CN115403928B - Electronic packaging material with heat conduction electromagnetic shielding performance and preparation method thereof - Google Patents
Electronic packaging material with heat conduction electromagnetic shielding performance and preparation method thereof Download PDFInfo
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- C09K5/14—Solid materials, e.g. powdery or granular
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
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- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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Abstract
The invention discloses an electronic packaging material with heat conduction electromagnetic shielding performance and a preparation method thereof. The metal interface layer in the invention enables the thermosetting resin particles to be fully wetted by the low-melting-point alloy, and the metal interface layer and the low-melting-point alloy generate intermetallic compounds, thereby promoting the low-melting-point alloy to coat the resin particles and further forming the isolation structure composite material. The low-melting-point alloy bonds thermosetting resin particles through solid-liquid phase transition, so that the problem that the thermosetting resin cannot be processed secondarily is solved. The existence of the metal interface layer and the isolation structure in the composite material ensures that the composite material realizes excellent heat conduction and electromagnetic shielding performance simultaneously.
Description
Technical Field
The invention belongs to the technical field of electronic packaging materials, and particularly relates to an electronic packaging material with heat conduction electromagnetic shielding electrical property and a preparation method thereof.
Background
Nowadays, electronic packaging technology increasingly shows a trend of high power and miniaturization, the size of a chip is reduced from micrometers to a few nanometers, heat generated by the operation of components is increased exponentially, and if the heat cannot be effectively removed, heat accumulation is generated, so that the components are thermally disabled, and the performance of the components is reduced and the service life of the components is shortened. In addition, the radiation of electromagnetic waves is not only harmful to the human body, but also has a radiation effect on the devices and adjacent equipment in operation. With the popularization of 5G information technology, the promotion of the working frequency band of devices and the development of radio frequency devices, electromagnetic radiation is inevitably present in various occasions, so that an electronic packaging material with good heat conduction and electromagnetic shielding performance is a highly-needed functional material.
Thermosetting resins are widely used for electronic packaging materials due to their light weight, low cost, chemical resistance, and the like. Although crystallization of the molecular chain of the resin can effectively improve the heat conductivity, the requirements of heat dissipation and electromagnetic shielding performance are still not satisfied. The general solution is to introduce filler with good heat and electric conductivity into thermosetting resin. The carbon material has good electrical conductivity and thermal conductivity, and is the first choice filler of the heat conduction and electromagnetic shielding composite material. To achieve good heat conduction and electromagnetic shielding performance, a large amount of carbon materials need to be filled, and due to the effects of pi-pi bonds and the like, the carbon materials are easy to agglomerate in a matrix, so that the processing is difficult, and the mechanical property of the composite material is reduced. There are studies on the realization that good dispersion can be achieved under low carbon material loading by structural design such as isolation structure, orientation structure, etc. (Composites Part A,2016,90,606-613;Small 2018,1704044), but the performance of the composite is not further improved. The metal particles have higher electrical conductivity and good thermal conductivity, but their melting points are higher than the processing temperature of the polymer, and are in a solid state during processing, which increases the melt viscosity and wears the processing equipment. In order to use the high conductivity of the metal material, there is a study of coating the surface of the metal material with a Carbon material or coating the surface of the Carbon material with a metal material (Carbon, 2011,49,1965-1971), but the metal material is relatively easy to fall off, and the conductivity is lowered or oxidized to lose the conductivity.
Disclosure of Invention
The invention aims to provide an electronic packaging material with heat conduction and electromagnetic shielding performance, which has excellent heat conduction and electromagnetic shielding performance, has high application value in the field of electronic packaging, and solves the problem that a metal material is easy to fall off in the prior art.
