CN114456588A - High-strength high-thermal-conductivity electromagnetic shielding nylon composite material and preparation method thereof - Google Patents
High-strength high-thermal-conductivity electromagnetic shielding nylon composite material and preparation method thereof Download PDFInfo
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- CN114456588A CN114456588A CN202210121527.4A CN202210121527A CN114456588A CN 114456588 A CN114456588 A CN 114456588A CN 202210121527 A CN202210121527 A CN 202210121527A CN 114456588 A CN114456588 A CN 114456588A
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- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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Abstract
The invention discloses a high-strength high-heat-conductivity electromagnetic shielding nylon composite material and a preparation method thereof, wherein the composite material is prepared from the following raw materials in parts by weight: 40-60 parts of nylon resin, 20-40 parts of carbon fiber, 20-40 parts of mesocarbon microbeads, 0.1-5 parts of dispersing agent and 0.1-1 part of antioxidant; the invention utilizes the bridging effect of the micron-sized spherical mesocarbon microbeads and the chopped carbon fibers to form a perfect heat conducting network, greatly improves the heat conducting performance and the electromagnetic shielding performance, and greatly improves the strength of the composite material under the reinforcing effect of the carbon fibers.
Description
Technical Field
The invention belongs to the technical field of electromagnetic shielding heat conduction materials, and particularly relates to a high-strength high-heat-conduction electromagnetic shielding nylon composite material and a preparation method thereof.
Background
With the technological progress, electronic devices are rapidly developed towards miniaturization and integration, the heat productivity of equipment is gradually increased, and the requirement on heat conduction materials is higher and higher. In addition, when the electronic component works, electromagnetic waves are generated, the electromagnetic waves can generate electromagnetic interference on the electronic component, and the normal work of other components can be influenced by the strong electromagnetic interference, so that the development of a novel electromagnetic shielding material is urgently needed to ensure the normal operation of the component.
Carbon materials such as graphene and carbon nanotubes have excellent heat conducting property and electric conductivity, but the graphene and the carbon nanotubes have small particle size and are easy to agglomerate, and good dispersion is difficult to achieve by simple melt blending. For example, CN104844795A discloses a high-strength heat-conducting nylon 6 and a preparation method thereof, and an author adds a modified graphene dispersion liquid into a caprolactam polymerization system, and successfully improves the dispersion degree of graphene in a nylon 6 matrix by matching with a magnetic field and ultrasonic treatment.
And the materials such as graphene and carbon nanotubes are high in price, and are not completely industrialized, so that the problem of cost is difficult to solve. For example, CN111040428A discloses an electromagnetic shielding high thermal conductivity nylon composite material, and the author prepares the composite material by extruding and injection molding fillers such as graphene, carbon nanotubes, silica, modified red mud and the like with nylon resin. Although the material has excellent performance, the content of graphene and carbon nanotubes is not low, and the cost of the composite material is high.
In order to solve the problems, the invention improves the performance of a nylon matrix by taking the one-dimensional mesocarbon microbeads and the two-dimensional carbon fibers as mixed fillers, and after melting and blending, the fillers achieve good dispersion and more heat conduction paths are constructed due to size difference, thereby obviously improving the heat conduction performance of the composite material. The mesocarbon microbeads have good chemical stability, thermal stability and excellent electric and thermal conductivity, and are isotropic materials. Carbon fibers belong to two-dimensional materials, and have excellent electrical conductivity and thermal conductivity along the fiber axis direction, but the thermal conductivity in the radial direction is not ideal, and orientation is easy to occur during melt blending injection molding, so that the composite material has high heat conductivity in the face direction, and the axial heat conductivity is not ideal. The combination of the two fillers can simultaneously improve the facing and axial heat conducting capability of the composite material. And the addition of the carbon fiber improves the overall mechanical property of the material, improves the dimensional stability and reduces the water absorption of the nylon.
