CN106825982A - A kind of anti-collapse leadless soldering tin paste of low viscosity and preparation method thereof - Google Patents
A kind of anti-collapse leadless soldering tin paste of low viscosity and preparation method thereof Download PDFInfo
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- CN106825982A CN106825982A CN201710067212.5A CN201710067212A CN106825982A CN 106825982 A CN106825982 A CN 106825982A CN 201710067212 A CN201710067212 A CN 201710067212A CN 106825982 A CN106825982 A CN 106825982A
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- soldering tin
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- tin paste
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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
- B23K35/22—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
- B23K35/40—Making wire or rods for soldering or welding
Abstract
The invention belongs to technical field of welding materials, disclose a kind of anti-collapse leadless soldering tin paste of low viscosity, the Pb-free coating glass putty contains cobalt and titanium, the scaling powder includes resin, activator, thixotropic agent and solvent, the resin is epoxy resin, the thixotropic agent is made up of aerosil, organobentonite and stearic amide, and the solvent is made up of propane diols, diethyl diethylene glycol dimethyl ether, cyclohexanone and ethyl acetoacetate.The invention also discloses the preparation method of the leadless soldering tin paste.The present invention adds cobalt in Pb-free coating glass putty, reduces viscosity, it is to avoid the phenomenon such as plug-hole and glutinous scraper, extends the solder(ing) paste resting period.Simultaneously by adding titanium, improve the means such as thixotropic agent and solvent, systematicness solve solder(ing) paste cave in, slump the problems such as.
Description
Technical field
The invention belongs to technical field of welding materials, more particularly to a kind of anti-collapse leadless soldering tin paste of low viscosity and its preparation
Method.
Background technology
Surface installation technique（SMT）It is a kind of technology and technique most prevailing in current electronic assembly industry, solder(ing) paste is
A kind of novel welding material arisen at the historic moment along with SMT.Solder(ing) paste is a system for complexity, is by solder powder, scaling powder
And the lotion of other additives mixeds.Solder(ing) paste has certain viscosity at normal temperatures, will can be glued at the beginning of electronic component
In commitment positions, under welding temperature, with the volatilization of solvent and portions additive, will be by weldering component and printed circuit pad
It is welded together to form permanently connected.
Solder(ing) paste is widely used in high-accuracy electronic component, wherein, on the one hand solder(ing) paste can cause electronics
Component and air insulated, and then realize isolation and anti-oxidation；On the other hand solder(ing) paste ensure that the weldering of electronic component
Connect performance by force, and then realize resistance high and prevent the effect of rosin joint phenomenon appearance.
The viscosity of solder(ing) paste is generally in 200Pa/s or so, it is however generally that, high-viscosity solder(ing) paste, solder joint is into pile-type effect
It is good, it is adapted to thin space printing；Low viscous solder(ing) paste, have in printing very fast whereabouts, the disposable brush of instrument, it is time saving the features such as.
Current leadless soldering tin paste easily sticks scraper, and this is also the common defect in typography of leadless soldering tin paste, causes scolding tin
The main cause of the glutinous scraper of cream is that solder(ing) paste viscosity is too big, and another major reason is that angle chemically is said, tin alloy powder
It is dispersed in scaling powder with ultrafine dust, tin alloy powder can be intimately associated and slow reaction occurs with scaling powder, becomes its performance
It is bad, it is therefore desirable to low-temp storage, and the time of storage can not be oversize.
Another too big consequence of solder(ing) paste viscosity is easily blocked in solder(ing) paste printing process, the solder(ing) paste of high viscosity
It is easily sticked on small hole wall, is easily detected by aperture after printing and intactly falls on circuit boards.
Although viscosity can be adjusted by changing whipping temp, time, the low viscosity solder(ing) paste meeting being obtained by
Collapse.In fact, it is also one of common undesirable condition of solder(ing) paste to collapse, caving in may cause the company of postwelding to be welded, especially
Be at thin space position, and solder joint displacement and element perpendicular upright stone tablet a problem that.In the phenomenon of caving in of solder(ing) paste, can be with
It is divided into two stages, stage is caving in before welding, and another stage is caving in heating process.
