CN113909738B - Preparation method and application of ceramic soldering tin head surface treatment coating - Google Patents
Preparation method and application of ceramic soldering tin head surface treatment coating Download PDFInfo
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- CN113909738B CN113909738B CN202111303253.2A CN202111303253A CN113909738B CN 113909738 B CN113909738 B CN 113909738B CN 202111303253 A CN202111303253 A CN 202111303253A CN 113909738 B CN113909738 B CN 113909738B
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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
- B23K35/40—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
- 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
- B23K35/365—Selection of non-metallic compositions of coating materials either alone or conjoint with selection of soldering or welding materials
Abstract
The invention discloses a preparation method and application of a ceramic soldering tin head surface treatment coating, which relate to the technical field of soldering of electronic and electric products and aim at solving the problems of high cost, short service life and difficult maintenance in the prior art; after the paint is sintered, a compact and non-oxidized metal layer can be formed on the surface of the ceramic soldering tin head, so that the soldering capability is not reduced due to the oxidation of the electric soldering tin head.
Description
Technical Field
The invention relates to the technical field of soldering of electronic and electrical products, in particular to a ceramic soldering tin head surface treatment coating, a preparation method and application of the coating on a ceramic soldering tin head.
Background
Solder is an important industrial raw material for connecting electronic components in a welding circuit, is solder with a low melting point, and mainly refers to solder made of tin-based alloy. The solder is produced by first melting to produce ingot and then pressing to produce material.
Traditional soldering of electronic and electrical products is achieved by means of metal electrocautery tools. However, the metal electrocautery head is in a high-temperature working state (250-350 ℃) for a long time in the using process. The metal electric soldering head is easy to oxidize and turn black, and the soldering capability is reduced along with the increase of the oxidation degree of the metal electric soldering head, so that the working efficiency is reduced, the soldering quality of the product is unstable, and the phenomena of cold soldering and desoldering occur.
In addition, the main body of the metal electrocautery head is copper, and the surface of the main body is required to be plated with iron, nickel, chromium and tin in sequence to slow down the oxidation speed of the metal electrocautery head. The traditional metal electric soldering head has high cost, short service life and difficult maintenance, and causes large use cost and poor soldering quality for enterprises.
Disclosure of Invention
In view of the problems existing in the prior art, the invention discloses a preparation method and application of a ceramic soldering tin head surface treatment coating, and the adopted technical scheme is that the ceramic soldering tin head surface treatment coating comprises the following components in parts by weight: 5-10 parts of silver salt, 1-50 parts of silver oxide, 0.5-1 part of silver chloride, 0.5-5 parts of gold trichloride, 5-10 parts of sulfur, 20-30 parts of water, 5-20 parts of stabilizer, 0.5-2 parts of dispersing agent, 2-5 parts of adhesive, 30-50 parts of low-tension solvent and 1-2 parts of plasticizer.
As a preferable technical scheme of the invention, the silver salt is at least one of silver sulfate and silver nitrate, and the purity is 99-99.9%, so that silver ions are provided for subsequent reactions.
As a preferable technical scheme of the invention, the purities of the silver oxide, the silver chloride and the gold trichloride are all 99-99.9%, and the introduction of impurities is avoided.
The silver oxide is a tan cubic crystal system crystal or tan powder, is slightly soluble in water, is easily dissolved in acid and ammonia water, and is easily decomposed into silver simple substance and oxygen when heated to over 300 ℃;
gold trichloride is very hygroscopic and very soluble in water and ethanol. Decomposition occurs at temperatures above 160℃or upon light irradiation, and a variety of complexes with large amounts of ligands are produced.
As a preferable technical scheme of the invention, the sulfur is elemental sulfur, and the water is pure water.
As a preferred embodiment of the present invention, the stabilizer is rosin having a purity of 99.9%.
As a preferable technical scheme of the invention, the dispersing agent is acrylic ester, the adhesive is polyvinyl butyral, the low-tension solvent is at least one of nitrobenzene and turpentine, and the plasticizer is epoxy acetyl ricinoleic acid methyl ester.