Disclosure of Invention
The invention provides a high-strength high-heat-conductivity electromagnetic shielding nylon composite material and a preparation method thereof.
The high-strength high-heat-conductivity electromagnetic shielding nylon composite material prepared by the invention can simultaneously meet the performance requirements of injection molding, good mechanical property, high thermal deformation temperature, effective electromagnetic interference shielding, heat conduction generated by the work of electronic devices and the like, and the electromagnetic shielding property of the composite material mainly takes absorption loss and greatly reduces secondary pollution. The composite material is prepared without a solvent, is green and environment-friendly, only needs simple melt blending, has low manufacturing cost and wide application range, and is suitable for industrial production.
The invention utilizes the bridging effect of the micron-sized spherical mesocarbon microbeads and the chopped carbon fibers to form a perfect heat conducting network, greatly improves the heat conducting performance and the electromagnetic shielding performance, and greatly improves the strength of the composite material under the reinforcing effect of the carbon fibers.
The technical scheme of the invention is as follows:
the electromagnetic shielding nylon composite material with high strength and high heat conductivity is prepared from the following raw materials in parts by weight:
40-60 parts of nylon resin, 20-40 parts of carbon fiber, 20-40 parts of mesocarbon microbeads, 0.1-5 parts of dispersing agent and 0.1-1 part of antioxidant.
Further:
the nylon resin is one or a compound of PA6 and PA66, and the viscosity is 2.7; preferably, the weight ratio of PA6 to PA66 is 5: 1, compounding;
the diameter of the carbon fiber is 10-20 mu m, the length of the carbon fiber is 2-5 mm, and the carbon content is higher than 95%; preferably, the carbon fibers are short carbon fiber shreds coated with polar polymer bundling agent;
the particle size of the mesocarbon microbeads is 10-20 mu m, and the graphitization degree is more than 99%;
the dispersing agent is selected from one or more of silicone powder, TAF-A, EBS and zinc stearate;
the antioxidant is selected from 1098[ N, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine ] or 626[ bis (2, 4-di-tert-butylphenol) pentaerythritol diphosphite ], or a mixture of the two, preferably the weight ratio of the two is 1: 1-2.
The preparation method of the high-strength high-heat-conductivity electromagnetic shielding nylon composite material comprises the following steps:
(1) vacuum drying the raw materials at 85 ℃ for 12h, and mixing the nylon resin, the mesocarbon microbeads, the antioxidant and the dispersant according to the formula to obtain a premix;
(2) adding the premix from a main feed inlet of a double-screw extruder, adding the carbon fiber through a side feeding device, and performing melt extrusion, cooling, grain cutting and drying to obtain a nylon composite material;
preferably, the length-diameter ratio of a screw of the double-screw extruder is 36-46, and the temperature range in the extrusion process is 260-290 ℃; the fillers are uniformly distributed in the matrix, and the multi-size fillers are easy to form a good heat conduction path.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, three-dimensional and two-dimensional fillers are combined to construct a more compact interpenetrating conductive heat-conducting network (see a schematic diagram and a scanning electron microscope in figure 1), so that the heat-conducting electromagnetic shielding performance of the composite material is remarkably improved;
2. the mesocarbon microbeads are used as the filler, have excellent electrical conductivity and thermal conductivity and spherical microstructure, can play a role in improving the absorption of electromagnetic waves in a polymer matrix, and avoid secondary pollution of the electromagnetic waves;
3. according to the invention, the carbon fiber is used as the filler, the carbon fiber has good electrical conductivity and thermal conductivity along the fiber axis direction, the axial thermal conductivity of the material can be greatly improved without influencing the heat conductivity of the composite material by compounding with the mesocarbon microbeads, and the carbon fiber has high strength and modulus along the fiber axis direction, so that the mechanical property of the composite material can be greatly improved;
4. according to the invention, nylon 6 and nylon 66 are compounded to serve as matrix materials, so that the compatibility of the nylon 6 and the nylon 66 is very good, the crystallinity is reduced, and the toughness is improved while the strength of the composite material is kept.
