CN116021859A - High-brittleness phase composite material with multilayer structure and preparation method thereof - Google Patents
High-brittleness phase composite material with multilayer structure and preparation method thereof Download PDFInfo
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- CN116021859A CN116021859A CN202310032626.XA CN202310032626A CN116021859A CN 116021859 A CN116021859 A CN 116021859A CN 202310032626 A CN202310032626 A CN 202310032626A CN 116021859 A CN116021859 A CN 116021859A
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- 239000002131 composite material Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000010410 layer Substances 0.000 claims abstract description 28
- 239000011347 resin Substances 0.000 claims abstract description 25
- 229920005989 resin Polymers 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 21
- 239000002356 single layer Substances 0.000 claims abstract description 15
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims abstract description 14
- 238000003825 pressing Methods 0.000 claims abstract description 14
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 7
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 230000007480 spreading Effects 0.000 claims abstract description 6
- 238000003892 spreading Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 13
- 239000000805 composite resin Substances 0.000 claims description 6
- 238000010030 laminating Methods 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 5
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 claims description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 2
- 239000004925 Acrylic resin Substances 0.000 claims description 2
- 229920000178 Acrylic resin Polymers 0.000 claims description 2
- UUAGAQFQZIEFAH-UHFFFAOYSA-N chlorotrifluoroethylene Chemical group FC(F)=C(F)Cl UUAGAQFQZIEFAH-UHFFFAOYSA-N 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 claims description 2
- 229920001568 phenolic resin Polymers 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000005007 epoxy-phenolic resin Substances 0.000 claims 1
- 238000007731 hot pressing Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 230000005669 field effect Effects 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 description 8
- 230000008569 process Effects 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000007767 bonding agent Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 210000001503 joint Anatomy 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000011185 multilayer composite material Substances 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
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Abstract
The invention relates to a high-brittleness phase composite material with a multilayer structure and a preparation method thereof. Firstly, uniformly mixing high-brittleness materials such as barium sulfate, melamine and the like with fluororesin and pressing the mixture into a series of single-layer sheets, then spreading resin materials on one single-layer sheet and prepressing the resin materials, then placing the other single-layer sheet and performing laminated prepressing, repeatedly spreading the resin, placing the sheet and performing laminated prepressing operation for a plurality of times, and finally obtaining the high-brittleness phase composite material with the tensile strength of up to 4.6MPa at 20 ℃. The invention adopts a multi-layer mixing hot-pressing technology to prepare the composite material with different macroscopic structures, the whole preparation process is simpler, the external field effect is not needed, the implementation and popularization are easy, and the designability and the operability are very strong.
Description
Technical Field
The invention relates to the technical field of layered composite materials, in particular to a high-brittleness phase composite material with a multi-layer structure and a preparation method thereof.
Background
With the increase in fuel economy and external loading, the preparation of functionalized, highly brittle matrix composites is becoming a research hotspot for designers. The high-brittleness phase composite material is a brittle matrix composite material composed of a high-brittleness phase matrix material and a small amount of additives, has the advantages of high strength, high modulus, excellent fracture toughness, stability and the like, is a development trend of the composite material industry in recent years, and is very widely applied to the fields of aeroengine parts, polymer-based bonded explosive filling, transportation, building materials, buffering and damping parts and the like.
Many high brittle phase composites are susceptible to fracture due to the excessive content of a particular brittle phase, especially in the case of chipping, scoring or internal defects, which greatly limits the wide range of applications for high brittle phase composites. In general, in order to obtain a high-brittleness phase composite material with excellent mechanical properties, a common method includes adding an adhesive into a matrix of the high-brittleness phase composite material, and preparing a Gao Cuixing matrix composite material by adopting an adhesive mode. The adhesive can improve the brittle phase matrix interface, and effectively improve the bonding strength on the premise of not influencing the balance state of the material, thereby improving the mechanical strength of the material. In addition, the bonding agent can also generate hydrogen bonds and other actions between the high-brittleness phase matrix and the bonding agent in a coupling mode and the like, and can be used as a bridge to improve interface bonding. However, the mere dependence of the coupling agent and the like on the regulation and control action in the interface has limitation because the bonding strength is not high and the distribution is uneven, the improvement effect is very limited, and the substantial improvement action cannot be achieved.
