CN109608827A - A kind of preparation method of vacuum flexible bag moulding high tenacity prepreg and its composite material - Google Patents
A kind of preparation method of vacuum flexible bag moulding high tenacity prepreg and its composite material Download PDFInfo
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- CN109608827A CN109608827A CN201811546202.0A CN201811546202A CN109608827A CN 109608827 A CN109608827 A CN 109608827A CN 201811546202 A CN201811546202 A CN 201811546202A CN 109608827 A CN109608827 A CN 109608827A
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- prepreg
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- composite material
- resin
- toughener
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
- C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2479/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2481/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
- C08J2481/06—Polysulfones; Polyethersulfones
-
- 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
- C08K7/06—Elements
Abstract
The invention belongs to prepreg and its technical field of composite material manufacturing, it is related to the preparation method of a kind of vacuum flexible bag moulding high tenacity prepreg and its composite material.Pre-preg vacuum bag pressure technique is a kind of Composites Molding Techniques of low cost, lower to equipment site requirements, easy to promote and utilize, but the problem that vacuum bag presses the generally existing toughness of composite material of technique preparation poor.The invention proposes a kind of vacuum flexible bag moulding high tenacity prepreg and its composite materials, resin is modified using the toughener of specific structure size, prepared prepreg is using the impregnated structures being partly impregnated with, after resin directed flow, toughener can be enriched to composite fiber interlayer region, form toughening layer.The composite structure is able to suppress the generation of crackle and the extension along interlayer under shock loading, reduces damaged area, greatly improves the toughness properties of composite material.
Description
Technical field
The invention belongs to prepreg and its technical field of composite preparation, and it is pre- to be related to a kind of vacuum flexible bag moulding high tenacity
The preparation method of leaching material and its composite material.
Background technique
The composite property of autoclave forming process preparation is excellent, quality is reliable and stable, is currently mostly important answer
Condensation material forming method, but its high process costs is denounced by people always.Vacuum flexible bag moulding technique (VBO) is not necessarily to autoclave
Tank pressure, only need to by vacuum pressure, since autoclave equipment cost is much higher than the baking oven of same volume, will presoak
Material is a kind of important inexpensive composite technology using vacuum bag pressure technological forming composite material.
Compared with autoclave process, the advantage of vacuum flexible bag moulding technique is that manufacturing cost is substantially reduced, but there is also
Two problems: first is that composite inner is second-rate.Since the briquetting pressure of vacuum bag pressure technique is far below autoclave process,
It is unfavorable for inhibiting the generation of composite inner hole, causes the porosity of composite inner after forming higher.It is true to reduce
Porosity in the molded composite material of empty bag, can be by optimizing the viscosity of resin system and the knot of reactivity, prepreg
The methods of configuration formula (most important method is using semi permeability impregnated structures) is controlled, to improve the inside of composite material
Quality.
Another problem is that the toughness properties of composite material are lower.The composite inner quality of vacuum bag pressure technological forming
When good, the basic mechanical performances such as stretching, compression, bending, short beam shear and autoclave molding composite material are comparable, but
Toughness properties are generally much lower.It is modified this is because prepreg generally requires addition toughener with resin matrix, toughening
The addition of agent can obviously increase the viscosity of resin system.When using autoclave molding, higher pressure can promote resin to flow,
And the gap of the formation such as not discharged gas, volatile matter is compressed, and ensure that composite inner quality after molding is preferable, and it is true
The molded operation pressure of empty bag is much lower, to ensure composite inner quality, can not only add or add in resin matrix and is few
The toughener of amount, thus cause the toughness of composite material poor.
For the toughening methods of composite material, presently the most effective method is interlayer toughened.Interlayer toughened is different from passing
The resin matrix entirety toughening of system, but the toughening area of composite material is mainly limited to the fiber interlayer of composite material.Interlayer
The composite material of toughening has certain thickness in fiber interlayer region, this significantly increases the area in interlayer area, is conducive to
The formation of crack tip plastic zone, extension of the crackle in interlayer area can also dissipate bigger energy, to reduce composite layer
Between damaged area, improve the toughness properties of composite material.In particular, by toughening layer control to composite material interlayer when, to tree
Required toughening agent content is little for resin system.
