CN101342641B - Method of producing tin-silver-zinc system leadless soldering plaster - Google Patents

Method of producing tin-silver-zinc system leadless soldering plaster Download PDF

Info

Publication number
CN101342641B
CN101342641B CN200810054271XA CN200810054271A CN101342641B CN 101342641 B CN101342641 B CN 101342641B CN 200810054271X A CN200810054271X A CN 200810054271XA CN 200810054271 A CN200810054271 A CN 200810054271A CN 101342641 B CN101342641 B CN 101342641B
Authority
CN
China
Prior art keywords
lead
silver
tin
powder
free solder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN200810054271XA
Other languages
Chinese (zh)
Other versions
CN101342641A (en
Inventor
刘永长
韦晨
余黎明
徐荣雷
马宗青
赵倩
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tianjin University
Original Assignee
Tianjin University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Tianjin University filed Critical Tianjin University
Priority to CN200810054271XA priority Critical patent/CN101342641B/en
Publication of CN101342641A publication Critical patent/CN101342641A/en
Application granted granted Critical
Publication of CN101342641B publication Critical patent/CN101342641B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

The invention relates to a tin silver zinc series lead-free solder paste and a preparation method thereof. The solder paste is made from the components with the following weight portions of 99.5-85 percent of tin silver zinc series lead-free alloy powder and 0.5-15 percent of soldering flux. The raw materials are mixed evenly by the portions and made into blocks under the pressure of 2-10MPa. The blocks are put in a high temperature differential scanning calorimetry instrument or a tube-typed sintering furnace, are sintered after argon gas is pumped in, and are heated to 455-535K with the velocity of 5-40K/min. The temperature is maintained for sintering for 0-2 hours, and then the temperature is reduced to room temperature with the velocity of 10-50K/min. The tin silver zinc series lead-free solder blocks after being sintered are processed by a atomization device and are made into the lead-free solder powder with the grain diameters of 10-50mum. The lead-free solder powder and the soldering flux are mixed evenly. The components of the invention are convenient and simple to be mixed evenly. More importantly, the mixing process does not to be carried out under high temperature, saves time and energy. Compared with other method, the sintering method of the invention has simple technology and low cost.