In Reflow Soldering preheating section, if solder(ing) paste heat resistanceheat resistant is caved in, effect is bad, before welding temperature（Solder starts melting
Before）The solder(ing) paste for having printed shaping starts to cave in, and some solder(ing) pastes are flowed to beyond pad.When weld zone is entered, solder starts
Melting, due to the effect of internal stress, solder(ing) paste is shrunk to solder joint and starts infiltration and rises to welding termination.Sometimes because solder flux lacks
Lose or other reasonses cause solder(ing) paste understrressing, there is the solder(ing) paste outside a small part pad not shrink back and come, it is current complete
Fusing is formed " tin sweat(ing) ".
Accordingly, it would be desirable to the problems such as researching and developing a kind of new solder(ing) paste to solve glutinous scraper, plug-hole, cave in.
The content of the invention
It is an object of the invention to provide a kind of anti-collapse, anti-oxidant, not plug-hole leadless soldering tin paste.
It is a further object of the present invention to provide the preparation method of the leadless soldering tin paste.
To reach one of above-mentioned purpose, the present invention uses following technical scheme：
A kind of anti-collapse leadless soldering tin paste of low viscosity, including Pb-free coating glass putty and scaling powder, the Pb-free coating glass putty contain cobalt and
Titanium, the scaling powder includes resin, activator, thixotropic agent and solvent, and the resin is epoxy resin, and the thixotropic agent is by gas phase
Silica, organobentonite and stearic amide composition, the solvent is by propane diols, diethyl diethylene glycol dimethyl ether, cyclohexanone and second
Ethyl acetoacetic acid ethyl ester is constituted.
Further, it includes 85 ~ 95 weight portion Pb-free coating glass puttys and 15 ~ 20 weight portion scaling powders.
Further, the Pb-free coating glass putty contains 5 ~ 10wt% cobalts and 0.1 ~ 0.4wt% titaniums.
Further, the Pb-free coating glass putty contains 88 ~ 94wt% tin, 0.5 ~ 3wt% silver, 0.2 ~ 0.5wt% copper, 5 ~ 10wt%
Cobalt and 0.1 ~ 0.4wt% titaniums.
Further, the composition of described scaling powder is：22~28wt% epoxy resin, 5~8wt% thixotropic agent, 4~8wt%
The solvent of activator and surplus.
Further, the scaling powder also includes antioxidant.
Further, the thixotropic agent is by 45wt% aerosils, 30wt% organobentonites and 25wt% stearic acid acyls
Amine is constituted.
Further, the solvent is by 20wt% propane diols, 22wt% diethyls diethylene glycol dimethyl ether, 40wt% cyclohexanones and 18wt% second
Ethyl acetoacetic acid ethyl ester is constituted.
Further, the activator is triethanolamine succinate and/or triethanolamine citrate.
A kind of method for preparing above-mentioned leadless soldering tin paste, comprises the following steps：
S1, resin and solvent are added reactor, heating stirring is to being completely melt；
S2, thixotropic agent and activator are sequentially added, stirring is obtained to being completely melt after being then cooled to room temperature and 36 ~ 72h of standing
Scaling powder；
S3, Pb-free coating glass putty and scaling powder are well mixed, obtain leadless soldering tin paste.
The invention has the advantages that：
1st, the present invention adds cobalt in Pb-free coating glass putty, and cobalt is a kind of big metal of density ratio tin, can make the density of solder(ing) paste
Appropriate increase, so as to reduce viscosity, it is to avoid the phenomenon such as plug-hole and glutinous scraper；And cobalt is a kind of excellent alloy material, with tin,
Copper etc. can form intermetallic compound, prevent tin alloy powder from being chemically reacted with solder flux, extend the solder(ing) paste resting period.
