CN104513456B - A kind of prepreg and forming method thereof and electromagnetic wave transparent material - Google Patents
A kind of prepreg and forming method thereof and electromagnetic wave transparent material Download PDFInfo
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Abstract
The invention provides a kind of prepreg, including fiber 20% 60%（Weight）；Advanced low-k materials 10% 30%（Weight）；And resin 20% 60%（Weight）.Carry out being mixed to form mixture present invention provides a kind of method for manufacturing prepreg, including by resin and advanced low-k materials；Mixture is coated on release liners formation resin glued membrane；And by the impregnation of resin glued membrane into fiber.Present invention also offers a kind of electromagnetic wave transparent material.Prepreg proposed by the present invention has the advantage of low-k and low-dielectric loss, can overcome defect present on prepreg property in correlation technique, helps to improve the quality of final finished；And prepreg forming method proposed by the present invention can not only process the more excellent prepreg of performance, and it can avoid, using processing steps such as heating, evaporations, so as to reduce the complexity and cost of technique, improving 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 to use resin impregnating continuous fibres or fabric under conditions of strict control, and resin matrix and enhancing is made
A kind of composition of body, i.e. composite.His properties details is brought into composite, is the basis of composite.It is multiple
The performance of condensation material is heavily dependent on the performance of prepreg.For composite Materials Design teacher, prepreg is that have
The construction unit of certain mechanical property, is used for structure design.For composite material I process engineer, prepreg is
The raw material of structure is manufactured, can be directly used for manufacturing various composites structures.Application and development of the prepreg to composite have
It is significant.
Classify by physical state, prepreg is divided into unidirectional pre-immersion material, one-way fabric prepreg, Fabric prereg；By resin
Matrix is different, and prepreg is divided into thermosetting resin prepreg and thermoplastic resin prepreg；It is different by reinforcing material, it is divided into carbon fine
Tie up (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, by portion
Divide fusing, form resin discontinuously, a kind of compound that fiber is not thoroughly impregnated by resin.The method of other manufacture prepregs is also
There is solution dipping method, refer to resin being dissolved in solvent, become certain density solution, then by fibre bundle or fabric
At a predetermined rate by resin matrix solution, it is soaked quantitative resin matrix, removed again by the method for heating thereafter
Solvent, ultimately forms prepreg.But in the prior art used production prepreg method technique is complex and energy consumption compared with
Greatly.
Prepreg has good mechanical property and chemical stability and the prospect with good industrialized production, because
This, it is widely used in the field that electronic device etc. needs high reliability.Although however, existing prepreg has well
Mechanical property and chemical stability, but its dielectric properties and not fully up to expectations.Infiltration material and similar application the most frequently used at present
Part is that epoxy resin is used as raw matrix materials as reinforcing material using glass fibre, carbon fiber or aramid fiber.But be based on
The prepreg or the dielectric constant of application ware and dielectric loss that above-mentioned composition is processed into are larger, and it is left that dielectric constant is generally 4.5
Right and dielectric loss is 0.025 or so.Therefore, it is desirable to develop a kind of prepreg with low-k low-dielectric loss and
Related manufacture method.
The content of the invention
For prepreg in the prior art high-k high dielectric loss the problem of, the invention provides one kind preimpregnation
Material and forming method thereof and electromagnetic wave transparent material.
According to an aspect of the invention, there is provided a kind of prepreg, the prepreg has low-k and low dielectric
Loss.Included according to the prepreg of the present invention：
Fiber 20%-60%（Weight）；
Advanced low-k materials 10%-30%（Weight）；And
Resin 20%-60%（Weight）.
In certain embodiments, advanced low-k materials are low-k macromolecule micro mist.
In certain embodiments, resin is thermosetting resin or resin is thermoplastic resin.
In certain embodiments, prepreg further comprises 1%（Weight）Processing aid.
There is provided a kind of method for manufacturing prepreg according to another aspect of the present invention.
This method includes：
Resin and advanced low-k materials are carried out being mixed to form mixture；
Mixture is coated on release liners formation resin glued membrane；And
By the impregnation of resin glued membrane into fiber.
In certain embodiments, in the step of being mixed 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, in the step of being mixed resin and advanced low-k materials, low-k material
The weight of material is the 10%-30% of prepreg gross weight.
