CN118006124A - Prepreg for preparing composite antenna housing, composite antenna housing and preparation method thereof - Google Patents
Prepreg for preparing composite antenna housing, composite antenna housing and preparation method thereof Download PDFInfo
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- CN118006124A CN118006124A CN202410419015.5A CN202410419015A CN118006124A CN 118006124 A CN118006124 A CN 118006124A CN 202410419015 A CN202410419015 A CN 202410419015A CN 118006124 A CN118006124 A CN 118006124A
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- 239000002131 composite material Substances 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 147
- 239000011347 resin Substances 0.000 claims abstract description 98
- 229920005989 resin Polymers 0.000 claims abstract description 98
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 claims abstract description 90
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 84
- 239000000463 material Substances 0.000 claims abstract description 72
- 239000011521 glass Substances 0.000 claims abstract description 69
- 239000011324 bead Substances 0.000 claims abstract description 63
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 53
- 239000012745 toughening agent Substances 0.000 claims abstract description 51
- 239000011159 matrix material Substances 0.000 claims abstract description 43
- 239000000835 fiber Substances 0.000 claims abstract description 36
- 239000010453 quartz Substances 0.000 claims abstract description 29
- 239000012779 reinforcing material Substances 0.000 claims abstract description 14
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims description 44
- 239000004831 Hot glue Substances 0.000 claims description 28
- HCNHNBLSNVSJTJ-UHFFFAOYSA-N 1,1-Bis(4-hydroxyphenyl)ethane Chemical compound C=1C=C(O)C=CC=1C(C)C1=CC=C(O)C=C1 HCNHNBLSNVSJTJ-UHFFFAOYSA-N 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 21
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 20
- 238000004519 manufacturing process Methods 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 12
- 238000007598 dipping method Methods 0.000 claims description 11
- 239000002313 adhesive film Substances 0.000 claims description 10
- 238000000465 moulding Methods 0.000 claims description 9
- 239000004643 cyanate ester Substances 0.000 claims description 8
- 239000012943 hotmelt Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000012360 testing method Methods 0.000 claims description 7
- 238000005498 polishing Methods 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 5
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- 229920001971 elastomer Polymers 0.000 claims description 4
- 229920005992 thermoplastic resin Polymers 0.000 claims description 4
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 claims description 3
- 238000010030 laminating Methods 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 abstract description 10
- 238000011161 development Methods 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 26
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- 239000000377 silicon dioxide Substances 0.000 description 6
- 239000003292 glue Substances 0.000 description 5
- 238000002834 transmittance Methods 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
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- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical group C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
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- DXCXWVLIDGPHEA-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-3-[(4-ethylpiperazin-1-yl)methyl]pyrazol-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C=1C(=NN(C=1)CC(=O)N1CC2=C(CC1)NN=N2)CN1CCN(CC1)CC DXCXWVLIDGPHEA-UHFFFAOYSA-N 0.000 description 1
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- Details Of Aerials (AREA)
Abstract
The invention provides a prepreg for preparing a composite material radome, the composite material radome and a preparation method thereof, wherein the prepreg for preparing the composite material radome comprises a resin matrix and a reinforcing material; the reinforcing material is quartz fiber; the resin matrix comprises the following components in parts by weight: 50-100 parts of cyanate, 10-65 parts of hollow glass beads, 0.5-2 parts of nano silicon dioxide and 2-12 parts of toughening agent. The radome prepared from the prepreg meets the development requirements of light weight, low dielectric wave transmission requirement and bearing strength of wave transmission materials.
Description
Technical Field
The invention belongs to the technical field of wave-transparent radomes, and particularly relates to a prepreg for preparing a composite material radome, the composite material radome and a preparation method thereof.
Background
Radomes are structures that protect the antenna system from the external environment. It is required to have good electromagnetic wave transmission characteristics in terms of electrical performance and to withstand the action of an external severe environment in terms of mechanical performance. The composite material radome is formed by compounding reinforcing fibers and a resin matrix. The quartz fiber has excellent wave-transmitting performance and can be used as a reinforcing fiber for preparing radomes. The Cyanate (CE) has excellent mechanical properties, heat resistance and humidity resistance, and has stable and extremely low epsilon (2.8-3.2) and tg delta (0.002, 0.006) in a very wide temperature range (160-220 ℃) and frequency range (10 4 -10 square Hz). More and more autonomously synthesized cyanate ester compounds are being applied to various occasions with high requirements on electromagnetic performance, such as wave-transparent radomes, stealth wave-transparent functional layers and the like of aerospace and ships.
At present, the dielectric constant of the quartz fiber reinforced cyanate composite material used for the wave-transparent functional layer is generally more than 3.1, and the density is about 1.8g/cm 3. Because the antenna is usually placed in an open air environment, the antenna is directly affected by various external factors in the natural world, so that the accuracy of the antenna is reduced, the service life is shortened and the reliability is deteriorated. In some environments with severe conditions, such as underwater, air pressure and the like, the radome is required to have high pressure resistance and ensure the accuracy and reliability of the internal antenna. However, the existing radome wave-transmitting functional layer generally cannot have low dielectric, light weight and pressure resistance, so that the requirements of wave transmission, light weight of equipment and underwater pressure resistance cannot be met. The Chinese patent document with publication number CN 108481763A discloses a broadband wave-transparent low-dielectric antenna housing material and a rapid preparation method thereof, wherein the antenna housing is obtained by taking quartz fiber cloth as a reinforcing material, taking cyanate as a resin matrix and carrying out compression molding. The dielectric constant of the radome can reach about 2.5, the density is about 1.4 g/cm 3, but the pressure resistance is insufficient, and the pressure resistance requirements of environments with severe conditions such as underwater, air pressure and the like can not be met.
