CN111940947B - Halogen-free tin paste and preparation method thereof - Google Patents
Halogen-free tin paste and preparation method thereof Download PDFInfo
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- CN111940947B CN111940947B CN202010827877.3A CN202010827877A CN111940947B CN 111940947 B CN111940947 B CN 111940947B CN 202010827877 A CN202010827877 A CN 202010827877A CN 111940947 B CN111940947 B CN 111940947B
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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
- B23K35/02—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
-
- 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
- B23K35/3612—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 organic compounds as principal constituents
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Electric Connection Of Electric Components To Printed Circuits (AREA)
Abstract
The invention belongs to the technical field of solder paste and preparation, and provides halogen-free solder paste and a preparation method thereof, wherein the halogen-free solder paste comprises 80-90 parts by weight of Sn-X alloy powder, 0.5-1.5 parts by weight of halogen-free activating agent, 2-4 parts by weight of organic solvent, 3-5 parts by weight of liquid rosin resin, 0.5-1 part by weight of thixotropic agent and 0.05-0.5 part by weight of flatting agent, so that the influence of halogen on the weldability after welding is solved, and the halogen-free solder paste has the advantages of less residues after welding, no cleaning, environmental protection, no toxicity, lower cost and strong market competitiveness. The halogen-free solder paste has good adhesion with the welding substrate, and can effectively solve the problem of poor welding performance of the conventional solder paste.
Description
Technical Field
The invention belongs to the technical field of solder paste and preparation, and particularly relates to halogen-free solder paste and a preparation method thereof.
Background
Solder paste is a new type of soldering material which is produced along with SMT. The solder paste is a complex system and is a paste formed by mixing tin powder, soldering flux and other additives. The tin paste has certain viscosity at normal temperature, can initially adhere the electronic component to a set position, and welds the welded component and the printed circuit pad to form permanent connection along with the volatilization of the solvent and part of the additive at the welding temperature.
The Chinese patent application CN101143407A discloses a solder paste and a preparation method thereof, wherein the solder paste comprises the following components in percentage by weight; 80-90% of alloy welding powder; 6-8% of an organic solvent; 1-8% of organic acid; 2-10% of resin; 0.2 to 2 percent of surfactant. The alloy welding powder consists of 95.5 to 99.5 weight percent of tin, 0.3 to 4 weight percent of silver and 0.1 to 0.7 weight percent of copper. Although the soldering flux of the solder paste does not contain halide, the solder paste has strong adaptability, no residue is left around the soldered joint after soldering, and the solder paste is free from cleaning. But the alloy welding powder of the solder paste has poor thinning degree, uneven distribution, low elongation of the alloy welding powder and poor mechanical property of the solder paste.
Disclosure of Invention
In order to solve the above problems, the present invention provides a halogen-free solder paste and a method for preparing the same, wherein halogen is not detected in the halogen-free solder paste, and the adhesive force and the expansion rate are stronger than those of solder pastes composed of conventional formulations, and the present invention has the following technical scheme:
the invention aims to provide a halogen-free tin paste, which has the technical points that: the halogen-free tin paste is prepared by mixing 80-90 parts by weight of Sn-X alloy powder, 0.5-1.5 parts by weight of halogen-free activating agent, 2-4 parts by weight of organic solvent, 3-5 parts by weight of liquid rosin resin, 0.5-1 part by weight of thixotropic agent and 0.05-0.5 part by weight of leveling agent.
In some embodiments of the present invention, the weight of the element X is 0.1 to 2wt% based on 100wt% of the Sn-X alloy powder.
In some embodiments of the present invention, the X element in the Sn-X alloy powder is at least one of a silver element, a bismuth element, an aluminum element, and a tellurium element.
In some embodiments of the present invention, the halogen-free activating agent is at least one of acetic acid, lactic acid, pyruvic acid, propionic acid, butyric acid, isobutyric acid, methanesulfonic acid, and ethanesulfonic acid.
In some embodiments of the present invention, the organic solvent is at least one of alcohol ester dodeca, terpineol, tributyl citrate and butyl carbitol acetate.
In some embodiments of the present invention, the liquid rosin resin has a density of 1 to 1.1g/cm2The solid content of the liquid rosin resin is 48-50wt%, and the pH value is 4.5-6.5.
In some embodiments of the present invention, the thixotropic agent is at least one of fumed silica, clay particles, hydrogenated castor oil, and dodecahydroxystearic acid.