The acrylic ester can be used as a dispersing agent, an adhesive and a film forming agent in the coating; in the technology, the dispersion effect is mainly achieved, and the adhesion effect is achieved before sintering;
polyvinyl butyral (PVB) is a product of acid-catalyzed condensation of polyvinyl alcohol with butyraldehyde. Because PVB molecules contain longer branched chains, the PVB molecules have good flexibility, low glass transition temperature and high tensile strength and impact strength; PVB has excellent transparency, good solubility, and good light resistance, water resistance, heat resistance, cold resistance and film forming property. The functional group contained in the modified polyethylene glycol can carry out various reactions such as saponification reaction of the phthalide group, acetification and sulfonation reaction of the hydroxyl group, and has high adhesive force with materials such as glass, metal and the like.
The invention also discloses a method for preparing the ceramic soldering tin head surface treatment coating, which adopts the technical scheme that the method comprises the following steps:
step 1, preparing materials, and weighing the materials of all components according to weight for standby;
step 2, adding the weighed silver salt and gold trichloride into water, and fully stirring to obtain a mixture A; silver nitrate in silver salt is easy to dissolve in water, and silver sulfate is slightly soluble in water, so that undissolved silver sulfate exists in the mixture A obtained in the process;
step 3, mixing and dissolving turpentine, sulfur and a stabilizer which are rosin, and preserving heat for 2 hours at 170 ℃, wherein the following reaction occurs in the heat preservation process:
S+C19H29COOH→[C19H29COOS]
fully reacting to obtain a vulcanized balsam mixture; turpentine can volatilize during the reaction process, and turpentine needs to be supplemented into the reaction system in good time;
step 4, mixing the mixture A obtained in the step 2 with the vulcanized balsam mixture obtained in the step 3, then preserving the heat at 55 ℃ and stirring, and stirring to obtain [ C19H29COOS ]]With Au + And Ag + Fully contacting, reacting to generate water-insoluble vulcanized rosin ester salt which is soluble in turpentine to become solution with density greater than that of water, so that the upper layer is water after the reaction, the lower layer is turpentine mixed solution, and separating the upper layer from water to obtain vulcanized rosin ester salt; during the complex reaction, silver ions are continuously complexed by the vulcanized balsam to generate organic metal salt which is insoluble in water and soluble in organic solvent, so that the concentration of silver ions in water is continuously reduced, and according to the ionization balance principle of insoluble matters, undissolved silver sulfate is gradually dissolved and is complexed into new matters;
the following reactions occur during the incubation:
[C19H29COOS]+Au + →[C19H29COAu]
[C19H29COOS]+Ag + →[C19H29COAg]
step 5, adding silver oxide, silver chloride, a dispersing agent, an adhesive, a plasticizer and a low-tension solvent into the vulcanized balsam salt obtained in the step 4, and uniformly stirring to obtain a mixture B;
the dispersing agent can uniformly disperse silver oxide and silver chloride in the system, and can prevent sedimentation and agglomeration of particles;
step 6, ball milling the mixture B obtained in the step 5 for 2-3 hours by using a polyurethane ball milling tank, fully crushing large particles in the mixture B, filtering by a 350-mesh nylon screen to remove coarse particles in the coating, and cutting bubbles in the coating by a screen wire of the screen to ensure that the obtained mixed coating system is uniform;
and 7, adding nitrobenzene into the mixed paint obtained in the step 6, increasing the viscosity of the paint, and uniformly stirring the paint under a vacuum condition if the viscosity is too low to cause sagging of the paint, so that bubbles can be prevented from being generated in the mixing process.
