CN104513456A - Prepreg, forming method thereof and wave-transmitting material - Google Patents
Prepreg, forming method thereof and wave-transmitting material Download PDFInfo
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Abstract
The invention provides a prepreg. The prepreg comprises 20%-60% by weight of fiber, 10%-30% by weight of a low-dielectric-constant material and 20%-60% by weight of resin. The invention also provides a method for manufacturing the prepreg. The method comprises: mixing resin and the low-dielectric-constant material to form a mixture; coating release paper with the mixture to form a resin coating; and dipping the resin coating in fiber. The invention also provides a wave-transmitting material. The provided prepreg has the advantages of low dielectric constant and low dielectric loss, is capable of overcoming property disadvantages of a prepreg in an associated technology, and is beneficial for improving the quality of a final product. The provided prepreg forming method is capable of processing the prepreg with relatively excellent performances, and also is capable of avoiding heating, evaporation and other technological steps, thereby reducing the complexity and the cost of the technology and improving the production efficiency.
Description
Technical field
The present invention relates to field of compound material, in particular to a kind of prepreg and forming method thereof and electromagnetic wave transparent material.
Background technology
Prepreg is with resin impregnating continuous fibres or fabric under the strict condition controlled, and makes the composition of resin matrix and reinforcement, that is, a kind of matrix material.His properties details is brought in matrix material, is the basis of matrix material.The performance of matrix material depends on the performance of prepreg to a great extent.For composite Materials Design teacher, prepreg is the structural unit with certain mechanical property, can in order to carry out structure design.For composite material I process engineer, prepreg is the raw material of manufacturing structure, can be directly used in and manufacture various matrix material structure.The application and development of prepreg to matrix material is significant.
By physical condition classification, prepreg is divided into unidirectional pre-immersion material, one-way fabric prepreg, Fabric prereg; Different by resin matrix, prepreg is divided into thermosetting resin prepreg and thermoplastic resin prepreg; Different by strongthener, be divided into carbon fiber (fabric) prepreg, glass fibre (fabric) prepreg, aramid fiber (fabric) prepreg.
The method of existing manufacture prepreg is powder prepreg method, refers to that toner is attached on fiber, through partial melting, forms resin discontinuous, and fiber is not by a kind of mixture that resin fully soaks into.Other methods manufacturing prepreg also have solution dipping method, refer to resin dissolves in solvent, become certain density solution, then fibrous bundle or fabric are passed through resin matrix solution with predetermined speed, it is made to soak quantitative resin matrix, thereafter remove solvent by the method for heating again, finally form prepreg.But the method technique of the production prepreg used in prior art is comparatively complicated and energy consumption is larger.
Prepreg has good mechanical property and chemical stability and has the prospect of good suitability for industrialized production, and therefore, it is widely used in electron device etc. needs in the field of high reliability.But although existing prepreg has good mechanical property and chemical stability, its dielectric properties are also not fully up to expectations.Infiltration material the most frequently used at present and similar application part adopt glass fibre, carbon fiber or aramid fiber as strongthener, and epoxy resin is as raw matrix materials.But the specific inductivity of the prepreg be processed into based on above-mentioned composition or application ware and dielectric loss are comparatively large, specific inductivity be generally about 4.5 and dielectric loss about 0.025.Therefore, expect that exploitation is a kind of and there is the prepreg of low-k low-dielectric loss and relevant manufacture method.
Summary of the invention
For the problem of the high-k height dielectric loss of prepreg in prior art, the invention provides a kind of prepreg and forming method thereof and electromagnetic wave transparent material.
According to an aspect of the present invention, provide a kind of prepreg, this prepreg has low-k and low-dielectric loss.Prepreg according to the present invention comprises:
Fiber 20%-60%(weight);
Advanced low-k materials 10%-30%(weight); And
Resin 20%-60%(weight).
In certain embodiments, advanced low-k materials is low-k polymer micro mist.
In certain embodiments, resin is thermosetting resin or resin is thermoplastic resin.
In certain embodiments, prepreg comprises 1%(weight further) processing aid.
According to a further aspect in the invention, a kind of method for the manufacture of prepreg is provided.
