CN113977130B - High-temperature-resistant soldering paste capable of being sintered at low temperature under no pressure and preparation method and use method thereof - Google Patents
High-temperature-resistant soldering paste capable of being sintered at low temperature under no pressure and preparation method and use method thereof Download PDFInfo
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- CN113977130B CN113977130B CN202111407853.3A CN202111407853A CN113977130B CN 113977130 B CN113977130 B CN 113977130B CN 202111407853 A CN202111407853 A CN 202111407853A CN 113977130 B CN113977130 B CN 113977130B
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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
- 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 preparation method of high-temperature-resistant soldering paste capable of being sintered at low temperature without pressure, which comprises the following steps: and mixing the soldering flux with 4:5 in volume ratio and a dispersion liquid to obtain the soldering paste, wherein the dispersion liquid comprises 150 to 200nm copper nanoparticles and 10 to 15nm copper-nickel alloy nanoparticles, and the mass ratio of the copper nanoparticles to the copper-nickel alloy nanoparticles is 5:2. According to the invention, copper-nickel alloy nanoparticles with the particle size of 10 to 15nm are compounded with copper nanoparticles with the particle size of 150 to 200nm, so that large-size particles are used as a support, small-size particles are filled into gaps to be used as an adhesive, the porosity is effectively reduced, the density of a sintered layer is improved, the bonding temperature is reduced, and the pressureless low-temperature sintering is realized; meanwhile, the copper-nickel alloy nanoparticles accounting for 29 wt% of Cu and 71 wt% of Ni are adopted, so that the small-size copper particles can be effectively prevented from being oxidized to form a copper oxide film layer in the sintering process, the melting temperature is increased, the compatibility is poor, and the copper-nickel alloy nanoparticles have excellent oxidation stability.
Description
Technical Field
The invention relates to a high-temperature-resistant soldering paste capable of being sintered at low temperature without pressure, a preparation method and a use method thereof, belonging to the technical field of high-performance soldering paste.
Background
In recent years, miniaturized and integrated third-generation semiconductor devices are gradually applied to the field of severe environments such as aerospace, automobiles and the like, and although the use temperature of potential raw materials of the third-generation semiconductor devices, such as silicon carbide and gallium nitride, can be above 200 ℃ and even can work at 350 ℃ for a long time, the overhigh use temperature far exceeds the temperature of the traditional connecting materials. At present, the traditional connecting materials mainly comprise tin-based, lead-based, bismuth-based, gold-based, zinc-based and other solders, the tin-based lead-free solder has a lower melting point, is remelted in the using process and cannot be applied at high temperature; other high melting point lead-based, bismuth-based, gold-based, and zinc-based solders have their own disadvantages, including environmental damage, high cost, high process temperatures, and poor electrical conductivity. Therefore, it becomes important to develop a connecting material capable of withstanding high temperatures.
The use of metal nanoparticles as solder for third generation semiconductors is by far the most promising connection technology, which can achieve the functions of low temperature connection, high temperature service. Due to the small size effect of the metal nanoparticles, the melting point of the metal nanoparticles is much lower than that of the bulk metal, which has significant advantages over conventional solders, including environmental protection, high heat resistance, no lead, high electrical and thermal conductivity, etc.
Among them, low temperature bonding of silver nanoparticles has been reported. However, practical application of silver nanoparticles as a connection material is limited due to severe electromigration and high cost. Since copper is cheaper than silver (the cost is one percent of silver), and has good ion mobility, and the electrical property and the thermal property of copper are equivalent to those of silver, the copper nanoparticles show huge application potential as a low-temperature connecting material.
However, when the copper nanoparticles are used as a soldering paste in a melting mode, the porosity among the particles is large, the stacking density of a sintering layer is low, the sintering temperature is high, bonding is difficult under a non-pressure condition, and the semiconductor chip can be damaged by high temperature and high pressure.
Disclosure of Invention
The invention aims to provide a high-temperature-resistant soldering paste capable of being sintered at low temperature without pressure, a preparation method and a use method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of a high-temperature resistant soldering paste capable of being sintered at low temperature under no pressure comprises the following steps:
and mixing the soldering flux with 4:5 in volume ratio and a dispersion liquid to obtain the soldering paste, wherein the dispersion liquid comprises 150 to 200nm copper nanoparticles and 10 to 15nm copper-nickel alloy nanoparticles, and the mass ratio of the copper nanoparticles to the copper-nickel alloy nanoparticles is 5:2.
Further, the soldering flux is a mixture of polyethylene glycol and C18 alcohol, and the molar ratio of the polyethylene glycol to the C18 alcohol is 2~5.
Further, the soldering flux is a mixture of isopropanol and diethylene glycol butyl ether, and the molar ratio of the isopropanol to the diethylene glycol butyl ether is 2~5.
