CN106695158A - Soft solder containing graphene and preparation method of soft solder - Google Patents
Soft solder containing graphene and preparation method of soft solder Download PDFInfo
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- CN106695158A CN106695158A CN201611231422.5A CN201611231422A CN106695158A CN 106695158 A CN106695158 A CN 106695158A CN 201611231422 A CN201611231422 A CN 201611231422A CN 106695158 A CN106695158 A CN 106695158A
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- graphene
- soft solder
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Classifications
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- 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
-
- 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
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
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Abstract
The invention discloses a soft solder containing graphene and a preparation method of the soft solder, and belongs to the technical field of soft soldering materials. The soft solder has the characteristics of high strength, high conductivity, high heat conduction and the like, and can be in the shape of a strip, a belt, a wire, powder, a pre-formed soldering lug and the like. The preparation method comprises the following two technological processes: graphene pelleting and soft solder preparation. The graphene is added in the soft solder by a graphene masterbatch mode, the problems that the graphene which is used as an alloy adding ingredient is agglomerated and floats, uniformity is difficult to control and the like are solved effectively, and therefore, the soft solder is suitable for large-scale industrial production.
Description
Technical field
The soft solder and its manufacture method of a kind of graphene-containing, obtain graphene dispersion uniformly female using the method for granulation
Grain, and the Graphene master batch is added into soft solder, lift the mechanical property and electric heating property of solder.Belong to solderable material technology
Field.
Background technology
Graphene (Graphene) is a kind of cellular flat film formed with sp2 hybrid forms by carbon atom, is one
The quasi- two-dimensional material of only one of which atomic layer level thickness is planted, so be called doing monoatomic layer graphite.Its thickness is about
, there are different fluctuatings according to the difference of preparation method in 0.335nm, generally in height about 1nm or so of vertical direction, water
Square to width about 10nm to 25nm, be in addition to diamond all carbon crystals (such as zero dimension fullerene, one-dimensional CNT,
Said three-dimensional body is to graphite) basic structural unit.
Graphene as the most strong a kind of novel nano-material of the most thin, maximum intensity, electrical and thermal conductivity performance that have now been found that,
It is referred to as " dark fund ", its thermal conductivity factor is up to 5300W/m, higher than CNT and diamond, its electron mobility surpasses under normal temperature
Cross 15000cm2/ Vs, and higher than CNT or silicon crystal, and resistivity only about 10-8 Ω/m, it is lower than copper or silver, and by
In its unique two-dimensional nanostructure so that the composite that with the addition of Graphene often has excellent physical property.
However, how to make graphene uniform be dispersed in the metallic matrix being added, and retain its build-in attribute and do not broken
Bad is industry general character difficult point.The feasible method having been reported is using the method for mechanical alloying, i.e. by stone in certain medium
Black alkene is rolled repeatedly, adds the purpose of Graphene in a metal so as to reach.Complex technical process, the production cycle is long.
On the other hand, soft solder plays a part of mechanical connection, signal transmission and the system integration in electronic product, is electricity
One of critical material of sub- industry.As electronic product just develops towards miniaturization, integrated and light-weighted direction, in production
Miniature solder joint is continuously increased, and the reliability of butt welding point proposes requirement higher.
The content of the invention
An object of the present invention is exactly to develop a kind of soft solder, and its good mechanical performance, electric conductivity, thermal conductivity are good,
Extension postwelding service life；It is a further object of the present invention to provide the preparation method of above-mentioned soft solder, particularly a kind of Graphene
The simple prilling process of master batch.
A kind of soft solder of graphene-containing of the present invention, it is characterised in that：By soft solder matrix and graphene dispersion
Mutually it is composited, form includes bar, band, silk, powder and preformed soldering.
Further, the soft solder of graphene-containing of the present invention, it is characterised in that：Soft solder matrix is Sn-Bi systems
Low-temperature lead-free solder.
Further, the soft solder of graphene-containing of the present invention, it is characterised in that：Soft solder matrix is Sn-Ag-Cu
Series lead-free solder.
Further, the soft solder of graphene-containing of the present invention, it is characterised in that：Soft solder matrix is high-temp leadless
Solder.
The soft solder of graphene-containing of the present invention, it is characterised in that：The content of Graphene is 0.001-0.2wt%.
Further, the soft solder of graphene-containing of the present invention, it is characterised in that：The content of Graphene is preferably
0.005-0.01wt%.
A kind of preparation method of the soft solder of graphene-containing of the present invention, it is characterised in that：First Graphene is granulated,
Then added finely dispersed Graphene master batch as raw material in soft solder matrix again.