2nd, the present invention adds titanium in Pb-free coating glass putty, and titanium is a kind of high duty metal, and with fairly good extension
Property, the addition of a small amount of titanium can ensure solder(ing) paste situations such as being also not in slump in the case of low viscosity, caving in；Titanium has simultaneously
There is excellent resistance to corrosion, acid, the erosion of oxygen can be prevented, it is ensured that pad consolidates firm.
3rd, the formula by optimizing scaling powder of the invention, low viscosity solder(ing) paste is solved well, and easily collapsing for appearance is asked
Topic.Research finds, in caving in before welding, thixotropic agent plays very important effect, and the present invention is specific by compounding three kinds
The thixotropic agent of consumption, can strengthen the thixotropy of soldering paste, the phenomenon such as prevent from hangover, adhesion in press occur, cave in；It is heated
Caving in journey is then closely related with solvent, is the key point for preventing solder(ing) paste heat to cave in from appropriate solvent, appropriate
Solvent is arranged in pairs or groups including appropriate consumption and appropriate species, and considers the compatibility of solvent and other materials in whole system,
Be not in that heat is caved in phenomenon to ensure in the heating period, the present invention is by compounding the relatively low alcohols of specific consumption, boiling point, ether
Class, ketone, esters solvent solve this problem, and in heating, the gap that low boiling point solvent can pass through between welding powder evaporate into weldering
Outside cream, the gap that just can pass through between welding powder is evaporate into outside soldering paste, and now the deformation extent of soldering paste is simultaneously little, whole shaping
Also persistently overheating and remain to and be completely melt, final solder paste all arrives at the surface of solder joint to soldering paste, and welds in this process
Cream does not occur phenomenon of caving in, and has been finally completed welding, whereas if using high boiling solvent, because it is difficult to volatilize, meeting
Expansion leaves bubble, ultimately results in and has printed the soldering paste of shaping and cave in.
4th, the present invention uses epoxy resin in scaling powder, and solder(ing) paste can be made to have good adhesiveness, and certain journey
Printed circuit board (PCB) can be prevented to be oxidized on degree, epoxy resin is a kind of thermosetting resin, can prevent slump；Antioxidant plus
Enter also for playing anti-oxidation effect.
Specific embodiment
With reference to specific embodiment, the present invention is described further.
Embodiment 1
A kind of anti-collapse leadless soldering tin paste of low viscosity, including 85kg Pb-free coatings glass putty and 20kg scaling powders, the group of Pb-free coating glass putty
Turn into：88wt% tin, 2.1wt% silver, 0.5wt% copper, 9wt% cobalts and 0.4wt% titaniums, the composition of scaling powder is：22wt% epoxy resin,
8wt% thixotropic agent, 8wt% activators and 62wt% solvents, thixotropic agent by 45wt% aerosils, 30wt% organobentonites and
25wt% stearic amides are constituted, and solvent is by 20wt% propane diols, 22wt% diethyls diethylene glycol dimethyl ether, 40wt% cyclohexanones and 18wt% second
Ethyl acetoacetic acid ethyl ester is constituted, and activator is triethanolamine succinate.
Leadless soldering tin paste is prepared according to following steps：
S1, propane diols, diethyl diethylene glycol dimethyl ether, cyclohexanone and ethyl acetoacetate are re-dubbed mixed solvent according to quantity, by asphalt mixtures modified by epoxy resin
Fat and mixed solvent add reactor, and heating stirring is to being completely melt；
S2, aerosil, organobentonite and stearic amide are re-dubbed mixing thixotropic agent according to quantity, sequentially add mixing
Thixotropic agent and activator, stirring obtain scaling powder to being completely melt after being then cooled to room temperature, and 36 ~ 72h of standing；
S3, Pb-free coating glass putty and scaling powder are placed and be thoroughly mixed in de-airing mixer uniform, obtain leadless soldering tin paste.