The invention also discloses an application of the ceramic soldering tin head surface treatment coating, which adopts the technical scheme that the method comprises the following steps:
step a, preparing materials, adding nitrobenzene and turpentine into the paint according to the processing technology required by the workpiece to be sprayed so as to adjust the viscosity of the paint to obtain paint A for later use;
step b, sizing, namely coating the coating A obtained in the step a on the surface of a ceramic soldering tin head at normal temperature by using a processing technology of spraying, silk screen printing, pad printing or showering, and obtaining a primary processing workpiece after the coating A on the surface layer is dried;
c, performing biscuit firing, namely placing the primary processing workpiece obtained in the step b into an electric furnace, slowly heating the electric furnace to 150-250 ℃ at the speed of 10 ℃/min, and thoroughly oxidizing and decomposing the organic matters in the coating A to obtain a semi-processed workpiece;
and d, sintering and forming, namely placing the semi-manufactured workpiece obtained in the step c into an electric furnace at 450-800 ℃ for heat preservation for 2-4 hours, and naturally cooling after heat preservation is finished.
The invention has the beneficial effects that: according to the invention, the silver salt, the gold trichloride and the [ C19H29COOS ] are used for reacting to obtain the vulcanized rosin salt, and the silver oxide, the silver chloride, the dispersing agent, the adhesive and the plasticizer are added into the vulcanized rosin salt to obtain the coating, so that no toxic or harmful organic solvent is used in the preparation process, the process is environment-friendly, and the physical and mental health of workers can be protected; after the paint is sintered, a compact and non-oxidized metal layer can be formed on the surface of the ceramic soldering tin head, so that the soldering capability is not reduced due to the oxidation of the electric soldering tin head.
Furthermore, the ceramic soldering tin head is treated by the coating, so that the treatment cost is low, the service life is long after treatment, and the maintenance is easy.
Furthermore, the total content of organic matters in the coating is small, the density of the coating is high, the shrinkage rate during sintering is only about 5%, the deformation is small, and the coating structure is compact.
Detailed Description
Example 1
The example discloses a first implementation mode of a ceramic soldering tin head surface treatment coating, which adopts the technical scheme that the coating comprises 10 parts of silver salt, 10 parts of silver oxide, 0.5 part of silver chloride, 0.5 part of gold trichloride, 10 parts of sulfur, 30 parts of water, 20 parts of rosin, 0.5 part of acrylic ester, 2 parts of polyvinyl butyral (PVB), 25 parts of nitrobenzene, 20 parts of turpentine and 1 part of methyl epoxyacetyl ricinoleate.
As a preferred embodiment of the present invention, the silver salt is 6 parts of silver sulfate and 4 parts of silver nitrate.
As a preferable embodiment of the present invention, the purity of the silver sulfate, the silver nitrate, the silver oxide, the silver chloride, and the gold trichloride is 99%.
The embodiment also discloses a first implementation mode of a preparation method of the ceramic soldering tin head surface treatment coating, which adopts the technical scheme that the preparation method comprises the following steps:
step 1, preparing materials, and weighing the materials of all components according to weight for standby;
step 2, adding weighed silver sulfate, silver nitrate and gold trichloride into water, and fully stirring to obtain a mixture A;
step 3, mixing and dissolving turpentine, sulfur and a stabilizer which are rosin, and preserving heat for 2 hours at 170 ℃ to obtain a vulcanized balsam mixture A after full reaction; turpentine can volatilize during the reaction process, and turpentine needs to be supplemented into the reaction system in time to maintain the system stable and prevent solute precipitation;
step 4, mixing the mixture A obtained in the step 2 with the mixture A obtained in the step 3After the mixture B is mixed, stirring is carried out at a constant temperature of 55 ℃ to lead [ C19H29COOS ]]With Au + And Ag + Fully contacting, separating upper water and a product after reaction to obtain vulcanized balsam salt;
step 5, adding silver oxide, silver chloride, acrylic ester, polyvinyl butyral, epoxy acetyl ricinoleic acid methyl ester and nitrobenzene into the vulcanized balsam salt obtained in the step 4, and uniformly stirring to obtain a mixture B; step 6, ball milling the mixture B obtained in the step 5 for 3 hours by using a polyurethane ball milling tank, fully crushing large particles, filtering to remove coarse particles in the coating by using a 350-mesh nylon screen after crushing treatment, and removing bubbles to ensure that the obtained mixed coating system is uniform;
and 7, adding nitrobenzene into the mixed paint obtained in the step 6, increasing the viscosity of the paint, optimizing the use effect, and uniformly stirring under the vacuum condition, so that bubbles can be prevented from being generated in the mixing process, and the compactness of a paint layer is reduced.
