CN102513734B - Method for preparing paste soldering flux - Google Patents
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Abstract
The invention provides a method for preparing a paste soldering flux. The soldering flux comprises the following raw materials: resin, a solvent, an amine activating agent, a thixotropic agent, an organic acid activating agent and a corrosion inhibitor. The preparation method comprises the following steps of: a) stirring the resin and the solvent, heating until the resin is dissolved completely, cooling, adding the amine activating agent, and stirring until the amine activating agent is dissolved completely; b) adding the thixotropic agent, and emulsifying and dispersing by using emulsification equipment at constant temperature, so that the thixotropic agent forms a thixotropic gel network structure; c) adding the organic acid activating agent, reacting with the amine activating agent to form a salt compound, and adding the corrosion inhibitor and stirring to dissolve the salt compound; and d) stirring and cooling slowly to room temperature to obtain the paste soldering flux. The prepared paste soldering flux is mainly applied to soldering paste formed by stirring and mixing the paste soldering flux and superfine solder powder under vacuum, and has high heat collapse resistance, and high viscosity stability in the processes of storage and printing to avoid the 'post-thickening' phenomenon.
Description
Technical field
The invention belongs to electronics industry solder and use solder(ing) paste field, be specifically related to a kind of preparation method of paste soldering flux.This scaling powder is mainly used in prepares solder(ing) paste, is particularly useful for the surface mount process of electronics industry.
Background technology
Electronics industry will be installed to a large amount of electronic devices and components on printed circuit board by the mode of welding.Good solder joint reliably forms needs the scolder of melting to infiltrate in very clean metal surface, diffusion and metallurgical binding.And the metal surface of printed circuit board, electronic devices and components or soldered material oxidized possibility in the links such as manufacture, storage, transport is almost 100%.Thereby, electronics industry is very crucial to the processing of welding material surface oxide layer in producing, often need to use a large amount of oxide layer of weldering chemicals to metal surface and pollutants of helping clean to increase wetting, accelerate the process of welding, thereby improve the yield of production and the reliability of product.
The a large amount of welding processing procedures that use of electronics industry have two kinds, and one is wave-soldering, and another kind is Reflow Soldering.Wave-soldering process is applicable to placing components, and the wlding material that helps of use is called scaling powder or liquid scaling powder.Reflow Soldering processing procedure is applicable to Surface Mount Component, and the wlding material that helps of use is called solder(ing) paste or tin cream.Solder(ing) paste is the body of paste with certain viscosity and thixotropic behavior being mixed together by superfine alloy solder powder (20-75 micron) and paste soldering flux (weld-aiding cream).The paste performance of solder(ing) paste can apply to automatic printing equipment, therefore can realize at a high speed, large batch of production.In the time of mount components, solder(ing) paste, as the adhesives between component lead (or electrode) and printed board pad, locates element in printed board; In the time of reflow welding, the alloy powder fusing in solder(ing) paste forms solder joint later between component lead and pad, completes the double action of electrical connection and mechanical connection.
Paste soldering flux comprises resin, thixotropic agent, solvent, activator, corrosion inhibiter and other auxiliary agents.Scaling powder has two functions in solder(ing) paste: the one, help welding, in the time being heated, remove metal oxide, in scaling powder, need to add activator (for example: the organic amines such as organic acid, triethanolamine such as succinic acid), the 2nd, as the carrier of solder powder, scaling powder need add resin, solvent etc. and be deployed into suitable paste.
Scaling powder need add thixotropic agent so that it possesses rheological properties, thereby makes scaling powder possess following function: 1) in the time of storage and use, can be used as the carrier that solder powder suspends; 2), in solder(ing) paste typography, solder(ing) paste is easily flowed in printing, but can not flow after being completed for printing; 3) in reflux course, be heated and there will not be slump, and then reduce the bridge joint phenomenon of welding.The common thixotropic agent using in solder(ing) paste has: rilanit special, modified hydrogenated castor oil, stearic amide, ethylenebis stearic amide etc.
