WO2018223779A1 - 一种吸波浸渍胶液和吸波蜂窝及其制备方法 - Google Patents
一种吸波浸渍胶液和吸波蜂窝及其制备方法 Download PDFInfo
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- WO2018223779A1 WO2018223779A1 PCT/CN2018/083678 CN2018083678W WO2018223779A1 WO 2018223779 A1 WO2018223779 A1 WO 2018223779A1 CN 2018083678 W CN2018083678 W CN 2018083678W WO 2018223779 A1 WO2018223779 A1 WO 2018223779A1
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- Prior art keywords
- absorbing
- epoxy resin
- honeycomb
- component epoxy
- preparation
- Prior art date
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- 239000003292 glue Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000007788 liquid Substances 0.000 title claims abstract description 12
- 238000005470 impregnation Methods 0.000 title abstract description 4
- 239000003822 epoxy resin Substances 0.000 claims abstract description 91
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 91
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 36
- 229920000570 polyether Polymers 0.000 claims abstract description 36
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 26
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000002904 solvent Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims description 38
- 239000003795 chemical substances by application Substances 0.000 claims description 32
- 238000007654 immersion Methods 0.000 claims description 28
- 239000000080 wetting agent Substances 0.000 claims description 25
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 18
- 239000004760 aramid Substances 0.000 claims description 17
- 229920003235 aromatic polyamide Polymers 0.000 claims description 17
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- 229920001296 polysiloxane Polymers 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 210000002421 cell wall Anatomy 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 8
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 7
- 210000004027 cell Anatomy 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 claims description 5
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 3
- VNKYTQGIUYNRMY-UHFFFAOYSA-N methoxypropane Chemical compound CCCOC VNKYTQGIUYNRMY-UHFFFAOYSA-N 0.000 claims description 2
- 238000009736 wetting Methods 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims 1
- 239000000843 powder Substances 0.000 claims 1
- 241000264877 Hippospongia communis Species 0.000 description 75
- 239000000853 adhesive Substances 0.000 description 17
- 230000001070 adhesive effect Effects 0.000 description 17
- 238000003756 stirring Methods 0.000 description 13
- 239000006096 absorbing agent Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 5
- 239000011358 absorbing material Substances 0.000 description 4
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 229930185605 Bisphenol Natural products 0.000 description 2
- 230000003254 anti-foaming effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- DHXVGJBLRPWPCS-UHFFFAOYSA-N Tetrahydropyran Chemical compound C1CCOCC1 DHXVGJBLRPWPCS-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
Images
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- C—CHEMISTRY; METALLURGY
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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- B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C—CHEMISTRY; METALLURGY
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
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- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
- C08G59/22—Di-epoxy compounds
- C08G59/24—Di-epoxy compounds carbocyclic
- C08G59/245—Di-epoxy compounds carbocyclic aromatic
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
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- C08G59/502—Polyalkylene polyamines
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/50—Additional features of adhesives in the form of films or foils characterized by process specific features
Definitions
- the invention relates to the field of composite materials, in particular to a absorbing impregnating glue liquid and a absorbing wave honeycomb and a preparation method thereof.
- the absorbing materials can be coated on various weapons and military equipment such as aircraft, missiles, tanks, ships, warehouses, etc., it is possible to absorb the reconnaissance waves and attenuate the reflected signals, thereby breaking through the enemy radar's defense zone.
- This is a powerful means of anti-radar reconnaissance, which can reduce the attack of weapons systems by missiles and laser weapons. Therefore, the study of absorbing materials is also of great value in enhancing our military capabilities and improving the combat effectiveness of the military.
- the honeycomb structure has a material shape similar to that of a natural honeycomb. It has a unique hexagonal structure that can withstand the force applied from the outside and is lighter in weight, ensuring sufficient strength while minimizing the weight of the material. Therefore, the material of the honeycomb structure is an important matrix material.
- Coating the absorbing adhesive on the honeycomb structure is one of the important means to prepare the absorbing honeycomb. It can meet the requirements of the absorbing material for "thin thickness, light weight, frequency bandwidth and absorption", but the existing honeycomb
- the impregnation process is to use a hair dryer or a compressed gas to blow off the glue hole of the cell hole of the honeycomb, which easily causes the phenomenon of plugging, which seriously affects the quality of the punched honeycomb.
- the present invention has studied a method for preparing a absorbing honeycomb to provide a absorbing honeycomb which is not blocked, has no deformation, and has excellent absorbing properties.
- a absorbing immersion glue comprising: a two-component epoxy resin; a solvent; a polyether siloxane; a carbon powder; wherein the two-component epoxy resin and the The mass ratio of the solvent is 1:3 to 1:5, the ratio of the mass of the two-component epoxy resin to the carbon powder is from 3:1 to 6:1, and the absorbing immersion glue is
- the polyether siloxane has a mass fraction of 0.05% to 0.2%.
- the ratio of the mass of the two-component epoxy resin to the solvent is 1:4, and the ratio of the mass of the two-component epoxy resin to the carbon powder is 5: 1, and the mass fraction of the polyether siloxane in the absorbing impregnating gum is 0.1%.
