CN1981978A - Lead-free soldering tin crease and its production - Google Patents
Lead-free soldering tin crease and its production Download PDFInfo
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- CN1981978A CN1981978A CN 200510121503 CN200510121503A CN1981978A CN 1981978 A CN1981978 A CN 1981978A CN 200510121503 CN200510121503 CN 200510121503 CN 200510121503 A CN200510121503 A CN 200510121503A CN 1981978 A CN1981978 A CN 1981978A
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Abstract
A non-lead tin solder cream with high storage stability, wetting power for soldering, heat shock resistance, and solder strength is proportionally prepared from Sn-Zn based non-lead alloy powder, flux and protective activated film layer containing neutral organic solvent with high boiling point, neutral resin and activating agent with high decomposing temp through mixing and grinding said alloy powder with the raw materials of said activated film in vacuum, adding flux, and stirring.
Description
Technical field
The present invention relates to a kind of solder(ing) paste and preparation method thereof, particularly relate to a kind of microelectronics welding leadless soldering tin paste and preparation method thereof.
Background technology
Because human society is imperative to the control of the materials that are harmful to health such as lead, cadmium, mercury to the attention of environmental protection.In the microelectronics welding, the application of lead-free solder has formally started.Leadless soldering tin paste then is an important materials in the microelectronics Packaging.In the leadless soldering tin paste product of existing using value, with Sn-Ag-Cu, Sn-Bi series is comparatively extensive.But they respectively have shortcoming, and for example: Sn-Ag-Cu series solder(ing) paste cost is too high, and the melting temperature height more than 220 ℃, has proposed higher requirement to the electronic devices and components and the welding equipment of electronic product wiring board.Add the shortage of Ag resource, be unfavorable for that the large tracts of land of Sn-Ag-Cu series leadless solder(ing) paste is promoted.Though Sn-Bi series leadless solder(ing) paste has lower melting temperature, its weld strength is low excessively, and fragility is big, and tough is low etc., has influenced its application performance, cream product that neither be very good.
Some studies show that, Sn-Zn base system row product can overcome the cost height of above leadless soldering tin paste alloy material, resource shortage, the deficiency that fusing point height and resistance to sudden heating are low excessively, the Zn metals resources is abundant, and with low cost, Sn-Zn is that alloy melting point is lower, between 185～210 ℃, add other necessary metals again,, can obviously improve resistance to sudden heating as Bi, In etc.
But, compare with Sn-Ag-Cu or Sn-Ag or Sn-Bi lead-free solder, the non-constant of the wetability of Sn-Zn base lead-free solder, the storage stability wretched insufficiency, tackify is fast.Generally speaking, because the above-mentioned defective of Sn-Zn base lead-free solder, the pad place easily forms the defective of forms such as bead, space, rosin joint, welding slag.Because the Zn metal in the Sn-Zn alloy material has very low oxidizing potential, oxidizing potential than pb is low, when therefore in air, welding, be oxidized to the oxide of Zn easily, this oxide is salt for the activation acid group in the scaling powder is reacted into again in preheating or fusion process subsequently, consume a large amount of activation compositions on the one hand, oxide self can't be gone in the welding material in fusion on the other hand, and being excluded becomes scolding tin or scolding tin slag, causes forming in the pad space, rosin joint etc.Such solder(ing) paste also is because Zn is easily oxidized, and tackify is fast in storage process, instability, and difficult printing is off line or the like.
For this reason, at how to weaken even prevent that Zn is oxidized in solder(ing) paste in the Sn-Zn base lead-free alloy powder, people have carried out many researchs and trial.For example be proposed in the inert metal that welding powder particle surface coating one deck is difficult for oxidation, as Au, Ni etc., but this kind method is with high costs, and operation easier is big; Also have plenty of the novel scaling powder of research and development,, bigger gap is still arranged from reaching satisfactory state though certain effect is arranged.
Summary of the invention
Technical problem to be solved by this invention is, a kind of storage stability height, solder wettability and thermal shock resistance is good, weld strength is high, cost is low leadless soldering tin paste are provided.
For solving above technical problem, product technology scheme of the present invention is: a kind of leadless soldering tin paste, comprise Sn-Zn base lead-free alloy welding powder and scaling powder, key is: also comprise buffer protection activation rete, described Sn-Zn base lead-free alloy welding powder, scaling powder account for 88～91%, 6～11% of whole leadless soldering tin paste gross mass respectively, and all the other components are described buffer protection activation rete; The component of described buffer protection activation rete and each component shared mass percent in described whole buffer protection activation rete is respectively: the neutral organic solvent of 38～70% higher boiling; 10～35% is neutral or near resinene; All the other content have high decomposition temperature and contain naphthene series or the aromatic series activator that is no less than 6 C atoms.