Slump is one of important indicator of solder(ing) paste.Solder(ing) paste slump related check method has: 1) China " tin lead plaster shape scolder general specification " (SJ/T 11186-1998); 2) U.S.'s " soldering paste requirement " (IPC/J-STD-005); 3) Japan " soldering paste requirement " (JIS Z3284).In these detection methods, all specified two kinds of test conditions, a kind of is the test board that is printed with soldering paste figure to be placed in to the environment that temperature is (50 ± 10) % for (25 ± 5) DEG C, relative humidity stop 10-15 minute, is referred to as cold slump test; The second is that the test board that is printed with soldering paste figure is placed in to 10-15 minute under the condition that temperature is (150 ± 10) DEG C, is referred to as hot slump.Solder(ing) paste produces slump a lot of reasons, and the main cause that causes cold slump is because solder(ing) paste thixotropy is too low caused.Hot slump refers to the rising along with printed circuit board temperature in reflux course, solder(ing) paste reduced viscosity, and the gel thixotroping structural failure that thixotropic agent forms, paste soldering flux has lost the enabling capabilities to solder powder, and there is avalanche in solder(ing) paste printed pattern.Heat resistanceheat resistant slump refers to that solder(ing) paste kept the ability of the shape of solder(ing) paste in the time of printing before solder fusing, shape when most solder(ing) paste use occasions all requires the front maintenance printing of solder fusing.
Modified hydrogenated castor oil is widely used in coating, ink industry as thixotropic agent, thickener, is mainly used in improving levelability, the anti-sag performance of coating, ink.In coating, ink industry, be applicable to medium polar solvent as the modified hydrogenated castor oil of thixotropic agent and use, simple high speed dispersion can reach the effect of high thixotroping, anti-sag.It is common in solder(ing) paste scaling powder, using modified hydrogenated castor oil to do thixotropic agent, has patent and documents and materials to look into.It improves the know-why of the anti-slump ability of lotion with similar at coating, ink industry anti-sag performance.But under general operation, can only solve the cold slump problem of solder(ing) paste, can not the hot slump problem of fine solution.
The stability that three kinds of glass putty surface treatment methods improve tin cream is disclosed in patent CN1123210A.This patent does not relate to flux composition.In patent CN1184017A, point out, the poly-halogen aliphatic compound with 10 more than carbon atom or ester ring type compound are as activator, and the solder(ing) paste that allotment forms so had both had good wettability and had good bin stability.By repeating this patent working example, we find its printing particularly heat resistanceheat resistant slump be not very good.Patent CN100336626C discloses a kind of rosin halogen-free scaling powder for lead-free soldering paste, improve and helped weldering performance by optimization of C/C composites, solved the serious problem of high-temperature oxydation, by repeating this patent working example, we find that its heat resistanceheat resistant slump is not very good.
Provide the technology path of the good heat resistanceheat resistant slump of solder(ing) paste to mainly contain two kinds.One of technology path is to select conventional thixotropic agent to use under relatively simple dispersion and emulsion technique, and in formulations of solder flux, adding room temperature or low temperature has the activator of removing oxide ability.Technique has two kinds conventionally: 1) cooling after heating for dissolving together with the component such as rosin, solvent, cooling rear use three-roll grinder grinds sometimes; 2) cooling after the component such as rosin, solvent heating for dissolving, use high-speed emulsifying machine to carry out dispersion and emulsion at 40-60 degree temperature, low rate mixing is cooling afterwards.In above-mentioned two kinds of techniques, solder(ing) paste is well positioned to meet and solder powder is suspended and solve cold slump problem, but heat resistanceheat resistant slump poor performance, the activator adding has the ability of removing glass putty oxide on surface under room temperature or low temperature, the oxide of glass putty is removed between rear glass putty particle and produces cohesiveness, makes solder(ing) paste be unlikely to occur avalanche.Article 2 technology path is preferred suitable thixotropic agent, regulate appropriate solvent polarity, adopt appropriate dispersion and emulsion technique, even if the gel thixotroping structure that thixotropic agent is formed is heated to 150 DEG C of above high temperature, still do not lose efficacy, sustainable to solder powder generation supporting role, there is not avalanche in printed pattern.Article 1, the activator adding in route formulations of solder flux has stronger removal oxide ability in room temperature or low temperature, and in storage and printing process, glass putty oxide on surface is removed, clean metal surface will produce strong cohesiveness, cause the viscosity of solder(ing) paste to improve, when serious, solder(ing) paste loses flowability and can not print smoothly, and solder(ing) paste must refrigerate stores the variation that slows down viscosity.There is not this situation in Article 2 route, solder(ing) paste can add under room temperature or low temperature without the activator of removing oxide ability, activator at high temperature just performance remove oxide effect, solder(ing) paste changes minimum from the viscosity that is stored to printing and produces, can realize the storage at normal temperature of solder(ing) paste.Patent, document that solder(ing) paste solves hot slump problem employing Article 2 route are little.Patent CN 100349688C points out, the cold-and-heat resistent slump that the composite rheology system that two Asias (to methyl) benzyl D-sorbite with fusing point up to 245-250 DEG C is main body can improve solder(ing) paste, this patent emphasis has been told about the composition of composite rheology system, does not relate to its preparation method.
