CN102350599B - Halogen-free high-impedance water-based washing-free scaling powder as well as preparation method and application thereof - Google Patents
Halogen-free high-impedance water-based washing-free scaling powder as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a halogen-free high-impedance water-based washing-free scaling powder as well as a preparation method and application thereof. The scaling powder disclosed by the invention comprises the following components in percentage by weight: 1.50-6.00% of activating agent, 0.10-0.45% of nonionic surfactant, 0.05-2.00% of film forming agent, 0.15-0.40% of corrosion inhibitor, 4.00-25.00% of cosolvent and the balance of deionized water. The scaling powder disclosed by the invention does not contain halogen and uses the deionized water as the main component of a scaling powder solvent, thus the scaling powder is safe and environment-friendly. In the invention, the coordination mode and dosage of each component of the scaling powder are accurately computed; the scaling powder has the advantages of good stability and excellent soldering performance; and the obtained soldered dots are full, thereby effectively reducing the occurrence of defects such as continuous soldering or missing soldering and the like. The composition materials of the scaling powder disclosed by the invention can be periodically volatilized in the soldering process; the residuals after the soldering are less; the electric insulating property is excellent; the surface insulating resistance after the soldering is larger than 1.0*108; and the washing is not needed.
Description
Technical field
The present invention relates to a kind of scaling powder for electronic packaging, assembling and soldering, refer to especially to be applied to the halogen-free free high-impedance water-based washing-free scaling in the lead-free solder wave-soldering technique.
Technical background
Halogen is the general name of periodic table of elements VIIA family element, comprises fluorine (F), chlorine (Cl), bromine (Br), iodine (I), five kinds of elements of astatine (At).The efficient fire retardant of organohalogen compounds Chang Zuowei is applied in the macromolecular material assemblies such as cable, printed circuit board.Part flux activity composition also contains halogen, halogen have an oxide layer that helps remove fast bond pad surface, accelerate solder speed, improve the porefilling capability of scolder.But halogen all has adverse effect to reliability and the ecological environment of electronic product, and for example: the ionic state halogen that postwelding remains in the PCB surface can form conducting medium under hot and humid environment, so that the printing board surface insulaion resistance reduces, the electric leakage possibility increases; Covalency attitude halogen is stable under normal temperature environment, but is heated or can produces Halogen gas when burning, and such as HCl, HBr etc., Halogen gas enters the acidity that atmosphere will increase precipitation, corrosion building and harm humans health.IEC " IEC 61249-2-21 " is made regulation for the Halogen circuit board: single homogeneous materials contains total chlorine (Cl)＜900ppm, total bromine (Br)＜900ppm, total chlorine (Cl)+total bromine (Br)＜1500ppm; International electronics industry connects the standard J-STD-004B of association (IPC) regulation: quantitative measurment scaling powder fluorine-containing (F), chlorine (Cl), bromine (Br), iodine (I), total halogen is considered as halogen-free scaling powder less than the scaling powder of 500ppm.Along with the environmental requirement of increasing electronics manufacturing enterprise choice for use halogen-free scaling powder with the reply increasingly stringent, so the halogen-free type scaling powder is the inexorable trend of scaling powder development.
The solvent of scaling powder is used for other material auxiliary agent of dissolving as carrier, and each composition is uniformly dispersed, and is easy to apply, and solvent commonly used is the Organic Alcohols such as methyl alcohol, ethanol and isopropyl alcohol.Strong and the viscosity Xiao Yi of the solvability of low-boiling point alcohol applies, but the volatilization of being heated is fast, and activating agent easily causes active deficiency because losing too early the ionization environment at warm-up phase; High-boiling point alcohol viscosity is large, and good heat conduction effect can prevent effectively that the pad of removing oxide-film from reoxidizing, but postwelding is easily residual, affects the aesthetics of printed board.Lower boiling alcohol, ether, ester, hydrocarbon mostly are VOC (Volatile Organic Compound, VOC).VOC can vapor away at warm-up phase as the scaling powder solvent, causes the waste of industrial chemicals; A large amount of VOC materials spill into and easily cause photochemical fog in the atmosphere, and pollutant atmosphere jeopardizes human health; When human body sucks finite concentration VOC, headache, limbs fatigue can be felt, the symptoms such as failure of memory, stupor, serious harm human health can be caused when serious; And VOC mostly is combustible material, and flash-point is low, has serious disaster hidden-trouble in scaling powder production and use procedure.The primary solvent of water-based scaling powder is deionized water, and product cost is low, uses safety, and is little to the harm of human health and ecological environment, is the development trend of scaling powder environmental protection.