Furthermore, in the nanoparticles of the copper-nickel alloy, the weight ratio of copper element to nickel element is
。
The invention also provides a technical scheme that: a high-temperature resistant soldering paste capable of being sintered at low temperature without pressure is prepared by the method.
The invention also provides a technical scheme that: a method of using a pressureless low-temperature sinterable high temperature resistant solder paste, the method comprising:
a1: polishing the bottom surface of the substrate by using sand paper, and respectively carrying out ultrasonic cleaning in hydrochloric acid and absolute ethyl alcohol;
a2: coating the prepared high-temperature-resistant soldering paste on the surface of the bottom surface of the substrate, and sintering by using a hot-pressing sintering machine under no pressure, wherein the sintering temperature is 200-250 ℃, and the sintering time is 10-30min.
Further, the substrate is a copper substrate.
The invention also provides a technical scheme that: a method of making copper-nickel alloy nanoparticles, the method comprising the steps of:
s1: mixing 30 moles of oleylamine and 1.7 moles of copper acetylacetonate, and heating at the temperature of 180-220 ℃ for 0.5-1.5 h;
s2: cooling the mixture obtained in the step S1 to 15-35 ℃ to form a nano copper dispersion, adding 41.7-50.5 mmol of nickel chloride and 2.4 mmol of reducing agent, and heating in an inert gas atmosphere at the temperature of 180-220 ℃ for 0.5-1.5 h;
s3: adding a pH regulator to regulate the pH to 13 to 15, heating to 45 to 55 ℃, and keeping the temperature for 10 to 15min;
s4: and finally, carrying out centrifugal separation on the colloidal dispersion obtained in the step S3, wherein the centrifugal rotation speed is 1000 to 2000rpm, the separation time is 2 to 3min, and removing the solution to obtain copper-nickel alloy nanoparticles of 10 to 15nm.
Further, the reducing agent is one or more of trioctylphosphine and triphenylphosphine.
Further, the pH regulator is one or more of hydrazine hydrate and tetrabutyl borohydride.
Further, the reducing agent is trioctylphosphine, the pH regulator is hydrazine hydrate, and the molar ratio of the trioctylphosphine to the hydrazine hydrate is 1 to 2.6: 2~6.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
1. according to the high-temperature-resistant soldering paste capable of being sintered at a low temperature and a preparation method and a using method thereof, the copper nanoparticles are used as the main solder, and the polyethylene glycol and the C18 alcohol are matched, so that the soldering paste is not remelted at a high temperature, the connecting effect of an electronic component and a substrate is ensured, the connecting surface of the substrate and the electronic component can be well infiltrated, and the connecting strength is improved; in addition, the soldering paste is easy to clean and convenient to remove.
2. According to the high-temperature-resistant welding paste capable of being sintered at a low temperature under no pressure and the preparation method and the using method thereof, copper nickel alloy nanoparticles of 10-15nm are compounded with copper nanoparticles of 150-200nm, so that large-size particles are used as a support, small-size particles are filled into gaps to be used as an adhesive, the void ratio is effectively reduced, the density of a sintered layer is improved, the bonding temperature is reduced, and the low-temperature sintering without pressure is realized; meanwhile, the weight ratio of copper element to nickel element is adopted as
The copper-nickel alloy nano particles have excellent oxidation stability, and can effectively avoid the phenomenon that small-size copper particles are oxidized to form a copper oxide film layer in the sintering process, so that the melting temperature is increased and the compatibility is poor; in addition, the nickel can also improve the binding force and the binding strength of the substrate and the sintered copper particles, thereby improving the connecting effect of the soldering paste.
3. The invention relates to a high-temperature-resistant soldering paste capable of being sintered at a low temperature under no pressure and a preparation method and a using method thereof.A liquid phase reduction method is used for preparing copper-nickel alloy nanoparticles, trioctylphosphine and hydrazine hydrate are added, the molar ratio of the trioctylphosphine and the hydrazine hydrate is controlled, and the size of a crystal grain is artificially controlled to obtain the copper-nickel alloy nanoparticles of 10 to 15nm; in addition, trioctylphosphine is not only used as a reducing agent, but also catalyzes the reaction, and improves the reaction rate; the hydrazine hydrate used in cooperation is oxidized into nitrogen in the reduction process to overflow a reaction system, so that impurities cannot be brought to reaction products, and meanwhile, the hydrazine hydrate can reduce carbonyl into methylene and can perform catalytic reduction under the action of a catalyst.
Drawings
FIG. 1 is a microscopic view of the Cu-Ni alloy nanoparticles prepared by the present invention;
FIG. 2 is an XRD pattern of the copper-nickel alloy nanoparticles prepared by the invention.
