CN108943767B - Toughening modification method of composite material - Google Patents
Toughening modification method of composite material Download PDFInfo
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- CN108943767B CN108943767B CN201710867858.1A CN201710867858A CN108943767B CN 108943767 B CN108943767 B CN 108943767B CN 201710867858 A CN201710867858 A CN 201710867858A CN 108943767 B CN108943767 B CN 108943767B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/40—Shaping or impregnating by compression not applied
- B29C70/42—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles
- B29C70/44—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles using isostatic pressure, e.g. pressure difference-moulding, vacuum bag-moulding, autoclave-moulding or expanding rubber-moulding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/54—Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
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Abstract
The invention discloses a toughening modification method of a composite material, which relates to the technical field of preparation of composite materials.
Description
Technical Field
The invention relates to the technical field of preparation of composite materials, in particular to a strengthening and toughening modification method of a composite material.
Background
The continuous carbon fiber reinforced resin matrix composite material has high specific strength and specific stiffness, so that the continuous carbon fiber reinforced resin matrix composite material is widely applied to the fields of high-end material application, such as aerospace, ships, energy sources and the like. With the continuous reduction of the cost of the carbon fiber, the application of the continuous carbon fiber reinforced resin matrix composite material gradually expands to the field of civil equipment. Continuous carbon fiber reinforced resin based composite materials are typically formed by layering carbon fiber plies, with the resin matrix filling the entire material space. Due to the structural characteristics of the composite material and the problems of brittleness, low electric and thermal conductivity of a resin matrix, the composite material has the problems of insufficient interlayer electric and thermal conductivity, poor interlayer impact resistance and delamination performance and the like, and the problems of lightning protection, easy impact damage, uneven thermal deformation and the like are caused.
The electric conductivity, the thermal conductivity or the impact resistance of the composite material can be improved by utilizing the interlayer nano modification of the composite material, or a plurality of the performances can be simultaneously improved. Such as adding carbon nanotube paper, carbon fiber/carbon nanotube and other hybrid conductive materials into the composite material, adding carbon nanotubes to improve the conductivity, and the like. Most of the measures for improving the thermal conductivity of the composite material are focused on directly adding fillers with higher thermal conductivity into the thermosetting resin, and related reports include that: 46th International SAMPE Symposium and inhibition, 2001: Materials and Processes Odyssey (2): 1530-1537, boron nitride micro powder is directly added between layers, but the low-speed impact resistance performance is inevitably reduced; 1135, 1145, 2011 adding graphite nanometer sheet paper between layers; carbon, 49 (8): 2817-2833,2010 incorporate carbon nanotubes, but the individual carbon nanotubes have dispersion problems. However, the above addition of only nanoparticles has a limited improvement in electrical conductivity, thermal conductivity and toughness.
The biggest problem encountered with the use of electrically and thermally conductive particle packing is that the formation of an effective electrically or thermally conductive network is somewhat difficult and is limited to high contact resistance and thermal contact resistance between the particles, so that even if the volume content of these particles is high, the electrical and thermal conductivity is much lower than that of a continuous material. The electrical conductivity of carbon nanotube-filled composites is typically less than 10 even at high loadings-2S/cm, using continuousThe conductivity of the composite material prepared by the long carbon nano tube in the direction of the nano tube is higher than 103S/cm; the thermal conductivity of the composite material doped with graphene is only 0.4W/mk, the thermal conductivity of a continuous graphene sheet layer measured by a Raman spectrometer can reach 5000W/mk, and the three-dimensional framework graphene reported by J. Mater. Chem 2011, 21:17366-17370 has the electrical conductivity of 600S/cm, so that the biggest reason for improving the electrical conductivity or poor thermal conductivity of the composite material by the filler particles is high contact resistance and contact thermal resistance among the particles.