In order to achieve the above purpose, the present invention adopts the following technical scheme: the electronic packaging material with the heat conduction electromagnetic shielding performance comprises thermosetting resin particles and low-melting-point alloy filled among the thermosetting resin particles, wherein the surfaces of the thermosetting resin particles are coated with metal interface layers, the metal interface layers are metal layers formed by connecting single metal particles, the metal elements of the low-melting-point alloy are different from the metal elements of the metal interface layers, and the metal elements of the low-melting-point alloy react with the metal elements in the metal interface layers to form intermetallic compounds on the surface of the low-melting-point alloy connected with the metal interface layers; the melting point of the low melting point alloy is lower than the melting point of the thermosetting resin particles.
Further improvement of the electronic packaging material with heat conduction electromagnetic shielding performance:
preferably, in the electronic packaging material, the content of the low-melting-point alloy is 3-50 wt%, the content of the metal interface layer is 0.5-15 wt%, the content of the intermetallic compound is 2-12 wt%, and the sum of the content percentages of the total components is 100wt%.
Preferably, the thermosetting resin particles have a spherical structure and a particle diameter of 800nm to 800. Mu.m.
Preferably, the material of the thermosetting resin particles is one of epoxy resin and polyimide resin.
Preferably, the low-melting-point alloy is an alloy of two or more elements selected from tin, bismuth, lead, indium, gallium, zinc, cadmium, mercury, silver and copper.
Preferably, the melting point of the low melting point alloy is 105-232 ℃.
Preferably, the metal interface layer is one of a silver interface layer, a copper interface layer, a magnesium interface layer, a nickel interface layer, a gold interface layer and an aluminum interface layer, and the size of metal particles composing the metal interface layer is 20 nm-500 nm.
The second object of the present invention is to provide a method for preparing the electronic packaging material with heat conduction electromagnetic shielding performance, which comprises the following steps:
s1, coating a layer of metal interface layer on the surface of thermosetting resin particles in a chemical plating, electroplating or spraying mode, wherein the thickness of the interface metal layer is 20 nm-1 mu m, and the mass ratio of the thermosetting resin particles to the metal interface layer is 1.5-188 to obtain modified thermosetting resin particles;
s2, uniformly mixing the low-melting-point alloy with the modified thermosetting resin particles, wherein the mass ratio of the low-melting-point alloy in the mixture is 3-50wt%, placing the mixture in a model, and hot-pressing at a temperature higher than the melting point of the low-melting-point alloy and lower than the melting point of the modified thermosetting resin particles to obtain the electronic packaging material with heat conduction electromagnetic shielding performance.
The preparation method of the electronic packaging material with the heat conduction electromagnetic shielding performance is further improved:
preferably, the thermosetting resin particles are produced by any one of precipitation polymerization, vapor-induced phase separation, mechanical disruption, emulsion polymerization, and solution polymerization.
Preferably, the hot press molding time in the step S2 is 10 min-50 min, and the hot press pressure is 5 MPa-30 MPa.
The principle of the invention is as follows:
the melting point of the low-melting-point alloy is lower than that of the thermosetting resin, and the low-melting-point alloy is in a liquid state in the hot pressing process, so that the viscosity of a composite system can be reduced, the processing performance can be improved, and the equipment abrasion can be reduced. In order to increase the combination of the low-melting-point alloy and the thermosetting resin, the invention obtains the thermosetting resin particles with regular structures, introduces a metal interface layer on the surfaces of the polymer particles, and carries out hot pressing processing at the temperature above the melting point of the low-melting-point alloy and below the melting point of the thermosetting resin to obtain the composite material with the isolation structure, and the composite material has good heat conduction and electromagnetic shielding performance. The low-melting-point alloy can bond thermosetting resin particles, and solves the problem that thermosetting resin cannot be hot pressed.
The spherical thermosetting resin particles are not deformed in hot pressing, and are a good matrix template of the isolation structure. The metallic interfacial layer on the surface of the thermosetting resin enables the thermosetting resin particles to be sufficiently wetted by the low melting point alloy. The hot pressing temperature is above the melting point of the low-melting-point alloy, the low-melting-point alloy can flow in a thermosetting resin particle system to be fully dispersed, and metal elements in alloy components and metal elements in a metal interface layer generate intermetallic compounds, so that the flowing low-melting-point alloy is directionally coated among the thermosetting resin particles to form the composite material with the isolation structure. Under the synergistic effect of the heat-conducting and electricity-conducting metal interface layer and the low-melting-point alloy isolation structure, the composite material has good heat conduction and electromagnetic shielding performance.
