CN101412168B - Scaling powder for aluminium soldering tin wire core and preparation method thereof - Google Patents
Scaling powder for aluminium soldering tin wire core and preparation method thereof Download PDFInfo
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- CN101412168B CN101412168B CN200810219442XA CN200810219442A CN101412168B CN 101412168 B CN101412168 B CN 101412168B CN 200810219442X A CN200810219442X A CN 200810219442XA CN 200810219442 A CN200810219442 A CN 200810219442A CN 101412168 B CN101412168 B CN 101412168B
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Abstract
The invention relates to a soldering flux for a soldering tin wire core through aluminium soldering and a preparation method thereof. The soldering flux is used for an inner core of a soldering tin wire through aluminium soldering or aluminium alloy soldering. The soldering flux comprises the following compositions in a formula in weight percentage: 14 to 28 percent of modified resin, 12 to 24 percent of ammonium borofluoride, 38 to 56 percent of organic amine, 4 to 10 percent of zinc source, 0.5 to 8 percent of tin salt and 0.1 to 2 percent of a fluorin surfactant. The zinc source is zinc salt, zinc powder or activated zinc oxide; the tin salt is inorganic tin salt or organic acid tin; and the fluorin surfactant is one or two of FC4430, FC4432, F5010, FSN-100, F501, F502 and FS-300. The soldering flux is in a solid state at normal temperature, has the characteristics of having good stiffness, high activity and simple preparation process, remarkably improving solderability of a soldering material and the cleanness of a weld spot and the like and is suitable for producing the soldering tin wire containing the soldering flux in the core and soldering aluminum and aluminum alloy.
Description
Technical field
The present invention relates to a kind of aluminium and aluminum alloy soft soldering scaling powder and preparation method thereof.This scaling powder is used for the solder stick inner core of aluminium and aluminum alloy soft soldering, and affiliated technical field is the soldering of electronic and electrical equipment.Scaling powder for aluminium soldering tin wire core of the present invention also is applicable to the solder to nickel-base alloy and stainless steel material simultaneously.
Background technology
The heat conduction of aluminium and aluminium alloy and electric conductivity and copper are close, but its production cost and price are low than copper.For a long time, wish to adopt aluminium to come the use of instead of copper in electronics industry always.Yet the soldering solderability of aluminium and alloy thereof wants difficult a lot of than other metal (alloy), and its main cause is that aluminium and alloy surface thereof have the very fine and close oxide film (Al of one deck
2O
3).This one deck oxide-film character is highly stable, is difficult to remove during general soldering; And this oxide-film when soldering destroyed after, matrix can produce new oxide-film very soon.The oxide-film of how removing effectively on aluminium and the alloy surface thereof is the key of aluminium and aluminium alloy brazing.
The aluminum soft soldering scaling powder is meant that brazing temperature is lower than 450 ℃ of used scaling powders.Can be divided into liquid weldering aluminium scaling powder and solid-state welding aluminium scaling powder by physical state branch under the normal temperature.Liquid weldering aluminium scaling powder is mainly used in wave-soldering; As a kind of weldering aluminium scaling powder of describing among the day disclosure special permission JP 586591979: ZnCl
2(48.6%, percentage by weight descends together), SnCl
2(32.4%), KCl (15.0%), KF (2.0%) and AgCl (2.0%).The characteristics of this scaling powder are (as ZnCl by several salt
2, SnCl
2, KCl etc.) salt-mixture formed, with adding some fluorides as the rupture of membranes agent often, belong to the response type soft solder flux.This class flux activity is stronger; But the dirty and easy cleaning not of solder joint after the soldering, film of flux residue butt welding point corrosion simultaneously is very serious.Zhang Qiyun and Zhuan Hongshou chief editor's " soldering handbook (China Machine Press, in November, 1998 version) two kinds of liquid weldering aluminium scaling powders reporting in the book are composed as follows: (1) triethanolamine (62%, percentage by weight, down with), monoethanolamine (20%), Zn (BF