Therefore, how by toughening layer control to composite material interlayer region, prepared using vacuum flexible bag moulding technique
The composite material of high tenacity is particularly important.
Summary of the invention
The purpose of the present invention is to propose to a kind of vacuum flexible bag moulding high tenacity prepreg and its composite material and preparation method thereof,
Wherein, resin matrix is modified using the toughener of specific structure size, and prepared prepreg is using the dipping being partly impregnated with
Structure selects resin viscosity in the corresponding temperature range of 5~15Pas, and setting keeps the temperature platform, and resin is not impregnated with area to prepreg
Flowing, so that toughener be made to be enriched to fiber interlayer region, greatly improves the toughness properties of composite material.
Technical solution of the present invention is as follows: the preparation side of a kind of vacuum flexible bag moulding high tenacity prepreg and its composite material
Method, which comprises the steps of:
1) resin matrix is modified using toughener；
It 2) is the prepreg for being partly impregnated with structure by the modified resin base bluk recombination in reinforcing fiber and step 1)；
3) prepreg for being partly impregnated with structure in step 2 is pressed into technological forming using vacuum bag, by resin directed flow,
Under the filtering effect of reinforcing fiber, toughener is made to be enriched to composite fiber interlayer region, forms toughening layer.
Preferably, toughener described in step 1) is polysulfones, polyether sulfone, polyether-ketone, polyether-ether-ketone, polyether ketone ketone, gathers
The combination of one or both of amide, polyimides, polyetherimide, polyurethane, polyphenylene oxide or more.
Preferably, toughener described in step 1) is having a size of 2~10 μm.
Preferably, resin matrix being modified described in step 1) using toughener, toughener weight content is 3~
10%.
Preferably, reinforcing fiber described in step 2) is carbon fiber, glass fibre, basalt fibre.
Preferably, structure prepreg is partly impregnated with described in step 2), degree of steeping is 30~70%.
Preferably, composite material described in step 3), fiber volume fraction are 50~60%.
Preferably, resin directed flow described in step 3), method are selection resin viscosities at 5~15Pas pairs
The temperature range answered, setting heat preservation platform make resin be not impregnated with area to prepreg and flow.
It is an advantage of the invention that the vacuum flexible bag moulding high tenacity prepreg and its composite material that propose, using low cost
Method can form the composite material of high tenacity, facilitate the toughness properties of composite material close to the level of autoclave process
The large scale application of composite material will generate high economic benefit.
Detailed description of the invention
Fig. 1 is high tenacity prepreg structure evolution schematic diagram
Fig. 2 is the non-toughening composition laminate microstructure that technological forming is pressed using vacuum bag
Fig. 3 is the toughening composition laminate microstructure that technological forming is pressed using vacuum bag
Specific embodiment
The present invention is described in further details below by embodiment.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention.It should be pointed out that those skilled in the art, not departing from structure of the present invention
The several modifications and improvements made under the premise of think of, belong to protection scope of the present invention.