The method comprises:
Resin and advanced low-k materials are carried out being mixed to form mixture;
Mixture is coated on separate-type paper and forms resin glued membrane; And
By the impregnation of resin glued membrane in fiber.
In certain embodiments, undertaken in the step mixed by resin and advanced low-k materials, the weight of resin is the 20%-60% of prepreg gross weight.
In certain embodiments, resin is thermosetting resin or thermoplastic resin.
In certain embodiments, undertaken in the step mixed by resin and advanced low-k materials, the weight of advanced low-k materials is the 10%-30% of prepreg gross weight.
In certain embodiments, advanced low-k materials is low-k polymer micro mist.
In certain embodiments, resin and advanced low-k materials are being carried out, in the step mixed, adding processing aid, the weight of processing aid is 1% of prepreg gross weight.
In certain embodiments, adhesive applicator is used to implement mixture to be coated on the step of separate-type paper.
In certain embodiments, in the scope of 30 DEG C to 150 DEG C, implement mixture to be coated on the step that separate-type paper forms resin glued membrane.
In certain embodiments, under the condition of 50 DEG C, implement mixture to be coated on the step that separate-type paper forms resin glued membrane.
In certain embodiments, in step mixture being coated on separate-type paper formation resin glued membrane, the pulling speed of mixture coating is between 2.5m/min to 3.5m/min.
In certain embodiments, in step mixture being coated on separate-type paper formation resin glued membrane, the pulling speed of mixture coating is 3m/min
In certain embodiments, implement mixture to be coated on the step that separate-type paper forms resin glued membrane under the pressure of 0.01MPa.
In certain embodiments, the thickness of resin glued membrane is 0.1mm to 2mm.
In certain embodiments, the grammes per square metre of resin glued membrane is 130g/m
2to 140g/m
2.
In certain embodiments, the grammes per square metre of resin glued membrane is 133g/m
2to 137g/m
2.
In certain embodiments, after step mixture being coated on separate-type paper formation resin glued membrane, the step detecting Resin adhesive film thickness is comprised further.
In certain embodiments, the step of infrared film thickness measuring instrument examinations Resin adhesive film thickness is used.
In certain embodiments, by the impregnation of resin glued membrane in the step in fiber, the weight of fiber is the 20%-60% of prepreg gross weight.
In certain embodiments, the resinous amount of prepreg is 20%-60%.
In certain embodiments, implement the impregnation of resin glued membrane in the scope of 50 DEG C to 100 DEG C to the step in fiber.
In certain embodiments, implement the impregnation of resin glued membrane under the condition of 80 DEG C to the step in fiber.
In certain embodiments, by the impregnation of resin glued membrane in the step in fiber, the pulling speed of resin glued membrane impregnation is in the scope of 0.5m/min to 1.5m/min.
In certain embodiments, by the impregnation of resin glued membrane in the step in fiber, the pulling speed of resin glued membrane impregnation is 1m/min.
In certain embodiments, implement the impregnation of resin glued membrane under the pressure of 0.05MPa to the step in fiber.
In accordance with a further aspect of the present invention, present invention also offers a kind of electromagnetic wave transparent material shaping by above-mentioned prepreg.
In certain embodiments, electromagnetic wave transparent material is shaping by vacuum-bag process or autoclave molding.
In certain embodiments, electromagnetic wave transparent material is for the preparation of radome, antenna back panel or HF link plate.
The prepreg that the present invention proposes has the advantage of low-k and low-dielectric loss, can overcome the defect that in correlation technique, prepreg exists in nature, contribute to the quality improving final finished; And the prepreg formation method that the present invention proposes can not only process the more excellent prepreg of performance, and can avoid adopting the processing steps such as heating, evaporation, thus reduce complexity and the cost of technique, improve production efficiency.
Accompanying drawing explanation
Fig. 1 be according to the embodiment of the present invention for the manufacture of the schema of method of prepreg with low-k and low-dielectric loss.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain, all belongs to the scope of protection of the invention.
The manufacture method of prepreg
As shown in the step S101 of Fig. 1, use stirrer resin and advanced low-k materials to be mixed, mixing time is 30 minutes to 1 hour.The mixture of resin and advanced low-k materials is formed after mixing completely.