4)
2(8%), Sn (BF
4)
2(5%) and NH
4BF
4(5%); (2) triethanolamine (37%), monoethanolamine (30%), Zn (BF
4)
2(10%), Sn (BF
4)
2(8%) and NH
4BF
4(15%).This scaling powder characteristics are with some borofluorides, as Zn (BF
4)
2And Sn (BF
4)
2Deng, be dissolved into the solution that organic amine (as monoethanolamine, diethanol amine etc.) is made, belong to organic soft solder flux.Lower and the bright cleaning of solder joint of organic soft solder flux corrosivity is one of focus of research at present.Solid-state welding aluminium scaling powder is mainly used in the manufacturing solder stick, as the inner core of solder stick.At present, less for the solid-state welding aluminium scaling powder research report that is used for soldering tin core, when main cause is aluminium soldering flux activity is required highly, and add the processing performance that helps weldering effect and solder stick that some carriers that play solidification (as common rosin etc.) can have a strong impact on scaling powder.Therefore, finding a kind of suitable carriers is the key and the difficult point of research and development solid-state welding aluminium scaling powder.A kind of almag scaling powder of describing among day disclosure special permission JP 61232092 is mainly composed as follows: strontium fluoride (24%, molar percentage, down with), potassium fluoride (48%) and aluminum fluoride (28%).This scaling powder belongs to the response type scaling powder, and corrosivity is stronger.Simultaneously, this scaling powder must be in the temperature competence exertion effectiveness more than 450 ℃, and this scaling powder can't become uniform fluid under 130 ℃ of temperature, thereby be not suitable for the solder stick inner core.The brazing flux composition of describing in " aluminium and aluminum alloy soft soldering brazing flux and uses thereof " (patent No. 88100868) of Fujian Normal University's application (percentage by weight) is: contain amino organic matter borofluoride 1～50%, heavy metal borofluoride 0.5～50% and amino alcohol 10～98%; Scaling powder is the thickness liquid state under the higher and normal temperature of this brazing flux welding temperature (300 ℃), is difficult to use in the production that contains the scaling powder core solder stick.Used weldering aluminium scaling powder is made up of fluosilicic acid heavy metallic salt (5～20%), fluoboric acid heavy metallic salt (5～20%), polyethylene polyamine (60～80%) and vaseline (5～10%) in " the weldering aluminium tin silk " of China Patent No. 01128512.5 report; This scaling powder is carrier with vaseline, be the production that the thickness liquid state is unfavorable for solder stick equally under the scaling powder normal temperature, and flux activity is limited.
Summary of the invention
The invention reside in the shortcoming that overcomes prior art, a kind of scaling powder for aluminium soldering tin wire core is provided, be solid-state under the normal temperature and have certain deflection, and have high activity, high reliability, high-insulativity and significantly improve the solderability of scolder and characteristics such as solder joint cleaning.
Purpose of the present invention is achieved through the following technical solutions;
A kind of scaling powder for aluminium soldering tin wire core, by weight percentage, its prescription consists of:
(1) modified rosin 14～28%
(2) ammonium fluoroborate 12～24%
(3) organic amine 38～56%
(4) the zinc source 4～10%
(5) tin salt 0.5～8%
(6) fluorine surfactant 0.1～2%
Described zinc source is zinc salt, zinc powder or activated zinc oxide;
Described organic amine is a kind of in diamines and the polyamine; Or described organic amine is multiple in monoamine, diamines and the polyamine, contains a kind of diamines or polyamine at least in wherein multiple; Described monoamine is monoethanolamine, diethanol amine or triethanolamine; Described diamines or polyamine are NN-dimethyl lauryl amine, beta-hydroxyethyl ethylenediamine, diethylamide, diethylene diamine, diethylenetriamine, triethylene tetramine, tri-n-octyl amine, tetramethylethylenediamine or diethylenetriamines;
Described tin salt is inorganic tin salt or organic acid tin salt;
Described fluorine surfactant is 1～2 kind among FC4430, FC4432, F5010, FSN-100, F501, F502 and the FS-300.