- the two-component epoxy resin comprises an epoxy resin and a curing agent, wherein the epoxy resin comprises a bisphenol A type epoxy resin, a bisphenol F type epoxy resin or A mixture of the curing agent comprising one or more of diethylenetriamine, triethylenetetramine or tetraethylenepentamine.
- the mass ratio of the epoxy resin to the curing agent in the two-component epoxy resin is from 100:5 to 100:20.
- the mass ratio of the epoxy resin to the curing agent in the two-component epoxy resin is 10:1.
- the solvent is a combination of one or more of methanol, ethanol, ethyl acetate, acetone, methyl ethyl ketone or methyl propyl ether.
- the polyether siloxane is a polyether siloxane wetting agent A-008h, a polyether siloxane wetting agent A-004h or a polyether siloxane.
- the polyether-based siloxane After dissolving the two-component epoxy resin in the solvent, the polyether-based siloxane is added to be wetted, and after uniformly mixing, carbon powder used as a absorbing agent is added, and after uniformly mixing, the obtained Absorbing the impregnating glue.
- the preparation method comprises: dissolving the two-component epoxy resin in a solvent, adding a polyether-based silicone wetting agent for wetting, stirring at a high speed for 8-12 minutes, and uniformly mixing, Obtaining a two-component epoxy resin mixed solution; adding carbon powder to the two-component epoxy resin mixed solution, stirring for 20-40 minutes, ball milling for 1.5-2.5 hours, and uniformly mixing to obtain the absorbing impregnating rubber liquid.
- a method for preparing a absorbing honeycomb comprising: impregnating a honeycomb into the above-mentioned absorbing immersion glue, and impregnating the absorbing immersion glue The honeycomb is taken out and solidified to obtain an absorbing honeycomb.
- the honeycomb is immersed in the absorbing immersion glue for 4 to 6 minutes, and the absorbing immersion glue of the honeycomb cell wall is taken out and blown at 80 to 120 ° C.
- the absorbing honeycomb was obtained by curing at a temperature for 1 to 2 hours.
- the honeycomb is an aramid honeycomb.
- the invention provides an absorbing wave dipping glue and a absorbing wave honeycomb and a preparation method thereof.
- the invention obtains an absorbing adhesive liquid by using a two-component epoxy resin, a solvent, a polyether siloxane, and a absorbing agent carbon powder, wherein the ratio of the mass of the two-component epoxy resin to the solvent is a ratio of 1:2 to 1:5, the mass of the two-component epoxy resin and the carbon powder is from 3:1 to 6:1, and the polyether silicon in the absorbing immersion glue The mass fraction of oxane is 0.05% to 0.2%.
- the honeycomb was impregnated with the absorbing gel and solidified to obtain an absorbing honeycomb.
- the invention reduces the tension of the surface of the absorbing adhesive by adding a polyether silicone wetting agent having extremely low surface tension and having antifoaming property, so that the coating is quickly and uniformly spread on the honeycomb surface, thereby obtaining no plugging.
- the absorbing honeycomb material with pores, no deformation and excellent absorbing properties can be widely used in aerospace, aircraft, radome and the like.
- FIG. 1 is a flow chart for preparing a absorbing immersion glue according to an embodiment of the present invention.
- FIG. 2 is a flow chart of preparing a absorbing cell in accordance with an embodiment of the present invention.
- FIG. 3 is an overall flow diagram of the preparation of a absorbing cell in accordance with a preferred embodiment of the present invention.
- the preparation method of the absorbing immersion glue and the absorbing wave honeycomb provided by the invention comprises the following steps:
- step S101 in Fig. 1 the two-component epoxy resin is dissolved in a solvent, a wetting agent is added, and the mixture is uniformly mixed to obtain a mixture.
- the mass ratio of the two-component epoxy resin to the solvent is 1:3 to 1:5, and the mixture is stirred at a stirring rate of 1600 rpm to 2000 rpm for 8 to 12 minutes, preferably, The mixture was stirred at a stirring rate of 1800 rpm for 10 minutes, and the mixture was uniformly mixed to obtain the mixture.
- the solvent is a combination of one or more of ethanol, ethyl acetate, acetone, methyl ethyl ketone, and methyl alcohol methyl ether.
- the wetting agent is a combination of one or more of polyether silicone wetting agent A-008, polyether silicone wetting agent A-004 or polyether silicone wetting agent W-23. And the mass fraction of the polyether siloxane in the absorbing impregnating gum is 0.05% to 0.2%.
- the two-component epoxy resin comprises an epoxy resin and a curing agent, wherein the epoxy resin comprises a bisphenol A type epoxy resin, a bisphenol F type epoxy resin or a mixture thereof, and the curing agent comprises: diethylene triamine A combination of one or more of triethylenetetramine or tetraethylenepentamine.
- the mass ratio of the epoxy resin to the curing agent in the two-component epoxy resin is from 100:5 to 100:20.
