CN104384755A - Low-residue high-storage-stability lead-free tin paste and preparation method thereof - Google Patents

Low-residue high-storage-stability lead-free tin paste and preparation method thereof Download PDF

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Publication number
CN104384755A
CN104384755A CN201410562566.3A CN201410562566A CN104384755A CN 104384755 A CN104384755 A CN 104384755A CN 201410562566 A CN201410562566 A CN 201410562566A CN 104384755 A CN104384755 A CN 104384755A
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soldering tin
low
storage stability
high storage
powder
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CN201410562566.3A
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CN104384755B (en
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赵麦群
韩帅
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Xian University of Technology
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Xian University of Technology
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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
    • B23K35/24Selection of soldering or welding materials proper
    • B23K35/26Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
    • B23K35/262Sn as the principal constituent
    • 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
    • B23K35/362Selection of compositions of fluxes
    • 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
    • B23K35/40Making wire or rods for soldering or welding

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Electric Connection Of Electric Components To Printed Circuits (AREA)

Abstract

The invention relates to low-residue high-storage-stability lead-free tin paste, which comprises the following ingredients in percentage by mass: 10 percent to 15 percent of soldering flux and 85 percent to 90 percent of soldering tin powder, wherein the soldering flux comprises the following ingredients in percentage by mass: 20 to 30 percent of film forming agents, 15 percent to 20 percent of active agents, 3 percent to 6 percent of thixotropic agents, 3 percent to 6 percent of thickening agents and the balance solvents. The invention also disclose a preparation method of the low-residue high-storage-stability lead-free tin paste, and the preparation method comprises the following steps that the solvents and the thickening agents are added into a reaction kettle and are stirred at 75 DEG C into a transparent state; the temperature is lowered to 65 DEG C, the film forming agents and the active agents are added and are stirred to the transparent state; the temperature is lowered to 55 DEG C, the thixotropic agents are added and are stirred to the transparent state; the temperature is lowered to 30 DEG C, the soldering tin powder is added and is fast stirred, the stirring is carried out for 15 minutes after the cooling, and the low-residue high-storage-stability lead-free tin paste is obtained. The low-residue high-storage-stability lead-free tin paste has the advantages that the residue is little after reflow soldering, in addition, the residue is in a transparent crystal shape, the residue is not corrosive, and the cleaning after welding can be omitted.