For realizing that further purpose of the present invention, described modified rosin are preferably 1～2 kind in ForalAXE perhydrogenated rosin, KE-604 rosin, KE-100 rosin, dimerization colophonium 145, KR-610 rosin, B140 newtrex, B115 newtrex, B90 newtrex, Polypale newtrex, ice galbanum, water-white rosin and the disproportionated rosin.
Described zinc salt is inorganic zinc salt or organic acid zinc salt; Described inorganic zinc salt is preferably ZnCl
2, ZnBr
2, ZnF
2, ZnBr
2Or Zn (BF
4)
2Described organic acid zinc salt is preferably zinc stearate.
Described inorganic tin salt is preferably SnCl
2, SnF
2, SnBr
2Or Sn (BF
4)
2
Described organic acid tin salt is preferably stannous octoate.
The preparation method of above-mentioned described scaling powder for aluminium soldering tin wire core: in reactor, press the described prescription proportion of scaling powder for aluminium soldering tin wire core and add ammonium fluoroborate, zinc source, tin salt, fluorine surfactant and organic amine; Continuous stirring 30～45min makes raw material fully dissolve mixing under 80～100 ℃ of temperature; Add modified rosin then and simultaneously temperature is raised to 120～140 ℃ and the continuous 10～25min of stirring, obtain yellow transparent liquid; This liquid cools to room temperature is promptly obtained solid-state scaling powder for aluminium soldering tin wire core.
The principle that the present invention utilizes is as follows:
(1) modified rosin is as the scaling powder solidified carrier.
(2) ammonium fluoroborate is a stripper, can remove the oxide-film on aluminium surface when soldering rapidly.The thermal coefficient of expansion of aluminium and aluminium oxide differs greatly, and aluminium material surface oxide-film place is easy to generate be full of cracks during soldering.The NH that the ammonium fluoroborate decomposes produces
3, HF and BF
3Gas can infiltrate be full of cracks place rapidly and peel off oxide-film, simultaneously HF and BF
3Gas and aluminium oxide can react striping; Reaction equation is as follows:
Al
2O
3+6HF→2Al+3H
2O (1)
Al
2O
3+2BF
3→2AlF
3+B
2O
3 (2)
(3) zinc source and tin salt are coverture, and the surface that can be deposited on aluminium when soldering forms reactive metal layer.Zinc powder is easy to oxidation, so in fact the oxidized zinc oxide in zinc powder surface covers.Zinc oxide is amphoteric oxide, be dissolved in be alkalescence amine in and exist with ionic state.After the surface film oxide of aluminium was removed, because the specific activity zinc of aluminium is strong, aluminium cemented out zinc ion and stannous ion on the surface that covers aluminium and forms reactive metal layer, is beneficial to sprawling of solder.The reaction equation of this process is as follows:
2Al+3M
2+→2Al
3++3M (3)
M in the formula (3)
2+Represent Zn
2+, Sn
2+Deng.
(4) organic amine and fluorine surfactant are the interfacial agent of scaling powder, can reduce the surface tension of molten solder itself and the interfacial tension between molten solder and aluminium when soldering, promote solder wetting on aluminium.Discover, organic amine help the weldering effect very obvious, especially diamine and polyamine.The present invention welds the requirement of aluminium scaling powder and adds a kind of diamine or polyamine (as NN-dimethyl lauryl amine, beta-hydroxyethyl ethylenediamine, diethylenetriamine etc.) at least, has higher activity to guarantee scaling powder.Fluorine surfactant is all or part of surfactant that is replaced by fluorine atom of the hydrogen atom of hydrocarbon chain in a kind of molecule.Because carbon-fluorine bond is a weak point, strong, stable and key with very low polarity, causes Organic fluoride surfactant activity intensity very high; And heat-resisting, oxidative resistance good.Discover that the weldering effect that helps of scaling powder obviously strengthens behind a spot of fluorine surfactant of adding in this aluminium soldering scaling powder system.
