CN114310038A - Silver salt nano silver composite soldering paste, preparation method, sintering method and application - Google Patents

Silver salt nano silver composite soldering paste, preparation method, sintering method and application Download PDF

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CN114310038A
CN114310038A CN202210177520.4A CN202210177520A CN114310038A CN 114310038 A CN114310038 A CN 114310038A CN 202210177520 A CN202210177520 A CN 202210177520A CN 114310038 A CN114310038 A CN 114310038A
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silver
nano
silver salt
particles
salt
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CN114310038B (en
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周国云
邱娟
梁志杰
王守绪
何为
陈苑明
唐耀
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University of Electronic Science and Technology of China
Zhuhai Founder Technology High Density Electronic Co Ltd
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University of Electronic Science and Technology of China
Zhuhai Founder Technology High Density Electronic Co Ltd
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Abstract

The invention provides a silver salt nano-silver composite soldering paste, a preparation method thereof, a sintering method and an application thereof, wherein the raw materials comprise nano-silver particles, silver salt and glycol, the surface of the nano-silver particles is uniformly coated with a layer of polyvinylpyrrolidone, and the preparation method comprises the following steps: s1: preparing a nano silver solution by using nano silver particles with PVP uniformly coated on the surfaces and ethylene glycol; s2: grinding silver salt, adding silver salt particles into the nano-silver solution to obtain a silver salt and nano-silver mixed solution; s3: uniformly mixing the silver salt and nano-silver mixed solution by adopting mechanical oscillation to obtain uniform silver salt nano-silver composite soldering paste; the invention utilizes the reducibility of ethylene glycol to form the synergistic effect of reduced silver salt and nano-silver soldering paste sintering, improves the density of the sintered body, reduces the oxidation degree of nano-silver particles in the whole sintering process, improves the interface bonding force between the sintered body and a substrate, improves the density of the sintered body, reduces the overall sintering temperature, and meets the requirements of high shear strength and low porosity of the sintered body.

Description

Silver salt nano silver composite soldering paste, preparation method, sintering method and application
Technical Field
The invention belongs to the field of connection of metal nanoparticles, and particularly relates to silver salt nano-silver composite soldering paste, a preparation method, application and a sintering method thereof.
Background
With the higher and higher operating temperature of power devices such as power electronics, microwave radio frequency and the like, great challenges are brought to the operating stability of the packaging interconnection material. The raw materials for power devices, such as SiC and GaN, typically operate at temperatures of 200 c and even above 350 c for long periods of time, which are too high for conventional die attach materials that are currently in widespread use. At present, the main high-temperature packaging interconnection materials comprise Pb-based solder, Zn-based solder, Au-based solder and the like with high melting points. The disadvantage of Pb-based solders is environmental damage; the Zn-based solder has the disadvantages of high hardness and poor stress relaxation capability; the alloy formed by the Au-based solder is hard, so that the thermal stress generated by the joint is easily and directly transferred to the semiconductor device, and the failure of the whole packaging device is caused. In addition, the Au-based solder has high cost and is not suitable for popularization and application, and the key point for solving the problems lies in finding out a packaging interconnection material suitable for high-temperature work and a corresponding packaging interconnection process. The nano silver material can be sintered at low temperature due to the characteristics of small size effect, surface effect and the like, the melting point of a sintered sample can be compared favorably with that of a silver block, and the nano silver material has good performances of shearing, electric conduction and the like and can realize low-temperature connection and high-temperature service.
Due to the different particle sizes, shapes and the like of the nano-silver particles, the affinity to different sintering processes is different, and the appropriate sintering process is required to match the nano-silver particles in different states. Because the surface of the nano silver particles is easy to oxidize, the existence of the surface oxidation layer hinders the material exchange, and the sintering temperature of the nano silver particles can be increased. Meanwhile, the existence of the oxide can weaken the binding force between the sintered body and the substrate, and the application difficulty in low-temperature packaging interconnection is increased.
