CN103317260A - Solder paste for soft brazing of aluminum and aluminum alloy and preparation method thereof - Google Patents
Solder paste for soft brazing of aluminum and aluminum alloy and preparation method thereof Download PDFInfo
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- CN103317260A CN103317260A CN 201310247991 CN201310247991A CN103317260A CN 103317260 A CN103317260 A CN 103317260A CN 201310247991 CN201310247991 CN 201310247991 CN 201310247991 A CN201310247991 A CN 201310247991A CN 103317260 A CN103317260 A CN 103317260A
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Abstract
The invention relates to a solder paste for soft brazing of aluminum and aluminum alloy and a preparation method thereof. The solder paste consists of two parts, i.e., braze alloy powder and a flux, wherein the composition of the braze alloy powder comprises the following components in percentage by weight: 15-30 percent of tin, 1-3 percent of silver and the balance of lead; the composition of the flux comprises the following components in percentage by weight: 5-15 percent of heavy metal fluoride, 65-75 percent of hydrofluoride of aminopolyether polyol and 10-25 percent of ethylene glycol. According to the solder paste and the preparation method thereof, the tin-lead-silver alloy is used as a braze for brazing the aluminum; during brazing, the silver and the aluminum in the braze react, a layer of silver-aluminum solid solution is formed on a boundary surface of the braze and the aluminum, the electrode potential difference between the aluminum and the braze is relieved, and the corrosion resistance of a brazed joint is greatly improved.
Description
Technical field
The present invention relates to a kind of soldering paste of using for aluminium and aluminum alloy soft soldering and preparation method thereof.The solder of affiliated technical field electronics, electrical equipment, heat exchanger product etc. also can be used for the soldering of Solder for Al-Cu Joint Welding joint.
Background technology
Soldering is method common in the electronics manufacturing engineering, usually be divided into solder brazing and solder two classes: with 450 ℃ brazing temperatures as boundary, the technique that is higher than this temperature is called solder brazing, be lower than this temperature and then be called solder, wherein, solder brazing has larger limitation because technological temperature is higher in the connection technique of the products such as electronics, electrical equipment; The brazing temperature of solder is lower, and brazing process is little to the heat affecting of product, and the soldering that is specially adapted to some product such as electronics, electrical equipment connects.Soldering paste by soldering alloyed metal powder and scaling powder modulation form owing to the soldering of applicable printed circuit and some large tracts of land lap joints, and is subject to special attention.
The conduction of aluminium and thermal conductivity slightly are inferior to copper, but its proportion is little, only reach 1/3 of copper, and the cost performance of aluminium is occupied larger advantage with respect to copper.As conductive material, the base material of increasing brass ware and wire is replaced by aluminium and aluminium alloy, but aluminium and aluminum alloy surface cover the oxide-film of one deck densification, very stable and difficult removal, therefore, how to make and carry out efficient, reliably connection between aluminium and aluminium alloy and other metal devices and just become obstacle larger on the soldering processes.
The critical process of aluminum soft soldering at first is rapidly, effectively to remove this layer oxide-film.Therefore require the striping ability strong to the scaling powder in the soldering paste, active high, postwelding residue corrosivity is little; Next requires scaling powder and brazing alloy powder can form well stable lotion, in order to be coated on the position that needs connection; The 3rd, require soldered fitting that preferably corrosion resistance is arranged.
By retrieval, Chinese invention patent CN200810187295 " paste composition for aluminum brazing " describes a kind of aluminium soldering soldering paste constituent, and it is by 45～60% metal dusts, 5～35% fluoride fluxs, 1～10% methacrylate base polymer and 10～40% solvent compositions.
The brazing temperature of this soldering paste is higher than 450 ℃, is difficult to the solder in the electronic applications.In being applicable to the patent report of aluminum alloy soft soldering, only limit to the patent of solder stick and scaling powder, find no the patent that is applicable to the aluminum alloy soft soldering soldering paste.