Disclosure of Invention
The invention solves the technical problem of providing a prepreg for preparing a composite material radome, the composite material radome and a preparation method thereof, and meets the development requirements of light weight, low dielectric wave transmission requirements and bearing strength of wave transmission materials.
In order to solve the above problems, a first aspect of the present invention provides a prepreg for preparing a composite radome, comprising a resin matrix and a reinforcing material; the reinforcing material is quartz fiber; the resin matrix comprises the following components in parts by weight: 50-100 parts of cyanate, 10-65 parts of hollow glass beads, 0.5-2 parts of nano silicon dioxide and 2-12 parts of toughening agent.
Preferably, the resin matrix comprises the following components in parts by weight: 55-90 parts of cyanate, 10-41 parts of hollow glass beads, 0.5-2 parts of nano silicon dioxide and 3.7-10 parts of toughening agent.
Preferably, the ratio of the total mass of the cyanate ester and the toughening agent to the total mass of the nano silicon dioxide and the hollow glass beads is 3-9:3.
Preferably, the mass content of the resin matrix in the prepreg is 30-45%
Preferably, the cyanate is one or a mixture of more of tetramethyl bisphenol F type cyanate, bisphenol E type cyanate and dicyclopentadiene type cyanate; the cyanate resin is a prepolymer, and the viscosity of the cyanate resin is 3000-15000 mPa.s at 80 ℃.
Preferably, the particle size of the hollow glass beads is 30-120 mu m, the wall thickness is 1-4 mu m, and the density is 0.1-0.7 g/m 3.
Preferably, the particle size of the nano silicon dioxide is 20-100 nm; the toughening agent is one or a mixture of more of rubber and thermoplastic resin.
The second aspect of the invention provides a composite antenna housing, which is prepared from the prepreg for preparing the composite antenna housing.
The third aspect of the present invention provides a method for manufacturing the composite radome, which comprises the following steps:
s1, mixing the cyanate, the hollow glass beads, the nano silicon dioxide and the toughening agent to obtain a mixture;
S2, preparing the mixture into a hot melt adhesive film;
s3, laminating quartz fibers and the hot melt adhesive film, and melting and dipping the hot melt adhesive film on the quartz fibers to obtain prepreg;
S4, arranging the prepreg on a die of the radome, and performing curing molding to obtain the composite material radome.
Preferably, the step S1 specifically includes the following steps:
Heating and blending the cyanate and the toughening agent to obtain a material A, and testing the viscosity of the material A to ensure that the viscosity of the material A is 3000 mPas-5000 mPas at 70 ℃; mixing the nano silicon dioxide and the hollow glass beads to obtain a material B; and then mixing the material A with the material B to obtain the mixture.
Preferably, step S2 specifically includes the following steps:
Preparing the mixture into a hot melt adhesive film by adopting a hot melt prepreg machine; the temperature of the hot melt prepreg machine gum dipping roller is 75-85 ℃, the traction rate of conveying release paper is 3-6 m/min, and the unit mass of the hot melt adhesive film reaches the required prepreg resin content by adjusting the distance between the gum dipping rollers.
Preferably, in step S4, the curing and forming of the radome is performed in several times, the thickness of the radome is not greater than 10mm each time, polishing is performed on the surface of the product formed in the previous time before the latter time, a layer of cyanate adhesive film is laid, and then prepreg is set for curing again until the target thickness is reached.
Compared with the prior art, the invention has the following beneficial effects:
The prepreg for preparing the composite antenna housing takes the quartz fiber as the reinforcing material, and the quartz fiber has excellent wave-transmitting performance; the cyanate is used as a resin matrix, has excellent mechanical property, heat resistance and damp-heat resistance, and has stable and extremely low dielectric constant; and hollow glass beads, nano silicon dioxide and a toughening agent are added into the resin matrix, and the excellent comprehensive performance of the prepreg is endowed by introducing a third phase of filler. The hollow glass beads introduced have the advantages of light weight, low dielectric property and the like, can reduce the density of the composite material radome, and meet the requirement of light weight of equipment; the nano silicon dioxide has the functions of thickening and reducing resin defects, and the nano silicon dioxide is easy to fill the air hole defects of the prepreg composite material product, so that the mechanical property of the composite material product is improved; the toughening agent can improve the toughness of the resin, thereby improving the mechanical property of the composite material product. In addition, the resin components and the proportions are adopted, the resin matrix can meet the requirements of a hot melt adhesive film method prepreg preparation process, the resin content in the prepreg can be controlled more accurately by the hot melt adhesive film method prepreg, the high performance of the prepreg is ensured, and the production cost is lower.
The prepreg for preparing the composite material radome has the advantages that the density of the prepared composite material laminated board is 1.3-1.8 g/cm 3, the dielectric constant (2-18 GHz) is 2.5-3.1, the design can be adjusted, and the prepreg can meet various task requirements, such as gradient dielectric composite material radomes. The pressure-resistant radome prepared by the prepreg has the wave transmittance of more than or equal to 80 percent, the thickness of 8-35mm and the pressure-resistant strength of more than or equal to 6MPa in the X wave band and the Ku wave band, and solves the problem that the general radome cannot achieve both the wave transmittance performance and the pressure-resistant mechanical strength.
Drawings
Fig. 1 is a schematic structural view of an inverted U-shaped radome according to embodiments 8-10 of the present invention;
fig. 2 is a schematic structural view of a radome having a flat plate structure according to embodiments 11 to 13 of the present invention.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
At present, the existing radome generally cannot simultaneously have low dielectric, light weight and pressure resistance, so that the requirements of wave transmission, light weight of equipment and underwater pressure resistance cannot be met.