In the present invention, we invented a reduced silver salt, nano-silver composite solder paste and a synergistic method thereof. The boiling point of ethylene glycol is 197.3 ℃, and ethylene glycol itself has reducing properties at high temperatures. In the method, glycol is used as a solvent and a reducing agent, and silver salt and nano-silver particles are used as a filler to prepare the nano-silver soldering paste. The sintering process of the nano-silver soldering paste is carried out in sections, and the heat preservation is carried out for a period of time at the temperature that the glycol has reducibility, so that silver salt and silver oxide are fully reduced; meanwhile, in the process of sintering the nano-silver soldering paste, silver salt particles reduced by glycol are filled among the nano-silver particles to perform a synergistic effect, so that the density of a sintered body is improved to a certain extent. The method can reduce the oxidation degree of the nano silver particles in the whole sintering process as much as possible, remove the oxide on the surfaces of the nano silver particles, and the added silver salt has no corrosion to the packaging body and has environmental protection. The method realizes effective sintering of nano silver particles, improves the interface bonding force between the sintered body and the substrate, improves the density of the sintered body, reduces the overall sintering temperature, and meets the requirements of high shear strength and low porosity of the sintered body.
Disclosure of Invention
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of silver salt nano-silver composite soldering paste comprises the following steps of uniformly coating a layer of nano-silver particles of polyvinylpyrrolidone PVP on the surface, silver salt and glycol, wherein the nano-silver particles uniformly coated with PVP on the surface account for 70% -90% of the total mass of the raw materials, the silver salt accounts for 5% -10% of the total mass of the raw materials, and the glycol accounts for 5% -20% of the total mass of the raw materials;
the preparation method comprises the following steps:
s1: preparing a nano silver solution by using nano silver particles with PVP uniformly coated on the surfaces and ethylene glycol;
s2: grinding silver salt, adding silver salt particles into the nano-silver solution to obtain a silver salt and nano-silver mixed solution;
s3: and uniformly mixing the silver salt and nano-silver mixed solution by adopting mechanical oscillation for 15-60min to obtain uniform silver salt nano-silver composite soldering paste.
As a preferred mode, the nano silver particles with PVP uniformly wrapped on the surface are ball-like, the particle size is 50 nm-150 nm, and the PVP is used as a dispersing agent of the nano silver particles, so that the nano silver particles are independent, uniformly distributed and tightly arranged.
Preferably, the silver salt is selected from any one of silver oxalate and silver acetate.
The silver salt does not introduce N, F element, and the silver salt is not selected from silver nitrate and silver trifluoroacetate. The use of nitrogen-containing compounds breaks the N cycle balance in the environment, and causes environmental pollution. The fluorine-containing compound is easy to cause fluorine pollution, and pollutes water and soil.
Preferably, in step S3, the mechanical agitation is performed by using a screw oscillator, and the time for the uniform mixing treatment is 30 minutes and the temperature is 25 ℃.
The invention also provides silver salt nano-silver composite soldering paste obtained by the method.
The invention also provides an application of the silver salt nano silver composite soldering paste in the sintering process, which comprises the following steps: in the sintering process of the nano-silver composite soldering paste, the reducibility of glycol in the sintering process can fully reduce silver salt and silver oxide generated in the sintering process of nano-silver particles, and the glycol and the silver salt have a synergistic sintering effect, so that the oxidation degree of the nano-silver particles in the sintering process is reduced, oxides on the surfaces of the nano-silver particles are removed, and the interface bonding force between a nano-silver sintered body and a substrate is improved; meanwhile, silver salt particles reduced by glycol are filled among the nano silver particles, so that the density of the nano silver composite soldering paste sintered body is improved.
The invention also provides a sintering method of the silver salt nano-silver composite soldering paste, which comprises the following steps:
s1: coating silver salt nano silver composite soldering paste on a silver-plated copper-clad ceramic substrate in a screen printing mode;
s2: attaching the chip to silver salt nano-silver composite soldering paste to form an interconnection structure among the chip, the silver salt nano-silver composite soldering paste and the silver-plated copper-clad ceramic substrate;
s3: and placing the interconnection structure in a heating furnace for sintering, controlling the heating rate, the sintering temperature and the heat preservation time, and cooling along with the furnace to obtain the sintered connecting device.