" rear thickening " is the FAQs of coating material production.Thickening definition after coating: the phenomenon that after coating preparation, viscosity constantly changes in storage process.Prepared by solder(ing) paste also can produce similar phenomenon in some situation.For example: use rilanit special as thickener, add a large amount of soluble amine compounds in formulations of solder flux, the paste soldering flux preparing and solder(ing) paste all can be As time goes on and viscosity rise at lay up period.The true cause that solder(ing) paste preparation produces " rear thickening " phenomenon is unknown, can explain like this understanding of " rear thickening " phenomenon with reference to coating industry: soluble amine compounds provides a large amount of polar groups in scaling powder, these polar groups help thixotropic agent to form gel thixotroping structure in scaling powder emulsion dispersion production process, have the effect of thickening, thixotroping.But store and stir into follow-up continuous the playing a role of solder(ing) paste at scaling powder, form new gel thixotroping structure, make viscosity rise.
Summary of the invention
For above-mentioned deficiency of the prior art, the object of the present invention is to provide a kind of preparation method of paste soldering flux, prepared paste soldering flux is mainly used in ultra-fine solder powder and is mixed to form the prepared solder(ing) paste of solder(ing) paste by vacuum stirring, there is good heat resistanceheat resistant slump, in storage and printing process, there is good viscosity stability simultaneously, avoid producing " rear thickening " phenomenon.
For achieving the above object, the present invention is achieved by the following technical solutions:
A preparation method for paste soldering flux, the raw material of preparing this paste soldering flux comprises: resin, solvent, amine activator, thixotropic agent, organic acid for activating agent and corrosion inhibiter.
The method of preparing scaling powder comprises the steps:
A) resin and stirring solvent are heated to after resin dissolves completely and are cooled to 80 DEG C ± 2 DEG C, then add amine activator to be stirred to completely to dissolve;
B) add thixotropic agent, with emulsifying device constant temperature emulsion dispersion at 50 DEG C ± 2 DEG C, make thixotropic agent form thixotropy gel network structure;
C) add organic acid for activating agent, react with amine activator and generate salt compounds, then add corrosion inhibiter stirring and dissolving salt compounds;
D) low rate mixing is cooled to room temperature and obtains paste soldering flux.
Above-mentioned resin is selected from the one in newtrex, Foral, modified rosin or acrylic rosin, and the addition of resin is the 20-60% of scaling powder gross mass.
The boiling point of above-mentioned solvent is 200-300 DEG C, and described solvent is that the weak solvent of solvent that a kind of polarity is stronger and a kind of polarity is composite.The solvent that described polarity is relatively strong is alcohols solvent, ester class organic solvent, alcohol ether solvent, and the relatively weak solvent of described polarity is hydrocarbon class organic solvent or aromatic organic solvent.Amount of solvent is the 20-50% of scaling powder gross mass.
Above-mentioned thixotropic agent is modified hydrogenated castor oil, and the addition of thixotropic agent is the 3-8% of scaling powder gross mass.
Above-mentioned amine activator is the one in MEA, diethanol amine, triethanolamine, N-methylimidazole, N-ethyl imidazol(e), phenylimidazole, 2-ethyl imidazol(e) or cyclohexylamine preferably, and the addition of amine activator is the 2-5 % of scaling powder gross mass.
Above-mentioned organic acid for activating agent is selected from the one in malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, malic acid or maleic acid.
Above-mentioned corrosion inhibiter is selected from the one in 1,2,3-benzotriazole, benzimidazole or TTA, and the addition of corrosion inhibiter is the 0.05-10 % of scaling powder gross mass.