To this end, one aspect of an embodiment of the present invention provides a prepreg for preparing a composite radome, comprising a resin matrix and a reinforcing material; the reinforcing material is quartz fiber; the resin matrix comprises the following components in parts by weight: 50-100 parts of cyanate, 10-65 parts of hollow glass beads, 0.5-2 parts of nano silicon dioxide and 2-12 parts of toughening agent.
The prepreg for preparing the composite material radome takes the quartz fiber as the reinforcing material, and the quartz fiber has excellent wave-transmitting performance; the cyanate is used as a resin matrix, has excellent mechanical property, heat resistance and damp-heat resistance, and has stable and extremely low dielectric constant; and hollow glass beads, nano silicon dioxide and a toughening agent are added into the resin matrix, and the excellent comprehensive performance of the prepreg is endowed by introducing a third phase of filler. The hollow glass beads introduced have the advantages of light weight, low dielectric property and the like, can reduce the density of the composite material radome, and meet the requirement of light weight of equipment; the nano silicon dioxide has the functions of thickening and reducing resin defects, and the nano silicon dioxide is easy to fill the air hole defects of the prepreg composite material product, so that the mechanical property of the composite material product is improved; the toughening agent can improve the toughness of the resin, thereby improving the mechanical property of the composite material product. In addition, the resin components and the proportions are adopted, the resin matrix can meet the requirements of a hot melt adhesive film method prepreg preparation process, the resin content in the prepreg can be controlled more accurately by the hot melt adhesive film method prepreg, the high performance of the prepreg is ensured, and the production cost is lower.
Preferably, the resin matrix comprises the following components in parts by weight: 55-90 parts of cyanate, 10-41 parts of hollow glass beads, 0.5-2 parts of nano silicon dioxide and 3.7-10 parts of toughening agent. By adopting the proportion of the parts by weight, the composite material prepared by the prepreg can have the quality, dielectric property and mechanical property which are more in line with the application requirements of the radome.
In some embodiments, the mixing of cyanate ester and toughening agent as material a and the mixing of nano silica and hollow glass microspheres as material B, the mass ratio between material a and material B can affect the performance of the resulting composite radome in various aspects. As a preferable implementation mode, the ratio of the total mass of cyanate ester and the toughening agent to the total mass of the nano silicon dioxide and the hollow glass microsphere is 3-9:3. In the range of the proportion, the composite antenna housing has quality, dielectric property and mechanical property which meet the requirements better. More preferably, the ratio of the total mass of cyanate and the toughening agent to the total mass of the nano silicon dioxide and the hollow glass beads is 6-9:3. Most preferably, the ratio of the total mass of cyanate ester and toughening agent to the total mass of nano silica and hollow glass microsphere is 7:3. Under the proportion, the obtained composite material radome has the best comprehensive performance and best meets the requirement of the use environment of the radome.
In some embodiments, the mass content of the resin matrix in the prepreg may affect the mechanical properties of the composite radome, preferably the mass content of the resin matrix in the prepreg is 30% -45%.
In some embodiments, the cyanate ester is selected from the cyanate ester classes having a dielectric constant of less than 3.0. Preferably, the cyanate is one or a mixture of more of tetramethyl bisphenol F type cyanate, bisphenol E type cyanate and dicyclopentadiene type cyanate.
Preferably, the cyanate resin is a prepolymer, and the cyanate resin has a viscosity of 3000 to 15000 mPa.s at 80 ℃. In the viscosity range, the property of the obtained resin matrix composition can meet the requirements of a hot melt adhesive film method prepreg preparation process.
In some embodiments, the specific form of the reinforcing material quartz fibers is not limited, and quartz fiber cloth, quartz fiber yarn, or other types of fiber fabrics may be employed. Preferably, quartz fiber cloth is adopted as quartz fiber cloth, specifically, the quartz fiber cloth is high-purity plain weave or twill quartz fiber cloth, and the silicon dioxide purity is more than or equal to 99.9 percent.
In some embodiments, the particle size of the hollow glass microspheres can directly affect the uniformity of the distribution of the fillers in the resin. Preferably, the particle size of the hollow glass beads is 30-120 mu m, further preferably, the particle size of the hollow glass beads is 30-60 mu m, and the hollow glass beads with the particle size range are beneficial to the dispersion of the hollow glass beads in the cyanate resin and ensure the moderate viscosity of the resin. The wall thickness of the hollow glass beads can directly influence the strength and the density of the hollow glass beads, preferably, the wall thickness of the hollow glass beads is 1-4 mu m, and the wall thickness range can reduce the density of the composite material radome to the greatest extent while ensuring the strength of the composite material radome. Preferably, the density of the hollow glass beads is 0.1-0.7 g/m 3. Preferably hollow glass microspheres with high silica purity.
In some embodiments, the particle size of the nanosilica can affect its uniformity of distribution in the resin matrix, as well as the effectiveness of the nanosilica to fill the pore defects in the resin, thereby affecting the mechanical properties of the composite article. Preferably, the particle size of the nano silicon dioxide is 20-100 nm, and the nano silicon dioxide can be uniformly distributed in the resin and can also effectively fill the air hole defects in the resin.
In some embodiments, the toughening agent acts to increase the toughness of the resin matrix to improve its mechanical properties. Preferably, the toughening agent is one or a mixture of several of rubber and thermoplastic resin. The cyanate resin has excellent electrical property due to the regular triazine ring structure, and adopts a rubber toughening agent or a thermoplastic resin toughening agent, the toughening mechanism is phase separation toughening, and the toughening principle does not damage the triazine ring structure after the cyanate resin is cured, so that the electrical property structure of the cyanate resin can be reserved, the dielectric loss tangent of the resin matrix is not increased after the resin matrix is modified by the toughening agent, and the mechanical property of the prepreg is improved, and meanwhile, the low dielectric property of the prepreg is ensured. Preferably, the toughening agent is one or more of nitrile rubber, acrylic resin and fluorocarbon resin.