Disclosure of Invention
The invention aims to provide a high-brittleness phase composite material with a multi-layer structure, which comprises at least 2 layers, wherein the high-brittleness phase composite material is formed by alternately arranging high-brittleness material-resin composite layers and resin layers in sequence.
Further, the number of layers of the composite material is an even number, preferably an even number between 2 and 16.
Further, the resin raw materials selected for each layer are the same or different, preferably the same.
Still further, the resin is at least one selected from the group consisting of a fluororesin, an epoxy resin, a phenolic resin, and an acrylic resin, preferably a fluororesin, and more preferably a copolymer of vinylidene fluoride and chlorotrifluoroethylene in a mass ratio of=1:4.
Further, the high brittle materials selected for the high brittle material-resin composite layer may be the same or different, and preferably the same.
Further, the high brittleness material is at least one selected from barium sulfate and melamine.
Furthermore, the high brittleness material is specifically a mixture of barium sulfate and melamine, and the mass ratio of the barium sulfate to the melamine is 18-20:71-75, preferably 20:75.
Further, the mass part ratio of the high-brittleness material to the resin in the high-brittleness material-resin composite layer is 90-95:5-10, preferably 95:5, 94:6, 93:7, 92:8, 91:9, and 90:10.
Further, the ratio of the total mass of all resin layers to the mass of the entire composite is 5-10:100.
Further, the total thickness of the whole composite material and the thickness of the single resin layer are 29.40-30.50mm and 0.04-1.11mm respectively.
The second object of the present invention is to provide a method for preparing the high brittleness phase composite material with the multi-layer structure, which mainly comprises the following steps: (a) Uniformly mixing a high-brittleness material and resin according to a certain proportion, and paving and prepressing to obtain a single-layer prepressing sheet; (b) Spreading resin on the single-layer prepressing sheet, prepressing, putting another single-layer prepressing sheet, and laminating; and (c) repeating the step (b), and finally performing hot press molding.
Further, the average particle diameter of the highly brittle material in the step (a) is 20 μm to 40. Mu.m. The particle size of the highly brittle material must be within a suitable range and if too large can result in a composite with a low density.
Further, in the step (a), the pre-pressing temperature is normal temperature, the pre-pressing pressure is not more than 50MPa, and the thickness of the pre-pressed sheet is 1.8mm-15mm.
Further, in the step (b), the laminating pre-pressing temperature is normal temperature, and the laminating pre-pressing pressure is not more than 50MPa.
Further, in the step (c), the hot press molding temperature is 80-200 ℃ and the pressure is 1GPa-4GPa.
According to the invention, the thickness of the layered structure is controlled, and multi-layer mixed material hot pressing is carried out at the glass transition temperature of the high-brittleness phase matrix, so that the multi-layer composite material with excellent mechanical property is finally obtained. Experimental comparison shows that the interface joint in the multilayer structure is tightly, uniformly and flatly bonded in the stretching process, and good layer-to-layer bonding can be maintained, so that the strength of the multilayer structure composite material is greatly improved compared with that of the single-layer structure composite material.
The beneficial effects of the invention are summarized as follows: (1) The composite materials with different macroscopic structures are prepared by adopting a multilayer mixing hot-pressing technology, and the multilayer structure can be flexibly designed and accurately controlled; (2) The dynamic tensile test result shows that the multilayer structure high brittleness composite material prepared by the method has good tensile strength and toughness, the tensile strength at 20 ℃ is up to 4.6MPa, and the tensile strength is improved by 206% compared with a single-layer sample; (3) The integrated preparation process adopted by the invention is simpler, does not need to use external field effect, is easy to implement and popularize, and has strong designability and operability.
Drawings
FIG. 1 is a process flow chart and a physical photograph of the invention;
FIG. 2 is a stress-strain curve of the composite samples prepared in examples 1-5;
FIG. 3 is a stress-strain curve of the composite samples prepared in examples 6-9;
FIG. 4 is a stress-strain curve of the composite samples prepared in examples 10-13;
FIG. 5 is a scanning electron micrograph of a composite sample prepared in examples 1-13.
Detailed Description
In order to make the technical scheme and the beneficial effects of the present invention fully understood by those skilled in the art, the following description is further made with reference to specific embodiments and drawings.