The embodiment also discloses a first implementation mode of the application of the ceramic soldering tin head surface treatment coating, which adopts the technical scheme that the method comprises the following steps:
step a, preparing materials, adding nitrobenzene and turpentine into the paint according to a processing technology required by a workpiece to be sprayed, so as to adjust the paint viscosity to obtain paint A for standby, wherein the nitrobenzene can increase the paint viscosity, and the turpentine can reduce the viscosity;
step b, sizing, namely uniformly coating the coating A obtained in the step a on the surface of a ceramic soldering tin head by using a spraying process at normal temperature, and obtaining a preliminary processing workpiece after the coating A on the surface layer is dried, wherein the coating A is uniformly adhered to the surface of the preliminary processing workpiece and is solidified into a film;
c, performing biscuit firing, namely placing the primary processing workpiece obtained in the step b into an electric furnace for baking, slowly heating the electric furnace to 150 ℃ at the speed of 10 ℃/min, and thoroughly oxidizing and decomposing the organic matters in the coating A to obtain a semi-processed workpiece;
and d, sintering and forming, namely placing the semi-manufactured workpiece obtained in the step c into an electric furnace at 450 ℃ for heat preservation for 4 hours, sintering a paint film on the surface of the semi-manufactured workpiece, and naturally cooling after heat preservation is finished.
Example 2
This example differs from example 1 in that the silver salt is 10 parts silver sulfate.
Example 3
This example differs from example 1 in that the silver salt is 10 parts silver nitrate.
Example 4
This example differs from example 1 in that it comprises 8 parts of silver salt, 20 parts of silver oxide, 0.6 part of silver chloride, 2 parts of gold trichloride, 8 parts of sulfur, 25 parts of water, 15 parts of turpentine, 1 part of acrylic ester, 3 parts of polyvinyl butyral (PVB), 25 parts of turpentine and 1.3 parts of methyl epoxyacetyl ricinoleate.
As a preferable technical scheme of the invention, the silver salt comprises 4 parts of silver sulfate and 4 parts of silver nitrate.
Example 5
This example differs from example 4 in that the silver salt is 8 parts silver sulfate.
Example 6
This example differs from example 4 in that the silver salt is 8 parts silver nitrate
Example 7
This example differs from example 1 in that it comprises 6 parts of silver salt, 30 parts of silver oxide, 0.8 part of silver chloride, 4 parts of gold trichloride, 6 parts of sulfur, 25 parts of water, 10 parts of rosin, 1.5 parts of acrylic ester, 4 parts of polyvinyl butyral (PVB), 5 parts of turpentine and 1.7 parts of methyl epoxyacetyl ricinoleate.
As a preferable technical scheme of the invention, the silver salt comprises 4 parts of silver sulfate and 2 parts of silver nitrate.
Example 8
This example differs from example 7 in that the silver salt is 6 parts of silver sulfate.
Example 9
This example differs from example 7 in that the silver salt is 6 parts of silver nitrate.
Example 10
This example differs from example 1 in that it comprises 8 parts of silver salt, 40 parts of silver oxide, 1 part of silver chloride, 5 parts of gold trichloride, 10 parts of sulfur, 20 parts of water, 5 parts of rosin, 2 parts of acrylic ester, 5 parts of polyvinyl butyral (PVB), 15 parts of turpentine and 2 parts of methyl epoxyacetyl ricinoleate.
As a preferable technical scheme of the invention, the silver salt comprises 2 parts of silver sulfate and 6 parts of silver nitrate.