Summary of the invention
The invention provides a kind of scaling powder for aluminium and aluminum alloy soft soldering, and with the soldering paste of soldering alloyed metal powder modulation.This scaling powder active high, deoxidation film ability is strong, viscosity is high, with the lotion good stability of soldering alloyed metal powder modulation, the precipitated and separated of soldering alloyed metal powder can not occur in the soldering paste storage process, easily being coated on needs the position that connects.The corrosion resistance of soldered fitting is good.
The present invention realizes that the technical scheme of purpose is as follows:
A kind of scaling powder for aluminium and aluminum alloy soft soldering, raw material components and percentage by weight are:
Heavy metal fluoride activating agent 5～15%
The hydrofluoride 65～75% of polyhydroxy amine
Ethylene glycol 10～25%.
And the preparation method of the hydrofluoride of described polyhydroxy amine is as follows:
⑴ place polyhydroxy amine in the evaporation boiler of anti-rotten coating, is dissolved in water, and the weight ratio of polyhydroxy amine and water is 1:1;
⑵ dropwise add the hydrofluoric acid that concentration is 10～15wt% in evaporation boiler, prevent from splashing, until the pH value reaches 6～8;
⑶ evaporation material to 140～150 ℃;
⑷ be cooled to 100～110 ℃ with reaction mass, pours into and continue to be cooled to room temperature in the polypropylene containers, gets white waxy solid, is the hydrofluoride of described polyhydroxy amine.
And the preparation method of described scaling powder is as follows:
The hydrofluoride of described polyhydroxy amine is dropped into reactor, be heated to 110～130 ℃, after the hydrofluoride of polyhydroxy amine melts fully, add described heavy metal fluoride activating agent, after the heavy metal fluoride activating agent dissolves fully, stir, add ethylene glycol, namely get scaling powder after the cooling.
And, optional 1～3 kind the composition from monoethanolamine, diethanol amine, triethanolamine, AEEA, dihydroxy ethyl ethylenediamine, tetrahydroxyethy-lethylenediamine, triisopropanolamine or trishydroxymethylaminomethane of described polyhydroxy amine, mixed proportion is not limit.
And described heavy metal fluoride activating agent is selected from zinc fluoride, stannous fluoride, fluoridizes bismuth and arbitrarily two or more combination of copper fluoride.
A kind of soldering paste for aluminium and aluminum alloy soft soldering, comprise that soldering alloyed metal powder and scaling powder two parts form, constituent and the percentage by weight between the composition of soldering alloyed metal powder are: tin 15～30%, silver 1～3%, surplus is plumbous, and scaling powder is used for the scaling powder of aluminium and aluminum alloy soft soldering.
And the percentage by weight of described soldering alloyed metal powder and scaling powder is 80～90%:10～20%.
And the preparation method of described soldering paste is as follows:
⑴ prepare soldering alloyed metal powder: tin, lead, silver are weighed in proportion, and silver adds in the fritter mode, melts under 320～380 ℃ of conditions, and melting forms uniform brazing filler metal alloy, and dusting with conventional method makes less than 300 purpose soldering alloyed metal powders;
⑵ be that the scaling powder of 80～90% soldering alloyed metal powder and 10～20% mixes with percentage by weight, stirs with mixer, namely makes soldering paste.
Advantage of the present invention and good effect are:
1, the present invention adopts tin, lead, silver alloy as solder brazing aluminium, during soldering, silver and aluminium in the solder react, at solder with at the interface formation one deck silver of aluminium-aluminium solid solution, alleviated the difference in Electrode Potential between aluminium and the solder, improved the corrosion resistance of soldered fitting, because the silver content in the solder is higher, so have better corrosion resistance.