Have following advantage with respect to prior art the present invention:
(1) scaling powder for aluminium soldering tin wire core of the present invention is developed at the solder of aluminium in the Electronic Packaging and aluminium alloy.Be solid-state and have certain degree of hardness under this scaling powder normal temperature, and solidification effect good, lamination does not take place, be fit to very much be used as the inner core of solder stick.Simultaneously, this flux activity is big, spreading ratio is high, can bring into play good striping effect when aluminium soldering, obtains bright, saturated solder joint, and the postwelding residue is less.
(2) the solid-state scaling powder of aluminium soldering tin wire core of the present invention can utilize mechanical-hydraulic equipment to be pressed in the solder alloy (as Sn-Ag-Cu, Sn-Zn scolder etc.), is drawn into silk, and forming outer is that solder, inner core are the solder stick of scaling powder.
(3) scaling powder for aluminium soldering tin wire core of the present invention can carry out soldering to aluminium and aluminium alloy in 250～300 ℃ of temperature ranges.
(4) scaling powder for aluminium soldering tin wire core of the present invention also is fit to the solder to nickel-base alloy and stainless steel material simultaneously.
The specific embodiment
The invention will be further described below in conjunction with specific embodiment, need to prove that embodiment does not constitute the restriction to the claimed scope of the present invention.
Embodiment 1:
A kind of scaling powder for aluminium soldering tin wire core, by weight percentage, its prescription consists of:
(1) Foral AXE perhydrogenated rosin 22%
(2) ammonium fluoroborate 24%
(3) triethanolamine 12%
(4) the beta-hydroxyethyl ethylenediamine 35.1%
(5) zinc chloride (ZnCl
2) 6%
(6) stannic chloride (SnCl
2) 0.8%
(7)FC4432 0.1％
Preparation method: in reactor, add ammonium fluoroborate, zinc chloride (ZnCl according to the above ratio
2), stannic chloride (SnCl
2), fluorocarbon surfactant (FC4432), triethanolamine, beta-hydroxyethyl ethylenediamine, be heated to 90 ℃ and continuous stirring 32min.Raw material is raised to 130 ℃ with temperature after fully dissolving mixing, and adds Foral AXE perhydrogenated rosin, obtains yellow transparent liquid behind the continuous stirring 12min.This liquid cools to room temperature is promptly obtained solid-state scaling powder for aluminium soldering tin wire core.
Embodiment 2:
A kind of scaling powder for aluminium soldering tin wire core, by weight percentage, its prescription consists of:
(1) KE-100 rosin 14%
(2) ammonium fluoroborate 16%
(3) diethanol amine 15%
(4) triethylene tetramine 38%
(5) zinc stearate 10%
(6) stannous octoate 6%
(7)FC4430 1％
Preparation method: in reactor, add ammonium fluoroborate, stannous octoate, zinc stearate, diethanol amine, triethylene tetramine, FC4430 in proportion and be heated to 95 ℃ and continuous stirring 32min.Raw material is raised to 135 ℃ with temperature after fully dissolving mixing, obtains yellow transparent liquid after adding KE-100 rosin and continuous stirring 12min then.This liquid cools to room temperature is promptly obtained solid-state scaling powder for aluminium soldering tin wire core.
Embodiment 3:
A kind of scaling powder for aluminium soldering tin wire core, by weight percentage, its prescription consists of:
(1) the B140 newtrex 12%
(2) KR-610 rosin 10%
(3) ammonium fluoroborate 12%
(4) triethanolamine 11%
(5) NN-dimethyl lauryl amine 42%
(6) activated zinc oxide 8%
(7) stannous octoate 4%
(8)F502 1％
Preparation method: in reactor, add ammonium fluoroborate, activated zinc oxide, stannous octoate, triethanolamine, F502, NN-dimethyl lauryl amine in proportion, be heated to 92 ℃ and continuous stirring 36min.Treat after raw material fully dissolves mixing temperature to be raised to 135 ℃, obtain yellow transparent liquid after adding B140 newtrex and KR610 rosin and continuous stirring 15min then.This liquid cools to room temperature is promptly obtained solid-state scaling powder for aluminium soldering tin wire core.