Example 11
This example differs from example 10 in that the silver salt is 8 parts of silver sulfate.
Example 12
This example differs from example 10 in that the silver salt is 8 parts of silver nitrate.
The coatings obtained in examples 1-12 were compared with the coating used in comparative example 1 using an existing metallic electrocautery tip as comparative example 1, with the following results:
as can be seen from the comparison, the invention does not contain toxic components such as 6-valent chromium, volatile organic compounds and the like compared with the prior art.
The ceramic solder heads obtained in examples 1-12 were compared with comparative example 1, and the results were as follows:
according to the comparison, when the ceramic soldering tin head surface treatment coating prepared by the preparation method is applied to the ceramic soldering tin head, the processing technology is pollution-free, non-oxidized and good in soldering capability stability, and meets the European RoHS standard; the metal electrocautery head of comparative example 1 needs to be used in electroplating and electroless plating processes, and has the advantages of complex process, environmental pollution, easy oxidation and poor welding capability, and does not meet the European Union RoHS standard.
By comparison, example 7 is the preferred embodiment.
Working principle: the coating comprises silver sulfate or silver nitrate, which chemically reacts with other components such as gold trichloride and rosin, and when the coating is applied to a ceramic soldering tin head, the coating is sintered at 450-800 ℃ and cooled to form a metal surface layer with strong adhesive force and no oxidation.
Although the specific embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes and modifications without inventive labor may be made within the scope of the present invention without departing from the spirit of the present invention, which is within the scope of the present invention.
Claims (6)
1. The ceramic soldering tin head surface treatment coating is characterized by comprising the following components:
silver salt, silver oxide, silver chloride, gold trichloride, sulfur, water, a stabilizer, a dispersing agent, an adhesive, a low-tension solvent and a plasticizer;
the components in parts by weight are as follows:
5-10 parts of silver salt, 1-50 parts of silver oxide, 0.5-1 part of silver chloride, 0.5-5 parts of gold trichloride, 5-10 parts of sulfur, 20-30 parts of water, 5-20 parts of stabilizer, 0.5-2 parts of dispersing agent, 2-5 parts of adhesive, 30-50 parts of low-tension solvent and 1-2 parts of plasticizer;
the silver salt is at least one of silver sulfate and silver nitrate, and the purity is 99-99.9%;
the stabilizer adopts rosin with the purity of 99.9 percent;
the dispersing agent is acrylic ester, the adhesive is polyvinyl butyral, the low-tension solvent is at least one of nitrobenzene and turpentine, and the plasticizer is epoxy acetyl ricinoleic acid methyl ester.
2. The ceramic solder head surface treatment coating according to claim 1, wherein: the purities of the silver oxide, the silver chloride and the gold trichloride are all 99-99.9%.
3. The ceramic solder head surface treatment coating according to claim 1, wherein: the sulfur is elemental sulfur, and the water is pure water.
4. A method of preparing a ceramic solder head surface treatment coating according to claim 1, comprising the steps of:
step 1, preparing materials, and weighing the materials of all components according to weight for standby;
step 2, adding silver salt and gold trichloride into water and fully stirring to obtain a mixture A;
step 3, mixing and dissolving turpentine, sulfur and a stabilizer which are rosin, and preserving heat for 2 hours at 170 ℃ to fully react to obtain a vulcanized balsam mixture;
step 4, mixing the mixture A obtained in the step 2 with the vulcanized balsam mixture obtained in the step 3, preserving heat at 55 ℃, keeping stirring, and removing an upper water solution after full reaction to obtain vulcanized balsam salt;
step 5, adding silver oxide, silver chloride, a dispersing agent, an adhesive, a plasticizer and a low-tension solvent into the vulcanized balsam salt obtained in the step 4, and uniformly stirring to obtain a mixture B;
step 6, ball milling the mixture B obtained in the step 5 for 2-3 hours by using a polyurethane ball milling tank, filtering the coating by using a 350-mesh nylon screen, and collecting the coating passing through the nylon screen to obtain a mixed coating;
and 7, adding nitrobenzene into the mixed paint obtained in the step 6, and stirring uniformly under the vacuum condition.