Preferably, in step S3, the sintering temperature and the holding time are increased in steps, the holding time is divided into two stages, the first stage is at 140-160 ℃ for 30min-1h, the glycol at the temperature has reducibility, can fully reduce silver salt and oxide, and synergistically promote the sintering process; the second stage is heat preservation at 200-300 ℃ for 30min-1h, and the sintering process can be further completed.
Preferably, in step S3, the temperature increase rate is 1 ℃/min to 10 ℃/min.
Preferably, the heating furnace is one selected from a tube furnace and a constant temperature heating table.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a silver salt nano-silver composite soldering paste and a preparation method thereof, which fully reduces silver salt and silver oxide in the sintering process of the nano-silver soldering paste by utilizing the reducibility of ethylene glycol to form the synergistic effect of reducing silver salt and sintering the nano-silver soldering paste. Meanwhile, in the process of sintering the nano-silver soldering paste, silver salt particles reduced by glycol are filled among the nano-silver particles to perform a synergistic effect, so that the density of a sintered body is improved to a certain extent. The method can reduce the oxidation degree of the nano silver particles in the whole sintering process as much as possible, remove the oxide on the surfaces of the nano silver particles, and the added silver salt has no corrosion to the packaging body and has environmental protection. The oxidation degree of the sintered silver salt and the nano-silver composite soldering paste sintered body is represented by XRD, and whether the silver oxide peak appears or not and the strength of the peak are judged, so that the effective sintering of nano-silver particles is realized, the interface bonding force between the sintered body and the substrate is improved, the density of the sintered body is improved, the overall sintering temperature is reduced, and the requirements of high shear strength and low porosity of the sintered body are met. The sintered body has the characteristics of high shear strength and low porosity, the shear strength is measured by a push-pull force tester, and the porosity is quantitatively analyzed on the microscopic morphology of the sintered body through the cross section of the sintered body and MATLAB software.
Drawings
FIG. 1 is a schematic view of a temperature rise curve in the present invention;
FIG. 2 is an XRD pattern of a sintered silver salt nano-silver composite paste of the present invention;
FIG. 3 is an SEM image of a cross section of a sintered body of a silver salt nano-silver composite solder paste of the present invention;
FIG. 4 is an SEM photograph of a sintered silver salt nano-silver composite solder paste of the present invention;
FIG. 5 is a SEM image of a pore distribution diagram of a sintered silver salt nano-silver composite solder paste of the present invention after being processed by MATLAB software.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
As can be seen from fig. 3, 4 and 5, the porosity of the silver salt nano silver composite paste sintered body is less than 10%, and the nano silver particles are densely arranged and completely sintered.
Example 1
The embodiment provides a preparation method of silver salt nano-silver composite solder paste, wherein the raw materials comprise nano-silver particles, silver salt and glycol, the surfaces of the nano-silver particles are uniformly coated with a layer of polyvinylpyrrolidone PVP, the nano-silver particles are uniformly coated with PVP, the silver salt is 10% of the total mass of the raw materials, and the glycol is 20% of the total mass of the raw materials; the nano silver particles with PVP uniformly wrapped on the surface are ball-like, the particle size is 50nm, and the PVP is used as a dispersing agent for the nano silver particles. The silver salt is silver oxalate.
The preparation method comprises the following steps:
s1: preparing a nano silver solution by using nano silver particles with PVP uniformly coated on the surfaces and ethylene glycol;
s2: grinding silver oxalate salt, adding silver oxalate salt particles into a nano-silver solution to obtain a silver salt and nano-silver mixed solution;
s3: and uniformly mixing the silver salt and nano-silver mixed solution by adopting mechanical oscillation for 15-60min to obtain uniform silver salt nano-silver composite soldering paste.
In step S3, a spiral oscillator is used to perform mechanical oscillation, and the time for uniform mixing treatment is 30 minutes, and the temperature is 25 ℃.