The prepreg for preparing the composite material radome provided by the embodiment of the invention has the advantages that the density of the prepreg laminated plate is in the range of 1.3-1.8 g/cm 3, the dielectric constant is designed and adjustable in the range of 2.5-3.1 at 2-18 GHz, and various task requirements such as gradient dielectric composite material radomes can be met. The wave transmittance of the radome prepared by the prepreg in the X wave band is more than or equal to 80%, the thickness is 20-35mm, and the pressure resistance is more than or equal to 6MPa. The problem that the general radome cannot achieve both wave transmission performance and compressive mechanical strength is solved.
The second aspect of the embodiment of the invention provides a composite antenna housing, which is prepared from the prepreg for preparing the composite antenna housing.
In some embodiments, the shape of the composite radome may be inverted U-shaped or flat, and may be adjusted according to actual needs.
In some embodiments, the thickness of the composite radome is 8-35mm, and can be adjusted according to actual needs.
Another aspect of the embodiments of the present invention provides a method for manufacturing the composite radome, including the following steps:
s1, mixing the cyanate, the hollow glass beads, the nano silicon dioxide and the toughening agent to obtain a mixture;
S2, preparing the mixture into a hot melt adhesive film;
s3, laminating quartz fibers and the hot melt adhesive film, and melting and dipping the hot melt adhesive film on the quartz fibers to obtain prepreg;
S4, arranging the prepreg on a die of the radome, and performing curing molding to obtain the lightweight and pressure-resistant composite material radome.
According to the preparation method of the light and pressure-resistant composite antenna housing, provided by the embodiment of the invention, the prepreg is prepared by adopting the hot melt adhesive film method, the resin content in the prepreg can be accurately controlled, and the preparation method is simple and low in cost.
In some embodiments, to improve the mixing uniformity of the components in the resin matrix, step S1 specifically includes the following steps:
Heating and blending the cyanate and the toughening agent to obtain a material A; mixing the nano silicon dioxide and the hollow glass beads to obtain a material B; and then mixing the material A with the material B to obtain the mixture.
Wherein, the mixing speed of the material A and the material B is lower than 100 revolutions per minute, and the hollow glass beads are prevented from being smashed by an excessively fast stirring paddle. After the hollow glass beads are wetted with the resin, the hollow glass beads can be uniformly dispersed in the resin after being stirred and blended for 10 min.
In some embodiments, after obtaining the material A, the viscosity of the material A is also tested, ensuring that the viscosity of the material A is 3000 mPas to 5000 mPas at 70 ℃. The adhesive has low viscosity and good fluidity, and is not easy to form a film on a glue spreader. Too high a viscosity, poor flowability and poor wetting effect of the resin on the fibers. When the viscosity is adopted, the hot-melt prepreg process can be conveniently implemented, and the fiber is conveniently coated while the film forming property is realized.
In some embodiments, step S2 specifically includes the steps of:
Preparing the mixture into a hot melt adhesive film by adopting a hot melt prepreg machine; the temperature of the hot melt prepreg machine gum dipping roller is 75-85 ℃, preferably 80 ℃; the traction rate of the conveying release paper is 3-6 m/min, preferably 4m/min, and the unit mass of the hot melt adhesive film reaches the required prepreg resin content by adjusting the distance between the dipping rollers.
Specifically, firstly, the gap between a metering roller and a coating roller of a hot melt prepreg machine is adjusted according to the unit area mass of a glue film, the width of the glue film is correspondingly adjusted according to the width of the prepreg, and two ends of the metering roller and the coating roller are provided with glue blocking plates and scrapers.
In some embodiments, step S3 specifically includes the steps of:
Quartz fibers on an unreeling device are led out under the action of a certain tension, flattened by a flattening roller, pressed together with a prepared hot melt adhesive film, melted and impregnated in the fibers by a heating roller with the temperature controlled between 60 and 80 ℃, cooled, added with a PE film and rolled to prepare the prepreg. The heated roll temperature is preferably 70 ℃.
In some embodiments, in step S4, the curing and molding is accomplished using a hot press or autoclave.
In some embodiments, in step S4, the curing process is: curing for 1h at 130 ℃, then curing for 1h at 150 ℃, then curing for 1h at 180 ℃, and finally curing for 2h at 200 ℃, wherein the molding pressure is 2-6 MPa.
In some embodiments, in step S4, the curing and molding of the radome is performed in several times, the thickness of the radome is not greater than 10mm each time, polishing is performed on the surface of the product formed in the previous time before the latter time, a layer of cyanate adhesive film is laid, and then prepreg is set again to cure again until the target thickness is reached. The curing quality of the product can be ensured through multiple curing, the defects of the product are reduced, and the defects of heating and pressing of large-thickness curing and uneven glue discharge of the prepreg are avoided.
Example 1
The prepreg of the radome of the embodiment comprises a resin matrix and a reinforcing material; the mass content of the resin matrix is 37%; the reinforcing material is high-purity plain quartz fiber cloth, and the purity of silicon dioxide is more than or equal to 99.9%; the resin matrix comprises the following components in parts by weight: 56.8 parts of tetramethyl bisphenol F cyanate, 2.85 parts of bisphenol E cyanate resin, 2.85 parts of acrylic resin toughening agent, 2 parts of nano silicon dioxide and 60.5 parts of hollow glass beads. Wherein the particle size of the hollow glass beads is 30-60 mu m, the wall thickness is 1-4 mu m, and the density is 0.1-0.7 g/m 3. The particle size of the nano silicon dioxide is 20-100 nm. Tetramethyl bisphenol F cyanate, bisphenol E cyanate resin and a toughening agent form a material A, nano silicon dioxide and hollow glass beads form a material B, and in the embodiment, the material A: the material B is 1:1.