2, scaling powder provided by the present invention has been abandoned active relatively poor borofluoride, and adopted active higher perfluoro-compound as activating agent, simultaneously in order to dissolve this perfluoro-compound, the hydrofluoride that has been used in conjunction with highly active polyhydroxy amine is matrix, does not contain the charges of non-activity in the scaling powder fully.
3, the matrix that adopts of scaling powder of the present invention itself just has the characteristic of extremely strong removal oxide-film, has improved thus the overall activity of scaling powder.In brazing process, owing to having high fluorine ion relative amount in the scaling powder, can remove rapidly the oxide-film on aluminium surface, meanwhile heavy metal fluoride is reduced by aluminium base in brazing process, separate out that heavy metal is in a liquid state and with the mother metal alloying, reduce the interfacial tension between melt solder and the aluminium base, guaranteed the activity of scaling powder maximum.
4, scaling powder provided by the invention has higher proportion and suitable viscosity, makes soldering paste stable in storage process, and the sedimentation layering of soldering alloyed metal powder can not occur.Soldering paste has good coating at weld.
The specific embodiment
The invention will be further described below by specific embodiment, and following examples are descriptive, is not determinate, can not limit protection scope of the present invention with this.
The hydrofluoride of related polyhydroxy amine makes by polyhydroxy amine and hydrofluoric acid reaction among the present invention, described polyhydroxy amine is certainly optional: 1～3 kind composition of monoethanolamine, diethanol amine, triethanolamine, AEEA, dihydroxy ethyl ethylenediamine, tetrahydroxyethy-lethylenediamine, triisopropanolamine or trishydroxymethylaminomethane, each included component of above-mentioned composition can ratio as required be mixed.
The heavy metal fluoride activating agent is selected from zinc fluoride, stannous fluoride, fluoridizes combination any 1～4 kind in bismuth and the copper fluoride.
Embodiment 1:
A kind of soldering paste for aluminium and aluminum alloy soft soldering is comprised of soldering alloyed metal powder and scaling powder two parts, wherein:
The raw material components and the weight that form soldering alloyed metal powder are: tin 15Kg, silver-colored 1Kg, plumbous 84Kg;
The raw material components and the weight that form scaling powder are: zinc fluoride 1.8Kg, the hydrofluoride 70Kg of stannous fluoride 13.2Kg, polyhydroxy amine, ethylene glycol 15Kg.
The preparation process of above-mentioned soldering paste for aluminium and aluminum alloy soft soldering is:
⑴ prepare soldering alloyed metal powder: tin, lead, silver are weighed in proportion, be smelted into uniform brazing filler metal alloy under 320～380 ℃ of conditions, dust with conventional method, make less than 300 purpose soldering alloyed metal powders.
⑵ get percentage by weight, and to be 80% soldering alloyed metal powder (80kg) mix with 20% scaling powder (20kg), stirs with mixer, namely makes soldering paste.
The preparation method of scaling powder is as follows in the present embodiment:
1. in the present embodiment, used polyhydroxy amine is comprised of triethanolamine, tetrahydroxyethy-lethylenediamine and trishydroxymethylaminomethane,
Above-mentioned triethanolamine, tetrahydroxyethy-lethylenediamine and trishydroxymethylaminomethane equal proportion (weight ratio) are mixed and place in the evaporation boiler of corrosion-resistant finishes, be dissolved in water, the mixture of polyhydroxy amine and the weight ratio of water are 1:1;
2. dropwise add concentration in the evaporation boiler and be 10～15% hydrofluoric acid, prevent from splashing, regulate the pH value until 6～8;
3. stopped heating behind the material to 140 behind the ER～150 ℃,
4. material in the evaporation boiler is cooled to 100～110 ℃, pours into and continue to be cooled to room temperature in the polypropylene containers, get white waxy solid, be the hydrofluoride of described polyhydroxy amine;
5. take by weighing the hydrofluoride of polyhydroxy amine and drop into reactor by specified wt (85Kg), be heated to 110～130 ℃, add until completely melted zinc fluoride 1.8Kg and stannous fluoride 13.2Kg; After zinc fluoride and stannous fluoride dissolve fully, stir 10min, add ethylene glycol 15Kg, namely get scaling powder after the cooling.
