CN108299825A - Compound electromagnetic wave transparent material of fire resistant resin base and preparation method thereof when a kind of long - Google Patents
Compound electromagnetic wave transparent material of fire resistant resin base and preparation method thereof when a kind of long Download PDFInfo
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- CN108299825A CN108299825A CN201810244205.2A CN201810244205A CN108299825A CN 108299825 A CN108299825 A CN 108299825A CN 201810244205 A CN201810244205 A CN 201810244205A CN 108299825 A CN108299825 A CN 108299825A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 239000011347 resin Substances 0.000 title claims abstract description 33
- 229920005989 resin Polymers 0.000 title claims abstract description 33
- 150000001875 compounds Chemical class 0.000 title claims abstract description 28
- 239000012780 transparent material Substances 0.000 title claims abstract description 16
- 230000009970 fire resistant effect Effects 0.000 title claims abstract description 10
- 229920001721 polyimide Polymers 0.000 claims abstract description 43
- 239000002131 composite material Substances 0.000 claims abstract description 42
- 239000009719 polyimide resin Substances 0.000 claims abstract description 41
- 239000010453 quartz Substances 0.000 claims abstract description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000007711 solidification Methods 0.000 claims abstract description 25
- 230000008023 solidification Effects 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000000835 fiber Substances 0.000 claims abstract description 15
- 238000004804 winding Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000007731 hot pressing Methods 0.000 claims description 20
- 238000010792 warming Methods 0.000 claims description 20
- 239000003960 organic solvent Substances 0.000 claims description 14
- 238000009413 insulation Methods 0.000 claims description 13
- 239000004753 textile Substances 0.000 claims description 13
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 12
- 238000001291 vacuum drying Methods 0.000 claims description 9
- 238000009835 boiling Methods 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 7
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 4
- 239000004642 Polyimide Substances 0.000 claims description 3
- WFKAJVHLWXSISD-UHFFFAOYSA-N isobutyramide Chemical compound CC(C)C(N)=O WFKAJVHLWXSISD-UHFFFAOYSA-N 0.000 claims description 3
- 238000005253 cladding Methods 0.000 claims description 2
- OXHNLMTVIGZXSG-UHFFFAOYSA-N 1-Methylpyrrole Chemical class CN1C=CC=C1 OXHNLMTVIGZXSG-UHFFFAOYSA-N 0.000 claims 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 150000003384 small molecules Chemical class 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 239000002904 solvent Substances 0.000 description 5
- 230000002708 enhancing effect Effects 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000010422 painting Methods 0.000 description 3
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 102000004895 Lipoproteins Human genes 0.000 description 1
- 108090001030 Lipoproteins Proteins 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- -1 acetenyl Chemical group 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000000805 composite resin Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 125000000532 dioxanyl group Chemical group 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 150000003949 imides Chemical class 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/10—Silicon-containing compounds
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Reinforced Plastic Materials (AREA)
- Moulding By Coating Moulds (AREA)
Abstract
The present invention relates to it is a kind of long when the compound electromagnetic wave transparent material of fire resistant resin base and preparation method thereof.The preparation method includes the following steps：(1) preparation of polyimide resin solution；(2) resin and quartz fibre is compound；(3) heat treatment under vacuum condition；(4) laying or winding；(5) solidification and rear solidification.Composite material prepared by the present invention is released without small molecule in the curing process, and gained composite material porosity is low；There is preferable temperature classification simultaneously, using still having preferable mechanical property and dielectric properties under the conditions of when high temperature is long, preparation process is simple, and production efficiency is high, has important engineering application value.
Description
Technical field
The present invention relates to electromagnetic wave transparent material technical field more particularly to it is a kind of long when the compound electromagnetic wave transparent material of fire resistant resin base and
Preparation method.
Background technology
Traditional fiber-reinforced resin matrix compound material (the compound electromagnetic wave transparent material of such as epoxy resin-matrix) has high specific strength, height
The excellent mechanical properties such as specific stiffness, good fatigue crack-resistant performance, but often heat resistance is poor, navigates in national defence, aviation
The application in the fields such as it is limited by larger.
