CN110508973B - High-temperature service soldering paste realized by doping nano particles and preparation method thereof - Google Patents
High-temperature service soldering paste realized by doping nano particles and preparation method thereof Download PDFInfo
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- CN110508973B CN110508973B CN201910855450.1A CN201910855450A CN110508973B CN 110508973 B CN110508973 B CN 110508973B CN 201910855450 A CN201910855450 A CN 201910855450A CN 110508973 B CN110508973 B CN 110508973B
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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
- B23K35/362—Selection of compositions of fluxes
Abstract
The invention belongs to a nano-particle doped high-temperature service soldering paste, which is particularly suitable for application of a service temperature higher than 270 ℃ after welding, and comprises tin alloy, nano metal, rare earth alloy and soldering paste, wherein the tin alloy powder is one or a mixture of two of tin-silver alloy powder, tin-antimony alloy powder and tin-copper alloy powder; the nano metal powder is one or a mixture of copper powder, nickel powder, titanium powder, cobalt powder and gold powder; the effective components of the flux paste comprise hydrogenated rosin, diethylene glycol monohexyl ether, succinic acid, methyl benzotriazole and citric acid; the manufacturing method comprises the steps of preparing tin alloy powder, nano metal powder, rare earth alloy powder, soldering paste and mixing.
Description
Technical Field
The invention belongs to a solder paste for realizing high-temperature service by doping nano particles and a preparation method thereof, and is particularly suitable for application of the service temperature of more than 270 ℃ after welding.
Background
Along with the high speed of communication equipment and the high density of integrated circuits, the complexity of semiconductor devices is higher and higher, higher requirements are put forward on packaging technology, along with the expansion of multi-stage packaging, Printed Circuit Boards (PCBs) can be welded for multiple times, in order to improve the production speed, after the A surface is welded for the first time, when B surface welding is carried out next time, the temperature of the PCBs is higher and is usually above 240 ℃, when soldering paste with low service melting point (usually 216 ℃) is adopted, because the temperature of the PCBs is higher than that of the soldering paste with low melting point during the secondary (or multiple) welding, the soldered soldering paste with low service melting point of the A surface can be melted again, the soldered A surface is not welded really, the welding quality is seriously influenced, and the product performance is reduced; when the soldering paste with high service melting point is adopted, the melting point requirement of the soldering paste is high, the technical problem that the soldered A-surface soldering paste is not easy to melt during secondary (or multiple) soldering is solved, but the first A-surface soldering requires high melting point and is high in cost. In the prior art, the solder paste can not completely meet the requirements, or has high cost, or can not reach the performance, or has narrow application range.
Disclosure of Invention
The invention aims to solve the technical problem of providing a nano-particle doped high-temperature service solder paste, and solving the technical problem that the existing solder paste has low welding melting point and high melting point under the condition of high service temperature.
In order to solve the technical problems, the invention provides a nano-particle doped high-temperature service solder paste, which comprises tin alloy powder, nano metal powder, rare earth alloy powder and a soldering paste, wherein the tin alloy powder is one or a mixture of two of tin-silver alloy powder, tin-antimony alloy powder and tin-copper alloy powder; the nano metal powder is one or a mixture of copper powder, nickel powder, titanium powder, cobalt powder and gold powder; the effective components of the flux paste comprise hydrogenated rosin, diethylene glycol monohexyl ether, succinic acid, methyl benzotriazole and citric acid.
Further, the tin alloy powder also comprises tin-lead alloy powder.
Further, in the tin alloy powder, 1 to 98 mass% of tin: 0-95% of lead and 0.5-5% of silver: 0.01% -1% of copper: 5 to 30 percent of stibium.
Further, the nano metal powder is defined as containing 2-60% of copper by mass percent: 0.5% -15% of nickel: 0.1-5% of titanium: 0.1-5% of cobalt: 0.1 to 10 percent of gold.
Further, in the rare earth alloy powder, according to the mass percentage, the rare earth alloy powder is 0.01% -2%: 98-99.9 percent of nano metal powder.