The resin used in step S101 can be thermosetting resin, comprises epoxy resin, vibrin, epoxy resin, resol, cyanate ester resin, bimaleimide resin, terpolycyantoamino-formaldehyde resin, furane resin, silicone resin or polybutadiene etc.Although only illustrate the example of spendable thermosetting resin in this article, it will be understood by those skilled in the art that and thermoplastic resin also can be used to substitute thermosetting resin.In step S101, the advanced low-k materials used is generally low-k macromolecular material, comprises tetrafluoroethylene, polyimide, polyaryl ether, PAEK, benzoxazine polymkeric substance, benzocyclobutane olefine resin and SiLK etc.
As shown in the step S103 of Fig. 1, under the condition of 30 DEG C to 150 DEG C, use adhesive applicator to be coated in separate-type paper by the mixture in step S101 and form resin glued membrane, wherein gluing temperature should be 30 DEG C to 100 DEG C.In gluing process, the rate of migration of tractor is 2.5m/min to 3.5m/min, and preferred value is 3.0m/min; The pressure of adhesive applicator is 0.01MPa.In the process by tractor traction resin glued membrane, monitor rubberization thickness accurately through infrared equipment and detection equipment.After gumming step terminates, the thickness of the gummy glued membrane in separate-type paper is 0.1mm to 2mm, and preferred value is 0.2mm; And the grammes per square metre of resin glued membrane is 120g/m
2to 150g/m
2, preferred value is 133g/m
2.In step s 103, the separate-type paper used can comprise super sub-machine-glazed paper, saturated platen, dimensional stabilizing paper, polyethylene coated paper or the one side of adding of latex adds platen etc.
As shown in the step 105 of Fig. 1, finished product prepreg will be formed in the resin glued membrane impregnation to fiber that formed in step S103.In step 105, implement in the scope of 50 DEG C to 100 DEG C containing soaking technology; And be 0.05MPa containing the pressure of soaking technology.Containing in soaking technology, the pulling speed of tractor is 0.5m/min to 1.5m/min, and preferred value is 1.0m/min.The thickness of the finished product prepreg of final formation is 0.5mm to 2.5mm; And the resinous amount of finished product prepreg is 20% to 60%.In step S105, the fiber of use comprises superhigh molecular weight polyethylene fibers, silica fiber, aramid fiber, glass fibre, carbon fiber, polypropylene fibre, polyacrylonitrile fibre, polyvinyl formal fibre, tynex or polyethylene terephthalate etc.
Embodiment 1
As shown in table 1, use stirrer the processing aid of the epoxy resin of 99.6g, the tetrafluoroethylene of 31.54g and 1.66g is mixed, mixing time be 30 minutes to 1 hour, after mixing completely, form mixture.Under the condition of 30 DEG C to 150 DEG C, adhesive applicator is used mixture to be coated on separate-type paper (polyethylene coated paper) upper formation resin glued membrane.After gluing completes, the grammes per square metre of resin glued membrane is 133g/m
2.Then finished product prepreg will be formed in resin glued membrane impregnation to the superhigh molecular weight polyethylene fibers of 33.2g.The resinous amount of the finished product prepreg made is 60%.
Embodiment 2
As shown in table 1, use stirrer the processing aid of the epoxy resin of 65g, the tetrafluoroethylene of 61.75g and 3.25g is mixed, mixing time be 30 minutes to 1 hour, after mixing completely, form mixture.Under the condition of 30 DEG C to 150 DEG C, adhesive applicator is used mixture to be coated on separate-type paper (polyethylene coated paper) upper formation resin glued membrane.After gluing completes, the grammes per square metre of resin glued membrane is 130g/m
2.Then finished product prepreg will be formed in resin glued membrane impregnation to the superhigh molecular weight polyethylene fibers of 195g.The resinous amount of the finished product prepreg made is 20%.
