CN106624431A - Tin-zinc lead-free solder and preparation method thereof - Google Patents
Tin-zinc lead-free solder and preparation method thereof Download PDFInfo
- Publication number
- CN106624431A CN106624431A CN201611081765.8A CN201611081765A CN106624431A CN 106624431 A CN106624431 A CN 106624431A CN 201611081765 A CN201611081765 A CN 201611081765A CN 106624431 A CN106624431 A CN 106624431A
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- China
- Prior art keywords
- free solder
- zinc
- graphene
- stannum
- preparation
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
- B23K35/262—Sn as the principal constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
Abstract
The invention provides a tin-zinc lead-free solder and a preparation method thereof. The tin-zinc lead-free solder comprises, by weight, 5%-10% of zinc, 0.1%-0.2% of nickel, 0.6%-2.4% of graphene and the balance tin. The preparation method comprises the steps that (1) a pure zinc ingot, a pure nickel ingot and a pure tin ingot are sealed in a vacuum quartz tube, and then the vacuum quartz tube is filled with high-purity nitrogen protective gas; (2) the raw materials sealed in the step (1) are put into a reaction furnace to be subjected to smelting heat treatment, and the raw materials are completely melted into molten liquid; (3) the graphene is placed in a stirring type ball mill, the stirring type ball mill is filled with liquid nitrogen till a milling ball is completely submerged, then ball milling is conducted, powder obtained through ball milling is taken out and added into the molten liquid in the step (2), and stirring and heat preservation treatment are conducted; and (4) after the graphene in the step (3) and the molten liquid are uniformly smelted, slagging off is conduced, the molten raw materials are subjected to casting forming, and thus the tin-zinc lead-free solder is obtained. The tin-zinc lead-free solder has good welding spot bonding strength and meanwhile can have good oxidation resistance.
Description
Technical field
The invention belongs to technical field of welding materials, and in particular to a kind of stannum zinc lead-free solder and preparation method thereof.
Background technology
Sn-Pb solders in the application existing considerable time of electronics industry, because it has relatively low fusing point, higher
Cost performance and accessibility so as to become topmost solder system, be widely used in non-ferrous metal, food containers,
The fields such as the welding of building, machinery and plumbing installation.However, with the arrival of information age, electronic product emerges in an endless stream, this
A little electronic products are while promoting the well-being of mankind, and the lead contained by it also increasingly pollution of ecological environment and the mankind's is healthy.Root
According to WEEE instructions and the requirement of RoHS instructions, from 1 day July in 2006, the electronics and electric equipment of sale on European market
In prohibit the use of 6 kinds of poisonous and harmful substances such as lead, the mass fraction of wherein lead to must not exceed 0.10%.The states such as the U.S., Japan
The bill of related restriction solder containing pb has been put into effect in succession, and the Chinese government also formulates in time《Electronics and IT products production pollution is anti-
Control management method》, and start to perform in July, 2006.
Sn-Zn systems solder is a kind of lead-free solder for substituting Sn-Pb solders in electronic packaging industry at present, with Sn-Pb
The fusing point of eutectic solder is sufficiently close to, therefore attracts attention.Many-side has been carried out to it to Sn-Zn systems solder people
Research, also obtain many substantial progress and achievement, but also show some shortcomings part in practice.Sn-Zn systems
Solder is poor with the reliability of the bond strength of substrate and solder joint.Additionally, Zn is the element for easily aoxidizing, containing the more melts of Zn
Surface is more readily formed oxide, and the effect of the unprotected melt of oxide for being formed, so as to cause the non-oxidizability of solder
It is poor, limit the application of solder alloy.
The content of the invention
The present invention proposes a kind of stannum zinc lead-free solder, and the solder has good solder joint bond strength, while can have
Preferable non-oxidizability.
The technical scheme is that what is be achieved in that：
A kind of stannum zinc lead-free solder, calculates according to percetage by weight, including following raw material is made：
Zinc 5～10%, nickel 0.1～0.2% and Graphene 0.6～2.4%, balance of stannum.