5. Use of a ceramic solder head surface treatment coating according to claim 1, comprising the steps of:
step a, preparing materials, adding nitrobenzene and turpentine into the paint according to the requirement to adjust the viscosity of the paint to obtain paint A for later use;
step b, sizing, namely coating the coating A obtained in the step a on the surface layer of the ceramic soldering tin head in a spraying, silk screen printing, pad printing or showering mode at normal temperature, and airing the coating A on the surface layer to obtain a primary processing workpiece;
c, performing biscuit firing, namely slowly heating the primary processing workpiece obtained in the step b to 150-250 ℃ in an electric furnace to thoroughly oxidize and decompose the organic matters in the coating A, so as to obtain a semi-processed workpiece;
and d, sintering and forming, namely placing the semi-manufactured workpiece obtained in the step c into an electric furnace at 450-800 ℃ for heat preservation for 2-4 hours, and naturally cooling after heat preservation is finished.
6. The application of the ceramic solder head surface treatment coating according to claim 5, wherein: and c, the heating rate of the electric furnace in the step is 10 ℃/min.
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| CN202111303253.2A CN113909738B (en) | 2021-11-09 | 2021-11-09 | Preparation method and application of ceramic soldering tin head surface treatment coating |
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| US4795076A (en) * | 1986-12-08 | 1989-01-03 | Wilfried Gottschild | Soldering iron tip |
| CN1066863A (en) * | 1991-05-17 | 1992-12-09 | 约翰逊马西有限公司 | Precious metal composition |
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| CN1687992A (en) * | 2005-05-13 | 2005-10-26 | 范琳 | Electrode thick liquid without lead and silver and mfg. method thereof |
| CN101609724A (en) * | 2008-06-20 | 2009-12-23 | 北京有色金属研究总院 | A kind of electrode thick liquid without lead and silver and preparation method thereof |
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| CN110382632A (en) * | 2017-03-10 | 2019-10-25 | 默克专利股份有限公司 | Metal preparation and coating prepared therefrom |
| CN110653475A (en) * | 2019-09-25 | 2020-01-07 | 江苏科技大学 | Electrode tip coating and preparation method and application thereof |
| CN112735631A (en) * | 2020-12-21 | 2021-04-30 | 有研工程技术研究院有限公司 | Low-viscosity organic gold paste capable of being sintered on surface of circuit board substrate at low temperature |
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2021
- 2021-11-09 CN CN202111303253.2A patent/CN113909738B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4795076A (en) * | 1986-12-08 | 1989-01-03 | Wilfried Gottschild | Soldering iron tip |
| CN1066863A (en) * | 1991-05-17 | 1992-12-09 | 约翰逊马西有限公司 | Precious metal composition |
| CN1072699A (en) * | 1991-11-22 | 1993-06-02 | 尹维平 | A kind of coating with new function |
| CN1687992A (en) * | 2005-05-13 | 2005-10-26 | 范琳 | Electrode thick liquid without lead and silver and mfg. method thereof |
| CN101609724A (en) * | 2008-06-20 | 2009-12-23 | 北京有色金属研究总院 | A kind of electrode thick liquid without lead and silver and preparation method thereof |
| CN110382632A (en) * | 2017-03-10 | 2019-10-25 | 默克专利股份有限公司 | Metal preparation and coating prepared therefrom |
| CN108213762A (en) * | 2018-01-17 | 2018-06-29 | 宁国市顺鑫金属制品有限公司 | A kind of high rigidity mash welder soldering tip and preparation method thereof |
| CN110653475A (en) * | 2019-09-25 | 2020-01-07 | 江苏科技大学 | Electrode tip coating and preparation method and application thereof |
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| CN113909738A (en) | 2022-01-11 |
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