Compared with the prior art, the invention has the beneficial effects that:
(1) The composite material with the isolation structure has excellent heat conduction and electromagnetic shielding performance.
(2) The surface metal interface layer treatment technology of the thermosetting resin particles in the composite material has good applicability and obvious effect.
(3) The low-melting-point alloy provided by the invention has fluidity above the melting point, can fully wet thermosetting resin particles, and can synchronously realize excellent heat conduction and electromagnetic shielding performance with a low content by coating the thermosetting resin particles with the metal interface layer through intermetallic compounds.
(4) The low-melting-point alloy can solve the problem that thermosetting resin cannot be processed secondarily.
(5) The method for preparing the composite material has wide applicability, is simple and feasible, and is suitable for large-scale production and processing.
Drawings
FIG. 1 is a block diagram of a composite material produced in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of the composite material of example 1 of the present invention;
FIG. 3 is an X-ray diffraction pattern of the composite material of example 1 of the present invention.
Detailed Description
The present invention will be further described in detail with reference to the following examples, in order to make the objects, technical solutions and advantages of the present invention more apparent, and all other examples obtained by those skilled in the art without making any inventive effort are within the scope of the present invention based on the examples in the present invention.
Example 1
The embodiment provides a preparation method of a low-melting-point alloy/polyimide composite material with heat conduction electromagnetic shielding performance, which comprises the following steps:
s1, weighing 5g of polyimide resin in 50ml of N, N-dimethylformamide, stirring for 10 hours in a water bath kettle at 70 ℃, transferring the mixed solution to a constant temperature and humidity box at 90% humidity and 30 ℃ for 24 hours, collecting a product, washing with deionized water for 5 times, and drying. 100mg of dopamine hydrochloride and 1g of polyimide particles are added into 250ml (Tri solution: absolute ethyl alcohol=3:1) mixed solution with the pH of 8.5, oxygen is introduced for reaction for 48 hours, resin microspheres coated with dopamine are obtained, the resin microspheres coated with dopamine and 0.5g of glucose are added into 100ml of silver ammonia solution for reaction for 6 hours, and polyimide particles with silver interface layers coated on the surfaces, namely modified polyimide particles, are obtained.
S2, preparing a composite material: weighing 1.2-gSn-58 Bi and 2g of the modified polyimide particles obtained in the step 2, uniformly mixing, placing the mixture in a model, and hot-pressing at 220 ℃ and 10MPa for 15min to obtain the low-melting-point alloy/polyimide composite material.
FIG. 1 is a schematic diagram of a composite material with an isolation structure, wherein a cross-sectional scan of the composite material is shown in FIG. 2, modified polyimide particles are kept in a regular sphere shape, and alloy particles are coated on the surfaces of the modified polyimide particles to form the composite material shown in FIG. 1. As is clear from the X-ray diffraction pattern, the (201) crystal face at 34.8 DEG is attributed to the low-melting-point alloy and silver interface layer to generate Ag 3 And the Sn intermetallic compound enables the low-melting-point alloy to be directionally coated on the surfaces of the polyimide particles to form the isolation structure composite material.