- the absorbing agent carbon powder is added to the mixture, and the mixture is uniformly mixed and then ball-milled to obtain a absorbing adhesive.
- the ratio of the mass of the two-component epoxy resin to the carbon powder is from 3:1 to 6:1, and after mixing for 20 to 40 minutes, the mixture is uniformly mixed, and then poured into a ball mill tank for 1.5 to 2.5 hours, preferably, After stirring for 30 minutes, the mixture was uniformly mixed, and poured into a ball mill jar for 2 hours to obtain a absorbing impregnating glue.
- the honeycomb is impregnated into the absorbing immersion glue prepared in step S102, in which the honeycomb is immersed in the absorbing gel for 4 to 6 minutes, Preferably, it is immersed for 5 minutes.
- step S104 in Fig. 2 the honeycomb impregnated with the absorbing immersion glue is taken out and solidified to obtain an absorbing honeycomb.
- the honeycomb impregnated with the absorbing immersion glue is taken out, the glue of the honeycomb cell wall is blown off, and cured in an oven at a temperature of 80 to 120 ° C for 1 to 2
- the absorbing honeycomb was produced in an hour.
- the honeycomb is an aramid honeycomb.
- step S105 after dissolving the two-component epoxy resin in a solvent, a polyether silicone wetting agent is added to obtain a two-component epoxy resin mixture; in step S106, the bicomponent ring is obtained. Adding carbon powder to the oxygen resin mixture, stirring for 20-40 minutes, ball milling for 1.5-2.5 hours, mixing and then ball milling to obtain a absorbing impregnating glue; in step 107, impregnating the honeycomb into the absorbing impregnating glue, impregnating The honeycomb having the absorbing immersion glue is taken out and solidified to obtain an absorbing honeycomb.
- step S105 after dissolving the two-component epoxy resin in a solvent, a polyether silicone wetting agent is added to obtain a two-component epoxy resin mixture; in step S106, the bicomponent ring is obtained. Adding carbon powder to the oxygen resin mixture, stirring for 20-40 minutes, ball milling for 1.5-2.5 hours, mixing and then ball milling to obtain a absorbing impregnating glue; in step 107, impre
- the preparation method of the absorbing wave honeycomb obtaineds the absorbing wave glue by using the two-component epoxy resin, the solvent, the wetting agent and the carbon powder, impregnating the honeycomb with the absorbing adhesive liquid, and solidifying to obtain the absorbing wave. honeycomb.
- the absorbing adhesive prepared by the method can be uniformly applied to the surface of the honeycomb. Therefore, the prepared absorbing honeycomb is non-blocking, non-deformable and has excellent absorbing properties, and can be widely applied to the aerospace field, aircraft. , radome and other fields.
- the mass ratio of the epoxy resin to the curing agent is 20:1.
- the aramid honeycomb was immersed in the absorbing gel for 5 minutes, taken out, and the glue in the cell wall of the aramid honeycomb was blown off, and cured in an oven at a temperature of 80 ° C for 1 hour to obtain the suction. Wave honeycomb.
- the two-component epoxy resin was dissolved in 400 g of ethyl acetate, 1 g of a polyether-based silicone wetting agent A-008 was added, and the mixture was stirred at a stirring rate of 2000 rpm for 10 minutes, and uniformly mixed to obtain a mixture.
- 20 g of absorbing agent carbon powder was added to the mixture, stirred for 30 minutes, uniformly mixed, and then ball-milled in a ball mill for 2 hours to obtain a absorbing adhesive, wherein the two-component epoxy resin included bisphenol F-type epoxy resin and A curing agent, the curing agent is triethylenetetramine.
- the mass ratio of epoxy resin to curing agent in the two-component epoxy resin is 5:1.
- the aramid honeycomb was immersed in the absorbing gel for 5 minutes, taken out, and the glue in the cell wall of the aramid honeycomb was blown off, and solidified in an oven at a temperature of 120 ° C for 2 hours to obtain the suction. Wave honeycomb.
- the two-component epoxy resin was dissolved in 400 g of acetone, 0.5 g of a polyether siloxane wetting agent A-008 was added, and the mixture was stirred at a stirring rate of 1800 rpm for 10 minutes, and uniformly mixed to obtain a mixture.
- 20 g of absorbing agent carbon powder was added to the mixture, stirred for 30 minutes, uniformly mixed, and then ball-milled in a ball mill for 2 hours to obtain a absorbing adhesive, wherein the two-component epoxy resin included bisphenol A type epoxy resin and A curing agent, the curing agent is tetraethylene pentamine.
- the mass ratio of the epoxy resin to the curing agent in the two-component epoxy resin is 10:1.
- the aramid honeycomb was immersed in the absorbing gel for 5 minutes, taken out, and the glue in the cell wall of the aramid honeycomb was blown off, and cured in an oven at a temperature of 100 ° C for 1.5 hours to obtain a absorbing honeycomb. .