Embodiment 4:
A kind of scaling powder for aluminium soldering tin wire core, by weight percentage, its prescription consists of:
(1) ice galbanum 28%
(2) ammonium fluoroborate 24%
(3) monoethanolamine 9.5%
(3) diethylenetriamines 30%
(4) zinc fluoride (ZnF
2) 6%
(5) tin fluoride (SnFl
2) 0.5%
(6)F501 2％
Preparation method: in reactor, add ammonium fluoroborate, monoethanolamine, diethylenetriamines, SnF in proportion
2, ZnF
2And F501, be heated to 90 ℃ after continuous stirring 40min.Treat to be warmed up to 130 ℃ and adding ice galbanum after raw material fully dissolves mixing, obtain yellow transparent liquid behind the continuous stirring 18min.This liquid cools to room temperature is promptly obtained solid-state scaling powder for aluminium soldering tin wire core.
Embodiment 5:
A kind of scaling powder for aluminium soldering tin wire core, by weight percentage, its prescription consists of:
(1) KE-604 rosin 28%
(2) ammonium fluoroborate 24%
(4) the beta-hydroxyethyl ethylenediamine 38%
(5) the Sn powder 8%
(6) stannic chloride (SnCl
2) 1.5%
(7)FC4432 0.5％
Preparation method: in reactor, add ammonium fluoroborate, Sn powder, stannic chloride (SnCl according to the above ratio
2), fluorine surfactant (FC4432), beta-hydroxyethyl ethylenediamine, be heated to 90 ℃ and continuous stirring 32min.Raw material is raised to 135 ℃ with temperature after fully dissolving mixing, and adds KE-604 rosin, obtains yellow transparent liquid behind the continuous stirring 12min.This liquid cools to room temperature is promptly obtained solid-state scaling powder for aluminium soldering tin wire core.
Embodiment 6:
A kind of scaling powder for aluminium soldering tin wire core, by weight percentage, its prescription consists of:
(1) the B90 newtrex 6%
(2) water-white rosin 10%
(2) ammonium fluoroborate 20%
(4) NN-dimethyl lauryl amine 38%
(5) activated zinc oxide 8%
(6) stannous fluoboric acid (Sn (FB
4)
2) 1.5%
(7)FS-300 0.5％
Preparation method: in reactor, add ammonium fluoroborate, activated zinc oxide (ZnO), stannous fluoboric acid (Sn (FB according to the above ratio
4)
2), fluorine surfactant (FS-300), NN-dimethyl lauryl amine, be heated to 95 ℃ and continuous stirring 35min.Raw material is raised to 130 ℃ with temperature after fully dissolving mixing, and adds the B90 newtrex, obtains yellow transparent liquid behind the continuous stirring 15min.This liquid cools to room temperature is promptly obtained solid-state scaling powder for aluminium soldering tin wire core.
More than the scaling powder for aluminium soldering tin wire core of each embodiment preparation all have good solid molding and certain rigidity, and under plus load (with the approximate equal-volume of solid-state scaling powder sample, weight be the counterweight of 50g) still have a good solid molding outward appearance.Use the scaling powder of each embodiment, cooperate the Sn-3.9Ag-0.6Cu scolder to carry out spreadability test on L2 aluminium base and ni substrate, scolder is sprawled even light, spreading ratio result of the test such as following table 1.Spreading ratio is an index of estimating processing performances such as solder wettability, and spreading ratio numerical value height shows that then the wetability of scolder is good, and processing performance is good.From table 1 spreading ratio result as seen, embodiment 1 to 6 scaling powder and scolder are engaged in the al and ni substrate and all show well wetting and spreading ability.