Detailed Description
Example 1: a method of making copper-nickel alloy nanoparticles, the method comprising the steps of:
s1: mixing 30 moles of oleylamine oleate and 1.7 moles of copper acetylacetonate, and heating at 180 ℃ for 0.5h;
s2: cooling the mixture obtained in the step S1 to 15 ℃ to form a nano copper dispersion, adding 41.7 mmol of nickel chloride and 2.4 mmol of trioctylphosphine serving as a reducing agent, and heating in a nitrogen atmosphere at the temperature of 180 ℃ for 0.5h;
s3: then 5.6 millimole of hydrazine hydrate is added to adjust the pH value to 14, the temperature is raised to 45 ℃, and the temperature is kept for 10min;
s4: and finally, carrying out centrifugal separation on the colloidal dispersion obtained in the step S3, wherein the centrifugal rotation speed is 1000rpm, the separation time is 2min, and removing the solution to obtain the copper-nickel alloy nanoparticles with the particle size of 10-15nm.
Example 2: a method of making copper-nickel alloy nanoparticles, the method comprising the steps of:
s1: mixing and heating 30 moles of oleylamine oleate and 1.7 moles of copper acetylacetonate at the temperature of 200 ℃ for 1 hour;
s2: cooling the mixture obtained in the step S1 to 15 ℃ to form a nano copper dispersion, adding 45 mmol of nickel chloride and 2.4 mmol of trioctylphosphine serving as a reducing agent, and heating in a nitrogen atmosphere at 200 ℃ for 1h;
s3: adding 5.6 mmol hydrazine hydrate to adjust pH to 14, heating to 50 deg.C, and maintaining for 13min;
s4: and finally, carrying out centrifugal separation on the colloidal dispersion obtained in the step S3, wherein the centrifugal rotation speed is 1500rpm, the separation time is 2.5min, and removing the solution to obtain copper-nickel alloy nanoparticles with the particle size of 10-15nm.
Example 3: a method of making copper-nickel alloy nanoparticles, the method comprising the steps of:
s1: mixing 30 moles of oleylamine oleate and 1.7 moles of copper acetylacetonate, and heating at 220 ℃ for 1.5 hours;
s2: cooling the mixture obtained in the step S1 to 15 ℃ to form a nano copper dispersion, adding 50.5 mmol of nickel chloride and 2.4 mmol of reducing agent triphenylphosphine, and heating in a nitrogen atmosphere at 220 ℃ for 1.5h;
s3: then adding 5.6 millimoles of tetrabutyl borohydride to adjust the pH value to 14, heating to 45 ℃, and preserving the temperature for 10min;
s4: and finally, performing centrifugal separation on the colloidal dispersion obtained in the step S3, wherein the centrifugal rotation speed is 1000rpm, the separation time is 2min, and removing the solution to obtain copper-nickel alloy nanoparticles with the particle size of 10 to 15nm.
Example 4: a preparation method of high-temperature-resistant soldering paste capable of being sintered at low temperature without pressure comprises the following steps:
mixing the soldering flux with the volume ratio of 4:5 and a dispersion liquid to obtain a soldering paste, wherein the dispersion liquid comprises 150 to 200nm copper nanoparticles and 10 to 15nm copper-nickel alloy nanoparticles, and the mass ratio of the copper nanoparticles to the copper-nickel alloy nanoparticles is 5:2; the soldering flux is a mixture of polyethylene glycol and C18 alcohol, the molar ratio of the polyethylene glycol to the C18 alcohol is 2~5, and 3 is preferred; in the nanoparticles of the copper-nickel alloy, the weight ratio of copper element to nickel element is
. The copper-nickel alloy nanoparticles 10 to 15nm were prepared by the method described in any one of examples 1~3.
Example 5: a preparation method of high-temperature-resistant soldering paste capable of being sintered at low temperature without pressure comprises the following steps:
mixing the soldering flux with 4:5 in volume ratio and a dispersion liquid to obtain the soldering paste, wherein the dispersion liquid comprises 150 to 200nm copper nanoparticles and 10 to 15nm copper-nickel alloy nanoparticles, and the soldering paste is prepared from the soldering flux and the dispersion liquidThe mass ratio of the copper nanoparticles to the copper-nickel alloy nanoparticles is 5:2; the soldering flux is a mixture of isopropanol and diethylene glycol butyl ether, the molar ratio of the isopropanol to the diethylene glycol butyl ether is 2~5, and 3 is preferred; in the nanoparticles of the copper-nickel alloy, the weight ratio of copper element to nickel element is
。
Wherein, the copper-nickel alloy nano particles with the particle size of 10 to 15nm are prepared by the method of any embodiment of 1~3.
Example 6: a pressureless low temperature sinterable high temperature solder paste made by the method of any of embodiments 4~5.