The preparation method of the composite material radome of the embodiment comprises the following steps:
(1) Heating tetramethyl bisphenol F cyanate, bisphenol E cyanate resin and a toughening agent to 80 ℃, and putting the materials into a stainless steel container according to the mass part ratio of the materials to be mixed to obtain a material A, and testing the viscosity of the material A at 70 ℃ by using a rheometer to ensure that the testing result is within the range of 3000 mPa.s-5000 mPa.s; uniformly mixing and stirring nano silicon dioxide and hollow glass beads according to the mass part ratio of the nano silicon dioxide and the hollow glass beads to obtain a material B; and mixing the material A and the material B according to the mass ratio of 7:3, wherein the mixing speed is lower than 100 revolutions per minute, the hollow glass beads are prevented from being smashed by an excessively fast stirring paddle, and the hollow glass beads are uniformly dispersed in the resin after being wetted with the resin by stirring and blending for 10 minutes, so that the mixture is obtained.
(2) And preparing the mixture into a hot melt adhesive film by a hot melt adhesive film presoaking machine. The gap between the metering roller and the coating roller of the hot melt adhesive film presoaking machine is adjusted according to the unit area quality of the hot melt adhesive film, the width of the adhesive film is correspondingly adjusted according to the width of the prepreg, and two ends of the metering roller and the coating roller are provided with adhesive blocking plates and scrapers. The temperature of a gum dipping roller of the hot melting presoaking machine is controlled to be 80 ℃, the traction rate of conveying release paper is 4m/min, the distance between the gum dipping rollers is adjusted, and the thickness is detected by a beta-ray instrument, so that the unit mass of a resin film meets the requirement of the resin content of the presoaked material. The hot melt adhesive film with the adhesive film surface density of 32+/-5 g/cm 2 is obtained.
(3) And (3) leading out the quartz fiber cloth on the unreeling device under the action of a certain tension, wherein the thickness of a cloth layer of the quartz fiber cloth is 0.1mm, the surface density is 106+/-5 g/cm 2, flattening by a flattening roller, pressing the quartz fiber cloth with a prepared hot melt adhesive film, melting and impregnating a resin matrix in the fiber by a heating roller with the temperature controlled at 70 ℃, and cooling, adding a PE film and reeling to prepare the prepreg. The areal density of the prepreg was 164.+ -.10 g/cm 2 and the gel content was 37%.
(4) The prepared prepreg is paved on a radome mould coated with a release agent, 300 layers are paved according to the thickness of 0.1mm of each layer, and a radome with the thickness of 30mm is obtained, specifically, the radome is not more than 10mm in each forming thickness, namely, when in first forming, 100 layers of prepreg are paved, then the mould or other auxiliary materials are covered, the prepreg is cured and formed in hot pressing, when in second forming, the outer surface of the first forming is polished, a layer of cyanate adhesive film is paved, then 100 layers of prepreg are paved, and the prepreg is cured again until the target thickness is reached, and the prepreg is cured for 3 times in 30 mm. The curing process comprises the following steps: curing at 130 ℃ for 1h, then curing at 150 ℃ for 1h, then curing at 180 ℃ for 1h, and finally curing at 200 ℃ for 2h, wherein the molding pressure is 5MPa.
(5) And naturally cooling the formed radome along with a furnace, and then taking out the radome from the mold to obtain the composite material radome.
Example 2
The prepreg of the radome of this embodiment differs from that of embodiment 1 in that the resin matrix includes the following components in parts by weight: 64.9 parts of tetramethyl bisphenol F cyanate, 3.25 parts of bisphenol E cyanate resin, 3.25 parts of acrylic resin toughening agent, 1.73 parts of nano silicon dioxide and 51.8 parts of hollow glass beads.
The manufacturing method of the composite radome of the embodiment is different from that of embodiment 1 in that: in the step (1), the material A mixed by the tetramethyl bisphenol F cyanate, bisphenol E cyanate resin and the toughening agent according to the mass part ratio of the material A to the nano silicon dioxide and the hollow glass beads is mixed by the material B mixed by the nano silicon dioxide and the hollow glass beads according to the mass part ratio of the material A to the material B according to the mass ratio of 4:3.
Example 3
The prepreg of the radome of this embodiment differs from that of embodiment 1 in that the resin matrix includes the following components in parts by weight: 71 parts of tetramethyl bisphenol F cyanate, 3.55 parts of bisphenol E cyanate resin, 3.55 parts of acrylic resin toughening agent, 1.51 parts of nano silicon dioxide and 45.36 parts of hollow glass beads.
The manufacturing method of the composite radome of the embodiment is different from that of embodiment 1 in that: in the step (1), the material A mixed by the tetramethyl bisphenol F cyanate, bisphenol E cyanate resin and the toughening agent according to the mass part ratio of the material A to the nano silicon dioxide and the hollow glass beads is mixed by the material B mixed by the nano silicon dioxide and the hollow glass beads according to the mass part ratio of the material A to the material B according to the mass ratio of 5:3.
Example 4
The prepreg of the radome of this embodiment differs from that of embodiment 1 in that the resin matrix includes the following components in parts by weight: 75.76 parts of tetramethyl bisphenol F cyanate, 3.79 parts of bisphenol E cyanate resin, 3.79 parts of acrylic resin toughening agent, 1.34 parts of nano silicon dioxide and 40.32 parts of hollow glass beads.
