CN116833620A - Bi-containing solder and preparation method and application thereof - Google Patents
Bi-containing solder and preparation method and application thereof Download PDFInfo
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- CN116833620A CN116833620A CN202311091746.3A CN202311091746A CN116833620A CN 116833620 A CN116833620 A CN 116833620A CN 202311091746 A CN202311091746 A CN 202311091746A CN 116833620 A CN116833620 A CN 116833620A
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- 229910000679 solder Inorganic materials 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims abstract description 8
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 238000010791 quenching Methods 0.000 claims abstract description 5
- 230000000171 quenching effect Effects 0.000 claims abstract description 5
- 238000012216 screening Methods 0.000 claims abstract description 5
- 238000005303 weighing Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 238000007789 sealing Methods 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 238000005476 soldering Methods 0.000 claims description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 230000005693 optoelectronics Effects 0.000 claims description 4
- 230000004927 fusion Effects 0.000 claims description 3
- 229910018068 Li 2 O Inorganic materials 0.000 claims description 2
- 238000002844 melting Methods 0.000 abstract description 2
- 230000008018 melting Effects 0.000 abstract description 2
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 239000000306 component Substances 0.000 description 25
- 230000003287 optical effect Effects 0.000 description 24
- 238000003466 welding Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 230000009477 glass transition Effects 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 238000004806 packaging method and process Methods 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- 229910052594 sapphire Inorganic materials 0.000 description 4
- 239000010980 sapphire Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 229920001187 thermosetting polymer Polymers 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 229910052732 germanium Inorganic materials 0.000 description 2
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 2
- 229910000833 kovar Inorganic materials 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000005304 optical glass Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- PFNQVRZLDWYSCW-UHFFFAOYSA-N (fluoren-9-ylideneamino) n-naphthalen-1-ylcarbamate Chemical compound C12=CC=CC=C2C2=CC=CC=C2C1=NOC(=O)NC1=CC=CC2=CC=CC=C12 PFNQVRZLDWYSCW-UHFFFAOYSA-N 0.000 description 1
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- -1 etc. Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- B23K35/3601—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with inorganic compounds as principal constituents
-
- 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
-
- 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
-
- 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
- B23K2101/00—Articles made by soldering, welding or cutting
- B23K2101/36—Electric or electronic devices
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
A Bi-containing solder and a preparation method and application thereof relate to the technical field of solder and solve the problem of overhigh expansion coefficient of the existing solder. Comprises the following components in parts by weight: al (Al) 2 O 3 : 3-11 parts of SiO 2 : 4-13.5 parts of CuO: 0.8-2.2 parts of B 2 O 3 :0 to 12 parts of Fe 2 O 3 : 0.6-1.6 parts of ZnO: 2.6-4.9 parts of BaO:2.9 to 4.8 parts of Bi 2 O 3 : 59-82 parts, li 2 O: 0.5-3.3 parts. Weighing the components according to a proportion and uniformly stirring; putting the mixture into a dry pot, putting into a muffle furnace, heating and melting uniformly, and pouring into deionized water for water quenching; pulverizing and grinding the product to obtain primary solder powder, and thenAnd screening by a screen to obtain the solder.
Description
Technical Field
The invention relates to the technical field of solders, in particular to a Bi-containing solder, a preparation method and application thereof.
Background
With the development of technology, the variety of optoelectronic devices is increasing, and the packaging technology of the optoelectronic devices is also an important part in the field of optoelectronic technology. In the process of packaging the photoelectric component, a proper packaging optical window is needed to package and protect core components such as a chip and the like, and the optical window is isolated from the external environment, and meanwhile, effective light emission or receiving is ensured, so that strict requirements are put on the airtight reliability, the light emergent caliber and the like of the optical window.
Packaged optical windows of reliable performance are typically formed by soldering, direct fusion or adhesion of an optical window lens, typically made of optical glass, quartz, sapphire, germanium, etc., and a metal shell, typically made of a low expansion alloy, to a material that transmits the infrared spectrum.
The direct welding mode is adopted, the temperature is high, the airtight sealing of high-melting-point optical window materials such as quartz, sapphire, silicon, germanium, zinc selenide, zinc sulfide and the like and a metal shell is not easy to realize, and the optical window manufacturing method is also not suitable for the precise optical requirements, the manufacturing of optical windows such as a coated lens and the like; by adopting the bonding mode, the optical window product with high air tightness and high radiation application cannot be realized. Therefore, the adoption of solder to weld the window material and the metal shell becomes the first choice for realizing the photoelectric packaging optical window, and the low-temperature solder material with high performance becomes the key point.
