CN118684997A - A high-conductivity epoxy resin-based composite material and preparation method thereof - Google Patents
A high-conductivity epoxy resin-based composite material and preparation method thereof Download PDFInfo
- Publication number
- CN118684997A CN118684997A CN202310287733.7A CN202310287733A CN118684997A CN 118684997 A CN118684997 A CN 118684997A CN 202310287733 A CN202310287733 A CN 202310287733A CN 118684997 A CN118684997 A CN 118684997A
- Authority
- CN
- China
- Prior art keywords
- epoxy resin
- preparation
- conductive
- volatile solvent
- composite material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000003822 epoxy resin Substances 0.000 title claims abstract description 61
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 61
- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000011231 conductive filler Substances 0.000 claims abstract description 21
- 239000011148 porous material Substances 0.000 claims abstract description 8
- 239000000853 adhesive Substances 0.000 claims abstract description 7
- 230000001070 adhesive effect Effects 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 21
- 239000003292 glue Substances 0.000 claims description 19
- 239000002904 solvent Substances 0.000 claims description 17
- 239000011268 mixed slurry Substances 0.000 claims description 14
- 238000011282 treatment Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 4
- 239000004020 conductor Substances 0.000 claims description 4
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 4
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- YSUQLAYJZDEMOT-UHFFFAOYSA-N 2-(butoxymethyl)oxirane Chemical compound CCCCOCC1CO1 YSUQLAYJZDEMOT-UHFFFAOYSA-N 0.000 claims description 2
- QXONIHMUSQFKJU-UHFFFAOYSA-N 2-(prop-1-enoxymethyl)oxirane Chemical compound CC=COCC1CO1 QXONIHMUSQFKJU-UHFFFAOYSA-N 0.000 claims description 2
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 2
- 239000004641 Diallyl-phthalate Substances 0.000 claims description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- FQYUMYWMJTYZTK-UHFFFAOYSA-N Phenyl glycidyl ether Chemical compound C1OC1COC1=CC=CC=C1 FQYUMYWMJTYZTK-UHFFFAOYSA-N 0.000 claims description 2
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 2
- QUDWYFHPNIMBFC-UHFFFAOYSA-N bis(prop-2-enyl) benzene-1,2-dicarboxylate Chemical compound C=CCOC(=O)C1=CC=CC=C1C(=O)OCC=C QUDWYFHPNIMBFC-UHFFFAOYSA-N 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 238000009849 vacuum degassing Methods 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 230000007704 transition Effects 0.000 abstract description 5
- 229920001187 thermosetting polymer Polymers 0.000 abstract description 4
- 229920005989 resin Polymers 0.000 abstract description 3
- 239000011347 resin Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 10
- 230000008569 process Effects 0.000 description 7
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 6
- MWSKJDNQKGCKPA-UHFFFAOYSA-N 6-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1CC(C)=CC2C(=O)OC(=O)C12 MWSKJDNQKGCKPA-UHFFFAOYSA-N 0.000 description 4
- ITZGNPZZAICLKA-UHFFFAOYSA-N bis(oxiran-2-ylmethyl) 7-oxabicyclo[4.1.0]heptane-3,4-dicarboxylate Chemical compound C1C2OC2CC(C(=O)OCC2OC2)C1C(=O)OCC1CO1 ITZGNPZZAICLKA-UHFFFAOYSA-N 0.000 description 4
- 238000007872 degassing Methods 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 3
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 description 1
- 101001121408 Homo sapiens L-amino-acid oxidase Proteins 0.000 description 1
- 102100026388 L-amino-acid oxidase Human genes 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- AUSGLDHLCBXRML-UHFFFAOYSA-N bis(oxiran-2-ylmethyl) 2-[(3-methyloxiran-2-yl)methyl]butanedioate Chemical compound C(C1CO1)OC(=O)CC(CC1C(C)O1)C(=O)OCC1CO1 AUSGLDHLCBXRML-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000007859 condensation product Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- RPQRDASANLAFCM-UHFFFAOYSA-N oxiran-2-ylmethyl prop-2-enoate Chemical compound C=CC(=O)OCC1CO1 RPQRDASANLAFCM-UHFFFAOYSA-N 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000002002 slurry Substances 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
技术领域Technical Field
本发明属于材料制备技术领域，具体涉及一种高导电性环氧树脂基复合材料及其制备方法。The invention belongs to the technical field of material preparation, and particularly relates to a high-conductivity epoxy resin-based composite material and a preparation method thereof.