The boiling point of water and specific heat will be higher than traditional alcohols solvent, when using, water-based scaling powder needs suitably to improve preheat temperature or prolong preheating time, guarantee at warm-up phase deionized water to be evaporated fully the problem such as solder system was quick-fried when moisture entrapment easily caused wave soldering.The active material of water-based scaling powder mainly is organic acid, and activating agent is condensed into acidic liquid with solvent evaporates at the equipment top in warm, causes equipment accelerated corrosion.So, use the Wave soldering apparatus of water-based scaling powder suitably to reequip: to increase preheating zone length, accelerate ventilation speed, at the top, preheating zone the vapor collection device is set as far as possible.
Relevant lead-free solder has some relevant reports with water-based scaling powder.The patent of invention of publication number CN1836825 provides a kind of water-soluble soldering flux dedicated for lead-free solder, be comprised of following weight percentage material: boric acid and organic acid for activating agent 5.0%-10.0%, non-ionic surface active agent and cationic surfactant 0.1%-1.0%, cosolvent 8.0%-20.0%, film forming agent 0.1%-1.0%, corrosion inhibiter 0.1%-0.5%, all the other are deionized water.This scaling powder has reduced the consumption of VOC in the scaling powder, does not contain rosin, and halogen-free, solder joint is even, helps weldering functional.But the acidity of boric acid a little less than, for the use amount that keeps flux activity boric acid is larger, can't in welding process, vapor away fully, the residue that postwelding forms has stronger corrosivity, needs in time to clean.Postwelding clean to need is equipped with special-purpose cleaning equipment, also will face processing and the emission problem of waste water, has prolonged production technology, has increased the production cost, so non-ly exempt to clean the class water-soluble flux exist larger difficulty aspect practical application.Publication number is that the patent name of CN1843684 is non-volatility organic matter halogen-free low-solid-contained water-base washing-free scaling, be comprised of following weight percentage material: organic acid organic amine activating agent 1.8%-4.0%, film forming agent 0.5%-1.0%, wetting agent 0.03%-0.20%, corrosion inhibiter 0.04%-0.10%, all the other are deionized water.This scaling powder does not contain volatile organic matter fully, safety and environmental protection, but film forming agent polyethylene glycol oxide, polyacrylamide, D-sorbite and the PVP selected are hydroaropic substance, the film forming agent that postwelding remains in the PCB surface forms one deck hydrophilic film, the easy moisture absorption, cause postwelding PCB surface insulation resistance to reduce, the risk of printed board electric leakage increases.
The development trend of electronic product high-performance, lightening and miniaturization is so that the integrated level of electronic devices and components improves constantly, and packaging density significantly promotes, and package dimension constantly dwindles, and the component's feet spacing is more and more less.In the pin thin space situation, displacement occurs in the ion residues thing on PCB surface in electric field environment, easily cause short circuit between component's feet, causes components and parts to lose efficacy.The existence of residue or residual ion is the maximum hidden danger of product usage reliability, and especially in hot and humid situation (such as rainy season in south China area time, environment temperature is high and air humidity is large), the reliability of electronic product faces huge test.The use of no-clean scaling powder will primarily guarantee the postwelding reliability of electronic product, and this solder flux postwelding of will seeking help should have higher surface insulation resistance, and the residual particularly ion residues of postwelding should be controlled at a rational level.