At present, a low-temperature low-expansion solder containing lead has good soldering effect in many solders for directly soldering optical lenses and metal shells. However, lead is a toxic and harmful substance, affects the health of operators, and is harmful to the environment and human health. At present, with the development of industry, policy guidance and enhancement of environmental awareness of people, lead-free environment-friendly solder has become an industry development trend. However, existing low temperature lead-free solders have too high a coefficient of expansion (> 7X 10) -6 I deg.c), the matching seal with the low expansion material lens cannot be realized.
Therefore, there is a need to develop a lead-free, low temperature environmentally friendly solder with a low expansion coefficient, which is of great importance for environmentally friendly production and use as well as for operator health.
Disclosure of Invention
In order to solve the problem of overhigh expansion coefficient of the existing low-temperature lead-free solder, the invention provides a Bi-containing solder, and a preparation method and application thereof.
The technical scheme of the invention is as follows:
the Bi-containing solder comprises the following components in parts by weight:
Al 2 O 3 : 3-11 parts of SiO 2 : 4-13.5 parts of CuO: 0.8-2.2 parts of B 2 O 3 :0 to 12 parts of Fe 2 O 3 : 0.6-1.6 parts of ZnO: 2.6-4.9 parts of BaO:2.9 to 4.8 parts of Bi 2 O 3 : 59-82 parts, li 2 O: 0.5-3.3 parts.
Preferably, the composition comprises the following components in parts by weight:
Al 2 O 3 :4.19 parts to 10.21 parts of SiO 2 :4.34 parts to 11.52 parts of CuO:1.02 to 1.23 parts of B 2 O 3 :0 to 10 parts of Fe 2 O 3 : 0.81-0.97 parts of ZnO: 3.7-4.43 parts of BaO:3.67 to 4.41 parts of Bi 2 O 3 :66.46 to 79.68 parts of Li 2 O: 0.74-2.6 parts.
Preferably, the solder has a density of 4.5g/cm 3 ~6.2g/cm 3 。
Preferably, the solder has a density of 4.95g/cm 3 ~5.97g/cm 3 。
Preferably, the fusion sealing temperature of the solder is 420-500 ℃.
Preferably, the expansion coefficient of the solder is 2.0X10 -6 /℃~5.6×10 -6 /℃。
The invention also provides a preparation method of the Bi-containing solder, which comprises the following steps:
s1, weighing the components according to a proportion, pouring the components into a mixing barrel one by one, and uniformly stirring and mixing;
s2, placing the mixture into a muffle furnace after the mixture is put into a dry pot, heating the mixture to enable the mixture to react and fuse, and pouring the mixture into deionized water for water quenching after the mixture is melted uniformly;
s3, drying, crushing and grinding the product obtained in the step S2 to obtain primary solder powder, and screening by a screen to obtain the target solder.
Preferably, the heating treatment in step S2 is specifically: heating to 920-1250 ℃, and preserving heat for 1-3 h.
Preferably, the mesh number of the screen mesh in the step S3 is 400-600 mesh.
The invention also provides an application of the Bi-containing solder, which is used for package welding of photoelectric devices.
Compared with the prior art, the invention has the following specific beneficial effects:
1. the invention provides a low-temperature environment-friendly solder which does not contain toxic and harmful components such as lead, is environment-friendly and safe and meets the RoHS standard;
2. the invention adopts Fe 2 O 3 The CuO component can increase the meltability of the material, and Bi 2 O 3 The component replaces PbO to play a role in reducing the melting point, the use temperature is as low as below 500 ℃, and the alloy is suitable for welding glass, ceramics and metal materials, particularly for sealing optical glass, sapphire, quartz and iron-nickel alloy, and has strong binding force and low cost; by Li 2 The O component can control the expansion coefficient to be further reduced, the BaO component improves the surface tension and the fluidity when the solder is melted, and the rest components can adjust crystallization and the composition of the solder.
The invention can be applied to sealing and manufacturing light emitting devices (such as UV LEDs), photoelectric detectors, packaging light windows of optical communication products and the like.