Example 7: a method of using a pressureless low-temperature sinterable high temperature resistant solder paste, the method comprising:
a1: polishing the bottom surface of the substrate by using sand paper, and respectively carrying out ultrasonic cleaning in hydrochloric acid and absolute ethyl alcohol;
a2: the high temperature resistant solder paste prepared in example 4~5 was coated on the surface of the bottom surface of the substrate and sintered without pressure using a hot press sintering machine at a sintering temperature of 200-250 ℃ for 10-30min.
Here, the substrate is a copper substrate.
By adopting the scheme, the copper nanoparticles are used as the main solder, and the polyethylene glycol and the C18 alcohol are matched, so that the solder paste does not have the remelting phenomenon at high temperature, the connection effect of the electronic component and the substrate is ensured, the connection surface of the substrate and the electronic component can be well infiltrated, and the connection strength is improved; in addition, the soldering paste is easy to clean and convenient to remove.
Copper nickel alloy nanoparticles of 10-15nm are compounded with copper nanoparticles of 150-200nm, large-size particles are used as a support, small-size particles are filled into gaps and used as an adhesive, the void ratio is effectively reduced, the density of a sintering layer is improved, the bonding temperature is reduced, and the pressureless low-temperature sintering is realized; meanwhile, the copper-nickel alloy nanoparticles of 29 wt% Cu and 71 wt% Ni have excellent oxidation stability, and can effectively avoid the phenomenon that small-size copper particles are oxidized to form a copper oxide film layer in the sintering process, so that the melting temperature is increased and the compatibility is poor; in addition, the nickel can also improve the binding force and the binding strength of the substrate and the sintered copper particles, thereby improving the connecting effect of the soldering paste.
Preparing copper-nickel alloy nanoparticles by a liquid phase reduction method, adding trioctylphosphine and hydrazine hydrate, controlling the molar ratio of the copper-nickel alloy nanoparticles and the hydrazine hydrate, and manually controlling the size of crystal grains to obtain the copper-nickel alloy nanoparticles with the particle size of 10 to 15nm; in addition, trioctylphosphine is used as a reducing agent, and catalyzes the reaction, so that the reaction rate is improved.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (3)
1. A preparation method of high-temperature-resistant soldering paste capable of being sintered at low temperature without pressure is characterized by comprising the following steps:
mixing the soldering flux with the volume ratio of 4:5 and a dispersion liquid to obtain a soldering paste, wherein the dispersion liquid comprises 150 to 200nm copper nanoparticles and 10 to 15nm copper-nickel alloy nanoparticles, and the mass ratio of the copper nanoparticles to the copper-nickel alloy nanoparticles is 5:2;
the soldering flux is a mixture of polyethylene glycol and C18 alcohol, and the molar ratio of the polyethylene glycol to the C18 alcohol is 2~5; in the copper-nickel alloy nano particles, the weight ratio of copper element to nickel element is
；
The preparation process of the copper-nickel alloy nanoparticles comprises the following steps:
s1: mixing 30 moles of oleylamine and 1.7 moles of copper acetylacetonate, and heating at 180-220 ℃ for 0.5-1.5 h;
s2: cooling the mixture obtained in the step S1 to 15-35 ℃ to form a nano copper dispersion, adding 41.7-50.5 mmol of nickel chloride and 2.4 mmol of trioctylphosphine serving as a reducing agent, and heating in an inert gas atmosphere at the temperature of 180-220 ℃ for 0.5-1.5 h;
s3: adding hydrazine hydrate serving as a pH regulator to regulate the pH to 13 to 15, heating to 45 to 55 ℃, and keeping the temperature for 10 to 15min; wherein the molar ratio of the trioctylphosphine to the hydrazine hydrate is 1 to 2.6: 2~6;
s4: and finally, carrying out centrifugal separation on the colloidal dispersion obtained in the step S3, wherein the centrifugal rotation speed is 1000 to 2000rpm, the separation time is 2 to 3min, and removing the solution to obtain copper-nickel alloy nanoparticles of 10 to 15nm.
2. A high temperature resistant solder paste sinterable at pressureless low temperatures, characterized by being produced by the process of claim 1.
3. A method for using a high temperature resistant solder paste capable of pressureless low temperature sintering, the method comprising:
a1: polishing the bottom surface of the substrate by using abrasive paper, and respectively carrying out ultrasonic cleaning in hydrochloric acid and absolute ethyl alcohol;
a2: the high temperature resistant solder paste prepared in claim 1 is coated on the surface of the bottom surface of the substrate and is sintered without pressure using a hot pressing sintering machine, the sintering temperature is 200-250 ℃, and the sintering time is 10-30min.
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| CN114850726B (en) * | 2022-06-10 | 2023-04-28 | 郑州机械研究所有限公司 | Nickel core coating brazing material, preparation method thereof and brazing method |
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| JP2011054892A (en) * | 2009-09-04 | 2011-03-17 | Nihon Superior Co Ltd | Solder bonding using conductive paste |
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