CN116140863B - High-heat-resistance lead-free tin bar and preparation method thereof - Google Patents
High-heat-resistance lead-free tin bar and preparation method thereof Download PDFInfo
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- CN116140863B CN116140863B CN202310164513.5A CN202310164513A CN116140863B CN 116140863 B CN116140863 B CN 116140863B CN 202310164513 A CN202310164513 A CN 202310164513A CN 116140863 B CN116140863 B CN 116140863B
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Classifications
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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
- B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
- B23K35/262—Sn as the principal constituent
-
- 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
-
- 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
Abstract
The application relates to the technical field of tin solder, and particularly discloses a high-heat-resistance lead-free tin bar and a preparation method thereof. The high heat-resistant lead-free tin bar comprises the following components in parts by weight: 96-99 parts of tin, 1-4 parts of nano titanium powder, 2-4 parts of silver, 3-5 parts of nickel, 1.5-3 parts of antimony, 0.2-0.5 part of copper and 0.02-0.05 part of nano silicon carbide powder; the preparation method comprises the following steps: melting tin to 350-370deg.C, adding antimony, copper, nickel and silver, heating to 420-450deg.C, stirring for 20-30min, maintaining the temperature, and standing; adding nano titanium powder and nano silicon carbide powder, continuously heating to 600-800 ℃, performing ultrasonic treatment at 18-20KHZ for 10-15min, maintaining the temperature, fully stirring for 20-30min to obtain a molten liquid, casting the obtained molten liquid into a mould, and cooling to obtain the high heat resistance lead-free tin bar. The high heat-resistant lead-free tin bar has the advantages of good heat resistance, less tin slag during high-temperature operation and the like.
Description
Technical Field
The application relates to the technical field of tin solder, in particular to a high-heat-resistance lead-free tin bar and a preparation method thereof.
Background
Tin bars are commonly used electronic components, and along with the development of technology, the tin bars are widely applied to the electronic industry, the household appliance manufacturing industry, the automobile manufacturing industry, the maintenance industry and the like, and can also be used for connecting electronic components, such as resistors, capacitors, inductors and the like. In addition, the tin bars may also be used to connect electronic components to circuit boards, as well as to circuit boards and external devices. After welding, the common tin bar can only have stable performance in an environment lower than 280 ℃, and tin becomes brittle at a temperature higher than the temperature, but the operation temperature of a transformer inductor, a demagnetizing coil, an aluminum copper enameled wire, a relay, an electromagnetic filter and the like with a high Wen Jinxi is required to be 380-450 ℃, and the common tin bar is easy to deform, brittle fracture, rapid oxidation of a tin surface, more tin slag and the like in the high-temperature environment, so that the problems of incapability of operation, high reject ratio and the like are caused.
Disclosure of Invention
In order to improve the heat resistance of the tin bar and ensure the normal operation of the tin bar at high temperature, the application provides a high heat resistance lead-free tin bar and a preparation method thereof.
In a first aspect, the application provides a high heat-resistant lead-free tin bar and a preparation method thereof, and the technical scheme is as follows: the high heat-resistant lead-free tin bar comprises the following components in parts by weight:
96-99 parts of tin, 1-4 parts of nano titanium powder, 2-4 parts of silver, 3-5 parts of nickel, 1.5-3 parts of antimony, 0.2-0.5 part of copper and 0.02-0.05 part of nano silicon carbide powder.
By adopting the technical scheme, the nano titanium powder and the nano silicon carbide powder are added to react with tin, so that intermetallic compounds are not formed, normal performance of tin is not affected, the heat resistance of the tin bar and the toughness and the hardness of the tin bar at high temperature are improved by utilizing the property that the hardness and the heat resistance of the nano titanium and the nano silicon carbide are better than those of the tin of a base material, meanwhile, the nano titanium and the silicon carbide can refine grains, so that the number of the grains in a certain volume is increased, the grain boundary area is increased, the crystal phase structure of the tin is enhanced, the generation of tin orthorhombic crystals is inhibited, the toughness and the strength of the tin bar at high temperature are improved while the normal operation of the tin bar is ensured, and the generation of brittle tin is avoided. The tin bar has higher heat resistance and corrosion resistance and higher electric conductivity and thermal conductivity.
