CN113061415B - In-situ self-heating packaging material and preparation method and application thereof - Google Patents
In-situ self-heating packaging material and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of packaging, and particularly relates to an in-situ self-heating packaging material and a preparation method and application thereof. The in-situ self-heating packaging material comprises the following components in percentage by mass: 0-5% of solvent, 4-90% of organic resin, 0-5% of activating agent, 0.2-2% of slow-release agent, 0.3-2% of thixotropic agent, 0.1-5% of surfactant, 0.1-5% of first metal magnetic nano particles and 0.1-90% of second metal powder, wherein the heat required by self-curing can be achieved under the action of an external magnetic field, and the oxide on the bonding pad is removed and the bonding pad and the melting bonding pad are cured, so that the phenomenon that a circuit board where components are connected is deformed or other connecting elements are damaged due to overheating is avoided, the deformation and warping of the circuit board of the components caused by the traditional electronic connection process is avoided, various defects such as false soldering, cavities and the like caused by incomplete connection are reduced, the product yield of the electronic connection process is improved, and the electronic connection process has good service performance.
Description
Technical Field
The invention belongs to the technical field of packaging, and particularly relates to an in-situ self-heating packaging material and a preparation method and application thereof.
Background
With the trend of slight microblog of electronic product products, the electronic connecting material applied to artificial intelligence, AI, Lot of the Internet of things and Micro-electrical systems (Mini-LED and Micro-LED) develops towards ultramicro size, low melting point temperature and various applications, such as dispensing, spray printing, low-temperature reflow, laser welding and other various process modes.
At present, the heat energy source of the traditional connection forming mode is mainly obtained through the heat conduction mode of the component and the circuit board, and the component and the circuit board can be solidified or melted only when the temperature of the component and the circuit board is higher than the temperature of solidification or melting of the connecting material, so that the purpose of connection is achieved. For example, chinese patent CN112375340A discloses a wafer-level package sealing circuit laminated film, a preparation method and an application thereof, wherein the laminated film comprises 40-60 parts by mass of a first epoxy resin, 15-30 parts by mass of a second epoxy resin, 25-50 parts by mass of a curing agent, 0.1-5 parts by mass of a curing accelerator, 5-20 parts by mass of an auxiliary agent, 320-650 parts by mass of an inorganic filler, and 0.01-5 parts by mass of a silane coupling agent; the auxiliary agent is obtained by the reaction of epoxy resin and a dendritic cross-linking agent with polyhydroxy at the tail end. The laminated film obtained by the invention has good fluidity when being heated and cured, and can completely fill the gaps among the wafers to finish the packaging. In the process of the packaging material, the heat is transferred through the following routes: heating a reflow soldering or electric furnace heating element → heating airflow as a heat carrier → heating the circuit board and the component → connecting the packaging material to obtain the required heat energy → exciting the chemical energy of the soldering flux or the sizing material → removing the oxide on the surface of the packaging material and the surface of the bonding pad → melting and cooling the packaging material or curing the bonding pad → completing the connection. In practice, in such a heat transfer path, deformation and warpage of components and circuit board substrates are inevitable under the action of a thermal field in the process, and meanwhile, the time for realizing energy conversion from electricity to solidification heat energy of a connecting material or the time for realizing the reaction of melting heat energy and soldering flux is long, and the time for realizing the heat energy acquisition and the heat energy acquisition of the connecting part is large and short, so that the efficiency and the quality of the process of electronic connection are influenced.
Disclosure of Invention
The invention aims to provide an in-situ self-heating packaging material and a preparation method and application thereof, the in-situ self-heating packaging material can achieve the heat required by self-curing under the action of an external magnetic field, and oxide on a bonding pad is removed and cured to connect the bonding pad and melt the bonding pad, thereby avoiding the deformation or damage to other connecting elements caused by overheating of a circuit board on which a connecting element is positioned, avoiding the deformation and warpage of the circuit board of the element caused by the traditional electronic connection process, reducing various defects of insufficient soldering, cavities and the like caused by imperfect connection, improving the product yield of the electronic connection process, and having good service performance.
