CN105237958A - Preparation method of high-performance epoxy resin based carbon fiber composite material - Google Patents
Preparation method of high-performance epoxy resin based carbon fiber composite material Download PDFInfo
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Abstract
The invention provides a preparation method of a high-performance epoxy resin based carbon fiber composite material. The preparation method comprises the steps of preparing an NY9200GB resin system from glycidyl ether type epoxy resin, o-cresol formaldehyde epoxy resin, an L-curing agent, an acetone diluting agent and a polyaryletherketone flexibilizer, preparing a carbon fiber or glass fiber prepreg by virtue of a hot melting method, determining forming process parameters of the carbon fiber prepreg by virtue of a process parameter research test, and preparing a composite material component by virtue of an autoclave method or a mold pressing method. Various indexes of the epoxy resin based carbon fiber composite material prepared by virtue of the preparation method are hardly changed after the epoxy resin based carbon fiber composite material is preserved at natural conditions for 15 years.
Description
Technical field
The present invention relates to a kind of carbon-fibre composite and moulding process thereof, carbon-fibre composite preparing technical field.
Background technology
When resin-based carbon fiber composite uses under field conditions (factors), the interface of resin matrix and fiber and resin is subject to the impact of environmental factors, will cause interfacial failure, and degradation, state change, so that scrap.The aging of polymer matrix composite is divided into atmospheric ageing and artificial accelerated aging, and due to weather aging length consuming time, after the weathering test of more than ten years, will not catch up with the update of material, therefore, artificial accelerated aging is favored by investigator day by day.
Hygrothermal environment condition produces material impact to the matrix of polymer matrix composite, the difference of fiber and the basic thermal expansivity of resin under high temperature, causes interface to produce internal stress, under the effect of moisture, make interface produce tiny crack, destroy interface structure, reduce the bonding force between interface.Based on this understanding, provide according to the moisture absorption rate of diffusion under DIFFERENT WET thermal environment or the test of the hydrothermal effect under DIFFERENT WET thermal environment the experience engineering formula accelerating moisture absorption (aging) and calculate speedup factor.
The present invention is by adding a certain proportion of o-cresol formaldehyde epoxy resin (PGCN-700-3S) in diglycidyl ether type epoxy resin (E-54), use L-solidifying agent, add thermoplastic resin polyaryletherketone (PEK-C), be prepared into epoxy-resin systems.By the debugging of formula, achieve two step hot melt processs and prepare epoxy resin base carbon fiber prepreg; Grope test by processing parameter, determine best molding technique parameter.The advanced epoxy resin base carbon fiber composite material of preparation is put 15 years under field conditions (factors), and property indices does not almost change.
Summary of the invention
The object of the present invention is to provide a kind of performance resins system of weather resistance, for the preparation of the composite product of aviation main load-bearing part.
The present invention is by suitable proportioning, diglycidyl ether type epoxy resin, o-cresol formaldehyde epoxy resin, L-solidifying agent, acetone diluted agent, polyaryletherketone toughner are configured to NY9200GB resin system, carbon fiber or glass cloth prepreg is prepared into through hot melt process, by processing parameter research trial, determine the molding technique parameter of carbon fiber prepreg, adopt autoclave method or compression molding to be prepared into composite product.
A kind of high-performance epoxy resin, is characterized in that: prepare according to the following steps:
1) by diglycidyl ether type epoxy resin and o-cresol formaldehyde epoxy resin with (75 ~ 85): the mass ratio of (25 ~ 15), by two kinds of mixed with resin, dissolves and obtains component A;
2) mix with the mass ratio of 85:12 by component A and PEK-C, when being warming up to 40 DEG C ~ 45 DEG C, turn on agitator keeps 8min ~ 12min, continues to be warming up to 135 DEG C ~ 155 DEG C, and insulation 1h ~ 2h, to as clear as crystal, is called B component;
3) by component A and L-solidifying agent with 15:(6 ~ 10) quality than pre-mixing, put into three roller runner millings and mill, roll spacing is successively reduced to two rods by 0.1mm and contacts with each other, and is called component C;
4) take required weight by B component and component C with the requirement of 97:23, put into the mixing that the double star wall-hanging mixing machine of 70 DEG C ~ 75 DEG C or kneader carry out 0.5h ~ 1h, make it evenly namely to obtain NY9200GB resin system.