- the two-component epoxy resin was dissolved in 400 g of methyl ethyl ketone, 0.5 g of a polyether siloxane wetting agent W-23 was added, and the mixture was stirred at a stirring rate of 1,700 rpm for 10 minutes, and uniformly mixed to obtain a mixture.
- 20 g of absorbing agent carbon powder was added to the mixture, stirred for 30 minutes, uniformly mixed, and then ball-milled in a ball mill for 2 hours to obtain a absorbing adhesive, wherein the two-component epoxy resin included bisphenol A type epoxy resin and A curing agent, the curing agent is triethylenetetramine.
- the mass ratio of epoxy resin to curing agent in the two-component epoxy resin is 15:1.
- the aramid honeycomb was immersed in the absorbing gel for 5 minutes, taken out, and the glue in the cell wall of the aramid honeycomb was blown off, and cured in an oven at a temperature of 85 ° C for 2 hours to obtain the suction. Wave honeycomb.
- the aramid honeycomb was immersed in the absorbing gel for 6 minutes, taken out, and the glue in the cell wall of the aramid honeycomb was blown off, and cured in an oven at a temperature of 110 ° C for 1.5 hours to obtain the suction. Wave honeycomb.
- the two-component epoxy resin includes bisphenol A type epoxy resin and A curing agent, the curing agent is triethylenetetramine.
- the mass ratio of epoxy resin to curing agent in the two-component epoxy resin is 8:1.
- the aramid honeycomb was immersed in the absorbing gel for 4 minutes, taken out, and the glue in the cell wall of the aramid honeycomb was blown off, and cured in an oven at a temperature of 100 ° C for 1 hour to obtain the suction. Wave honeycomb.
- the two-component epoxy resin was dissolved in 500 g of methyl ethyl ketone, 0.8 g of a polyether siloxane wetting agent was added, and the mixture was stirred at a stirring rate of 1,700 rpm for 12 minutes, and uniformly mixed to obtain a mixture.
- 30 g of absorbing agent carbon powder was added to the mixture, stirred for 40 minutes, uniformly mixed, and then ball-milled in a ball mill for 1.5 hours to obtain a absorbing adhesive, wherein the two-component epoxy resin included bisphenol A type epoxy resin and A curing agent, the curing agent is triethylenetetramine.
- the mass ratio of epoxy resin to curing agent in the two-component epoxy resin is 18:1.
- the aramid honeycomb was immersed in the absorbing gel for 5 minutes, taken out, and the glue in the cell wall of the aramid honeycomb was blown off, and cured in an oven at a temperature of 85 ° C for 2 hours to obtain the suction. Wave honeycomb.
- the absorbing adhesives prepared in Examples 1 to 7 were subjected to a surface tension test by a hanging sheet method, and the test results were as follows:
- the absorbing honeycombs prepared in Examples 1 to 7 were subjected to microwave absorbing chamber method for microwave absorbing performance test.
- the test results are as follows:
- the present invention provides a absorbing impregnating glue liquid and a absorbing wave honeycomb and a preparation method thereof, which are prepared by using a two-component epoxy resin, a solvent, a wetting agent and a carbon powder to obtain an absorbing adhesive liquid.
- the absorbing gel is impregnated with the honeycomb and solidified to obtain an absorbing honeycomb.
- the invention reduces the tension of the surface of the absorbing adhesive by adding a polyether silicone wetting agent having extremely low surface tension and having antifoaming property, so that the coating is quickly and uniformly spread on the honeycomb surface, thereby obtaining no plugging.
- the absorbing honeycomb material with pores, no deformation and excellent absorbing properties can be widely used in aerospace, aircraft, radome and the like.
