CN113385857A - Multi-size micro-nano metal particle soldering paste in-situ interconnection process and product thereof - Google Patents
Multi-size micro-nano metal particle soldering paste in-situ interconnection process and product thereof Download PDFInfo
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- CN113385857A CN113385857A CN202110661846.XA CN202110661846A CN113385857A CN 113385857 A CN113385857 A CN 113385857A CN 202110661846 A CN202110661846 A CN 202110661846A CN 113385857 A CN113385857 A CN 113385857A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
- B23K35/0244—Powders, particles or spheres; Preforms made therefrom
- B23K35/025—Pastes, creams, slurries
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/302—Cu as the principal constituent
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Abstract
The invention discloses a multi-size micro-nano metal particle soldering paste in-situ interconnection process and a product thereof, and the multi-size micro-nano metal particle soldering paste in-situ interconnection process comprises the following steps: (a) dissolving a copper salt in a solvent, adding a reducing agent and micron metal particles in the solvent, and stirring for reaction to obtain a multi-size micro-nano metal particle dispersion liquid; (b) concentrating the multi-size micro-nano metal particle dispersion liquid prepared in the step (a). The in-situ interconnection process of the multi-size micro-nano metal particle soldering paste realizes more convenient, rapid and efficient preparation of the metal soldering paste, has simple process and convenient storage and application, and the oxidation degree of nano copper particles in the soldering paste is low, so that the density of a sintered body can be effectively improved, and the shearing strength and the electric conductivity can be enhanced.
Description
Technical Field
The invention relates to the technical field of electronic manufacturing, in particular to an in-situ interconnection process of multi-size micro-nano metal particle soldering paste and a product thereof.
Background
Electronic technology has rapidly developed, and the goal of electronic component packaging and interconnection is to achieve stable electrical interconnection, thermal connection, and mechanical connection of sufficient strength. The stable encapsulation and interconnection ensures that the electronic components work better. The development of high-temperature devices of silicon carbide and gallium nitride enables power electronic modules to be used at high temperatures, and the use requirements of high-power devices cannot be met by soldering paste and conductive adhesive as traditional interconnection materials. The above problems put higher demands on the packaging and interconnection: (1) the mechanical connection is ensured to be reliable; (2) high conductivity is ensured to realize high-speed transmission between the substrate and the chip; (3) the high heat conductivity is ensured to realize the heat dissipation of the chip, and the burning of the chip caused by overhigh temperature is avoided; (4) and the low-temperature interconnection avoids the phenomenon that the thermal expansion degrees of the substrate, the chip and the interconnection material are different to form larger thermal stress due to overlarge temperature change. Nanometer metal materials with special physicochemical properties become a research hotspot of the current packaging interconnection materials. The copper is used as a good heat dissipation material and has good conductivity, and the micro-nano copper metal paste is a research hotspot with the advantages of low cost, easily available materials, low electric mobility and the like.
The existing preparation methods of micro-nano copper paste are generally a liquid phase reduction method, an electrolytic method, a mechanical grinding method and an explosion method. The most widely applied method is to prepare the micro-nano copper soldering paste by a liquid phase reduction method. The preparation method of the liquid-phase micro-nano copper paste generally comprises the following steps: (1) mixing a precursor copper source, a reducing agent, a dispersing agent or a protective agent and the like in a liquid phase to obtain a micro-nano copper particle liquid phase; (2) separating liquid phase and micro-nano copper particles; (3) and preparing micro-nano copper paste. However, the micro-nano copper has the defect of easy oxidation, and in the process of preparing the micro-nano copper paste by liquid phase reduction, the step (2) comprises the steps of washing and separating micro-nano copper particles for many times, so that the nano copper particles are exposed to the air for many times, and the oxidation of the micro-nano copper is aggravated. Although the nano-copper particles can already diffuse at a lower temperature, a Cu-Cu metal bond is formed. But this temperature is still too high relative to the conventional solder paste interconnect temperature. In the interconnection process, due to different thermal expansion coefficients of the substrate, the chip and the interconnection material, too high interconnection temperature can cause the three to generate larger expansion in different degrees, and larger stress is formed after cooling. Multiple thermal cycles can cause fatigue cracking during chip operation, causing interconnect failure.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide an in-situ interconnection process of a multi-size micro-nano metal particle soldering paste, which realizes more convenient, rapid and efficient preparation of the metal soldering paste, has simple process and convenient storage and application and solves the problems of complex preparation process, high paste sintering temperature and easy oxidation of nano copper particles of the existing soldering paste.
The invention also aims to provide the multi-size micro-nano metal particle soldering paste prepared by the multi-size micro-nano metal particle soldering paste in-situ interconnection process, which has the advantages that the oxidation degree of nano copper particles in the soldering paste is low, the density of a sintered body can be effectively improved, the shear strength and the electric conductivity are enhanced, and the problems that the nano copper particles in the existing soldering paste are easy to oxidize and hinder sintering are solved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a multi-size micro-nano metal particle solder paste in-situ interconnection process comprises the following steps:
(a) dissolving a copper salt in a solvent, adding a reducing agent and micron metal particles in the solvent, and stirring for reaction to obtain a multi-size micro-nano metal particle dispersion liquid;
(b) concentrating the multi-size micro-nano metal particle dispersion liquid prepared in the step (a) to prepare multi-size micro-nano metal particle soldering paste;
(c) and (c) coating the multi-size micro-nano metal particle soldering paste prepared in the step (b) on a substrate, and then sintering.
More specifically, in the step (a), the size of the micron metal particles is 0.1 to 100 μm.
In the step (a), the size of the nano-copper particles generated by the stirring reaction is 50-800 nm.
More specifically, in the step (a), the molar ratio of the copper salt to the reducing agent is 1: 1-1: 10, the molar ratio of the copper salt to the micron metal particles is 1000: 1-1: 10.
further, in the step (a), the copper salt is any one of copper acetate, copper hydroxide, copper formate, copper acetylacetonate or copper oxalate, the micro metal is one or more of copper particles, silver particles, gold particles, tin particles and aluminum particles, the solvent is one or more of water, toluene, butylbenzene, diethyl ether, ethyl acetate, ethanol, ethylene glycol, diethylene glycol, dipropylene glycol, glycerol, acetone, glycerol and terpineol, and the reducing agent is any one of hydrazine hydrate, phenylhydrazine, ascorbic acid and glucose.
Further, in the step (a), the reaction temperature of the stirring reaction is 20 to 80 ℃, and the reaction time is 10 to 180 min.
Further, in the step (b), the concentration is performed by using one or more of a rotary evaporator, a vacuum drying oven, a centrifuge, a filter device, and natural sedimentation.
Further, the mass percentage of the micro-nano metal in the multi-size micro-nano metal particle soldering paste is 30-99%.
In the step (c), the sintering temperature is 20 to 600 ℃, and the sintering pressure is 0 to 20 MPa.
A multi-size micro-nano metal particle soldering paste is prepared by using the multi-size micro-nano metal particle soldering paste in-situ interconnection process.
Compared with the prior art, the embodiment of the invention has the following beneficial effects:
the invention provides an in-situ interconnection process of a multi-size micro-nano metal particle soldering paste, which effectively realizes in-situ preparation of the micro-nano metal soldering paste by adding micro-nano metal particles in advance, the multi-size micro-nano metal dispersion is concentrated to obtain the multi-size micro-nano metal soldering paste, the multi-size micro-nano metal soldering paste is directly coated on a substrate and then sintered to realize in-situ interconnection, the in-situ preparation of the multi-size micro-nano metal soldering paste is realized by adopting the method of adding the micro-nano metal in advance, the operations of centrifuging, washing, drying and the like of the micro-nano metal are not needed, the preparation flow of the metal soldering paste is greatly simplified, the micro-nano metal particles are prevented from further contacting with air, the agglomeration and oxidation of nano materials are avoided, the accurate mixing proportion of the nano particles and the micro particles can be obtained, and the micro-nano metal is tightly stacked, the density of the paste sintered body is improved, the yield of the soldering paste is improved on the basis of not reducing the connection performance, the problem of high sintering temperature of the paste is effectively solved, the metal soldering paste is more conveniently, quickly and efficiently prepared, the storage and the application are convenient, the defects and the defects of the existing preparation method are overcome, such as the problems of complex process and easy oxidation of nano copper particles, the method has the advantages of simple process and low production cost, and is suitable for the fields of low-temperature interconnection and three-dimensional packaging electronic manufacturing;
and then providing the multi-size micro-nano metal particle soldering paste prepared by the multi-size micro-nano metal particle soldering paste in-situ interconnection process, mixing by adopting an in-situ method, obtaining nano copper particles by adopting copper salt reaction and mixing, fully contacting the surfaces of the generated nano copper particles with a solvent, adding the micron metal particles at the moment, fully contacting the surfaces of the micron metal particles with a solvent in a reaction process, and forming a more uniform and compact mixture and better combination with the solvent in the reaction process, thereby being beneficial to forming a compact three-dimensional stacking structure. The large-sized particles in the solder paste serve as a framework for interconnection and provide high shear strength, high electrical conductivity and high thermal conductivity, and the small-sized particles serve as a binder to connect the large-sized particles to form complete and compact interconnection. The oxidation degree of the nano-copper particles in the prepared multi-size micro-nano metal particle soldering paste is low, the density of a sintered body can be effectively improved, and the shear strength and the electric conductivity are enhanced.
Drawings
Fig. 1 is a schematic illustration of a micro-metallic particle and nano-metallic particle adsorption stack.
Detailed Description
A multi-size micro-nano metal particle solder paste in-situ interconnection process comprises the following steps:
(a) dissolving a copper salt in a solvent, adding a reducing agent and micron metal particles in the solvent, and stirring for reaction to obtain a multi-size micro-nano metal particle dispersion liquid;
(b) concentrating the multi-size micro-nano metal particle dispersion liquid prepared in the step (a) to prepare multi-size micro-nano metal particle soldering paste;
(c) and (c) coating the multi-size micro-nano metal particle soldering paste prepared in the step (b) on a substrate, and then sintering.
The invention dissolves the copper salt in the solvent, adds the reducing agent and the micron metal particles in the solution, and then stirs the solution to react, so that the nano copper particles generated by the reaction are attached to the surface of the micron metal particles, thereby avoiding the oxidation and agglomeration of the nano copper particles (if the nano copper particles are oxidized or agglomerated, the oxide of copper has a melting point higher than that of copper, the oxidation of nano copper can cause the sintering inhibition, so that the oxide and the copper are not sintered together, further reducing the shearing strength and the conductivity, furthermore, the sintering is based on the size principle, the smaller the size, the smaller the required sintering energy, the smaller the nano particles, the larger the surface energy, once the nano particles are agglomerated, the surface energy of the particles is reduced, the sintering inhibition is performed, the multi-size micro-nano metal particle dispersion liquid obtained in the step (a) is obtained after the reaction, and the multi-size micro-nano metal particle dispersion liquid obtained in the step (a) is concentrated, the multi-size micro-nano metal particle soldering paste is prepared after concentration, the multi-size micro-nano metal particle soldering paste is coated on a substrate and then sintered, the characteristics of low melting point and easiness in sintering of nano copper particles are utilized, the characteristics of high strength and high conductivity of micro metal are utilized, the micro metal particles and the nano metal particles form three-dimensional tight stacking in different particle sizes (the three-dimensional tight stacking means that after the large-size particles are tightly stacked, gaps are formed in close contact of spheres, the small-size particles can fill the gaps to form the three-dimensional tight stacking), the micro metal and the nano metal are mixed in situ, the micro metal and the nano metal form tight stacking, the density of a paste sintered body is improved, the shearing strength and the conductivity are enhanced, in addition, the energy generated when the small-size metal spheres are melted can melt the large-size metal spheres, and the melting of the large-size metal particles at a lower temperature is realized, the interconnection between the metals is formed, and the problem of high sintering temperature of the paste is effectively solved.
Further, the multi-size micro-nano metal particles described in the present invention specifically refer to metal particles with various sizes, for example, the prepared solder paste contains 50nm metal particles, 500nm metal particles and 1000nm metal particles.
The invention effectively realizes the in-situ preparation of the micro-nano metal soldering paste by adding the micro-nano metal particles in advance, the multi-size micro-nano metal soldering paste is obtained by concentrating the multi-size micro-nano metal dispersion liquid, the multi-size micro-nano metal soldering paste is directly coated on the substrate and then sintered to realize in-situ interconnection, the in-situ preparation of the multi-size micro-nano metal soldering paste is realized by adopting the method of adding the micro-nano metal in advance, the operations of centrifuging, washing, drying and the like of the micro-nano metal are not needed, the preparation flow of the metal soldering paste is greatly simplified, the micro-nano metal particles are prevented from further contacting with air, the agglomeration and oxidation of nano materials are avoided, the accurate mixing ratio of the micro-nano particles and the micro particles can be obtained, the micro-nano metal is formed into tight stacks, the density of a paste body is improved, and the yield of the soldering paste is improved on the basis of not reducing the connection performance, the method effectively solves the problem of high paste sintering temperature, realizes more convenient, rapid and efficient preparation of the metal soldering paste, is convenient to store and apply, overcomes the defects and shortcomings of the existing preparation method, such as complex process and easy oxidation of nano-copper particles, has the advantages of simple process and low production cost, and is suitable for the fields of low-temperature interconnection and three-dimensional packaging electronic manufacturing.
More specifically, in the step (a), the size of the micron metal particles is 0.1 to 100 μm.
In the step (a), the size of the micro-metal particles is in this range, and if the size of the micro-metal particles is too small, the high-strength and high-conductivity properties of the micro-metal particles are easily affected, so that the micro-metal particles may be easily oxidized, and if the size of the micro-metal particles is too large, low-temperature and low-pressure sintering is difficult to achieve.
In the step (a), the size of the nano-copper particles generated by the stirring reaction is 50-800 nm.
According to the invention, the copper salt is dissolved in the solvent, the reducing agent and the micron metal particles are added into the solution, and then the solution is stirred to react, so that the nano copper particles generated by the reaction are attached to the surfaces of the micron metal particles, the oxidation and agglomeration of the nano copper particles are avoided, the size of the nano copper particles generated by the stirring reaction is 50-800 nm, the small-size nano copper particles can provide better sintering power but are easy to oxidize, the large-size nano copper particles are not easy to oxidize, but the provided sintering power is not as good as that of the small-size nano copper particles.
Preferably, in the step (a), the molar ratio of the copper salt to the reducing agent is 1: 1-1: 10, the molar ratio of the copper salt to the micron metal particles is 1000: 1-1: 10.
if the molar ratio of the copper salt to the reducing agent is too high or too low, the molar ratio of the copper salt to the micro-metal particles is too high or too low, which will result in that the micro-metal particles and the nano-metal particles cannot form the most compact three-dimensional packing, thus affecting the compactness of the paste sintered body and reducing the shear strength and the electrical conductivity.
Preferably, in the step (a), the copper salt is any one of copper acetate, copper hydroxide, copper formate, copper acetylacetonate or copper oxalate, the micro metal is one or more of copper particles, silver particles, gold particles, tin particles and aluminum particles, the solvent is one or more of water, toluene, butylbenzene, diethyl ether, ethyl acetate, ethanol, ethylene glycol, diethylene glycol, dipropylene glycol, glycerol, acetone, glycerol and terpineol, and the reducing agent is any one of hydrazine hydrate, phenylhydrazine, ascorbic acid and glucose.
The copper salt is dissolved in the solvent, the reducing agent and the micron metal particles are added into the solution, and then the solution is stirred to react, so that the nano copper particles generated by the reaction are attached to the surfaces of the micron metal particles, the oxidation and agglomeration of the nano copper particles are avoided, and the in-situ preparation of the multi-size micro-nano metal soldering paste is realized by adopting a method of adding the micro-nano metal in advance. The solvent adopted by the invention is volatile or has low decomposition temperature, and is easy to remove in the low-temperature sintering process, so that the in-situ sintering of the micro-nano metal is realized.
Preferably, in the step (a), the reaction temperature of the stirring reaction is 20-80 ℃, and the reaction time is 10-180 min.
In the step (a), the reaction temperature of the stirring reaction is 20-80 ℃, the nano-copper particles prepared at different temperatures have different sizes and appearances, the nano-copper particles prepared at high temperature or low temperature have different sizes, and if the reaction temperature is too high or too low, the reaction of reducing copper salt is easily influenced, so that the micron metal particles and the nano-metal particles cannot form the most compact three-dimensional stacking, the density of a paste sintered body is influenced, and the shear strength and the electric conductivity are reduced.
Preferably, in the step (b), the concentration is performed by using one or more of a rotary evaporator, a vacuum drying oven, a centrifuge, a filter device and natural sedimentation.
Concentrating the multi-size micro-nano metal particle dispersion liquid obtained in the step (a), and preparing the multi-size micro-nano metal particle soldering paste after concentrating, wherein the concentrating effect is good, and the using effect of the multi-size micro-nano metal particle soldering paste is ensured.
Further, additives such as a thickening agent, a sintering aid, a film forming agent and a thixotropic agent can be added into the multi-size micro-nano metal particle dispersion liquid prepared in the step (a), or the additives are added into the multi-size micro-nano metal particle soldering paste prepared after the concentration in the step (b) and are uniformly stirred, so that the performance of the finally prepared multi-size micro-nano metal particle soldering paste is improved.
Preferably, the mass percentage of the micro-nano metal in the multi-size micro-nano metal particle soldering paste is 30-99%.
The micro-nano metal in the multi-size micro-nano metal particle soldering paste refers to all metal particles of the multi-size micro-nano metal particle soldering paste after a solvent is removed, namely all metal particles in the multi-size micro-nano metal particle soldering paste.
Preferably, in the step (c), the sintering temperature for sintering is 20-600 ℃, and the sintering pressure is 0-20 MPa.
If the sintering temperature in the step (c) is too low, the solder paste may be poorly sintered or may not be sintered, and a sintered body may not be formed, and if the sintering temperature is too high, the component may be damaged, and interconnection failure due to the difference of thermal expansion coefficients of the solder paste and the component may also be caused;
the sintering pressure provides sintering energy for the soldering paste, the pressurization can enable the sintering to be better carried out, poor sintering and poor sintering effects can be caused if the sintering pressure is too low, components can be damaged by too high sintering pressure if the sintering pressure is too high, and when the sintering pressure is 0MPa, the pressurization is not needed.
Specifically, in the step (c), the multi-size micro-nano metal particle solder paste prepared in the step (b) is coated on a substrate by adopting a screen printing, coating or spraying mode, wherein the substrate is any substrate such as a copper substrate, a semiconductor substrate, an organic/inorganic thin film flexible substrate, a porous substrate, a ceramic substrate or an aluminum substrate, but is not limited to the above substrate.
A multi-size micro-nano metal particle soldering paste is prepared by using the multi-size micro-nano metal particle soldering paste in-situ interconnection process.
The method adopts an in-situ method for mixing, and because the nano copper particles are obtained by adopting copper salt reaction mixing, the surfaces of the generated nano copper particles are fully contacted with a solvent, the micron metal particles are added at the moment, the surfaces of the micron metal particles are fully contacted with a solvent in the reaction process, the micron metal particles and the solvent are mixed more uniformly and tightly in a better dissolution combination manner in the reaction process, and a tight three-dimensional stacking structure is formed. The large-sized particles in the solder paste serve as a framework for interconnection and provide high shear strength, high electrical conductivity and high thermal conductivity, and the small-sized particles serve as a binder to connect the large-sized particles to form complete and compact interconnection. The oxidation degree of the nano-copper particles in the prepared multi-size micro-nano metal particle soldering paste is low, the density of a sintered body can be effectively improved, and the shear strength and the electric conductivity are enhanced.
The technical solution of the present invention is further explained by the following embodiments.
In order to facilitate an understanding of the present invention, a more complete description of the present invention is provided below. The present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1
A multi-size micro-nano metal particle solder paste in-situ interconnection process comprises the following steps:
(a) dissolving a copper salt (specifically copper acetate) in a solvent (specifically 500mL of ethylene glycol) at 50 ℃, and adding a reducing agent (specifically ascorbic acid) and micron metal particles (specifically 1 micron copper particles) into the solvent, wherein the molar ratio of the copper salt to the reducing agent is 1: 6, the molar ratio of the copper salt to the micron metal particles is 1: 1, stirring and reacting for 20min to obtain a multi-size micro-nano metal particle dispersion liquid;
(b) concentrating the multi-size micro-nano metal particle dispersion liquid prepared in the step (a), pouring the multi-size micro-nano metal particle dispersion liquid prepared in the step (a) into a centrifuge tube, centrifuging the multi-size micro-nano metal particle dispersion liquid in a centrifuge for 5min under the condition of 12000r/min, and stirring to prepare multi-size micro-nano metal particle soldering paste (the mass percentage of micro-nano metal in the multi-size micro-nano metal particle soldering paste is 80%);
(c) coating the multi-size micro-nano metal particle soldering paste prepared in the step (b) on a substrate (specifically a copper substrate), covering an interconnection chip on the coated soldering paste, putting the interconnection chip into a hot pressing furnace, and sintering under the conditions that the sintering temperature is 300 ℃ and the sintering pressure is 2MPa to obtain the connecting joint.
Example 2
A multi-size micro-nano metal particle solder paste in-situ interconnection process comprises the following steps:
(a) dissolving a copper salt (specifically copper acetate) in a solvent (specifically 500mL of ethylene glycol) at 50 ℃, and adding a reducing agent (specifically ascorbic acid) and micron metal particles (specifically 1 micron copper particles) into the solvent, wherein the molar ratio of the copper salt to the reducing agent is 1: 1, the molar ratio of the copper salt to the micron metal particles is 1000: 1, stirring and reacting for 20min to obtain a multi-size micro-nano metal particle dispersion liquid;
(b) concentrating the multi-size micro-nano metal particle dispersion liquid prepared in the step (a), pouring the multi-size micro-nano metal particle dispersion liquid prepared in the step (a) into a centrifuge tube, centrifuging the multi-size micro-nano metal particle dispersion liquid in a centrifuge for 5min under the condition of 12000r/min, and stirring to prepare multi-size micro-nano metal particle soldering paste (the mass percentage of micro-nano metal in the multi-size micro-nano metal particle soldering paste is 80%);
(c) coating the multi-size micro-nano metal particle soldering paste prepared in the step (b) on a substrate (specifically a copper substrate), covering an interconnection chip on the coated soldering paste, putting the interconnection chip into a hot pressing furnace, and sintering under the conditions that the sintering temperature is 300 ℃ and the sintering pressure is 2MPa to obtain the connecting joint.
Example 3
A multi-size micro-nano metal particle solder paste in-situ interconnection process comprises the following steps:
(a) dissolving a copper salt (specifically copper acetate) in a solvent (specifically 500mL of ethylene glycol) at 50 ℃, and adding a reducing agent (specifically ascorbic acid) and micron metal particles (specifically 1 micron copper particles) into the solvent, wherein the molar ratio of the copper salt to the reducing agent is 1: 10, the molar ratio of the copper salt to the micron metal particles is 1: 10, stirring and reacting for 20min to obtain a multi-size micro-nano metal particle dispersion liquid;
(b) concentrating the multi-size micro-nano metal particle dispersion liquid prepared in the step (a), pouring the multi-size micro-nano metal particle dispersion liquid prepared in the step (a) into a centrifuge tube, centrifuging the multi-size micro-nano metal particle dispersion liquid in a centrifuge for 5min under the condition of 12000r/min, and stirring to prepare multi-size micro-nano metal particle soldering paste (the mass percentage of micro-nano metal in the multi-size micro-nano metal particle soldering paste is 80%);
(c) coating the multi-size micro-nano metal particle soldering paste prepared in the step (b) on a substrate (specifically a copper substrate), covering an interconnection chip on the coated soldering paste, putting the interconnection chip into a hot pressing furnace, and sintering under the conditions that the sintering temperature is 300 ℃ and the sintering pressure is 2MPa to obtain the connecting joint.
Example 4
A multi-size micro-nano metal particle solder paste in-situ interconnection process comprises the following steps:
(a) dissolving a copper salt (specifically copper acetylacetonate) in a solvent (specifically 300mL of ethylene glycol) at 50 ℃, and adding a reducing agent (specifically glucose) and micron metal particles (specifically 1 μm copper particles and 1 μm silver particles) into the solvent, wherein the molar ratio of the copper salt to the reducing agent is 1: 6, the molar ratio of the copper salt to the micron metal particles is 1: 1, stirring and reacting for 20min to obtain a multi-size micro-nano metal particle dispersion liquid;
(b) concentrating the multi-size micro-nano metal particle dispersion liquid prepared in the step (a), pouring the multi-size micro-nano metal particle dispersion liquid prepared in the step (a) into a centrifuge tube, centrifuging the multi-size micro-nano metal particle dispersion liquid in a centrifuge for 5min under the condition of 12000r/min, and stirring to prepare multi-size micro-nano metal particle soldering paste (the mass percentage of micro-nano metal in the multi-size micro-nano metal particle soldering paste is 80%);
(c) coating the multi-size micro-nano metal particle soldering paste prepared in the step (b) on a substrate (specifically a copper substrate), covering an interconnection chip on the coated soldering paste, putting the interconnection chip into a hot pressing furnace, and sintering under the conditions that the sintering temperature is 300 ℃ and the sintering pressure is 2MPa to obtain the connecting joint.
Example 5
A multi-size micro-nano metal particle solder paste in-situ interconnection process comprises the following steps:
(a) dissolving a copper salt (specifically, copper hydroxide) in a solvent (specifically, 600mL terpineol) at 80 ℃, and adding a reducing agent (specifically, ascorbic acid) and micron metal particles (specifically, 50 μm silver particles) in the solvent, wherein the molar ratio of the copper salt to the reducing agent is 1: 5, the molar ratio of the copper salt to the micron metal particles is 1: 1, stirring and reacting for 30min to obtain a multi-size micro-nano metal particle dispersion liquid;
(b) concentrating the multi-size micro-nano metal particle dispersion liquid prepared in the step (a), pouring a supernatant of the multi-size micro-nano metal particle dispersion liquid prepared in the step (a), and stirring to prepare a multi-size micro-nano metal particle soldering paste (the mass percentage of micro-nano metal in the multi-size micro-nano metal particle soldering paste is 70%);
(c) coating the multi-size micro-nano metal particle soldering paste prepared in the step (b) on a substrate (specifically a copper substrate), covering an interconnection chip on the coated soldering paste, putting the interconnection chip into a hot pressing furnace, and sintering under the conditions that the sintering temperature is 350 ℃ and the sintering pressure is 5MPa to obtain the connecting joint.
Example 6
A multi-size micro-nano metal particle solder paste in-situ interconnection process comprises the following steps:
(a) dissolving a copper salt (specifically copper acetate) in a solvent (specifically 100mL of ethylene glycol) at 80 ℃, adding a reducing agent (specifically ascorbic acid) and micron metal particles (specifically 200nm silver particles and 1 μm tin particles) in the solvent, wherein the molar ratio of the copper salt to the reducing agent is 1: 10, the molar ratio of the copper salt to the micron metal particles is 1: 1, stirring and reacting for 30min to obtain a multi-size micro-nano metal particle dispersion liquid;
(b) concentrating the multi-size micro-nano metal particle dispersion liquid prepared in the step (a), pouring the multi-size micro-nano metal particle dispersion liquid prepared in the step (a) into a centrifuge tube, centrifuging the multi-size micro-nano metal particle dispersion liquid in a centrifuge for 5min under the condition of 12000r/min, and stirring to prepare multi-size micro-nano metal particle soldering paste (the mass percentage of micro-nano metal in the multi-size micro-nano metal particle soldering paste is 80%);
(c) coating the multi-size micro-nano metal particle soldering paste prepared in the step (b) on a substrate (specifically a copper substrate), covering an interconnection chip on the coated soldering paste, putting the interconnection chip into a hot pressing furnace, and sintering under the conditions that the sintering temperature is 260 ℃ and the sintering pressure is 2MPa to obtain the connecting joint.
Example 7
A multi-size micro-nano metal particle solder paste in-situ interconnection process comprises the following steps:
(a) dissolving a copper salt (specifically, copper formate) in a solvent (specifically, 100mL of ethylene glycol) at 50 ℃, and adding a reducing agent (specifically, hydrazine hydrate) and micron metal particles (specifically, 2 mu m tin particles) into the solvent, wherein the molar ratio of the copper salt to the reducing agent is 1: 10, the molar ratio of the copper salt to the micron metal particles is 1: 1, stirring and reacting for 10min to obtain a multi-size micro-nano metal particle dispersion liquid;
(b) concentrating the multi-size micro-nano metal particle dispersion liquid prepared in the step (a), pouring the multi-size micro-nano metal particle dispersion liquid prepared in the step (a) into a rotary evaporator, evaporating for 10min under the conditions that the rotating speed is 120r/min, the evaporating temperature is 60 ℃ and the vacuum degree is 180Pa, and stirring to prepare a multi-size micro-nano metal particle soldering paste (the mass percentage of micro-nano metals in the multi-size micro-nano metal particle soldering paste is 95%);
(c) coating the multi-size micro-nano metal particle soldering paste prepared in the step (b) on a substrate (specifically a copper substrate), covering an interconnection chip on the coated soldering paste, putting the interconnection chip into a rapid annealing furnace, and sintering at the sintering temperature of 260 ℃ under a non-pressure condition to obtain the connecting joint.
Example 8
A multi-size micro-nano metal particle solder paste in-situ interconnection process comprises the following steps:
(a) dissolving a copper salt (specifically, copper hydroxide) in a solvent (specifically, 100mL of ethylene glycol) at 80 ℃, and adding a reducing agent (specifically, ascorbic acid) and micron metal particles (specifically, 2 μm tin particles) in the solvent, wherein the molar ratio of the copper salt to the reducing agent is 1: 10, the molar ratio of the copper salt to the micron metal particles is 1: 3, stirring and reacting for 30min to obtain a multi-size micro-nano metal particle dispersion liquid;
(b) concentrating the multi-size micro-nano metal particle dispersion liquid prepared in the step (a), pouring the multi-size micro-nano metal particle dispersion liquid prepared in the step (a) into a centrifuge tube, centrifuging for 5min in a centrifuge under the condition of 12000r/min, then drying in a vacuum drying oven under the conditions of vacuum degree of 0.1MPa and temperature of 60 ℃ to obtain a micro-nano metal paste body with the mass percent of 98%, and then adding a proper amount of glycol for stirring and diluting to prepare the multi-size micro-nano metal particle soldering paste (the mass percent of micro-nano metal in the multi-size micro-nano metal particle soldering paste is 80%);
(c) coating the multi-size micro-nano metal particle soldering paste prepared in the step (b) on a substrate (specifically a copper substrate), covering an interconnection chip on the coated soldering paste, putting the interconnection chip into a hot pressing furnace, and sintering under the conditions that the sintering temperature is 260 ℃ and the sintering pressure is 2MPa to obtain the connecting joint.
Comparative example 1
(a) At the temperature of 60 ℃, copper acetate, ascorbic acid and PVP-K30 (polyvinylpyrrolidone) are mixed according to the molar ratio of 1: 2: 2000, putting the mixture into 100mL of ethanol solvent for reaction, obtaining nano metal solution after the reaction is carried out for 15min, pouring the nano metal solution into a centrifuge tube, and centrifuging the solution in a centrifuge for 5min under the condition of 12000 r/min; adding ethanol again, and repeating the centrifugation operation to remove PVP-K30;
(b) centrifuging for many times, then placing the mixture into a vacuum drying oven to be dried under the conditions that the vacuum degree is 0.1MPa and the temperature is 40 ℃ to obtain a nano metal paste body with the mass fraction of 99%, and then adding a proper amount of soldering flux to be stirred to obtain the nano metal paste body with the mass percentage of 80%;
(c) the paste was coated on a copper substrate, an interconnection chip was covered on the coated copper paste, which was put in a hot pressing furnace and sintered at a sintering temperature of 260 ℃ and a sintering pressure of 2MPa to obtain a connection joint.
Comparative example 2
Comparison is made with example 1, wherein the molar ratio of copper salt to reducing agent is 2: 1, the molar ratio of the copper salt to the micron metal particles is 1: 15, the remaining raw materials and the preparation method were the same as in example 1, to obtain a linker.
Comparative example 3
In comparison with example 1, the reaction temperature of the stirring reaction in step (a) was 100 ℃, and the remaining raw materials and the preparation method were the same as those of example 1, to obtain a linker.
Comparative example 4
In comparison with example 1, the reaction temperature of the stirring reaction in step (a) was 10 ℃, and the remaining raw materials and the preparation method were the same as those of example 1, to obtain a linker.
Comparative example 5
In comparison with example 1, the micron metal particles were replaced with 80nm nano copper particles, and the remaining raw materials and preparation method were the same as example 1, to obtain a connection joint.
Comparative example 6
In comparison with example 1, the micron metal particles were copper particles of 150 μm, and the remaining raw materials and preparation method were the same as those of example 1, to obtain a joint.
Comparative example 7
In comparison with example 1, the sintering temperature in step (c) was 15 ℃, and the remaining raw materials and the preparation method were the same as those of example 1, to obtain a joint.
Comparative example 8
In comparison with example 1, the sintering temperature in step (c) was 650 ℃, and the remaining raw materials and the preparation method were identical to those of example 1, to obtain a junction joint.
And (3) performance testing: the connection joints obtained in examples 1 to 7 and comparative examples 1 to 8 were subjected to a shear strength test using an IC package weld strength tester (SERIES-4000-DONDESTER), and the test results are shown in the following table:
from the embodiments 1 to 8, it can be known that in-situ preparation of micro-nano metal solder paste is effectively realized by adding micro-nano metal particles in advance, multi-size micro-nano metal dispersion is concentrated to obtain multi-size micro-nano metal solder paste, the multi-size micro-nano metal solder paste is directly coated on a substrate and then sintered to realize in-situ interconnection, the micro-metal particles and the nano metal particles form three-dimensional compact stacking with different particle sizes, and the shearing force of the prepared connecting joint is high, in addition, XRD detection is performed on the multi-size micro-nano metal particle solder paste prepared in the embodiments 1 to 8, and a test result shows that no oxidation peak of copper oxide and cuprous oxide exists, which indicates that no oxide of copper is detected, the multi-size micro-nano metal particle solder paste is prepared by the in-situ preparation method, and in-situ preparation of the multi-size micro-nano metal is realized by the method of adding micro-nano metal in advance, the operations of centrifuging, washing, drying and the like are not needed to be carried out on the micro-nano metal, so that the preparation process of the metal soldering paste is greatly simplified, the micro-nano metal particles are prevented from further contacting with air, and the agglomeration and oxidation of nano materials are avoided;
comparative example 1 a solder paste was prepared by a liquid phase reduction method, and since the nano-copper particles were washed and separated several times during the process of separating the liquid phase from the nano-copper particles, the nano-copper particles were exposed to the air, which aggravated the oxidation of the nano-copper particles and hindered sintering, thereby reducing the shear strength of the joint;
in the comparative example 2, the molar ratio of the copper salt to the reducing agent is too high, and the molar ratio of the copper salt to the micron metal particles is too low, so that the micron metal particles and the nanometer metal particles cannot form the most compact three-dimensional stacking, the compactness of a paste sintered body is influenced, and the shear strength of a connecting joint is reduced;
the stirring reaction temperature of the comparative example 3 in the step (a) is too high, and the stirring reaction temperature of the comparative example 4 in the step (a) is too low, so that the reaction of reducing copper salt in the step (a) is influenced, the size and the appearance of the formed nano particles can not reach the standard, and the effect of forming a compact three-dimensional structure with the micro particles can not be achieved, the most compact three-dimensional stacking density of the micro metal particles and the nano metal particles can not be formed, the sintered body of the paste is influenced, and the shear strength of the connecting joint is finally reduced;
comparative example 5 since the size of the nano-copper particles is too small, the nano-copper particles used in comparative example 5 have poor strength compared to the micro-metal particles of the original example 1, so that the shear strength of the prepared connection joint is poor compared to example 1, and the size of the micro-metal particles added in comparative example 6 is too large, so that the sintering effect is deteriorated and the shear strength of the prepared connection joint is deteriorated;
the temperature of comparative example 7 when sintering is too low for the intensity of sintered body worsen, and the temperature of comparative example 8 when sintering is too high, because the temperature difference of different component device damage, after part components and parts damaged under the sintering of too high temperature, can't test shear strength, when the device of sintering is copper connection high-power device, then can not damage the device, shear strength is also high, but the energy waste is big, and the course of working is dangerous.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The in-situ interconnection process of the multi-size micro-nano metal particle solder paste is characterized by comprising the following steps of:
(a) dissolving a copper salt in a solvent, adding a reducing agent and micron metal particles in the solvent, and stirring for reaction to obtain a multi-size micro-nano metal particle dispersion liquid;
(b) concentrating the multi-size micro-nano metal particle dispersion liquid prepared in the step (a) to prepare multi-size micro-nano metal particle soldering paste;
(c) and (c) coating the multi-size micro-nano metal particle soldering paste prepared in the step (b) on a substrate, and then sintering.
2. The in-situ interconnection process of multi-sized micro-nano metal particle solder paste according to claim 1, wherein in the step (a), the size of the micro-nano metal particles is 0.1 μm to 100 μm.
3. The in-situ interconnection process of the multi-size micro-nano metal particle solder paste according to claim 1, wherein in the step (a), the size of the nano copper particles generated by the stirring reaction is 50-800 nm.
4. The in-situ interconnection process of multi-sized micro-nano metal particle solder paste according to claim 1, wherein in the step (a), the molar ratio of the copper salt to the reducing agent is 1: 1-1: 10, the molar ratio of the copper salt to the micron metal particles is 1000: 1-1: 10.
5. the in-situ interconnection process of multi-sized micro-nano metal particle solder paste according to claim 1, wherein in the step (a), the copper salt is any one of copper acetate, copper hydroxide, copper formate, copper acetylacetonate or copper oxalate, the micro metal is one or more of copper particles, silver particles, gold particles, tin particles and aluminum particles, the solvent is one or more of water, toluene, butylbenzene, diethyl ether, ethyl acetate, ethanol, ethylene glycol, diethylene glycol, dipropylene glycol, glycerol, acetone, glycerol and terpineol, and the reducing agent is any one of hydrazine hydrate, phenylhydrazine, ascorbic acid and glucose.
6. The in-situ interconnection process of the multi-size micro-nano metal particle solder paste according to claim 1, wherein in the step (a), the reaction temperature of the stirring reaction is 20-80 ℃, and the reaction time is 10-180 min.
7. The in-situ interconnection process of multi-sized micro-nano metal particle solder paste according to claim 1, wherein in the step (b), the concentration is performed by using one or more of a rotary evaporator, a vacuum drying oven, a centrifuge, a filtering device, and natural sedimentation.
8. The in-situ interconnection process of the multi-size micro-nano metal particle solder paste according to claim 1, wherein the mass percent of the micro-nano metal in the multi-size micro-nano metal particle solder paste is 30-99%.
9. The in-situ interconnection process of multi-size micro-nano metal particle solder paste according to claim 1, wherein in the step (c), the sintering temperature is 20-600 ℃ and the sintering pressure is 0-20 MPa.
10. A multi-size micro-nano metal particle soldering paste is characterized by being prepared by the in-situ interconnection process of the multi-size micro-nano metal particle soldering paste according to any one of claims 1 to 9.
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