Example 2
The embodiment provides a preparation method of a low-melting-point alloy/epoxy resin composite material with heat conduction electromagnetic shielding performance, which comprises the following steps:
s1, uniformly mixing 0.6g of triglycidyl aminophenol and diethyl toluenediamine (the molar ratio is 3:4) in 200ml of polypropylene glycol solvent by magnetic stirring, then placing the mixture in an oven for curing for 18 hours at 140 ℃, washing the obtained precipitate by using hot ethanol, and drying the precipitate at 80 ℃ in a vacuum drying oven. 100mg of dopamine hydrochloride and 1g of epoxy resin are added into 250ml (Tri solution: absolute ethyl alcohol=3:1) mixed solution with the pH of 8.5, oxygen is introduced for reaction for 48 hours, resin microspheres coated with dopamine are obtained, the microspheres and 0.5g of glucose are added into 100ml of silver ammonia solution for reaction for 6 hours, and epoxy resin particles with silver interface layers coated on the surfaces, namely modified epoxy resin particles, are obtained.
S2, weighing 1.2gSn-58Bi and 2g of the modified epoxy resin particles obtained in the step 2, uniformly mixing, placing the mixture in a model, and hot-pressing at 180 ℃ and 10MPa for 15min to obtain the low-melting-point alloy/epoxy resin composite material.
Example 3
The embodiment provides a preparation method of a low-melting-point alloy/epoxy resin composite material with heat conduction electromagnetic shielding performance, which comprises the following steps:
s1, weighing 500g of epoxy resin in an ultralow temperature freezing pulverizer, introducing liquid nitrogen, crushing the epoxy resin at a speed of 5000r/min, and selecting 300-mesh and 200-mesh molecular sieve filtered epoxy resin particles. And treating the epoxy resin particles with the particle size of 800 nm-800 mu m through a magnetron sputtering instrument for 20min under the condition that the vacuum degree is 2Pa, so as to obtain the epoxy resin particles with the surface coated with the silver interface layer, namely the modified epoxy resin particles.
S2, weighing 1.8g of Sn-58Bi and 2g of the modified epoxy resin particles obtained in the step 2, uniformly mixing, placing the mixture in a model, and hot-pressing at 180 ℃ and 10MPa for 15min to obtain the low-melting-point alloy/epoxy resin composite material.
Table 1 comparison of thermal conductivity and shielding effectiveness for examples 1, 2 and 3
| Sample of | Thermal conductivity (W/mk) | Shielding effectiveness (dB@10GHz) |
| Example 1 | 0.81 | 36.42 |
| Example 2 | 1.92 | 45.39 |
| Example 3 | 3.08 | 52.47 |
As can be seen from Table 1, the insulation structure composite material obtained by compounding the polyimide resin or the epoxy resin which is introduced with the silver interface layer and the low-melting-point alloy has good heat conductivity and electromagnetic shielding performance. As is apparent from the test results of table 1, comparative examples 1 and 2 differ in thermal conductivity properties at the same low melting point alloy content because the obtained resin particles differ in particle size due to the different preparation methods of the thermosetting resin particles. The larger the resin particles are, the more favorable is for reducing the interface between the matrix and the filler, so as to reduce phonon scattering, and the more favorable is for improving the heat conduction performance of the composite material. Therefore, in the application, particles with larger resin particle size are selected as the matrix as much as possible. As can be seen from comparative examples 2 and 3, the thermal conductivity and electromagnetic shielding properties of the composite material increase with the increase in the content of the low melting point alloy, and the properties of the composite material can be adjusted by adjusting the filler content.
Those skilled in the art will appreciate that the foregoing is merely a few, but not all, embodiments of the invention. It should be noted that many variations and modifications can be made by those skilled in the art, and all variations and modifications which do not depart from the scope of the invention as defined in the appended claims are intended to be protected.