Preferably, calculate according to percetage by weight, including following raw material is made：
Zinc 7%, nickel 0.16% and Graphene 1.6%, balance of stannum.
It is a further object to provide a kind of preparation method of stannum zinc lead-free solder, comprises the following steps：
1) pure zinc ingot, pure nickel ingot and pure tin ingot are encapsulated in vitreosil pipe, are then charged with highly purified nitrogen and protect
Shield property gas；
2) by step 1) in packaged raw material be put into melting heat treatment in reacting furnace, the liquation after being completely melt；
3) Graphene is placed in stirring ball mill, is filled with liquid nitrogen to being totally submerged after abrading-ball, ball milling is carried out, by ball milling
Rear powder takes out, and adds step 2) liquation in be stirred and isothermal holding；
4) after step 3) after Graphene and liquation melting are uniform, skim, fused raw material cast molding, obtain final product.
Further, the step 1) vacuum of vitreosil pipe reaches below 2.5Pa, is filled with highly purified nitrogen protection
Property gas is to 1.1～1.3 × 105Pa。
Further, the step 2) melting heat treatment temperature be 600～700 DEG C.
Further, the step 3) isothermal holding temperature be 650～680 DEG C.
Further, the step 3) ratio of grinding media to material be 6～8:1.
Beneficial effects of the present invention：
1st, because Graphene itself has stable conjugated electron system, thus it is special to show many excellent physics
Property.For example：The intensity of Graphene is more than 100 times of steel, is the material of the maximum intensity for obtaining at present up to 130GPa；Graphene
Thermal conductivity is 5 × 103W·m-1K-1, it is 3 times of diamond；Graphene has known highest carrier mobility, be 1.5 ×
104cm2·V-1S-1；In addition, Graphene also has some other special nature, the such as ferromagnetism and room-temperature quantum of room temperature suddenly
Your effect etc..The Graphene that the present invention passes through addition proper proportion, can reduce the contact resistance of contact, improve resistance fusion welding etc.
Performance so as to as the enhancing phase of lead-free solder, reaches environmental protection, the reliable requirement of welding, instead of traditional stannum-lead welding
Material, improves the performance of lead-free solder.Additionally, Graphene and solid solution nickel hydroxide (Ni) crystal interact so that solid solution Ni preferentially with
Oxygen reacts, and in the liquid level moment of fusion welding one layer of thin and compact oxide-film is formed, and the oxide-film can be effectively isolated outer
The oxygen on boundary is entered in film, the Zn in fusion welding can be suppressed to aoxidize, so as to significantly improve the non-oxidizability of solder alloy
Energy.
2nd, preparation method of the invention is first processed alloy raw material by nitrogen protection in a vacuum, then will be through grinding
The Graphene of process carries out high-temperature fusion process rather than carries out the sintering processes of a step with molten alloy, improves stannum zinc unleaded
The fusing point of solder so that fusing point reaches 240 DEG C (higher than fusing points of 200 DEG C or so of common tin zinc lead-free solder).
Specific embodiment
Embodiment 1
A kind of stannum zinc lead-free solder, calculates according to percetage by weight, including following raw material is made：
Zinc 7%, nickel 0.16% and Graphene 1.6%, balance of stannum.
Preparation method, comprises the following steps：
1) pure zinc ingot, pure nickel ingot and pure tin ingot are encapsulated in vitreosil pipe, vacuum reaches below 2.5Pa, so
After be filled with highly purified nitrogen protective gas to 1.2 × 105Pa；
2) by step 1) in packaged raw material be put into 600 DEG C of heat treatments of melting in reacting furnace, the liquation after being completely melt；
3) Graphene is placed in stirring ball mill, is filled with liquid nitrogen to being totally submerged after abrading-ball, carry out ball milling, ball material matter
Amount is than being 6:1, the powder after ball milling is taken out, add step 2) liquation in be stirred and isothermal holding, isothermal holding temperature
Spend for 650 DEG C, the time is 2h；
4) after step 3) after Graphene and liquation melting are uniform, skim, fused raw material cast molding, obtain final product.