Optionally, the particle size of the nano titanium powder and the nano silicon carbide is between 50 and 80 nm.
By adopting the technical scheme, the nano titanium and the nano silicon carbide are distributed in the tin to serve as rigid supporting points, and the method is similar to physical crosslinking, so that the hardness and strength of the tin bar at high temperature are improved, and the proper particle size is selected to avoid adverse effects on the appearance of the finished tin bar and influence the product performance.
Optionally, the feedstock also contains 0.04-0.08 parts germanium and 0.04-0.08 parts rhenium.
By adopting the technical scheme, germanium has the characteristic of surface segregation, can be separated out on the surface of the tin bar after being melted at high temperature, improves the surface oxidation resistance of the tin bar, and can change the liquid phase temperature of tin together with rhenium, so that the tin can normally and stably work at high temperature, and the generation of tin oxide slag is reduced.
In a second aspect, the application provides a preparation method of a high heat-resistant lead-free tin bar, which adopts the following technical scheme:
a preparation method of a high heat-resistant lead-free tin bar comprises the following steps:
(1) Weighing the components according to the weight proportion, melting tin to 350-370 ℃, adding antimony, copper, nickel and silver, heating to 420-450 ℃, continuously stirring for 20-30min, preserving heat and standing;
(2) Adding nano titanium powder and nano silicon carbide powder, continuously heating to 600-800 ℃, performing ultrasonic treatment at 18-20KHZ for 10-15min, and maintaining the temperature and fully stirring for 20-30min to obtain molten liquid;
(3) Casting the obtained melt into a mould, and cooling to obtain the high heat resistance lead-free tin bar.
By adopting the technical scheme, the addition of the metals is controlled by gradually heating, so that the metals are fully reacted and smelted and uniformly distributed; by ultrasonic treatment, alternating low-pressure and high-pressure circulation is generated in the melt to generate high-temperature and high-pressure chemical micro-reaction, so that heterogeneous nucleation is controlled, the refinement degree of crystal grains in the alloy is improved, the crystal phase structure is enhanced, the strength and toughness are improved, and nano raw materials are uniformly dispersed to better play a role in the material.
Optionally, after casting the molten liquid in a mould, immersing the molten liquid in a heat treatment liquid at 100-200 ℃ to cool to 200-240 ℃, reheating to 300-330 ℃, and then slowly cooling to room temperature in a cooling liquid to obtain the high heat resistance lead-free tin bar.
According to the technical scheme, the molded high Wen Xitiao is immersed into the heat treatment liquid for heat treatment to further refine grains, the hardness and strength of the tin bars are improved, the repeated heating is carried out, the internal stress caused by too fast cooling is relieved, and then the tin bars are placed into the oil phase cooling liquid with slower cooling for slow cooling, so that the hardness is further improved.
Optionally, the heat treatment liquid is a mixture of aluminum chloride, trimethyl ethyl ammonium chloride and sodium aluminum hydride.
Optionally, the weight ratio of aluminum chloride, trimethyl ethyl ammonium chloride and sodium aluminum hydride in the heat treatment liquid is 1.2-1.5:1:0.1.
Through adopting above-mentioned technical scheme, form the dense oxide film on the tin bar surface when the aluminium layer receives the high temperature at the tin bar surface, stop the contact of high Wen Xiaxi and oxygen, avoid tin to be oxidized under the high temperature, reduce the production of tin slag, strengthen the heat resistance of tin bar.
Optionally, the cooling liquid is a mixed solution of mineral oil and n-hexane.
Optionally, the weight ratio of the mineral oil of the cooling liquid to the n-hexane is 3-3.5:1.
by adopting the technical scheme, the mixed solution formed by the mineral oil and the n-hexane has strong surface affinity and infiltration capacity with metal, and can infiltrate into the inner parts of the capillary holes of the metal to remove water vapor and moisture, so as to form a compact protective film and isolate air and moisture in the capillary holes of the surface area of the metal.