In order to achieve the purpose, the invention adopts the following technical scheme:
an in-situ self-heating packaging material comprises the following components in percentage by mass:
0-5% of solvent, 4-90% of organic resin, 0-5% of activating agent, 0.2-2% of slow-release agent, 0.3-2% of thixotropic agent, 0.1-5% of surfactant, 0.1-5% of first metal magnetic nano particles and 0.1-90% of second metal powder.
The invention starts from the composition of the electronic connecting material, introduces the first metal magnetic nano-particles, and realizes the action of an external electromagnetic field (electromagnetic heating) on the positions where welding spots are formed under the action of an external magnetic field or the action of external magnetism and physical pressure, so that the packaging material with the first metal magnetic nano-particles can be self-heated or the first metal magnetic nano-particles on the electrodes and the welding pads can be self-heated, the heat energy required by curing can be reached, the temperature of warping of a circuit board substrate can not be reached, the electronic connecting process can be further completed, and the high-quality electric conduction and heat conduction connection points can be obtained.
The transmission route of the heat required by the in-situ self-heating packaging material is as follows: electromagnetic conversion → magnetic field energy → first metal magnetic material heating → packaging material and pad heat energy needed for connection → chemical energy excitation of soldering flux → surface of packaging material and pad oxide is removed → packaging material is melted and cooled or the connection pad is solidified → connection is completed.
Further, the in-situ self-heating type packaging material comprises the following components in percentage by mass:
0-5% of solvent, 4-90% of organic resin, 0-5% of activating agent which is not zero, 0.2-2% of slow release agent, 0.3-2% of thixotropic agent, 0.1-5% of surfactant, 0.1-5% of first metal magnetic nano particles and 0.1-90% of second metal powder.
Further, the first metal magnetic nanoparticles comprise one or more of nickel nanoparticles, iron nanoparticles, cobalt nanoparticles, silver-coated nickel nanoparticles and silver-coated iron nanoparticles.
Further, the particle size of the first metal magnetic nano-particles is 10-800 nm.
Further, the second metal powder comprises one or more of tin-based alloy powder, silver-based metal powder and copper-based metal powder.
Further, the specification of the second metal powder comprises one or more of 45-75 μm, 25-45 μm, 20-38 μm, 15-25 μm, 5-15 μm, 2-11 μm, 2-8 μm, 1-5 μm, 1-3 μm and 50-1000 nm.
Further, the tin-based alloy powder comprises one or more of SnAgCu, SnBi, SnBiAg, SnBiAgCu, SnZn, SnBiCu, SnSb, SnGa, SnInGa and SnBiGa.
Further, the silver-based metal powder includes micro-nano silver powder.
Further, the copper-based metal powder comprises micro-nano copper powder and micro-nano silver-coated copper powder.
Further, the organic resin comprises one or more of modified rosin resin, epoxy resin, acrylic resin and organic silicon resin.
Further, the solvent is at least one of dioctyl adipate, diethylene glycol monohexyl ether, diethylene glycol butyl ether, isopropanol and benzyl alcohol.
Further, the activator is a first activator, or consists of a first activator and a second activator; the first activator comprises at least one of thiodisuccinic acid, phenylsuccinic acid and methylsuccinic acid; the second activator comprises at least one of diphenylguanidine, glutaric acid, adipic acid, succinic acid, sebacic acid, salicylic acid, and malic acid.
Further, the slow release agent comprises one or more of an antioxidant 168, an antioxidant 1010, an antioxidant 3030, hydroquinone and 1,2, 3-benzotriazole.
Further, the thixotropic agent includes a thixotropic agent 6500.
Further, the surfactant comprises one or more of DYNOL 607, Dynol 980, Defom 6800 and Letensol XL-90.
The second purpose of the invention is to provide the application of any one of the in-situ self-heating type packaging materials in electronic packaging.