In addition, prepare in the raw material of this paste soldering flux and can also comprise antioxidant or lubricant, to strengthen the anti-oxidant or greasy property of scaling powder.
The invention has the beneficial effects as follows: in preparation process, first resin, solvent are added in reactor, to be stirred and heated to resin and to dissolve completely, then cooling, then add amine activator to be stirred to completely to dissolve.Add thixotropic agent and use high speed shear emulsifying device to carry out constant temperature emulsion dispersion, under emulsify at a high speed condition, thixotropic agent forms prosperity and has thixotropy gel network structure, the amine activator adding can improve the polarity of rosin solution, promote the formation of gel network structure, make thixotropic agent activate more fully and shorten the soak time of modified hydrogenated castor-oil plant oils thixotropic agent.After emulsify at a high speed a period of time, thixotropic agent activated, add again organic acid for activating agent, organic acid for activating agent produces chemical reaction with the amine activator adding before and forms salt compounds, salt compounds is separated out in the mode of small grains, add other auxiliary agent stirring and dissolving such as corrosion inhibiter, the last cooling paste soldering flux that obtains of low rate mixing.Paste soldering flux and Alloy soldering powder stir and can make finished product solder(ing) paste with planetary mixer after proportioning by a certain percentage.Add organic acid for activating agent by strict calculating, appropriateness is excessive, amine activator is almost all separated out, and recovers the initial polarity of solution, slows down thixotropic agent and continues to form gel thixotroping structure, has avoided rear thickening phenomenon.The prepared solder(ing) paste thixotropy of this method is good, and heat resistanceheat resistant slump is improved significantly, and solder(ing) paste is at long time stored viscosity stabilization, and other aspect performances such as printing, welding also meet.
Specifically, can be to obtain by centrifugal or ultrasonic atomization process atomization or screening for stirring the solder powder of solder(ing) paste.Solder powder is normally spherical, and granular size, with conventional used identical, is generally 25-45 μ m, 20-38 μ m or thinner.Selected solder alloy is also not particularly limited, can uses traditional Sn63Pb37, Sn62Pb36Ag2 alloy, also can use novel lead-free alloy, for example: SnAgCu, SnAg, SnBi, SnBiCu, SnBiAg, SnBiCuSb etc.These solder alloys also can comprise one or more Bi, In, Ag, Ni, Co, Mo, Fe, P, Ge or analog.
In addition, the boiling point of solvent that the present invention adopts is preferably 200-300 DEG C, available alcohols, alcohol ethers, ester class, hydrocarbon class or aromatic organic solvent, for example: diethylene glycol (DEG), triethylene glycol, ethohexadiol, diethylene glycol monobutyl ether, diethylene glycol monohexyl ether, diethylene glycol list octyl ether, dibutyl ethylene glycol ether, DGDE, propane diols phenylate, dimethylbenzene etc.Diethylene glycol (DEG), the dissolution with solvents rosin that triethylene glycol isopolarity is relatively strong, activator ability is strong, and the salt that can cause acid amide neutralization reaction to generate is not separated out, and it is unsuitable using separately.There is too poor or poor with the solder powder compatibility phenomenon of rosin dissolubility in the relatively weak solvent of hydrocarbon class, aromatic series isopolarity.The present invention preferably mixing of two kind solvents is composite, and amount of solvent is the 20-50 % of scaling powder quality.
Further, thixotropic agent of the present invention is modified hydrogenated castor oil, can on market, buy this product.Example comprises: CRAYVALLAC SF(CRAY VALLEY company), Luvotix R-RF (Lehmann & Voss & Co. KG), RC-HST(Changxing consonance macromolecular material Co., Ltd) etc., the preferred addition of thixotropic agent is the 3-8% of scaling powder quality.
Organic acid for activating agent of the present invention is preferably from organic acids such as malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, malic acid, maleic acids.The addition of organic acid for activating agent is through strict calculating, calculate the amido quantity of amine activator, draw for and the quantity of the required organic acid for activating agent of amido carboxyl, extrapolate organic acid addition, actual addition is preferably 105%-130%, the organic acid addition obtaining based on reckoning.