In summary, the application has the following beneficial effects:
1. the application adopts the high temperature resistant nano titanium powder and the nano silicon carbide powder, the added titanium and silicon carbide do not influence the normal performance of tin, the crystal phase structure of tin can be enhanced at high temperature, and the generation of tin orthorhombic crystals is inhibited, so that the normal operation of tin bars is ensured, and the strength of the tin bars at high temperature is enhanced.
2. According to the application, the heat treatment liquid is preferably used for rapidly cooling the high Wen Xitiao to a medium temperature region so as to improve the strength and toughness of the tin bar, and meanwhile, the heat treatment liquid can form an aluminum coating on the surface of the tin bar to isolate the contact between tin and oxygen and avoid the phenomena of bluing of tin surface, excessive tin slag and the like caused by oxidation of tin at high temperature; the tin bar is slowly cooled to the room temperature by using the cooling liquid, a compact film can be formed on the surface of the tin bar by the cooling liquid, water vapor and air are removed, and impurities on the surface of the tin bar are avoided.
3. According to the method, the metal elements are gradually added, the ultrasonic treatment helps the reaction, the heat treatment liquid accelerates the cooling process, the performance of the tin bar is enhanced, the cooling liquid further enhances the performance, and the steps are mutually matched to enhance the heat resistance of the tin bar.
Detailed Description
The present application will be described in further detail with reference to examples.
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Examples
Example 1
A preparation method of the high heat-resistant lead-free tin bar comprises the following steps:
(1) Heating 96kg of tin to 350 ℃, adding 1kg of antimony, 0.5kg of copper, 3kg of nickel and 3kg of silver, heating to 420 ℃, continuously stirring for 25min, and keeping the temperature and standing for 20min;
(2) Adding nano titanium powder and nano silicon carbide powder, continuously heating to 800 ℃, carrying out ultrasonic treatment at 18KHZ for 10min, and keeping the temperature and fully stirring for 20min to obtain a molten liquid;
(3) Casting the obtained melt into a mould, and cooling to obtain the high heat resistance lead-free tin bar.
Example 2
A preparation method of the high heat-resistant lead-free tin bar comprises the following steps:
(1) Heating 97.5kg of tin to 370 ℃, adding 2.2kg of antimony, 0.35kg of copper, 4kg of nickel and 4kg of silver, heating to 435 ℃ and continuously stirring for 20min, and keeping the temperature and standing for 20min;
(2) Adding nano titanium powder and nano silicon carbide powder, continuously heating to 700 ℃, carrying out ultrasonic treatment at 19KHZ for 15min, and keeping the temperature and fully stirring for 20min to obtain a molten liquid;
(3) Casting the obtained melt into a mould, and cooling to obtain the high heat resistance lead-free tin bar.
Example 3
A preparation method of the high heat-resistant lead-free tin bar comprises the following steps:
(1) Heating 97.5kg of tin to 370 ℃, adding 2.2kg of antimony, 0.35kg of copper, 4kg of nickel and 4kg of silver, heating to 435 ℃ and continuously stirring for 20min, and keeping the temperature and standing for 20min;
(2) Adding nano titanium powder and nano silicon carbide powder, continuously heating to 700 ℃, carrying out ultrasonic treatment at 19KHZ for 15min, and keeping the temperature and fully stirring for 20min to obtain a molten liquid;
(3) Casting the obtained melt into a mould, and cooling to obtain the high heat resistance lead-free tin bar.
Example 4
The high heat resistance lead-free tin bar is different from the embodiment 1 in that the raw materials also comprise 0.04kg of germanium and 0.04kg of rhenium, and the preparation steps are as follows:
(1) Heating 96kg of tin to 350 ℃, adding 1kg of antimony, 0.5kg of copper, 3kg of nickel and 3kg of silver, heating to 420 ℃, adding 0.04kg of germanium and 0.04kg of rhenium, continuously stirring for 25min, and keeping the temperature and standing for 20min;
(2) Adding nano titanium powder and nano silicon carbide powder, continuously heating to 800 ℃, carrying out ultrasonic treatment at 18KHZ for 10min, and keeping the temperature and fully stirring for 20min to obtain a molten liquid;
(3) Casting the obtained melt into a mould, and cooling to obtain the high heat resistance lead-free tin bar.