The interlayer conductive modification of the composite material by utilizing a continuous or quasi-continuous three-dimensional nano structure is also developed in recent years, for example, CN201210251285.7 utilizes a tough three-dimensional structure to carry a one-dimensional silver nanowire material, so that the conductivity of the composite material is greatly improved, and simultaneously, the toughness of the composite material is also improved, for example, CN201310008295.2 utilizes a three-dimensional continuous carbon nano structure to modify the composite material, so that the conductivity of the composite material is improved, but only the three-dimensional continuous carbon nano structure is utilized to modify the composite material, and the interlayer fracture toughness of the composite material is still insufficient.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provide a toughening modification method for a composite material, which can obtain a three-dimensional graphene toughening high-conductivity composite material.
In order to realize the technical purpose, the invention relates to a strengthening and toughening modification method of a composite material, which is characterized in that a three-dimensional continuous graphene sheet is compounded with a solution of a blend resin of a thermoplastic resin and an uncured composite material matrix resin, a three-dimensional continuous graphene/resin composite toughening conductive structure layer is obtained after a solvent is removed, the three-dimensional continuous graphene/resin composite toughening conductive structure layer is intercalated between carbon fiber fabrics or carbon fiber prepreg layers, and then the final composite material is obtained according to a preparation process and a curing process of a laminated composite material;
wherein the thermoplastic resin is soluble in the uncured matrix resin of the composite material, and the proportion of the thermoplastic resin to the matrix resin of the composite material is 1: 20-1: the viscosity of the blended resin is lower than 20Pa.s at the resin curing temperature, and the viscosity of the thermoplastic resin or the solution of the blended resin is lower than 2Pa.s at the compounding temperature.
Preferably, the thickness of the three-dimensional skeleton graphene sheet used for intercalation is more than 10 μm under the no-pressure effect and less than 60 μm under the 1.2MPa pressure effect;
preferably, the amount of the blending resin in the three-dimensional continuous graphene/resin composite structure is 10-40 g/m2。
Preferably, the carbon fiber and the fabric thereof are selected from commercial carbon fibers T300, T800, T700, CCF300, woven in a unidirectional, plain, twill, satin weave, and the carbon fiber prepreg is obtained by compounding a carbon fiber fabric and a matrix resin.
Preferably, the matrix resin is selected from the group consisting of epoxy resins, benzoxazine resins, bismaleimide resins, and polyimide resins.
Preferably, the molding and curing process of the composite material is autoclave molding, or RTM, molding, vacuum assisted or vacuum bag molding. The specific operation is performed in accordance with the molding conditions of the base resin.
The finished product prepared by the method is a laminated carbon fiber composite product with one or more layers of compressed three-dimensional continuous graphene composite structures.
After the technical scheme is adopted, the three-dimensional continuous graphene is modified to obtain the three-dimensional continuous graphene/resin composite structure, and then the continuous carbon fiber laminated composite material is modified among layers, so that the electrical conductivity, the thermal conductivity and the toughness of the laminated composite material are improved through the electrical conductivity and the thermal conductivity of the composite structure and the toughness structure, and the modified laminated composite material is obtained. The composite structure has good heat conduction and electric conductivity, and simultaneously has better toughening effect on the composite material, thereby efficiently improving the electric conductivity and the heat conductivity of the composite material and having better reinforcing and toughening effects on the composite material.
Further details regarding the advantageous effects of the present invention will be further explained below with reference to the description of the embodiments and the drawings.
Drawings
Fig. 1 is an under-mirror view of a scanning electron microscope of three-dimensional continuous graphene in one embodiment of the invention;
fig. 2 is an under-mirror image of a scanning electron microscope of a three-dimensional continuous graphene/resin composite structure according to an embodiment of the present invention.
Detailed Description
In order that the present invention may be more clearly understood, the following detailed description of the present invention is provided in conjunction with the examples.