Description

A kind of low-residual high storage stability lead-free tin cream and preparation method thereof
Technical field
The invention belongs to electronic circuit surface mounting technology field, be specifically related to a kind of low-residual high storage stability leadless soldering tin paste, the invention still further relates to the preparation method of this leadless soldering tin paste.
Background technology
The microminiaturization of electronic product makes surface mounting technology occupy leading position in the assembling of electronic devices and components.In surface mounting technology, solder(ing) paste directly affects the quality of welding as its critical material.The solder(ing) paste product of high-quality should have good processing performance, welding performance, less postwelding remain, high storage stability etc.
Solder(ing) paste by scaling powder and soldering tin powder according to a certain percentage Homogeneous phase mixing form.Traditional solder(ing) paste scaling powder contains rosin and the derivative thereof of 40% ~ 70%, and rosin can give out the smog that some contain resin acid particulate and other pernicious gas composition after temperature is higher than 200 DEG C, can cause allergic, stimulate eyes and the upper respiratory tract, cause the symptoms such as occupational asthma, serious harm health, and cause environmental pollution.And, solid nonvolatile matter components a large amount of in rosin will be attached on solder joint and periphery as postwelding residue, these postwelding residues not only affect solder joint outward appearance, also cause, because of the circuit board corrosion problem of the postwelding residue moisture absorption, causing circuit board operational failure.Therefore, must clean postwelding residue.Cleaning agent used is at present mainly to fluoridize and chlorinated solvent, and its use can cause the consumption of Ozone in Atmosphere, so the use of these cleaning agents is prohibited gradually.But just current research, does not also find the suitable alternative of rosin.Therefore, the low rosin low-residual No clean solder(ing) paste reducing rosin consumption will become an important directions of solder(ing) paste development.
First scaling powder will possess certain activity, to remove the oxide-film on soldering tin powder in welding process, electric circuit metal surface.In scaling powder, rosin and activating agent provide active as active material, and activity is higher, more easily welds.But high activity exacerbates the corrosion to material, wherein scaling powder is to the corrosion of soldering tin powder, the viscosity of solder(ing) paste storage process can be caused to increase, active reduction, solder ball defect etc., has a strong impact on storage and the use of solder(ing) paste.Therefore, reduce the activity of activating agent under room temperature or storage temperature in scaling powder, improve solder(ing) paste product storage stability significant.
Summary of the invention
The object of this invention is to provide a kind of low-residual high storage stability leadless soldering tin paste, not only residue is few for this paste reflows postwelding, and transparent crystal shaped of residue, residue non-corrosiveness, can remove postwelding cleaning from.
Another object of the present invention is to provide a kind of preparation method of low-residual high storage stability leadless soldering tin paste.
The technical solution adopted in the present invention is, a kind of low-residual high storage stability leadless soldering tin paste, composed of the following components according to mass percent: scaling powder 10% ~ 15%, soldering tin powder 85% ~ 90%, above constituent mass percent value and be 100%; Wherein said scaling powder is composed of the following components according to mass percent: film forming agent 20% ~ 30%, activating agent 15% ~ 20%, and thixotropic agent is 3% ~ 6%, tackifier 3% ~ 6%, and surplus is solvent, and above constituent mass percentage sum is 100%.
Feature of the present invention is also,
Film forming agent is one or both the mixture in water-white rosin, newtrex.
Activating agent is a kind of or several arbitrarily mixture of glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, decanedioic acid.
Thixotropic agent is rilanit special, stearmide one wherein.
Tackifier are pentalyn.
Solvent is ethyl acetoacetate.
Soldering tin powder is 3 #sn0.3Ag0.7Cu alloy powder.
Another technical scheme of the present invention is, a kind of preparation method of low-residual high storage stability leadless soldering tin paste, implements according to the following steps:
Step 1, takes scaling powder 10% ~ 15% by mass percentage respectively, soldering tin powder 85% ~ 90%, above constituent mass percent value and be 100%; Wherein said scaling powder is composed of the following components according to mass percent: film forming agent 20% ~ 30%, activating agent 15% ~ 20%, and thixotropic agent is 3% ~ 6%, tackifier 3% ~ 6%, and surplus is solvent, and above constituent mass percentage sum is 100%;
Step 2, adds solvent in reactor, adds tackifier simultaneously, is heated to 75 DEG C, and it is transparent and homogeneous shape that constant temperature is stirred to solution;
Step 3, solution step 2 obtained is reduced to 65 DEG C, adds film forming agent and activating agent, and being stirred to solution is transparent and homogeneous shape;
Step 4, solution step 3 obtained is reduced to 55 DEG C, adds thixotropic agent, and being stirred to solution is transparent and homogeneous shape;
Step 5, flux solvent step 4 obtained is reduced to 30 DEG C, adds soldering tin powder, and continues to stir rapidly, after being cooled to room temperature, continuing to stir 15min, namely obtains low-residual high storage stability leadless soldering tin paste.
Feature of the present invention is also,
Film forming agent is one or both the mixture in water-white rosin, newtrex; Activating agent is a kind of or several arbitrarily mixture of glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, decanedioic acid; Thixotropic agent is rilanit special, stearmide one wherein; Tackifier are pentalyn; Solvent is ethyl acetoacetate; Soldering tin powder is 3 #sn0.3Ag0.7Cu alloy powder.
The invention has the beneficial effects as follows,
1. low-residual high storage stability leadless soldering tin paste of the present invention, adds the consumption of activating agent to make up the problem that rosin amount reduces the flux activity deficiency brought, and does not affect the film forming of rosin.In addition, due to the appropriate selection of solvent composition, activating agent can evenly be separated out at normal temperatures, not only reduce scaling powder activity at normal temperatures, the scaling powder viscosity that the minimizing that compensate for again rosin brings reduces problem, and selected activating agent can volatilize completely at postwelding, and this just makes the present invention on the basis ensureing solder(ing) paste processing performance, welding performance, effectively reduce postwelding to remain, improve storage stability.