Description

The preparation method of tin-silver-zinc system leadless soldering plaster
Technical field
The present invention relates to a kind of soldering paste and its preparation method, particularly tin-silver-zinc system leadless soldering plaster and preparation method thereof.
Background technology
Work closely-related various electronic product when promoting the well-being of mankind with the human lives, also because of the use of solder containing pb in the electronic product healthy and ecological environment of harm humans day by day.The discarded tissue of electronic electric equipment under the leader of European Union (WEEE) requirement stopped in the electronic assemblies industry in 2006 uses lead-containing materials.American National electronics manufacturing association (NEMI) specially for carrying out one " the unleaded plan of the welding of NEMI " by name for this reason comes the unleaded use problem that is assemblied in the electronics industry of system research; The main consumer electronics manufacturing enterprise of Japan also promises to undertake round Realization leadless electronic assembling as early as possible one after another, and everything makes the research of lead-free solder extremely urgent.For meeting the unleaded tide of global synchronization welding, the lead-free solder patent barrier of avoiding having developed is in the world formulated the task of top priority that the lead-free solder development strategy that is fit to China's actual conditions has become China Electronics's assembly industry.
Along with the develop rapidly of electronic industry, science and technology is brought in constant renewal in, and the microminiaturized trend of electronic device is more and more obvious, and traditional welding wire, welding rod more and more can not satisfy microminiaturized requirement, and soldering paste then becomes the direction of Future Development.Soldering paste is mixed with scaling powder by scolder and forms, thus necessarily required in the research and development process of soldering paste corresponding scaling powder can with the supporting use of scolder.
In the Sn-Ag-Zn alloy, Zn can combine with anticorrosive elements A g and generate intermetallic compound, corrosion potential is sharply reduced, and wetability is suitable with the Sn-Ag eutectic solder.Compare with Sn-Ag, Sn-Ag-Zn can provide superior mechanical performance in many aspects, and it has preferably intensity and does not lose a bit ductility, and high temperature creep property significantly improves, and reduces alloy melting point a little.With this high-performance solder alloy is research object, adds scaling powder, solves and compares with traditional Sn-Pb scolder, and the lead-free solder wetability is poor, and easily oxidation, and the high deficiency of fusing point obtain the lead-free solder paste of excellent performance.
At present, the preparation of soldering paste gets so that certain proportion is mixed with scaling powder mainly by after the block powder process with scolder.The preparation raw material of scolder is generally the block of each metal or alloy, prepare scolder by melting, the poly-partially of component taken place in fusion process easily, for obtaining the uniform product of component, need to stir for a long time (according to the scope of the enterprise difference, this process required time difference, even but small business also need to stir about 2 hours).Because be to be stirred under the molten condition to carry out, then preparation process will remain on hot conditions, and this will cause heat energy loss, consumes energy.
Summary of the invention
In order to solve the deficiencies in the prior art, the object of the invention provides tin-silver-zinc system leadless soldering plaster and preparation method thereof:
The present invention is realized by following technical proposals:
Tin-silver-zinc system leadless soldering plaster of the present invention, the component of soldering paste and mass percent are respectively 99.5-85% tin-silver-zinc series lead-free alloy powder and 0.5-15% scaling powder.
The particle diameter of described tin-silver-zinc series lead-free alloyed powder is 10-50 μ m.
The component of described tin-silver-zinc series lead-free alloyed powder and mass percent are:
Tin 99-85
Silver 0.01-4.5
Zinc 0.01-5
Bismuth 0-5
Indium 0-4
Rare earth element 0-5
Gallium 0-2.5
Phosphorus 0-3.
The preparation method of tin-silver-zinc system leadless soldering plaster of the present invention, step is as follows:
1) in proportion raw material is fully mixed, under the pressure of 2-10MPa, make block, described block is put into high temperature difference scanning calorimeter instrument or tubular type sintering furnace, feed argon gas, carrying out sintering, is 5K/min-40K/min with speed, is warming up to 455-535K, at this temperature heat preservation sintering 0-2 hour, reduce to room temperature with the speed of 10K/min-50K/min then;
2) the lead-free solder of tin silver zinc series block behind the sintering is passed through atomization plant, making particle diameter is the lead-free solder powder of 10-50 μ m;
3) prepared lead-free solder powder is mixed with scaling powder also evenly.
The particle diameter of described lead-free solder of tin silver zinc series powder is 10-50 μ m, be that each alloying element of 99.99% is made into tin silver zinc lead-free solder by mass ratio 99-85:0.01-4.5:0.01-5 with purity, can add the bismuth of 0-5 and the indium of 0-4 for improving wetability on this basis, the rare earth element that can add 0-5 for thinning microstructure is for improving gallium and the 0-3 phosphorus that non-oxidizability can add 0-2.5.
It is 2008101071494 scaling powders of being applied for that described scaling powder adopts application number.
The raw material state that the present invention uses is Powdered, and it is convenient and even easily that each component is mixed, and the most important thing is that this process need not high temperature and carries out.So this mixed process has been saved the time on the one hand, saved the energy on the other hand.Method by sintering is prepared into bulk then, although the finished product composition that obtains after the preparation is even, its porosity is big, and is not really fine and close, so can not make welding wire or welding rod uses, but can eliminate above-mentioned influence by the required powder by atomization process of preparation soldering paste.Scolder behind the sintering is made solder powder by powder by atomization, again with the mixed soldering paste that gets of scaling powder.Make that by said method preparing soldering paste by the powdered form metal becomes possibility, so just avoided the energy resource consumption that long-time high temperature heating is caused in the fusion process.Comparing with the soldering paste that makes by melting by the soldering paste that the method makes, only is to have changed preparation process, to not influence of end properties.
Described preparation method is a powder applicable to the reset condition of each metal element, and sintering method is compared with other method, and its technology is simple, and cost is low.
The specific embodiment
Example 1
Earlier be that 99.99% tin, silver, zinc powder are that 96.5:3.49:0.01 fully mixes by mass ratio with purity, then under the pressure of 2MPa, make block, described block is put into high temperature difference scanning calorimeter instrument or tubular type sintering furnace, feed argon gas, carrying out sintering, is 5K/min with speed, is warming up to 495K, at this temperature heat preservation sintering 10min, reduce to room temperature with the speed of 10K/min then.By atomization plant, making particle diameter is the lead-free solder powder of 10 μ m with the silver of the tin behind sintering zinc lead-free solder block.Prepared lead-free solder powder mixes by 99.5:0.5 with the 2008101071494 scaling powder embodiment one that applied for and is full and uniform.
Example 2
Earlier be that 99.99% tin, silver, zinc, gallium, indium, phosphor powder are that 99:0.01:0.69:0.1:0.1:0.1 fully mixes by mass ratio with purity, then under the pressure of 5MPa, make block, described block is put into high temperature difference scanning calorimeter instrument or tubular type sintering furnace, feed argon gas, carrying out sintering, is 10K/min with speed, is warming up to 500K, at this temperature heat preservation sintering 30min, reduce to room temperature with the speed of 25K/min then.By atomization plant, making particle diameter is the lead-free solder powder of 25 μ m with the silver of the tin behind sintering zinc lead-free solder block.Prepared lead-free solder powder mixes by 95:5 with the 2008101071494 scaling powder embodiment two that applied for and is full and uniform.
Example 3
Earlier be that 99.99% tin, silver, zinc, indium, bismuth, rare earth element powder are that 96:2.4:5:4:5:5 fully mixes (wherein rare earth element adds with pre-assigned tin rare earth intermediate alloy form of powder) by mass ratio with purity, then under the pressure of 8MPa, make block, described block is put into high temperature difference scanning calorimeter instrument or tubular type sintering furnace, feed argon gas, carry out sintering, with speed is 20K/min, be warming up to 505K, at this temperature heat preservation sintering 60min, reduce to room temperature with the speed of 40K/min then.By atomization plant, making particle diameter is the lead-free solder powder of 40 μ m with the silver of the tin behind sintering zinc lead-free solder block.Prepared lead-free solder powder mixes by 90:10 with the 2008101071494 scaling powder embodiment three that applied for and is full and uniform.
Example 4
Earlier be that 99.99% tin, silver, zinc, bismuth, phosphorus, gallium, rare earth element powder are that 85:4.5:3.4:1.5:3:2.5:0.1 fully mixes (wherein rare earth element adds with pre-assigned tin rare earth intermediate alloy form of powder) by mass ratio with purity, then under the pressure of 10MPa, make block, described block is put into high temperature difference scanning calorimeter instrument or tubular type sintering furnace, feed argon gas, carry out sintering, with speed is 40K/min, be warming up to 490K, at this temperature heat preservation sintering 120min, reduce to room temperature with the speed of 50K/min then.By atomization plant, making particle diameter is the lead-free solder powder of 50 μ m with the silver of the tin behind sintering zinc lead-free solder block.Prepared lead-free solder powder mixes by 85:15 with the 2008101071494 scaling powder embodiment four that applied for and is full and uniform.
The present invention is not limited to the technology described in the example; its description is illustrative; and it is nonrestrictive; authority of the present invention is limited by claim; based on present technique field personnel according to the present invention can change, technology related to the present invention that method such as reorganization obtains, all in protection scope of the present invention.

