CN102205472A - Soldering flux and solder composition - Google Patents

Soldering flux and solder composition Download PDF

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Publication number
CN102205472A
CN102205472A CN2011100759140A CN201110075914A CN102205472A CN 102205472 A CN102205472 A CN 102205472A CN 2011100759140 A CN2011100759140 A CN 2011100759140A CN 201110075914 A CN201110075914 A CN 201110075914A CN 102205472 A CN102205472 A CN 102205472A
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composition
scaling powder
scolder
molecular weight
solder
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CN102205472B (en
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中谷隆
吉本哲也
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Arakawa Chemical Industries Ltd
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Arakawa Chemical Industries Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/36Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
    • B23K35/3612Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with organic compounds as principal constituents
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01JMEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28Investigating the spectrum
    • G01J3/42Absorption spectrometry; Double beam spectrometry; Flicker spectrometry; Reflection spectrometry
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/62Detectors specially adapted therefor
    • G01N30/72Mass spectrometers

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Abstract

The invention provides a soldering flux which can provide solder composition, of which soldering performance is excellent, and the residue has excellent color, and which has less residue that is invisible to the naked eye. The soldering flux is characterized by containing rosins (A), of which the maximal absorbance A is less than 0.15 within a scope of 254 nm according to Ultraviolet Spectrophotometry (testing under the conditions that the sample concentration is 1g/dm3, and the optical path is 1cm in length). According to gas chromatography-mass spectrometry analysis, the chromatographic peak area of components having a molecular weight of 320 accounts for 95% of the total chromatographic peak area of the components having a molecular weight of 314-320.

Description

Scolder scaling powder and solder composition
Technical field
The present invention relates to scolder scaling powder and solder composition.
Background technology
Rosin based have the oxide-film of removing the solder powder surface effect (cleaning action), prevent the effect (base resin effect) that solder powder reoxidizes, therefore at scolder with being extensive use of (referring to for example patent documentation 1) in the scaling powder.
Yet rosin based comprises abietane (abietane) the resinoid acid (rosin acid (abietic acid), levopimaric acid, parastrinic acid, neoabietic acid etc.) that has conjugated double bond in the molecule usually.The acid of abietane resinoid is very easy to oxidation, therefore has the such problems of poor heat stability such as producing variable color or degradation.
Therefore, for the purpose of the stabilisation that realizes rosin based etc., proposed to use hydrogenated products (Foral), the disproportionation products (referring to for example patent documentations 2) such as (disproportionated rosins) of rosin.Under the situation of using Foral or disproportionated rosin, can improve variable color or degradation to a certain extent, but require further to improve.In addition, the applicant has proposed to contain the solder soldering fluid (referring to patent documentation 3) of the good hydrogenation newtrex of the colourity of back residue that refluxes, but requires the better solder soldering fluid of scaling powder residue colourity.
Patent documentation 1: the spy opens flat 9-10988 communique
Patent documentation 2: the spy opens the 2002-144077 communique
Patent documentation 3: the spy opens the 2009-285715 communique
Summary of the invention
The purpose of this invention is to provide a kind of scaling powder, described scaling powder can provide that weldability is good, the colourity excellence of scaling powder residue, visually do not have residue, and the solder composition that reduces of scaling powder residue and the solder composition of this class.
The inventor has carried out meticulous research, found that, contains the rosin based of special component by use, can solve above-mentioned problem, thereby finish the present invention.
That is, the present invention relates to the scolder scaling powder, described scaling powder contains rosin based (A), and (condition determination is: sample solution concentration is 1g/dm according to the ultraviolet light absorption photometry 3, optical path length is 1cm), the maximum absorbance A of described rosin based (A) in the above scope of 254nm is below 0.15; According to the gas chromatography-mass spectrometry analysis of the handled thing that methylates, the gas-chromatography peak area that records molecular weight and be 320 composition accounts for more than 95% of gas-chromatography peak area summation that molecular weight is 314~320 composition; The invention still further relates to and contain powder scolder and the solder composition of this scolder with scaling powder.