Embodiment 2
A kind of stannum zinc lead-free solder, calculates according to percetage by weight, including following raw material is made：
Zinc 5%, nickel 0.2% and Graphene 2.4%, balance of stannum.
Preparation method, comprises the following steps：
1) pure zinc ingot, pure nickel ingot and pure tin ingot are encapsulated in vitreosil pipe, vacuum reaches below 2.5Pa, so
After be filled with highly purified nitrogen protective gas to 1.1 × 105Pa；
2) by step 1) in packaged raw material be put into 650 DEG C of heat treatments of melting in reacting furnace, the liquation after being completely melt；
3) Graphene is placed in stirring ball mill, is filled with liquid nitrogen to being totally submerged after abrading-ball, carry out ball milling, ball material matter
Amount is than being 7:1, the powder after ball milling is taken out, add step 2) liquation in be stirred and isothermal holding, isothermal holding temperature
Spend for 650 DEG C, the time is 2h；
4) after step 3) after Graphene and liquation melting are uniform, skim, fused raw material cast molding, obtain final product.
Embodiment 3
A kind of stannum zinc lead-free solder, calculates according to percetage by weight, including following raw material is made：
Zinc 10%, nickel 0.1% and Graphene 0.6%, balance of stannum.
Preparation method, comprises the following steps：
1) pure zinc ingot, pure nickel ingot and pure tin ingot are encapsulated in vitreosil pipe, vacuum reaches below 2.5Pa, so
After be filled with highly purified nitrogen protective gas to 1.3 × 105Pa；
2) by step 1) in packaged raw material be put into 700 DEG C of heat treatments of melting in reacting furnace, the liquation after being completely melt；
3) Graphene is placed in stirring ball mill, is filled with liquid nitrogen to being totally submerged after abrading-ball, carry out ball milling, ball material matter
Amount is than being 8:1, the powder after ball milling is taken out, add step 2) liquation in be stirred and isothermal holding, isothermal holding temperature
Spend for 680 DEG C, the time is 1.5h；
4) after step 3) after Graphene and liquation melting are uniform, skim, fused raw material cast molding, obtain final product.
Embodiment 4
Stannum zinc lead-free solder that embodiment 1-3 is obtained carries out DSC tests using Germany Netzsch STA 404, in room
Between warm to 180 DEG C, heating rate is 8 DEG C/min, and between 180～360 DEG C, heating rate is 2 DEG C/min, the results are shown in Table 1,
As can be seen from Table 1 the fusion temperature scope of stannum zinc lead-free solder of the invention is 236～243 DEG C.
The fusion temperature of the embodiment 1-3 stannum zinc lead-free solder of table 1
Presently preferred embodiments of the present invention is the foregoing is only, not to limit the present invention, all essences in the present invention
Within god and principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (7)
1. a kind of stannum zinc lead-free solder, it is characterised in that calculate according to percetage by weight, including following raw material is made：
Zinc 5～10%, nickel 0.1～0.2% and Graphene 0.6～2.4%, balance of stannum.
2. stannum zinc lead-free solder according to claim 1, it is characterised in that calculate according to percetage by weight, including it is following
Raw material is made：
Zinc 7%, nickel 0.16% and Graphene 1.6%, balance of stannum.
3. the preparation method of stannum zinc lead-free solder according to claim 1 and 2, it is characterised in that comprise the following steps：
1) pure zinc ingot, pure nickel ingot and pure tin ingot are encapsulated in vitreosil pipe, are then charged with highly purified nitrogen protectiveness
Gas；
2) by step 1) in packaged raw material be put into melting heat treatment in reacting furnace, the liquation after being completely melt；
3) Graphene is placed in stirring ball mill, is filled with liquid nitrogen to being totally submerged after abrading-ball, ball milling is carried out, after ball milling
Powder takes out, and adds step 2) liquation in be stirred and isothermal holding；
4) after step 3) after Graphene and liquation melting are uniform, skim, fused raw material cast molding, obtain final product.