Example 1:
(1-1) the density was adjusted to 0.01g/cm3Cutting flexible three-dimensional continuous graphene foam into thin sheets with the thickness of 1mm for later use; taking phenolphthalein modified polyaryletherketone and epoxy resin 5228, wherein the mass ratio of the two is 0.5: 1 or 0.3:1, preparing a 15wt% solution by using tetrahydrofuran, uniformly adsorbing the solution on three-dimensional continuous graphene foam according to the amount of 30g solute per square meter, naturally drying, and drying at 60 ℃ to obtain a three-dimensional graphene/resin composite structure;
(1-2) placing the obtained composite structure sheets one by one between the layers of the continuous carbon fiber unidirectional reinforced epoxy resin-based prepreg for layering, heating carbon fibers T300 and 3K and epoxy resin 5228 (product of Beijing aviation materials institute) to 120 ℃, keeping the pressure at 0.6MPa, compressing and sizing for 30min, and obtaining a composite material prefabricated body of the intercalated sheets;
and (1-3) according to the curing process specified by the epoxy resin prepreg, carrying out molding curing on the composite material preform by using a conventional mould pressing method to obtain the composite material product with the epoxy resin matrix improved in electric conductivity, heat conductivity and toughness.
(1-4) if necessary, (1-1) three-dimensional continuous graphene foam sheets can be laid on one or two outer surfaces of the composite material prefabricated body of (1-2), and after the composite material is molded and cured according to (1-4), the composite material also has excellent surface conductive property and is particularly suitable for lightning protection of the composite material.
As can be seen from fig. 1 and 2, the three-dimensional continuous graphene is composed of continuous lamellar graphene, the lamellar layer of the graphene forms a tubular hollow micron fiber shape and forms a three-dimensional continuous foam structure, the blended resin in the composite structure enters the graphene tube and the lamellar layer under the capillary action preferentially, the three-dimensional continuous toughening structure is formed, the aggregation of the graphene under the pressure is avoided, and the better toughening effect is achieved.
Example 2:
(2-1) the density was adjusted to 0.002g/cm3Cutting flexible three-dimensional skeleton graphene into slices with the thickness of 2.5mm for later use; taking phenolphthalein modified polyaryletherketone, liquid Benzoxazine (BOZ) resin and product Epsilon of Germany Henkel company, wherein the mass ratio of the two is 0.5: 1 or 1:1, preparing 5wt% or 15wt% or 20wt% solution by using tetrahydrofuran, uniformly adsorbing the solution on three-dimensional continuous graphene foam according to the amount of 20g or 35g solute per square meter, naturally drying and drying at 60 ℃ to obtain a three-dimensional graphene/resin composite structure;
(2-2) placing the obtained composite structure sheet between layers of continuous carbon fiber reinforced satin fabric for layering, heating carbon fibers T700 and 12K to 80 ℃, and adding 1MPa pressure for shaping to obtain a composite material prefabricated body of the intercalated sheet;
and (2-3) injecting BOZ resin into the preform by using an RTM process, completely impregnating, and then molding and curing according to the process specified by the BOZ resin to finally obtain the RTM-molded benzoxazine resin-based composite material product with improved electrical and thermal conductivity and toughness.
Example 3:
(3-1) preparation of a density of 0.01g/cm by a vapor chemical deposition method in the prior art3The thickness of the three-dimensional skeleton graphene sheet is 70 mu m and has a multilayer graphene structure for standby; taking liquid epoxy resin 3266 (product of Beijing aviation material research institute) and PKHH thermoplastic resin, wherein the mass ratio of the liquid epoxy resin 3266 to the PKHH thermoplastic resin is 15:1 or 5:1, dissolving with THF to prepare a 22wt% solution; uniformly adsorbing the solution onto three-dimensional continuous graphene foam according to the amount of 18g or 25g solute per square meter, naturally drying, and drying at 60 ℃ to obtain a three-dimensional graphene/resin composite structure;
(3-2) placing the obtained composite structure between layers of continuous carbon fiber reinforced satin fabric for layering, wherein the placing amount of the composite structure is 6 layers in the middle, and heating carbon fibers T700 and T3K to 60 ℃, pressurizing to 1.2MPa and shaping to obtain a composite material preform of an intercalated sheet;
and (3-3) injecting liquid epoxy resin 3266 (a product of Beijing aviation material research institute) according to the process requirement of vacuum bag forming by using a vacuum bag forming process, and then carrying out forming and curing according to the process specified by the resin to finally obtain the composite material product with the improved interlayer electrical conductivity and good thermal conductivity and toughness of the intermediate layer.