According to the present invention, can provide that a kind of weldability is good, the colourity excellence of scaling powder residue, visually not have residue, and the scolder scaling powder that reduces of scaling powder residue.In addition, scolder of the present invention can provide excellent heat resistance, the good solder composition of colourity with scaling powder.
The specific embodiment
Scolder of the present invention is characterised in that with scaling powder, and described scaling powder contains rosin based (A) (below, be called composition (A)), and (condition determination is: sample solution concentration is 1g/dm according to the ultraviolet light absorption photometry 3, optical path length is 1cm), the maximum absorbance A of described rosin based (A) in the above scope of 254nm is below 0.15; According to the gas chromatography-mass spectrometry analysis of the handled thing that methylates, the gas-chromatography peak area that records molecular weight and be 320 composition accounts for more than 95% of gas-chromatography peak area summation that molecular weight is 314~320 composition.
According to the ultraviolet light absorption photometry, (A) (condition determination: sample solution concentration is 1g/dm to the maximum absorbance A of composition in the above scope of 254nm 3, optical path length is 1cm) surpass under 0.15 the situation, or according to the gas chromatography-mass spectrometry analysis of the handled thing that methylates, the gas-chromatography peak area that records molecular weight and be 320 composition accounts under the situation of gas-chromatography peak area summation less than 95% that molecular weight is 314~320 composition, contain reactive high conjugated double bond or various impurity in the molecule, therefore, under the situation as solder composition, when welding, the heat-resistant stability variation.In addition, in composition (A), according to the ultraviolet light absorption photometry, the absorbance in the above scope of 254nm mainly relates to the peak of carbon-to-carbon unsaturated bond, and this value means that more greatly intramolecular unsaturated bond is more.In addition, think that this value is just big more if the impurity of coloring is many more.Carbon-to-carbon unsaturated bond reactive high, therefore easily and the various compositions in oxygen or the solder composition react, become painted reason, relevant with the generation of unwanted compound.In addition, the molecular weight of the so-called handled thing that methylates is 320 composition, is equivalent to make the carboxyl of the resin acid composition of composition (A) to be methylated with in the material that forms carboxylate the material that intramolecular carbon-to-carbon unsaturated bond all is hydrogenated.So-called molecular weight is 314 composition, is equivalent to have in molecule the material of 3 carbon-to-carbon unsaturated bonds.Therefore, molecular weight is that the gas-chromatography peak area of 320 composition accounts for more than 95% of gas-chromatography peak area summation that molecular weight is 314~320 composition, is meant that the composition with carbon-to-carbon unsaturated bond contained in this composition (A) is few.
Composition (A) normally with wood rosin, toll oil rosin, gum rosin natural rosin classes such as (gum rosin) and rosin derivatives such as disproportionated rosin, Foral (a) (below, be called composition (a)) hydrogenation, thereby obtain the handled things that methylate such as tetrahydrochysene rosin acid and tetrahydropimaric acid, according to the gas chromatography-mass spectrometry analysis of the handled thing that methylates, the gas-chromatography peak area that records molecular weight and be 320 composition accounts for more than 95% of gas-chromatography peak area summation that molecular weight is 314~320 composition.In addition, by composition (a) is made with extra care, thereby can improve colourity and reduce impurity, be preferred therefore.As process for purification, there is no particular limitation, specifically, can for example enumerate distill, recrystallization, extraction etc.Under the situation of distillation, for example, unpurified composition (a) carries out under the distillation condition of about 200~300 ℃ of temperature, pressure 130~1300Pa left and right sides scope usually.Distillation time can determine according to distillation condition.Under the situation of recrystallization, for example, (a) dissolves in good solvent with unpurified composition, and then distillation removes and desolvates, and obtains dense solution, interpolation poor solvent in this solution and carrying out.As good solvent, can enumerate benzene,toluene,xylene, chloroform, carbon number and be acetate esters such as ketone, ethyl acetate such as 1~3 lower alcohol, acetone etc.As poor solvent, can enumerate n-hexane, normal heptane, cyclohexane, isooctane etc.In addition, above-mentioned refining can also be to make unpurified composition (a) form aqueous alkali with buck, the insoluble unsaponifiable matter matter that produces is taken out with organic solvent extracting, then in and water layer.