Example 5
A high heat resistance lead-free tin bar differs from example 4 in that 0.06kg germanium and 0.08kg rhenium are added to the feed.
Example 6
A high heat resistance lead-free tin bar differs from example 4 in that 0.08kg germanium and 0.04kg rhenium are added to the feed.
Example 7
The difference between the high heat-resistant lead-free tin bar and the embodiment 5 is that the preparation method comprises the following steps:
(1) Heating 96kg of tin to 350 ℃, adding 1kg of antimony, 0.5kg of copper, 3kg of nickel and 3kg of silver, heating to 420 ℃, adding 0.04kg of germanium and 0.04kg of rhenium, continuously stirring for 25min, and keeping the temperature and standing for 20min;
(2) Adding nano titanium powder and nano silicon carbide powder, continuously heating to 800 ℃, carrying out ultrasonic treatment at 18KHZ for 10min, and keeping the temperature and fully stirring for 20min to obtain a molten liquid;
(3) Casting the obtained molten liquid into a mould, immersing the mould into a heat treatment liquid at 100 ℃ to cool to 240 ℃, reheating to 330 ℃, and then slowly cooling the mould in a cooling liquid at 35 ℃ to obtain the high heat resistance lead-free tin bar.
The heat treatment liquid is a mixed solution of 36kg of aluminum chloride, 30kg of trimethyl ethyl ammonium chloride and 3kg of sodium aluminum hydride, and the cold treatment liquid is 35kg of mineral oil and 10kg of normal hexane.
Example 8
The difference between the high heat-resistant lead-free tin bar and the embodiment 5 is that the preparation method comprises the following steps:
(1) Heating 96kg of tin to 350 ℃, adding 1kg of antimony, 0.5kg of copper, 3kg of nickel and 3kg of silver, heating to 420 ℃, adding 0.04kg of germanium and 0.04kg of rhenium, continuously stirring for 25min, and keeping the temperature and standing for 20min;
(2) Adding nano titanium powder and nano silicon carbide powder, continuously heating to 800 ℃, carrying out ultrasonic treatment at 18KHZ for 10min, and keeping the temperature and fully stirring for 20min to obtain a molten liquid;
(3) Casting the obtained melt into a mould, demoulding after forming, immersing in a heat treatment liquid with the temperature of 200 ℃ to be reduced to 200 ℃, reheating to 320 ℃, and slowly cooling in a cooling liquid with the temperature of 40 ℃ to obtain the high heat resistance lead-free tin bar.
The heat treatment liquid is a mixed solution of 45kg of aluminum chloride, 30kg of trimethyl ethyl ammonium chloride and 3kg of sodium aluminum hydride, and the cold treatment liquid is 30kg of mineral oil and 10kg of normal hexane.
Comparative example
Comparative example 1
The difference between the high heat-resistant lead-free tin bar and the embodiment 1 is that the nano titanium powder and the nano silicon carbide powder are not added into the raw materials in the embodiment.
Comparative example 2
A high heat resistance lead-free tin bar is different from example 6 in that water is used as the heat treatment liquid in this example.
Performance test
Detection method/test method
Tensile strength test: the expansion rates of the solder bars prepared in the above examples and comparative examples were examined according to YST1580-2022, tin and tin alloy tensile test method, respectively; expansion ratio test: according to GB/11364-89 test method for solder spreadability and joint filling property, the expansion rate of the soldering bars prepared in the above examples and comparative examples is respectively detected, and the larger the expansion rate is, the better the weldability of the soldering bars is; compared with the welding effect, the burning loss rate of the tin bar is observed after the tin bar is kept at 400 ℃ for 10 hours, and the smaller the burning loss rate is, the smaller the loss of the tin bar at high temperature is, and the better the heat resistance of the tin bar is.
TABLE 1 Performance test results
As can be seen from the combination of examples 1 to 3 and comparative example 1 and table 1, the test data of examples 1 to 3 are significantly better than comparative example 1, which demonstrates that the addition of nano titanium powder and nano silicon carbide powder can improve the heat resistance and tensile strength of tin bars and reduce the generation of tin slag in high temperature working environment.