Embodiment 3
As shown in table 1, use stirrer the processing aid of the epoxy resin of 99.9g, the tetrafluoroethylene of 29.97g and 3.33g is mixed, mixing time be 30 minutes to 1 hour, after mixing completely, form mixture.Under the condition of 30 DEG C to 150 DEG C, adhesive applicator is used mixture to be coated on separate-type paper (polyethylene coated paper) upper formation resin glued membrane.After gluing completes, the grammes per square metre of resin glued membrane is 133g/m
2.Then finished product prepreg will be formed in resin glued membrane impregnation to the superhigh molecular weight polyethylene fibers of 199.8g.The resinous amount of the finished product prepreg made is 30%.
Embodiment 4
As shown in table 1, use stirrer the processing aid of the bimaleimide resin of 103.2g, the polyimide of 30.96g and 2.58g is mixed, mixing time be 30 minutes to 1 hour, after mixing completely, form mixture.Under the condition of 30 DEG C to 150 DEG C, adhesive applicator is used mixture to be coated on separate-type paper (one side adds platen) upper formation resin glued membrane.After gluing completes, the grammes per square metre of resin glued membrane is 137g/m
2.Then finished product prepreg will be formed in resin glued membrane impregnation to the super polypropylene fibre of 121.26g.The resinous amount of the finished product prepreg made is 40%.
Embodiment 5
As shown in table 1, use stirrer the processing aid of the polybutadiene of 115g, the tetrafluoroethylene of 23g and 2.3g is mixed, mixing time be 30 minutes to 1 hour, after mixing completely, form mixture.Under the condition of 30 DEG C to 150 DEG C, adhesive applicator is used mixture to be coated on separate-type paper (polyethylene coated paper) upper formation resin glued membrane.After gluing completes, the grammes per square metre of resin glued membrane is 140g/m
2.Then finished product prepreg will be formed in resin glued membrane impregnation to the super-high molecular weight polyacrylonitrile fiber of 89.7g.The resinous amount of the finished product prepreg made is 50%.
Those of ordinary skill in the art should understand, when the resin used is for thermoplastic resin, in the above-described embodiments, processing aid also should add solidifying agent, to ensure the shaping of in course of processing thermoplastic resin.
Comparative example 1
As shown in table 1, use stirrer the processing aid of the epoxy resin 1.7g of 100g is mixed, mixing time be 30 minutes to 1 hour, after mixing completely, form mixture.Under the condition of 30 DEG C to 150 DEG C, adhesive applicator is used mixture to be coated on separate-type paper (polyethylene coated paper) upper formation resin glued membrane.After gluing completes, the grammes per square metre of resin glued membrane is 100g/m
2.Then finished product prepreg will be formed in resin glued membrane impregnation to the glass fibre of 66.7g.The resinous amount of the finished product prepreg made is about 60%.
Each composition weight and weight percent in table 1 embodiment 1 to embodiment 5 and comparative example 1
Specific inductivity test and dielectric loss test
AET high frequency (microwave) specific inductivity analyser is used to carry out specific inductivity test and dielectric loss test to finished product prepreg made in embodiment 1 to embodiment 5 respectively.Test result is as follows:
| Specific inductivity | Dielectric loss | |
| Embodiment 1 | 2.20 | 0.003 |
| Embodiment 2 | 2.25 | 0.003 |
| Embodiment 3 | 2.57 | 0.008 |
| Embodiment 4 | 2.34 | 0.005 |
| Embodiment 5 | 2.50 | 0.007 |
| Comparative example 1 | 4.5 | 0.025 |
Table 2 specific inductivity and dielectric loss test result
As shown in table 2, compared with comparative example 1, prepreg of the present invention all has lower specific inductivity and low-dielectric loss, and the specific inductivity of the prepreg of the method manufacture of use embodiment 1 to embodiment 5 is all less than 2.60 and its dielectric loss is all less than 0.009.And as can be seen from Table 2, the embodiment 3 less compared to advanced low-k materials addition, the more embodiment 1 of advanced low-k materials addition shows lower specific inductivity and low-dielectric loss.