In some embodiments of the present invention, the leveling agent is at least one of polyether polyester modified organosiloxane and alkyl modified organosiloxane.
According to the formula, the invention aims to provide a preparation method of halogen-free tin paste, which has the technical points that: the preparation method of the halogen-free solder paste comprises the following steps:
the method comprises the following steps: accurately weighing the components of each raw material by using an analytical balance, and uniformly mixing an organic solvent, a halogen-free activating agent and liquid rosin resin in a stirrer to obtain a mixture A, wherein the rotating speed of the stirrer is 500-700rmp, and the stirring time is 10-20 min;
step two: placing Sn-X alloy powder into the mixture A prepared in the step one, and uniformly mixing in a homogenizer to obtain a mixture B, wherein the rotation speed of the homogenizer is 1000-1200rmp, and the homogenizing time is 3-5 min;
step three: and adding a thixotropic agent and a leveling agent into a homogenizer according to the condition of the mixture B, and uniformly mixing to obtain the halogen-free tin paste, wherein the rotation speed of the homogenizer is 1000-1200rmp, and the homogenizing time is 3-5 min.
In some embodiments of the present invention, the viscosity of the halogen-free solder paste at a rotation speed of 10rmp is 190-270 Pa.s/25 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the halogen-free tin paste comprises Sn-X alloy powder, a halogen-free activating agent, an organic solvent, liquid rosin resin, a thixotropic agent and a leveling agent, solves the problem of influence of halogen on the weldability, has few residues after welding, is free of cleaning, is environment-friendly and non-toxic, has low cost and has strong market competitiveness. The halogen-free solder paste has good adhesion with the welding substrate, and the problem of poor welding performance of the conventional solder paste can be effectively solved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below so that those skilled in the art can better understand the advantages and features of the present invention, and thus the scope of the present invention will be more clearly defined. The embodiments described herein are only a few embodiments of the present invention, rather than all embodiments, and all other embodiments that can be derived by one of ordinary skill in the art without inventive faculty based on the embodiments described herein are intended to fall within the scope of the present invention.
Example 1
The halogen-free tin paste is prepared by mixing 85 parts by weight of Sn-X alloy powder, 1 part by weight of halogen-free activating agent, 3 parts by weight of organic solvent, 4 parts by weight of liquid rosin resin, 0.75 part by weight of thixotropic agent and 0.2 part by weight of leveling agent.
Wherein, the weight of the Sn-X alloy powder is 100wt%, and the weight of the X element is 1 wt%.
Wherein, the X element in the Sn-X alloy powder is silver element.
Wherein the halogen-free activator is acetic acid.
Wherein, the organic solvent is alcohol ester twelve.
Wherein the density of the liquid rosin resin is 1.05/cm2The solid content of the liquid rosin ester is 49 wt%, and the pH value is 5.5.
Wherein the thixotropic agent is fumed silica.
Wherein the leveling agent is polyether polyester modified organic siloxane.
According to the formula, the invention aims to provide a preparation method of the halogen-free tin paste, which comprises the following steps:
the method comprises the following steps: accurately weighing the components of each raw material by using an analytical balance, and uniformly mixing an organic solvent, a halogen-free activating agent and liquid rosin resin in a stirrer to obtain a mixture A, wherein the rotating speed of the stirrer is 600rmp, and the stirring time is 15 min;
step two: placing Sn-X alloy powder into the mixture A prepared in the step one, and uniformly mixing in a homogenizer to obtain a mixture B, wherein the rotation speed of the homogenizer is 1100rmp, and the homogenizing time is 4 min;
step three: and adding a thixotropic agent and a leveling agent into a homogenizer according to the condition of the mixture B, and uniformly mixing to obtain the halogen-free tin paste, wherein the rotation speed of the homogenizer is 1100rmp, and the homogenizing time is 5 min.
Wherein the viscosity of the halogen-free solder paste at a rotation speed of 10rmp is 230 pas/25 ℃.
Example 2
The halogen-free tin paste is prepared by mixing 90 parts by weight of Sn-X alloy powder, 1.5 parts by weight of halogen-free activating agent, 4 parts by weight of organic solvent, 5 parts by weight of liquid rosin resin, 1 part by weight of thixotropic agent and 0.5 part by weight of leveling agent.
Wherein, the weight of the Sn-X alloy powder is 100wt%, and the weight of the X element is 2 wt%.
Wherein, the X element in the Sn-X alloy powder is bismuth element.
Wherein the halogen-free activator is lactic acid.
Wherein the organic solvent is terpineol.