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Abstract
一种吸波浸渍胶液,包括:双组份环氧树脂;溶剂;聚醚类硅氧烷;以及炭粉;其中,所述双组份环氧树脂与所述溶剂的质量之比为1:3~1:5,所述双组份环氧树脂与所述炭粉的质量之比为3:1~6:1,并且所述吸波浸渍胶液中所述聚醚类硅氧烷的质量份数为0.05%~0.2%。公开了所述胶液的制备方法,还公开了一种吸波蜂窝及其制备方法。
Description
本发明涉及复合材料领域,具体而言,涉及一种吸波浸渍胶液和吸波蜂窝及其制备方法。
随着现代技术的不断发展,越来越多的电子产品进入到我们的日常生活和工作中,人们对电子产品的依赖度也越来越高,但是它们在给我们的生活带来越来越多的便利的同时,其产生的大量的电磁辐射也对我们的健康造成很大的威胁。例如,在机场,飞机航班因电磁波干扰无法起飞而误点;在医院,移动电话常会干扰各种电子诊疗仪器的正常工作。因此,研究一种能较好地抵挡并削弱电磁波辐射的吸波材料具有十分重要的意义。
此外,在军事上,如果能在飞机、导弹、坦克、舰艇、仓库等各种武器装备和军事设施上涂覆吸收材料,就可以吸收侦察电波、衰减反射信号,从而突破敌方雷达的防区,这是反雷达侦察的一种有力手段,可以减少武器***遭受导弹和激光武器的袭击。因此,对吸波材料的研究在增强我国的军事能力,提高军队的战斗力方面也具有极其重大的价值。
蜂窝形结构的材料外形与自然界的蜂窝类似,具有独特的六边形结构,能均匀地承受外界施加的力,并且质量较轻,可以在保证足够的强度的同时,最大限度的减轻材料的重量,因此蜂窝形结构的材料是一种重要的基体材料。
在蜂窝形结构上涂覆吸波胶液是制备吸波蜂窝的重要手段之一,它能够满足吸波材料对“厚度薄、质量轻、频带宽、吸收强”的要求,但是现有的蜂窝浸渍工艺是使用电吹风机或者压缩气体吹除蜂窝的格孔壁洞的胶液,很容易导致堵孔现象,严重影响打孔蜂窝质量。
发明内容
针对相关技术中的问题,本发明研究了一种吸波蜂窝的制备方法,以提供一种不堵孔、不变形、吸波性能优异的吸波蜂窝。
根据本发明的一个方面,提供了一种吸波浸渍胶液,包括:双组份环氧树脂;溶剂;聚醚类硅氧烷;炭粉;其中,所述双组份环氧树脂与所述溶剂的质量之比为1:3~1:5,所述双组份环氧树脂与所述炭粉的质量之比为3:1~6:1,并且所述吸波浸渍胶液中所述聚醚类硅氧烷的质量分数为0.05%~0.2%。
在上述吸波浸渍胶液中,所述双组份环氧树脂与所述溶剂的质量之比为1:4,所述双组份环氧树脂与所述炭粉的质量之比为5:1,并且所述吸波浸渍胶液中所述聚醚类硅氧烷的质量分数为0.1%。
在上述吸波浸渍胶液中,所述双组份环氧树脂包括环氧树脂和固化剂,其中,所述环氧树脂包括双酚A型环氧树脂、双酚F型环氧树脂或者它们的混合物,所述固化剂包括:二乙烯三胺、三乙烯四胺或四乙烯五胺中的一种或者多种的组合。
在上述吸波浸渍胶液中,所述双组份环氧树脂中所述环氧树脂和所述固化剂的质量比为100:5~100:20。
在上述吸波浸渍胶液中,所述双组份环氧树脂中所述环氧树脂和所述固化剂的质量比为10:1。
在上述吸波浸渍胶液中,所述溶剂为甲醇、乙醇、乙酸乙酯、丙酮、丁酮或丙醇甲醚的一种或多种的组合。
在上述吸波浸渍胶液中,所述聚醚类硅氧烷为聚醚类硅氧烷润湿剂A-008h、聚醚类硅氧烷润湿剂A-004h或聚醚类硅氧烷润湿剂W-23h中的一种或多种的组合。
根据本发明的另一方面,还提供了上述吸波浸渍胶液的吸波浸渍胶液制备方法,所述制备方法包括:
将所述双组份环氧树脂用所述溶剂溶解后,加入所述聚醚类硅氧烷进行润湿,混合均匀后,加入用作吸波剂的炭粉,混合均匀后,得到所述吸波浸渍胶液。
在上述制备方法中,所述制备方法包括:将所述双组份环氧树脂用溶剂溶解后,加入聚醚类硅氧烷润湿剂进行润湿,高速搅拌8-12分钟混合均匀后,得到双组份环氧树脂混合溶液;以及向所述双组份环氧树脂混合溶液中加入炭粉,搅拌20-40分钟,球磨1.5-2.5小时,混合均匀后,得到所述吸波浸渍胶液。
根据本发明的另一方面,还提供了一种吸波蜂窝的制备方法,所述制备方法包括:将蜂窝浸渍到上述的吸波浸渍胶液中,将浸渍有所述吸波浸渍胶液的所述蜂窝取出、固化,制得吸波蜂窝。
在上述制备方法中,将所述蜂窝在所述吸波浸渍胶液中浸渍4~6分钟,取出,吹去所述蜂窝孔格壁的所述吸波浸渍胶液,在80~120℃的温度下固化1~2小时,制得所述吸波蜂窝。