In certain embodiments, advanced low-k materials are low-k macromolecule micro mist.
In certain embodiments, in the step of being mixed resin and advanced low-k materials, processing aid is added,
The weight of processing aid is the 1% of prepreg gross weight.
In certain embodiments, the step of implementing mixture being coated on release liners using gluing machine.
In certain embodiments, in the range of 30 DEG C to 150 DEG C, implement mixture being coated on release liners formation resin
The step of glued membrane.
In certain embodiments, under conditions of 50 DEG C, implement mixture being coated on release liners formation resin glued membrane
Step.
In certain embodiments, in the step of mixture is coated on to release liners formation resin glued membrane, mixture coating
Hauling speed between 2.5m/min to 3.5m/min.
In certain embodiments, in the step of mixture is coated on to release liners formation resin glued membrane, mixture coating
Hauling speed be 3m/min
In certain embodiments, implement mixture being coated on release liners formation resin glued membrane under 0.01MPa pressure
The step of.
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/m2To 140g/m2。
In certain embodiments, the grammes per square metre of resin glued membrane is 133g/m2To 137g/m2。
In certain embodiments, after the step of mixture is coated on to release liners formation resin glued membrane, further wrap
The step of including detection resin film thickness.
In certain embodiments, using infrared film thickness measuring instrument examinations resin film thickness the step of.
In certain embodiments, in the step that resin glued membrane is impregnated with into fiber, the weight of fiber is total for prepreg
The 20%-60% of weight.
In certain embodiments, the resinous amount of prepreg is 20%-60%.
In certain embodiments, implement resin glued membrane being impregnated with the step into fiber in the range of 50 DEG C to 100 DEG C.
In certain embodiments, implement resin glued membrane being impregnated with the step into fiber under conditions of 80 DEG C.
In certain embodiments, in the step that resin glued membrane is impregnated with into fiber, the traction speed of resin glued membrane impregnation
Degree is in the range of 0.5m/min to 1.5m/min.
In certain embodiments, in the step that resin glued membrane is impregnated with into fiber, the traction speed of resin glued membrane impregnation
Spend for 1m/min.
In certain embodiments, implement resin glued membrane being impregnated with the step into fiber under 0.05MPa pressure.
In accordance with a further aspect of the present invention, present invention also offers a kind of wave transparent material being molded by above-mentioned prepreg
Material.
In certain embodiments, electromagnetic wave transparent material is molded by vacuum-bag process or autoclave molding.
In certain embodiments, electromagnetic wave transparent material is used to prepare antenna house, antenna back panel or HF link plate.
Prepreg proposed by the present invention has the advantage of low-k and low-dielectric loss, can overcome in correlation technique
Defect present on prepreg property, helps to improve the quality of final finished；And prepreg forming method proposed by the present invention
The more excellent prepreg of performance can not only be processed, and can be avoided using processing steps such as heating, evaporations, so as to reduce
The complexity and cost of technique, improve production efficiency.
Brief description of the drawings
Fig. 1 is the side for being used to manufacture the prepreg with low-k and low-dielectric loss according to embodiments of the present invention
The flow chart of method.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on
Embodiment in the present invention, the every other embodiment that those of ordinary skill in the art are obtained belongs to what the present invention was protected
Scope.
The manufacture method of prepreg
As shown in Fig. 1 step S101, resin and advanced low-k materials are mixed using mixer, incorporation time
For 30 minutes to 1 hour.The mixture of resin and advanced low-k materials is formed after being mixed thoroughly.
Resin used in step S101 can be thermosetting resin, including epoxy resin, polyester resin, asphalt mixtures modified by epoxy resin
Fat, phenolic resin, cyanate ester resin, bimaleimide resin, melamine resin, furane resins, organic siliconresin
Or polybutadiene etc..Although being only exemplified by the example of workable thermosetting resin, the common skill in this area herein
Art personnel are it should be understood that can also use thermoplastic resin to substitute thermosetting resin.In step S101, used low dielectric
Constant material is usually low-k high polymer material, including polytetrafluoroethylene (PTFE), polyimides, polyaryl ether, polyaryl ether
Ketone, benzoxazine polymer, benzocyclobutane olefine resin and SiLK etc..