Further, preparation method of the present invention, it is characterised in that：The prilling process of the Graphene is by soft pricker
Feed powder is stirred in adding finely dispersed Graphene suspension, makes graphene coated in the soft solder powder surface, then leach,
Drying, granulation.
Further, preparation method of the present invention, it is characterised in that：The prilling process of the Graphene is by pure tin
Powder is stirred in adding finely dispersed Graphene suspension, makes graphene coated in glass putty surface, is then leached, dries, is granulated.
Further, preparation method of the present invention, it is characterised in that：The prilling process of the Graphene is by pure tin
After being processed in the CTAB living solutions that powder is first added, stirring in finely dispersed reduced graphene suspension is added, make graphite
Alkene is coated on glass putty surface, then leaches, dries, granulates.
Beneficial effect：The soft solder of graphene-containing of the present invention belongs to composite solder, because Graphene does not react with matrix composition,
The Graphene of even dispersion distribution maintains its intrinsic characteristic in solder, and matrix can be reduced under soft solder fusion temperature
In solid solution oxygen impurities content, it is thus possible to lift its mechanical property, electric conductivity, thermal conductivity kimonos during postwelding use
Labour reliability.
Preparation method of the present invention first prepares finely dispersed Graphene master batch, then again by graphite by the way of granulation
Alkene master batch adds soft solder matrix, efficiently solves simple Graphene and adds difficult, incident reunion, floating, uniformity hardly possible
The problems such as to control.Graphene dispersion is formed finite concentration by the present invention in the solution using most simple directly process for dispersing
Suspension, soft solder powder or pure tin powder are then added thereto stirring, are leached, Graphene is attached to powder surface.This
The method of invention is more easy to be simpler than ball-milling method addition, suitable for scale production.
Below by drawings and Examples, the present invention is described in detail.It should be understood that described embodiment is only
The preferred embodiments of the invention are only related to, in the case of the spirit and scope of the present invention are not departed from, various components and content
Changes and improvements are all possible.
Brief description of the drawings
Fig. 1 is the preparation facilities schematic diagram of the soft solder of graphene-containing of the present invention.
Fig. 2 is the Raman spectrogram of this experiment Graphene.
In Fig. 1：1 is stirring motor；2 is Graphene charge door；3 is suspension closed container；4 is ultrasonic generator.
Specific embodiment
The preparation of SnBi58 low-temperature lead-free solder tin bar of the embodiment 1 containing 0.001wt% Graphenes：
The first step：Graphene is granulated, that is, prepare the master batch of certain Graphene content.
1) 100g Graphenes are weighed, and is conducted into the closed container equipped with 10L alcohol, there is the container ultrasonic disperse to stir
Device is mixed, ultrasonic 1h makes the uniform suspension with 10g/L Graphene concentration；
2) the pure tin powder (T4 powder) of the 20-38um granularities of 1.0kg is weighed, and is slowly added under constant agitation supreme
State the Graphene suspension containing 10g/L concentration；
3) glass putty is leached, it is 0.5L to weigh the loss of Graphene suspension, and the Graphene weight for as being adhered to by glass putty is 5g；
4) dried under argon atmosphere, form the uniform hardened thing of complex powder containing Graphene；
5) above-mentioned hardened thing is directly crushed and is selected, prepare Graphene master batch；
6) weight and its amount of the Graphene for adhering to out according to glass putty, calculate master batch in Graphene content be
0.5wt%.
Second step：The SnBi58 low-temperature lead-free solder tin bars containing 0.001wt% Graphenes of bar shaped are prepared, i.e.,：.Take above-mentioned
The master batch 100g of the graphene-containing that the first step is obtained is added in the SnBi58 low-temperature lead-free solder melts of 50kg, strengthens stirring simultaneously
It is cast into soldering tin bar.
The preforming preparation of SnAg3.0Cu0.5 lead-free solder of the embodiment 2 containing 0.2wt% Graphenes：
The first step：Graphene is granulated, that is, prepare the master batch of certain Graphene content.