在上述制备方法中,所述蜂窝为芳纶蜂窝。
根据本发明的又一方面,还提供了一种由上述制备方法制备的吸波蜂窝。
本发明提供了一种吸波浸渍胶液和一种吸波蜂窝及其制备方法。本发明通过利用双组份环氧树脂、溶剂、聚醚类硅氧烷、吸波剂炭粉制得吸波胶液,其中,所述双组份环氧树脂与所述溶剂的质量之比为1:3~1:5,所述双组份环氧树脂与所述炭粉的质量之比为3:1~6:1,并且所述吸波浸渍胶液中所述聚醚类硅氧烷的质量分数为0.05%~0.2%。用该吸波胶液浸渍蜂窝,固化,制得吸波蜂窝。本发明通过添加具有极低表面张力和具有消泡性质的聚醚类硅氧烷润湿剂来降低吸波胶液表面的张力,使其在蜂窝表面快速均匀地铺展涂覆,从而得到不堵孔、不变形且具有优异的吸波性能的吸波蜂窝材料,其可广泛地应用于航空航天,飞机、雷达罩等领域。
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。
图1是根据本发明实施例的制备吸波浸渍胶液的流程图。
图2是根据本发明实施例的制备吸波蜂窝的流程图。
图3是根据本发明优选实施例的制备吸波蜂窝的整体流程图。
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员所获得的所有其他实施例,都属于本发明保护的范围。
本发明提供的吸波浸渍胶液和吸波蜂窝的制备方法,包括以下步骤:
吸波浸渍胶液的制备:
如图1中的步骤S101所示,将双组份环氧树脂用溶剂溶解后,加入润湿剂,混合均匀后,得到混合物。在该步骤中,双组份环氧树脂与溶剂的质量之比为1:3~1:5,在1600转/分钟~2000转/分钟的搅拌速率下搅拌8~12分钟,优选地,在1800转/分钟的搅拌速率下搅拌10分钟,混合均匀后得到所述混合物。其中,溶剂为乙醇、乙酸乙酯、丙酮、丁酮、丙醇甲醚的一种或多种的组合。润湿剂为聚醚硅氧烷润湿剂A-008、聚醚类硅氧烷润湿剂A-004或聚醚类硅氧烷润湿剂W-23中的一种或多种的组合,并且吸波浸渍胶液中聚醚类硅氧烷的质量份数为0.05%~0.2%。其中,双组份环氧树脂包括环氧树脂和固化剂,其中,环氧树脂包括双酚A型环氧树脂、双酚F型环氧树脂或者它们的混合物,固化剂包括:二乙烯三胺、三乙烯四胺或四乙烯五胺中的一种或者多种的组合。双组份环氧树脂中所述环氧树脂和所述固化剂的质量比为100:5~100:20。
如图1中的步骤S102所示,向混合物中加入吸波剂炭粉,混合均匀后球磨,得到吸波胶液。在该步骤中,双组份环氧树脂与炭粉的质量之比为3:1~6:1,搅拌20~40分钟混合均匀后,倒入球磨罐中球磨1.5~2.5小时,优选地,搅拌30分钟混合均匀后,倒入球磨罐中球磨2小时,得到吸波浸渍胶液。
吸波蜂窝的制备:
如图2中的步骤S103所示,将蜂窝浸渍到在步骤S102中制备的吸波浸渍胶液中,在该步骤中,将所述蜂窝在所述吸波胶液中浸渍4~6分钟,优选地,浸渍5分钟。
如图2中的步骤S104所示,将浸渍有所述吸波浸渍胶液的所述蜂窝取出、固化,制得吸波蜂窝。在该步骤中,将浸渍有所述吸波浸渍胶液的所述蜂窝取出,吹去所述蜂窝孔格壁的所述胶液,在烘箱中在80~120℃的温度下固化1~2小时,制得所述吸波蜂窝。其中,蜂窝为芳纶蜂窝。
图3是根据本发明优选实施例的制备吸波蜂窝的整体流程图。具体地,在步骤S105中,将双组份环氧树脂用溶剂溶解后,加入聚醚类硅氧烷润湿剂,得到双组份环氧树脂混合物;在步骤S106中,向双组份环氧树脂混合物中加入碳粉,搅拌20-40分钟,球磨1.5-2.5小时,混合均匀后球磨,得到吸波浸渍胶液;在步骤107中,将蜂窝浸渍到吸波浸渍胶液中,将浸渍有所述吸波浸渍胶液的所述蜂窝取出、固化,制得吸波蜂窝。上述步骤中的具体的操作工艺参见图1和图2中的相应步骤。
本发明提供的吸波蜂窝的制备方法,通过利用双组份环氧树脂、溶剂、润湿剂、炭粉制得吸波胶液,用该吸波胶液浸渍蜂窝,固化,制得吸波蜂窝。通过该方法制备的吸波胶液可以均匀地涂覆于蜂窝表面,因此,所制备的吸波蜂窝不堵孔、不变形且具有优异的吸波性能,可广泛地应用于航空航天领域,飞机、雷达罩等领域。
实施例1