The hydrogenation of composition (a) can be undertaken by known method.Specifically, for example in the presence of hydrogenation catalyst, usually about 1~25MPa, under the pressurized with hydrogen of preferred 5~20MPa, with composition (a) heating about 0.5~7 hour, preferred 1~5 hour.As hydrogenation catalyst, can use on carriers such as aluminium oxide, silica, diatomite, carbon, titanium dioxide load that the supported catalyst of metals such as palladium, rhodium, ruthenium, platinum and nickel is arranged; Metal dust such as nickel, platinum; Various known catalyst such as iodide such as iodine, ferric iodide.Wherein, set out preferred palladium, rhodium, ruthenium or platinum class catalyst from the viewpoint of hydrogenation efficiency (hydrogenation ratio is good, and hydrogenation time is short).With respect to the composition (a) of 100 weight portions, the use amount of this catalyst is generally about 0.01~10 weight portion, is preferably 0.01~5 weight portion.In addition, hydrogenation temperature is about 100~300 ℃, is preferably 150~290 ℃.In addition, as required, can also be in solvent carry out hydrogenation under the state of dissolving rosin.There is no particular limitation to the solvent that uses, preferably in reaction inertia, can easily dissolve the solvent of raw material and product.For example, can use cyclohexane, n-hexane, normal heptane, naphthalane, oxolane, two
Figure BSA00000462091100041
1 kind of alkane etc. or will be used in combination more than 2 kinds.Use amount to solvent has no particular limits, and usually, with respect to material resin, is that amount above about 10 weight % is used solvent, the scope of preferred 10~70 weight % with solid constituent.In addition, under the situation of the Foral that hydrogenation under the common hydrogenation conditions obtains, according to the gas chromatography-mass spectrometry analysis of the handled thing that methylates, it is that the percentage of the gas-chromatography peak area summation of 314~320 composition only is increased to about 20% that the gas-chromatography peak area that records molecular weight and be 320 composition accounts for molecular weight.Therefore, in order to obtain composition (A), the hydrogenation of necessary repetition composition (a), increase catalyst use amount, improve harsh hydrogenation conditions and selecting catalyst kinds such as hydrogenation temperature, raising Hydrogen Vapor Pressure, prolongation reaction time.
There is no particular limitation to the softening point (ring and ball method) of the composition (A) that obtains thus, is preferably about more than 60 ℃ usually.The composition that the softening point less than is 60 ℃ (A) because decarbonate etc. increases low molecular composition, is accompanied by the reduction of acid value and active reduce etc.There is no particular limitation to the acid value of composition (A), be preferably about 150mg KOH/g usually more than.The composition (A) of acid value is not enough 150mg KOH/g, because decarbonates etc. increase low molecular composition, active reduce etc. along with the reduction of acid value.Be adjusted into the following water white transparency of 300Hazen (JIS K 0071-1) by the colourity with composition (A), thereby the colourity of scaling powder residue being good, is preferred therefore.In addition, by making composition (A) in the thermogravimetric analysis of 5 ℃/minute of programming rates, weightless 99% o'clock temperature is the rosin derivative below 500 ℃, and the scaling powder residue is less, is preferred therefore.
Herein, described " weightless 99% o'clock temperature " is meant in thermogravimetric analysis, loses 99% o'clock temperature of the preceding weight of heating, that is, only residue heats 1% o'clock temperature of preceding weight.
Use in the scaling powder of the resin-oatmeal core scolder (ヤ ニ goes into り は ん だ) that uses in the scaling powders such as emulsifiable paste scolder that use in the back scaling powder (post flux) that scolder of the present invention can use in the welding of flowing with scaling powder, the reflow soldering, the manual welding etc.