In the sintering process of the nano-silver composite soldering paste prepared by the embodiment, the reducibility of the glycol in the sintering process can fully reduce silver salt and silver oxide generated in the sintering process of nano-silver particles, and the glycol and the silver salt perform a synergistic sintering effect, so that the oxidation degree of the nano-silver particles in the sintering process is reduced, oxides on the surfaces of the nano-silver particles are removed, and the interface bonding force between a nano-silver sintered body and a substrate is improved; meanwhile, silver salt particles reduced by glycol are filled among the nano silver particles, so that the density of the nano silver composite soldering paste sintered body is improved.
Example 2
The embodiment provides a preparation method of silver salt nano-silver composite solder paste, wherein the raw materials comprise nano-silver particles, silver salt and glycol, the surfaces of the nano-silver particles are uniformly coated with a layer of polyvinylpyrrolidone PVP, the nano-silver particles, the silver salt and the glycol are 90% of the total mass of the raw materials, the silver salt and the glycol are 5% of the total mass of the raw materials, and the PVP is uniformly coated on the surfaces of the nano-silver particles; the nano silver particles with PVP uniformly wrapped on the surface are ball-like, and the particle size is 150 nm. The silver salt is silver acetate.
The preparation method comprises the following steps:
s1: preparing a nano silver solution by using nano silver particles with PVP uniformly coated on the surfaces and ethylene glycol;
s2: grinding silver salt, adding silver salt particles into the nano-silver solution to obtain a silver salt and nano-silver mixed solution;
s3: and uniformly mixing the silver salt and nano-silver mixed solution by adopting mechanical oscillation for 15-60min to obtain uniform silver salt nano-silver composite soldering paste.
In step S3, a spiral oscillator is used to perform mechanical oscillation, and the time for uniform mixing treatment is 30 minutes, and the temperature is 25 ℃.
In the sintering process of the nano-silver composite soldering paste prepared by the embodiment, the reducibility of the glycol in the sintering process can fully reduce silver salt and silver oxide generated in the sintering process of nano-silver particles, and the glycol and the silver salt perform a synergistic sintering effect, so that the oxidation degree of the nano-silver particles in the sintering process is reduced, oxides on the surfaces of the nano-silver particles are removed, and the interface bonding force between a nano-silver sintered body and a substrate is improved; meanwhile, silver salt particles reduced by glycol are filled among the nano silver particles, so that the density of the nano silver composite soldering paste sintered body is improved.
Example 3
The embodiment provides a preparation method of silver salt nano-silver composite solder paste, wherein the raw materials comprise nano-silver particles, silver salt and glycol, the surfaces of the nano-silver particles are uniformly coated with a layer of polyvinylpyrrolidone PVP, the nano-silver particles are uniformly coated with PVP, the silver salt is 10% of the total mass of the raw materials, and the glycol is 10% of the total mass of the raw materials; the nano silver particles with PVP uniformly coated on the surface are sphere-like, and the particle size is 100 nm. The silver salt is selected from silver oxalate.
The preparation method comprises the following steps:
s1: preparing a nano silver solution by using nano silver particles with PVP uniformly coated on the surfaces and ethylene glycol;
s2: grinding silver salt, adding silver salt particles into the nano-silver solution to obtain a silver salt and nano-silver mixed solution;
s3: and uniformly mixing the silver salt and nano-silver mixed solution by adopting mechanical oscillation for 15-60min to obtain uniform silver salt nano-silver composite soldering paste.
In step S3, a spiral oscillator is used to perform mechanical oscillation, and the time for uniform mixing treatment is 30 minutes, and the temperature is 25 ℃.
In the sintering process of the nano-silver composite soldering paste prepared by the embodiment, the reducibility of the glycol in the sintering process can fully reduce silver salt and silver oxide generated in the sintering process of nano-silver particles, and the glycol and the silver salt perform a synergistic sintering effect, so that the oxidation degree of the nano-silver particles in the sintering process is reduced, oxides on the surfaces of the nano-silver particles are removed, and the interface bonding force between a nano-silver sintered body and a substrate is improved; meanwhile, silver salt particles reduced by glycol are filled among the nano silver particles, so that the density of the nano silver composite soldering paste sintered body is improved.