Drawings
FIG. 1 is a graph of thermal expansion of solder in example 1;
FIG. 2 is a schematic diagram of the soldering position of a sample using the solder of example 1;
fig. 3 is a thermal expansion graph of the solder in example 2.
Detailed Description
In order to make the technical solution of the present invention clearer, the technical solution of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings of the present invention, and it should be noted that the following embodiments are only used for better understanding of the technical solution of the present invention, and should not be construed as limiting the present invention.
Example 1.
S1, weighing the following components in proportion: al (Al) 2 O 3 :8.67 parts of SiO 2 :9.68 parts of CuO:1.08 parts of Fe 2 O 3 :0.85 parts of ZnO:3.89 parts of BaO:3.86 parts of Bi 2 O 3 :69.84 parts, li 2 O:2.12 parts of the components are poured into a mixing barrel one by one and stirred and mixed uniformly;
s2, placing the mixture into a muffle furnace after being put into a dry pot, heating to 1100 ℃, and preserving heat for 2 hours to enable the mixture to react and fuse, and pouring the mixture into deionized water for water quenching after the mixture is melted uniformly;
s3, drying, crushing and grinding the prepared product to obtain primary solder powder, and screening by a screen to obtain the target solder.
Putting 12g of solder into a mould, pressing into a cylinder with the diameter of 8mm, sintering into a block body, polishing to prepare a cylinder sample with the diameter of 6 multiplied by 50mm, putting the sample into a thermal expansion coefficient meter, and measuring a thermal expansion curve graph as shown in figure 1 to obtain the thermal expansion coefficient, the glass transition temperature and the softening temperature.
The solder density was measured to be 5.176g/cm 3 Expansion coefficient of 2.6X10 -6 At a temperature of 439℃and 468℃for glass transition temperature and softening temperature.
By applying the solder prepared in the embodiment, welding a quartz hemispherical lens with the diameter of 2.0mm with a kovar alloy tube shell, and performing a drop test on the welded part by using a sample welding position schematic diagram of the solder in the embodiment, wherein the solder is free to fall 10 times at a position 1m away from the floor surface of the floor paint, and no falling and no breakage of the solder are observed; and (3) carrying out a red ink experiment, wherein no leakage exists at 100 ℃ for 2 hours, and the result is qualified.
And (3) performing airtight test on the welded optical window component, wherein the test process comprises the following steps: and sealing and bonding the bottom of the optical window component and the glass sheet firmly by adopting HASENCAST 736-5 thermosetting adhesive, curing and baking for 1h at 100 ℃, and completely curing the thermosetting adhesive to form a sealed cavity inside the optical window component. Placing 30ml of fluorine oil in a 150ml beaker, setting the temperature of a heating table to be 100 ℃, heating to a constant temperature, placing the bonded optical window sealing component in the beaker, observing that the solder welding area of the optical window component does not emit bubbles, and proving that the solder welding effect is ideal and the airtight welding performance is good.
Example 2.
S1, weighing the following components in proportion: al (Al) 2 O 3 :5.8 parts of SiO 2 :6.26 parts of CuO:1.17 parts, B 2 O 3 :8.55 parts of Fe 2 O 3 :0.93 parts of ZnO:4.237 parts of BaO:4.21 parts of Bi 2 O 3 :76.15 parts, li 2 O:1.24 parts of the components are poured into a mixing barrel one by one and stirred and mixed uniformly;
s2, placing the mixture into a muffle furnace after being put into a dry pot, heating to 1100 ℃, and preserving heat for 2 hours to enable the mixture to react and fuse, and pouring the mixture into deionized water for water quenching after the mixture is melted uniformly;
s3, drying, crushing and grinding the product to obtain primary solder powder, and screening by a screen to obtain the solder.
The density of the obtained solder powder is 5.655g/cm 3 Expansion coefficient of 2.8X10 -6 /℃。
Putting 12g of solder into a mould, pressing into a cylinder with the diameter of 8mm, sintering into a block body, polishing to prepare a cylinder sample with the diameter of 6 multiplied by 50mm, putting the sample into a thermal expansion coefficient meter, and measuring a thermal expansion curve graph as shown in figure 3 to obtain the thermal expansion coefficient, the glass transition temperature and the softening temperature.