, will be mixed in step S101 using gluing machine under conditions of 30 DEG C to 150 DEG C as shown in Fig. 1 step S103
Compound is coated on formation resin glued membrane in release liners, and wherein gluing temperature should be 30 DEG C to 100 DEG C.During gluing, traction
The migration rate of machine is 2.5m/min to 3.5m/min, and preferred value is 3.0m/min；The pressure of gluing machine is 0.01MPa.Logical
During crossing traction machine travel resin glue film, rubberization thickness is accurately monitored through infrared equipment and detecting devices.Gluing is walked
Suddenly after terminating, the thickness of the gummy glued membrane in release liners is 0.1mm to 2mm, and preferred value is 0.2mm；And the grammes per square metre of resin glued membrane
For 120g/m2To 150g/m2, preferred value is 133g/m2.In step s 103, used release liners can include super matt
Paper, latex saturation pressurization paper, dimensionally stable paper, polyethylene coated paper or one side pressurization paper etc..
As shown in Fig. 1 step 105, the resin glued membrane formed in step S103 is impregnated with into fiber to form finished product
Prepreg.In step 105, implement to contain soaking technology in the range of 50 DEG C to 100 DEG C；And the pressure containing soaking technology is
0.05MPa.In containing soaking technology, the pulling speed of hauling machine is 0.5m/min to 1.5m/min, and preferred value is 1.0m/min.Most
End form into finished product prepreg thickness be 0.5mm to 2.5mm；And the resinous amount of finished product prepreg is 20% to 60%.In step
In rapid S105, it is fine that the fiber used includes superhigh molecular weight polyethylene fibers, quartz fibre, aramid fiber, glass fibre, carbon
Dimension, polypropylene fibre, polyacrylonitrile fibre, vinylon, Fypro or PET
Deng.
Embodiment 1
As shown in table 1, using mixer by the processing of 99.6g epoxy resin, 31.54g polytetrafluoroethylene (PTFE) and 1.66g
Auxiliary agent is mixed, and incorporation time is 30 minutes to 1 hour, and mixture is formed after being mixed thoroughly.At 30 DEG C to 150 DEG C
Under conditions of, mixture is coated on release liners using gluing machine（Polyethylene coated paper）Upper formation resin glued membrane.Gluing is completed
The grammes per square metre of resin glued membrane is 133g/m afterwards2.Then by resin glued membrane impregnation into 33.2g superhigh molecular weight polyethylene fibers from
And form finished product prepreg.The resinous amount for the finished product prepreg being made is 60%.
Embodiment 2
As shown in table 1, the processing of 65g epoxy resin, 61.75g polytetrafluoroethylene (PTFE) and 3.25g is helped using mixer
Agent is mixed, and incorporation time is 30 minutes to 1 hour, and mixture is formed after being mixed thoroughly.At 30 DEG C to 150 DEG C
Under the conditions of, mixture is coated on release liners using gluing machine（Polyethylene coated paper）Upper formation resin glued membrane.After the completion of gluing
The grammes per square metre of resin glued membrane is 130g/m2.Then by resin glued membrane impregnation into 195g superhigh molecular weight polyethylene fibers so as to
Form finished product prepreg.The resinous amount for the finished product prepreg being made is 20%.
Embodiment 3
As shown in table 1, using mixer by the processing of 99.9g epoxy resin, 29.97g polytetrafluoroethylene (PTFE) and 3.33g
Auxiliary agent is mixed, and incorporation time is 30 minutes to 1 hour, and mixture is formed after being mixed thoroughly.At 30 DEG C to 150 DEG C
Under conditions of, mixture is coated on release liners using gluing machine（Polyethylene coated paper）Upper formation resin glued membrane.Gluing is completed
The grammes per square metre of resin glued membrane is 133g/m afterwards2.Then by the impregnation of resin glued membrane into 199.8g superhigh molecular weight polyethylene fibers
So as to form finished product prepreg.The resinous amount for the finished product prepreg being made is 30%.
Embodiment 4
As shown in table 1, using mixer by 103.2g bimaleimide resin, 30.96g polyimides and
2.58g processing aid is mixed, and incorporation time is 30 minutes to 1 hour, and mixture is formed after being mixed thoroughly.
Under conditions of 30 DEG C to 150 DEG C, mixture is coated on release liners using gluing machine（One side pressurization paper）Upper formation resin glued membrane.