4. the preparation method of stannum zinc lead-free solder according to claim 3, it is characterised in that the step 1) vitreosil
The vacuum of pipe reaches below 2.5Pa, is filled with highly purified nitrogen protective gas to 1.1～1.3 × 105Pa。
5. the preparation method of stannum zinc lead-free solder according to claim 3, it is characterised in that the step 2) at smelting heat
The temperature of reason is 600～700 DEG C.
6. the preparation method of stannum zinc lead-free solder according to claim 3, it is characterised in that the step 3) insulation at
Reason temperature is 650～680 DEG C.
7. the preparation method of stannum zinc lead-free solder according to claim 6, it is characterised in that the step 3) ratio of grinding media to material is
6～8:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611081765.8A CN106624431A (en) | 2016-11-30 | 2016-11-30 | Tin-zinc lead-free solder and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611081765.8A CN106624431A (en) | 2016-11-30 | 2016-11-30 | Tin-zinc lead-free solder and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106624431A true CN106624431A (en) | 2017-05-10 |
Family
ID=58814491
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611081765.8A Pending CN106624431A (en) | 2016-11-30 | 2016-11-30 | Tin-zinc lead-free solder and preparation method thereof |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1198117A (en) * | 1995-09-29 | 1998-11-04 | 松下电器产业株式会社 | Lead-free solder |
| CN1304344A (en) * | 1999-03-16 | 2001-07-18 | 日本板硝子株式会社 | Leadless solder |
| CN101049659A (en) * | 2007-05-17 | 2007-10-10 | 戴国水 | Tin, zinc, copper, and nickel solder without lead |
| CN102513720A (en) * | 2011-12-23 | 2012-06-27 | 哈尔滨工业大学深圳研究生院 | High-performance tin-based solder alloy and preparation method thereof |
| CN103706962A (en) * | 2013-12-30 | 2014-04-09 | 大连理工大学 | Sn-Zn-Ni lead-free solder alloy for aluminum copper soldering |
| CN103737195A (en) * | 2013-12-30 | 2014-04-23 | 大连理工大学 | Sn-Zn-Bi-base lead-free solder alloy for soft soldering of aluminum and copper |
| US20140199115A1 (en) * | 2011-08-02 | 2014-07-17 | Alpha Metals, Inc. | Solder compositions |
| CN106001979A (en) * | 2016-05-19 | 2016-10-12 | 厦门圣之岛金属科技有限公司 | Grapheme, zinc oxide crystal whisker and tin base composite material and preparation method thereof |
-
2016
- 2016-11-30 CN CN201611081765.8A patent/CN106624431A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1198117A (en) * | 1995-09-29 | 1998-11-04 | 松下电器产业株式会社 | Lead-free solder |
| CN1304344A (en) * | 1999-03-16 | 2001-07-18 | 日本板硝子株式会社 | Leadless solder |
| CN101049659A (en) * | 2007-05-17 | 2007-10-10 | 戴国水 | Tin, zinc, copper, and nickel solder without lead |
| US20140199115A1 (en) * | 2011-08-02 | 2014-07-17 | Alpha Metals, Inc. | Solder compositions |
| CN102513720A (en) * | 2011-12-23 | 2012-06-27 | 哈尔滨工业大学深圳研究生院 | High-performance tin-based solder alloy and preparation method thereof |
| CN103706962A (en) * | 2013-12-30 | 2014-04-09 | 大连理工大学 | Sn-Zn-Ni lead-free solder alloy for aluminum copper soldering |
| CN103737195A (en) * | 2013-12-30 | 2014-04-23 | 大连理工大学 | Sn-Zn-Bi-base lead-free solder alloy for soft soldering of aluminum and copper |
| CN106001979A (en) * | 2016-05-19 | 2016-10-12 | 厦门圣之岛金属科技有限公司 | Grapheme, zinc oxide crystal whisker and tin base composite material and preparation method thereof |
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| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
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Application publication date: 20170510 |
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| RJ01 | Rejection of invention patent application after publication |