Polyimide resin (PI) is a kind of very superior heat-proof macromolecule material of performance, it has higher heat resistance
(Tg>350 DEG C), preferable dielectric properties (in 50MHz hereinafter, dielectric constant is 3.1~3.3, dielectric loss is 0.006~
0.007), mechanical performance, chemical-resistant and dimensional stability are also more outstanding, are a kind of wave transparent materials with development potentiality
Material resin matrix has irreplaceable role in high temperature resistant wave-permeable material field.
The preparation method of conventional fiber-reinforced resin matrix compound material generally comprises glue preparation, prepreg system at present
Standby, three steps of curing molding.During curing molding, high temperature thermal decomposition generates carbon distribution, is easy to cause Jie of composite material
Electrical property significantly declines.It adds, the polyimide resin composite material of prepared quartz fibre enhancing at this stage is generally long
Time temperature in use is 300 DEG C~350 DEG C, and it is impossible to meet the performance requirements used for a long time under higher temperature.Simultaneously because
Thermal decomposition generates carbon distribution, its dielectric properties is caused to decline to a great extent.Currently, continued to develop with field of aerospace, it is multiple to wave transparent
The performance requirement of condensation material is higher and higher, and common composite material cannot be satisfied demand, therefore prepares a kind of high intensity, high resistance to
The composite material of hot grade is very crucial.
Invention content
(1) technical problems to be solved
The purpose of the present invention is to provide a kind of high intensity, vitreosil fiber reinforced polyimide resin composite materials.
The composite material is used in 450~500 DEG C of long-times (30min) still has mechanical property and dielectric properties, and is molded
It is released without small molecule in journey, gained composite material porosity is low.
(2) technical solution
In order to solve the above technical problem, the present invention provides following technical solutions：
The preparation method of the compound electromagnetic wave transparent material of fire resistant resin base, includes the following steps when a kind of long：
(1) preparation of polyimide resin solution：Polyimide resin is dissolved in organic solvent, polyimides is configured to
Resin solution；
(2) resin and quartz fibre is compound：Polyimide resin solution is compound with quartz textile, tree is made
Fat/quartz fibre composite material；
(3) heat treatment under vacuum condition：Composite material is hung, is then heat-treated under vacuum；
(4) laying or winding：By step (3), treated that composite material is cut into is suitably sized, by setting means into
Row laying or winding；
(5) solidification and rear solidification：Composite material temperature-pressure after laying or winding cure and is cured with after, is obtained
To the compound electromagnetic wave transparent material of resin base.
Preferably：In step (3), at 0~40 DEG C, humidity dries in the air to composite material in 40% environment below
It sets.
Preferably, the time control hung was at 5~24 hours.
Preferably：It in step (3), is heat-treated using vacuum drying oven, vacuum degree is -0.09~-0.1MPa, temperature
It it is 150 DEG C~250 DEG C, the time is 1.5~3h.
Preferably：The solidification and rear solidification are carried out stage by stage using vacuum hotpressing machine, and the process conditions in each stage are：
First cure stage：Vacuum hotpressing machine is warming up to 250 DEG C~300 DEG C and keeps the temperature 1~1.5h；
Second cure stage：Vacuum hotpressing machine is warming up to 320 DEG C~350 DEG C 5~15min of heat preservation while applying 5~20MPa
Pressure, 0.5~1h of heat-insulation pressure keeping；
Third cure stage：Vacuum hotpressing machine is warming up to 370 DEG C~380 DEG C and 2~4h of heat-insulation pressure keeping；
Cure stage after 4th：Vacuum hotpressing machine is warming up to 390 DEG C~400 DEG C and 2~4h of heat-insulation pressure keeping.
Preferably：It is using cladding process that polyimide resin solution painting is compound with quartz textile.
Preferably：Resin quality is the 50%~100% of quartz textile quality.
Preferably：The organic solvent is boiling point in 100 DEG C or more of high boiling organic solvent, preferably dioxane,
Dimethylacetylamide, N,N-dimethylformamide, N-Methyl pyrrolidone any one or more of.
Preferably：In polyimide resin solution, the mass concentration of polyimides is 15%~50%.
The present invention provides it is a kind of long when the compound electromagnetic wave transparent material of fire resistant resin base, using above-mentioned preparation method prepare and
At.