Claims (1)

1. the preparation method of a tin-silver-zinc system leadless soldering plaster, the component of soldering paste and mass percent are respectively 99.5-85% tin-silver-zinc series lead-free alloy powder and 0.5-15% scaling powder; The particle diameter of tin-silver-zinc series lead-free alloyed powder is 10-50 μ m; The component of tin-silver-zinc series lead-free alloyed powder and mass percent are:
Tin 99-85
Silver 0.01-4.5
Zinc 0.01-5
Bismuth 0-5
Indium 0-4
Rare earth element 0-5
Gallium 0-2.5
Phosphorus 0-3;
It is characterized in that step is as follows:
1) in proportion raw material is fully mixed, under the pressure of 2-10MPa, make block, described block is put into high temperature difference scanning calorimeter instrument or tubular type sintering furnace, feed argon gas, carrying out sintering, is 5K/min-40K/min with speed, is warming up to 455-535K, at this temperature heat preservation sintering 0-2 hour, reduce to room temperature with the speed of 10K/min-50K/min then;
2) the lead-free solder of tin silver zinc series block behind the sintering is passed through atomization plant, making particle diameter is the lead-free solder powder of 10-50 μ m;
3) prepared lead-free solder powder is mixed with scaling powder also evenly.
CN200810054271XA 2008-08-25 2008-08-25 Method of producing tin-silver-zinc system leadless soldering plaster Expired - Fee Related CN101342641B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN200810054271XA CN101342641B (en) 2008-08-25 2008-08-25 Method of producing tin-silver-zinc system leadless soldering plaster

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN200810054271XA CN101342641B (en) 2008-08-25 2008-08-25 Method of producing tin-silver-zinc system leadless soldering plaster