The third purpose of the invention is to provide a preparation method of any in-situ self-heating packaging material, which comprises the following steps:
s1) sequentially putting a solvent, an organic resin, an activating agent, a slow release agent and a thixotropic agent into a reaction kettle at a temperature of 80-130 ℃, stirring for 60-150 min until solid particles are completely dissolved and are clear and transparent, then adding first metal magnetic nanoparticles, mechanically dispersing at high speed or/and ultrasonically dispersing into a suspension, cooling to room temperature, adding a surfactant, continuing mechanical high-speed dispersing or/and ultrasonically dispersing, transferring materials in the reaction kettle into a cooling container, and sealing to obtain an in-situ self-heating type packaging material carrier;
s2) adding the second metal powder into the in-situ self-heating packaging material carrier obtained in the step S1, stirring the mixture into a paste, and placing the paste in a refrigerated cabinet at the temperature of less than 4 ℃ for later use to obtain the packaging material.
Further, the linear speed of the mechanical high-speed dispersion is 40-100 m/s, and the dispersion time is 30-90 min.
Furthermore, the power of ultrasonic dispersion is 1-3 kw, the frequency is 20-40 KHz, and the ultrasonic dispersion time is 30-50 min.
The fourth purpose of the invention is to provide a using method of the in-situ self-heating packaging material prepared by the preparation method, which comprises the following steps: and after an electromagnetic field is applied to the in-situ self-heating packaging material, the in-situ self-heating packaging material reaches a curing point so as to form electronic connection between the component and the circuit board substrate.
The fifth purpose of the invention is to provide a using method of the in-situ self-heating packaging material, which comprises the following steps:
1) preparing an in-situ self-heating packaging material; sequentially putting a solvent, an organic resin, an activating agent, a slow release agent and a thixotropic agent into a reaction kettle at a temperature of 80-130 ℃, stirring for 60-150 min until solid particles are completely dissolved and are clear and transparent, cooling to room temperature, adding a surfactant, mechanically dispersing at high speed or/and ultrasonically dispersing, transferring materials in the reaction kettle into a cooling container, and sealing to obtain an in-situ self-heating packaging material carrier; adding the second metal powder into the in-situ self-heating packaging material carrier obtained in the step S1, stirring the mixture into a paste, and placing the paste in a refrigerated cabinet at the temperature of less than 4 ℃ for later use;
2) processing the first metal magnetic nanoparticles; covering the first metal magnetic nano particles on the component and the circuit board substrate by adopting a thermal spraying, electroplating, chemical plating or vapor deposition method;
3) curing; and placing the in-situ self-heating packaging material between the element and the circuit board substrate, and applying an electromagnetic field to the in-situ self-heating packaging material until the in-situ self-heating packaging material reaches a curing point so as to form electronic connection between the element and the circuit board substrate, wherein the element and the circuit board cannot be adsorbed by the first metal magnetic nanoparticles.
Furthermore, when the electromagnetic field is applied, 0.05-10 MPa of pressure can be applied to the element or/and the circuit board substrate.
Furthermore, the electromagnetic field is applied from the upper part of the circuit board connected with the element or/and from the lower part of the circuit board connected with the circuit board substrate.
Furthermore, the electromagnetic field is applied with the intensity of 5-60 KHz, the temperature is 5-10 ℃ above the melting point of the tin alloy, and the time is 0.5-20 min.
Furthermore, the temperature of the refrigerated cabinet is less than 4 ℃, can be more than or equal to 0 and less than or equal to 4, and can be more than-10 and less than or equal to 0.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the in-situ self-heating packaging material, the first metal magnetic nanoparticles enable the in-situ self-heating packaging material to be self-heated and welded under the action of an external magnetic field, the curing and welding are completed without being heated by a reflow soldering circuit, an electric heating plate or an oven, selective parts are heated for microelectronics, namely the packaging material and a bonding pad applied to a PCB are only heated, the deformation and warping of a circuit board of a component caused by the traditional electronic connection process are avoided, various defects such as insufficient soldering, holes and the like caused by incomplete connection are reduced, and the product yield of the electronic connection process is improved.
(2) The first metal magnetic nanoparticles in the in-situ self-heating packaging material are dispersed in the packaging material and uniformly distributed in the welding spots after solidification and welding, so that the electric and heat conduction and high reliability of the welding spots are enhanced.
(3) The invention adopts electromagnetic induction heating, has high heat conversion efficiency, saves energy, reduces consumption, is green and environment-friendly, and reduces the production cost.
Drawings
Fig. 1 is a schematic view of a method for using the in-situ self-heating type encapsulating material according to embodiment 1.
FIG. 2 is a schematic diagram illustrating a method for using the in-situ self-heating type packaging material in accordance with embodiment 2.
FIG. 3 is a schematic view of a method for using the in-situ self-heating type encapsulating material according to embodiment 7.
In the figure, 1, a packaging material; 2. applying pressure; 3. a circuit board substrate; 4. an element; 5. an electromagnetic wire; 6. a magnetic nickel pad.
Detailed Description
The present invention will be described in further detail with reference to the following examples. It should not be understood that the scope of the above-described subject matter of the present invention is limited to the following examples.
TABLE 1
The preparation method comprises the following steps:
s1) taking organic resin, an activating agent, a slow release agent and a thixotropic agent, sequentially putting the organic resin, the activating agent, the slow release agent and the thixotropic agent into a reaction kettle at 80 ℃, stirring for 60min until solid particles are completely dissolved and are clear and transparent, then adding first metal magnetic nanoparticles, mechanically dispersing at high speed (the linear speed of the mechanical high-speed dispersion is 100m/S, and the dispersion time is 60min), cooling to room temperature, adding a surfactant, continuing to mechanically disperse at high speed, transferring the materials in the reaction kettle into a cooling container, and sealing to obtain an in-situ self-heating type packaging material carrier;
s2) adding the second metal powder into the in-situ self-heating packaging material carrier obtained in the step S1, stirring the mixture into a paste, and placing the paste in a refrigerated cabinet at the temperature of 2 ℃ for later use.
The using method comprises the following steps: and after an electromagnetic field is applied to the in-situ self-heating packaging material, the in-situ self-heating packaging material reaches a curing point so as to form electronic connection between the component and the circuit board substrate.
Wherein, when the electromagnetic field is applied, 0.1MPa pressure is applied to the element; the application time of the electromagnetic field is 5 min; applied from the lower portion of the wiring board to which the wiring board substrate is attached, as shown in fig. 1.
TABLE 2
The preparation method comprises the following steps:
s1) taking a solvent, an organic resin, an activating agent, a slow release agent and a thixotropic agent, sequentially putting the solvent, the organic resin, the activating agent, the slow release agent and the thixotropic agent into a reaction kettle at 100 ℃, stirring for 90min until solid particles are completely dissolved and are clear and transparent, then adding first metal magnetic nanoparticles, dispersing mechanically at high speed (the linear speed of mechanical high-speed dispersion is 80m/S, the dispersion time is 30min) and ultrasonically (the power of ultrasonic dispersion is 1.5kw, the frequency is 30KHz, and the ultrasonic dispersion time is 30min) to form a suspension, cooling to room temperature, adding a surfactant, continuing mechanical high-speed dispersion and ultrasonic dispersion, transferring materials in the reaction kettle into a cooling container, and sealing to obtain an in-situ self-heating type packaging material carrier;
s2) adding the second metal powder into the in-situ self-heating packaging material carrier obtained in the step S1, stirring the mixture into a paste, and placing the paste in a refrigerated cabinet at 1 ℃ for later use.
The using method comprises the following steps: and after an electromagnetic field is applied to the in-situ self-heating packaging material, the in-situ self-heating packaging material reaches a curing point so as to form electronic connection between the component and the circuit board substrate.
Wherein, when the electromagnetic field is applied, 0.1MPa pressure is applied to the circuit board substrate; the application time of the electromagnetic field is 5 min; applied from the lower portion of the wiring board to which the wiring board substrate is attached, as shown in fig. 2.
TABLE 3
The preparation method comprises the following steps:
s1) taking a solvent, an organic resin, an activating agent, a slow release agent and a thixotropic agent, sequentially putting the solvent, the organic resin, the activating agent, the slow release agent and the thixotropic agent into a reaction kettle at 110 ℃, stirring for 90min until solid particles are completely dissolved and are clear and transparent, then adding first metal magnetic nanoparticles, ultrasonically dispersing (the power of ultrasonic dispersion is 2kw, the frequency is 25KHz, and the ultrasonic dispersion time is 30min) to form a suspension, cooling to room temperature, adding a surfactant, continuing to ultrasonically disperse, transferring the materials in the reaction kettle into a cooling container, and sealing to obtain an in-situ self-heating type packaging material carrier;
s2) adding the second metal powder into the in-situ self-heating packaging material carrier obtained in the step S1, stirring the mixture into a paste, and placing the paste in a refrigerated cabinet at 3 ℃ for later use.
The using method comprises the following steps: and after an electromagnetic field is applied to the in-situ self-heating packaging material, the in-situ self-heating packaging material reaches a curing point so as to form electronic connection between the component and the circuit board substrate.
Wherein, when the electromagnetic field is applied, 0.15MPa pressure is applied to the element and the circuit board substrate; applied from the lower part of the circuit board to which the circuit board substrate is connected.
TABLE 4
The preparation method comprises the following steps:
s1) taking a solvent, an organic resin, an activating agent, a slow release agent and a thixotropic agent, sequentially putting the solvent, the organic resin, the activating agent, the slow release agent and the thixotropic agent into a reaction kettle at 100 ℃, stirring for 120min until solid particles are completely dissolved and are clear and transparent, then adding first metal magnetic nanoparticles, ultrasonically dispersing (the power of ultrasonic dispersion is 2kw, the frequency is 25KHz, and the ultrasonic dispersion time is 90min) to form a suspension, cooling to room temperature, adding a surfactant, continuing to ultrasonically disperse, transferring the materials in the reaction kettle into a cooling container, and sealing to obtain an in-situ self-heating type packaging material carrier;
s2) adding the second metal powder into the in-situ self-heating packaging material carrier obtained in the step S1, stirring the mixture into a paste, and placing the paste in a refrigerated cabinet at 3 ℃ for later use.
The using method comprises the following steps: and after an electromagnetic field is applied to the in-situ self-heating packaging material, the in-situ self-heating packaging material reaches a curing point so as to form electronic connection between the component and the circuit board substrate.
The electromagnetic field is applied from the upper part of the circuit board connected with the element and from the lower part of the circuit board connected with the circuit board substrate.
TABLE 5
The preparation method is the same as that of example 1.
The procedure was as in example 1.
TABLE 6
The preparation method is the same as that of example 1.
The procedure was as in example 1.
Embodiment 7 an in-situ self-heating type packaging material
TABLE 7
The using method comprises the following steps:
1) preparing an in-situ self-heating packaging material; sequentially putting a solvent, an organic resin, an activating agent, a slow release agent and a thixotropic agent into a 120 ℃ reaction kettle, stirring for 150min until solid particles are completely dissolved and are clear and transparent, cooling to room temperature, adding a surfactant, and performing mechanical high-speed dispersion (the linear speed of the mechanical high-speed dispersion is 40m/s, the dispersion time is 30min) and ultrasonic dispersion (the power of the ultrasonic dispersion is 2kw, the frequency is 25KHz, and the ultrasonic dispersion time is 30min), transferring the materials in the reaction kettle into a cooling container, and sealing to obtain an in-situ self-heating packaging material carrier; adding the second metal powder into the in-situ self-heating packaging material carrier obtained in the step S1, stirring the mixture into a paste, and placing the paste in a refrigerated cabinet at the temperature of 2 ℃ for later use;
2) processing the first metal magnetic nanoparticles; covering the first metal magnetic nano particles on the component and the circuit board substrate by adopting an electroplating method;
3) curing; and after the electromagnetic field is applied, the in-situ self-heating packaging material reaches a curing point so as to form electronic connection between the component and the circuit board substrate.
Wherein, when the electromagnetic field is applied, 0.1MPa pressure is applied to the element and the circuit board substrate; the electromagnetic field is applied from the lower portion of the wiring board connected to the wiring board substrate, as shown in fig. 3.
Embodiment 8 an in-situ self-heating type packaging material
TABLE 8
The using method comprises the following steps:
1) preparing an in-situ self-heating packaging material; sequentially putting a solvent, an organic resin, an activating agent, a slow release agent and a thixotropic agent into a 120 ℃ reaction kettle, stirring for 60min until solid particles are completely dissolved and are clear and transparent, cooling to room temperature, adding a surfactant, and performing mechanical high-speed dispersion (the linear speed of the mechanical high-speed dispersion is 40m/s, the dispersion time is 30min) and ultrasonic dispersion (the power of the ultrasonic dispersion is 2kw, the frequency is 25KHz, and the ultrasonic dispersion time is 30min), transferring the materials in the reaction kettle into a cooling container, and sealing to obtain an in-situ self-heating packaging material carrier; adding the second metal powder into the in-situ self-heating packaging material carrier obtained in the step S1, stirring the mixture into a paste, and placing the paste in a refrigerated cabinet at the temperature of-1 ℃ for later use;
2) processing the first metal magnetic nanoparticles; covering the first metal magnetic nano particles on the component and the circuit board substrate by adopting a thermal spraying method;
3) curing; and after the electromagnetic field is applied, the in-situ self-heating packaging material reaches a curing point so as to form electronic connection between the component and the circuit board substrate.
Wherein, when the electromagnetic field is applied, 0.15MPa pressure is applied to the element and the circuit board substrate; the electromagnetic field is applied from the upper part of the wiring board to which the element is connected and from the lower part of the wiring board to which the substrate of the wiring board is connected.
Example 9 in-situ self-heating type Package Material
The formulation is the same as in example 1.
The using method comprises the following steps:
1) preparing an in-situ self-heating packaging material; sequentially putting a solvent, an organic resin, an activating agent, a slow release agent and a thixotropic agent into a reaction kettle at a temperature of 80 ℃, stirring for 60min until solid particles are completely dissolved and are clear and transparent, cooling to room temperature, adding a surfactant, mechanically dispersing at a high speed (the linear speed of the mechanical high-speed dispersion is 100m/s, the dispersion time is 60min), transferring the materials in the reaction kettle into a cooling container, and sealing to obtain an in-situ self-heating packaging material carrier; adding the second metal powder into the in-situ self-heating packaging material carrier obtained in the step S1, stirring the mixture into a paste, and placing the paste in a refrigerated cabinet at the temperature of 2 ℃ for later use;
2) processing the first metal magnetic nanoparticles; covering the first metal magnetic nano particles on the component and the circuit board substrate by adopting a thermal spraying method;
3) curing; and after the electromagnetic field is applied, the in-situ self-heating packaging material reaches a curing point so as to form electronic connection between the component and the circuit board substrate.
Wherein, when the electromagnetic field is applied, 0.1MPa pressure is applied to the element; the application time of the electromagnetic field is 5 min; applied from the lower part of the circuit board to which the circuit board substrate is connected.
Comparative example 1 in-situ self-heating packaging material
Similar to example 1, except that the first metal magnetic nanoparticles were not added. In the case of the method of use, curing and welding were not completed in a manner similar to that of example 1, and curing and welding were carried out by conventional heat radiation.
Comparative example 2, in-situ self-heating packaging material
Similar to example 7, except that the first metal magnetic nanoparticles were not added. In the case of the method of use, curing and welding were not completed in a manner similar to that of example 1, and curing and welding were carried out by conventional heat radiation.
Comparative example 3 in-situ self-heating packaging material
Similar to example 1, except that the first activator was not added.
Comparative example 4, in-situ self-heating packaging material
The formulation is the same as in example 1.
The preparation method comprises the following steps:
s1) taking a solvent, an organic resin, an activating agent, a slow release agent and a thixotropic agent, sequentially putting the solvent, the organic resin, the activating agent, the slow release agent and the thixotropic agent into a 80 ℃ reaction kettle, stirring for 60min until solid particles are completely dissolved and are clear and transparent, then adding a first metal magnetic nano particle and second metal powder, mechanically dispersing at a high speed (the linear speed of the mechanical high-speed dispersion is 100m/S, and the dispersion time is 60min), cooling to room temperature, adding a surfactant, continuing to mechanically disperse at a high speed, transferring the materials in the reaction kettle into a cooling container, sealing, and putting the cooling container into a 2 ℃ refrigerated cabinet for later use to obtain the magnetic nano-material.
The procedure was as in example 1.
This comparative example differs from example 1 in the order of addition of the second metal powder.
Comparative example 5 in-situ self-heating packaging material
SAC305T5 solder paste, a conventional solder paste product of packaging materials of Japan, is commercially available. In the case of the method of use, curing and welding were not completed in a manner similar to that of example 1, and curing and welding were carried out by conventional heat radiation.
Comparative example 6 in-situ self-heating packaging material
The low-temperature conventional solder paste product SnBi58T5 solder paste is sold by certain packaging material company in the United states. In the case of the method of use, curing and welding were not completed in a manner similar to that of example 1, and curing and welding were carried out by conventional heat radiation.
Comparative example 7 in-situ self-heating packaging material
I know the high temperature conventional tin glue product SnSb10T7 tin glue. In the case of the method of use, curing and welding could not be performed in a similar manner to example 1, and thus curing and welding were performed by conventional heat radiation.
Experiment I, Performance test
The shear strength and the thermal conductivity of the welding spot are respectively tested by a push-pull force tester and an ASTM D5470 thermal resistance tester.
TABLE 9
As can be seen from table 9, in examples 1 to 9, curing can be completed, the circuit board substrate is not warped, the solder joint shear strength is high, and the thermal conductivity is high.
Comparative example 1 compared to example 1, comparative example 1 compared to example 7, the heat required for curing and welding the encapsulating material cannot be generated under the action of the electromagnetic field without adding the first metal magnetic nanoparticles, the curing and welding must be completed by conventional heat radiation, the temperature and time required for curing and welding are higher than those of the in-situ self-heating type encapsulating material, and the warpage phenomenon occurs.
Compared with example 1, comparative example 3 does not add the first activator, and although the curing temperature and the curing time are not affected, and the warping condition of the circuit board substrate is not affected, the solder joint shear strength and the thermal conductivity coefficient are reduced, which shows that the first activator can affect the performance of the packaging material, and is supposed to be beneficial to improving the diffusion of the first metal magnetic nanoparticles or the second metal powder; comparative example 4 the solder joint shear strength and thermal conductivity were also reduced depending on the order of addition of the second metal powder, and it was presumed that there was a possibility of association with the diffusion of the second metal powder, and the mechanism was further investigated.
Comparative examples 5-7 are conventional commercial products SAC305T5 tin paste, SnBi58T5 tin paste and I SnSb10T7 conventional tin paste in sequence, the overall performance of the conductive adhesive is not good, particularly the conductive adhesive needs higher curing temperature, and the shear strength and the heat conductivity of a welding spot are lower than those of an in-situ self-heating type packaging material containing magnetic nanoparticles.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (6)
1. The in-situ self-heating packaging material is characterized by comprising the following components in percentage by mass:
0-5% of solvent, 4-90% of organic resin, 0-5% of activating agent which is not zero, 0.2-2% of corrosion inhibitor, 0.3-2% of thixotropic agent, 0.1-5% of surfactant, 0.1-5% of first metal magnetic particles and 0.1-90% of second metal powder;
the organic resin comprises one or more of modified rosin resin, epoxy resin, acrylic resin and organic silicon resin;
the activator consists of a first activator and a second activator; the first activator comprises at least one of thiodisuccinic acid, phenylsuccinic acid and methylsuccinic acid; the second activator comprises at least one of diphenylguanidine, glutaric acid, adipic acid, succinic acid, sebacic acid, salicylic acid, and malic acid;
the first metal magnetic particles comprise one or more of nickel particles, iron particles, cobalt particles, silver-coated nickel particles and silver-coated iron particles;
the particle size of the first metal magnetic particles is 10-800 nm;
the second metal powder comprises one or more of tin-based alloy powder, silver-based metal powder and copper-based metal powder.
2. An in-situ self-heating type packaging material as recited in claim 1, wherein the specification of the second metal powder comprises one or more of 45-75 μm, 25-45 μm, 20-38 μm, 15-25 μm, 5-15 μm, 2-11 μm, 1-5 μm and 50-1000 nm.
3. The use of the in-situ self-heating type packaging material according to any one of claims 1-2 in electronic packaging.
4. The method for preparing an in-situ self-heating type packaging material according to any one of claims 1-2, comprising the following steps:
s1) sequentially putting a solvent, an organic resin, an activating agent, a corrosion inhibitor and a thixotropic agent into a reaction kettle at a temperature of 80-130 ℃, stirring for 60-150 min until solid particles are completely dissolved and are clear and transparent, then adding first metal magnetic particles, mechanically dispersing at a high speed and/or ultrasonically dispersing into a suspension, cooling to room temperature, adding a surfactant, continuing mechanical high-speed dispersing and/or ultrasonically dispersing, transferring materials in the reaction kettle into a cooling container, and sealing to obtain an in-situ self-heating packaging material carrier;
s2) adding the second metal powder into the in-situ self-heating packaging material carrier obtained in the step S1, stirring the mixture into a paste, and placing the paste in a refrigerated cabinet at the temperature of less than 4 ℃ for later use to obtain the packaging material.
5. The use method of the in-situ self-heating type packaging material prepared by the preparation method according to claim 4 is characterized by comprising the following steps: and after an electromagnetic field is applied to the in-situ self-heating packaging material, the in-situ self-heating packaging material reaches a curing point so as to form electronic connection between the component and the circuit board substrate.
6. The use method of the in-situ self-heating packaging material is characterized by comprising the following steps of:
1) preparing an in-situ self-heating packaging material; the weight percentage of the material is as follows: sequentially putting 0-5% of solvent, 4-90% of organic resin, 0-5% of activating agent which is not zero, 0.2-2% of corrosion inhibitor and 0.3-2% of thixotropic agent into a reaction kettle at 80-130 ℃, stirring for 60-150 min until solid particles are completely dissolved and are clear and transparent, cooling to room temperature, adding 0.1-5% of surfactant, mechanically dispersing at high speed and/or ultrasonically dispersing, transferring the materials in the reaction kettle into a cooling container, and sealing to obtain an in-situ self-heating packaging material carrier; adding 0.1-90% of second metal powder into the in-situ self-heating packaging material carrier obtained in the step S1, stirring the mixture into a paste, and then placing the paste in a refrigerated cabinet at the temperature of less than 4 ℃ for later use;
the organic resin comprises one or more of modified rosin resin, epoxy resin, acrylic resin and organic silicon resin;
the activator consists of a first activator and a second activator; the first activator comprises at least one of thiodisuccinic acid, phenylsuccinic acid and methylsuccinic acid; the second activator comprises at least one of diphenylguanidine, glutaric acid, adipic acid, succinic acid, sebacic acid, salicylic acid, and malic acid;
the second metal powder comprises one or more of tin-based alloy powder, silver-based metal powder and copper-based metal powder;
2) processing the first metal magnetic particles; covering 0.1-5% of the first metal magnetic particles on the element and the circuit board substrate by adopting a thermal spraying, electroplating, chemical plating or vapor deposition method;
the first metal magnetic particles comprise one or more of nickel particles, iron particles, cobalt particles, silver-coated nickel particles and silver-coated iron particles;
the particle size of the first metal magnetic particles is 10-800 nm;
3) curing; and after the electromagnetic field is applied, the in-situ self-heating packaging material reaches a curing point so as to form electronic connection between the component and the circuit board substrate.
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