Embodiment 1
The present embodiment is vacuum flexible bag moulding high tenacity prepreg and its composite material and preparation method thereof.As shown in Figure 1, step
It is as follows:
1) resin selects vacuum bag pressure technique with epoxy resin LT90 (composite material Co., Ltd, Air China product).Using flat
The thermoplastic polyimide powder that equal partial size is 5 μm carries out toughening modifying to epoxy resin LT90, and polyimides powder is in epoxy
Weight accounting in resin is 7%, and mixture is uniformly mixed through three-roller；
2) reinforcing material is used as using CCF800 carbon fiber (Tuozhan Fiber Co., Ltd., Weihai's product), using hot melt work
Skill prepares prepreg, and prepreg fiber areal densities are 145g/m2, resin content 35%.The compound temperature of carbon fiber and resin film
Degree is 80 DEG C, throughput rate 2mm/min, and prepared prepreg is partly to be impregnated with state, degree of steeping 40% at this time；
3) prepreg is subjected to blanking, paving, then using vacuum bag pressure technique to being packaged.In curing molding process
In, 120 DEG C are selected as heat preservation step, and time 90min, epoxy resin LT90 viscosity exists in 10Pas or so, resin at this time
Area is not impregnated with to prepreg under vacuum pressure effect to migrate, and thermoplastic polyimide powder is by fibrous insulation, no normal direction preimpregnation
It is not impregnated with area's flowing inside material, so that polyimides powder be made to be enriched to fiber interlayer, being formed has certain thickness toughening
Layer.As shown in Figure 2 and Figure 3, prepreg laminate is warming up to 180 DEG C of heat preservation 2h later, completes the curing molding of composite material.
4) composite material is subjected to sample processing and test according to corresponding testing standard, from the point of view of test result, before toughening
The basic poor mechanical property of composite material is different less afterwards, but the toughness properties (CAI) of composite material improve 60% after toughening, toughening
Front and back composite property is as follows:
| Test item | Test method | Before toughening | After toughening |
| 0 ° of tensile strength/MPa | ASTM D3039 | 2503 | 2579 |
| 0 ° of stretch modulus/GPa | ASTM D3039 | 161 | 155 |
| 0 ° of compressive strength/MPa | ASTM D6641 | 1075 | 1058 |
| 0 ° of compression modulus/GPa | ASTM D6641 | 146 | 145 |
| Bending strength/MPa | ASTM D7264 | 1898 | 1976 |
| Bending modulus/GPa | ASTM D7264 | 139 | 137 |
| Longitudinal-transverse shear intensity/MPa | ASTM D3518 | 84.2 | 97.6 |
| Longitudinal-transverse shear modulus/GPa | ASTM D3518 | 3.8 | 4.0 |
| CAI/MPa | ASTM D7136&7137 | 153 | 245 |
Embodiment 2
The present embodiment is vacuum flexible bag moulding high tenacity prepreg and its composite material and preparation method thereof.Steps are as follows:
1) resin selects vacuum bag to press technique epoxy resin LT90.Use average grain diameter for 3 μm of thermoplastic poly ether sulfone
Powder carries out toughening modifying to epoxy resin LT90, and the weight accounting of polyether sulfone powder in the epoxy is 6%, by mixture
It is uniformly mixed through three-roller；
2) reinforcing material is used as using CCF300 carbon fiber (Tuozhan Fiber Co., Ltd., Weihai's product), using hot melt work
Skill prepares prepreg, and prepreg fiber areal densities are 133g/m2, resin content 34%.The compound temperature of carbon fiber and resin film
Degree is 80 DEG C, throughput rate 2mm/min, and prepared prepreg is partly to be impregnated with state, degree of steeping 50% at this time；
3) prepreg is subjected to blanking, paving, then using vacuum bag pressure technique to being packaged.In curing molding process
In, 120 DEG C are selected as heat preservation step, and time 90min, epoxy resin LT90 viscosity exists in 10Pas or so, resin at this time
Area is not impregnated with to prepreg under vacuum pressure effect to migrate, and thermoplastic poly ether sulfone powder is by fibrous insulation, no normal direction prepreg
Internal is not impregnated with area's flowing, so that polyether sulfone powder be made to be enriched to fiber interlayer, being formed has certain thickness toughening layer.It
Prepreg laminate is warming up to 180 DEG C of heat preservation 2h afterwards, completes the curing molding of composite material.