Embodiment 2:
A kind of soldering paste for aluminium and aluminum alloy soft soldering is comprised of soldering alloyed metal powder and scaling powder two parts.
The raw material components and the weight that form soldering alloyed metal powder are: tin 30Kg, silver-colored 3Kg, plumbous 67Kg;
The raw material components and the weight that form scaling powder are: the hydrofluoride 85Kg of zinc fluoride 0.6Kg, stannous fluoride 3.9Kg, copper fluoride 0.5Kg, polyhydroxy amine, ethylene glycol 10Kg.
The preparation process of above-mentioned soldering paste for aluminium and aluminum alloy soft soldering is:
⑴ prepare soldering alloyed metal powder: tin, lead, silver are weighed in proportion, be smelted into uniform brazing filler metal alloy under 320～380 ℃ of conditions, dust with conventional method, make less than 300 purpose soldering alloyed metal powders;
⑵ to be 85% soldering alloyed metal powder (85kg) with percentage by weight mix with 15% scaling powder (15kg), stirs with mixer, namely makes soldering paste.
The preparation method of the present embodiment scaling powder is as follows:
1. in the present embodiment, polyhydroxy amine is comprised of trishydroxymethylaminomethane and the monoethanolamine of geometric ratio.
In the evaporation boiler that trishydroxymethylaminomethane and the monoethanolamine of above-mentioned geometric ratio placed corrosion-resistant finishes, be dissolved in water, the weight ratio of trishydroxymethylaminomethane+monoethanolamine and water is 1:2;
2. dropwise add concentration in the evaporation boiler and be 10～15% hydrofluoric acid, prevent from splashing, regulate the pH value until 6～8;
3. with material evaporation to 140 in the evaporation boiler～150 ℃;
When treating that 4. a pot interior material is cooled to 100～110 ℃, pour into and be cooled to room temperature in the polypropylene containers, get white waxy solid, be the hydrofluoride of described polyhydroxy amine;
5. take by weighing the hydrofluoride of above-mentioned trishydroxymethylaminomethane+monoethanolamine and drop into reactor by specified wt (95Kg), be heated to 110～130 ℃, melt rear adding zinc fluoride, stannous fluoride and copper fluoride fully until it; After zinc fluoride, stannous fluoride and copper fluoride dissolve fully, stir 10min, add ethylene glycol, namely get scaling powder after the cooling.
Embodiment 3:
A kind of soldering paste for aluminium and aluminum alloy soft soldering, identical with embodiment 1 and 2, same soldering alloyed metal powder and scaling powder two parts form, wherein:
The raw material components and the weight that form soldering alloyed metal powder are: tin 16Kg, silver-colored 2Kg, plumbous 82Kg;
The raw material components and the weight that form scaling powder are: zinc fluoride 1.2Kg, stannous fluoride 7.2Kg, the hydrofluoride 70Kg that fluoridizes bismuth 1.6Kg, polyhydroxy amine, ethylene glycol 20Kg.
⑴ the preparation process of above-mentioned soldering paste for aluminium and aluminum alloy soft soldering is:
Preparation soldering alloyed metal powder: tin, lead, silver are weighed in proportion, under 320～380 ℃ of conditions, be smelted into uniform brazing filler metal alloy, dust with conventional method, make less than 300 purpose soldering alloyed metal powders;
⑵ to be 90% soldering alloyed metal powder (90kg) with percentage by weight mix with 10% scaling powder (10kg), stirs with mixer, namely makes soldering paste.