The manufacturing method of the composite radome of the embodiment is different from that of embodiment 1 in that: in the step (1), the material A mixed by the tetramethyl bisphenol F cyanate, bisphenol E cyanate resin and the toughening agent according to the mass part ratio of the material A to the nano silicon dioxide and the hollow glass beads is mixed by the material B mixed by the nano silicon dioxide and the hollow glass beads according to the mass part ratio of the material A to the material B according to the mass ratio of 2:1.
Example 5
The prepreg of the radome of this embodiment differs from that of embodiment 1 in that the resin matrix includes the following components in parts by weight: 79.5 parts of tetramethyl bisphenol F cyanate, 4 parts of bisphenol E cyanate resin, 4 parts of acrylic resin toughening agent, 1.21 parts of nano silicon dioxide and 36.29 parts of hollow glass beads.
The manufacturing method of the composite radome of the embodiment is different from that of embodiment 1 in that: in the step (1), the material A mixed by the tetramethyl bisphenol F cyanate, bisphenol E cyanate resin and the toughening agent according to the mass part ratio of the material A to the nano silicon dioxide and the hollow glass beads is mixed by the material B mixed by the nano silicon dioxide and the hollow glass beads according to the mass part ratio of the material A to the material B according to the mass ratio of 7:3.
Example 6
The prepreg of the radome of this embodiment differs from that of embodiment 1 in that the resin matrix includes the following components in parts by weight: 82.64 parts of tetramethyl bisphenol F cyanate, 4.13 parts of bisphenol E cyanate resin, 4.13 parts of acrylic resin toughening agent, 1.10 parts of nano silicon dioxide and 32.99 parts of hollow glass beads.
The manufacturing method of the composite radome of the embodiment is different from that of embodiment 1 in that: in the step (1), the material A mixed by the tetramethyl bisphenol F cyanate, bisphenol E cyanate resin and the toughening agent according to the mass part ratio of the material A to the nano silicon dioxide and the hollow glass beads is mixed by the material B mixed by the nano silicon dioxide and the hollow glass beads according to the mass part ratio of the material A to the material B according to the mass ratio of 8:3.
Example 7
The prepreg of the radome of this embodiment differs from that of embodiment 1 in that the resin matrix includes the following components in parts by weight: 85.23 parts of tetramethyl bisphenol F cyanate, 4.26 parts of bisphenol E cyanate resin, 4.26 parts of acrylic resin toughening agent, 1.01 parts of nano silicon dioxide and 30.24 parts of hollow glass beads.
The manufacturing method of the composite radome of the embodiment is different from that of embodiment 1 in that: in the step (1), the material A mixed by the tetramethyl bisphenol F cyanate, bisphenol E cyanate resin and the toughening agent according to the mass part ratio of the material A to the nano silicon dioxide and the hollow glass beads is mixed by the material B mixed by the nano silicon dioxide and the hollow glass beads according to the mass part ratio of the material A to the material B according to the mass ratio of 3:1.
Example 8
The radome prepared in this embodiment is an inverted U-shaped radome as shown in fig. 1. The radius of the arc-shaped inner surface of the inverted U-shaped structure is 184mm, the radius of the outer surface is 200mm, the height of the bottom is 300mm, and the wall thickness is 16mm.
The preparation method of the composite radome is the same as that of the embodiment 5, except that the hemispherical radome mold in the step (4) has different dimensions, 160 layers are paved according to the thickness of 0.1mm of each layer to obtain a radome with the thickness of 16mm when the prepreg is paved, the thickness of 8mm is formed each time of the radome, the surface is polished when the radome is formed for the second time, a layer of cyanate adhesive film is paved, then the prepreg is paved for curing again until the target thickness is reached, and the total curing is carried out for 2 times for 16 mm.
Example 9
The radome prepared in this embodiment is an inverted U-shaped radome as shown in fig. 1. The radius of the arc-shaped inner surface of the inverted U-shaped structure is 138mm, the radius of the outer surface is 150mm, the height of the bottom is 200mm, and the wall thickness is 12mm.
The preparation method of the composite radome is the same as that of the embodiment 5, except that the hemispherical radome mold in the step (4) has different dimensions, when the prepreg is paved, 120 layers are paved according to the thickness of 0.1mm of each layer to obtain the radome with the thickness of 12mm, the thickness of each time of forming the radome is 6mm, polishing is performed on the surface during the second forming, a layer of cyanate adhesive film is paved, then the prepreg is paved for curing again until the target thickness is reached, and the total curing is performed for 2 times for 12 mm.
Example 10
The radome prepared in this embodiment is an inverted U-shaped radome as shown in fig. 1. The radius of the arc-shaped inner surface of the inverted U-shaped structure is 92mm, the radius of the outer surface is 100mm, the height of the bottom is 150mm, and the wall thickness is 8mm.
The preparation method of the composite radome of the embodiment is the same as that of the embodiment 5, except that the hemispherical radome mold in the step (4) has different dimensions, and when the prepreg is paved, 80 layers are paved according to the thickness of 0.1mm of each layer to obtain the radome with the thickness of 8mm, and the radome is obtained by one-step curing molding.
Example 11
The radome prepared in this embodiment is a radome with a flat plate structure as shown in fig. 2. The wall thickness was 16mm.
The preparation method of the composite radome is the same as that of the embodiment 5, and the difference is that in the step (4), a flat radome mold is adopted, when the prepreg is paved, 160 layers are paved according to the thickness of 0.1mm of each layer to obtain the radome with the thickness of 16mm when the prepreg is paved, the thickness of 8mm is formed each time of the radome, polishing is carried out on the surface when the radome is formed for the second time, a layer of cyanate adhesive film is paved, then the prepreg is paved for curing again until the target thickness is reached, and the total curing is carried out for 2 times for 16 mm.