(3) advantageous effect
The above-mentioned technical proposal of the present invention has the following advantages that：
The composite material of resin and quartz fibre composition can remove organic solvent and complete when being handled in vacuum drying oven
Imidization releases small-molecule substance.Therefore it releases, effectively reduces multiple without small molecule in temperature-pressure solidification process
Condensation material porosity improves temperature classification and heat-resistant time.Solidification and rear program curing are carried out in vacuum hotpressing machine, it can
Simple flow improves efficiency, can effectively eliminate the internal stress of product, ensures to remain to keep preferable when high temperature uses for a long time
Mechanical property and dielectric properties.
The present invention prepares quartz fibre enhancing modified polyimide resin composite material and is put in the curing process without small molecule
Go out, gained composite material porosity is low；There is preferable temperature classification simultaneously, it is preferable using still having under the conditions of when high temperature is long
Mechanical property and dielectric properties, preparation process is simple, and production efficiency is high, has important engineering application value.
Description of the drawings
Fig. 1 is the flow diagram of preparation method provided by the invention.
Specific implementation mode
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this hair
Bright technical solution is clearly and completely described.Obviously, described embodiment is a part of the embodiment of the present invention, and
The embodiment being not all of.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creative work
Under the premise of the every other embodiment that is obtained, shall fall within the protection scope of the present invention.
The present invention provides it is a kind of long when the compound electromagnetic wave transparent material of fire resistant resin base preparation method, as shown in Figure 1, described
Preparation method includes the following steps：
(1) preparation of polyimide resin solution
Resin adhesive liquid used in the present invention is polyimide resin solution, is formulated using polyimide resin, solvent
Select organic solvent.When preparation, polyimide resin and organic solvent are mixed.Certainly, in order to make polyimide resin
Fully dissolving, can be stirred it, and mixing speed is no more than 400 revs/min, is advisable with 200~300 revs/min, is avoided
A large amount of bubbles are generated in solution.
In this step, there is no particular limitation for the type of polyimide resin used, existing polyimide resin
, preferably TgPolyimide resin more than 400 DEG C, for example, PMR types, acetenyl end-sealed type, soluble type.Used has
Also there is no particular limitation for the type of solvent, can dissolve polyimide resin, and (boiling point exists with higher boiling point
100 DEG C or more) organic solvent can be with, but it is preferred that organic solvent used can select dioxane, diformazan
Yl acetamide, N,N-dimethylformamide, N-Methyl pyrrolidone any one or more of.Above-mentioned organic solvent not only meets
Requirement of the boiling point at 100 DEG C or more, and there is stronger polarity, it is highly suitable for preparing polyimide resin solution.
There is no particular limitation for the concentration of polyimide resin solution used, but is preferably, prepared polyamides is sub-
The mass concentration of polyimide resin solution is 15%~50%, for example, can be specially 15%, 20%, 25%, 30%, 35%,
40%, 45%, 50%.
(2) resin and quartz fibre is compound
Polyimide resin solution is applied to, obtained resin/quartz fibre composite material compound with quartz textile.It is compound
The methods of dipping, coating, preferably painting method may be used in method.Painting method can be operated as follows：
Polyimide resin solution is dipped using coated tools such as hairbrush, is coated uniformly at least one surface of quartz textile
On.In this step, the quality of the resin of coating is the 50%~100% of quartz textile quality, for example, can be specially
50%, 60%, 70%, 80%, 90%, 100%.
When carrying out compound tense using infusion process, the tools such as steeping vat may be used and impregnated, and keep constant temperature steeping vat
Temperature makes resin solution be maintained at molten condition within the scope of 150 DEG C~180 DEG C, to impregnate.At this point, the tree in steeping vat
The mass concentration of lipoprotein solution is preferably 30%~40%.Dipping method is identical with routine techniques, and it is not described here in detail.
(3) heat treatment under vacuum condition
Composite material is hung, is then heat-treated under vacuum.In this step, composite material is dried in the air
When setting, the temperature of the environment hung is preferably at 0~40 DEG C, humidity 40% hereinafter, the time can control at 5~24 hours.
Vacuum drying oven may be used to be heat-treated, vacuum degree is -0.09~-0.1MPa, and temperature is 150 DEG C~250 DEG C, and the time is
1.5~3h.