Further, the flux paste is limited to have a mass percentage of 3% -8% of hydrogenated rosin: 1-6% of diethylene glycol monohexyl ether: succinic acid 0.1-0.8 wt%, methyl benzotriazole 0.03-0.1 wt% and citric acid 0.01-0.2 wt%.
The invention also provides a preparation method of the solder paste for realizing high-temperature service by doping nano particles, which solves the problem that the preparation method of the solder paste has low welding melting point and is suitable for high melting point under the condition of high service temperature.
In order to solve the technical problems, the invention provides a preparation method of a nano-particle doped high-temperature service solder paste, which comprises the following steps,
step one, preparing tin alloy powder, wherein the step of preparing the tin alloy powder comprises preparing tin-silver alloy powder, tin-copper alloy powder and tin-antimony alloy powder, and comprises the following specific steps,
a. adding raw materials for smelting the tin-silver master alloy into an intermediate frequency furnace through a feed inlet according to the tin-silver ratio of 3:7 in percentage by mass, setting the temperature of the intermediate frequency furnace at 1100-1200 ℃, inclining the furnace body after the temperature is reached, pouring the prepared master alloy into a stainless steel container, and cooling for later use;
b. adding raw materials for smelting a tin-copper master alloy into an intermediate frequency furnace through a feed inlet according to the tin-copper ratio of 1:10 in percentage by mass, setting the temperature of the intermediate frequency furnace at 1100-1200 ℃, pouring the prepared master alloy into a stainless steel container, and cooling for later use;
c. adding raw materials for smelting a tin-antimony master alloy into a vacuum furnace through a feeding hole according to the tin-antimony ratio of 1:10 in percentage by mass, setting the temperature of the vacuum furnace at 650-800 ℃, pouring the prepared master alloy into a stainless steel container, and cooling for later use;
d. pouring one or two of the master alloys obtained in the steps a, b and c into a stainless steel container, fully mixing the master alloys with 10 mass percent of tin powder at the temperature of 200-300 ℃, stirring for 60 minutes, standing for 180 minutes to prepare an alloy for later use;
e. when the temperature is reduced to 150-;
f. the alloy is processed by powder atomization molding equipment and classified screening to prepare tin alloy powder for later use;
step two, preparing nano metal powder,
g. one of copper, nickel, titanium, cobalt and gold is smelted or a plurality of materials are smelted into alloy, and the alloy is prepared into nano metal powder for standby through centrifugal grading screening by nano powder forming equipment;
step three, preparing rare earth alloy powder,
h. passing the rare earth alloy through powder forming equipment, and preparing rare earth alloy powder for later use through graded screening;
step four, preparing the flux paste,
i. preparing the flux paste: adding 3-8% of hydrogenated rosin into a reaction kettle, stirring and melting at 120-140 ℃, adding 1-6% of diethylene glycol monohexyl ether, uniformly stirring, cooling to 80-110 ℃, adding 0.1-0.8% of succinic acid and 0.03-0.1% of methyl benzotriazole, uniformly stirring, cooling to 40-50 ℃, adding 0.01-0.2% of citric acid, uniformly stirring, cooling to room temperature, and preparing into a backup solder paste;
step five, stirring and mixing the components to form solder paste,
j. and sequentially adding the prepared flux paste, tin alloy powder, nano metal (or alloy) powder and rare earth alloy powder into a full-automatic planetary stirrer, uniformly stirring under a vacuum condition, subpackaging, and storing at 2-10 ℃.
Further, the preparation method for realizing the high-temperature service solder paste by limiting the doping of the nano particles comprises the first step of preparing tin alloy powder, and the preparation method further comprises the following specific steps of: 37, adding the raw materials for smelting the tin-lead master alloy into an intermediate frequency furnace through a feed inlet, setting the temperature of the intermediate frequency furnace at 1300-1400 ℃, inclining the furnace body after reaching the temperature, pouring the prepared master alloy into a stainless steel container, and cooling for later use.