Example 12
The radome prepared in this embodiment is a radome with a flat plate structure as shown in fig. 2. The wall thickness was 12mm.
The preparation method of the composite radome is the same as that of the embodiment 5, and the difference is that in the step (4), a flat radome mold is adopted, when the prepreg is paved, 120 layers are paved according to the thickness of 0.1mm of each layer to obtain a radome with the thickness of 12mm when the prepreg is paved, the thickness of each layer of the radome is 6mm, polishing is carried out on the surface when the radome is molded for the second time, a layer of cyanate adhesive film is paved, then the prepreg is paved for curing again until the target thickness is reached, and the total curing is carried out for 2 times for 12 mm.
Example 13
The radome prepared in this embodiment is a radome with a flat plate structure as shown in fig. 2. The wall thickness was 8mm.
The preparation method of the composite radome of the embodiment is the same as that of embodiment 5, except that in the step (4), a flat radome mold is adopted, and when the prepreg is paved, 80 layers are paved according to the thickness of 0.1mm of each layer to obtain the radome with the thickness of 8mm, and the radome is obtained by one-step curing molding.
Comparative example 1
The prepreg of the radome of the present comparative example is different from that of example 5 in that the resin matrix is composed of only tetramethyl bisphenol F cyanate and bisphenol E cyanate resin, and no toughening agent, nano silica and hollow glass beads are added, and the ratio of tetramethyl bisphenol F cyanate to bisphenol E cyanate resin is the same as that of example 5. The composite radome of this embodiment is the same as the preparation method of the composite radome of embodiment 5.
Comparative example 2
The prepreg of the radome of the present comparative example is different from example 5 in that the resin matrix includes the following components in parts by weight: 79.5 parts of tetramethyl bisphenol F cyanate, 4 parts of bisphenol E cyanate resin, 1.21 parts of nano silicon dioxide and 36.29 parts of hollow glass beads, namely no toughening agent is added. The composite radome of this embodiment is the same as the preparation method of the composite radome of embodiment 5.
Comparative example 3
The prepreg of the radome of the present comparative example is different from example 5 in that the resin matrix includes the following components in parts by weight: 79.5 parts of tetramethyl bisphenol F cyanate, 4 parts of bisphenol E cyanate resin, 4 parts of acrylic resin toughening agent and 36.29 parts of hollow glass beads, namely no nano silicon dioxide is added. The composite radome of this embodiment is the same as the preparation method of the composite radome of embodiment 5.
Comparative example 4
The prepreg of the radome of the present comparative example is different from example 5 in that the resin matrix includes the following components in parts by weight: 79.5 parts of tetramethyl bisphenol F cyanate, 4 parts of bisphenol E cyanate resin, 4 parts of acrylic resin toughening agent and 1.21 parts of nano silicon dioxide, namely no hollow glass bead is added. The composite radome of this embodiment is the same as the preparation method of the composite radome of embodiment 5.
Prepregs of examples 1 to 7 and comparative examples 1 to 4 were prepared into laminates by the above-described method, and the strength properties, dielectric constant, density and the like of the resultant laminates were measured, and the test results were shown in table 1 below. As can be seen from the data in table 1, comparative examples 1 and 4, to which no hollow glass microsphere component was added, have high flexural strength (493 mpa,503 mpa) and interlaminar strength (21.4 mpa,21.8 mpa) compared with other examples, mainly due to the higher fiber content and high mechanical properties of the composite material; whereas the dielectric constant is opposite to the high density. Compared with the examples 5, 6 and 7, the tensile strength and the compressive strength of the comparative examples 1 and 4 are lower than those of the examples 5, 6 and 7, mainly because the mechanical properties of the composite materials are improved by adding the toughening agent and the nano SiO 2. The density and dielectric constant of comparative examples 2 and 3 were reduced, but the mechanical properties were also significantly reduced.
Examples 1 to 4 are compared with examples 5 to 7, the density and dielectric constant of the composite material are obviously reduced, but the tensile strength, the bending strength, the compressive strength and the interlayer strength are also greatly reduced, and the main reason is that the mechanical property is reduced due to the reduction of the fiber content in the composite material along with the increase of the content of the hollow glass beads. The performance of examples 5-7 is better than examples 1-4, taking into account the combination of mechanical properties, dielectric constant, density and electrical properties, and is the preferred embodiment. Example 5 the greatest decrease in composite density and dielectric constant is beneficial to increasing the wave transmission rate and reducing the weight of the product with a smaller decrease in mechanical properties. Thus, example 5 is the preferred embodiment, the obtained prepreg molded plate has a density of not more than 1.36g/cm 3, a dielectric constant (Dk, 10 GHz) of not more than 2.7-2.8, an electrical property phase uniformity of not more than + -4 DEG, an areal density uniformity of not more than + -5%, a gel content variation of + -5%, and meets the light-weight, low-dielectric wave-transmitting requirements of wave-transmitting materials and the development requirements of bearing strength.
The radomes of U-shaped structures with different sizes prepared in examples 8, 9 and 10 were measured for compressive strength, and the test results are shown in table 2 below. It can be seen that the prepreg of the present invention can be used to produce radomes of different size, weight and compressive strength.
The radomes of the flat plate structures with different thicknesses prepared in examples 11, 12 and 13 were measured for the wave transmittance, and the test results are shown in table 3 below. It can be seen that radomes of different thickness can meet different wave transmission requirements.
TABLE 1
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 | |
| Tensile Strength (MPa) | 613 | 608 | 625 | 631 | 476 | 520 | 572 | 587 | 629 | 633 | 637 |
| Tensile modulus (GPa) | 22.9 | 20.9 | 19.5 | 21.9 | 22.8 | 22.4 | 22.5 | 21.4 | 21.3 | 20.8 | 20.6 |
| Poisson's ratio | 0.13 | 0.14 | 0.14 | 0.13 | 0.13 | 0.13 | 0.13 | 0.14 | 0.14 | 0.14 | 0.14 |
| Compressive Strength (MPa) | 230 | 242 | 246 | 225 | 235 | 239 | 244 | 249 | 253 | 257 | 258 |
| Compression modulus (GPa) | 13.3 | 14.2 | 13.3 | 14.1 | 13.4 | 13.6 | 13.7 | 13.7 | 13.9 | 14.1 | 14.2 |
| Flexural Strength (MPa) | 493 | 362 | 375 | 508 | 351 | 362 | 367 | 378 | 395 | 406 | 421 |
| Flexural modulus (GPa) | 21.9 | 18.7 | 19.8 | 20.2 | 19.6 | 19.9 | 20.3 | 20.8 | 20.9 | 21.1 | 21.5 |
| Layer shear strength (MPa) | 21.4 | 18.0 | 17. 9 | 21. 8 | 17.6 | 17.8 | 18.1 | 18.3 | 18.6 | 18.7 | 19.1 |
| Dielectric constant (C/X/Ku) | 3.10-3.14 | 2.69-2.81 | 2.79-2.92 | 3.08-3.12 | 2.41-2.53 | 2.48-2.58 | 2.53-2.61 | 2.59-2.66 | 2.71-2.80 | 2.83-2.91 | 2.92-3.02 |
| Dielectric loss (C/X/Ku) | <0.008 | <0.006 | <0.007 | <0.008 | <0.005 | <0.005 | <0.006 | <0.006 | <0.007 | <0.007 | <0.008 |
| Density (g/cm 3) | 1.78 | 1.38 | 1.35 | 1.77 | 1.26 | 1.29 | 1.31 | 1.33 | 1.36 | 1.44 | 1.65 |
TABLE 2
| Weight/kg (ρ=1.4 g/mm 3) | Thickness/mm | Compressive Strength/MPa | |
| Example 8 | 14.5 | 16 | 11.86 |
| Example 9 | 6.1 | 12 | 13.98 |
| Example 10 | 2.1 | 8 | 13.13 |
TABLE 3 Table 3
| Thickness/mm | Wave transmittance | |
| Example 11 | 16 | 86% |
| Example 12 | 12 | 80% |
| Example 13 | 8 | 95% |
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (10)
1. A prepreg for preparing a composite radome, characterized in that:
Comprises a resin matrix and a reinforcing material; the reinforcing material is quartz fiber; the resin matrix comprises the following components in parts by weight: 50-100 parts of cyanate, 10-65 parts of hollow glass beads, 0.5-2 parts of nano silicon dioxide and 2-12 parts of toughening agent.
2. A prepreg for making a composite radome of claim 1, wherein:
the resin matrix comprises the following components in parts by weight: 55-90 parts of cyanate, 10-41 parts of hollow glass beads, 0.5-2 parts of nano silicon dioxide and 3.7-10 parts of toughening agent.
3. A prepreg for making a composite radome of claim 1, wherein:
The ratio of the total mass of the cyanate ester and the toughening agent to the total mass of the nano silicon dioxide and the hollow glass beads is 3-9:3; the mass content of the resin matrix in the prepreg is 30% -45%.
4. A prepreg for making a composite radome of claim 1, wherein:
The cyanate is one or a mixture of more of tetramethyl bisphenol F cyanate, bisphenol E cyanate and dicyclopentadiene cyanate; the cyanate resin is a prepolymer, and the viscosity of the cyanate resin is 3000-15000 mPa.s at 80 ℃.
5. A prepreg for making a composite radome of claim 1, wherein:
The particle size of the hollow glass beads is 30-120 mu m, the wall thickness is 1-4 mu m, and the density is 0.1-0.7 g/m 3; the particle size of the nano silicon dioxide is 20-100 nm; the toughening agent is one or a mixture of more of rubber and thermoplastic resin.
6. A composite radome prepared from the prepreg of any one of claims 1-5.
7. A method of making a composite radome of claim 6, comprising the steps of:
s1, mixing the cyanate, the hollow glass beads, the nano silicon dioxide and the toughening agent to obtain a mixture;
S2, preparing the mixture into a hot melt adhesive film;
s3, laminating quartz fibers and the hot melt adhesive film, and melting and dipping the hot melt adhesive film on the quartz fibers to obtain prepreg;
S4, arranging the prepreg on a die of the radome, and performing curing molding to obtain the composite material radome.
8. The method of manufacturing according to claim 7, wherein:
the step S1 specifically comprises the following steps:
Heating and blending the cyanate and the toughening agent to obtain a material A, and testing the viscosity of the material A to ensure that the viscosity of the material A is 3000 mPas-5000 mPas at 70 ℃; mixing the nano silicon dioxide and the hollow glass beads to obtain a material B; and then mixing the material A with the material B to obtain the mixture.
9. The method of manufacturing according to claim 7, wherein:
the step S2 specifically comprises the following steps:
Preparing the mixture into a hot melt adhesive film by adopting a hot melt prepreg machine; the temperature of the hot melt prepreg machine gum dipping roller is 75-85 ℃, the traction rate of conveying release paper is 3-6 m/min, and the unit mass of the hot melt adhesive film reaches the required prepreg resin content by adjusting the distance between the gum dipping rollers.
10. The method of manufacturing according to claim 7, wherein:
in the step S4, the curing and forming of the radome are carried out in multiple times, the thickness of the radome is not more than 10mm each time, polishing is carried out on the surface of the product formed in the previous time before the next time of forming, a layer of cyanate adhesive film is laid, and then prepreg is arranged for curing again until the target thickness is reached.
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