Wherein the density of the liquid rosin resin is 1g/cm2The solid content of the liquid rosin resin is 48 wt%, and the pH value is 4.5.
Wherein the thixotropic agent is argil particles.
Wherein the leveling agent is alkyl modified organic siloxane.
According to the formula, the invention aims to provide a preparation method of the halogen-free tin paste, which comprises the following steps:
the method comprises the following steps: accurately weighing the components of each raw material by using an analytical balance, and uniformly mixing an organic solvent, a halogen-free activating agent and liquid rosin resin in a stirrer to obtain a mixture A, wherein the rotating speed of the stirrer is 700rmp, and the stirring time is 10 min;
step two: placing Sn-X alloy powder into the mixture A prepared in the first step, and uniformly mixing in a homogenizer to obtain a mixture B, wherein the rotating speed of the homogenizer is 1000rmp, and the homogenizing time is 5 min;
step three: and adding a thixotropic agent and a leveling agent into a homogenizer according to the condition of the mixture B, and uniformly mixing to obtain the halogen-free tin paste, wherein the rotating speed of the homogenizer is 1000rmp, and the homogenizing time is 5 min.
Wherein the viscosity of the halogen-free solder paste at a rotation speed of 10rmp is 270 pas/25 ℃.
Example 3
The halogen-free tin paste is prepared by mixing 80 parts by weight of Sn-X alloy powder, 0.5 part by weight of halogen-free activating agent, 2 parts by weight of organic solvent, 3 parts by weight of liquid rosin resin, 0.5 part by weight of thixotropic agent and 0.05 part by weight of leveling agent.
Wherein the weight of the Sn-X alloy powder is 100wt%, and the weight of the X element is 0.1 wt%.
Wherein, the X element in the Sn-X alloy powder is an aluminum element.
Wherein the halogen-free activator is pyruvic acid.
Wherein the organic solvent is tributyl citrate.
Wherein the density of the liquid rosin resin is 1g/cm2The solid content of the liquid rosin resin is 48 wt%, and the pH value is 4.5.
Wherein the thixotropic agent is gas-phase dodecahydroxystearic acid.
Wherein the leveling agent is a mixture of polyether polyester modified organic siloxane and alkyl modified organic siloxane.
According to the formula, the invention aims to provide a preparation method of the halogen-free tin paste, which comprises the following steps:
the method comprises the following steps: accurately weighing the components of each raw material by using an analytical balance, and uniformly mixing an organic solvent, a halogen-free activating agent and liquid rosin resin in a stirrer to obtain a mixture A, wherein the rotating speed of the stirrer is 700rmp, and the stirring time is 10 min;
step two: placing Sn-X alloy powder into the mixture A prepared in the step one, and uniformly mixing in a homogenizer to obtain a mixture B, wherein the rotation speed of the homogenizer is 1200rmp, and the homogenizing time is 3 min;
step three: and adding a thixotropic agent and a leveling agent into a homogenizer according to the condition of the mixture B, and uniformly mixing to obtain the halogen-free tin paste, wherein the rotation speed of the homogenizer is 1200rmp, and the homogenizing time is 3 min.
Wherein the viscosity of the halogen-free solder paste at a rotation speed of 10rmp is 190 pas/25 ℃.
Example 4
The halogen-free tin paste is prepared by mixing 88 parts by weight of Sn-X alloy powder, 1.2 parts by weight of halogen-free activating agent, 3.5 parts by weight of organic solvent, 4.5 parts by weight of liquid rosin resin, 0.9 part by weight of thixotropic agent and 0.35 part by weight of leveling agent.
Wherein, the weight of the Sn-X alloy powder is 100wt%, and the weight of the X element is 1.5 wt%.
Wherein, the X element in the Sn-X alloy powder is tellurium element.
Wherein the halogen-free activator is a mixture of butyric acid and ethylsulfonic acid.
Wherein the organic solvent is butyl carbitol acetate.
Wherein the density of the liquid rosin resin is 1.03g/cm2The solid content of the liquid rosin resin is 49 wt%, and the pH value is 5.
Wherein the thixotropic agent is dodecahydroxystearic acid.
Wherein the leveling agent is polyether polyester modified organic siloxane.