Furthermore, the size of the tin alloy powder for limiting the preparation method of the nano-particle doped solder paste for realizing high-temperature service has seven specifications, wherein the 1# is 75-150 um, the 2# is 45-75 um, the 3# is 25-45 um, the 4# is 20-38 um, the 5# is 10-20 um, the 6# is 5-15 um, and the 7# is 2-12 um.
Further, the preparation method for realizing the high-temperature service solder paste by limiting the doping of the nano particles comprises the following steps: according to the mass percentage, the content of the nano metal powder is 3% -60%, and the particle size range is 2-100 nm.
By adopting the technical scheme, the nano-particle doped high-temperature service solder paste is prepared by adding a certain proportion of nano simple substance metal particles or alloy particles into the solder paste and adding corresponding nano auxiliary additives, so that the preparation cost is lower than that of nano solder paste, the nano solder paste is easy to realize, and the application range is wider; by adopting the technical scheme, the preparation method of the high-temperature service solder paste by doping the nano particles is characterized in that the nano simple substance metal particles or alloy particles are added into the solder paste in a certain proportion, and the corresponding nano auxiliary additive is added, so that the application that the service temperature is higher than 300 ℃ after welding is achieved, the preparation cost is lower than that of nano solder paste, the service temperature is higher than that of the conventional high-temperature solder paste, the preparation method is easy to realize, and the application range is wider.
Detailed Description
Example 1
Taking 30 g of tin metal material and 70 g of silver metal material, adding the materials into an intermediate frequency furnace through a feeding hole, setting the temperature of the intermediate frequency furnace at 1100-1200 ℃, inclining the furnace body after reaching the temperature, pouring the prepared master alloy into a stainless steel container, and cooling for later use;
pouring the master alloy obtained in the step into a stainless steel container, fully mixing the master alloy with 1000 g of tin powder at the temperature of 200-300 ℃, stirring for 60 minutes, and standing for 180 minutes to prepare an alloy for later use;
when the temperature is reduced to 150-;
the alloy is processed by powder atomization molding equipment and classified screening to prepare tin alloy powder for later use;
then 25 g of copper and 0.8 g of nickel are melted into alloy, and the alloy is prepared into nano metal powder for standby through centrifugal grading screening by nano powder forming equipment;
then 0.15 g of rare earth alloy passes through powder forming equipment, and is prepared into rare earth alloy powder for later use through grading screening.
Starting to manufacture the soldering paste, adding 40 g of hydrogenated rosin into a reaction kettle, stirring and melting at 120-140 ℃, adding 16 g of diethylene glycol monohexyl ether, uniformly stirring, cooling to 80-110 ℃, adding 1.5 g of succinic acid and 5 g of methyl benzotriazole, uniformly stirring, cooling to 40-50 ℃, adding 1.5 g of citric acid, uniformly stirring, and cooling to room temperature to prepare the soldering paste for later use;
and finally, sequentially adding 1030 g of tin metal material, 70 g of silver metal material, 8 g of potassium metal powder, 25 g of copper powder, 0.15 g of rare earth alloy and soldering paste prepared from 40 g of hydrogenated rosin, 16 g of diethylene glycol monohexyl ether, 1.5 g of succinic acid, 5 g of methyl benzotriazole and 1.5 g of citric acid into a full-automatic planetary stirrer, uniformly stirring under a vacuum condition, subpackaging and storing at the temperature of 2-10 ℃.
Example 2
Taking 10 g of tin metal material and 100 g of copper metal material, adding the tin metal material and the copper metal material into an intermediate frequency furnace through a feed inlet, setting the temperature of the intermediate frequency furnace at 1100-1200 ℃, inclining the furnace body after reaching the temperature, pouring the prepared master alloy into a stainless steel container, and cooling for later use;
pouring the master alloy obtained in the step into a stainless steel container, fully mixing the master alloy with 1000 g of tin powder at the temperature of 200-300 ℃, stirring for 60 minutes, and standing for 180 minutes to prepare an alloy for later use;
when the temperature is reduced to 150-;
the alloy is processed by powder atomization molding equipment and classified screening to prepare tin alloy powder for later use;
smelting 25 g of copper and 0.4 g of gold into alloy, and preparing the alloy into nano metal powder for later use through centrifugal grading screening by using nano powder forming equipment;
then 0.2 g of rare earth alloy passes through powder forming equipment, and is prepared into rare earth alloy powder for later use through grading screening.