背景技术Background Art
环氧树脂是指分子中含有两个以上环氧基团的一类聚合物的总称。它是环氧氯丙烷与双酚A或多元醇的缩聚产物。由于环氧基的化学活性，可用多种含有活泼氢的化合物使其开环，固化交联生成网状结构，因此它是一种热固性树脂。Epoxy resin is a general term for a class of polymers containing two or more epoxy groups in the molecule. It is a condensation product of epichlorohydrin and bisphenol A or polyols. Due to the chemical activity of the epoxy group, it can be opened with a variety of compounds containing active hydrogen, cured and cross-linked to form a network structure, so it is a thermosetting resin.
导电复合材料目前主要是指复合型导电高分子材料，是将聚合物与各种导电物质通过一定的复合方式构成。在本领域，为了提高复合材料的导电性能，一般采取增加导电物质的用量来解决。Conductive composite materials currently mainly refer to composite conductive polymer materials, which are formed by combining polymers with various conductive substances in a certain way. In this field, in order to improve the conductive properties of composite materials, the amount of conductive substances is generally increased to solve the problem.
发明内容Summary of the invention
发明人通过研究发现，增加导电材料的用量一方面会导致复合材料的力学性能降低，另一方面也会增加成本。因此，开发一种导电物质用量少，且具有优异导电性能的导电复合材料具有重要的意义。The inventors have found through research that increasing the amount of conductive material will reduce the mechanical properties of the composite material and increase the cost. Therefore, it is of great significance to develop a conductive composite material with a small amount of conductive material and excellent conductive properties.
本发明提供了一种环氧树脂基复合材料的制备方法，具体包括以下步骤：The present invention provides a method for preparing an epoxy resin-based composite material, which specifically comprises the following steps:
S1、将导电材料加入环氧树脂基胶中，研磨分散处理；S1. Add the conductive material into the epoxy resin base glue and grind and disperse it;
S2、将经过步骤S1得到的分散处理后的样品中添加挥发性溶剂，继续研磨分散，得到混合浆料A；S2, adding a volatile solvent to the dispersed sample obtained in step S1, and continuing grinding and dispersing to obtain a mixed slurry A;
S3、将经过步骤S2得到的混合浆料倒入模具，真空加热，使其中的挥发性溶剂快速蒸发，产生大量的气孔；待气孔稳定之后，再继续加热，使环氧树脂固化成型，获得三维的环氧树脂导电网络；S3, pouring the mixed slurry obtained in step S2 into a mold, vacuum heating, so that the volatile solvent therein evaporates quickly, generating a large number of pores; after the pores are stabilized, continuing to heat, so that the epoxy resin is cured and formed, and a three-dimensional epoxy resin conductive network is obtained;
S4、提供与步骤S1相同的环氧树脂基胶或混合浆料B；S4, providing the same epoxy resin base glue or mixed slurry B as in step S1;
所述混合浆料B的制备方法包括以下步骤：The preparation method of the mixed slurry B comprises the following steps:
在与步骤S1相同的环氧树脂基胶中加入非挥发性溶剂，或，Add a non-volatile solvent to the same epoxy resin base glue as step S1, or,
在与步骤S1相同的环氧树脂基胶中加入导电填料和非挥发性溶剂；Adding conductive filler and non-volatile solvent to the same epoxy resin base adhesive as in step S1;
S5、将经过步骤S4得到的环氧树脂基胶或混合浆料B倒入经过步骤S3得到的三维的环氧树脂导电网络中，真空除泡；S5, pouring the epoxy resin base glue or mixed slurry B obtained in step S4 into the three-dimensional epoxy resin conductive network obtained in step S3, and removing bubbles in vacuum;
S6、固化处理，得到所述环氧树脂基复合材料。S6, curing treatment to obtain the epoxy resin-based composite material.
根据本发明一具体实施方式，According to a specific embodiment of the present invention,
在步骤S1中，所述环氧树脂基胶由TDE-85(4,5-环氧己烷-1,2-二甲酸二缩水甘油酯)和甲基四氢苯酐混合而成；In step S1, the epoxy resin base glue is prepared by mixing TDE-85 (4,5-epoxyhexane-1,2-dicarboxylic acid diglycidyl ester) and methyltetrahydrophthalic anhydride;
在步骤S1中，所述研磨分散处理是指使用球磨机或研磨机进行研磨分散处理；In step S1, the grinding and dispersing process refers to grinding and dispersing process using a ball mill or a grinder;
所述导电填料为具有导电性质的粉体，优选地，所述导电填料为具有导电性质的金属粉(如银粉)，石墨粉，石墨烯粉，碳黑粉中的一种或多种；The conductive filler is a powder with conductive properties. Preferably, the conductive filler is one or more of metal powder (such as silver powder), graphite powder, graphene powder, and carbon black powder with conductive properties.