The preparation method of the multilayer structure high brittleness phase composite material shown in fig. 1 comprises the following steps: uniformly mixing a high-brittleness material and resin, spreading the mixture in a die, and prepressing the mixture by a hot press to obtain a single-layer prepressing sheet with the thickness of 1.80-15 mm; secondly, putting a single-layer pre-pressing sheet into a die, spreading a layer of resin on the surface of the single-layer pre-pressing sheet, pre-pressing the resin, putting another single-layer pre-pressing sheet into the die, and then carrying out lamination pre-pressing by using a hot press; and thirdly, repeating the second step for a plurality of times according to the number of layers required to be prepared, and finally performing hot press molding at high temperature and high pressure.
The process conditions for examples 1-13 are shown in Table 1 below.
Table 1 comparison of process conditions for different examples
The compositions of the multilayer structured highly brittle phase composites prepared in examples 1-13 are shown in Table 2 below.
Table 2 comparative table of composition of composite materials prepared in different examples
In order to fully understand the performance of the layered structure high brittleness phase composite material prepared by each example, the test of mechanical properties and SEM (scanning electron microscope) analysis were performed by referring to GB/T6329-1996 method of determination of tensile Strength of adhesive butt joint, and the results are shown in figures 2-5.
As is clear from the stress-strain curves shown in fig. 2 to 4, as the number of layers increases, the tensile strength of the material increases, the maximum at 8 layers, and the corresponding tensile strength at 4% interlayer resin content reaches 4.6MPa (corresponding to example 4).
As can be seen from the SEM photograph of fig. 5, the present invention successfully constructs an interlayer resin structure, which deforms to absorb energy during the stretching process, avoids stress concentration and improves the mechanical properties of the composite material.
Claims (10)
1. A high brittle phase composite material of a multilayer structure, characterized in that: the composite material comprises at least 2 layers, and is formed by alternately arranging high brittleness material-resin composite layers and resin layers in sequence.
2. The composite material of claim 1, wherein: the number of layers of the composite material is even between 2 and 16.
3. The composite material of claim 1, wherein: the resin raw materials selected from each layer are the same or different, and the resin is at least one of fluororesin, epoxy resin, phenolic resin and acrylic resin; the high-brittleness materials selected from the high-brittleness material-resin composite layer are the same or different, and the high-brittleness material is at least one selected from barium sulfate and melamine.
4. A composite material according to claim 3, wherein: the resin is specifically a copolymer of vinylidene fluoride and chlorotrifluoroethylene in a mass ratio of = 1:4; the high-brittleness material is specifically a mixture of barium sulfate and melamine, and the mass ratio of the barium sulfate to the melamine is 18-20:71-75.
5. The composite material of claim 1, wherein: the mass ratio of the high-brittleness material to the resin in the high-brittleness material-resin composite layer is 90-95:5-10.
6. The composite material of claim 1, wherein: the ratio of the total mass of all resin layers to the mass of the entire composite is 5-10:100.
7. The composite material of claim 1, wherein: the total thickness of the whole composite material and the thickness of the single resin layer are 29.40-30.50mm and 0.04-1.11mm respectively.
8. A method for preparing a high brittleness phase composite material of a multi-layered structure according to any of claims 1-7, characterized in that the method comprises the steps of: (a) Uniformly mixing a high-brittleness material and resin according to a proportion, and paving and prepressing to obtain a single-layer prepressing sheet; (b) Spreading resin on the single-layer prepressing sheet, prepressing, putting another single-layer prepressing sheet, and laminating; and (c) repeating the step (b), and finally performing hot press molding.
9. The method as recited in claim 8, wherein: the average grain diameter of the high brittle material in the step (a) is 20-40 mu m, the pre-pressing temperature is normal temperature, the pre-pressing pressure is not more than 50MPa, and the thickness of the pre-pressed sheet is 1.8-15 mm.
10. The method as recited in claim 8, wherein: the laminating pre-pressing temperature in the step (b) is normal temperature, and the laminating pre-pressing pressure is not more than 50MPa; the hot press molding temperature in the step (c) is 80-200 ℃ and the pressure is 1GPa-4GPa.
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| CN109311293A (en) * | 2016-04-06 | 2019-02-05 | 沙特基础工业全球技术有限公司 | The hard resin multilayered structure of filler enhancing |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109311293A (en) * | 2016-04-06 | 2019-02-05 | 沙特基础工业全球技术有限公司 | The hard resin multilayered structure of filler enhancing |
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