Starting to manufacture a flux paste, adding 50 g of hydrogenated rosin into a reaction kettle, stirring and melting at 120-140 ℃, adding 16 g of diethylene glycol monohexyl ether, uniformly stirring, cooling to 80-110 ℃, adding 2 g of succinic acid and 9 g of methyl benzotriazole, uniformly stirring, cooling to 40-50 ℃, adding 1.8 g of citric acid, uniformly stirring, and cooling to room temperature to prepare the flux paste for later use;
finally, 1010 g of tin metal material, 100 g of copper metal material, 9 g of potassium metal powder, 25 g of copper, 0.4 g of gold, 0.2 g of rare earth alloy and soldering paste prepared from 50 g of hydrogenated rosin, 16 g of diethylene glycol monohexyl ether, 2 g of succinic acid, 9 g of methyl benzotriazole and 1.8 g of citric acid are sequentially added into a full-automatic planetary mixer, are uniformly stirred under a vacuum condition, are subpackaged and are stored at the temperature of 2-10 ℃.
Example 3
Taking 10 g of tin metal material and 100 g of antimony metal material, adding the tin metal material and the antimony metal material into an intermediate frequency furnace through a feeding hole, setting the temperature of the intermediate frequency furnace at 650-800 ℃, inclining the furnace body after reaching the temperature, pouring the prepared master alloy into a stainless steel container, and cooling for later use;
taking 63 g of tin metal material and 37 g of lead metal material, adding the materials into an intermediate frequency furnace through a feed inlet, setting the temperature of the intermediate frequency furnace at 1300-1400 ℃, inclining the furnace body after reaching the temperature, pouring the prepared master alloy into a stainless steel container, and cooling for later use;
pouring the master alloy obtained in the step into a stainless steel container, fully mixing the master alloy with 1000 g of tin powder at the temperature of 200-300 ℃, stirring for 60 minutes, and standing for 180 minutes to prepare an alloy for later use;
when the temperature is reduced to 150-;
the alloy is processed by powder atomization molding equipment and classified screening to prepare tin alloy powder for later use;
then 0.4 g of titanium, 0.4 g of cobalt and 0.4 g of gold are melted into alloy, and the alloy is prepared into nano metal powder for later use through centrifugal grading screening by nano powder forming equipment;
then 0.2 g of rare earth alloy passes through powder forming equipment, and is prepared into rare earth alloy powder for later use through grading screening.
Starting to manufacture the flux paste, adding 80 g of hydrogenated rosin into a reaction kettle, stirring and melting at 120-140 ℃, adding 20 g of diethylene glycol monohexyl ether, uniformly stirring, cooling to 80-110 ℃, adding 2 g of succinic acid and 10 g of methyl benzotriazole, uniformly stirring, cooling to 40-50 ℃, adding 3 g of citric acid, uniformly stirring, and cooling to room temperature to prepare the flux paste for later use;
finally, 1073 g of tin metal material, 100 g of antimony metal material, 37 g of lead metal material, 12 g of potassium metal powder, 0.4 g of titanium, 0.4 g of cobalt, 0.4 g of gold, 0.2 g of rare earth alloy, and soldering paste prepared from 80 g of hydrogenated rosin, 20 g of diethylene glycol monohexyl ether, 2 g of succinic acid, 10 g of tolyltriazole and 3 g of citric acid are sequentially added into a full-automatic planetary mixer, are uniformly stirred under a vacuum condition, are subpackaged and are stored at the temperature of 2-10 ℃.