Example 4
The embodiment provides a sintering method of silver salt nano-silver composite soldering paste, which comprises the following steps:
s1: coating the silver salt nano silver composite soldering paste obtained in the embodiment 1 on a silver-plated copper-clad ceramic substrate in a screen printing mode;
s2: attaching the chip to silver salt nano-silver composite soldering paste to form an interconnection structure among the chip, the silver salt nano-silver composite soldering paste and the silver-plated copper-clad ceramic substrate;
s3: and (2) placing the interconnection structure in a heating furnace for sintering, and controlling the heating rate, the sintering temperature and the heat preservation time, wherein the sintering temperature and the heat preservation time are increased in a step manner, and the heating furnace is a tubular furnace as shown in figure 1. The heating rate is 1 ℃/min, the heat preservation time is divided into two sections, the first section is heat preservation for 1h at 140 ℃, glycol at the temperature has reducibility, can fully reduce silver salt and oxide, and synergistically promote the sintering process; the second stage is heat preservation at 200 ℃ for 45min, and the sintering process can be further completed. And cooling along with the furnace to obtain the sintered connecting device.
The sintered connecting device prepared in this example was subjected to a shear strength test on a push-pull force tester, and the shear strength of the connecting device was found to be 31.52 MPa.
The microstructure of the sintered finished connector cross-section prepared in this example was analyzed quantitatively using MATLAB to determine a porosity of the connected layer of 7.13%.
Example 5
The embodiment provides a sintering method of silver salt nano-silver composite soldering paste, which comprises the following steps:
s1: coating the silver salt nano silver composite soldering paste obtained in the embodiment 2 on a silver-plated copper-clad ceramic substrate in a screen printing mode;
s2: attaching the chip to silver salt nano-silver composite soldering paste to form an interconnection structure among the chip, the silver salt nano-silver composite soldering paste and the silver-plated copper-clad ceramic substrate;
s3: and placing the interconnection structure in a heating furnace for sintering, and controlling the heating rate, the sintering temperature and the heat preservation time, wherein the heating furnace is a constant-temperature heating table. The sintering temperature and the holding time are increased in steps, as shown in FIG. 1, and the heating rate is 10 ℃/min. The heat preservation time is divided into two sections, the first section is heat preservation for 30min at 160 ℃, glycol at the temperature has reducibility, so that silver salt and oxide can be fully reduced, and the sintering process is synergistically promoted; the second stage is heat preservation at 300 ℃ for 30min, and the sintering process can be further completed. And cooling along with the furnace to obtain the sintered connecting device.
The sintered connecting device prepared in this example was subjected to a shear strength test on a push-pull force tester, and the shear strength of the connecting device was found to be 29.78 MPa.
The microstructure of the sintered connector cross-section prepared in this example was analyzed quantitatively using MATLAB to determine a porosity of the connector layer of 7.57%.
Example 6
The embodiment provides a sintering method of silver salt nano-silver composite soldering paste, which comprises the following steps:
s1: coating the silver salt nano silver composite soldering paste obtained in the embodiment 3 on a silver-plated copper-clad ceramic substrate in a screen printing mode;
s2: attaching the chip to silver salt nano-silver composite soldering paste to form an interconnection structure among the chip, the silver salt nano-silver composite soldering paste and the silver-plated copper-clad ceramic substrate;
s3: and (3) placing the interconnection structure in a heating furnace for sintering, and controlling the heating rate, the sintering temperature and the heat preservation time, wherein the sintering temperature and the heat preservation time are increased in a step manner, as shown in figure 1. The heating furnace is a tube furnace. The heating rate is 5 ℃/min, the heat preservation time is divided into two sections, the first section is heat preservation for 45min at 150 ℃, glycol at the temperature has reducibility, can fully reduce silver salt and oxide, and synergistically promote the sintering process; the second stage is heat preservation for 1h at 250 ℃. The sintering process can be further completed. And cooling along with the furnace to obtain the sintered connecting device.
The sintered connecting device prepared in this example was subjected to a shear strength test on a tensile tester, and the shear strength of the connecting device was measured to be 31.84 MPa.