The reactor using in the preparation of scaling powder is with heat conduction chuck, admittance deep fat in chuck, and conduction oil temperature can be controlled automatically by temperature controlling instruments, realizes the control to material in reactor temperature.Described reactor is accompanied with three groups of rabbling mechanisms, and one group is that anchor formula stirs for scraping wall, for the heat exchange of strength imparting material and conduction oil; One group is zigzag rabbling mechanism, together with stirring, reaches vigorous stirring material with anchor formula, accelerate dissolution, and without dead angle; The 3rd group is high-shearing dispersion emulsifying machine structure, for high cut disperse emulsification.
Detailed description of the invention
Describe the present invention in detail by embodiment and comparative example below, by the verification test of embodiment and comparative example, the remarkable effect that the present invention reaches is described, referring to table 1.Implement mode of the present invention and be not limited to embodiment, and only illustrate.
The component of the each scaling powder of table 1 and content proportioning
Embodiment 1 preparation technology:
By rosin, solvent adds in reactor, open anchor formula paddle and zigzag paddle, be stirred and heated to 150 DEG C, after dissolving completely, rosin is cooled to 80 DEG C, adding amine activator to be stirred to completely dissolves, be cooled to 50 DEG C, add Powdered thixotropic agent, open high-speed shearing emulsion machine structure and at 50 DEG C, carry out constant temperature emulsion dispersion 2 hours, thixotropic agent has activated, closing high-speed emulsification pretreatment mechanism, add organic acid for activating agent, corrosion inhibiter, and continue to open anchor formula paddle and sawtooth paddle and stir 1 hour, make organic acid for activating agent and the abundant chemical reaction of amine activator.Close sawtooth paddle, keep anchor formula to stir and open, when cooling down, vacuumize, be cooled to 25 DEG C, and grind with three-roll grinder, detect with the agent of scraper plate fineness, lotion fineness is less than 10 μ m and gets final product to obtain paste soldering flux.
Comparative example 1 preparation technology:
Rosin, solvent are added in reactor, open anchor formula paddle and zigzag paddle, be stirred and heated to 150 DEG C, add while hot amine activator, organic acid for activating agent, thixotropic agent, corrosion inhibiter stirring and dissolving, after dissolving completely, close sawtooth paddle, keeping anchor formula to stir opens, when cooling down, vacuumize, be cooled to 25 DEG C, and grind with three-roll grinder, detect with the agent of scraper plate fineness, lotion fineness is less than 10 μ m and gets final product to obtain paste soldering flux.
Comparative example 2 preparation technologies:
By rosin, solvent adds in reactor, open anchor formula paddle and zigzag paddle, be stirred and heated to 150 DEG C, after dissolving completely, rosin is cooled to 80 DEG C, add amine activator simultaneously, organic acid for activating agent, corrosion inhibiter is stirred to completely and dissolves, be cooled to 50 DEG C, add Powdered thixotropic agent, open high-speed shearing emulsion machine structure and at 50 DEG C, carry out constant temperature emulsion dispersion 2 hours, thixotropic agent has activated, closing high-speed emulsification pretreatment mechanism, close sawtooth paddle, keeping anchor formula to stir opens, when cooling down, vacuumize, be cooled to 25 DEG C, and grind with three-roll grinder, detect with the agent of scraper plate fineness, lotion fineness is less than 10 μ m and gets final product to obtain paste soldering flux.
Comparative example 3 preparation technologies:
By rosin, solvent adds in reactor, open anchor formula paddle and zigzag paddle, be stirred and heated to 150 DEG C, after dissolving completely, rosin is cooled to 80 DEG C, adding amine activator to be stirred to completely dissolves, be cooled to 50 DEG C, add Powdered thixotropic agent, open high-speed shearing emulsion machine structure and at 50 DEG C, carry out constant temperature emulsion dispersion 2 hours, thixotropic agent has activated, closing high-speed emulsification pretreatment mechanism, add organic acid for activating agent, corrosion inhibiter, and continue to open anchor formula paddle and sawtooth paddle and stir 1 hour, make organic acid for activating agent and the abundant chemical reaction of amine activator.Close sawtooth paddle, keep anchor formula to stir and open, when cooling down, vacuumize, be cooled to 25 DEG C, obtain paste soldering flux.
Comparative example 4 preparation technologies:
Rosin, solvent are added in reactor, open anchor formula paddle and zigzag paddle, be stirred and heated to 150 DEG C, add while hot thixotropic agent, amine activator, organic acid for activating agent, corrosion inhibiter stirring and dissolving, after dissolving completely, close sawtooth paddle, keep anchor formula to stir and open, when cooling down, vacuumize, be cooled to 25 DEG C to get final product to obtain paste soldering flux.
