CN101220211B - Anti-laser composite resin and method for producing the same - Google Patents
Anti-laser composite resin and method for producing the same Download PDFInfo
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- CN101220211B CN101220211B CN2007101918792A CN200710191879A CN101220211B CN 101220211 B CN101220211 B CN 101220211B CN 2007101918792 A CN2007101918792 A CN 2007101918792A CN 200710191879 A CN200710191879 A CN 200710191879A CN 101220211 B CN101220211 B CN 101220211B
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Abstract
The invention discloses a composite resin and a preparation method thereof. The composite resin is prepared by fully mixing of 100 portions of thermoset resin and curing agent, 1-70 portions of ceramic whisker and 1-70 portions of flake aluminum by weight, wherein, the ceramic whisker is carborundum, silicon nitride, titanium nitride, alumina, aluminum nitride, zirconia, titanium carbide, potassium titanate or aluminium borate. The anti-laser composite resin prepared by the invention has good mechanical property, ablation resistance and thermal insulation property and can be used as coating material, adhesive and matrix resin of composite materials, thereby having wide application.
Description
Technical field
The present invention relates to a kind of compound resin and preparation method thereof.
Background technology
Laser technology makes modern battlefield be flooded with various laser threats in the widespread use of military field, particularly high energy laser weapon is about to drop under battle conditions, its appearance makes aerial targets such as guided missile, aircraft, satellite face the danger that is directly destroyed, particularly pregnable position is as the positions such as optical window of various kinds of sensors on the radome of the target seeker nose cone of guided missile, rebecca, the satellite.Polymer matrix composites are the critical materials that are used to make these positions, and the quality of the anti-laser characteristics of matrix resin is the key of the anti-laser characteristics height of decision matrix material.Therefore, the development with new type resin and preparation method thereof of anti-laser characteristics has great importance.
Aspect anti-laser matrix material, obtained a series of scientific payoffss, representational system is that anti-laser sapphire whisker strengthens ceramic matric composite, carbon and silicon carbide fiber enhanced silicon oxide and titanium oxide matrix material etc.In being entitled as " research of the anti-laser hardening material of SiC fine ceramics " ([J] Arms Material scientific and engineering Vol.24 No.139-43) literary composition, disclosing a kind of is presoma with poly-carbon siloxanes, the method for preparing the anti-laser hardening material of SiC fine ceramics has overcome the shortcoming of existing manufacturability difference in the traditional preparation process method of SiC material.
Aspect anti-laser polymer matrix composites, people mainly prepare anti-laserable material by the structure formation that changes material, have obtained effect preferably.As being sandwich structure with composite Materials Design, promptly between two-layer heat-protection layer (constituting), dispose an anti-laser radiation layer by resol, Resins, epoxy etc., this layer is made of the carbon fiber and the heavy metal of solvent impregnated resin, and heavy metal can be powder or particle, with tungsten for well.No matter this shows, be that resin all is that it is mainly formed for heat-protection layer or antagonism laser layer.Yet general compound resin exists defectives such as interlaminar shear strength is low, and mechanical property has been subjected to certain influence.
Summary of the invention
In order to overcome the deficiency that prior art exists, the invention provides a kind of mechanics, heat insulation, high temperature resistant and ablation property with excellence, and the simple anti-laser composite resin of preparation technology and preparation method thereof.
The technical solution adopted in the present invention is: a kind of anti-laser composite resin is provided, and it is made up of thermosetting resin and solidifying agent, flake aluminum and ceramic whisker.
Above-mentioned compound resin is made up of 100 parts of thermosetting resins and solidifying agent, 1～70 part of flake aluminum and 1～70 part of ceramic whisker by weight.
Wherein, described ceramic whisker is silicon carbide, silicon nitride, titanium nitride, aluminum oxide, aluminium nitride, zirconium white, titanium carbide, potassium titanate or aluminum borate.
A kind of preparation method of anti-laser composite resin by weight, adds 1～70 part of ceramic whisker and 1～70 part of flake aluminum in 100 parts of thermosetting resins and solidifying agent, through thorough mixing, obtain anti-laser composite resin.