上述导电填料粉体的尺寸为50目-1000目，优选的为300目；The size of the conductive filler powder is 50-1000 mesh, preferably 300 mesh;
在步骤S1中，所述导电填料占步骤S1所得样品的质量百分比为0.1％～80％，优选为75％；In step S1, the mass percentage of the conductive filler in the sample obtained in step S1 is 0.1% to 80%, preferably 75%;
在步骤S1中，所述分散处理的时间为5min-10h，优选的为2h；In step S1, the dispersion treatment time is 5 min-10 h, preferably 2 h;
根据本发明一具体实施方式，为了加速固化，在环氧树脂基胶中可以加入一定量的促进剂和偶联剂。According to a specific embodiment of the present invention, in order to accelerate curing, a certain amount of accelerator and coupling agent can be added to the epoxy resin base glue.
在步骤S2中，所述挥发性溶剂为乙醇、甲醇邻苯二甲酸二丁酯、苯二甲酸二辛酯、苯乙烯、苯二甲酸二烯丙酯、甲苯、二甲苯、丙酮中的一种或多种；In step S2, the volatile solvent is one or more of ethanol, methanol, dibutyl phthalate, dioctyl phthalate, styrene, diallyl phthalate, toluene, xylene, and acetone;
在本发明中，上述挥发性溶剂用于稀释环氧树脂，但不参与环氧树脂固化反应；In the present invention, the above-mentioned volatile solvent is used to dilute the epoxy resin, but does not participate in the curing reaction of the epoxy resin;
根据本发明一具体实施方式，在步骤S2中，所述分散处理时间为5min-10h，优选的为2h。According to a specific embodiment of the present invention, in step S2, the dispersion treatment time is 5 min-10 h, preferably 2 h.
在步骤S3中，所述真空的真空度为1～3000Pa，优选的为1000Pa；In step S3, the vacuum degree is 1-3000 Pa, preferably 1000 Pa;
真空加热的温度在较低温度下进行，所述真空加热的温度为40℃～100℃，优选的为80℃。The vacuum heating is carried out at a relatively low temperature, which is 40°C to 100°C, preferably 80°C.
所述继续加热的温度为100～300℃，优选的为180℃。The temperature of the continued heating is 100-300°C, preferably 180°C.
在步骤S4中，上述非挥发性溶剂为丙烯基缩水甘油醚、丁基缩水甘油醚和苯基缩水甘油醚等中的一种或多种。In step S4, the non-volatile solvent is one or more of propenyl glycidyl ether, butyl glycidyl ether and phenyl glycidyl ether.
其中，S4步骤的环氧树脂基胶或混合浆料B中的环氧树脂基胶与步骤S1中的环氧树脂基胶的质量比为(0.1-10)：1；优选为1:1。The mass ratio of the epoxy resin adhesive in step S4 or the epoxy resin adhesive in the mixed slurry B to the epoxy resin adhesive in step S1 is (0.1-10):1, preferably 1:1.
在步骤S5中，优选地，在此过程中可以进行多次充放气处理，使步骤S4获得的环氧树脂基胶或混合浆料B能够充分填充进步骤S3获得的三维的环氧树脂导电网络中；进一步优选地，所述充放气处理次数为1～20次，优选的为5次；In step S5, preferably, multiple gas filling and degassing treatments can be performed during this process, so that the epoxy resin base glue or mixed slurry B obtained in step S4 can be fully filled into the three-dimensional epoxy resin conductive network obtained in step S3; further preferably, the number of gas filling and degassing treatments is 1 to 20 times, preferably 5 times;
优选地，在步骤S5中，所述真空除泡的压力为1～3000Pa，优选为1000Pa；Preferably, in step S5, the vacuum degassing pressure is 1-3000 Pa, preferably 1000 Pa;
在步骤S6中，所述固化处理温度为100～300℃，优选的为180℃。也可根据所用环氧树脂种类不同，选择相应的固化温度。In step S6, the curing treatment temperature is 100-300° C., preferably 180° C. The corresponding curing temperature can also be selected according to the type of epoxy resin used.