1) Graphene of 100g reducing process preparation is weighed, and is conducted into the closed container equipped with 10L distilled water, the container
With ultrasonic disperse agitating device, ultrasonic 2h makes the uniform suspension with 10g/L Graphene concentration；
2) the SAC305 solders powder (the T5 powder of SnAg3.0Cu0.5) of the 15-25um granularities of 1.0kg is weighed, addition concentration is
1.5% CTAB living solutions, are leached after stirring, and much filtrate then is added into the above-mentioned stone containing 10g/L concentration again
Black alkene suspension；
3) SAC305 solder powder is leached, the weight for weighing the loss of Graphene suspension is 0.5L, is as glued by SAC305 powder
Attached Graphene weight is 5g；
4) dried under hydrogen shield atmosphere, form the uniform hardened thing of complex powder containing Graphene；
5) granulated by above-mentioned hardened thing briquetting and by extruder, prepare Graphene master batch；
6) weight and its amount of the Graphene for adhering to out according to SAC305 solder powder, calculate the Graphene content in master batch
It is 0.5wt%.
Second step：Prepare the SnAg3.0Cu0.5 lead-free solders containing 0.2wt% Graphenes preforming, i.e.,：
The Graphene master batch that the above-mentioned first step of 200g is obtained is directly added into the soft solder matrix of 500g, melting, plus
Strong mixing and the ingot and through extruding-rolling-shaping of casting, that is, obtain the SAC305 containing 0.2wt% Graphenes preforming.
The preparation of SnCu0.7 tin silk of the embodiment 3 containing 0.01wt% Graphenes：
By the step first step in embodiment 1, Graphene master batch is prepared, take the SnCu0.7 lead-free solders that 200g adds 10kg
In, melt, stir after ingot casting, and by ingot blank be placed in tin silk extruder, through extruding-drawing procedure, that is, prepare and contain
The SnCu0.7 tin silk of 0.01wt% Graphenes.
The preparation of SnSb10 high-temp leadless welding of the embodiment 4 containing 0.005wt% Graphenes：
By the step first step in embodiment 1, Graphene master batch is prepared, weigh the SnSb10 lead-free solders that 200g adds 20kg
In, melt, stir after ingot casting, and ingot blank be placed in welding forming machine carry out extruder-rolling, that is, prepare and contain
The SnSb10 high-temp leadless weldings of 0.005wt% Graphenes.
The preparation of BiAg2.5 high-temp leadless welding powder of the embodiment 5 containing 0.01wt% Graphenes：
By the step first step in embodiment 1, prepare Graphene master batch, weigh 200g add 10kg BiAg2.5 high temperature without
After in kupper solder, melting, stirring, directly atomization is dusted, that is, prepare the BiAg2.5 high temperature containing 0.01wt% Graphenes without
Lead welding powder.
The preparation of SnPb37 preforming weld-ring of the embodiment 6 containing 0.008wt% Graphenes：
In the first step 2) by the step first step in embodiment 2, Graphene master batch is prepared, what it was different from embodiment 2 is
Use SnPb37 powder and substitute SAC305 powder.
In weighing the SnPb37 solders that 800g Graphenes master batch adds 50kg, melt, stir after cast ingot casting, go forward side by side
Row extrudes-rolls-rush ring, that is, prepare the preforming weld-rings of SnPb37 containing 0.008wt% Graphenes.
The preparation of SnPb92.5Ag2.5 preformed soldering of the embodiment 7 containing 0.006wt% Graphenes：
In the first step 2) by the step first step in embodiment 2, Graphene master batch is prepared, what it was different from embodiment 2 is
Use SnPb92.5Ag2.5 powder and substitute SAC305 powder.
Weigh 600g Graphenes master batch add 50kg SnPb92.5Ag2.5 solders in, melt, stir after cast casting
Ingot, and carry out extruding-rolling-compressing tablet, that is, prepare the SnPb92.5Ag2.5 preformed solderings containing 0.006wt% Graphenes.
The preparation technology of the soft solder sample of the graphene-containing of embodiment of the present invention 8- embodiments 20 is specific as follows：
The first step：Graphene is granulated, that is, prepare the master batch of certain Graphene content.
1) quantitative graphite alkene is weighed, and is conducted into the closed container equipped with quantitative alcohol or distilled water, the container has
Ultrasonic disperse agitating device, ultrasonic 20min-2h makes the uniform suspension with certain Graphene concentration；
2) the corresponding soft solder powder of pure tin powder of quantitative certain particle size is weighed, and is added slowly under constant agitation
The above-mentioned Graphene suspension containing quantitative concentrations；
3) glass putty or corresponding soft solder powder are leached, the weight of Graphene suspension loss is weighed, is as adhered to by glass putty
Graphene suspension weight；
4) dry or dry under argon gas or hydrogen shield atmosphere, form the uniform complex powder containing Graphene hardened
Thing；
5) above-mentioned hardened thing is directly crushed and selects or granulated by extruder, prepare Graphene master batch；
6) amount of the weight and its Graphene for adhering to out according to glass putty or corresponding soft solder powder, calculates the graphite in master batch
Alkene content.