Summary of the invention
The object of the invention is to solve water-based scaling powder surface insulation resistance technological deficiency on the low side, and a kind of halogen-free free high-impedance water-based washing-free scaling that is applicable to lead-free solder wave-soldering technique and preparation method thereof is provided.The present invention complies with the development trend of liquid soldering flux environmental protection, with the main component of deionized water as the scaling powder solvent, and safety and environmental protection, the film forming matter in the while choose reasonable scaling powder, Effective Raise postwelding surface insulation resistance.
The halogen-free free high-impedance water-based washing-free scaling of the present invention, its percetage by weight consists of:
Preparation method: under the normal temperature deionized water is added in the clean reactor with agitating device, adding cosolvent begins to stir, add again activating agent and non-ionic surface active agent, stirred 15-20 minute, then adding film forming agent stirred 15-20 minute, add again corrosion inhibiter, continue to be stirred to and stop after solid material dissolves fully stirring, leave standstill rear filtration and be product.
Described activating agent is comprised of organic acid and organic amine, and part by weight is 5: 1-25: 1.Organic acid is aliphatic acid, aromatic acid, amino acid, be selected from acrylic acid, succinic acid, glutaric acid, adipic acid, maleic acid, isoamyl acetic acid, tartaric acid, citric acid, malic acid, benzoic acid, phthalic acid, diethyl alkyd, glutamic acid, optional wherein one or more combinations; Organic amine is selected from diethanol amine, triethanolamine, triisopropanolamine, optional wherein one or more combinations.The soldering process temperature of the activation temperature of selected activating agent and lead-free solder is complementary, most activating agents gasifiable vaporing away of in welding process, being heated, the activity of different activities agent and activation temperature mutual difference, reasonably select the activating agent combination can increase the activation temperature scope of activating agent, make scaling powder can keep enough activity in the different soldering stages, help weldering function admirable and the postwelding residue is few.Neutralization reaction can occur during the composite use of organic acid and organic amine, but the neutralized reaction product that reaction generates is unsettled, can again be decomposed into organic acid and organic amine under heating status, remaining acid and amine neutralize again after the welding, can effectively reduce the corrosivity of residue.
Described nonionic surface active agent is selected from OPEO TX-10, APES OP-10, AEO AEO, polyoxyethylene sorbitan monooleate Tween-60, optional wherein one or more combinations.The surface tension of water is unfavorable for that as solvent scaling powder is wetting in the coating of PCB surface and through hole inside with deionized water apparently higher than alcohols solvents commonly used such as ethanol, isopropyl alcohols, needs to add efficient surfactant to reduce the surface tension of water in scaling powder.Nonionic surface active agent does not ionize in water, is not subjected to the impact of solution ionization environment, and stability is high, can significantly reduce the surface tension of water-based scaling powder, promotes the wetting of lead-free solder.Than other type, the postwelding of nonionic surface active agent is residual not to be ionized, less on the impact of PCB electrical insulation capability.
Described film forming agent is the hydrophobicity ester, the isoamyl valerate of selecting oneself, diethyl malonate, dimethyl succinate, diethyl succinate, butene dioic acid dibenzyl ester, diethylene adipate, octyl benzoate, optional wherein one or more combinations.Film forming agent can form fine and close organic film in brazing process, secluding air prevents the oxidation of molten solder and pad metal.The part film forming agent can vapor away in welding process, and the film forming agent that remains on a small quantity the PCB surface can form the hydrophobicity organic film, has moistureproof and anticorrosive effect, is of value to the electrical insulation properties that improves PCB.
Described corrosion inhibiter is BTA.BTA can be adsorbed on the hydrophobic membrane that the pad metal surface forms rapidly one deck densification, and the protection pad metal is avoided the corrosion of atmosphere and hazardous medium, and the corrosion inhibiter of reasonable concentration can be realized the timely repairing to damaged diaphragm.