本发明的另一目的是提供采用上述制备方法制备得到的环氧树脂基复合材料。Another object of the present invention is to provide an epoxy resin-based composite material prepared by the above preparation method.
有益效果：Beneficial effects:
本发明基于环氧树脂的热固性特点，提前架构起高导电的三维树脂导电网络，然后再在孔隙中继续填充环氧树脂。大大降低了导电填料之间的距离，减小了电子在导电填料之间的跃迁阻力，解决了环氧树脂基胶因加入大量的导电填料而导致加工性能降低的问题。Based on the thermosetting characteristics of epoxy resin, the present invention constructs a highly conductive three-dimensional resin conductive network in advance, and then continues to fill the pores with epoxy resin. This greatly reduces the distance between the conductive fillers, reduces the transition resistance of electrons between the conductive fillers, and solves the problem that the processing performance of epoxy resin-based glue is reduced due to the addition of a large amount of conductive fillers.
在热固性环氧树脂中加入高比例的导电填料，并使其分散均匀，然后添加一定比例的热挥发性溶剂，溶剂的加入能够为复合材料的浆料提供较好的流动性，可加工性能被大大提高。此外，在真空中，热挥发性溶剂在蒸发过程中会产生气泡，使环氧树脂形成多孔的三维结构，还会使导电填料的间隔距离缩短，降低电子在填料间跃迁的阻力。A high proportion of conductive fillers is added to the thermosetting epoxy resin and evenly dispersed, and then a certain proportion of hot volatile solvent is added. The addition of solvent can provide better fluidity for the composite material slurry, and the processability is greatly improved. In addition, in a vacuum, the hot volatile solvent will produce bubbles during the evaporation process, making the epoxy resin form a porous three-dimensional structure, and also shortening the spacing between the conductive fillers, reducing the resistance of electron transition between the fillers.
附图说明BRIEF DESCRIPTION OF THE DRAWINGS
图1为使用该方法时电子在不同导电填料之间跃迁的阻力变化示意图；FIG1 is a schematic diagram showing the change in resistance of electrons transitioning between different conductive fillers when using this method;
符号说明Explanation of symbols
1为导电填料；1 is a conductive filler;
2为环氧树脂层；2 is an epoxy resin layer;
31为不使用可挥发性溶剂时电子在导电填料之间跃迁的阻力；31 is the resistance of electron transition between conductive fillers when no volatile solvent is used;
32为本方法制备的三维导电网络中电子在不同导电填料之间跃迁的阻力。32 is the resistance of electron transition between different conductive fillers in the three-dimensional conductive network prepared by this method.
具体实施方式DETAILED DESCRIPTION
下面进一步例举实施例以详细说明本发明。同样应理解，以下实施例只用于对本发明进行进一步说明，不能理解为对本发明保护范围的限制，本领域的技术人员根据本发明的上述内容作出的一些非本质的改进和调整均属于本发明的保护范围，下述示例具体的工艺参数等也仅是合适范围中的一个示例，即本领域技术人员可以通过本文的说明做合适的范围内选择，而并非要限定于下文示例的具体数值。The following further exemplifies the present invention in detail. It should also be understood that the following examples are only used to further illustrate the present invention and cannot be understood as limiting the scope of protection of the present invention. Some non-essential improvements and adjustments made by those skilled in the art based on the above content of the present invention belong to the scope of protection of the present invention. The specific process parameters and the like in the following examples are only examples in a suitable range, that is, those skilled in the art can make a selection within a suitable range through the description herein, and are not limited to the specific values exemplified below.