Embodiment and comparative example gained paste soldering flux are fully uniformly mixed to production solder(ing) paste with tinbase spherical solder powder vacuumizing respectively under condition.Using more common low cost lead-free solder powder SnAg0.3Cu0.7(particle diameter 25-45 μ m), is that 11:89 prepares by the mass ratio of paste soldering flux and solder powder, by the time 5 kinds of different solder(ing) pastes.
Above-mentioned 5 kinds of solder(ing) pastes are tested according to following test method respectively:
1) hot slump test
Paste soldering flux is placed 24 hours stable rear allotment solder(ing) pastes after producing.The method of testing specifying with reference to the hot slump of JIS Z 3284 is tested, and is 10-15 minute under the condition of (150 ± 10) DEG C in temperature, chooses 3.0mm X 0.7mm figure wherein for evaluating.If the not bridging of 0.2mm of spacing minimum is outstanding, be labeled as " A "; If 0.2mm bridging and not bridging of 0.3mm is good, is labeled as " B "; If 0.3mm bridging and not bridging of 0.4mm is good, is labeled as " C "; If the 0.4mm bridging that spacing is larger thinks defective, be labeled as " X ";
2) storage viscosity variable quantity test
Paste soldering flux is placed 24 hours stable rear allotment solder(ing) pastes after producing, solder(ing) paste uses the PCU205 of Malcom company model viscosimeter to test (25 DEG C of set temperatures, rotating speed 10RPM, unit is Pa S), when record is tested 10 minutes, viscosity number is as initial viscosity, paste soldering flux is placed after 30 days and configured under solder(ing) paste the same terms again and carry out viscosimetric analysis in the constant temperature oven of 30 DEG C, and this viscosity number is as final viscosity.Final viscosity value is deducted to initial viscosity and obtain viscosity variable quantity.If variable quantity <10 is outstanding, be labeled as " A "; If 10≤variable quantity≤30 are good, be labeled as " B "; If 30≤variable quantity≤50 are qualified, be labeled as " C "; If variable quantity >50 is defective, be labeled as " X ";
3) stir the test of viscosity variable quantity
Paste soldering flux is placed 24 hours stable rear allotment solder(ing) pastes after producing, solder(ing) paste uses the PCU205 of Malcom company model viscosimeter to test (25 DEG C of set temperatures, rotating speed 10RPM), when record is tested 10 minutes, viscosity number is as initial viscosity, viscosimeter rotor continues to stir test 8 hours, records final viscosity value 8 hours time.Final viscosity value is deducted to initial viscosity and obtain viscosity variable quantity.If variable quantity <10 is outstanding, be labeled as " A "; If 10≤variable quantity≤20 are good, be labeled as " B "; If 20≤variable quantity≤30 are qualified, be labeled as " C "; If variable quantity >30 is defective, be labeled as " X ";
4) activator is separated out situation test
The paste soldering flux that takes a morsel is placed on slide, scrapes thinly with scraper, is placed in height and shows dimension Microscopic observation.If there is solid to exist in paste soldering flux, under microscope, can obviously see particle, be labeled as " having "; If it is transparent there is no solid, be labeled as " nothing ".Note: only for analyzing purposes, be not used in the quality of evaluating paste soldering flux.
