic siliconresin and phenolic resin
Mass ratio is about 5.5: 1.
In the present embodiment, a diameter of 60 microns~90 microns of crystalline flake graphite.
In the present embodiment, epoxide modified organic siliconresin is specific to use from epoxide modified organic siliconresin solution
The epoxy modified silicone resin solution of Jiangsu Jiangyin Osaka coating Co., Ltd production, product designation TR613, its solid content
For 50%.That is, epoxide modified organic siliconresin quality contained in epoxide modified organic siliconresin solution accounts for above-mentioned
The 38% of four kinds of coating material gross masses.
A kind of preparation method of the protective coating of the anti-light laser ablation of above-mentioned the present embodiment, concrete operation step and technique
Parameter is substantially the same manner as Example 1, and difference is：
Step（1）Weigh 50g crystalline graphite powders, 5g SiC whiskers, 76g epoxy modified silicone resins solution (solution
In epoxide modified organic siliconresin mass content be 50%, solvent quality content is 50%）, and 7g phenolic resin.
Step（1）The diluent added afterwards is 60g, and the diluent used in the present embodiment is acetone.
Described above is only the preferred embodiment of the present invention, and protection scope of the present invention is not limited to above-mentioned implementation
Example.All technical schemes belonged under thinking of the present invention belong to protection scope of the present invention.It is noted that for the art
Those of ordinary skill for, modification and retouching under the premise without departing from the principles of the invention, also should be regarded as the present invention guarantor
Protect scope.
Claims (9)
1. a kind of protective coating of anti-light laser ablation, it is characterised in that the protective coating be by crystalline flake graphite, SiC whiskers,
Epoxide modified organic siliconresin and phenolic resin are prepared and formed, wherein, as mass fraction, the crystalline flake graphite is 50%~
60%, the SiC whiskers are 5%~10%, and the epoxide modified organic siliconresin and phenolic resin are 35%~45% altogether, and institute
The mass ratio for stating epoxide modified organic siliconresin and phenolic resin is 2~6: 1.
2. the protective coating of anti-light laser ablation according to claim 1, it is characterised in that the diameter of the crystalline flake graphite
For 50 microns~100 microns.
3. a kind of preparation method of the protective coating of anti-light laser ablation as claimed in claim 1 or 2, comprises the following steps：
（1）Crystalline flake graphite, SiC whiskers, epoxide modified organic siliconresin and phenolic resin are weighed respectively by the mass fraction；
Epoxide modified organic siliconresin and phenolic resin are added in diluent and dissolved, and is stirred, obtains mixing bonding agent；
Crystalline flake graphite and SiC whiskers are mixed, after wet ball grinding, mixed powder is obtained；
（2）By step（1）Obtained mixing bonding agent and mixed powder is mixed, and after ball milling, obtains coating slurry；
（3）By step（2）Gained coating slurry is coated on matrix material, is heating and curing, and repeats the coating and heating
The process of solidification, until reaching required coating layer thickness, obtains the protective coating of anti-light laser ablation on matrix material.
4. preparation method according to claim 3, it is characterised in that the step（3）In, the process being heating and curing
For：110 DEG C~130 DEG C are first warming up to, 1h~2h is incubated, 140 DEG C~160 DEG C are then heated to, 1h~2h is incubated, then be warming up to
180 DEG C~200 DEG C, it is incubated 2h~4h.
5. preparation method according to claim 3, it is characterised in that the step（3）In, the mode of the coating is spray
Apply.
6. the preparation method according to any one of claim 3~5, it is characterised in that the step（1）In, it is described dilute
The quality for releasing agent is the 100%~200% of the epoxide modified organic siliconresin and phenolic resin gross mass.
7. the preparation method according to any one of claim 3~5, it is characterised in that the step（1）In, it is described dilute
It is one kind in mixed solvent, alcohol or the acetone of dimethylbenzene and n-butanol to release agent.
8. the preparation method according to any one of claim 3~5, it is characterised in that the step（1）In, the squama
The incorporation time of piece graphite and SiC whiskers is 2h~4h, and the time of the wet ball grinding is 4h~8h.
9. the preparation method according to any one of claim 3~5, it is characterised in that the step（2）In, the ball
The time of mill is 4h~6h.
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| CN107177307B (en) * | 2017-05-24 | 2019-08-23 | 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 |
| CN107201171B (en) * | 2017-05-24 | 2019-08-23 | 中南大学 | A kind of boron bakelite resin/epoxy modified silicone resin coating of resistance to ablation protection and preparation method thereof |
| 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 |
| 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 |
| CN113549862B (en) * | 2020-04-08 | 2022-08-23 | 北京理工大学 | High-energy laser protection multilayer composite material coating structure and manufacturing method thereof |
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