Composite material can remove organic solvent when being handled in vacuum drying oven and complete imidization, release small point
Sub- substance.Therefore it is released without small molecule in temperature-pressure solidification process, effectively reduces composite material voidage, improve resistance to
Hot grade and heat-resistant time.
(4) laying or winding
By step (3), treated that composite material is cut into is suitably sized, and laying or winding are carried out by setting means.
(5) solidification and rear solidification
Will through laying or winding treated composite material temperature-pressure carries out solidification and after cure, the resin base is made
Compound electromagnetic wave transparent material.
The solidification and rear solidification are carried out stage by stage using vacuum hotpressing machine, and the process conditions in each stage are：
First cure stage：Vacuum hotpressing machine is warming up to 250 DEG C~300 DEG C and keeps the temperature 1~1.5h；
Second cure stage：Vacuum hotpressing machine is warming up to 320 DEG C~350 DEG C 5~15min of heat preservation while applying 5~20MPa
Pressure, 0.5~1h of heat-insulation pressure keeping；
Third cure stage：Vacuum hotpressing machine is warming up to 370 DEG C~380 DEG C and 2~4h of heat-insulation pressure keeping；
Cure stage after 4th：Vacuum hotpressing machine is warming up to 390 DEG C~400 DEG C and 2~4h of heat-insulation pressure keeping.
Conventional moulded solidification is carried out using common hot press or autoclave, then using vacuum drying oven or by the way of vacuumizing
Cure after progress, wastes the plenty of time.And the present invention carries out solidification and rear solidification using vacuum hotpressing machine, is not only able to simplify stream
Journey puies forward high efficiency, but also can effectively eliminate the internal stress of product, ensures to remain to keep preferable when high temperature uses for a long time
Mechanical property and dielectric properties.
The present invention also provides it is a kind of long when the compound electromagnetic wave transparent material of fire resistant resin base, using above-mentioned preparation method prepare and
At.
It is the embodiment that the present invention enumerates below.
Embodiment 1
The first step：Polyimide resin solution is prepared, solvent is dioxane mixing dimethylacetylamide (DMAC), solvent
Middle dioxane proportion is 70%, and polyimide resin mass percent content is 45% in solution.
Second step：Polyimide resin solution is dipped with hairbrush, is coated uniformly on quartz textile, resin quality is
Polyimide resin/quartz fibre composite material is made in the 66% of quartz textile quality.
Third walks：By above-mentioned composite material temperature be 25 DEG C, humidity be 20% environment in hang 12 hours, place into
Vacuum degree is the vacuum drying oven 200 DEG C/2h processing of -0.096MPa.
4th：The rectangle that will walk treated through third, composite material is cut into 250mm × 130mm, cuts 20 altogether
Layer, is then coated in mold.
5th step：The composite material being coated with is put into vacuum hotpressing machine and carries out cured in stages and rear solidification, it is rear to cure
After Temperature fall with pressure demoulded to 80 DEG C, obtain quartz fibre enhancing polyimide resin composite material.Wherein, respectively
Stage, specific curing process was：
First cure stage：It is warming up to 300 DEG C of heat preservation 1h；
Second cure stage：350 DEG C of heat preservation 7min are warming up to, the 10MPa that then pressurizes keeps the temperature 0.8h；
Third cure stage：It is warming up to 370 DEG C of heat-insulation pressure keeping 2.5h；
Cure stage after 4th：It is warming up to 400 DEG C of heat-insulation pressure keeping 3h.
Embodiment 2
The first step：Polyimide resin solution is prepared, solvent is n,N-Dimethylformamide, polyimide resin in solution
Mass percent content is 50%.
Second step：Resin solution is placed in steeping vat, steeping vat keeps 150 DEG C of constant temperature, will be gathered by impregnation technology
Imide resin and quartz textile are compound, polyimide resin/quartz fibre composite material are made, wherein resin solution
Quality account for quartz textile quality 50%.
Third walks：By above-mentioned composite material temperature be 30 DEG C, humidity be 20% environment in hang 24 hours, place into
Vacuum degree is the vacuum drying oven 150 DEG C/3h processing of -0.093MPa.