实施例一1：Embodiment 1:
本实施例提供一种高导电性环氧树脂基复合材料及其制备方法，其具体步骤为：This embodiment provides a highly conductive epoxy resin-based composite material and a preparation method thereof, the specific steps of which are as follows:
(1)按照质量比3：1将300目的银粉加入TDE-85和甲基四氢苯酐混合的环氧树脂基胶中，使用球磨机对其进行第一步的研磨分散处理2h，此时，导电填料的比例为75％；(1) Add 300-mesh silver powder to an epoxy resin base adhesive mixed with TDE-85 and methyltetrahydrophthalic anhydride in a mass ratio of 3:1, and use a ball mill to grind and disperse it for 2 hours. At this time, the proportion of the conductive filler is 75%;
(2)在分散处理后的样品中添加与环氧树脂基胶同等质量的乙醇，继续进行研磨分散处理2h；(2) Add ethanol of the same mass as the epoxy resin base glue to the dispersed sample and continue the grinding and dispersion treatment for 2 hours;
(3)将步骤(2)获得的混合浆料倒如合适的模具中，置于1000Pa真空中，先在85℃下进行加热，使其中的乙醇快速蒸发，产生大量的气孔。待气孔稳定之后，再继续加热至180℃，维持3h，使环氧树脂固化成型，获得三维的环氧树脂导电网络；(3) Pour the mixed slurry obtained in step (2) into a suitable mold, place it in a vacuum of 1000Pa, and heat it at 85°C to quickly evaporate the ethanol therein to generate a large number of pores. After the pores are stabilized, continue to heat to 180°C and maintain for 3 hours to solidify the epoxy resin and obtain a three-dimensional epoxy resin conductive network;
(4)同样使用TDE-85和甲基四氢苯酐混合的环氧树脂基胶(与步骤(1)中的环氧树脂基胶的质量比为1:1)，加入质量比10％的丙烯基缩水甘油醚；(4) using the epoxy resin base glue mixed with TDE-85 and methyltetrahydrophthalic anhydride (the mass ratio of the epoxy resin base glue in step (1) is 1:1), adding 10% by mass of acryl glycidyl ether;
(5)将步骤(4)获得的环氧树脂基胶倒入步骤(3)获得的三维导电网络中，并继续置于1000Pa的真空中进行除泡，使步骤(4)获得的环氧树脂基胶能够充分填充进步骤(3)获得的三维导电网络中，在此过程中可以进行5次充放气处理，以使填充的更加彻底；(5) pouring the epoxy resin base glue obtained in step (4) into the three-dimensional conductive network obtained in step (3), and continuing to place it in a vacuum of 1000 Pa for degassing, so that the epoxy resin base glue obtained in step (4) can be fully filled into the three-dimensional conductive network obtained in step (3). During this process, the filling and degassing treatment can be performed 5 times to make the filling more thorough;
(6)将环氧树脂基胶填充进三维导电网络后，继续加热至180℃固化处理，维持3h，即可获得一种高导电性环氧树脂基复合材料。(6) After the epoxy resin-based glue is filled into the three-dimensional conductive network, it is further heated to 180°C for curing and maintained for 3 hours to obtain a highly conductive epoxy resin-based composite material.
实施例2：Embodiment 2:
本实施例提供一种高导电性环氧树脂基复合材料的方法，其具体方法参考实施例1，区别在于：步骤(1)的银粉更改为石墨烯，比例改为1：1。This embodiment provides a method for preparing a highly conductive epoxy resin-based composite material. The specific method is similar to that of Embodiment 1, except that the silver powder in step (1) is replaced with graphene, and the ratio is changed to 1:1.
实施例3：Embodiment 3:
本实施例提供一种高导电性环氧树脂基复合材料的方法，其具体方法参考实施例1，区别在于：步骤(4)中加入5％的石墨粉。This embodiment provides a method for preparing a highly conductive epoxy resin-based composite material. The specific method is similar to that of Embodiment 1, except that 5% of graphite powder is added in step (4).
对比例1：Comparative Example 1:
(1)按照1.5：1的比例将300目的银粉加入TDE-85和甲基四氢苯酐混合的环氧树脂基胶中，使用球磨机或研磨机对其进行第一步的研磨分散处理2h；(1) Add 300-mesh silver powder to epoxy resin base glue mixed with TDE-85 and methyltetrahydrophthalic anhydride in a ratio of 1.5:1, and use a ball mill or grinder to grind and disperse it for 2 hours;
(2)将混合浆料倒入模具中，并在180℃条件下加热固化3h；(2) Pour the mixed slurry into a mold and heat and cure it at 180°C for 3 hours;
对比例2：Comparative Example 2:
本对比例参考对比例1，区别在于将使用的银粉改为石墨粉，比例改为0.5：1。This comparative example refers to comparative example 1, except that the silver powder used is replaced by graphite powder, and the ratio is changed to 0.5:1.
对比例3：Comparative Example 3:
本对比例参考对比例1，区别在于在银粉中多加5％的石墨粉。This comparative example refers to comparative example 1, except that 5% more graphite powder is added to the silver powder.