A kind of preparation method of high-performance epoxy resin base carbon fiber composite material, it is characterized in that step is as follows: with T700SC-12000-50C carbon fiber for strongthener and NY9200GB resin system for NY9200GB/T700SC carbon-fibre composite prepared by body material, size needed for the paving of NY9200GB/T700SC carbon fiber prepreg is become, complete with vacuum bag sealing, during product laying, every 8 layers of prepreg once vacuumize, vacuum pressure keeps 25 minutes, glue-line is inhaled depending on feelings lay, pre-compacted and exhaust, the vacuum pressure of prefabricated component is not less than-0.095MPa and enters autoclave, unloading vacuum pressure, be warming up within the scope of 145 DEG C ± 5 DEG C with the speed of≤3 DEG C/min, be forced into 0.6MPa ~ 0.7MPa, insulation 40min ~ 60min, be warming up between 175 DEG C ~ 180 DEG C with the speed of≤3 DEG C/min, after insulation 2h ~ 2.5h, room temperature is down to the speed of≤3 DEG C/min.
Advantage of the present invention: NY9200GB resin system is applicable to a step hot melt process and two step hot melt processs produce carbon fiber prepreg and glass cloth prepreg; Carbon-fibre composite and glass cloth composite is prepared by autoclave method and compression molding.In the carbon-fibre composite 70 DEG C of preparation and 85%RH environmental cabinet, accelerated deterioration in 70 days is equivalent to the weather aging of storing 14 years and storing under condition 1 year under storehouse condition in the open.Therefore, the environmental resistance of this matrix material is better, can store at ambient temperature for a long time.
Accompanying drawing explanation
Fig. 1 is the viscosity-temperature curve of NY9200GB resin system.
Fig. 2 is the gel time of resin and prepreg.
Fig. 3 is the dsc analysis of NY9200GB resin curing time.
Fig. 4 is molding technique parameter figure.
Embodiment
Embodiment 1
One, NY9200GB resin system preparation
NY9200GB resin system is prepared according to the following steps:
1) by diglycidyl ether type epoxy resin (E-54) and o-cresol formaldehyde epoxy resin (PGCN-700-3S) with the proportioning of 80:20 (mass ratio) by two kinds of mixed with resin, when being warming up to 125 DEG C ~ 130 DEG C, turn on agitator, until two kinds of resins dissolve completely.Be called component A.
2) bi-material is mixed with the proportioning of 85:12 by component A and PEK-C, when being warming up to 40 DEG C ~ 45 DEG C, turn on agitator keeps 8min ~ 12min, continue to be warming up to 135 DEG C ~ 155 DEG C, insulation 1h ~ 2h, to as clear as crystal (depending on amount), is called B component.
3) by component A and L-solidifying agent with the proportioning pre-mixing of 15:8, put into three roller runner millings (roller temperature is no more than 40 DEG C and is advisable) and carry out being no less than three times milling, roll spacing is successively reduced to two rods by 0.1mm and contacts with each other, and is called component C.
4) required weight is taken by B component and component C with the requirement of 97:23, put into the mixing that the double star wall-hanging mixing machine of 70 DEG C ~ 75 DEG C or kneader carry out 0.5h ~ 1h, make it evenly (can visual inspection after very thin painting one deck on silex glass) and namely obtain NY9200GB resin system.
The physicals of NY9200GB resin system and typical mechanical property are in table 1.
The physicals of table 1NY9200GB resin system and typical mechanical property
Two, viscosity-temperature curve and gel time
Prepare by two step hot melt processs the preparation that resin base prepreg first need carry out glued membrane, then carry out the preparation of prepreg, compare and a step hot melt process, the precision controlling of gel content is higher, can reduce the waste of resin and fiber, is conducive to improving composite product qualification rate.When carrying out two step hot melt processs and preparing, masking temperature and resin viscosity are very important processing parameters, directly affect the fiber volume fraction of follow-up composite product, fiber volume fraction number directly affect the strength and modulus size of matrix material.According to regulation in MIL-HDBK-17K " matrix material handbook ", the fiber volume fraction of matrix material is most suitable between 45% ~ 65%, in conjunction with the demand of model design strength, we specify that fiber volume fraction is 60%, according to the density of T700SC-12000-50C fibre density and NY9200GB resin system, the gel content massfraction calculating composite product is best 30% ± 3%.