The preparation method of the present embodiment scaling powder is as follows:
1. in the present embodiment, polyhydroxy amine is comprised of diethanol amine and triisopropanolamine, the diethanol amine triisopropanolamine is mixed according to the ratio (weight ratio) of 1:3 and place in the evaporation boiler of corrosion-resistant finishes, be dissolved in water, the weight ratio of polyhydroxy amine and water is 1:1;
2. dropwise add concentration in the evaporation boiler and be 10～15% hydrofluoric acid, prevent from splashing, regulate the pH value until 6～8;
2. with stopped heating behind material evaporation to 140 in the evaporation boiler～150 ℃;
3. behind the material to 100 of cooling evaporation～110 ℃, pour into and be cooled to room temperature in the polypropylene containers, get white waxy solid, be the hydrofluoride of described polyhydroxy amine;
4. take by weighing the hydrofluoride of above-mentioned polyhydroxy amine and drop into reactor by specified wt (90Kg), be heated to 110～130 ℃, melt rear adding zinc fluoride, stannous fluoride fully and fluoridize bismuth until it; Until zinc fluoride, stannous fluoride with fluoridize bismuth and dissolve rear stirring 10min fully, add ethylene glycol, namely get scaling powder after the cooling;
Need to prove, stannous fluoride involved in the present invention, the heavy metal fluoride activating agent collocation of fluoridizing the multiple combinations such as bismuth, copper fluoride and zinc fluoride are not limited to selection and the ratio that above-mentioned 3 embodiment provide, zinc fluoride, stannous fluoride, fluoridize bismuth and copper fluoride arbitrarily two or more combinations all can be used as various heavy fluoride activating agent, and each component is chosen ratio and is not limit.
Detect test
1, embodiment 1～3 made soldering paste is carried out spreadability test at the L2 aluminium sheet, test method is as follows: 0.5 gram soldering paste is placed on the L2 aluminium sheet that cleaned with acetone aluminium plate thickness 1mm, area 40 * 40mm
2, then aluminium sheet is placed on heating-up temperature and is on 300 ℃ the electric hot plate, keep 30s.After the soldering paste fusing and sprawling, take off test piece from electric hot plate, after cleaning, measures water the angle of wetting of solder.
The angle of wetting of table 1 soldering paste on aluminium sheet
2, use and by the made soldering paste of embodiment 1～3 L2 aluminium is carried out soldering and form soldered fitting, water cleans up joint, then by GB GB/T242.3.17-2008 element in aluminium joint is carried out salt spray test, concentration of saline fog is 5%NaCl solution, and test temperature is 35 ℃.
Result of the test is listed in table 2:
Table 2: soldered fitting corrosion resistance
Claims (8)
1. scaling powder that is used for aluminium and aluminum alloy soft soldering, it is characterized in that: raw material components and percentage by weight are:
Heavy metal fluoride activating agent 5～15%
The hydrofluoride 65～75% of polyhydroxy amine
Ethylene glycol 10～25%.
2. the scaling powder for aluminium and aluminum alloy soft soldering according to claim 1, it is characterized in that: the preparation method of the hydrofluoride of described polyhydroxy amine is as follows:
⑴ place polyhydroxy amine in the evaporation boiler of anti-rotten coating, is dissolved in water, and the weight ratio of polyhydroxy amine and water is 1:1;
⑵ dropwise add the hydrofluoric acid that concentration is 10～15wt% in evaporation boiler, prevent from splashing, until the pH value reaches 6～8;
⑶ evaporation material to 140～150 ℃;
⑷ be cooled to 100～110 ℃ with reaction mass, pours into and continue to be cooled to room temperature in the polypropylene containers, gets white waxy solid, is the hydrofluoride of described polyhydroxy amine.
3. the scaling powder for aluminium and aluminum alloy soft soldering according to claim 1, it is characterized in that: the preparation method of described scaling powder is as follows:
The hydrofluoride of described polyhydroxy amine is dropped into reactor, be heated to 110～130 ℃, after the hydrofluoride of polyhydroxy amine melts fully, add described heavy metal fluoride activating agent, after the heavy metal fluoride activating agent dissolves fully, stir, add ethylene glycol, namely get scaling powder after the cooling.