According to the formula, the invention aims to provide a preparation method of the halogen-free tin paste, which comprises the following steps:
the method comprises the following steps: accurately weighing the components of each raw material by using an analytical balance, and uniformly mixing an organic solvent, a halogen-free activating agent and liquid rosin resin in a stirrer to obtain a mixture A, wherein the rotating speed of the stirrer is 550rmp, and the stirring time is 18 min;
step two: placing Sn-X alloy powder into the mixture A prepared in the step one, and uniformly mixing in a homogenizer to obtain a mixture B, wherein the rotation speed of the homogenizer is 1000rmp, and the homogenizing time is 5 min;
step three: and adding a thixotropic agent and a leveling agent into a homogenizer according to the condition of the mixture B, and uniformly mixing to obtain the halogen-free tin paste, wherein the rotating speed of the homogenizer is 1000rmp, and the homogenizing time is 5 min.
Wherein the viscosity of the halogen-free solder paste at a rotation speed of 10rmp is 200 pas/25 ℃.
Comparative example 1
The same procedure as in example 1 was repeated except that "liquid rosin resin" in example 1 was changed to "rosin resin" of the same quality.
Comparative example 2
The operation was carried out in the same manner as in example 1 except that "Sn-X alloy powder" in example 1 was changed to "tin powder".
Examples of the experiments
The mechanical green content and the spreading rate of the solder paste prepared in the embodiments 1 to 4 are measured, and the adhesive force of the solder paste after welding is detected, and the specific results are shown in the table 1:
TABLE 1
| Halogen content | Expansion ratio/% | adhesion/N | |
| Example 1 | Not detected out | 82.2 | 4.2 |
| Example 2 | Not detected out | 83.5 | 4.3 |
| Example 3 | Undetected | 86.1 | 4.6 |
| Example 4 | Not detected out | 82.1 | 4.2 |
| Comparative example 1 | Not detected out | 75.3 | 4.1 |
| Comparative example 2 | Not detected out | 84.2 | 3.5 |
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (6)
1. A halogen-free solder paste is characterized in that: the halogen-free tin paste is prepared by mixing 80-90 parts by weight of Sn-X alloy powder, 0.5-1.5 parts by weight of halogen-free activating agent, 2-4 parts by weight of organic solvent, 3-5 parts by weight of liquid rosin resin, 0.5-1 part by weight of thixotropic agent and 0.05-0.5 part by weight of flatting agent, wherein the density of the liquid rosin resin is 1-1.1g/cm3The solid content of the liquid rosin resin is 48-50wt%, the pH value is 4.5-6.5, the weight of the element X is 0.1-2wt% calculated by 100wt% of the Sn-X alloy powder, the element X in the Sn-X alloy powder is at least one of silver element, bismuth element, aluminum element and tellurium element, and the thixotropic agent is at least one of fumed silica, argil particles, hydrogenated castor oil and dodecahydroxystearic acid.
2. The halogen-free solder paste as claimed in claim 1, wherein: the halogen-free activator is at least one of acetic acid, lactic acid, pyruvic acid, propionic acid, butyric acid, isobutyric acid, methanesulfonic acid and ethanesulfonic acid.
3. The halogen-free solder paste as claimed in claim 1, wherein: the organic solvent is at least one of alcohol ester dodeca, terpineol, tributyl citrate and butyl carbitol acetate.
4. The halogen-free solder paste as claimed in claim 1, wherein: the leveling agent is at least one of polyether polyester modified organic siloxane and alkyl modified organic siloxane.
5. The halogen-free solder paste according to any one of claims 1 to 4, wherein: the preparation method of the halogen-free solder paste comprises the following steps:
the method comprises the following steps: accurately weighing the components of each raw material by using an analytical balance, and uniformly mixing an organic solvent, a halogen-free activating agent and liquid rosin resin in a stirrer to obtain a mixture A, wherein the rotating speed of the stirrer is 500-700rmp, and the stirring time is 10-20 min;
step two: placing Sn-X alloy powder into the mixture A prepared in the step one, and uniformly mixing in a homogenizer to obtain a mixture B, wherein the rotation speed of the homogenizer is 1000-1200rmp, and the homogenizing time is 3-5 min;
step three: and adding a thixotropic agent and a leveling agent into a homogenizer according to the condition of the mixture B, and uniformly mixing to obtain the halogen-free tin paste, wherein the rotation speed of the homogenizer is 1000-1200rmp, and the homogenizing time is 3-5 min.