Embodiment 2
A kind of anti-collapse leadless soldering tin paste of low viscosity, including 91kg Pb-free coatings glass putty and 18kg scaling powders, the group of Pb-free coating glass putty
Turn into：94wt% tin, 0.5wt% silver, 0.2wt% copper, 5.2wt% cobalts and 0.1wt% titaniums, the composition of scaling powder is：28wt% asphalt mixtures modified by epoxy resin
Fat, 5wt% thixotropic agent, 4wt% activators and 63wt% solvents, thixotropic agent is by 45wt% aerosils, 30wt% organobentonites
With 25wt% stearic amides composition, solvent is by 20wt% propane diols, 22wt% diethyls diethylene glycol dimethyl ether, 40wt% cyclohexanones and 18wt%
Ethyl acetoacetate is constituted, and activator is triethanolamine succinate.
Prepared according to step same as Example 1.
Embodiment 3
A kind of anti-collapse leadless soldering tin paste of low viscosity, including 95kg Pb-free coatings glass putty and 15kg scaling powders, the group of Pb-free coating glass putty
Turn into：91.4wt% tin, 3wt% silver, 0.4wt% copper, 5wt% cobalts and 0.2wt% titaniums, the composition of scaling powder is：25wt% epoxy resin,
6wt% thixotropic agent, 5wt% activators, 63wt% solvents, 1wt% antioxidant, thixotropic agent are had by 45wt% aerosils, 30wt%
Machine bentonite and 25wt% stearic amides are constituted, and solvent is by 20wt% propane diols, 22wt% diethyls diethylene glycol dimethyl ether, 40wt% cyclohexanones
With 18wt% ethyl acetoacetates composition, activator is triethanolamine citrate.
Prepared according to step same as Example 1.
Embodiment 4
A kind of anti-collapse leadless soldering tin paste of low viscosity, including 88kg Pb-free coatings glass putty and 16kg scaling powders, the group of Pb-free coating glass putty
Turn into：88.2wt% tin, 1.2wt% silver, 0.3wt% copper, 10wt% cobalts and 0.3wt% titaniums, the composition of scaling powder is：25wt% asphalt mixtures modified by epoxy resin
Fat, 7wt% thixotropic agent, 6wt% activators, 61wt% solvents, 1wt% antioxidant, thixotropic agent is by 45wt% aerosils, 30wt%
Organobentonite and 25wt% stearic amides are constituted, solvent by 20wt% propane diols, 22wt% diethyls diethylene glycol dimethyl ether, 40wt% rings
Ketone and 18wt% ethyl acetoacetates are constituted, and activator is triethanolamine succinate and triethanolamine citrate.
Prepared according to step same as Example 1.
Embodiment 5
A kind of anti-collapse leadless soldering tin paste of low viscosity, including 90kg Pb-free coatings glass putty and 18kg scaling powders, the group of Pb-free coating glass putty
Turn into：90wt% tin, 1.5wt% silver, 0.3wt% copper, 8wt% cobalts and 0.2wt% titaniums, the composition of scaling powder is：26wt% epoxy resin,
6wt% thixotropic agent, 8wt% activators, 59wt% solvents, 1wt% antioxidant, thixotropic agent are had by 45wt% aerosils, 30wt%
Machine bentonite and 25wt% stearic amides are constituted, and solvent is by 20wt% propane diols, 22wt% diethyls diethylene glycol dimethyl ether, 40wt% cyclohexanones
With 18wt% ethyl acetoacetates composition, activator is triethanolamine citrate.
Prepared according to step same as Example 1.
Comparative example 1
A kind of anti-collapse leadless soldering tin paste of low viscosity, substantially the same manner as Example 1, difference is, no in Pb-free coating glass putty to add
Enter cobalt.
Comparative example 2
A kind of anti-collapse leadless soldering tin paste of low viscosity, substantially the same manner as Example 1, difference is, no in Pb-free coating glass putty to add
Enter titanium.
Comparative example 3
A kind of anti-collapse leadless soldering tin paste of low viscosity, substantially the same manner as Example 1, difference is, in scaling powder, thixotropic agent is hard
Resin acid acid amides, solvent is propane diols.