The grammes per square metre of resin glued membrane is 137g/m after the completion of gluing2.Then by the impregnation of resin glued membrane into 121.26g super polypropylene fibre
So as to form finished product prepreg.The resinous amount for the finished product prepreg being made is 40%.
Embodiment 5
As shown in table 1, using mixer by the processing of 115g polybutadiene, 23g polytetrafluoroethylene (PTFE) and 2.3g
Auxiliary agent is mixed, and incorporation time is 30 minutes to 1 hour, and mixture is formed after being mixed thoroughly.At 30 DEG C to 150 DEG C
Under conditions of, mixture is coated on release liners using gluing machine（Polyethylene coated paper）Upper formation resin glued membrane.Gluing is completed
The grammes per square metre of resin glued membrane is 140g/m afterwards2.Then by the impregnation of resin glued membrane into 89.7g super-high molecular weight polyacrylonitrile fiber
So as to form finished product prepreg.The resinous amount for the finished product prepreg being made is 50%.
Those of ordinary skill in the art it will be clearly understood that used resin be thermoplastic resin in the case of, in above-mentioned reality
Apply in example, processing aid should also add curing agent, to ensure the shaping of thermoplastic resin in process.
Comparative example 1
As shown in table 1,100g epoxy resin 1.7g processing aid is mixed using mixer, incorporation time is
30 minutes to 1 hour, mixture is formed after being mixed thoroughly., will be mixed using gluing machine under conditions of 30 DEG C to 150 DEG C
Compound is coated on release liners（Polyethylene coated paper）Upper formation resin glued membrane.The grammes per square metre of resin glued membrane is 100g/ after the completion of gluing
m2.Then resin glued membrane is impregnated with into 66.7g glass fibre to form finished product prepreg.The finished product prepreg being made
Resinous amount is about 60%.
The embodiment 1 of table 1 each component weight and percentage by weight into embodiment 5 and comparative example 1
Dielectric constant is tested and dielectric loss test
It is pre- to the finished product made into embodiment 5 of embodiment 1 respectively using AET high frequencies (microwave) dielectric constant analyzer
Leaching material carries out dielectric constant test and dielectric loss test.Test result is as follows：
| Dielectric constant | 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 |
The dielectric constant of table 2 and dielectric loss test result
As shown in table 2, compared with comparative example 1, prepreg of the invention is respectively provided with relatively low dielectric constant and low dielectric is damaged
Consumption, the dielectric constant of the prepreg manufactured using the method for embodiment 1 to embodiment 5 is respectively less than 2.60 and its dielectric loss is small
In 0.009.And from Table 2, it can be seen that the embodiment 3 less compared to advanced low-k materials addition, low dielectric is normal
The more embodiment 1 of number material addition shows lower dielectric constant and low-dielectric loss.
The shaping of prepreg
Any prepreg that embodiment 1 is formed into embodiment 5 is added in predetermined mould.Added by prepreg
To before mould, the brushing external release agent in mould, releasing agent can include oleic acid, paraffin, stearic acid, zinc stearate, organic
Silicone oil, silicone grease and silicon rubber etc..Prepreg is preheated and precharge after, prepreg is put into molding apparatus.
In molding apparatus, the dwell time in the range of 20 minutes to 120 minutes, scope of the briquetting pressure between 15MPa to 29MPa
Interior, forming temperature is in the range of 150 DEG C to 180 DEG C, and soaking time is in the range of 3 minutes to 5 minutes.In some realities
Apply in example, used moulding process can be vacuum-bag process or autoclave molding etc..Obtained by above-mentioned technological forming
Wave material.The temperature in use of prepared electromagnetic wave transparent material is in the range of about -50 DEG C to 200 DEG C, and temperature in use preferably is situated between
In the range of about -50 DEG C to 80 DEG C, further preferred temperature in use is in the range of about -10 DEG C to 80 DEG C.It is resulting
Electromagnetic wave transparent material can be used for preparing antenna house, antenna back panel or HF link plate etc..
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God is with principle, and any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.
Claims (23)
1. a kind of prepreg, it is characterised in that by weight percentage, including：
Polypropylene fibre 20%-60%；
Advanced low-k materials 10%-30%；And
Bimaleimide resin 20%-60%, wherein, the advanced low-k materials are polyimides, and the low dielectric is normal
Number material is low-k macromolecule micro mist.