Scolder of the present invention is characterised in that with scaling powder and contains composition (A), in addition, can also contain in addition known scaling powder base resin of composition (A), thixotropic agent (thixotropic agent), activating agent, other additive etc.
As the scaling powder base resin, as long as different with composition (A), just there is no particular limitation, can use known material.Specifically, can enumerate for example synthetic resin such as gum rosin, newtrex, Foral, disproportionated rosin, other various rosin derivatives or mylar, phenoxy resin, terpene resin, polyamide etc.
As solvent, short of special qualification just can be used known material.Specifically, can enumerate alcohols such as ethanol, normal propyl alcohol, isopropyl alcohol, isobutanol; Glycol ethers such as BC, hexyl carbitol; Ester classes such as isopropyl acetate, ethyl propionate, butyl benzoate, diethylene adipate; Hydro carbons such as n-hexane, dodecane, tetradecene etc.
As thixotropic agent, there is no particular limitation, can use known material.Specifically, can use for example rilanit special, beeswax, Brazil wax, stearmide, ethylidene-two-hydroxyl stearmide etc.
As activating agent, there is no particular limitation, can use known material.Specifically, can enumerate for example hydrogen halides hydrochlorate, organic acid or the organic amine etc. of amine.
As additive,, can use known material in the preparation of scaling powder so long as the material that can use usually just has no particular limits.Can contain additives such as antioxidant, mould inhibitor, delustering agent.
Solder composition of the present invention contains solder powder and above-mentioned scolder scaling powder.
There is no particular limitation to the alloy composition of the solder powder that uses among the present invention, can use various known materials.For example, as the alloy composition of solder powder, be the tin-silver alloy, tin-zinc class alloy etc. of present known tin-lead alloy or lead-free solder exploitation; In addition, in above-mentioned solder alloy, can also use the alloy that has added copper, bismuth, indium, antimony etc.There is no particular limitation for the use amount of each composition of emulsifiable paste scolder, and usually, with respect to the solder powder about 80~95 weight portions, the scolder scaling powder is about 5~20 weight portions.
In solder composition of the present invention, except solder powder, scolder with the scaling powder, usually, can also use the known additives such as solvent that in the preparation of solder composition, use.
Embodiment
Below, by embodiment the present invention is carried out more specific description.But the present invention is not subjected to the qualification of these embodiment.In addition, in an embodiment, short of special qualification, " % " and " part " just refers to " weight % ", " weight portion ".
Production Example 1
In 1 liter of flask, add homemade Foral (Wuzhou Richenglin Chemical Co., Ltd., Guangxi's manufacturing) among the 600g, under the decompression of 400Pa, distill, obtain the composition that under 195~250 ℃, distills out.In 1 liter autoclave, composition that adding 200g distills out under 195~250 ℃ and palladium-aluminium oxide, the 200g cyclohexane of 3.0g 5%, to fully replace with hydrogen in the system, making the initial reaction stage Hydrogen Vapor Pressure then is 6MPa, be warming up to 200 ℃, making Hydrogen Vapor Pressure then is 10MPa, when suitably supplementary pressure reduces, reaction is carried out 4 hours.Filtering catalyst, cyclohexane is removed in decompression distillation, obtains rosin based 1.Gas chromatography-mass spectrometry analysis according to the handled thing that methylates, the gas-chromatography peak area that records molecular weight and be 320 composition account for molecular weight be 314~320 composition gas-chromatography peak area summation 100%, colourity is 200H, acid value 174mg KOH/g, 84.5 ℃ of softening points.