Drawings
FIG. 1 is a schematic view of the structure of the composite material of the present invention and a scanning electron microscope image of a cross section.
FIG. 2 scanning electron microscope cross-sectional images of the composites of example 3.
Detailed Description
The invention is further described below by means of specific examples, without the scope of protection of the invention being limited thereto.
The mesocarbon microbeads used in the following examples have a particle size of 10 to 20 μm and a graphitization degree of 99% or more, and are provided by Tianjin Aimin corporation; the carbon fiber has the diameter of 10-20 mu m and the length of 2-5 mm, the carbon content is higher than 95 percent, and the carbon fiber is a polar polymer bundling agent coated carbon fiber short cut filament provided by Shanghai Yu Tonghuai engineering and technology Limited liability company, and the preferred mark is CBZ-HT 2; the silicone powder is provided by Kejie plastic, preferably with the brand name polyamide lubricant PA-B.
Example 1
1kg of nylon 6, 200g of nylon 66, 800g of carbon fiber, 10g of silicone powder, 4g of antioxidant 1098 and 4g of antioxidant 626 are dried for 12 hours in vacuum at 85 ℃, and are extruded and granulated by a double screw, and then a mechanical test sample strip, a heat conduction test wafer and an electromagnetic shielding test sample strip are formed by injection molding.
Temperature of each zone of the extruder: a first area: 260 ℃ and a second zone: 265 ℃ and three zones: 270 ℃ and four zones: 275 ℃ and five zones: 280 ℃ and six regions: 280 ℃ and seven regions: 275 ℃ and eight regions: 270 ℃ and nine zones: 270 ℃ and ten regions: 275 ℃. The specific properties are shown in Table II.
Example 2
1kg of nylon 6, 200g of nylon 66, 200g of mesophase carbon microspheres, 600g of carbon fibers, 10g of silicone powder, 4g of antioxidant 1098 and 4g of antioxidant 626 are dried in vacuum at 85 ℃ for 12h, and are extruded and granulated by a double screw, and then a mechanical test sample strip, a heat conduction test wafer and an electromagnetic shielding test sample strip are injection-molded.
Temperature of each zone of the extruder: a first area: 260 ℃ and a second zone: 265 ℃ and three zones: 270 ℃ and four zones: 275 ℃ and five zones: 280 ℃ and six regions: 280 ℃ and seven regions: 275 ℃ and eight zones: 270 ℃ and nine zones: 270 ℃ and ten regions: 275 ℃. The specific properties are shown in Table II.
Example 3
1kg of nylon 6, 200g of nylon 66, 400g of mesocarbon microbeads, 400g of carbon fibers, 10g of silicone powder, 4g of antioxidant 1098 and 4g of antioxidant 626 are dried in vacuum at 85 ℃ for 12h, and are extruded and granulated by a double screw, and then a mechanical test sample strip, a heat conduction test wafer and an electromagnetic shielding test sample strip are formed by injection molding.
Temperature of each zone of the extruder: a first area: 260 ℃ and a second zone: 265 ℃ and three zones: 270 ℃ and four zones: 275 ℃ and five zones: 280 ℃ and six regions: 280 ℃ and seven regions: 275 ℃ and eight regions: 270 ℃ and nine zones: 270 ℃ and ten regions: 275 ℃. The specific properties are shown in Table II.
Example 4
1kg of nylon 6, 200g of nylon 66, 600g of mesophase carbon microspheres, 200g of carbon fibers, 10g of silicone powder, 4g of antioxidant 1098 and 4g of antioxidant 626 are dried in vacuum at 85 ℃ for 12 hours, and are extruded and granulated by a double screw, and then a mechanical test sample strip, a heat conduction test wafer and an electromagnetic shielding test sample strip are injection-molded.