2. the preparation method of low-residual high storage stability leadless soldering tin paste of the present invention, ensureing, under the prerequisite that each component can fully be dissolved, to reduce preparation temperature as far as possible, avoids the component physical property change caused because temperature is too high.In addition, when the unique distinction of this solder(ing) paste preparation method is 30 DEG C, carry out mixing of scaling powder and solder powder, avoid the problem that the solder(ing) paste uniformity that causes due to activating agent precipitation is at normal temperatures low.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in detail.
A kind of low-residual high storage stability of the present invention leadless soldering tin paste, composed of the following components according to mass percent: scaling powder 10% ~ 15%, soldering tin powder 85% ~ 90%, above constituent mass percent value and be 100%; Wherein said scaling powder is composed of the following components according to mass percent: film forming agent 20% ~ 30%, activating agent 15% ~ 20%, and thixotropic agent is 3% ~ 6%, tackifier 3% ~ 6%, and surplus is solvent, and above constituent mass percentage sum is 100%.
Film forming agent is one or both the mixture in water-white rosin, newtrex.
Activating agent is a kind of or several arbitrarily mixture of glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, decanedioic acid.
Thixotropic agent is rilanit special, stearmide one wherein.
Tackifier are pentalyn.
Solvent is ethyl acetoacetate.
Soldering tin powder is 3 #sn0.3Ag0.7Cu alloy powder.
The preparation method of above-mentioned low-residual high storage stability leadless soldering tin paste, implements according to the following steps:
Step 1, takes scaling powder 10% ~ 15% by mass percentage respectively, soldering tin powder 85% ~ 90%, above constituent mass percent value and be 100%; Wherein said scaling powder is composed of the following components according to mass percent: film forming agent 20% ~ 30%, activating agent 15% ~ 20%, and thixotropic agent is 3% ~ 6%, tackifier 3% ~ 6%, and surplus is solvent, and above constituent mass percentage sum is 100%;
Step 2, adds solvent in reactor, adds tackifier simultaneously, is heated to 75 DEG C, and it is transparent and homogeneous shape that constant temperature is stirred to solution;
Step 3, solution step 2 obtained is reduced to 65 DEG C, adds film forming agent and activating agent, and being stirred to solution is transparent and homogeneous shape;
Step 4, solution step 3 obtained is reduced to 55 DEG C, adds thixotropic agent, and being stirred to solution is transparent and homogeneous shape;
Step 5, flux solvent step 4 obtained is reduced to 30 DEG C, adds soldering tin powder, and continues to stir rapidly, after being cooled to room temperature, continuing to stir 15min, namely obtains low-residual high storage stability leadless soldering tin paste.
Embodiment 1
Step 1, takes 13% scaling powder and 87%3 respectively according to mass percent #sn0.3Ag0.7Cu alloy powder, wherein scaling powder takes 30% water-white rosin by mass percentage respectively, 20% azelaic acid, 3% rilanit special, 3% pentalyn, 44% ethyl acetoacetate;
Step 2, adds ethyl acetoacetate in reactor, adds pentalyn simultaneously, is heated to 75 DEG C, and it is transparent and homogeneous shape that constant temperature is stirred to solution;
Step 3, solution step 2 obtained is reduced to 65 DEG C, adds water-white rosin, azelaic acid, and being stirred to solution is transparent and homogeneous shape;
Step 4, solution step 3 obtained is reduced to 55 DEG C, adds rilanit special, and being stirred to solution is transparent and homogeneous shape;
Step 5, flux solvent step 4 obtained is reduced to 30 DEG C, adds 3 #sn0.3Ag0.7Cu alloy powder, and constantly stir, after being cooled to room temperature, continuing to stir 15min, obtain low-residual high storage stability leadless soldering tin paste.
Embodiment 2
Step 1, takes 15% scaling powder and 85%3 respectively according to mass percent #sn0.3Ag0.7Cu alloy powder, wherein scaling powder takes 10% water-white rosin by mass percentage respectively, 10% newtrex, 10% suberic acid, 8% decanedioic acid, 5% stearmide, 6% pentalyn, 49% ethyl acetoacetate;
Step 2, adds ethyl acetoacetate in reactor, adds pentalyn simultaneously, is heated to 75 DEG C, and it is transparent and homogeneous shape that constant temperature is stirred to solution;
Step 3, solution step 2 obtained is reduced to 65 DEG C, adds water-white rosin, azelaic acid, and being stirred to solution is transparent and homogeneous shape;
Step 4, solution step 3 obtained is reduced to 55 DEG C, adds rilanit special, and being stirred to solution is transparent and homogeneous shape;
Step 5, flux solvent step 4 obtained is reduced to 30 DEG C, adds 3 #sn0.3Ag0.7Cu alloy powder, and constantly stir, after being cooled to room temperature, continuing to stir 15min, obtain low-residual high storage stability leadless soldering tin paste.
Embodiment 3
Step 1, takes 10% scaling powder and 90%3 respectively according to mass percent #sn0.3Ag0.7Cu alloy powder, wherein scaling powder takes 20% water-white rosin by mass percentage respectively, 5% newtrex, 5% adipic acid, 11% pimelic acid, 3% rilanit special, 5% pentalyn, 51% ethyl acetoacetate;
Step 2, adds ethyl acetoacetate in reactor, adds pentalyn simultaneously, is heated to 75 DEG C, and it is transparent and homogeneous shape that constant temperature is stirred to solution;
Step 3, solution step 2 obtained is reduced to 65 DEG C, adds water-white rosin, azelaic acid, and being stirred to solution is transparent and homogeneous shape;
Step 4, solution step 3 obtained is reduced to 55 DEG C, adds rilanit special, and being stirred to solution is transparent and homogeneous shape;
Step 5, flux solvent step 4 obtained is reduced to 30 DEG C, adds 3 #sn0.3Ag0.7Cu alloy powder, and constantly stir, after being cooled to room temperature, continuing to stir 15min, obtain low-residual high storage stability leadless soldering tin paste.
Embodiment 4
Step 1, takes 12% scaling powder and 88%3 respectively according to mass percent #sn0.3Ag0.7Cu alloy powder, wherein scaling powder takes 20% newtrex by mass percentage respectively, 15% glutaric acid, 6% stearmide, 4% pentalyn, 55% ethyl acetoacetate;
Step 2, adds ethyl acetoacetate in reactor, adds pentalyn simultaneously, is heated to 75 DEG C, and it is transparent and homogeneous shape that constant temperature is stirred to solution;
Step 3, solution step 2 obtained is reduced to 65 DEG C, adds water-white rosin, azelaic acid, and being stirred to solution is transparent and homogeneous shape;
Step 4, solution step 3 obtained is reduced to 55 DEG C, adds rilanit special, and being stirred to solution is transparent and homogeneous shape;
Step 5, flux solvent step 4 obtained is reduced to 30 DEG C, adds 3 #sn0.3Ag0.7Cu alloy powder, and constantly stir, after being cooled to room temperature, continuing to stir 15min, obtain low-residual high storage stability leadless soldering tin paste.