Example 4:
(4-1) the density was adjusted to 0.02g/cm3Three-dimensional continuous graphene foam or 0.008g/cm3Cutting a three-dimensional continuous graphene sheet into sheets with the thickness of 1mm for later use; matrix resin corresponding to a polyimide resin-based prepreg mark LP 15 (product of Beijing aviation Material research institute) and polyether sulfone (PES) are mixed according to a mass ratio of 2: 1 or 7:1, dissolving with DMF to prepare a 25wt% solution, uniformly adsorbing the solution on three-dimensional continuous graphene foam according to the amount of 12g or 25g solute per square meter, and drying in vacuum at 100 ℃ to obtain a three-dimensional continuous graphene/resin composite structure;
(4-2) placing the obtained composite structure sheets one by one between layers of carbon fiber laminated polyimide resin-based prepreg for layering, heating the carbon fibers T700 and 12K and the polyimide resin-based prepreg mark LP 15 to 100 ℃, and applying pressure of 1.2MPa for compression and sizing to obtain a composite material preform with an intercalated conductive structure;
and (4-3) forming and curing the composite material preform by using an autoclave process according to the process specified by the prepreg to obtain the high-temperature-resistant polyimide composite material product with improved electric conductivity, heat conductivity and toughness.
Example 5:
(5-1) the density was adjusted to 0.007g/cm3Cutting flexible three-dimensional continuous graphene foam into thin sheets with the thickness of 3mm for later use; polyphenylene sulfide and epoxy resin 5228 (product of Beijing aviation materials institute) are taken, and the mass ratio of the polyphenylene sulfide to the epoxy resin is 0.2: 1 or 0.6:1, preparing 18wt% of solution by using tetrahydrofuran, uniformly adsorbing the solution on three-dimensional continuous graphene foam according to the amount of 18g of solute per square meter, naturally drying and drying at 60 ℃ to obtain a three-dimensional graphene/resin composite structure;
(5-2) placing the obtained composite structure sheet between a first prepreg layer and a second prepreg layer of continuous carbon fiber unidirectional reinforced epoxy resin-based prepreg, then layering the layers, heating the carbon fibers T300 and T3K and the epoxy resin 5228 to 120 ℃, compressing and shaping to obtain a composite material preform with a layer of sheet inserted;
(5-3) according to the curing process specified by the epoxy resin prepreg, the composite material preform inserted with the thin sheet is molded and cured by a conventional molding method to obtain a composite material product with improved surface conductivity and toughness.
Example 6:
(6-1) preparation of a density of 0.01g/cm by a vapor-phase chemical deposition method in the prior art3The thickness of the graphene sheet is 500 mu m, and the three-dimensional framework graphene sheet with a multilayer graphene structure is reserved; taking bismaleimide resin 6421 (product of Beijing aviation material institute) and thermoplastic resin PES or PEK-C, wherein the mass ratio of the bismaleimide resin to the thermoplastic resin is 5:1 or 3:1, using volume ratio of DMF to THF of 1:1, dissolving the mixed solvent and preparing a 15wt% solution, uniformly adsorbing the solution on three-dimensional continuous graphene foam according to the amount of 10g or 16g solute per square meter, naturally drying and vacuum drying at 90 ℃ to obtain a three-dimensional graphene/resin composite structure;
(6-2) placing the obtained composite structure sheet between layers of continuous carbon fiber reinforced twill fabric for layering, heating carbon fibers T700 and T3K to 110 ℃, pressurizing to 0.6MPa, compressing and shaping to obtain a composite material prefabricated body of the intercalated sheet;
(6-3) injecting liquid bismaleimide resin 6421 according to the RTM forming process by using a vacuum bag forming process, and then forming and curing according to the process specified by the resin to finally obtain the composite material product with improved electrical conductivity, thermal conductivity and toughness.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. A strengthening and toughening modification method of a composite material is characterized by comprising the following steps: compounding a three-dimensional continuous graphene sheet with a solution of a thermoplastic resin and a blend resin of uncured composite material matrix resin, removing a solvent to obtain a three-dimensional continuous graphene/resin composite toughening conductive structure layer, intercalating the three-dimensional continuous graphene/resin composite toughening conductive structure layer between carbon fiber fabrics or carbon fiber prepreg layers, and then obtaining a final composite material according to a preparation process and a curing process of a laminated composite material;
wherein the thermoplastic resin is soluble in the uncured matrix resin of the composite material, and the proportion of the thermoplastic resin to the matrix resin of the composite material is 1: 20-1: the viscosity of the blended resin is lower than 20Pa.s at the resin curing temperature, and the viscosity of the thermoplastic resin or the solution of the blended resin is lower than 2Pa.s at the compounding temperature.