Example 4
Taking 30 g of tin metal material and 70 g of silver metal material, adding the materials into an intermediate frequency furnace through a feeding hole, setting the temperature of the intermediate frequency furnace at 1100-1200 ℃, inclining the furnace body after reaching the temperature, pouring the prepared master alloy into a stainless steel container, and cooling for later use;
taking 10 g of tin metal material and 100 g of antimony metal material, adding the tin metal material and the antimony metal material into an intermediate frequency furnace through a feeding hole, setting the temperature of the intermediate frequency furnace at 1100-1200 ℃, inclining the furnace body after the temperature is reached, pouring the prepared master alloy into a stainless steel container, and cooling for later use;
pouring the master alloy obtained in the step into a stainless steel container, fully mixing the master alloy with 1000 g of tin powder at the temperature of 200-300 ℃, stirring for 60 minutes, and standing for 180 minutes to prepare an alloy for later use;
when the temperature is reduced to 150-;
the alloy is processed by powder atomization molding equipment and classified screening to prepare tin alloy powder for later use;
then 40 g of copper and 0.2 g of cobalt are melted into alloy, and the alloy is prepared into nano metal powder for later use through centrifugal grading screening by nano powder forming equipment;
then 0.16 g of rare earth alloy passes through powder forming equipment, and is prepared into rare earth alloy powder for later use through grading screening.
Starting to manufacture the soldering paste, adding 80 g of hydrogenated rosin into a reaction kettle, stirring and melting at 120-140 ℃, adding 20 g of diethylene glycol monohexyl ether, uniformly stirring, cooling to 80-110 ℃, adding 1.5 g of succinic acid and 5 g of methyl benzotriazole, uniformly stirring, cooling to 40-50 ℃, adding 2.5 g of citric acid, uniformly stirring, and cooling to room temperature to prepare the soldering paste for later use;
finally, adding 1040 g of the tin metal material, 70 g of the silver metal material, 100 g of the antimony metal material, 11 g of the potassium metal powder, 40 g of the copper powder, 0.16 g of the rare earth alloy and soldering paste prepared from 80 g of hydrogenated rosin, 20 g of diethylene glycol monohexyl ether, 1.5 g of succinic acid, 5 g of methyl benzotriazole and 2.5 g of citric acid into a full-automatic planetary mixer in sequence, uniformly stirring under a vacuum condition, subpackaging and storing at the temperature of 2-10 ℃.
The description of the specific embodiments is only intended to facilitate an understanding of the method of the invention and its core ideas. It should be noted that the material formulation can be formulated within a certain range by those skilled in the art without departing from the principle of the present invention, that is, the embodiments of the present invention can be modified and modified, and the modified and modified are also within the protection scope of the claims of the present invention.
Claims (6)
1. A nano-particle doped high-temperature service soldering paste comprises tin alloy powder, nano metal powder, rare earth alloy powder and soldering paste, wherein the tin alloy powder is one or a mixture of tin-silver alloy powder, tin-antimony alloy powder and tin-copper alloy powder; the nano metal powder is one or a mixture of copper powder, nickel powder, titanium powder, cobalt powder and gold powder; the effective components of the flux paste comprise hydrogenated rosin, diethylene glycol monohexyl ether, succinic acid, methyl benzotriazole and citric acid; the method is characterized in that: the nano metal powder comprises, by mass, 2-60% of copper, 0.5-15% of nickel, 0.1-5% of titanium, 0.1-5% of cobalt and 0.1-10% of gold.
2. The nano-particle doped high-temperature service solder paste as claimed in claim 1, wherein: in the rare earth alloy powder, according to the mass percentage, the rare earth alloy powder is 0.01-2 percent, and the nano metal powder is 98-99.9 percent.
3. The nano-particle doped high-temperature service solder paste as claimed in claim 1, wherein: in the soldering paste, according to the mass percentage, 3 to 8 percent of hydrogenated rosin, 1 to 6 percent of diethylene glycol monohexyl ether, 0.1 to 0.8 percent of succinic acid, 0.03 to 0.1 percent of methyl benzotriazole and 0.01 to 0.2 percent of citric acid.