Claims (5)
1. The electronic packaging material with the heat conduction electromagnetic shielding performance is characterized by comprising thermosetting resin particles which are uniformly dispersed and low-melting-point alloy filled among the thermosetting resin particles, wherein the surfaces of the thermosetting resin particles are coated with metal interface layers, the metal interface layers are metal layers formed by connecting single metal particles, the metal elements of the low-melting-point alloy are different from the metal elements of the metal interface layers, and at least one metal element in the low-melting-point alloy reacts with the metal element in the metal interface layers to form intermetallic compounds on the surface, connected with the metal interface layers, of the low-melting-point alloy; the melting point of the low-melting-point alloy is lower than that of the thermosetting resin particles;
in the electronic packaging material, the content of the low-melting-point alloy is 3 to 50 weight percent, the content of the metal interface layer is 0.5 to 15 weight percent, the content of intermetallic compounds is 2 to 12 weight percent, the sum of the content percentages of the total components is 100 weight percent, and the balance is thermosetting resin particles;
the thermosetting resin particles are made of one of epoxy resin and polyimide resin;
the low-melting-point alloy is an alloy of two or more elements of tin, bismuth, lead, indium, gallium, zinc, cadmium, mercury, silver and copper;
the melting point of the low-melting-point alloy is 105-232 ℃;
the metal interface layer is one of a silver interface layer, a copper interface layer, a magnesium interface layer, a nickel interface layer, a gold interface layer and an aluminum interface layer, and the size of metal particles composing the metal interface layer is 20 nm-500 nm.
2. The electronic packaging material with heat conducting electromagnetic shielding performance according to claim 1, wherein the thermosetting resin particles have a spherical structure and a particle size of 800 nm-800 μm.
3. A method for preparing an electronic packaging material having heat conductive electromagnetic shielding properties according to any one of claims 1 to 2, comprising the steps of:
s1, coating a layer of metal interface layer on the surface of thermosetting resin particles in a chemical plating, electroplating or spraying mode, wherein the thickness of the metal interface layer is 20 nm-1 mu m, and the mass ratio of the thermosetting resin particles to the metal interface layer is 1.5-188 to obtain modified thermosetting resin particles;
s2, uniformly mixing the low-melting-point alloy with the modified thermosetting resin particles, wherein the mass ratio of the low-melting-point alloy in the mixture is 3-50 wt%, placing the mixture in a model, and hot-pressing at a temperature higher than the melting point of the low-melting-point alloy and lower than the melting point of the modified thermosetting resin particles to obtain the electronic packaging material with the heat conduction electromagnetic shielding performance.
4. The method for producing an electronic packaging material having heat conductive electromagnetic shielding properties according to claim 3, wherein the thermosetting resin particles are produced by any one of precipitation polymerization, vapor-induced phase separation, mechanical disruption, emulsion polymerization, and solution polymerization.
5. The method for preparing an electronic packaging material with heat conduction electromagnetic shielding performance according to claim 3, wherein the time of hot press molding in the step S2 is 10 min-50 min, and the hot press pressure is 5 MPa-30 MPa.
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| CN103409094A (en) * | 2013-07-23 | 2013-11-27 | 合肥工业大学 | Composite glue made from micro-, nano-filler and epoxy resin, and preparation method and applications thereof |
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| CN113337231A (en) * | 2021-06-01 | 2021-09-03 | 中国科学院合肥物质科学研究院 | Epoxy composite material with heterostructure and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2017109878A1 (en) * | 2015-12-24 | 2017-06-29 | 三菱電機株式会社 | Electromagnetic shield structure of high frequency circuit, and high frequency module |
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|---|---|---|---|---|
| CN103409094A (en) * | 2013-07-23 | 2013-11-27 | 合肥工业大学 | Composite glue made from micro-, nano-filler and epoxy resin, and preparation method and applications thereof |
| WO2015190324A1 (en) * | 2014-06-10 | 2015-12-17 | 株式会社カネカ | Heat-conductive resin composition |
| CN111534016A (en) * | 2020-06-01 | 2020-08-14 | 中国科学院合肥物质科学研究院 | Electronic packaging material with heat conduction and electromagnetic shielding performance and preparation method thereof |
| CN113337231A (en) * | 2021-06-01 | 2021-09-03 | 中国科学院合肥物质科学研究院 | Epoxy composite material with heterostructure and preparation method thereof |
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| 金属复合织物的制备及其应用;杨晓凤;张葛成;钟菲菲;张瑞萍;;纺织科技进展(07);全文 * |
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