Described cosolvent is comprised of co-solvent and ethers scaling powder.Co-solvent is selected from methyl alcohol, ethanol, isopropyl alcohol, ethylene glycol, propane diols, diethylene glycol (DEG), polyethylene glycol PEG200-400, optional wherein one or more combinations.The ethers cosolvent is selected from ethylene glycol phenyl ether, diethylene glycol ether, diethylene glycol butyl ether, tri ethylene glycol ethyl ether, triethylene glycol butyl ether, TRIGLYME, dipropylene glycol methyl ether, tripropylene glycol methyl ether, glycerine isoamyl ether, tetraethyleneglycol dimethyl ether, optional wherein one or more combinations.Co-solvent is used for activating agent and the film forming matter that dissolving is insoluble in water; The ethers cosolvent boiling point of selecting is higher, and a small amount of use can improve the wetability of scaling powder, helps to promote the ability of the filling vias of lead-free solder.
The application process of the halogen-free free high-impedance water-based washing-free scaling of the present invention: can adopt the methods such as spraying, foaming, dipping evenly to be coated to scaling powder on the pcb board, pcb board is carried out preheating, preheat temperature is 95 ℃-120 ℃ (the plate top is measured), deionized water in the scaling powder is evaporated fully, connect through single ripple or double wave solder for wave crest welding slot welding again, solder temperature is decided on the lead-free solder kind, be generally 255 ℃-270 ℃, 4 °-6 ° at crest welder guide rail inclination angle, conveyer chain transfer rate 1.0-1.5m/min.
The halogen-free free high-impedance water-based washing-free scaling of the present invention is for the wave-soldering technological design of lead-free solder, realization is to the matched well of the interval technological temperature of difference, help the weldering function admirable, be applicable to the lead-free solders such as Sn-0.7Cu, Sn-0.3Ag-0.7Cu, Sn-0.5Ag-0.7Cu, Sn-3.0Ag-0.5Cu.The present invention has significantly reduced the consumption of VOC with the primary solvent composition of deionized water as scaling powder, uses safety, and is nonflammable.Adopt the built reactive agent of organic acid and organic amine, select simultaneously alcohols and the combined cosolvent of higher boiling ethers, the collocation of choose reasonable component can guarantee to have enough activity at wave-soldering different phase scaling powder, and performance seldom produces the postwelding residue when well helping the weldering performance.This scaling powder is selected the Halogen activating agent, does not use the fluorine carbon surfactant, and scaling powder does not contain halogen fully.The hydrophobic film-forming material postwelding of selecting residual few, residue forms fine and close hydrophobic film layer at circuit board surface, and effectively the moisture of secluding air makes circuit board have the electrical insulation properties of excellence.
The present invention is compared with the prior art and has the following advantages: the scaling powder not containing halide, do not use ionic halide and covalent type halide, and Composition Design and selection are reasonable, meet the Halogen-free requirement of each standards and norms; Adopt organic acid and the agent of organic amine built reactive and arrange in pairs or groups alcohols and the combined cosolvent of higher boiling ethers, all have enough activity at wave-soldering different phase scaling powder; Replace water-soluble resin with the hydrophobic film-forming material, postwelding forms fine and close hydrophobic film layer at circuit board surface, can wrap up the survival ion of circuit board surface, makes PCB still have higher insulaion resistance under hot and humid condition.The combination of each component of scaling powder and weight are through accurate calculating, the scaling powder good stability, can promote lead-free solder the wetting of bond pad surface and sprawling, solder joint is full, effectively reduce the generation that solder joint connects tin or empty weldering, composition material can vapor away in welding process in segmentation, and postwelding is residual few, electrical insulation capability is good, need not to clean.
The halogen-free free high-impedance water-based washing-free scaling of the present invention connects association criterion J-STD-004A according to international electronics industry and detects, and indices all reaches the requirement of L0 level.Can satisfy the solder requirement of printed circuit board in the durable consumption electronic products such as computer, television set fully.
The specific embodiment
Below in conjunction with embodiment enforcement of the present invention is described further, but enforcement of the present invention and protection domain are not limited to this.Following examples constituent content all is weight percentage.
Embodiment 1:
Preparation method: under the normal temperature deionized water is added in the clean reactor with agitating device, cosolvent begins to stir after adding, add activating agent and non-ionic surface active agent, stirred 20 minutes, then adding film forming agent stirred 20 minutes, add again other raw material, continue to be stirred to and stop after solid material dissolves fully stirring, leave standstill rear filtration and be product.