4. The method for preparing the nano-particle doped high-temperature service solder paste according to claim 1, which is characterized in that: comprises the following steps of (a) carrying out,
step one, preparing tin alloy powder, wherein the step of preparing the tin alloy powder comprises preparing tin-silver alloy powder, tin-copper alloy powder and tin-antimony alloy powder, and comprises the following specific steps,
a. adding raw materials for smelting the tin-silver master alloy into an intermediate frequency furnace through a feed inlet according to the tin-silver ratio of 3:7 in percentage by mass, setting the temperature of the intermediate frequency furnace at 1100-1200 ℃, inclining the furnace body after the temperature is reached, pouring the prepared master alloy into a stainless steel container, and cooling for later use;
b. adding raw materials for smelting a tin-copper master alloy into an intermediate frequency furnace through a feed inlet according to the tin-copper ratio of 1:10 in percentage by mass, setting the temperature of the intermediate frequency furnace at 1100-1200 ℃, pouring the prepared master alloy into a stainless steel container, and cooling for later use;
c. adding raw materials for smelting a tin-antimony master alloy into a vacuum furnace through a feeding hole according to the tin-antimony ratio of 1:10 in percentage by mass, setting the temperature of the vacuum furnace at 650-800 ℃, pouring the prepared master alloy into a stainless steel container, and cooling for later use;
d. pouring one or two of the master alloys obtained in the steps a, b and c into a stainless steel container, fully mixing the master alloys with 10 mass percent of tin powder at the temperature of 200-300 ℃, stirring for 60 minutes, standing for 180 minutes to prepare an alloy for later use;
e. when the temperature is reduced to 150-;
f. the alloy is processed by powder atomization molding equipment and classified screening to prepare tin alloy powder for later use;
step two, preparing nano metal powder,
g. one of copper, nickel, titanium, cobalt and gold is smelted or a plurality of materials are smelted into alloy, and the alloy is prepared into nano metal powder for standby through centrifugal grading screening by nano powder forming equipment;
step three, preparing rare earth alloy powder,
h. passing the rare earth alloy through powder forming equipment, and preparing rare earth alloy powder for later use through graded screening;
step four, preparing the flux paste,
i. preparing the flux paste: adding 3-8% of hydrogenated rosin into a reaction kettle, stirring and melting at 120-140 ℃, adding 1-6% of diethylene glycol monohexyl ether, uniformly stirring, cooling to 80-110 ℃, adding 0.1-0.8% of succinic acid and 0.03-0.1% of methyl benzotriazole, uniformly stirring, cooling to 40-50 ℃, adding 0.01-0.2% of citric acid, uniformly stirring, cooling to room temperature, and preparing into a backup solder paste;
step five, stirring and mixing the components to form solder paste,
j. and sequentially adding the prepared flux paste, tin alloy powder, nano metal powder and rare earth alloy powder into a full-automatic planetary stirrer, uniformly stirring under a vacuum condition, subpackaging and storing at 2-10 ℃.
5. The method for preparing the nano-particle doped high-temperature service solder paste according to claim 4, which is characterized in that: the tin alloy powder has seven specifications, wherein the 1# is 75-150 um, the 2# is 45-75 um, the 3# is 25-45 um, the 4# is 20-38 um, the 5# is 10-20 um, the 6# is 5-15 um, and the 7# is 2-12 um.
6. The method for preparing the nano-particle doped high-temperature service solder paste according to claim 4, which is characterized in that: according to the mass percentage, the content of the nano metal powder is 3% -60%, and the particle size range is 2-100 nm.
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| CN110653516B (en) * | 2019-10-31 | 2022-02-15 | 深圳群崴半导体材料有限公司 | Special soldering paste for welding multistage packaging patch elements |
| CN112399724B (en) * | 2020-11-04 | 2022-03-22 | 广东佛智芯微电子技术研究有限公司 | Bonding wire-based fine line repairing method |
| CN115781098B (en) * | 2023-01-19 | 2023-04-25 | 广东成利泰科技有限公司 | High-temperature-resistant and oxidation-resistant soldering tin powder and solder paste containing metal indium and preparation methods thereof |
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