6. The halogen-free solder paste as claimed in claim 5, wherein: the viscosity of the halogen-free solder paste tested at 25 ℃ at a rotation speed of 10rmp is 190-270 Pa.s.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010827877.3A CN111940947B (en) | 2020-08-17 | 2020-08-17 | Halogen-free tin paste and preparation method thereof |
| PCT/CN2020/135738 WO2022036950A1 (en) | 2020-08-17 | 2020-12-11 | Halogen-free solder paste and preparation method therefor |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010827877.3A CN111940947B (en) | 2020-08-17 | 2020-08-17 | Halogen-free tin paste and preparation method thereof |
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| CN111940947B true CN111940947B (en) | 2022-05-13 |
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| CN111940947B (en) * | 2020-08-17 | 2022-05-13 | 惠州市源德智科技有限公司 | Halogen-free tin paste and preparation method thereof |
| CN115091079A (en) * | 2022-06-16 | 2022-09-23 | 深圳市兴鸿泰锡业有限公司 | Antioxidant solder paste and preparation method thereof |
| CN115091074B (en) * | 2022-07-19 | 2023-08-15 | 深圳市鑫富锦新材料有限公司 | Solder paste with variable viscosity under heating and device for preventing solder paste from dripping |
| CN117548901B (en) * | 2023-12-29 | 2024-07-05 | 深圳市华远金属有限公司 | Low-cavity halogen-free solder paste and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100450700C (en) * | 2006-04-30 | 2009-01-14 | 北京市航天焊接材料厂 | Lead-free and halogen-free soldering paste and preparation method thereof |
| CN101642855B (en) * | 2009-08-19 | 2012-02-22 | 浙江一远电子材料研究院 | Rear-earth-containing halogen free Sn-Ag-C series tinol |
| CN101653876B (en) * | 2009-08-19 | 2012-05-02 | 浙江一远电子材料研究院 | Low-silver halogen free soldering paste |
| CN101966632B (en) * | 2010-09-29 | 2013-07-17 | 广州瀚源电子科技有限公司 | Wash-free soldering flux for leadless low-temperature soldering paste and preparation method thereof |
| CN102248321A (en) * | 2011-07-06 | 2011-11-23 | 江西理工大学 | Lead-free solder paste used for halogen-free LED (light-emitting diode) lamp |
| CN102489898B (en) * | 2011-11-30 | 2013-07-31 | 昆山成利焊锡制造有限公司 | Low-silver lead-free flux paste and preparation method thereof |
| CN102489899B (en) * | 2011-12-16 | 2013-07-31 | 昆山成利焊锡制造有限公司 | Lead-free soldering paste and preparation method thereof |
| CN102581523B (en) * | 2012-03-21 | 2015-06-17 | 北京鹏瑞中联科技有限公司 | Halogen-free solder paste |
| CN103706961B (en) * | 2012-09-28 | 2016-08-03 | 钟广飞 | Halogen-free tin paste |
| CN103706968B (en) * | 2012-09-28 | 2016-05-11 | 钟广飞 | Halogen-free flux |
| JP5877822B2 (en) * | 2013-08-22 | 2016-03-08 | 株式会社タムラ製作所 | Cold and heat shock resistant flux composition, solder paste composition, method for producing solder joints, and method for producing electronic circuit boards |
| TW201607992A (en) * | 2014-08-29 | 2016-03-01 | 昇貿科技股份有限公司 | Solder flux composition |
| CN104476016A (en) * | 2014-11-05 | 2015-04-01 | 苏州赛普特电子科技有限公司 | Lead-free and halogen-free soldering paste for semiconductors |
| CN104476007B (en) * | 2014-12-17 | 2015-10-28 | 东莞永安科技有限公司 | A kind of high-melting point lead-free halogen-free soldering tin paste and preparation method thereof |
| CN104668818B (en) * | 2015-01-16 | 2017-07-07 | 北京鹏瑞中联科技有限公司 | A kind of semiconductor die package low voidage soldering paste and preparation method thereof |
| JP6230674B2 (en) * | 2016-09-20 | 2017-11-15 | 株式会社タムラ製作所 | Lead-free solder alloy, electronic circuit board and electronic control device |
| CN106312361A (en) * | 2016-10-12 | 2017-01-11 | 哈尔滨工业大学（威海） | Ceramic substrate and copper clad foil low-temperature connecting soldering paste and production process thereof |
| CN111940947B (en) * | 2020-08-17 | 2022-05-13 | 惠州市源德智科技有限公司 | Halogen-free tin paste and preparation method thereof |
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- 2020-12-11 WO PCT/CN2020/135738 patent/WO2022036950A1/en active Application Filing
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| CN111940947A (en) | 2020-11-17 |
| WO2022036950A1 (en) | 2022-02-24 |
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