As shown in Figure 1, after temperature rises to 90 DEG C, the increase of viscosity with temperature tends towards stability, and is down to low spot, (90 DEG C time, gel time is longer, is conducive to the production of glued membrane and prepreg for the gel time (see Fig. 2) of binding resin and the industrialization demand of carbon fiber prepreg.), be finally selected in 90 DEG C and be filmed.
Three, moulding process
According to the result of gel time (see Fig. 2) and DSC curve (see Fig. 3), we have selected and carry out the test of different soaking time at 130 DEG C and 145 DEG C, and result shows, at 145 DEG C of insulation 30 ~ 60min, the thickness of veneer sheet is in teachings, and better performances.The results are shown in Table 2.
The different soaking time of table 2 is on the impact of laminate properties
In order to determine the impact on laminate properties under different pressures, We conducted the test of neutralizing layer pressing plate performance under different pressures, result shows, better in the veneer sheet over-all properties of 0.5MPa ~ 0.6MPa compacting, in table 3 and table 4.
The different solidifying pressure of table 3 is on the impact of laminate properties
Table 4 different set time is on the impact of laminate properties
In sum, first holding stage is within the scope of 145 DEG C ± 5 DEG C, and be incubated 40min ~ 60min, the viscosity of this stage resin is lower, and mobility is better, and fiber fully floods, and volatilizable thing volatilizees and discharges; Second holding stage, between 175 DEG C ~ 180 DEG C, makes resin fully solidify, and the viscosity of resin is tending towards maximum gradually, and structural strength have also been obtained increase simultaneously.Draw out the moulding process figure (Fig. 4) of carbon-fibre composite.
Size needed for the paving of NY9200GB/T700SC carbon fiber prepreg is become, complete with vacuum bag sealing, during product laying, every 8 layers of prepreg once vacuumize, vacuum pressure keeps 25 minutes, glue-line is inhaled depending on feelings lay, pre-compacted and exhaust, the vacuum pressure of prefabricated component is not less than-0.095MPa and enters autoclave, unloading vacuum pressure, be warming up within the scope of 145 DEG C ± 5 DEG C with the speed of≤3 DEG C/min, be forced into 0.6MPa ~ 0.7MPa, insulation 40min ~ 60min, be warming up between 175 DEG C ~ 180 DEG C with the speed of≤3 DEG C/min, after insulation 2h ~ 2.5h, room temperature is down to the speed of≤3 DEG C/min., as shown in Figure 4.
The basic mechanical performance representative value of the composite material laminated board of compacting is shown in Table 5, and B benchmark value is shown in Table 6.