The solder density was measured to be 5.655g/cm 3 Expansion coefficient of 4.8X10 -6 The glass transition temperature was 430℃and the softening temperature was 463 ℃.
The solder prepared in the embodiment is applied, a sapphire optical window lens with the diameter of 2.0mm is welded with a kovar alloy tube shell, then a drop experiment is carried out, the solder falls freely for 10 times at a position 1m away from the ground of the terrace paint, and no falling and no damage of the solder are observed; and (3) carrying out a red ink experiment, wherein no leakage exists at 100 ℃ for 2 hours, and the result is qualified.
And (3) performing airtight test on the welded optical window component, wherein the test process comprises the following steps: and sealing and bonding the bottom of the optical window component and the glass sheet firmly by adopting HASENCAST 736-5 thermosetting adhesive, curing and baking for 1h at 100 ℃, and completely curing the thermosetting adhesive to form a sealed cavity inside the optical window component. Placing 30ml of fluorine oil in a 150ml beaker, setting the temperature of a heating table to be 100 ℃, heating to a constant temperature, placing the bonded optical window sealing component in the beaker, observing that the solder welding area of the optical window component does not emit bubbles, and proving that the solder welding effect is ideal and the airtight welding performance is good.
Claims (10)
1. The Bi-containing solder is characterized by comprising the following components in parts by weight:
Al 2 O 3 : 3-11 parts of SiO 2 : 4-13.5 parts of CuO: 0.8-2.2 parts of B 2 O 3 :0 to 12 parts of Fe 2 O 3 : 0.6-1.6 parts of ZnO: 2.6-4.9 parts of BaO:2.9 to 4.8 parts of Bi 2 O 3 : 59-82 parts, li 2 O: 0.5-3.3 parts.
2. The Bi-containing solder according to claim 1, comprising the following components in parts by mass:
Al 2 O 3 :4.19 parts to 10.21 parts of SiO 2 :4.34 parts to 11.52 parts of CuO:1.02 to 1.23 parts of B 2 O 3 :0 to 10 parts of Fe 2 O 3 : 0.81-0.97 parts of ZnO: 3.7-4.43 parts of BaO:3.67 to 4.41 parts of Bi 2 O 3 :66.46 to 79.68 parts of Li 2 O: 0.74-2.6 parts.
3. The Bi-containing solder according to claim 1, wherein the density of the solder is 4.5g/cm 3 ~6.2g/cm 3 。
4. The Bi-containing solder according to claim 1, wherein the density of the solder is 4.95g/cm 3 ~5.97g/cm 3 。
5. The Bi-containing solder according to claim 1, wherein the solder has a fusion sealing temperature of 420 ℃ to 500 ℃.
6. The Bi-containing solder according to claim 1, wherein the expansion coefficient of the solder is 2.0 x 10 -6 /℃~5.6×10 -6 /℃。
7. A method for producing the Bi-containing solder according to any one of claims 1 to 6, comprising the steps of:
s1, weighing the components according to a proportion, pouring the components into a mixing barrel one by one, and uniformly stirring and mixing;
s2, placing the mixture into a muffle furnace after the mixture is put into a dry pot, heating the mixture to enable the mixture to react and fuse, and pouring the mixture into deionized water for water quenching after the mixture is melted uniformly;
s3, drying, crushing and grinding the product obtained in the step S2 to obtain primary solder powder, and screening by a screen to obtain the target solder.
8. The method for producing Bi-containing solder according to claim 7, wherein the heat treatment in step S2 is specifically: heating to 920-1250 ℃, and preserving heat for 1-3 h.
9. The method for producing a Bi-containing solder according to claim 7, wherein the mesh number of the screen in step S4 is 400 to 600 mesh.
10. Use of a Bi-containing solder according to claim 1 for package soldering of optoelectronic devices.
Priority Applications (1)
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|---|---|---|---|
| CN202311091746.3A CN116833620B (en) | 2023-08-29 | 2023-08-29 | Bi-containing solder and preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311091746.3A CN116833620B (en) | 2023-08-29 | 2023-08-29 | Bi-containing solder and preparation method and application thereof |
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| Publication Number | Publication Date |
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| CN116833620A true CN116833620A (en) | 2023-10-03 |
| CN116833620B CN116833620B (en) | 2023-12-01 |
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| CN116833620B (en) | 2023-12-01 |
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