4th：The rectangle that will walk treated through third, composite material is cut into 250mm × 130mm, cuts 20 altogether
Layer is simultaneously coated in mold.
5th step：The composite material being coated with is put into vacuum hotpressing machine and carries out cured in stages and rear solidification, it is rear to cure
After Temperature fall with pressure demoulded to 80 DEG C, obtain quartz fibre enhancing polyimide resin composite material.Wherein, respectively
Stage, specific curing process was：
First cure stage：It is warming up to 290 DEG C of heat preservation 1h；
Second cure stage：340 DEG C of heat preservation 5min are warming up to, the 20MPa that then pressurizes keeps the temperature 0.5h；
Third cure stage：It is warming up to 375 DEG C of heat-insulation pressure keeping 3h；
Cure stage after 4th：It is warming up to 390 DEG C of heat-insulation pressure keeping 4h.
Embodiment 3 is to embodiment 5
It is substantially the same that the preparation method is the same as that of Example 1, and difference is shown in Table 1.
Comparative example 1
The preparation method and embodiment 1 of comparative example 1 are substantially the same, the difference is that：
In the third step, prepreg is dried at normal temperatures, above-mentioned heat treatment is not carried out to it.
Comparative example 2
The preparation method and embodiment 1 of comparative example 2 are substantially the same, the difference is that：
In the third step, the prepreg after hanging is heat-treated in normal drying case, the temperature of heat treatment is 200
DEG C, time 2h.
Comparative example 3
The preparation method and embodiment 1 of comparative example 3 are substantially the same, the difference is that：
In the 4th step, cured using autoclave, is specifically comprised the following steps：The quartz fibre being coated with is enhanced
Modified polyimide resin prepreg, which is put into autoclave, to be cured, and specific curing process is：2h is kept the temperature at 240 DEG C, so
Keep the temperature 2h at 370 DEG C again afterwards.
After 10min being kept the temperature using resin composite materials made from the various embodiments described above and comparative example at 450 DEG C, test material
Mechanical property, specific performance test result are as shown in table 2.
Table 2
The prepreg in preparation method provided by the invention is can be seen that in vacuum drying oven from the testing result of table 2
Organic solvent can be removed when reason and completes imidization, release small-molecule substance, therefore in temperature-pressure solidification process
Middle no small molecule is released, and is effectively reduced composite material porosity, is improved temperature classification and heat-resistant time；In vacuum hotpressing machine
In carry out solidification and rear program curing, the internal stress of product can be effectively eliminated, ensure high temperature for a long time use when remain to protect
Hold preferable mechanical property and dielectric properties.Even if being made under 450 DEG C of this high temperature using composite material made from this method
Still there is preferable mechanical performance and electric property with 10min.By verification, composite material produced by the present invention makes at 500 DEG C
With still having preferable mechanical performance and electric property after 30min, there is important engineering application value.
Finally it should be noted that：The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, it will be understood by those of ordinary skill in the art that：It still may be used
With technical scheme described in the above embodiments is modified or equivalent replacement of some of the technical features；
And these modifications or replacements, various embodiments of the present invention technical solution that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (10)
1. the preparation method of the compound electromagnetic wave transparent material of fire resistant resin base when a kind of long, it is characterised in that：Include the following steps：
(1) preparation of polyimide resin solution：Polyimide resin is dissolved in organic solvent, polyimide resin is configured to
Solution；
(2) resin and quartz fibre is compound：Polyimide resin solution is compound with quartz textile, resin/stone is made
English fibrous composite；
(3) heat treatment under vacuum condition：Composite material is hung, is then heat-treated under vacuum；
(4) laying or winding：By step (3), treated that composite material is cut into is suitably sized, is spread by setting means
Layer or winding；
(5) solidification and rear solidification：Composite material temperature-pressure after laying or winding cure and is cured with after, institute is obtained
State the compound electromagnetic wave transparent material of resin base.
2. preparation method according to claim 1, it is characterised in that：In step (3), at 0~40 DEG C, humidity exists
Composite material is hung in 40% environment below.
3. preparation method according to claim 2, it is characterised in that：The time control hung was at 5~24 hours.