The mechanical properties value of table 5 composite material laminated board
| Sequence number | Test subject | Test-results |
| 1 | Degree of cure, % | 95.22 |
| 2 | Flexural strength, MPa | 1750 |
| 3 | Modulus in flexure, GPa | 129 |
| 4 | Interlaminar shear strength, MPa | 86.5 |
| 5 | Longitudinal-transverse shear intensity, MPa | 134 |
| 6 | Longitudinal-transverse shear modulus, GPa | 6.13 |
| 7 | Longitudinal tensile strength, MPa | 2647 |
| 8 | Longitudinal tensile, GPa | 149 |
| 9 | Poisson's ratio | 0.312 |
| 10 | Longitudinal compressive strength, MPa | 1262 |
| 11 | Longitudinal compression modulus, GPa | 111 |
| 12 | Horizontal compression intensity, MPa | 199 |
| 13 | Transverse compressive modulus, GPa | 9.4 |
| 14 | Transverse tensile strength, MPa | 61.8 |
| 15 | Cross directional stretch modulus, GPa | 9.94 |
| 16 | Perforate tensile strength, MPa | 516 |
| 17 | Perforate tensile modulus, GPa | 47.8 |
| 18 | Perforate compressive strength, MPa | 310 |
| 19 | Double shear crushing strength, MPa | 1109 |
| 20 | Post-impact compression, MPa | 224 |
The B benchmark value of table 6NY9200GB/T700SC matrix material
| Sequence number | Project | B benchmark value |
| 1 | Interlaminar shear strength, MPa | 75.3 |
| 2 | Transverse tensile strength, MPa | 54.2 |
| 3 | Longitudinal tensile strength, MPa | 1611 |
| 4 | Horizontal compression intensity, MPa | 154 |
| 5 | Longitudinal compressive strength, MPa | 1039 |
| 6 | Longitudinal-transverse shear intensity, MPa | 103 |
| 7 | Buckling strength, MPa | 1503 |
Four, environmental resistance and ageing-resistant performance
According to principle and the acceleration principle of accelerated deterioration, temperature lower than the wet glass transition temperature of epoxy matrix (this resin hygrometric state Tg is 120 DEG C), generally will be no more than 70 DEG C and be advisable, the additional of epoxy matrix can not be caused like this to degrade.In MIL-HDBK-17F, envrionment conditions epoxy matrix composite being accelerated to moisture absorption is also 70 DEG C and 85%RH.Result of study shows, hydrolytic action after mainly its moisture absorption that degrades of polymkeric substance, degrade under also all occurring in saturated sucting wet state, based on this understanding, just can provide according to the moisture absorption rate of diffusion under DIFFERENT WET thermal environment or the test of the hydrothermal effect under DIFFERENT WET thermal environment the experience engineering formula accelerating moisture absorption (aging) and calculate speedup factor.According to the condition of storage selected and accelerated deterioration environment, calculate acceleration hygroscopic coefficient according to the first method in " composite structure design manual " (aircraft industry press, ISBN7-80134-939-3,2001).
In formula:
K---time accelerator coefficient;
T
1---the actual time of exposing to the open air;
T
2---the time after acceleration;
T
1φ
1---the actual temperature (DEG C) that exposes to the open air and relative humidity;
T
2φ
2---the temperature (DEG C) of acceleration environment and relative humidity.
C---test coefficient, generally gets C=46.1.
Known according to table 7, after carrying out 15 years aging, the conservation rate of its properties is higher.
Table 7NY9200GB/T700SC composite material test piece accelerated weathering test result
The medium-resistance of table 8NY9200GB/T700SC matrix material
Embodiment 2
NY9200GB resin system is prepared according to the following steps:
1) by diglycidyl ether type epoxy resin (E-54) and o-cresol formaldehyde epoxy resin (PGCN-700-3S) with the proportioning of 75:25 (mass ratio) by two kinds of mixed with resin, when being warming up to 125 DEG C ~ 130 DEG C, turn on agitator, until two kinds of resins dissolve completely.Be called component A.
2) bi-material is mixed with the proportioning of 85:12 by component A and PEK-C, when being warming up to 40 DEG C ~ 45 DEG C, turn on agitator keeps 8min ~ 12min, continue to be warming up to 135 DEG C ~ 155 DEG C, insulation 1h ~ 2h, to as clear as crystal (depending on amount), is called B component.
3) by component A and L-solidifying agent with the proportioning pre-mixing of 15:10, put into three roller runner millings (roller temperature is no more than 40 DEG C and is advisable) and carry out being no less than three times milling, roll spacing is successively reduced to two rods by 0.1mm and contacts with each other, and is called component C.
4) required weight is taken by B component and component C with the requirement of 97:23, put into the mixing that the double star wall-hanging mixing machine of 70 DEG C ~ 75 DEG C or kneader carry out 0.5h ~ 1h, make it evenly (can visual inspection after very thin painting one deck on silex glass) and namely obtain NY9200GB resin system.