In detail result of the test is in table 2:
The performance comparison test of the each scaling powder of table 2
| Pilot project | Embodiment 1 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| Hot slump | A | X | X | A | B |
| Storage viscosity variable quantity | A | A | A | X | C |
| Stir viscosity variable quantity | A | A | A | B | C |
| Activator is separated out situation | Have | Have | Have | Nothing | Nothing |
Test result analysis:
A) formula materials of comparative example 1 is identical with embodiment, and different is amine activator, organic acid for activating agent, thixotropic agent add while hot simultaneously and dissolve, and only adopt simple heating process, do not use high-speed shearing emulsion machine structure to activate thixotropic agent.Comparative example 1 sundry item is identical with embodiment, but has shown poor hot slump test, shows that preparation technology's difference has a significant impact result of the test, and the preparation technology of embodiment 1 is obviously better than comparative example 1;
B) formula materials of comparative example 2 is identical with embodiment, and different is that amine activator, organic acid for activating agent are (this are different from embodiment) that simultaneously adds dissolving, uses equally high-speed shearing emulsion machine structure to activate thixotropic agent.Comparative example 2 sundry items are identical with embodiment, but have shown poor hot slump test, show that preparation technology's difference has a significant impact result of the test, and the preparation technology of embodiment 1 is obviously due to comparative example 2;
C) preparation technology of comparative example 3 is identical with embodiment, but the activator that comparative example 3 adopts (helps weldering ability more weak, normal condition has better viscosity stability), solvent is different from embodiment, the salt compounds that amine activator and organic acid for activating agent generate can dissolve, can not separate out, without grinding.Comparative example 3 has shown underproof storage viscosity stability, and this shows to have occurred " rear thickening " phenomenon, and embodiment has avoided this situation;
D) preparation technology of comparative example 4 is that amine activator, organic acid for activating agent, thixotropic agent add while hot simultaneously and dissolve, and only adopts simple heating process, does not use high-speed shearing emulsion machine structure to activate thixotropic agent, fairly simple.The activator, the solvent that add are different from embodiment, have and help weldering ability than faster when heating, and hot slump is had to positive effect, but storage viscosity stability, stir viscosity stability reduced some.Overall performance is more common, and this is the common thinking that current solder(ing) paste is prepared by paste soldering flux, and the indices of embodiment 1 is obviously better than comparative example 4, and this shows that the preparation method of paste soldering flux of the present invention possesses very large advantage.
Although the present invention has been carried out to concrete description about preferred embodiment, these embodiments are only to explain instead of restriction the present invention.Those skilled in the art will appreciate that not departing under the condition of the scope of the present invention of setting forth in claim, can carry out various amendments to above-mentioned embodiment.
Claims (5)
1. a preparation method for paste soldering flux, is characterized in that the raw material of preparing this paste soldering flux comprises: resin, solvent, amine activator, thixotropic agent, organic acid for activating agent and corrosion inhibiter, its preparation method comprises the steps:
A) resin and stirring solvent are heated to after resin dissolves completely and are cooled to 78-82 DEG C, then add amine activator to be stirred to completely to dissolve;
B) add thixotropic agent, with emulsifying device constant temperature emulsion dispersion at 48-52 DEG C, make thixotropic agent form thixotropy gel network structure;
C) add organic acid for activating agent, react with amine activator and generate salt compounds, then add corrosion inhibiter stirring and dissolving salt compounds;
D) low rate mixing is cooled to room temperature and obtains paste soldering flux;
The addition of described resin is the 20-60% of scaling powder gross mass; Described amount of solvent is the 20-50% of scaling powder gross mass; The addition of described thixotropic agent is the 3-8% of scaling powder gross mass; The addition of described amine activator is the 2-5 % of scaling powder gross mass; The addition of corrosion inhibiter is the 0.05-10 % of scaling powder gross mass; Described organic acid for activating agent is selected from the one in malonic acid, succinic acid, adipic acid, pimelic acid, suberic acid, malic acid or maleic acid; Described solvent is the one in ethohexadiol, diethylene glycol monobutyl ether, diethylene glycol monohexyl ether, diethylene glycol list octyl ether, dibutyl ethylene glycol ether, DGDE, propane diols phenylate, dimethylbenzene.
2. the preparation method of paste soldering flux according to claim 1, is characterized in that: described resin is selected from the one in newtrex, Foral, modified rosin or acrylic rosin.
3. the preparation method of paste soldering flux according to claim 1, is characterized in that: described thixotropic agent is modified hydrogenated castor oil.
4. the preparation method of paste soldering flux according to claim 1, is characterized in that: described amine activator is the one in MEA, diethanol amine, triethanolamine, N-methylimidazole, N-ethyl imidazol(e), phenylimidazole, 2-ethyl imidazol(e) or cyclohexylamine preferably.
5. the preparation method of paste soldering flux according to claim 1, is characterized in that: described corrosion inhibiter is selected from the one in 1,2,3-benzotriazole, benzimidazole or TTA.
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| CN102941420A (en) * | 2012-11-15 | 2013-02-27 | 重庆大学 | High-activity environmental-friendly low-sliver Sn-Ag-Cu system lead-free halogen-free tin paste |
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