Production Example 2
In 1 liter flask, add homemade Foral (Wuzhou Richenglin Chemical Co., Ltd., Guangxi's manufacturing) among the 600g, under the decompression of 400Pa, distill, obtain the composition that under 195~250 ℃, distills out.In 1 liter autoclave, composition that adding 200g distills out under 195~250 ℃ and palladium carbon (moisture content 50%), the 200g cyclohexane of 3.0g 5%, to fully replace with hydrogen in the system, making the initial reaction stage Hydrogen Vapor Pressure then is 6MPa, be warming up to 200 ℃, making Hydrogen Vapor Pressure then is 10MPa, when suitably supplementary pressure reduces, reaction is carried out 4 hours.Filtering catalyst, cyclohexane is removed in decompression distillation, obtains rosin based 2.Gas chromatography-mass spectrometry analysis according to the handled thing that methylates, the gas-chromatography peak area that records molecular weight and be 320 composition account for molecular weight be 314~320 composition gas-chromatography peak area summation 96%, colourity is 200H, acid value 176mgKOH/g, 84.5 ℃ of softening points.
Production Example 3
In 1 liter flask, add homemade disproportionated rosin (Wuzhou Rosin Plant manufacturing) among the 600g, under the decompression of 400Pa, distill, obtain the composition that under 195~250 ℃, distills out.In 1 liter autoclave, the composition that adding 200g distills out under 195~250 ℃, palladium carbon (moisture content 50%) and the 200g cyclohexane of 0.1g 5%, to fully replace with hydrogen in the system, making the initial reaction stage Hydrogen Vapor Pressure then is 6MPa, be warming up to 200 ℃, making Hydrogen Vapor Pressure then is 10MPa, when suitably supplementary pressure reduces, reaction is carried out 4 hours.Filtering catalyst, cyclohexane is removed in decompression distillation, obtains rosin based 3.Gas chromatography-mass spectrometry analysis according to the handled thing that methylates, the gas-chromatography peak area that records molecular weight and be 320 composition account for molecular weight be 314~320 composition gas-chromatography peak area summation 31%, colourity is 90H, acid value 167mg KOH/g, 85.5 ℃ of softening points.
Production Example 4
In 1 liter flask, add homemade Foral (Wuzhou Richenglin Chemical Co., Ltd., Guangxi's manufacturing) among the 600g, under the decompression of 400Pa, distill, the composition that obtains to distill out under 195~250 ℃ is as rosin based 4.Gas chromatography-mass spectrometry analysis according to the handled thing that methylates, the gas-chromatography peak area that records molecular weight and be 320 composition account for molecular weight be 314~320 composition gas-chromatography peak area summation 17%, colourity is 250H, acid value 176mg KOH/g, 79.0 ℃ of softening points.
Production Example 5
In 1 liter flask, add homemade gum rosin among the 600g (waste river, Guangxi chemical industry Co., Ltd makes), under the decompression of 400Pa, distill, obtain the composition that under 195~250 ℃, distills out.Add composition, 400g dimethylbenzene, 20g zinc chloride and 3g sulfuric acid that 450g distills out under 195~250 ℃, under nitrogen atmosphere, reacted 6 hours down at 100 ℃.With 250g 1N hydrochloric acid washing reaction product, in 250g warm water, wash 2 times again.With the washing after xylene solution under the condition of 200 ℃ of solution temperature less thaies, decompression degree 1300Pa, distillation removes removal xylene, under the condition of 200~275 ℃ of solution temperatures, decompression degree 400Pa, about 35g analyte and unreacted reactant are removed in distillation then, obtain newtrex.In 1 liter autoclave, add the palladium carbon (moisture content 50%) of 250g gained newtrex, 250g cyclohexane and 2.5g 5%, behind the oxygen in the system of removing, making Hydrogen Vapor Pressure is 10MPa, when suitably supplementary pressure reduces, reaction is carried out 4 hours.Filtering catalyst, cyclohexane is removed in decompression distillation, obtains rosin based 5.Gas chromatography-mass spectrometry analysis according to the handled thing that methylates, the gas-chromatography peak area that records molecular weight and be 320 composition account for molecular weight be 314~320 composition gas-chromatography peak area summation 53%, colourity is 300H, acid value 147mg KOH/g, 142.0 ℃ of softening points.