Temperature of each zone of the extruder: a first area: 260 ℃ and a second zone: 265 ℃ and three zones: 270 ℃ and four zones: 275 ℃ and five zones: 280 ℃ and six regions: 280 ℃ and seven regions: 275 ℃ and eight regions: 270 ℃ and nine zones: 270 ℃ and ten regions: 275 ℃. The specific properties are shown in Table II.
Example 5
1kg of nylon 6, 200g of nylon 66, 800g of mesophase carbon microspheres, 10g of silicone powder, 4g of antioxidant 1098 and 4g of antioxidant 626 are dried in vacuum at 85 ℃ for 12h, extruded and granulated by a double screw, and then injection molded into mechanical test sample strips, heat conduction test wafers and electromagnetic shielding test sample strips.
Temperature of each zone of the extruder: a first area: 260 ℃ and a second region: 265 ℃ and three zones: 270 ℃ and four zones: 275 ℃ and five zones: 280 ℃ and six regions: 280 ℃ and seven regions: 275 ℃ and eight regions: 270 ℃ and nine zones: 270 ℃ and ten regions: 275 ℃. The specific properties are shown in Table II.
The formula of the electromagnetic shielding nylon material with different heat conduction in the embodiment of the invention comprises the following raw materials in parts by weight as shown in the following table 1:
TABLE 1
The mechanical, thermal conductive and electromagnetic shielding properties of the heat-conducting electromagnetic shielding nylon composite material prepared by the embodiment of the invention are shown in the following table 2:
the mechanical properties of the composite material were tested using a universal tester ((Instron-5966, USA.) according to ISO 527-2, tensile tests were carried out at a speed of 50mm/min at 23 ℃ and 50% relative humidity using type A test specimens, for bending tests, test specimens were prepared according to ISO 178 standard, testing being carried out at a span of 64mm and at a speed of 2mm/min, respectively.
Based on the Hot plate transient planar source method, the thermal conductivity of the composite was quantitatively analyzed using a thermal constant analyzer (Hot Disk TPS2500S, Sweden). The thermal conductivity was measured at room temperature in an air atmosphere using a disc having a radius of 25 mm and a thickness of 2 mm.
And testing the electromagnetic shielding performance of the composite material by using a vector network analyzer. The test was carried out using rectangular strips 22.86 mm in length, 10.16 mm in width and 2mm in thickness under electromagnetic waves in the 8-12GHz band.
Table 2 shows the mechanical, thermal and electromagnetic shielding properties of different embodiments of the thermally conductive electromagnetic shielding nylon of the present invention.
TABLE 2
After the heat-conducting filler is added, compared with pure nylon (the heat-conducting coefficient is about 0.3W/mK), the heat-conducting property of the composite material is greatly improved. However, in example 5, only the mesophase carbon microspheres are used as the filler, which does not greatly improve the mechanical properties of the composite material, and the electromagnetic shielding effect is general. In example 1, only carbon fiber is used as filler, and although the mechanical properties are obviously improved, the thermal conductivity and the electromagnetic shielding performance are not obviously improved.
In the embodiment 3, a perfect heat conduction path is constructed by compounding the carbon fiber and the mesocarbon microbeads, so that the facing heat conductivity coefficient and the axial heat conductivity coefficient of the material both reach about 2W/m.K, and the composite material has a good electromagnetic shielding effect and excellent overall mechanical properties. FIG. 2 is a sectional scanning electron micrograph of example 3.
Claims (7)
1. The high-strength high-heat-conductivity electromagnetic shielding nylon composite material is characterized by comprising the following raw materials in parts by weight:
40-60 parts of nylon resin, 20-40 parts of carbon fiber, 20-40 parts of mesocarbon microbeads, 0.1-5 parts of dispersing agent and 0.1-1 part of antioxidant;
the nylon resin is one or a compound of PA6 and PA 66;
the diameter of the carbon fiber is 10-20 mu m, the length of the carbon fiber is 2-5 mm, and the carbon content is higher than 95%;
the particle size of the mesocarbon microbeads is 10-20 mu m, and the graphitization degree is more than 99%.