4. according to claim 1-3 any one of them preparation methods, it is characterised in that：In step (3), using vacuum drying oven
It is heat-treated, vacuum degree is -0.09~-0.1MPa, and temperature is 150 DEG C~250 DEG C, and the time is 1.5~3h.
5. preparation method according to claim 1, it is characterised in that：The solidification and rear solidification are using vacuum hotpressing machine point
Stage carries out, and the process conditions in each stage are：
First cure stage：Vacuum hotpressing machine is warming up to 250 DEG C~300 DEG C and keeps the temperature 1~1.5h；
Second cure stage：Vacuum hotpressing machine is warming up to 320 DEG C~350 DEG C 5~15min of heat preservation while applying the pressure of 5~20MPa
Power, 0.5~1h of heat-insulation pressure keeping；
Third cure stage：Vacuum hotpressing machine is warming up to 370 DEG C~380 DEG C and 2~4h of heat-insulation pressure keeping；
Cure stage after 4th：Vacuum hotpressing machine is warming up to 390 DEG C~400 DEG C and 2~4h of heat-insulation pressure keeping.
6. according to claim 1-3 any one of them preparation methods, it is characterised in that：Using cladding process by polyimide resin
Solution applies compound with quartz textile.
7. preparation method according to claim 6, it is characterised in that：Resin quality is the 50% of quartz textile quality
~100%.
8. according to claim 1-3 any one of them preparation methods, it is characterised in that：The organic solvent is boiling point 100
DEG C or more high boiling organic solvent, preferably dioxane, dimethylacetylamide, n,N-Dimethylformamide, N- methyl pyrroles
Pyrrolidone any one or more of.
9. preparation method according to claim 8, it is characterised in that：In polyimide resin solution, the matter of polyimides
Measure a concentration of 15%~50%.
10. fire resistant resin base compound electromagnetic wave transparent material when a kind of long, it is characterised in that：Described in claim any one of 1-9
Preparation method be prepared.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810244205.2A CN108299825B (en) | 2018-03-23 | 2018-03-23 | Long-time high-temperature-resistant resin-based composite wave-transmitting material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810244205.2A CN108299825B (en) | 2018-03-23 | 2018-03-23 | Long-time high-temperature-resistant resin-based composite wave-transmitting material and preparation method thereof |
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| CN109483908A (en) * | 2018-11-26 | 2019-03-19 | 航天特种材料及工艺技术研究所 | A kind of compound material insulation end hoop and preparation method thereof |
| CN112391052A (en) * | 2020-11-13 | 2021-02-23 | 航天特种材料及工艺技术研究所 | Foam material and preparation method thereof |
| CN114315690A (en) * | 2022-03-04 | 2022-04-12 | 北京玻钢院复合材料有限公司 | Imide ring-containing bisphthalonitrile compound, high-heat-resistance wave-transmitting composite material and preparation method thereof |
| CN115449219A (en) * | 2022-09-01 | 2022-12-09 | 中国建筑材料科学研究总院有限公司 | Silica aerogel quartz fiber polyimide ternary composite material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109483908A (en) * | 2018-11-26 | 2019-03-19 | 航天特种材料及工艺技术研究所 | A kind of compound material insulation end hoop and preparation method thereof |
| CN112391052A (en) * | 2020-11-13 | 2021-02-23 | 航天特种材料及工艺技术研究所 | Foam material and preparation method thereof |
| CN114315690A (en) * | 2022-03-04 | 2022-04-12 | 北京玻钢院复合材料有限公司 | Imide ring-containing bisphthalonitrile compound, high-heat-resistance wave-transmitting composite material and preparation method thereof |
| CN114315690B (en) * | 2022-03-04 | 2022-06-21 | 北京玻钢院复合材料有限公司 | Imide ring-containing bisphthalonitrile compound, high-heat-resistance wave-transmitting composite material and preparation method thereof |
| CN115449219A (en) * | 2022-09-01 | 2022-12-09 | 中国建筑材料科学研究总院有限公司 | Silica aerogel quartz fiber polyimide ternary composite material and preparation method and application thereof |
| CN115449219B (en) * | 2022-09-01 | 2024-02-02 | 中国建筑材料科学研究总院有限公司 | Silica aerogel quartz fiber polyimide ternary composite material and preparation method and application thereof |
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