2. prepreg according to claim 1, it is characterised in that by weight percentage, the prepreg further comprises
1% processing aid.
3. a kind of method for manufacturing prepreg, it is characterised in that including：
Bimaleimide resin and advanced low-k materials are carried out being mixed to form mixture, wherein, the low-k
Material is polyimides, and the advanced low-k materials are low-k macromolecule micro mist, the bimaleimide resin
Weight be prepreg gross weight 20%-60%, the weight of the advanced low-k materials is the 10%- of prepreg gross weight
30%；
The mixture is coated on release liners formation resin glued membrane；And
By resin glued membrane impregnation into polypropylene fibre, wherein, the weight of the polypropylene fibre is prepreg gross weight
20%-60%.
4. method according to claim 3, it is characterised in that described by bimaleimide resin and low-k
In the step of material is mixed, processing aid is added, the weight of the processing aid is the 1% of the prepreg gross weight.
5. method according to claim 3, it is characterised in that using gluing machine implement it is described mixture is coated on it is release
The step of paper.
6. method according to claim 3, it is characterised in that in the range of 30 DEG C to 150 DEG C, implements described by mixing
The step of thing is coated on release liners formation resin glued membrane.
7. method according to claim 6, it is characterised in that under conditions of 50 DEG C, implementation is described to coat mixture
The step of release liners formation resin glued membrane.
8. method according to claim 3, it is characterised in that mixture is coated on into release liners formation resin glue described
In the step of film, the hauling speed of the mixture coating is between 2.5m/min to 3.5m/min.
9. method according to claim 8, it is characterised in that mixture is coated on into release liners formation resin glue described
In the step of film, the hauling speed of the mixture coating is 3m/min.
10. method according to claim 3, it is characterised in that implement described to apply mixture under 0.01MPa pressure
The step of being overlying on release liners formation resin glued membrane.
11. method according to claim 3, it is characterised in that the thickness of the resin glued membrane is 0.1mm to 2mm.
12. method according to claim 3, it is characterised in that the grammes per square metre of the resin glued membrane is 130g/m2To 140g/
m2。
13. method according to claim 12, it is characterised in that the grammes per square metre of the resin glued membrane is 133g/m2To 137g/
m2。
14. method according to claim 3, it is characterised in that mixture is coated on into release liners formation resin described
After the step of glued membrane, the step of further comprising detecting the resin film thickness.
15. method according to claim 14, it is characterised in that implemented using infrared film thickness measuring instrument described in the detection
The step of resin film thickness.
16. method according to claim 3, it is characterised in that implement described by resin in the range of 50 DEG C to 100 DEG C
Glued membrane contains the step being dipped into polypropylene fibre.
17. method according to claim 16, it is characterised in that implement described to contain resin glued membrane under conditions of 80 DEG C
It is dipped into the step in polypropylene fibre.
18. method according to claim 3, it is characterised in that resin glued membrane is impregnated with into polypropylene fibre described
The step of in, the hauling speed of resin glued membrane impregnation is in the range of 0.5m/min to 1.5m/min.
19. method according to claim 18, it is characterised in that resin glued membrane is impregnated with into polypropylene fibre described
The step of in, the hauling speed of resin glued membrane impregnation is 1m/min.
20. method according to claim 3, it is characterised in that implement described by resin glued membrane under 0.05MPa pressure
Containing the step being dipped into polypropylene fibre.
21. a kind of electromagnetic wave transparent material of prepreg shaping according to any one of claim 1 to 2.
22. electromagnetic wave transparent material according to claim 21, it is characterised in that the electromagnetic wave transparent material passes through vacuum-bag process or heat
Press jug forming.
23. electromagnetic wave transparent material according to claim 21, it is characterised in that the electromagnetic wave transparent material is used to prepare antenna house, day
Line backboard or HF link plate.
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| CN108822543B (en) * | 2018-05-16 | 2020-06-16 | 西北工业大学 | Cyanate ester resin-based wave-transparent 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 |
| 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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| US20140335341A1 (en) * | 2011-12-12 | 2014-11-13 | Lg Chem, Ltd. | Cyanate esters-based adhesive resin composition for fabrication of circuit board and flexible metal clad laminate comprising the same |
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