The microstructure of the sintered finished connector cross-section prepared in this example was analyzed quantitatively using MATLAB to determine a porosity of the connected layer of 8.04%.
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 (9)

1. A preparation method of silver salt nano-silver composite soldering paste is characterized by comprising the following steps: the raw materials comprise nano silver particles, silver salt and glycol, wherein the surface of the nano silver particles is uniformly coated with a layer of polyvinylpyrrolidone (PVP), the nano silver particles are uniformly coated with PVP, the nano silver particles are 70-90% of the total mass of the raw materials, the silver salt is 5-10% of the total mass of the raw materials, and the glycol is 5-20% of the total mass of the raw materials;
the preparation method comprises the following steps:
s1: preparing a nano silver solution by using nano silver particles with PVP uniformly coated on the surfaces and ethylene glycol;
s2: grinding silver salt, adding silver salt particles into the nano-silver solution to obtain a silver salt and nano-silver mixed solution;
s3: and uniformly mixing the silver salt and nano-silver mixed solution by adopting mechanical oscillation for 15-60min to obtain uniform silver salt nano-silver composite soldering paste.
2. The method for producing a silver salt nano-silver composite solder paste according to claim 1, characterized in that: the nano silver particles with PVP uniformly wrapped on the surface are ball-like, the particle size is 50 nm-150 nm, and the PVP is used as a dispersing agent for the nano silver particles.
3. The method for producing a silver salt nano-silver composite solder paste according to claim 1, characterized in that: the silver salt is selected from any one of silver oxalate and silver acetate.
4. The method for producing a silver salt nano-silver composite solder paste according to claim 1, characterized in that: in step S3, a spiral oscillator is used to perform mechanical oscillation, and the time for uniform mixing treatment is 30 minutes, and the temperature is 25 ℃.
5. Silver salt nano silver composite solder paste obtained by the method of any one of claims 1 to 4.
6. The use of the silver salt nano silver composite solder paste according to claim 5 in a sintering process, characterized in that: in the sintering process of the nano-silver composite soldering paste, the reducibility of glycol in the sintering process can fully reduce silver salt and silver oxide generated in the sintering process of nano-silver particles, and the glycol and the silver salt have a synergistic sintering effect, so that the oxidation degree of the nano-silver particles in the sintering process is reduced, oxides on the surfaces of the nano-silver particles are removed, and the interface bonding force between a nano-silver sintered body and a substrate is improved; meanwhile, silver salt particles reduced by glycol are filled among the nano silver particles, so that the density of the nano silver composite soldering paste sintered body is improved.
7. The method of sintering a silver salt nano-silver composite solder paste according to claim 5, characterized by comprising the steps of:
s1: coating silver salt nano silver composite soldering paste on a silver-plated copper-clad ceramic substrate in a screen printing mode;
s2: attaching the chip to silver salt nano-silver composite soldering paste to form an interconnection structure among the chip, the silver salt nano-silver composite soldering paste and the silver-plated copper-clad ceramic substrate;
s3: and placing the interconnection structure in a heating furnace for sintering, controlling the heating rate, the sintering temperature and the heat preservation time, and cooling along with the furnace to obtain the sintered connecting device.
8. The method of sintering a silver salt nanosilver composite solder paste according to claim 7, characterized in that: in step S3, the sintering temperature and the heat preservation time are increased in a step manner, the heat preservation time is divided into two sections, the first section is at 140-160 ℃ and is kept for 30min-1h, and the second section is at 200-300 ℃ and is kept for 30min-1 h.
9. The method of sintering a silver salt nanosilver composite solder paste according to claim 7, characterized in that: in step S3, the temperature rise rate is 1-10 deg.C/min.
CN202210177520.4A 2022-02-24 2022-02-24 Silver salt nano silver composite soldering paste, preparation method, sintering method and application Active CN114310038B (en)

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CN113977130A (en) * 2021-11-24 2022-01-28 广东中实金属有限公司 High-temperature-resistant soldering paste capable of being sintered at low temperature under no pressure and preparation method and use method thereof

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