Performance test
The solder(ing) paste sealing preserve that will be prepared monthly tests a solder(ing) paste viscosity in 3~8 DEG C of refrigerators, and record viscosity becomes
The time used characterizes shelf-life of solder(ing) paste when changing 20%.
Viscosity is according to IPC-TM-650（2.4.34）Method of testing, at 25 ± 1 DEG C, using NDJ-7 type rotary viscosimeters
Meter is continuously rotated 2 minutes with 7.5 revs/min, reading after stabilization.
What thixotropic index Ti reflected is the speed degree that solder(ing) paste changes form under external force, general good Ti values
0.4~0.6 or so.
Viscosity not recovery rate R reflection be that solder(ing) paste returns to the ability of original state when external force reduces.R values can be
Negative value, zero and on the occasion of.When R be on the occasion of when, reflection when act on solder(ing) paste external force reduce or disappear when, solder(ing) paste can not be fast
Speed can not return to original state.With the extension of printing time, solder(ing) paste shows as the shape that trickles to namely what is often called, now easily
Cause tin sweat(ing) or company's tin phenomenon caused by solder(ing) paste trickling to pad outward；Optimal printing state as R=0, i.e., as
When reducing or disappear for the external force of solder(ing) paste, solder(ing) paste can quickly recover to original state；When R is negative value, numerical value is bigger,
Then with the extension of printing time, the viscosity of solder(ing) paste is bigger, and it is poor to easily cause solder(ing) paste rollability, and lower tin is difficult, is to increase
Lower tin amount, frequently with scraper dynamics is increased, but further results in steel mesh deformation, it is easier to cause weld defect.
After Solder-Paste Printing, under uniform temperature and damp condition, due to the effect of gravity and surface tension, figure is caused to collapse
Fall and outwardly extended from original boundary.This slump can cause the slime flux of soldering paste, be bridged between causing the pin in welding process
Defect.According to IPC-TM-650（2.4.35）Using 0.1mm thickness templates, heat is carried out and has collapsed experiment（In 150 ± 10 DEG C of metal hot plates
It is upper to place 10 minutes）.
Tin sweat(ing) is tested and detected by JIS.Z.3284 annex ten, according to grade classification, can be divided into 4 grades, etc.
Level one is required without tin sweat(ing)；Grade two requires that tin sweat(ing) quantity is necessarily less than 3, and size is no more than 75 μm；Grade three requires tin
Pearl quantity is more than 3 but not cyclic, and size requirement is no more than 75 μm.
Copper, Cu corrosion detection method：JIS.Z.3284 annex four；Wetting is determined with reference to the 2.4.45 methods of ICP TM 650
Property；Tenor is detected by JIS.Z.3282 methods.
The leadless soldering tin paste of embodiment 1 ~ 5 carries out printing performance test, as a result such as following table：
As seen from the above table, the present invention adds cobalt by Pb-free coating glass putty, reduces the viscosity of solder(ing) paste, solves glutinous scraping
The problems such as knife, plug-hole, while extending the shelf-life of solder(ing) paste.Comparative example 1 does not add metallic cobalt, and viscosity is larger, it is impossible to avoid
Glutinous scraper, the appearance of plug-hole.The present invention is improved by adding titanium in Pb-free coating glass putty to thixotropic agent and solvent, is
That unites solves the problem that solder(ing) paste caves in, and the minimum of solder(ing) paste caves in position for 0.15mm, 0.125mm, it is adaptable to ultra-fine
Away from solder(ing) paste print production, thixotropic index is suitable, does not have tin sweat(ing) phenomenon；Comparative example 2 does not add titanium, it is impossible to solve weldering very well
The problem that tin cream caves in, for 0.35mm, 0.20mm, recovery rate is not bigger than normal for viscosity, and tin sweat(ing) occurs for the position that caves in of solder(ing) paste；
Although the addition titanium of comparative example 3, use single thixotropic agent and solvent, the position only 0.30mm that caves in of solder(ing) paste,
0.175mm, thixotropic index deviates normal value, and recovery rate is not bigger than normal for viscosity, and tin sweat(ing) occurs.Leadless soldering tin paste of the invention is same
When it is up to standard with good wetability, tenor, tolerate copper, Cu corrosion.