Claims (9)

1. a low-residual high storage stability leadless soldering tin paste, is characterized in that, composed of the following components according to mass percent: scaling powder 10% ~ 15%, soldering tin powder 85% ~ 90%, above constituent mass percent value and be 100%; Wherein said scaling powder is composed of the following components according to mass percent: film forming agent 20% ~ 30%, activating agent 15% ~ 20%, and thixotropic agent is 3% ~ 6%, tackifier 3% ~ 6%, and surplus is solvent, and above constituent mass percentage sum is 100%.
2. low-residual high storage stability leadless soldering tin paste according to claim 1, is characterized in that, described film forming agent is one or both the mixture in water-white rosin, newtrex.
3. low-residual high storage stability leadless soldering tin paste according to claim 1, is characterized in that, described activating agent is a kind of or several arbitrarily mixture of glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, decanedioic acid.
4. low-residual high storage stability leadless soldering tin paste according to claim 1, is characterized in that, described thixotropic agent is rilanit special, stearmide one wherein.
5. low-residual high storage stability leadless soldering tin paste according to claim 1, is characterized in that, described tackifier are pentalyn.
6. low-residual high storage stability leadless soldering tin paste according to claim 1, is characterized in that, described solvent is ethyl acetoacetate.
7. low-residual high storage stability leadless soldering tin paste according to claim 1, is characterized in that, described soldering tin powder is 3 #sn0.3Ag0.7Cu alloy powder.
8. a preparation method for low-residual high storage stability leadless soldering tin paste, is characterized in that, implements according to the following steps:
Step 1, takes scaling powder 10% ~ 15% by mass percentage respectively, soldering tin powder 85% ~ 90%, above constituent mass percent value and be 100%; Wherein said scaling powder is composed of the following components according to mass percent: film forming agent 20% ~ 30%, activating agent 15% ~ 20%, and thixotropic agent is 3% ~ 6%, tackifier 3% ~ 6%, and surplus is solvent, and above constituent mass percentage sum is 100%;
Step 2, adds solvent in reactor, adds tackifier simultaneously, is heated to 75 DEG C, and it is transparent and homogeneous shape that constant temperature is stirred to solution;
Step 3, solution step 2 obtained is reduced to 65 DEG C, adds film forming agent and activating agent, and being stirred to solution is transparent and homogeneous shape;
Step 4, solution step 3 obtained is reduced to 55 DEG C, adds thixotropic agent, and being stirred to solution is transparent and homogeneous shape;
Step 5, flux solvent step 4 obtained is reduced to 30 DEG C, adds soldering tin powder, and continues to stir rapidly, after being cooled to room temperature, continuing to stir 15min, namely obtains low-residual high storage stability cleaning-free lead-free tin cream.
9. the preparation method of low-residual high storage stability leadless soldering tin paste according to claim 8, is characterized in that, film forming agent is one or both the mixture in water-white rosin, newtrex; Activating agent is a kind of or several arbitrarily mixture of glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, decanedioic acid; Thixotropic agent is rilanit special, stearmide one wherein; Tackifier are pentalyn; Solvent is ethyl acetoacetate; Soldering tin powder is 3 #sn0.3Ag0.7Cu alloy powder.
CN201410562566.3A 2014-10-21 A kind of low-residual high storage stability lead-free tin cream and preparation method thereof Expired - Fee Related CN104384755B (en)