As can be seen from the combination of examples 7 to 8 and comparative example 2 and table 1, the test data of examples 7 to 8 are far superior to comparative example 3, which shows that the heat treatment liquid of the present application can form an aluminum layer on the surface of the tin bar to prevent oxidation of the tin bar, and the heat treatment liquid can enhance the tensile strength of the tin bar, reduce the generation of tin slag during soldering and ensure the working performance of the tin bar at high temperature.
As can be seen from the combination of examples 1 and examples 4 to 6 and the combination of table 1, the various detection data of examples 4 to 5 are superior to example 1, which shows that germanium and rhenium can be separated out on the surface of tin at high temperature to protect tin from oxidation and lose effect, and meanwhile, the addition of the germanium and rhenium improves the liquid phase temperature of the tin bar to ensure the working performance of the tin bar at high temperature.
As can be seen from the combination of examples 4 and examples 7-8 and table 1, the experimental data of examples 7-8 are better than example 4, demonstrating that the heat resistance of the tin bars can be significantly improved after the heat treatment liquid and the cooling liquid are used for treating the cast high Wen Xitiao.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
Claims (8)
1. The high heat-resistant lead-free tin bar is characterized by comprising the following raw materials in parts by weight:
96-99 parts of tin, 1-4 parts of nano titanium powder, 2-4 parts of silver, 3-5 parts of nickel, 1.5-3 parts of antimony, 0.2-0.5 part of copper, 0.02-0.05 part of nano silicon carbide powder, 0.04-0.08 part of germanium and 0.04-0.08 part of rhenium.
2. A high heat resistant lead free tin bar as claimed in claim 1 wherein the particle size of the nano titanium powder and nano silicon carbide is between 50-80 nm.
3. A method for preparing a high heat resistance lead-free tin bar as claimed in any one of claims 1 to 2, comprising the steps of:
(1) Weighing the components according to the weight proportion, melting tin to 350-370 ℃, adding antimony, copper, nickel and silver, heating to 420-450 ℃, adding germanium and rhenium, continuously stirring for 20-30min, preserving heat and standing;
(2) Adding nano titanium powder and nano silicon carbide powder, continuously heating to 600-800 ℃, performing ultrasonic treatment at 18-20KHZ for 10-15min, and maintaining the temperature and fully stirring for 20-30min to obtain molten liquid;
(3) Casting the obtained melt into a mould, and cooling to obtain the high heat resistance lead-free tin bar.
4. The method for preparing the high heat-resistant lead-free tin bar according to claim 3, wherein the high heat-resistant lead-free tin bar is obtained by pouring the molten liquid into a die, immersing the molten liquid into a heat treatment liquid with the temperature of 100-200 ℃ to be reduced to 200-240 ℃, reheating the molten liquid to 300-330 ℃, and then slowly cooling the molten liquid in a cooling liquid with the temperature of 30-40 ℃.
5. The method for preparing the high heat resistance lead-free tin bar according to claim 4, wherein the method comprises the following steps: the heat treatment liquid is a mixed solution of aluminum chloride, trimethyl ethyl ammonium chloride and sodium aluminum hydride.
6. The method for preparing the high heat resistance lead-free tin bar according to claim 5, wherein the method comprises the following steps: the weight ratio of aluminum chloride, trimethyl ethyl ammonium chloride and sodium aluminum hydride in the heat treatment liquid is 1.2-1.5:1:0.1.
7. The method for preparing the high heat resistance lead-free tin bar according to claim 4, wherein the method comprises the following steps: the cooling liquid is a mixed solution of mineral oil and n-hexane.
8. The method for preparing the high heat resistance lead-free tin bar according to claim 7, wherein the method comprises the following steps: the weight ratio of the mineral oil of the cooling liquid to the n-hexane is 3-3.5:1.
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| CN116140863B true CN116140863B (en) | 2023-10-10 |
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| KR102187085B1 (en) * | 2019-01-24 | 2020-12-04 | 주식회사 경동엠텍 | lead-free solder composition for high-temperature and vibrational circumstance and manufacturing method thereof |
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