The using method of the halogen-free free high-impedance water-based washing-free scaling of the present invention: can adopt the methods such as spraying, foaming, dipping evenly to be coated to scaling powder on the pcb board, pcb board is carried out preheating, preheat temperature is 95 ℃-120 ℃ (the plate top is measured), deionized water in the scaling powder is evaporated fully, connect through single ripple or double wave solder for wave crest welding slot welding, solder temperature is decided on the lead-free solder kind again, is generally 255 ℃-270 ℃, 4 °-6 ° at guide rail inclination angle, transfer rate 1.0-1.5m/min.
Embodiment 2:
Preparation and application is identical with embodiment 1.
Embodiment 3:
Preparation and application is identical with embodiment 1.
Embodiment 4:
Preparation and application is identical with embodiment 1.
The halogen-free free high-impedance water-based washing-free scaling that above embodiment makes, according to the standard SJ/T11273-2002 of China Ministry of Industry and Information " exempting to clean liquid scaling powder " rate of spread, content of halogen, corrosivity and four the key technical indexes of postwelding surface insulation resistance of scaling powder are detected, all technical is as shown in table 1 below.
The table 1 scaling powder rate of spread, content of halogen, corrosivity and postwelding surface insulation resistance measurement result
By as seen from Table 1, scaling powder of the present invention is not halogen-containing, is the environment-friendly type scaling powder, meets the Halogen-free requirement of each standards and norms; The surface insulation resistance of PCB was all greater than 1.0 * 10 after welding was finished
8, reaching the surface insulation resistance requirement of alcohol radical no-clean scaling powder, the electric reliability of postwelding PCB is high; The scaling powder rate of spread is greater than 74% simultaneously, and the bronze mirror corrosion test is all qualified, can satisfy the unleaded Wave crest Welding technique of general electronic products.
The present invention adopts organic acid and the agent of organic amine built reactive and arrange in pairs or groups alcohols and the combined cosolvent of higher boiling ethers, all has enough activity at wave-soldering different phase scaling powder; Replace water-soluble resin with the hydrophobic film-forming material, postwelding forms fine and close hydrophobic film layer at circuit board surface, can wrap up the survival ion of circuit board surface, makes PCB still have higher insulaion resistance under hot and humid condition.The combination of each component of scaling powder and weight are through accurate calculating, the scaling powder good stability, can promote lead-free solder the wetting of bond pad surface and sprawling, solder joint is full, effectively reduce the generation that solder joint connects tin or empty weldering, composition material can vapor away in welding process in segmentation, and postwelding is residual few, electrical insulation capability is good, need not to clean.
The halogen-free free high-impedance water-based washing-free scaling of the present invention connects association criterion J-STD-004A according to international electronics industry and detects, and indices all reaches the requirement of L0 level.Can satisfy the solder requirement of printed circuit board in the durable consumption electronic products such as computer, television set fully.
Claims (1)
1. method for preparing halogen-free free high-impedance water-based washing-free scaling, it is characterized in that: under the normal temperature be that 84.05% deionized water joins in the clean reactor with agitating device with percentage by weight, add cosolvent ethanol 5.00%, propane diols 1.50%, PEG400:0.7%, behind dipropylene glycol methyl ether 2.50% and the tripropylene glycol butyl ether 1.00%, start and stir, add activating agent tartaric acid 0.80%, succinic acid 1.80%, glutaric acid 0.60%, diethyl alkyd 0.40%, triisopropanolamine 0.20% and non-ionic surfactant OP-10: 0.20%, stir after 15-20 minute, add film forming agent dimethyl succinate 1.00%, stir after 15-20 minute, add again corrosion inhibiter BTA 0.25%, be stirred to and stop after solid material dissolves fully stirring, leave standstill rear filtration and be product.
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| CN100496867C (en) * | 2007-05-11 | 2009-06-10 | 北京工业大学 | Cleaning-free soldering flux without halogen and rosin for solder without lead |
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