将100g双组份环氧树脂用400g乙醇溶解后,加入0.5g聚醚类硅氧烷润湿剂A-008,在1600转/分钟的搅拌速率下搅拌10分钟,混合均匀后得到混合物。向混合物中加入20g吸波剂炭粉,搅拌30分钟混合均匀后,倒入球磨罐中球磨2小时,得到吸波胶液,其中,双组份环氧树脂包括双酚A型环氧树脂和固化剂,固化剂为二乙烯三胺,双组份环氧树脂中,环氧树脂和所述固化剂的质量比为20:1。
将芳纶蜂窝在吸波胶液中浸渍5分钟,取出,吹去芳纶蜂窝的孔格壁中的所述胶液,在烘箱中在80℃的温度下固化1小时,制得所述吸波蜂窝。
实施例2
将100g双组份环氧树脂用400g乙酸乙酯溶解后,加入1g聚醚类硅氧烷润湿剂A-008,在2000转/分钟的搅拌速率下搅拌10分钟,混合均匀后得到混合物。向混合物中加入20g吸波剂炭粉,搅拌30分钟混合均匀后,倒入球磨罐中球磨2小时,得到吸波胶液,其中,双组份环氧树脂包括双酚F型环氧树脂和固化剂,固化剂为三乙烯四胺。双组份环氧树脂中环氧树脂和固化剂的质量比为5:1。
将芳纶蜂窝在吸波胶液中浸渍5分钟,取出,吹去芳纶蜂窝的孔格壁中的所述胶液,在烘箱中在120℃的温度下固化2小时,制得所述吸波蜂窝。
实施例3
将100g份双组份环氧树脂用400g丙酮溶解后,加入0.5g聚醚硅氧烷润湿剂A-008,在1800转/分钟的搅拌速率下搅拌10分钟,混合均匀后得到混合物。向混合物中加入20g吸波剂炭粉,搅拌30分钟混合均匀后,倒入球磨罐中球磨2小时,得到吸波胶液,其中,双组份环氧树脂包括双酚A型环氧树脂和固化剂,固化剂为四乙烯五胺。双组份环氧树脂中环氧树脂和固化剂的质量比为10:1。
将芳纶蜂窝在吸波胶液中浸渍5分钟,取出,吹去芳纶蜂窝的孔格壁中的所述胶液,在烘箱中在100℃的温度下固化1.5小时,制得吸波蜂窝。
实施例4
将100g双组份环氧树脂用400g丁酮溶解后,加入0.5g聚醚硅氧烷润湿剂W-23,在1700转/分钟的搅拌速率下搅拌10分钟,混合均匀后得到混合物。向混合物中加入20g吸波剂炭粉,搅拌30分钟混合均匀后,倒入球磨罐中球磨2小时,得到吸波胶液,其中,双组份环氧树脂包括双酚A型环氧树脂和固化剂,固化剂为三乙烯四胺。双组份环氧树脂中环氧树脂和固化剂的质量比为15:1。
将芳纶蜂窝在吸波胶液中浸渍5分钟,取出,吹去芳纶蜂窝的孔格壁中的所述胶液,在烘箱中在85℃的温度下固化2小时,制得所述吸波蜂窝。
实施例5
将100g双组份环氧树脂用300g丙醇甲醚溶解后,加入0.425g聚醚硅氧烷润湿剂A-004,在1900转/分钟的搅拌速率下搅拌8分钟,混合均匀后得到混合物。向混合物中加入25g吸波剂炭粉,搅拌20分钟混合均匀后,倒入球磨罐中球磨2.5小时,得到吸波胶液,其中,双组份环氧树脂包括双酚F型环氧树脂和固化剂,固化剂为四乙烯五胺。双组份环氧树脂中环氧树脂和固化剂的质量比为12:1。
将芳纶蜂窝在吸波胶液中浸渍6分钟,取出,吹去芳纶蜂窝的孔格壁中的所述胶液,在烘箱中在110℃的温度下固化1.5小时,制得所述吸波蜂窝。
实施例6
将100g双组份环氧树脂用450g丙醇甲醚溶解后,加入0.8聚醚类硅氧烷润湿剂A-008,在1700转/分钟的搅拌速率下搅拌12分钟,混合均匀后得到混合物。向混合物中加入18g吸波剂炭粉,搅拌25分钟混合均匀后,倒入球磨罐中球磨2.5小时,得到吸波胶液,其中,双组份环氧树脂包括双酚A型环氧树脂和固化剂,固化剂为三乙烯四胺。双组份环氧树脂中环氧树脂和固化剂的质量比为8:1。
将芳纶蜂窝在吸波胶液中浸渍4分钟,取出,吹去芳纶蜂窝的孔格壁中的所述胶液,在烘箱中在100℃的温度下固化1小时,制得所述吸波蜂窝。
实施例7
将100g双组份环氧树脂用500g丁酮溶解后,加入0.8g聚醚硅氧烷润湿剂,在1700转/分钟的搅拌速率下搅拌12分钟,混合均匀后得到混合物。向混合物中加入30g吸波剂炭粉,搅拌40分钟混合均匀后,倒入球磨罐中 球磨1.5小时,得到吸波胶液,其中,双组份环氧树脂包括双酚A型环氧树脂和固化剂,固化剂为三乙烯四胺。双组份环氧树脂中环氧树脂和固化剂的质量比为18:1。
将芳纶蜂窝在吸波胶液中浸渍5分钟,取出,吹去芳纶蜂窝的孔格壁中的所述胶液,在烘箱中在85℃的温度下固化2小时,制得所述吸波蜂窝。
对实施例1至实施例7中制备得到的吸波胶液通过吊片方法进行表面张力测试,测试结果如下:
表1 表面张力测试结果
结果显示:上述实施例的技术方案可以实现吸波胶液的较低的表面张力,从而可以实现在吸波胶液在蜂窝表面快速铺展涂覆,并且蜂窝不易堵孔。
对实施例1至实施例7中制备得到的吸波蜂窝通过微波暗室法方法进行吸波性能测试,测试结果如下:
表2 吸波性能测试结果
结果显示:上述实施例的技术方案所提供的吸波蜂窝具有优异的吸波性能。
可见,本发明提供了一种吸波浸渍胶液和一种吸波蜂窝及其制备方法,通过利用双组份环氧树脂、溶剂、润湿剂、炭粉制得吸波胶液,用该吸波胶液浸渍蜂窝,固化,制得吸波蜂窝。本发明通过添加具有极低表面张力和具有消泡性质的聚醚类硅氧烷润湿剂来降低吸波胶液表面的张力,使其在蜂窝表面快速均匀地铺展涂覆,从而得到不堵孔、不变形且具有优异的吸波性能的吸波蜂窝材料,其可广泛地应用于航空航天,飞机、雷达罩等领域。
以上仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (13)
- 一种吸波浸渍胶液,其特征在于,包括:双组份环氧树脂;溶剂;聚醚类硅氧烷;炭粉;其中,所述双组份环氧树脂与所述溶剂的质量之比为1:3~1:5,所述双组份环氧树脂与所述炭粉的质量之比为3:1~6:1,并且所述吸波浸渍胶液中所述聚醚类硅氧烷的质量分数为0.05%~0.2%。
- 根据权利要求1所述的吸波浸渍胶液,其特征在于,所述双组份环氧树脂与所述溶剂的质量之比为1:4,所述双组份环氧树脂与所述炭粉的质量之比为5:1,并且所述吸波浸渍胶液中所述聚醚类硅氧烷的质量分数为0.1%。
- 根据权利要求1所述的吸波浸渍胶液,其特征在于,所述双组份环氧树脂包括环氧树脂和固化剂,其中,所述环氧树脂包括双酚A型环氧树脂、双酚F型环氧树脂或者它们的混合物,所述固化剂包括:二乙烯三胺、三乙烯四胺或四乙烯五胺中的一种或者多种的组合。
- 根据权利要求3所述的吸波浸渍胶液,其特征在于,所述双组份环氧树脂中所述环氧树脂和所述固化剂的质量比为100:5~100:20。
- 根据权利要求4所述的吸波浸渍胶液,其特征在于,所述双组份环氧树脂中所述环氧树脂和所述固化剂的质量比为10:1。
- 根据权利要求1所述的吸波浸渍胶液,其特征在于,所述溶剂为甲醇、乙醇、乙酸乙酯、丙酮、丁酮或丙醇甲醚的一种或多种的组合。
- 根据权利要求1所述的吸波浸渍胶液,其特征在于,所述聚醚类硅氧烷为聚醚类硅氧烷润湿剂A-008h、聚醚类硅氧烷润湿剂A-004h或聚醚类硅氧烷润湿剂W-23h中的一种或多种的组合。
- 一种应用权利要求1-7任一项所述的吸波浸渍胶液的吸波浸渍胶液制备方法,其特征在于,所述制备方法包括:将所述双组份环氧树脂用所述溶剂溶解后,加入所述聚醚类硅氧烷进行润湿,混合均匀后,加入所述炭粉,混合均匀后,得到所述吸波浸渍胶液。
- 根据权利要求8所述的制备方法,其特征在于,所述制备方法包括:将所述双组份环氧树脂用所述溶剂溶解后,加入所述聚醚类硅氧烷润湿剂进行润湿,高速搅拌8-12分钟混合均匀后,得到双组份环氧树脂混合溶液;以及向所述双组份环氧树脂混合溶液中加入所述炭粉,搅拌20-40分钟,球磨1.5-2.5小时,混合均匀后,得到所述吸波浸渍胶液。
- 一种吸波蜂窝的制备方法,其特征在于,所述制备方法包括:将蜂窝浸渍到权利要求1-9中任一项所述的吸波浸渍胶液中,将浸渍有所述吸波浸渍胶液的所述蜂窝取出、固化,制得吸波蜂窝。
- 根据权利要求10所述的制备方法,其特征在于,将所述蜂窝在所述吸波浸渍胶液中浸渍4~6分钟,取出,吹去所述蜂窝孔格壁的所述吸波浸渍胶液,在80~120℃的温度下固化1~2小时,制得所述吸波蜂窝。
- 根据权利要求10所述的制备方法,其特征在于,所述蜂窝为芳纶蜂窝。
- 一种根据权利要求10-12任一项所述的制备方法制备的吸波蜂窝。
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US20200115598A1 (en) | 2020-04-16 |
JP7090697B2 (ja) | 2022-06-24 |
EP3620490A4 (en) | 2021-01-13 |
JP2020521869A (ja) | 2020-07-27 |
CN108997711A (zh) | 2018-12-14 |
US11866616B2 (en) | 2024-01-09 |
CN108997711B (zh) | 2023-04-07 |
EP3620490A1 (en) | 2020-03-11 |
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