2. The high-strength high-thermal-conductivity electromagnetic shielding nylon composite material as claimed in claim 1, wherein the nylon resins are PA6 and PA66 in a weight ratio of 5: 1, compounding.
3. The high-strength high-thermal-conductivity electromagnetic shielding nylon composite material as claimed in claim 1, wherein the carbon fibers are polar polymer bundling agent coated carbon fiber chopped filaments.
4. The high-strength high-thermal-conductivity electromagnetic shielding nylon composite material as claimed in claim 1, wherein the dispersing agent is one or more selected from silicone powder, TAF-A, EBS and zinc stearate.
5. The high-strength high-thermal-conductivity electromagnetic shielding nylon composite material as claimed in claim 1, wherein the antioxidant is selected from 1098[ N, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine ] or 626[ bis (2, 4-di-tert-butylphenol) pentaerythritol diphosphite ], or a mixture thereof.
6. The preparation method of the high-strength high-thermal-conductivity electromagnetic shielding nylon composite material as claimed in claim 1, wherein the preparation method comprises the following steps:
(1) vacuum drying the raw materials at 85 ℃ for 12h, and mixing the nylon resin, the mesocarbon microbeads, the antioxidant and the dispersant according to the formula to obtain a premix;
(2) adding the premix from a main feed inlet of a double-screw extruder, adding the carbon fiber through a side feeding device, and performing melt extrusion, cooling, granulating and drying to obtain the nylon composite material.
7. The preparation method of claim 6, wherein the double-screw extruder has a screw length-diameter ratio of 36-46 and a temperature range of 260-290 ℃ during the extrusion process.
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| US20020058743A1 (en) * | 2000-09-12 | 2002-05-16 | Masayuki Tobita | Thermally conductive polymer composition and thermally conductive molded article |
| CN101787645A (en) * | 2010-03-02 | 2010-07-28 | 东华大学 | Carbon fiber surface electropolymerization treatment method |
| CN102931560A (en) * | 2012-11-21 | 2013-02-13 | 天津市贝特瑞新能源科技有限公司 | Brush material with excellent performance, and preparation method and application thereof |
| US20170158513A1 (en) * | 2015-12-03 | 2017-06-08 | Aruna Zhamu | Chemical-free production of graphene materials |
| CN107118556A (en) * | 2017-06-21 | 2017-09-01 | 安徽江淮汽车集团股份有限公司 | A kind of PPS composites and preparation method thereof |
| CN110655413A (en) * | 2019-09-18 | 2020-01-07 | 济宁碳素集团有限公司 | Preparation method of isotropic graphite material |
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- 2022-02-09 CN CN202210121527.4A patent/CN114456588B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020058743A1 (en) * | 2000-09-12 | 2002-05-16 | Masayuki Tobita | Thermally conductive polymer composition and thermally conductive molded article |
| CN101787645A (en) * | 2010-03-02 | 2010-07-28 | 东华大学 | Carbon fiber surface electropolymerization treatment method |
| CN102931560A (en) * | 2012-11-21 | 2013-02-13 | 天津市贝特瑞新能源科技有限公司 | Brush material with excellent performance, and preparation method and application thereof |
| US20170158513A1 (en) * | 2015-12-03 | 2017-06-08 | Aruna Zhamu | Chemical-free production of graphene materials |
| CN107118556A (en) * | 2017-06-21 | 2017-09-01 | 安徽江淮汽车集团股份有限公司 | A kind of PPS composites and preparation method thereof |
| CN110655413A (en) * | 2019-09-18 | 2020-01-07 | 济宁碳素集团有限公司 | Preparation method of isotropic graphite material |
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