Prepreg shaping
Any one prepreg formed in embodiment 1 to embodiment 5 is added in predetermined mould.Before prepreg is joined mould, brushing external release agent in mould, releasing agent can comprise oleic acid, paraffin, stearic acid, Zinic stearas, organic silicone oil, silicone grease and silicon rubber etc.After preheating and precharge are carried out to prepreg, prepreg is put into molding apparatus.In molding apparatus, the dwell time, forming pressure was in the scope of 15MPa to 29MPa, and mold temperature is in the scope of 150 DEG C to 180 DEG C, and soaking time is in the scope of 3 minutes to 5 minutes in the scope of 20 minutes to 120 minutes.In certain embodiments, the moulding process used can be vacuum-bag process or autoclave molding etc.Electromagnetic wave transparent material is obtained by above-mentioned technological forming.The use temperature of prepared electromagnetic wave transparent material is in the scope of about-50 DEG C to 200 DEG C, and preferred use temperature is in the scope of about-50 DEG C to 80 DEG C, and preferred use temperature is in the scope of about-10 DEG C to 80 DEG C further.The electromagnetic wave transparent material obtained may be used for preparing such as radome, antenna back panel or HF link plate etc.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (31)
1. a prepreg, is characterized in that, comprising:
Fiber 20%-60%(weight);
Advanced low-k materials 10%-30%(weight); And
Resin 20%-60%(weight).
2. prepreg according to claim 1, is characterized in that, described advanced low-k materials is low-k polymer micro mist.
3. prepreg according to claim 1, is characterized in that, described resin is thermosetting resin or thermoplastic resin.
4. prepreg according to claim 1, is characterized in that, described prepreg comprises 1%(weight further) processing aid.
5. manufacture a method for prepreg, it is characterized in that, comprising:
Resin and advanced low-k materials are carried out being mixed to form mixture;
Described mixture is coated on separate-type paper and forms resin glued membrane; And
By the impregnation of described resin glued membrane in fiber.
6. method according to claim 5, is characterized in that, is undertaken in the step mixed described by resin and advanced low-k materials, and the weight of described resin is the 20%-60% of described prepreg gross weight.
7. method according to claim 5, is characterized in that, described resin is thermosetting resin or thermoplastic resin.
8. method according to claim 5, is characterized in that, is undertaken in the step mixed described by resin and advanced low-k materials, and the weight of described advanced low-k materials is the 10%-30% of described prepreg gross weight.
9. method according to claim 5, is characterized in that, described advanced low-k materials is low-k polymer micro mist.
10. method according to claim 5, is characterized in that, resin and advanced low-k materials are carried out, in the step mixed, adding processing aid described, the weight of described processing aid is 1% of described prepreg gross weight.
11. methods according to claim 5, is characterized in that, use adhesive applicator to implement described step mixture being coated on separate-type paper.
12. methods according to claim 5, is characterized in that, in the scope of 30 DEG C to 150 DEG C, implement described step mixture being coated on separate-type paper formation resin glued membrane.
13. methods according to claim 12, is characterized in that, under the condition of 50 DEG C, implement described step mixture being coated on separate-type paper formation resin glued membrane.
14. methods according to claim 5, is characterized in that, be coated on by mixture in the step of separate-type paper formation resin glued membrane described, the pulling speed of described mixture coating is between 2.5m/min to 3.5m/min.
15. methods according to claim 14, is characterized in that, be coated on by mixture in the step of separate-type paper formation resin glued membrane described, the pulling speed of described mixture coating is 3m/min.
16. methods according to claim 5, is characterized in that, implement described step mixture being coated on separate-type paper formation resin glued membrane under the pressure of 0.01MPa.
17. methods according to claim 5, is characterized in that, the thickness of described resin glued membrane is 0.1mm to 2mm.
18. methods according to claim 5, is characterized in that, the grammes per square metre of described resin glued membrane is 130g/m
2to 140g/m
2.
19. methods according to claim 18, is characterized in that, the grammes per square metre of described resin glued membrane is 133g/m
2to 137g/m
2.
20. methods according to claim 5, is characterized in that, to be coated on by mixture after separate-type paper forms the step of resin glued membrane, to comprise the step detecting described Resin adhesive film thickness further described.
21. methods according to claim 20, is characterized in that, use infrared film thickness measuring instrument to implement the step of the described Resin adhesive film thickness of described detection.
22. methods according to claim 5, is characterized in that, by the impregnation of described resin glued membrane in the step in fiber, the weight of described fiber is the 20%-60% of prepreg gross weight.
23. methods according to claim 5, is characterized in that, the resinous amount of described prepreg is 20%-60%.
24. methods according to claim 5, is characterized in that, implement in the scope of 50 DEG C to 100 DEG C described by the impregnation of resin glued membrane to the step in fiber.
25. methods according to claim 24, is characterized in that, implement under the condition of 80 DEG C described by the impregnation of resin glued membrane to the step in fiber.
26. methods according to claim 5, is characterized in that, described by the impregnation of resin glued membrane in the step in fiber, the pulling speed of described resin glued membrane impregnation is in the scope of 0.5m/min to 1.5m/min.
27. methods according to claim 26, is characterized in that, described by the impregnation of resin glued membrane in the step in fiber, the pulling speed of described resin glued membrane impregnation is 1m/min.
28. methods according to claim 5, is characterized in that, implement under the pressure of 0.05MPa described by the impregnation of resin glued membrane to the step in fiber.
The electromagnetic wave transparent material that 29. 1 kinds of prepregs according to any one of claim 1 to 4 are shaping.
30. electromagnetic wave transparent materials according to claim 29, is characterized in that, described electromagnetic wave transparent material is by vacuum-bag process or autoclave molding.
31. electromagnetic wave transparent materials according to claim 29, is characterized in that, described electromagnetic wave transparent material is for the preparation of radome, antenna back panel or HF link plate.
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| CN108822543A (en) * | 2018-05-16 | 2018-11-16 | 西北工业大学 | A kind of cyanate resin base wave-penetrating composite material and preparation method thereof |
| CN109401203A (en) * | 2018-11-30 | 2019-03-01 | 江苏中鹏新材料股份有限公司 | Environmental protection typed gold color epoxy mold sealing material and preparation method thereof |
| CN110218382A (en) * | 2019-06-24 | 2019-09-10 | 西安安聚德纳米科技有限公司 | A kind of radome material and preparation method thereof |
| CN111499997A (en) * | 2020-05-28 | 2020-08-07 | 亚天顿（廊坊）复合材料科技有限公司 | Method for manufacturing novel high-wave-transmission thermoplastic composite prepreg |
| CN111969316A (en) * | 2020-08-26 | 2020-11-20 | 中国航空工业集团公司济南特种结构研究所 | Variable-thickness front-part radome with unidirectional tape structure |
| CN113527737A (en) * | 2021-07-30 | 2021-10-22 | 中国航空工业集团公司济南特种结构研究所 | Preparation method of low-dielectric high-performance modified benzocyclobutene resin composite material |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108822543A (en) * | 2018-05-16 | 2018-11-16 | 西北工业大学 | A kind of cyanate resin base wave-penetrating composite material and preparation method thereof |
| CN109401203A (en) * | 2018-11-30 | 2019-03-01 | 江苏中鹏新材料股份有限公司 | Environmental protection typed gold color epoxy mold sealing material and preparation method thereof |
| CN110218382A (en) * | 2019-06-24 | 2019-09-10 | 西安安聚德纳米科技有限公司 | A kind of radome material and preparation method thereof |
| CN110218382B (en) * | 2019-06-24 | 2022-03-11 | 西安安聚德纳米科技有限公司 | Antenna housing material |
| CN111499997A (en) * | 2020-05-28 | 2020-08-07 | 亚天顿（廊坊）复合材料科技有限公司 | Method for manufacturing novel high-wave-transmission thermoplastic composite prepreg |
| CN111969316A (en) * | 2020-08-26 | 2020-11-20 | 中国航空工业集团公司济南特种结构研究所 | Variable-thickness front-part radome with unidirectional tape structure |
| CN113527737A (en) * | 2021-07-30 | 2021-10-22 | 中国航空工业集团公司济南特种结构研究所 | Preparation method of low-dielectric high-performance modified benzocyclobutene resin composite material |
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| CN104513456B (en) | 2017-08-08 |
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