As improvement of the present invention, the component of described Sn-Zn base lead-free alloy welding powder and wherein each component shared mass percent in described Sn-Zn base lead-free alloy welding powder be respectively: 4.5～10% Sn-Zn base; Can comprise that also one or more are selected from Bi, Ag, Cu, Ni, Ce, In, Mo, Co, Fe, P, Ge, the metal ingredient of Ga accounts for 0.10～3.5%; All the other are Sn and unavoidable impurities.
Further improve one as the present invention, the neutral organic solvent of described higher boiling is any one or its combination in organic alcohol, ether, ester, the hydrocarbons.
Further improve two as the present invention, described neutrality or be in organic crylic acid resin, alkyd resins, rosin and various modified rosin resin, organic siliconresin, polyurethane resin, the polyvinyl resin any one near resinene.
Further improve three as the present invention, described naphthene series or aromatic series activator are the activator of decomposition temperature in 135 ℃～240 ℃ scopes, and the H on its carbon atom partly or entirely replaces for halogen; Perhaps part replaces for halogen, and part replaces for other groups.
Further improve four as the present invention, described leadless soldering tin paste is an alloy powder type solder(ing) paste.
For solving above technical problem, the corresponding method and technology scheme of the present invention is: a kind of preparation method of leadless soldering tin paste the steps include:
A, with of the formation material agent of Sn-Zn base lead-free alloy welding powder with buffer protection activation rete, fully agitation grinding mixes under the condition of vacuumizing, and forms one deck is being less than or equal to cushioning effect in 150 ℃ normal temperature and the mesophilic range buffer protection activation rete on described Sn-Zn base leadless alloy powder particles surface;
Wherein, the component of described buffer protection activation rete and each component shared mass percent in described whole buffer protection activation rete is respectively: the neutral organic solvent of 38～70% higher boiling; 10～35% is neutral or near resinene; All the other content have high decomposition temperature and contain naphthene series or the aromatic series activator that is no less than 6 C atoms.
B, scaling powder is joined in the formed mixture of a step, and mix.
As the improvement of the inventive method scheme, the component of described Sn-Zn base lead-free alloy welding powder and wherein each component shared mass percent in described Sn-Zn base lead-free alloy welding powder be respectively: 4.5～10% Sn-Zn base; Can comprise that also one or more are selected from Bi, Ag, Cu, Ni, Ce, In, Mo, Co, Fe, P, Ge, the metal ingredient of Ga accounts for 0.10～3.5%; All the other are Sn and unavoidable impurities.
As the further improvement of the inventive method scheme, described buffer protection activation rete and scaling powder are pasty masses.
By implementing the technical solution of the present invention, buffer protection activation rete covered in advance be applied to Sn-Zn base alloy welding powder particle surface.When normal temperature storage; when paste reflows preheating (T≤150 ℃); composition in this layer lotion does not all decompose; not with the alloyed powder particle in Zn react; play the easy reactive group and Zn or the reaction of its oxide that intercept in the outer scaling powder simultaneously; it is not oxidated to play the protection alloy welding powder, thereby reaches the purpose that significantly improves storage stability, solder wettability and thermal shock resistance.Bead, rosin joint, void defects obviously reduce simultaneously, and weld strength height, preparation cost hang down also cheap.
The specific embodiment
Embodiment 1:
Component M. gets the Sn-Zn base lead-free alloy welding powder that is made into according to following mass percent: Sn-8.5Zn-1.5Bi (promptly Zn accounts for 8.5% in Sn-Zn base lead-free alloy welding powder, and Bi accounts for 1.5%, and all the other are Sn) ready, and particle size range is 25～45 μ m, weight 44.5kg.
Component P. prepares buffer protection reactivity cream layer: with the 900g carbitol, 495g Foral, 105g3-hydroxy-4-methyl benzoic acid are miscible even under heating condition.Mixture total weight amount 1500g.
Component F. self-control leadless soldering tin paste scaling powder: with salicylic acid 400g, dioctyl phthalate 1600g and natural rosin resins 2000g heating are miscible evenly, make total mixture 4000g.
The component M of whole total amounts is mixed in special-purpose airtight container with the component P of whole total amounts, and vacuumize simultaneously.Speed of agitator is decided to be 120rpm, mixes 30 minutes.The component F that adds total weight again continued to mix 20 minutes.Can obtain leadless soldering tin paste product of the present invention.This product all significantly is better than not containing the Sn-Zn base leadless soldering tin paste of component P (being the buffer protection active layer) in storage stability, resistance to sudden heating, bead, rosin joint, welding slag various aspects.