Because ceramic whisker not only has good high-temperature stability and ablation property, and has an excellent mechanical property, particularly it is in the arrangement of thickness direction, can play the booster action of similar " rivet ", therefore, the compound resin that makes of the present invention has solved the normal low problem of interlaminar shear strength that occurs of fibre composite effectively.On the other hand, adopt flake aluminum, can effectively bring into play its iris action, effectively heat insulation.Therefore, compared with prior art, the anti-laser composite resin that the present invention makes has outstanding performance synthesis advantage.
Description of drawings
Fig. 1 is the SEM figure by the anti-laser composite resin of the embodiment of the invention 1 technical scheme preparation.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is further described:
Embodiment 1:
The aluminum borate ceramic whisker is dried down at 120 ℃ and was handled 4 hours, the whisker of 10wt% is poured in the acetone soln of surface treatment agent γ-An Jibingjisanyiyangjiguiwan, stir with the high speed homogenization stirrer, after room temperature hangs 8 hours, dried 2 hours down at 80～90 ℃, the dry airtight storage of surface-treated aluminium borate whisker is standby.
In with the there-necked flask of thermometer, agitator, nitrogen introducing port, add 100g bisphenol A type epoxy resin (E51), be heated to 80 ℃ and make it to become low-viscosity (mobile) liquid, add aluminium borate whisker and the 42g flake aluminum of 30g after aforesaid method is handled, fully mixed 20 minutes, after being chilled to room temperature, add 3g solidifying agent imidazoles again, stir, promptly get anti-laser composite resin.
In technical solution of the present invention, the consumption of solidifying agent is decided on the resin kind with reference to conventional scheme.Ceramic whisker, flake aluminum also can not carry out surface treatment and directly use.
The compound resin that makes is cured processing according to following processing condition: 80 ℃/2h+110 ℃/2h+150 ℃/2h+180 ℃/2h, obtain the solidified compound resin.Adopt CO
2Laser apparatus carries out irradiation test to cured composite resin, and (irradiation parameters is operation wavelength 10.6 μ m, spot diameter 2mm, laser power 35W, laser intensity ≈ 1114Wcm
-2, irradiation time 4s), the mass ablative rate of compound resin is 0.0046g/s.The E51/ imidazoles resin of forming with 100g bisphenol A type epoxy resin (E51) and 3g solidifying agent imidazoles solidifies according to same process, and carries out identical laser irradiation experiment, and the mass ablative rate of this resin is 0.189g/s.The contrast experiment shows that anti-laser composite resin provided by the invention has good ablation resistance.
Referring to accompanying drawing 1, it is the SEM figure (X 4000) by the anti-laser composite resin of present embodiment technical scheme preparation.As seen from Figure 1, aluminium powder is arranged in the resin with sheet form, brings into play iris action, effectively improves the heat-proof quality of material.
Embodiment 2:
Flake aluminum is dropped into the homogenizer high speed to be stirred, treat to be incubated 10 minutes when the aluminium powder temperature is warming up to 110～120 ℃, add aluminate coupling agent (DL-411), continued high-speed stirring 10 minutes to remove the moisture content in the aluminium powder, cooling, the dry airtight storage of surface-treated aluminium powder is standby.
42g diallyl bisphenol (the modification body of bimaleimide resin) is added in the there-necked flask of having thermometer, agitator, nitrogen introducing port, add 1g potassium titanate ceramic whiskers and 20g surface-treated flake aluminum at 100～110 ℃, fully mixed 20 minutes.
With 58g 4,4-dimaleoyl imino ditane (BMI) adds in the above-mentioned there-necked flask, stirs to be warming up between 130～135 ℃, reacts 40 minutes, pours out cooling and promptly gets anti-laser composite resin.
Embodiment 3:
Carry out the surface treatment of aluminium borate whisker by embodiment 1 scheme.
Carry out the surface treatment of flake aluminum by embodiment 2 schemes.
In with the there-necked flask of thermometer, agitator, nitrogen introducing port, add the 100g bisphenol A cyanate ester resin, be heated to 100 ℃, add surface-treated 1g aluminium borate whisker and 70g flake aluminum, fully mixed 30 minutes.Then drip the 0.8g bisphenol A type epoxy resin, stir, promptly get anti-laser composite resin.Be chilled to room temperature, promptly get anti-laser composite resin.