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Cited By (11)

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CN104942461A (en) * 2015-04-14 2015-09-30 中山市智牛电子有限公司 Tin paste preparation method
CN106825995A (en) * 2015-09-30 2017-06-13 株式会社田村制作所 Solder flux composition and soldering paste
CN107914095A (en) * 2017-10-20 2018-04-17 西安理工大学 A kind of 0.25mm thin spaces leadless soldering tin paste and preparation method thereof
CN107914096A (en) * 2017-10-20 2018-04-17 西安理工大学 It is a kind of suitable for leadless soldering tin paste of the ultra-fine spacing of 0.15mm and preparation method thereof
CN108161269A (en) * 2018-01-03 2018-06-15 深圳市邦大科技有限公司 A kind of Halogen is without sulphur leadless soldering tin paste
CN108555475A (en) * 2018-04-27 2018-09-21 深圳市博士达焊锡制品有限公司 A kind of lead-free and halogen-free solder(ing) paste
CN109877484A (en) * 2019-03-22 2019-06-14 东莞永安科技有限公司 A kind of solder(ing) paste and preparation method thereof of noresidue free of cleaning
CN112643249A (en) * 2020-12-29 2021-04-13 深圳市福英达工业技术有限公司 Halogen-free water-washing soldering flux, lead-free halogen-free water-washing tin paste and preparation method thereof
WO2021115287A1 (en) * 2019-12-09 2021-06-17 青岛歌尔微电子研究院有限公司 Solder flux and preparation method thereof, tin paste and preparation method thereof
CN113798734A (en) * 2021-10-15 2021-12-17 浙江亚通焊材有限公司 Soldering flux for tin-based soldering paste and laser soft soldering paste for electronic packaging
CN114654126A (en) * 2022-04-29 2022-06-24 浙江亚通焊材有限公司 Silver-coated copper soldering paste and preparation method thereof

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104942461A (en) * 2015-04-14 2015-09-30 中山市智牛电子有限公司 Tin paste preparation method
CN106825995A (en) * 2015-09-30 2017-06-13 株式会社田村制作所 Solder flux composition and soldering paste
CN107914095A (en) * 2017-10-20 2018-04-17 西安理工大学 A kind of 0.25mm thin spaces leadless soldering tin paste and preparation method thereof
CN107914096A (en) * 2017-10-20 2018-04-17 西安理工大学 It is a kind of suitable for leadless soldering tin paste of the ultra-fine spacing of 0.15mm and preparation method thereof
CN108161269A (en) * 2018-01-03 2018-06-15 深圳市邦大科技有限公司 A kind of Halogen is without sulphur leadless soldering tin paste
CN108555475A (en) * 2018-04-27 2018-09-21 深圳市博士达焊锡制品有限公司 A kind of lead-free and halogen-free solder(ing) paste
CN109877484A (en) * 2019-03-22 2019-06-14 东莞永安科技有限公司 A kind of solder(ing) paste and preparation method thereof of noresidue free of cleaning
CN109877484B (en) * 2019-03-22 2020-04-14 东莞永安科技有限公司 No-clean and no-residue soldering paste and preparation method thereof
WO2021115287A1 (en) * 2019-12-09 2021-06-17 青岛歌尔微电子研究院有限公司 Solder flux and preparation method thereof, tin paste and preparation method thereof
CN112643249A (en) * 2020-12-29 2021-04-13 深圳市福英达工业技术有限公司 Halogen-free water-washing soldering flux, lead-free halogen-free water-washing tin paste and preparation method thereof
CN112643249B (en) * 2020-12-29 2022-07-22 深圳市福英达工业技术有限公司 Halogen-free water-washing soldering flux, lead-free halogen-free water-washing tin paste and preparation method thereof
CN113798734A (en) * 2021-10-15 2021-12-17 浙江亚通焊材有限公司 Soldering flux for tin-based soldering paste and laser soft soldering paste for electronic packaging
CN113798734B (en) * 2021-10-15 2023-02-24 浙江亚通新材料股份有限公司 Soldering flux for tin-based soldering paste and laser soft soldering paste for electronic packaging
CN114654126A (en) * 2022-04-29 2022-06-24 浙江亚通焊材有限公司 Silver-coated copper soldering paste and preparation method thereof

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