Embodiment 2:
Preparation process is with embodiment 1.Just the material of each component and content are to as follows:
Component M:Sn-Zn base lead-free alloy welding powder is Sn-9Zn (promptly Zn accounts for 9.0% in Sn-Zn base lead-free alloy welding powder, and all the other are Sn), changes the footpath scope: 25～45 μ m, weight 44kg.
Component P:880g butyl cellosolve, 520g newtrex resin, 100g dihydroxyphenyl acetic acid.
Component F: with embodiment 1.
Embodiment 3:
Preparation process is with embodiment 1, and just the material of each component and content are to as follows:
Component M:Sn-Zn base lead-free alloy welding powder is Sn-7.5Zn-1.0Bi (promptly Zn accounts for 7.5% in Sn-Zn base lead-free alloy welding powder, and Bi accounts for 1.0%, and all the other are Sn), particle size range: 25～45 μ m, weight 44kg.
Component P:850g propane diols list phenyl ether, 135g acrylic resin, 400g Foral resin, 150g dihydroxycinnamic acid.
Component F: succinic acid 380g, adipic acid 100g, dibutyl phthalate 1500g, Foral resin 2000g.
The variation of each component mainly is the actual requirement according to different electric appliance circuits plates, and the variation of alloy welding powder composition and corresponding adjustment, in the hope of obtaining optimum properties.
Claims (10)
1, a kind of leadless soldering tin paste; comprise Sn-Zn base lead-free alloy welding powder and scaling powder; it is characterized in that: also comprise buffer protection activation rete; described Sn-Zn base lead-free alloy welding powder, scaling powder account for 88～91%, 6～11% of whole leadless soldering tin paste gross mass respectively, and all the other components are described buffer protection activation rete.
2, leadless soldering tin paste according to claim 1 is characterized in that: the component of described buffer protection activation rete and each component shared mass percent in described whole buffer protection activation rete is respectively: the neutral organic solvent of 38～70% higher boiling; 10～35% is neutral or near resinene; All the other content have high decomposition temperature and contain naphthene series or the aromatic series activator that is no less than 6 C atoms.
3, leadless soldering tin paste according to claim 2 is characterized in that: the component of described Sn-Zn base lead-free alloy welding powder and wherein each component shared mass percent in described Sn-Zn base lead-free alloy welding powder be respectively: 4.5～10% Sn-Zn base; Can comprise that also one or more are selected from Bi, Ag, Cu, Ni, Ce, In, Mo, Co, Fe, P, Ge, the metal ingredient of Ga accounts for 0.10～3.5%; All the other are Sn and unavoidable impurities.
4, according to the described leadless soldering tin paste of any one claim in the claim 1 to 3, it is characterized in that: the neutral organic solvent of described higher boiling is any one or its combination in organic alcohol, ether, ester, the hydrocarbons.
5, according to the described leadless soldering tin paste of any one claim in the claim 1 to 3, it is characterized in that: described neutrality or be in organic crylic acid resin, alkyd resins, rosin and various modified rosin resin, organic siliconresin, polyurethane resin, the polyvinyl resin any one near resinene.
6, according to the described leadless soldering tin paste of any one claim in the claim 1 to 3, it is characterized in that: described naphthene series or aromatic series activator are the activator of decomposition temperature in 135 ℃～240 ℃ scopes, and the H on its carbon atom partly or entirely replaces for halogen; Perhaps part replaces for halogen, and part replaces for other groups.
7, according to the described leadless soldering tin paste of any one claim in the claim 1 to 3, it is characterized in that: described leadless soldering tin paste is an alloy powder type solder(ing) paste.
8, a kind of preparation method of leadless soldering tin paste the steps include:
A, with of the formation material agent of Sn-Zn base lead-free alloy welding powder with buffer protection activation rete, fully agitation grinding mixes under the condition of vacuumizing, and forms one deck is being less than or equal to cushioning effect in 150 ℃ normal temperature and the mesophilic range buffer protection activation rete on described Sn-Zn base leadless alloy powder particles surface;
Wherein, the component of described buffer protection activation rete and each component shared mass percent in described whole buffer protection activation rete is respectively: the neutral organic solvent of 38～70% higher boiling; 10～35% is neutral or near resinene; All the other content have high decomposition temperature and contain naphthene series or the aromatic series activator that is no less than 6 C atoms.
B, scaling powder is joined in the formed mixture of a step, and mix.