The above, specific embodiment only of the invention, but protection scope of the present invention is not limited thereto, and it is any
Belong to those skilled in the art the invention discloses technical scope in, the change or replacement that can be readily occurred in, all should
It is included within the scope of the present invention.Therefore, protection scope of the present invention should be defined by scope of the claims.
Claims (10)
1. a kind of anti-collapse leadless soldering tin paste of low viscosity, including Pb-free coating glass putty and scaling powder, it is characterised in that the Pb-free coating
Glass putty contains cobalt and titanium, and the scaling powder includes resin, activator, thixotropic agent and solvent, and the resin is epoxy resin, described
Thixotropic agent is made up of aerosil, organobentonite and stearic amide, and the solvent is by propane diols, diethanol diformazan
Ether, cyclohexanone and ethyl acetoacetate composition.
2. leadless soldering tin paste according to claim 1, it is characterised in that it include 85 ~ 95 weight portion Pb-free coating glass puttys and
15 ~ 20 weight portion scaling powders.
3. leadless soldering tin paste according to claim 1, it is characterised in that the Pb-free coating glass putty contain 5 ~ 10wt% cobalts and
0.1 ~ 0.4wt% titaniums.
4. leadless soldering tin paste according to claim 3, it is characterised in that the Pb-free coating glass putty contain 88 ~ 94wt% tin,
0.5 ~ 3wt% silver, 0.2 ~ 0.5wt% copper, 5 ~ 10wt% cobalts and 0.1 ~ 0.4wt% titaniums.
5. leadless soldering tin paste according to claim 1, it is characterised in that the composition of described scaling powder is：22~28wt%
The solvent of epoxy resin, 5~8wt% thixotropic agent, 4~8wt% activators and surplus.
6. leadless soldering tin paste according to claim 1, it is characterised in that the scaling powder also includes antioxidant.
7. leadless soldering tin paste according to claim 1, it is characterised in that the thixotropic agent by 45wt% aerosils,
30wt% organobentonites and 25wt% stearic amides are constituted.
8. leadless soldering tin paste according to claim 1, it is characterised in that the solvent is by 20wt% propane diols, 22wt% bis-
Dimethylamino ethanol ether, 40wt% cyclohexanones and 18wt% ethyl acetoacetates composition.
9. leadless soldering tin paste according to claim 1, it is characterised in that the activator is triethanolamine succinate
And/or triethanolamine citrate.
10. the method that one kind prepares the leadless soldering tin paste described in claim 1 ~ 9 any one, it is characterised in that including following
Step：
S1, resin and solvent are added reactor, heating stirring is to being completely melt；
S2, thixotropic agent and activator are sequentially added, stirring is obtained to being completely melt after being then cooled to room temperature and 36 ~ 72h of standing
Scaling powder；
S3, Pb-free coating glass putty and scaling powder are well mixed, obtain leadless soldering tin paste.
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| CN107745202A (en) * | 2017-06-23 | 2018-03-02 | 深圳市福英达工业技术有限公司 | Tinbase paste soldering solder and preparation method thereof |
| CN111037148A (en) * | 2020-01-07 | 2020-04-21 | 电子科技大学 | Soldering tin for rapidly conducting micro via hole and production process thereof |
| JP2020163404A (en) * | 2019-03-28 | 2020-10-08 | パナソニックＩｐマネジメント株式会社 | Solder paste and mounting structure |
| CN114799615A (en) * | 2022-04-06 | 2022-07-29 | 深圳先进电子材料国际创新研究院 | Silver powder surface modification method, silver solder paste, and preparation method and application of silver solder paste |
| CN115673598A (en) * | 2022-10-29 | 2023-02-03 | 江苏三沃电子科技有限公司 | Preparation process of soldering paste |
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