实施例1-3以及对比例1-3制备得到的复合材料的电导率见表1The electrical conductivity of the composite materials prepared in Examples 1-3 and Comparative Examples 1-3 is shown in Table 1
表1不同实施例中一种高导电性环氧树脂基复合材料电导率Table 1 Electrical conductivity of a high conductivity epoxy resin-based composite material in different embodiments
综合上述实施例和对比例的结果可以看出，利用本发明的方法得到的高导电性环氧树脂基复合材料性能优异。本发明提供的方法艺简单生产成本不会增加，具有很好的技术经济性。对比例没有采用本发明的方案，因而无法取得本发明的优良效果。It can be seen from the results of the above embodiments and comparative examples that the high-conductivity epoxy resin-based composite material obtained by the method of the present invention has excellent performance. The method provided by the present invention is simple in process and does not increase production costs, and has good technical and economic benefits. The comparative example does not adopt the solution of the present invention, and thus cannot achieve the excellent effects of the present invention.
申请人声明，本发明通过上述实施例来说明本发明的详细方法，但本发明并不局限于上述详细方法，即不意味着本发明必须依赖上述详细方法才能实施。所属技术领域的技术人员应该明了，对本发明的任何改进，对本发明产品各原料的等效替换及辅助成分的添加、具体方式的选择等，均落在本发明的保护范围和公开范围之内。The applicant declares that the present invention illustrates the detailed method of the present invention through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned detailed method, that is, it does not mean that the present invention must rely on the above-mentioned detailed method to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of various raw materials of the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.
Claims (10)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310287733.7A CN118684997A (en) | 2023-03-22 | 2023-03-22 | A high-conductivity epoxy resin-based composite material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310287733.7A CN118684997A (en) | 2023-03-22 | 2023-03-22 | A high-conductivity epoxy resin-based composite material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN118684997A true CN118684997A (en) | 2024-09-24 |
Family
ID=92765114
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310287733.7A Pending CN118684997A (en) | 2023-03-22 | 2023-03-22 | A high-conductivity epoxy resin-based composite material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN118684997A (en) |
-
2023
- 2023-03-22 CN CN202310287733.7A patent/CN118684997A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US7465503B2 (en) | Molding material for fuel cell separator and method for preparing the same | |
| CN102775705B (en) | Polymer-matrix composite material and preparation method thereof | |
| CN106047242B (en) | Epoxy resin-based conductive adhesive and preparation method thereof | |
| CN106810818B (en) | A kind of graphene modified epoxy resin and preparation method thereof | |
| CN114784307B (en) | Graphene reinforced expanded graphite/polyimide-polyether-ether-ketone composite bipolar plate and preparation method thereof | |
| JP5257497B2 (en) | Porous separator for fuel cell | |
| JP3573444B2 (en) | Carbonaceous separator member for polymer electrolyte fuel cell and method of manufacturing the same | |
| Wei et al. | Preparation and properties of graphite/polypropylene composite material reinforced by chopped carbon fibers for proton‐exchange membrane fuel cell bipolar plates | |
| CN103030807B (en) | In situ intercalation solution preparation of graphene oxide benzoxazine nanocomposite resins | |
| CN118344724A (en) | A kind of conductive and thermal conductive composite material and preparation method thereof | |
| CN102560530A (en) | Nano nickel mass point reinforced non-graphitized conductive carbon cathode material and preparation method thereof | |
| JP2000021421A (en) | Separator member for polymer electrolyte fuel cell and method of manufacturing the same | |
| CN118684997A (en) | A high-conductivity epoxy resin-based composite material and preparation method thereof | |
| CN101974207B (en) | Nano-graphite sheet-based composite material with high electric conductivity and preparation method thereof | |
| CN106009517B (en) | A kind of epoxy resin/nickel-coated carbon fibers composite conducting foam and preparation method thereof | |
| CN112310427A (en) | Preparation system of composite graphite bipolar plate | |
| CN116969438B (en) | Composite resin-based hard carbon material, sodium ion battery and preparation method thereof | |
| CN114759209A (en) | Expanded graphite/polyimide-polyether sulfone composite bipolar plate and preparation method thereof | |
| CN212676306U (en) | Layered ultra-thin carbon-based bipolar plate | |
| CN108232226B (en) | Preparation method of ceramic composite bipolar plate for vanadium battery | |
| CN108376785A (en) | A kind of preparation method of polyimides-graphite composite material bipolar plates | |
| CN101986392A (en) | A conducting material and preparation method and use thereof | |
| KR100781628B1 (en) | Graphite composite fuel cell separator and its manufacturing method | |
| CN118684995A (en) | A graphene/metal resin composite material and its preparation method and application | |
| CN116454307B (en) | Manufacturing method of composite graphite bipolar plate for fuel cell |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |