CN111408869A - Micro-nano copper particle soldering paste for low-temperature bonding and preparation method and application thereof - Google Patents
Micro-nano copper particle soldering paste for low-temperature bonding and preparation method and application thereof Download PDFInfo
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- CN111408869A CN111408869A CN202010281490.2A CN202010281490A CN111408869A CN 111408869 A CN111408869 A CN 111408869A CN 202010281490 A CN202010281490 A CN 202010281490A CN 111408869 A CN111408869 A CN 111408869A
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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
- B23K35/0255—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in 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
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/3612—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with organic compounds as principal constituents
Abstract
The invention belongs to the technical field of electronic manufacturing, and particularly discloses micro-nano copper particle soldering paste for low-temperature bonding and a preparation method and application thereof. The preparation method comprises the following steps: cleaning the micron copper particles to remove impurities, and then drying for later use; placing the dried micron copper particles in a preset environment for oxidation, thereby forming nano copper oxide on the surfaces of the micron copper particles; placing the oxidized micron copper particles in a reducing agent for reduction, so that the nano copper oxide on the surface is reduced into nano copper particles, and obtaining the micro-nano copper particles; and adding an organic thickener into the micro-nano copper particles, and stirring and defoaming to form the micro-nano copper particle soldering paste. The invention utilizes the pre-oxidation and reduction processes to form a nano structure on the surface and in the gap of the micron copper particles, effectively reduces the bonding temperature by utilizing the small-size effect, meets the packaging application requirements of power devices, solves the problems of complex process and high cost, and meets the application requirements of low-temperature service and high-temperature interconnection.
Description
Technical Field
The invention belongs to the technical field of electronic manufacturing, and particularly relates to micro-nano copper particle soldering paste for low-temperature bonding and a preparation method and application thereof.
Background
With the development of electronic devices in the direction of miniaturization, high density and high integration, third generation wide band gap semiconductor materials, represented by SiC and GaN, are widely used in high power electronic devices because they have stable performance at high temperatures of 500 ℃. Therefore, finding a suitable high temperature resistant and high stability packaging interconnection material is one of the main factors driving the development of power devices. Lead-containing solder can withstand high temperatures, but it presents serious environmental and human health hazards and is now banned from use in electronic devices. Lead-free solders developed in recent years can also meet the requirement of high temperature resistance, but all have respective disadvantages, such as higher cost of gold-based solders, easy corrosion of zinc-based solders, greater brittleness of bismuth-based solders, and the like, and the mismatch of thermal expansion coefficients between the interconnection layer and the substrate causes greater residual stress on the bonding layer after high-temperature reflow, thereby reducing the mechanical strength and the service life of the device.
In recent years, with the development of nanotechnology, metal nanomaterials have attracted much attention in various fields because of their excellent physicochemical properties. Based on the small-size effect of the nano material, the low-temperature bonding and high-temperature service can be realized, and the packaging requirement of the power device is met. The nano silver has excellent electric and heat conductivity and good sintering performance at low temperature, and becomes a research hotspot of a nano soldering paste technology. However, the cost of the metallic silver is high, the porosity is high after sintering, and electromigration is easy to generate, so that the interface fails. The nano copper particles have wide sources and low cost, have the electric and thermal conductivity similar to that of metal silver, and can replace nano silver soldering paste. However, the preparation process of the nano-copper particles is complex and easy to oxidize, the synthesis and storage difficulty is increased, and the sintering temperature is increased by the surface oxide to influence the conductivity. The micron copper particles are easy to prepare and low in cost, and the oxidation resistance is greatly improved compared with that of nano copper, but the micron copper particles cannot be sintered at low temperature. Partial research discusses the possibility of sintering and bonding micro-nano composite copper particles, but the problem of complicated preparation process is still not solved.
Disclosure of Invention
Aiming at the defects and/or improvement requirements of the prior art, the invention provides the micro-nano copper particle soldering paste for low-temperature bonding and the preparation method and application thereof, wherein a nano structure is formed on the surface of the micro-nano copper particle through pre-oxidation and reduction processes, so that the bonding temperature is favorably reduced, and the packaging application requirements of a power device are met.
In order to achieve the above object, according to an aspect of the present invention, a method for preparing micro-nano copper particle solder paste for low temperature bonding is provided, the method comprising the following steps:
s1, cleaning the micron copper particles to remove impurities, and then drying for later use;
s2, placing the dried micron copper particles in a preset environment for oxidation, so as to form nano copper oxide on the surfaces of the micron copper particles;
s3, placing the oxidized micro copper particles in a reducing agent for reduction, so that the nano copper oxide on the surface is reduced into nano copper particles, and thus obtaining the micro-nano copper particles;
s4, adding an organic thickener into the micro-nano copper particles, and stirring and defoaming to form the micro-nano copper particle soldering paste.
Preferably, in step S1, the micro-nano copper particles have a particle size of 1 μm to 10 μm, and HCl solution and H are used2SO4One or more of the solution and formic acid solution cleans the micron copper particles.
As a further preference, in step S2, the micron copper particles are placed at a temperature of 200 ℃ to 300 ℃ and kept for 20min to 60min, so that the micron copper particles are subjected to oxidation reaction.
As a further preferred, in step S2, the micron copper particles are placed in an oxygen-rich environment for 1 to 3 days, so that the micron copper particles are subjected to oxidation reaction.
More preferably, in step S2, the nano copper oxide is a mixture of cuprous oxide and cupric oxide, and the size of the nano copper oxide is 60nm to 150 nm.
As a further preferred, in step S3, the reducing agent is one or more of hydrochloric acid, sulfuric acid, formic acid and isopropanolamine.
As a further preferred, in step S4, the organic thickener is one or more of terpineol, ethylene glycol, n-butanol, absolute ethanol, glycerol, and isopropanol.
According to another aspect of the invention, the micro-nano copper particle solder paste for low-temperature bonding prepared by the method is provided.
According to another aspect of the present invention, there is provided a method for performing low temperature bonding by using the micro-nano copper particle solder paste, the method specifically comprises: and coating the micro-nano copper particle soldering paste on a substrate, and finishing bonding under a preset condition.
More preferably, in the bonding process, the bonding temperature is less than 300 ℃, the bonding pressure is less than 5MPa, and the bonding time is less than 30 minutes.
Generally, compared with the prior art, the above technical solution conceived by the present invention mainly has the following technical advantages:
1. the invention provides a novel preparation method aiming at the problem of complicated preparation process of micro-nano copper particles, wherein a nano structure is formed on the surface and in the gap of the micro-nano copper particles by utilizing the pre-oxidation and reduction processes, the bonding temperature is effectively reduced by utilizing the small-size effect of the nano structure, the packaging application requirement of a power device is met, the problems of complex process and high cost are solved, and the application requirement of low-temperature service and high-temperature interconnection is met;
2. particularly, the invention can effectively improve the efficiency of the oxidation-reduction process, save energy and reduce cost by optimizing the conditions of the oxidation process and the reduction process.
Drawings
FIG. 1 is a flow chart of the preparation of micro-nano copper particle solder paste for low-temperature bonding according to the present invention;
fig. 2 is SEM images of the micro-nano copper particles obtained in steps S2 and S3 in example 1 of the present invention, wherein (a) is an SEM image of the oxidized micro-nano copper particles obtained in step S2, and (b) is an SEM image of the micro-nano copper particles obtained in step S3;
fig. 3 is XRD patterns of the micro-nano copper particles obtained in steps S2 and S3 in example 2 of the present invention, wherein (a) is the XRD pattern of the oxidized micro-nano copper particles obtained in step S2, and (b) is the XRD pattern of the micro-nano copper particles obtained in step S3.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
As shown in fig. 1, an embodiment of the present invention provides a method for preparing micro-nano copper particle solder paste for low-temperature bonding, including the following steps:
s1 micron copper particles with particle size of 1-10 μm are selected and HCl solution and H are adopted2SO4Cleaning the solution with one or more of a formic acid solution and a formic acid solution to remove impurities, and then drying for later use;
s2, oxidizing the dried micron copper particles in a high-temperature or oxygen-enriched environment to form a nano copper oxide on the surfaces of the micron copper particles, wherein the nano copper oxide is a mixture of cuprous oxide and cupric oxide, and the size (thickness or particle diameter) of the nano copper oxide is 60 nm-150 nm;
s3, placing the oxidized micron copper particles in a reducing agent for reduction, so that the nano copper oxide on the surface is reduced into nano copper particles, and thus obtaining the micro-nano copper particles;
s4, adding an organic thickener into the micro-nano copper particles, and stirring and defoaming to form the micro-nano copper particle soldering paste.
Further, in step S2, the micron copper particles are placed at a temperature of 200 to 300 ℃ and kept warm for 20 to 60 minutes to control the oxidation reaction of the micron copper particles, and if the reaction temperature is too low and the reaction time is too short, the surface nano-oxides are less and the oxidation effect cannot be achieved; if the oxidation reaction is too severe, the reduction difficulty increases and the cost increases. And during the oxidation, the oxidation uniformity of the surface of the micron copper particles is ensured by continuously stirring.
Further, in step S2, the micron copper particles are placed in an oxygen-rich environment (oxygen concentration is greater than 23.5%) for 1 to 3 days, so that the micron copper particles are subjected to oxidation reaction, and the oxidation uniformity of the surfaces of the micron copper particles is ensured by continuously stirring the micron copper particles.
Further, in step S3, the reducing agent is one or more of hydrochloric acid, sulfuric acid, formic acid, and isopropanolamine.
Further, in step S4, the organic thickener is one or more of terpineol, ethylene glycol, n-butanol, absolute ethanol, glycerol, and isopropanol.
According to another aspect of the invention, the micro-nano copper particle solder paste for low-temperature bonding prepared by the method is provided.
According to another aspect of the present invention, there is provided a method for performing low temperature bonding by using the micro-nano copper particle solder paste, the method specifically comprises: coating micro-nano copper particle soldering paste on a substrate by utilizing a screen printing process, and completing bonding at low temperature and low pressure; in the bonding process, the bonding temperature is less than 300 ℃, the bonding pressure is less than 5MPa, and the bonding time is less than 30 minutes.
The present invention will be further described in detail with reference to the process flow shown in FIG. 1 in conjunction with the following examples.
Example 1
S1, selecting micron copper particles with the average particle size of 1 mu m, cleaning the micron copper particles by adopting an HCl solution (5 wt%) to remove impurities, and then drying the micron copper particles for later use;
s2, placing the dried micron copper particles in a high-temperature furnace for oxidation, wherein the heat preservation temperature is 250 ℃, the heat preservation time is 20 minutes, and during the period, the continuous stirring is carried out to improve the oxidation uniformity of the particle surfaces, so that nano copper oxide is formed on the surfaces of the particles;
s3, placing the oxidized micro copper particles in formic acid solution (10 wt%) for reduction, so that the nano copper oxide on the surface is reduced into a nano copper structure (a nano copper layer or nano copper particles), and thus obtaining micro-nano copper particles;
s4, adding n-butanol into the micro-nano copper particles as an organic thickener, and stirring and defoaming to form the micro-nano copper particle solder paste.
S5, coating the micro-nano copper particle solder paste on the ceramic substrate by utilizing a screen printing process, and carrying out bonding reaction, wherein the bonding temperature is 225 ℃, the bonding pressure is 1MPa, and the bonding time is 15 minutes.
Microscopic observation of the micron copper particles subjected to oxidation and reduction reactions in step S2 and step S3 resulted in SEM images shown in fig. 2. As can be seen from fig. 2 (a), an oxide layer is formed on the surface of the oxidized micro-nano particles, and the average thickness is about 120 nm; as can be seen from fig. 2 (b), a nano copper layer or nano copper particles are formed on the surface of or near the micro-nano copper particles, so that micro-nano composite copper particles are obtained, the bonding temperature can be effectively reduced, and the sintering performance can be improved.
Example 2
S1 micron copper particles with average particle size of 10 μm are selected and H is adopted2SO4Cleaning the solution (10 wt%) to remove impurities, and drying for later use;
s2, placing the dried micron copper particles in an oxygen-rich environment for 3 days for oxidation, and continuously stirring the micron copper particles during the oxidation to improve the oxidation uniformity of the particle surfaces, so that nano copper oxides are formed on the surfaces of the micron copper particles;
s3, placing the oxidized micron copper particles in an isopropanolamine solution (20 wt%) for reduction, so that the nano copper oxide on the surface is reduced into a nano copper structure (a nano copper layer or nano copper particles), and thus obtaining the micro-nano copper particles;
s4, adding ethylene glycol serving as an organic thickener into the micro-nano copper particles, and stirring and defoaming the mixture to form the micro-nano copper particle soldering paste.
S5, coating the micro-nano copper particle solder paste on the ceramic substrate by utilizing a screen printing process, and carrying out bonding reaction, wherein the bonding temperature is 275 ℃, the bonding pressure is 4MPa, and the bonding time is 25 minutes.
XRD phase analysis was performed on the micron copper particles after the oxidation and reduction reactions occurred in step S2 and step S3, resulting in XRD patterns as shown in fig. 3. As can be seen from fig. 3 (a), cuprous oxide and cupric oxide mixture is formed on the surface of the micron copper particles after oxidation; as can be seen from (b) in fig. 3, the oxidation peak of the micro-nano copper particles disappears, indicating that the reducing agent has completely reduced the oxide into the copper particles.
Example 3
S1, selecting micron copper particles with the average particle size of 2.5 mu m, cleaning the micron copper particles by adopting a formic acid solution (20 wt%) to remove impurities, and then drying the micron copper particles for later use;
s2, placing the dried micron copper particles in an oxygen-rich environment for 24h for oxidation, and continuously stirring the micron copper particles during the oxidation to improve the oxidation uniformity of the particle surfaces, so that nano copper oxides are formed on the surfaces of the micron copper particles;
s3, placing the oxidized micro copper particles in formic acid solution (15 wt%) for reduction, so that the nano copper oxide on the surface is reduced into a nano copper structure (a nano copper layer or nano copper particles), and thus obtaining micro-nano copper particles;
s4, adding terpineol serving as an organic thickener into the micro-nano copper particles, and stirring and defoaming the mixture to form the micro-nano copper particle soldering paste.
S5, coating the micro-nano copper particle solder paste on the ceramic substrate by utilizing a screen printing process, and carrying out bonding reaction, wherein the bonding temperature is 250 ℃, the bonding pressure is 2MPa, and the bonding time is 20 minutes.
Example 4
S1, selecting micron copper particles with the average particle size of 7.5 mu m, cleaning the micron copper particles by adopting an HCl solution (5 wt%) to remove impurities, and then drying the micron copper particles for later use;
s2, placing the dried micron copper particles in a high-temperature furnace for oxidation, wherein the heat preservation temperature is 200 ℃, the heat preservation time is 30 minutes, and during the period, the particles are continuously stirred to improve the oxidation uniformity of the particle surfaces, so that nano copper oxides are formed on the surfaces of the particles;
s3, placing the oxidized micro copper particles in a sulfuric acid solution (5 wt%) for reduction, so that the nano copper oxide on the surface is reduced into a nano copper structure (a nano copper layer or nano copper particles), and thus obtaining micro-nano copper particles;
s4, adding glycerol and absolute ethyl alcohol into the micro-nano copper particles to serve as an organic thickener, and stirring and defoaming the mixture to form the micro-nano copper particle soldering paste.
S5, coating the micro-nano copper particle solder paste on the ceramic substrate by utilizing a screen printing process, and carrying out bonding reaction, wherein the bonding temperature is 280 ℃, the bonding pressure is 3MPa, and the bonding time is 20 minutes.
Example 5
S1, selecting micron copper particles with the average particle size of 5 microns, cleaning the micron copper particles by adopting an HCl solution (5 wt%) to remove impurities, and drying the micron copper particles for later use;
s2, placing the dried micron copper particles in a high-temperature furnace for oxidation, wherein the heat preservation temperature is 300 ℃, the heat preservation time is 60 minutes, and during the period, the particles are continuously stirred to improve the oxidation uniformity of the particle surfaces, so that nano copper oxides are formed on the surfaces of the particles;
s3, placing the oxidized micro copper particles in a sulfuric acid solution (5 wt%) for reduction, so that the nano copper oxide on the surface is reduced into a nano copper structure (a nano copper layer or nano copper particles), and thus obtaining micro-nano copper particles;
s4, adding glycerol and absolute ethyl alcohol into the micro-nano copper particles to serve as an organic thickener, and stirring and defoaming the mixture to form the micro-nano copper particle soldering paste.
S5, coating the micro-nano copper particle solder paste on the ceramic substrate by utilizing a screen printing process, and carrying out bonding reaction, wherein the bonding temperature is 300 ℃, the bonding pressure is 5MPa, and the bonding time is 30 minutes.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A preparation method of micro-nano copper particle soldering paste for low-temperature bonding is characterized by comprising the following steps:
s1, cleaning the micron copper particles to remove impurities, and then drying for later use;
s2, placing the dried micron copper particles in a preset environment for oxidation, so as to form nano copper oxide on the surfaces of the micron copper particles;
s3, placing the oxidized micro copper particles in a reducing agent for reduction, so that the nano copper oxide on the surface is reduced into nano copper particles, and thus obtaining the micro-nano copper particles;
s4, adding an organic thickener into the micro-nano copper particles, and stirring and defoaming to form the micro-nano copper particle soldering paste.
2. The method for preparing micro-nano copper particle solder paste for low temperature bonding according to claim 1, wherein in step S1, the particle size of the micro copper particles is 1 μm to 10 μm, and HCl solution and H solution are adopted2SO4One or more of the solution and formic acid solution cleans the micron copper particles.
3. The method for preparing micro-nano copper particle solder paste for low temperature bonding according to claim 1, wherein in step S2, the micro copper particles are placed at a temperature of 200 ℃ to 300 ℃ and are kept for 20min to 60min, so that the micro copper particles are subjected to oxidation reaction.
4. The method for preparing micro-nano copper particle solder paste for low-temperature bonding according to claim 1, wherein in step S2, micron copper particles are placed in an oxygen-rich environment for 1 to 3 days, so that the micron copper particles are subjected to oxidation reaction.
5. The method for preparing micro-nano copper particle solder paste for low temperature bonding according to claim 1, wherein in step S2, the nano copper oxide is a mixture of cuprous oxide and cupric oxide, and the size of the nano copper oxide is 60nm to 150 nm.
6. The method for preparing micro-nano copper particle solder paste for low-temperature bonding according to claim 1, wherein in step S3, the reducing agent is one or more of hydrochloric acid, sulfuric acid, formic acid and isopropanolamine.
7. The method for preparing micro-nano copper particle solder paste for low temperature bonding according to claim 1, wherein in step S4, the organic thickener is one or more of terpineol, ethylene glycol, n-butanol, absolute ethyl alcohol, glycerol and isopropanol.
8. A micro-nano copper particle soldering paste for low-temperature bonding prepared by the method of claims 1-7.
9. A method for bonding the micro-nano copper particle solder paste according to claim 8 at a low temperature is characterized by comprising the following steps: and coating the micro-nano copper particle soldering paste on a substrate, and finishing bonding under a preset condition.
10. The method for bonding the micro-nano copper particle solder paste at the low temperature according to claim 9, wherein the bonding temperature is less than 300 ℃, the bonding pressure is less than 5MPa, and the bonding time is less than 30 minutes.
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| CN111975011A (en) * | 2020-07-20 | 2020-11-24 | 华南理工大学 | Nano copper paste for chip pressureless sintering interconnection and preparation method and application thereof |
| CN114043123A (en) * | 2021-12-15 | 2022-02-15 | 深圳先进技术研究院 | Nano copper soldering paste and application thereof in chip packaging interconnection structure |
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| CN117690869A (en) * | 2024-01-30 | 2024-03-12 | 安徽大学 | Copper-copper low-temperature direct bonding method in air environment |
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| CN111408869B (en) | 2021-05-18 |
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