2. The method for toughening and modifying a composite material according to claim 1, wherein: the thickness of the three-dimensional continuous graphene sheet used for intercalation is more than 10 μm under the non-pressure effect and less than 60 μm under the 1.2MPa pressure effect.
3. The method for toughening and modifying a composite material according to claim 1, wherein: the dosage of the blending resin in the three-dimensional continuous graphene/resin composite structure is 10-40 g/m2。
4. The method for toughening and modifying a composite material according to claim 1, wherein: the carbon fiber and its fabric are selected from commercial carbon fiber T300, T800, T700 or CCF300, and the weaving mode is unidirectional, plain weave, twill or satin, and the carbon fiber prepreg is obtained by compounding the carbon fiber fabric and matrix resin.
5. The method for toughening and modifying a composite material according to claim 1, wherein: the matrix resin is selected from epoxy resin, benzoxazine resin, bismaleimide resin or polyimide resin.
6. The method for toughening and modifying a composite material according to claim 1, wherein: the forming and curing process of the composite material comprises autoclave forming, RTM, mould pressing, vacuum assistance or vacuum bag forming.
7. The method for toughening and modifying a composite material according to claim 1, wherein: the finished product prepared by the method is a laminated carbon fiber composite product with one or more layers of compressed three-dimensional continuous graphene composite structures.
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| CN111877050B (en) * | 2020-07-28 | 2023-01-31 | 江苏奥神新材料股份有限公司 | Preparation method of 3D-doped layered porous graphene sheet paper-based friction material |
| CN115594945A (en) * | 2022-10-14 | 2023-01-13 | 中国科学院金属研究所（Cn） | Preparation method of structure/electromagnetic shielding integrated hybrid composite material |
| CN116082052A (en) * | 2022-12-30 | 2023-05-09 | 北京机科国创轻量化科学研究院有限公司 | Graphene-based carbon/carbon composite material and precursor thereof |
Citations (3)
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| CN102732037A (en) * | 2011-04-08 | 2012-10-17 | 中国科学院金属研究所 | Graphene foam/polymer high-conductivity composite material preparation method and application thereof |
| CN103057221A (en) * | 2013-01-10 | 2013-04-24 | 中国航空工业集团公司北京航空材料研究院 | Three-dimensional skeleton graphene foam modified laminated composite and preparation method thereof |
| CN104385615A (en) * | 2014-09-23 | 2015-03-04 | 江苏恒神纤维材料有限公司 | Carbon fiber shelter sub-frame and tank body bottom plate integrated curing forming process |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102732037A (en) * | 2011-04-08 | 2012-10-17 | 中国科学院金属研究所 | Graphene foam/polymer high-conductivity composite material preparation method and application thereof |
| CN103057221A (en) * | 2013-01-10 | 2013-04-24 | 中国航空工业集团公司北京航空材料研究院 | Three-dimensional skeleton graphene foam modified laminated composite and preparation method thereof |
| CN104385615A (en) * | 2014-09-23 | 2015-03-04 | 江苏恒神纤维材料有限公司 | Carbon fiber shelter sub-frame and tank body bottom plate integrated curing forming process |
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