Publications (2)

Publication Number Publication Date
CN101342641A CN101342641A (en) 2009-01-14
CN101342641B true CN101342641B (en) 2010-12-15

Family

ID=40244822

Family Applications (1)

Application Number Title Priority Date Filing Date
CN200810054271XA Expired - Fee Related CN101342641B (en) 2008-08-25 2008-08-25 Method of producing tin-silver-zinc system leadless soldering plaster

Country Status (1)

Country Link
CN (1) CN101342641B (en)

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102554489A (en) * 2011-12-28 2012-07-11 宁波圣之岛焊锡材料有限公司 Low-rosin halogen and lead-free solder paste and preparation method thereof
CN103212917B (en) * 2013-03-22 2015-11-25 宁波市鄞州品达电器焊料有限公司 A kind of lead-free solder adding mishmetal rhenium-cerium alloy
CN103551756A (en) * 2013-11-12 2014-02-05 宁波市鄞州恒迅电子材料有限公司 Sn-Ag-Cu system lead-free soldering paste
CN104191101B (en) * 2014-08-15 2016-03-23 郑州机械研究所 A kind of clean Sn-Zn solder of few shortcoming containing palladium and preparation method thereof
CN104690442A (en) * 2015-03-17 2015-06-10 湖南新瑞化工有限公司 Low-melting-point lead-free solder alloy and preparation method thereof
CN105269172B (en) * 2015-11-05 2017-07-28 广东轻工职业技术学院 A kind of environment-friendly soldering Alloy solder paste
CN105290641A (en) * 2015-11-30 2016-02-03 苏州龙腾万里化工科技有限公司 Cleaning-free soldering tin bar
CN106181117A (en) * 2016-07-07 2016-12-07 兰州理工大学 A kind of money base solder paste and preparation method thereof
CN110303269A (en) * 2019-07-02 2019-10-08 华侨大学 For the Sn-Cu-Ti solder of low temperature brazing diamond and application

Also Published As

Publication number Publication date
CN101342641A (en) 2009-01-14

Similar Documents

Publication Publication Date Title
CN101342641B (en) Method of producing tin-silver-zinc system leadless soldering plaster
CN102601542B (en) A kind of brazing solder alloy
CN100427261C (en) Aluminum alloy intermediate temperature solder for braze welding
CN103889644A (en) Lead-free and antimony-free tin solder reliable at high temperatures
CN102430874A (en) Titanium-based amorphous brazing alloy foil strip for brazing and preparation method for foil strip
CN102574251A (en) Low-silver-content solder alloy and solder paste composition
CN100558499C (en) A kind of manufacture method of cadmium-free silver brazing alloy
CN103358051A (en) Copper-based solder and preparation method thereof
CN102935558B (en) Preparation method of self-brazing material for welding aluminum-copper member
CN101050127A (en) High temperature solder in use for braze welding ceramics of silicon nitride and composite materials based on ceramics of silicon nitride
CN113714677A (en) Sn-based brazing filler metal capable of realizing high-strength interconnection of CSP (chip scale package) devices
CN103624415A (en) Boron-containing stannum-based lead-free solder and manufacturing method thereof
CN101318269B (en) Tin-Silver-Zinc system lead-free solder with low silver content
CN112518127B (en) Corrosion-resistant low-temperature welding material
CN102626838B (en) Silver-based cadmium-free medium temperature brazing filler metal and preparation method thereof
CN106001980A (en) High-temperature lead-free soldering lug for encapsulating power electronic module and preparation method thereof
CN114000028A (en) NiCoFeCuSiB high-entropy alloy brazing filler metal and preparation method thereof
CN109384474A (en) Ceramic low-temp active metallization lotion, ceramic metallization method and the vacuum electron device according to this method preparation
CN101362265B (en) Tin wire production method of welding material
CN1730696A (en) Tin-zinc-copper-nickel lead-free solder alloy
CN100398251C (en) Cadmium-free silver solder containing gallium and cerium
CN102248323B (en) Silver-based cadmium-free medium-temperature solder and preparation method thereof
CN103056551A (en) Novel tin-and-indium-containing multi-component cadmium-and-silver-free brazing filler metal
CN100463763C (en) Cu-P-Ag solder containing Ga, In and Ce
CN100496861C (en) A tin-zinc selenium alloy welding flux

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20101215

Termination date: 20210825

CF01 Termination of patent right due to non-payment of annual fee