4) composite material is subjected to sample processing and test according to corresponding testing standard, from the point of view of test result, before toughening
The basic poor mechanical property of composite material is different less afterwards, but the toughness properties (CAI) of composite material improve 52% after toughening, toughening
Front and back composite property is as follows:
| Test item | Test method | Before toughening | After toughening |
| 0 ° of tensile strength/MPa | ASTM D3039 | 1663 | 1675 |
| 0 ° of stretch modulus/GPa | ASTM D3039 | 128 | 124 |
| 0 ° of compressive strength/MPa | ASTM D6641 | 1235 | 1206 |
| 0 ° of compression modulus/GPa | ASTM D6641 | 122 | 120 |
| Bending strength/MPa | ASTM D7264 | 1546 | 1593 |
| Bending modulus/GPa | ASTM D7264 | 117 | 116 |
| Longitudinal-transverse shear intensity/MPa | ASTM D3518 | 126 | 122 |
| Longitudinal-transverse shear modulus/GPa | ASTM D3518 | 4.15 | 4.07 |
| CAI/MPa | ASTM D7136&7137 | 148 | 225 |
Claims (8)
1. the preparation method of a kind of vacuum flexible bag moulding high tenacity prepreg and its composite material, which is characterized in that including as follows
Step:
1) resin matrix is modified using toughener；
It 2) is the prepreg for being partly impregnated with structure by the modified resin base bluk recombination in reinforcing fiber and step 1)；
3) prepreg for being partly impregnated with structure in step 2 is being increased using vacuum bag pressure technological forming by resin directed flow
Under the filtering effect of strong fiber, toughener is made to be enriched to composite fiber interlayer region, forms toughening layer.
2. preparation method according to claim 1, which is characterized in that toughener described in step 1) is polysulfones, polyethers
One of sulfone, polyether-ketone, polyether-ether-ketone, polyether ketone ketone, polyamide, polyimides, polyetherimide, polyurethane, polyphenylene oxide
Or two kinds or more of combination.
3. preparation method according to claim 1, which is characterized in that toughener described in step 1) is having a size of 2~10 μm.
4. preparation method according to claim 1, which is characterized in that using toughener to resin base described in step 1)
Body is modified, and toughener weight content is 3~10%.
5. preparation method according to claim 1, which is characterized in that reinforcing fiber described in step 2) be carbon fiber,
Glass fibre, basalt fibre.
6. preparation method according to claim 1, which is characterized in that structure prepreg is partly impregnated with described in step 2),
Degree of steeping is 30~70%.
7. preparation method according to claim 1, which is characterized in that composite material described in step 3), corpus fibrosum
Product content is 50~60%.
8. preparation method according to claim 1, which is characterized in that resin directed flow, side described in step 3)
Method is selection resin viscosity in the corresponding temperature range of 5~15Pas, and setting heat preservation platform is not impregnated with resin to prepreg
Area's flowing.
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| Application Number | Priority Date | Filing Date | Title |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113199666A (en) * | 2021-03-22 | 2021-08-03 | 常州市宏发纵横新材料科技股份有限公司 | Semi-impregnated prepreg preparation method and prepreg structure |
| CN113896861A (en) * | 2021-11-26 | 2022-01-07 | 中航复合材料有限责任公司 | Dicyandiamide cured epoxy resin suitable for out-of-tank molding and preparation method thereof |
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| CN103396576A (en) * | 2006-08-07 | 2013-11-20 | 东丽株式会社 | Prepreg and carbon fiber-reinforced composite material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113199666A (en) * | 2021-03-22 | 2021-08-03 | 常州市宏发纵横新材料科技股份有限公司 | Semi-impregnated prepreg preparation method and prepreg structure |
| CN113199666B (en) * | 2021-03-22 | 2022-05-13 | 常州市宏发纵横新材料科技股份有限公司 | Semi-impregnated prepreg preparation method and prepreg structure |
| CN113896861A (en) * | 2021-11-26 | 2022-01-07 | 中航复合材料有限责任公司 | Dicyandiamide cured epoxy resin suitable for out-of-tank molding and preparation method thereof |
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Application publication date: 20190412 |