Table 1 scaling powder cooperates the spreading ratio of Sn-3.9Ag-0.6Cu scolder on aluminium sheet and nickel plate
| The embodiment numbering | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Spreading ratio (L2 aluminium sheet) | 88％ | 91％ | 88％ | 84％ | 86％ | 90％ |
| Spreading ratio (ni substrate) | 81％ | 85％ | — | — | 80％ | — |
The method of testing of spreading ratio is as follows:
(1) will be heavily for after the Sn-3.9Ag-0.6Cu solder ball (diameter is about 4mm) of 0.5g is stained with the scaling powder of an amount of preparation, place on L2 aluminium sheet (or ni substrate) test film after the prior cleaning (dipping in acetone with absorbent cotton carries out decontamination and handle); L2 aluminium sheet (or ni substrate) test film is 40 millimeters (mm) squares of the length of side, and thickness is 1 millimeter (mm);
(2) aluminium sheet (or the nickel plate) test film that will be placed with scolder and scaling powder places temperature to be set on 260 ℃ the hot plate electric furnace and keeps about 30 seconds, guarantees scaling powder and melt solder balls and sprawls;
(3) take off test film from the hot plate electric furnace, clean the height after back measurement scolder is sprawled, and calculate spreading ratio.
The spreading ratio computing formula of scolder is as follows:
In formula (4), the formula (5), σ is the spreading ratio of scolder, and D is the diameter (cm) of scolder, and H is solder fusing and the average height after sprawling on the test film (cm), and w is the quality of scolder, and ρ is the density (g/m of scolder
3).
Claims (6)
1. scaling powder for aluminium soldering tin wire core, it is characterized in that: by weight percentage, its prescription consists of:
(1) modified rosin 14～28%
(2) ammonium fluoroborate 12～24%
(3) organic amine 38～56%
(4) the zinc source 4～10%
(5) tin salt 0.5～8%
(6) fluorine surfactant 0.1～2%
Described zinc source is zinc salt, zinc powder or activated zinc oxide;
Described organic amine is a kind of in diamines and the polyamine; Or described organic amine is multiple in monoamine, diamines and the polyamine, contains a kind of diamines or polyamine at least in wherein multiple; Described monoamine is monoethanolamine, diethanol amine or triethanolamine; Described diamines or polyamine are NN-dimethyl lauryl amine, beta-hydroxyethyl ethylenediamine, diethylamide, diethylene diamine, diethylenetriamine, triethylene tetramine, tri-n-octyl amine, tetramethylethylenediamine or diethylenetriamines;
Described tin salt is inorganic tin salt or organic acid tin salt;
Described fluorine surfactant is 1～2 kind among FC4430, FC4432, F5010, FSN-100, F501, F502 and the FS-300.
2. scaling powder for aluminium soldering tin wire core according to claim 1 is characterized in that: described modified rosin is 1～2 kind in Foral AXE perhydrogenated rosin, KE-604 rosin, KE-100 rosin, dimerization colophonium 145, KR-610 rosin, B140 newtrex, B115 newtrex, B90 newtrex, Polypale newtrex, ice galbanum, water-white rosin and the disproportionated rosin.
3. scaling powder for aluminium soldering tin wire core according to claim 1 is characterized in that: described zinc salt is inorganic zinc salt or organic acid zinc salt; Described inorganic zinc salt is ZnCl
2, ZnBr
2, ZnF
2, ZnBr
2Or Zn (BF
4)
2Described organic acid zinc salt is a zinc stearate.
4. scaling powder for aluminium soldering tin wire core according to claim 1 is characterized in that: described inorganic tin salt is SnCl
2, SnF
2, SnBr
2Or Sn (BF
4)
2
5. scaling powder for aluminium soldering tin wire core according to claim 1 is characterized in that: described organic acid tin salt is a stannous octoate.
6. the preparation method of the described scaling powder for aluminium soldering tin wire core of claim 1 is characterized in that: add ammonium fluoroborate, zinc source, tin salt, fluorine surfactant and organic amine by the described prescription proportion of claim 1 in reactor; Continuous stirring 30～45min makes raw material fully dissolve mixing under 80～100 ℃ of temperature; Add modified rosin then and simultaneously temperature is raised to 120～140 ℃ and the continuous 10～25min of stirring, obtain yellow transparent liquid; This liquid cools to room temperature is promptly obtained solid-state scaling powder for aluminium soldering tin wire core.
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