Embodiment 3
NY9200GB resin system is prepared according to the following steps:
1) by diglycidyl ether type epoxy resin (E-54) and o-cresol formaldehyde epoxy resin (PGCN-700-3S) with the proportioning of 85:15 (mass ratio) by two kinds of mixed with resin, when being warming up to 125 DEG C ~ 130 DEG C, turn on agitator, until two kinds of resins dissolve completely.Be called component A.
2) bi-material is mixed with the proportioning of 85:12 by component A and PEK-C, when being warming up to 40 DEG C ~ 45 DEG C, turn on agitator keeps 8min ~ 12min, continue to be warming up to 135 DEG C ~ 155 DEG C, insulation 1h ~ 2h, to as clear as crystal (depending on amount), is called B component.
3) by component A and L-solidifying agent with the proportioning pre-mixing of 15:6, put into three roller runner millings (roller temperature is no more than 40 DEG C and is advisable) and carry out being no less than three times milling, roll spacing is successively reduced to two rods by 0.1mm and contacts with each other, and is called component C.
4) required weight is taken by B component and component C with the requirement of 97:23, put into the mixing that the double star wall-hanging mixing machine of 70 DEG C ~ 75 DEG C or kneader carry out 0.5h ~ 1h, make it evenly (can visual inspection after very thin painting one deck on silex glass) and namely obtain NY9200GB resin system.
Claims (5)
1. a high-performance epoxy resin, is characterized in that: prepare according to the following steps:
1) by diglycidyl ether type epoxy resin and o-cresol formaldehyde epoxy resin with (75 ~ 85): the mass ratio of (25 ~ 15), by two kinds of mixed with resin, dissolves and obtains component A;
2) mix with certain mass ratio by component A and PEK-C, when being warming up to 40 DEG C ~ 45 DEG C, turn on agitator keeps 8min ~ 12min, continues to be warming up to 135 DEG C ~ 155 DEG C, and insulation 1h ~ 2h, to as clear as crystal, is called B component;
3) by component A and solidifying agent with 15:(6 ~ 10) quality than pre-mixing, put into three roller runner millings and mill, roll spacing is successively reduced to two rods by 0.1mm and contacts with each other, and is called component C;
4) take required weight with certain mass than requirement by B component and component C, put into the mixing that the double star wall-hanging mixing machine of 70 DEG C ~ 75 DEG C or kneader carry out 0.5h ~ 1h, make it evenly namely to obtain NY9200GB resin system.
2. high-performance epoxy resin according to claim 1, is characterized in that: by the mass ratio of component A and PEK-C be: 85:12.
3. high-performance epoxy resin according to claim 1, is characterized in that: the mass ratio of B component and component C is 97:23.
4. the preparation method of a high-performance epoxy resin base carbon fiber composite material, it is characterized in that: with the NY9200GB resin system of T700SC-12000-50C carbon fiber prepared by strongthener and claim 1 for NY9200GB/T700SC carbon-fibre composite prepared by body material, size needed for the paving of NY9200GB/T700SC carbon fiber prepreg is become, complete with vacuum bag sealing, during product laying, every 8 layers of pre-prepreg of carbon fiber once vacuumize, glue-line is inhaled depending on feelings lay, pre-compacted and exhaust, unloading vacuum pressure, be warming up within the scope of 145 DEG C ± 5 DEG C, be forced into 0.6MPa ~ 0.7MPa, insulation 40min ~ 60min, be warming up between 175 DEG C ~ 180 DEG C, after insulation 2h ~ 2.5h, be down to room temperature.
5. the preparation method of high-performance epoxy resin base carbon fibre prepreg according to claim 4 and matrix material, is characterized in that: temperature rise rate≤3 DEG C/min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109624168A (en) * | 2018-10-31 | 2019-04-16 | 广东出入境检验检疫局检验检疫技术中心 | A kind of self-lubricating groove type rubbing device and preparation method thereof |
| CN112192864A (en) * | 2020-08-25 | 2021-01-08 | 航天材料及工艺研究所 | Automatic prepreg laying process parameter determining device |
| CN113418560A (en) * | 2021-06-29 | 2021-09-21 | 哈尔滨工业大学 | Equipment and method for rapidly formulating molding process parameters of resin-based composite material |
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