9, the preparation method of leadless soldering tin paste according to claim 8 is characterized in that: the component of described Sn-Zn base lead-free alloy welding powder and wherein each component shared mass percent in described Sn-Zn base lead-free alloy welding powder be respectively: 4.5～10% Sn-Zn base; One or more are selected from Bi, Ag, and Cu, Ni, Ce, In, Mo, Co, Fe, P, Ge, the metal ingredient of Ga accounts for 0.10～3.5%; All the other are Sn and unavoidable impurities.
10, the preparation method of leadless soldering tin paste according to claim 9 is characterized in that: described buffer protection activation rete and scaling powder are pasty masses.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101215035A CN100445017C (en) | 2005-12-28 | 2005-12-28 | Lead-free soldering tin crease and its production |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101215035A CN100445017C (en) | 2005-12-28 | 2005-12-28 | Lead-free soldering tin crease and its production |
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| CN1981978A true CN1981978A (en) | 2007-06-20 |
| CN100445017C CN100445017C (en) | 2008-12-24 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2005101215035A Expired - Fee Related CN100445017C (en) | 2005-12-28 | 2005-12-28 | Lead-free soldering tin crease and its production |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102198567A (en) * | 2011-05-09 | 2011-09-28 | 深圳市同方电子新材料有限公司 | Sn-Zn-based lead-free solder paste |
| CN103212919A (en) * | 2013-03-22 | 2013-07-24 | 宁波市鄞州品达电器焊料有限公司 | Improved lead-free solder wire and flux thereof |
| CN105033508A (en) * | 2015-07-31 | 2015-11-11 | 安徽江威精密制造有限公司 | Soldering flux material composite and soldering flux preparing method |
| CN107553007A (en) * | 2017-10-19 | 2018-01-09 | 广东工业大学 | A kind of preparation method of low temperature Nanometer Copper welding material |
| CN108203776A (en) * | 2017-12-21 | 2018-06-26 | 柳州智臻智能机械有限公司 | A kind of high-strength tin spelter soldering alloy and preparation method thereof |
| CN108500501A (en) * | 2018-04-09 | 2018-09-07 | 苏州科技大学 | A kind of epoxy tin cream |
| CN108526756A (en) * | 2018-04-11 | 2018-09-14 | 苏州龙腾万里化工科技有限公司 | A kind of cleaning-free scaling powder |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6416590B1 (en) * | 1998-07-02 | 2002-07-09 | Matsushita Electric Industrial Co., Ltd. | Solder powder and method for preparing the same and solder paste |
| JP4438974B2 (en) * | 2000-10-05 | 2010-03-24 | 千住金属工業株式会社 | Solder paste |
| JP3788335B2 (en) * | 2001-12-07 | 2006-06-21 | 千住金属工業株式会社 | Solder paste |
| US7357291B2 (en) * | 2002-01-30 | 2008-04-15 | Showa Denko K.K. | Solder metal, soldering flux and solder paste |
| JP4042418B2 (en) * | 2002-01-30 | 2008-02-06 | 昭和電工株式会社 | Soldering flux |
| JP4337326B2 (en) * | 2002-10-31 | 2009-09-30 | 千住金属工業株式会社 | Lead-free solder and soldered articles |
-
2005
- 2005-12-28 CN CNB2005101215035A patent/CN100445017C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102198567A (en) * | 2011-05-09 | 2011-09-28 | 深圳市同方电子新材料有限公司 | Sn-Zn-based lead-free solder paste |
| CN103212919A (en) * | 2013-03-22 | 2013-07-24 | 宁波市鄞州品达电器焊料有限公司 | Improved lead-free solder wire and flux thereof |
| CN105033508A (en) * | 2015-07-31 | 2015-11-11 | 安徽江威精密制造有限公司 | Soldering flux material composite and soldering flux preparing method |
| CN107553007A (en) * | 2017-10-19 | 2018-01-09 | 广东工业大学 | A kind of preparation method of low temperature Nanometer Copper welding material |
| CN108203776A (en) * | 2017-12-21 | 2018-06-26 | 柳州智臻智能机械有限公司 | A kind of high-strength tin spelter soldering alloy and preparation method thereof |
| CN108500501A (en) * | 2018-04-09 | 2018-09-07 | 苏州科技大学 | A kind of epoxy tin cream |
| CN108526756A (en) * | 2018-04-11 | 2018-09-14 | 苏州龙腾万里化工科技有限公司 | A kind of cleaning-free scaling powder |
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| Publication number | Publication date |
|---|---|
| CN100445017C (en) | 2008-12-24 |
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Granted publication date: 20081224 Termination date: 20101228 |