Embodiment 4:
The titanium nitride ceramic whisker was dried 4 hours down at 120 ℃, the 10wt% whisker is poured in the acetone soln of 5wt% surface treatment agent tetrabutyl titanate ester, after stirring with the high speed homogenization stirrer, 80 ℃ of down oven dry 24 hours, surface-treated titanium nitride whisker drying is airtight, store standby.
In with the there-necked flask of thermometer, agitator, nitrogen introducing port, add 100g bisphenol A type epoxy resin (E51), be heated to 80 ℃ and make it to become low-viscosity (mobile) liquid, add 70g flake aluminum and 70g surface-treated titanium nitride whisker, fully mixed 20 minutes.Then be chilled to room temperature, add the 100g low molecular polyamides, stir, promptly get anti-laser composite resin.
Embodiment 5:
In with the there-necked flask of thermometer, agitator, nitrogen introducing port, add 100g bisphenol A type epoxy resin (E51), be heated to 80 ℃ and make it to become low-viscosity (mobile) liquid, add 1g flake aluminum and 1g aluminum borate ceramic whisker, fully mixed 20 minutes.Then be chilled to room temperature, add 3g solidifying agent imidazoles, stir, promptly get anti-laser composite resin.
Embodiment 6:
Carry out the surface treatment of titanium nitride ceramic whisker by embodiment 4.
In with the there-necked flask of thermometer, agitator, nitrogen introducing port, add 100g Resins, epoxy E51 and 70g aminomethyl phenyl silicone resin (SY409); Be heated to 60 ℃ and make it to become low-viscosity (mobile) liquid, add 45g flake aluminum and 55g aluminium borate whisker, fully mixed 20 minutes, add the 7g curing agent dicyandiamide, stir, promptly get anti-laser composite resin.
The compound resin that makes is cured processing according to following processing condition: 100 ℃/1h+130 ℃/2h+150 ℃/2h+180 ℃/2h+200 ℃/2h, obtain the solidified compound resin.Adopt CO
2Laser apparatus carries out irradiation test to cured composite resin, and (irradiation parameters is operation wavelength 10.6 μ m, spot diameter 2mm, laser power 35W, laser intensity ≈ 1114Wcm
-2, irradiation time 4s), the mass ablative rate of compound resin is 0.0037g/s.
Claims (2)
1. anti-laser composite resin, it is characterized in that: by weight, it is made up of 100 parts of thermosetting resins and solidifying agent, 1～70 part of flake aluminum and 1～70 part of ceramic whisker; Described ceramic whisker is silicon carbide, silicon nitride, titanium nitride, aluminum oxide, aluminium nitride, zirconium white, titanium carbide, potassium titanate or aluminum borate.
2. the preparation method of an anti-laser composite resin is characterized in that: by weight, add 1～70 part of ceramic whisker and 1～70 part of flake aluminum in 100 parts of thermosetting resins and solidifying agent, through thorough mixing, obtain anti-laser composite resin; Described ceramic whisker is silicon carbide, silicon nitride, titanium nitride, aluminum oxide, aluminium nitride, zirconium white, titanium carbide, potassium titanate or aluminum borate.
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| CN105111931B (en) * | 2015-08-31 | 2017-10-03 | 中国人民解放军国防科学技术大学 | Protective coating of anti-light laser ablation and preparation method thereof |
| CN107999957B (en) * | 2016-10-28 | 2020-01-07 | 中国航空制造技术研究院 | Protective material for preventing laser hole-making from damaging opposite wall of cavity part and filling method |
| CN106893262B (en) * | 2017-03-16 | 2019-03-22 | 西安理工大学 | A kind of epoxy resin composite material and preparation method thereof of high intensity anti-ultraviolet ageing |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1693421A (en) * | 2005-06-17 | 2005-11-09 | 浙江大学 | Organic-inorganic fire-retarded high molecular material of few additive high performance |
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| CN1693421A (en) * | 2005-06-17 | 2005-11-09 | 浙江大学 | Organic-inorganic fire-retarded high molecular material of few additive high performance |
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