(molecular weight of the handled thing of measuring according to gas chromatography-mass spectrometry analysis that methylates be 320 composition content quantitatively)
Undertaken quantitatively by following gas chromatography-mass spectrometry analysis device
In mensuration, dissolving 0.005g sample (rosin based) in the methylating agent on the 0.5g post (the 0.2mol methanol solution of phenyl trimethylammonium hydroxide (PTHA), ジ one エ Le サ イ エ Application ス (strain)), in gas chromatography-mass spectrometry analysis (GC/MS), inject 1 μ l, measure.Determining molecular weight is that the gas-chromatography peak area of 320 composition accounts for the ratio that molecular weight is the gas-chromatography peak area summation of 314~320 composition, is the content of 320 composition as molecular weight with it.
Operative installations
Gas-chromatography: Agilent 6890 (trade name, Agilent Technologies Inc. makes)
Mass spectrometer: Agilent 5973 (trade name, Agilent Technologies Inc. makes)
Post: Advance-DS (trade name, letter and chemical industry (strain) are made)
(colourity)
According to JIS K 0071-1, measure with Hazen unit (H).For the rosin based of comparative example 4~6, measure Gardner (Gardner) colourity according to JIS 0071-2.
(acid value)
According to JIS K0070, measure by neutralization titration.
(softening point)
According to JIS K 5902, measure by ring and ball method.
(absorbance)
With the accurate weighing 25.0mg of 25ml measuring bottle sample (rosin based), after the cyclohexane dissolving, be settled to the weighing line of 25ml.By UV spectrophotometer ((strain) Hitachi makes, HITACHI u-3210 spectrophotometer), use the quartz cell of optical path length as 1cm, measure absorbance.Read out in the maximum absorbance of the above scope of 254nm.The result is shown in the table 1.
(mensuration of weightless 99% o'clock temperature in the calorimetric analysis)
Use sample (rosin based), under nitrogen atmosphere,, measure weightless temperature at 99% o'clock with 5 ℃/minute programming rate by differential thermal/thermogravimetric analyzer (セ イ コ イ Application ス Star Le (strain) is made, trade name " TG/DTA220 ").And then according to the state of residue after the following standard evaluation thermogravimetric analysis.The result is shown in the table 1.
1: Visual Confirmation does not have residue fully
2: confirming has residue slightly, but outward appearance is good
3: the residue of black or brown is arranged, appearance poor
Embodiment 1~2, comparative example 1~6
Use rosin based 1~8,, carry out the heat endurance of rosin based, the emulsifiable paste scolder is estimated (outward appearance and residue slip) and weldability with the scaling powder residue of scaling powder and back scaling powder evaluation by following method.
The result is shown in the table 1.
(adding heat endurance)
In the test tube of internal diameter 1.5cm, height 15cm, add 10g sample (rosin based), under air atmosphere, in 120 ℃ circulated air drying machine, leave standstill, observe colourity (Gardner's colourity is measured according to JIS0071-2) over time.In addition, the evaluation that adds heat endurance of this rosin based can be as inferring the scolder that contains rosin based scaling powder and the stable on heating index of back scaling powder.Think the heating back good rosin based of colourity have scolder with scaling powder etc. essential add heat endurance.
(preparation of scaling powder of emulsifiable paste scolder)
After 50 parts of samples (rosin based), 45 parts of diethylene glycol monohexyl ethers, 5 parts of ethylidene-two-12-hydroxyl stearmide heating for dissolving, cooling, preparation solder flux composition.
(preparation of emulsifiable paste scolder)
With 90 parts of solder powders (the Sn-Ag-Cu alloy with 5~20 μ m average grain diameters, 96.5 weight %/3 weight %/0.5 weight %) and 10 parts of scaling powder stirrings of preparation according to the method described above, preparation emulsifiable paste scolder.
(weldability of emulsifiable paste scolder)
For the emulsifiable paste scolder of preparation, according to " JIS Z3284 annex 10 " ぬ れ renders a service お I び デ イ ウ エ Star テ イ Application グ Try test (the wetting effectiveness and the test of drying) ", evaluation weldability (wellability) are well (zero: wide in range degree divide into 1 or 2).