4. according to claim 1 and 2 or 3 described scaling powders for aluminium and aluminum alloy soft soldering, it is characterized in that: optional 1～3 kind the composition from monoethanolamine, diethanol amine, triethanolamine, AEEA, dihydroxy ethyl ethylenediamine, tetrahydroxyethy-lethylenediamine, triisopropanolamine or trishydroxymethylaminomethane of described polyhydroxy amine, mixed proportion is not limit.
5. it is characterized in that according to claim 1 or 3 described scaling powders for aluminium and aluminum alloy soft soldering: described heavy metal fluoride activating agent is selected from zinc fluoride, stannous fluoride, fluoridizes bismuth and arbitrarily two or more combination of copper fluoride.
6. soldering paste that is used for aluminium and aluminum alloy soft soldering, comprise that soldering alloyed metal powder and scaling powder two parts form, it is characterized in that: constituent and the percentage by weight between the composition of soldering alloyed metal powder are: tin 15～30%, silver 1～3%, surplus is plumbous, and scaling powder is the described scaling powder for aluminium and aluminum alloy soft soldering of claim 1-5 to.
7. the soldering paste for aluminium and aluminum alloy soft soldering according to claim 6, it is characterized in that: the percentage by weight of described soldering alloyed metal powder and scaling powder is 80～90%:10～20%.
8. according to claim 6 or 7 described soldering paste for aluminium and aluminum alloy soft soldering, it is characterized in that: the preparation method of described soldering paste is as follows:
⑴ prepare soldering alloyed metal powder: tin, lead, silver are weighed in proportion, and silver adds in the fritter mode, melts under 320～380 ℃ of conditions, and melting forms uniform brazing filler metal alloy, and dusting with conventional method makes less than 300 purpose soldering alloyed metal powders;
⑵ be that the scaling powder of 80～90% soldering alloyed metal powder and 10～20% mixes with percentage by weight, stirs with mixer, namely makes soldering paste.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103769776A (en) * | 2014-01-14 | 2014-05-07 | 浙江新锐焊接材料有限公司 | Fluoride brazing flux for copper-aluminum dissimilar metal and preparation method for fluoride brazing flux |
| CN104625483A (en) * | 2014-12-17 | 2015-05-20 | 华南理工大学 | Low-residual and low-corrosivity aluminum soft soldering tin paste and manufacturing method thereof |
| CN104985351A (en) * | 2015-06-30 | 2015-10-21 | 苏州华日金菱机械有限公司 | Solder used for thick plates |
| CN110202295A (en) * | 2019-05-24 | 2019-09-06 | 何雪连 | A kind of low temperature aluminum soft soldering tin cream and preparation method thereof |
-
2013
- 2013-06-20 CN CN 201310247991 patent/CN103317260A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103769776A (en) * | 2014-01-14 | 2014-05-07 | 浙江新锐焊接材料有限公司 | Fluoride brazing flux for copper-aluminum dissimilar metal and preparation method for fluoride brazing flux |
| CN103769776B (en) * | 2014-01-14 | 2016-06-29 | 浙江新锐焊接材料有限公司 | A kind of copper aluminum dissimilar metal fluoride flux and preparation method thereof |
| CN104625483A (en) * | 2014-12-17 | 2015-05-20 | 华南理工大学 | Low-residual and low-corrosivity aluminum soft soldering tin paste and manufacturing method thereof |
| CN104985351A (en) * | 2015-06-30 | 2015-10-21 | 苏州华日金菱机械有限公司 | Solder used for thick plates |
| CN110202295A (en) * | 2019-05-24 | 2019-09-06 | 何雪连 | A kind of low temperature aluminum soft soldering tin cream and preparation method thereof |
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Application publication date: 20130925 |