(the scaling powder residue of emulsifiable paste scolder is estimated)
1. residue slip
On copper base, serigraphy emulsifiable paste scolder, the gained printed base plate welded by the nitrogen reflux stove (preheat condition: 180 ℃ of heating 100 seconds down, main heating condition: heated about 10 seconds down) at 240 ℃, measure residue (scaling powder residue) weight on the welding front-back baseboard, by following formula, calculate the slip of scaling powder residue.
Residue slip (%)=[(the scaling powder level of residue that scaling powder solid constituent amount in the emulsifiable paste scolder of printing-on copper base is residual)/(scaling powder solid constituent amount in the emulsifiable paste scolder of printing)] * 100
Solid constituent amount: the solvent in the emulsifiable paste scolder (diethylene glycol monohexyl ether) scaling powder composition in addition
2. outward appearance
In addition, observe the welding position by microscope VW-6000 ((strain) キ one エ Application ス makes: 30 times), according to the colourity of the visual judgement scaling powder of following standard residue.
1: visual do not have a scaling powder residue
2: the certain scaling powder residue of visual existence
3: a large amount of scaling powder residues of visual existence
(preparation of back scaling powder)
After 25 parts of samples (rosin based), 75 parts of isopropyl alcohol heating for dissolving, cooling, thereby preparation back scaling powder.
(back scaling powder residue is estimated)
1. residue slip
Thickness at 18mm * 60mm is on the glass plate of 1mm, and scaling powder behind the dropping 0.1g left standstill on 270 ℃ hot plate 10 seconds, measured the weight of heating front and back, calculated the residue slip of back scaling powder by following formula.
Residue slip (%)=[(the back scaling powder level of residue that solid constituent total amount in the back scaling powder-on glass plate is residual)/(the solid constituent total amount in the back scaling powder)] * 100
Solid constituent amount: solvent (isopropyl alcohol) the scaling powder composition in addition in the scaling powder of back
2. outward appearance
In addition, the visualization outward appearance is estimated according to following standard.
1: visual not back scaling powder residue
2: the certain back of visual existence scaling powder residue
3: a large amount of back of visual existence scaling powder residue
(weldability of back scaling powder)
According to " JIS Z3197 は ん だ Wide Ga り method (scolder diffusion method) ", estimate weldability (wellability), calculate diffusivity.
Figure BSA00000462091100111

Claims (5)

1. scolder scaling powder, it is characterized in that described scaling powder contains rosin based (A), according to the ultraviolet light absorption photometry, the maximum absorbance A of described rosin based (A) in the above scope of 254nm is below 0.15, and the condition determination of described ultraviolet light absorption photometry is that sample solution concentration is 1g/dm 3, optical path length is 1cm; According to the gas chromatography-mass spectrometry analysis of the handled thing that methylates, the gas-chromatography peak area that records molecular weight and be 320 composition accounts for more than 95% of gas-chromatography peak area summation that molecular weight is 314~320 composition.
2. scolder scaling powder as claimed in claim 1 is characterized in that, the colourity of described rosin based (A) is below the 300Hazen.
3. scolder scaling powder as claimed in claim 1 or 2 is characterized in that, described rosin based (A) is that weightless 99% o'clock temperature is the rosin derivative below 500 ℃ in programming rate is 5 ℃/minute thermogravimetric analysis.
4. solder composition, described composition contains solder powder and each described scolder scaling powder of claim 1~3.
5. solder composition as claimed in claim 4, wherein, described solder powder is the lead-free solder powder.
CN201110075914.0A 2010-03-30 2011-03-24 Soldering flux and solder composition Active CN102205472B (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2010077618 2010-03-30
JP2010-077618 2010-03-30

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CN102205472A true CN102205472A (en) 2011-10-05
CN102205472B CN102205472B (en) 2014-10-15

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