Second step：The soft solder of the graphene-containing of different shape is prepared, i.e.,：
1) the Graphene master batch that the quantitative above-mentioned first step is obtained is directly added into quantitative soft solder matrix, melting,
Reinforcement is stirred and is cast into soldering tin bar, that is, obtain the soft solder welding rod of graphene-containing；
2) the Graphene master batch that the quantitative above-mentioned first step is obtained is directly added into quantitative soft solder matrix, melting,
Reinforcement is stirred and the ingot and through extruding-rolling-shaping of casting, that is, obtain the soft solder containing quantitative graphite alkene preforming；
3) the quantitative graphite alkene master batch for obtaining the above-mentioned first step is directly added into soft solder melt, and reinforcement is stirred and cast
Into rod, and solder paste is equipped with, is squeezed into silk, that is, obtain the soft solder tin silk containing quantitative graphite alkene；
The quantitative graphite alkene master batch that the above-mentioned first step is obtained is directly added into soft solder melt, is stirred and direct mist
Chemical conversion powder, that is, obtain the soft solder solder powder containing quantitative graphite alkene.
The soft solder of graphene-containing of the present invention compares similar soft solder as can be seen from Table 1, and mechanical property is more excellent, conductive,
Thermal conductivity is more preferably.
The soft solder of graphene-containing and contrast solder performance in the embodiment of table 1
The soft solder component of the graphene-containing of 2 exemplary embodiments 8- embodiments of table 20
| Embodiment | Sample classification | Alloy compositions/title |
| 8 | Lead-free solder | 0.2wt%C+SnBi43Sb2 |
| 9 | Lead-free solder | 0.01wt%C+SnBi57Ag1 |
| 10 | Lead-free solder | 0.05wt%C+SnBi57.6Ag0.4 |
| 11 | Lead-free solder | 0.001wt%C+SnAg3.0Cu0.5 |
| 12 | Lead-free solder | 0.01wt%C+SnAg3.5Cu0.7 |
| 13 | Lead-free solder | 0.05wt%C+SnAg3.0Cu0.5 |
| 14 | Lead-free solder | 0.001wt%C+SnCu0.7Ni0.05 |
| 15 | Lead-free solder | 0.05wt%C+SnCu0.7Co0.05 |
| 16 | Lead-free solder | 0.1wt%C+SnSb5 |
| 17 | Lead-free solder | 0.005wt%C+BiAg10 |
| 18 | Kupper solder | 0.01wt%C+SnPb36Ag2 |
| 19 | Kupper solder | 0.005wt%C+SnPb40 |
| 20 | Kupper solder | 0.05wt%C+SnPb90 |
Claims (10)
1. a kind of soft solder of graphene-containing, it is characterised in that：Mutually it is composited with graphene dispersion by soft solder matrix, it is described
The form of soft solder includes bar, band, silk, powder and preformed soldering.
2. the soft solder of graphene-containing according to claim 1, it is characterised in that：The soft solder matrix is Sn-Bi systems
Low-temperature lead-free solder.
3. the soft solder of graphene-containing according to claim 1, it is characterised in that：The soft solder matrix is Sn-Ag-Cu
Series lead-free solder.
4. the soft solder of graphene-containing according to claim 1, it is characterised in that：The soft solder matrix is high-temp leadless
Solder.
5. the soft solder of the graphene-containing according to claim 1-4 any claims, it is characterised in that：The Graphene
Content be 0.001-0.2wt%.
6. the soft solder of graphene-containing according to claim 5, it is characterised in that：The content of the Graphene is 0.005-
0.01wt%.
7. a kind of preparation method of the soft solder of graphene-containing, it is characterised in that：First Graphene is granulated, then will disperse equal again
Even Graphene master batch is added in soft solder matrix as raw material.
8. preparation method according to claim 7, it is characterised in that：The prilling process of the Graphene is by soft solder powder
Stirring in finely dispersed Graphene suspension is added, makes graphene coated in the soft solder powder surface, then leached, dry
Dry, granulation.
9. preparation method according to claim 7, it is characterised in that：The prilling process of the Graphene is to add pure tin powder
Enter stirring in finely dispersed Graphene suspension, make graphene coated in glass putty surface, then leach, dry, granulate.
10. preparation method according to claim 9, it is characterised in that：The pure tin powder is first to add CTAB living solutions
Pure tin powder after middle treatment, the Graphene is Graphene prepared by reducing process.
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| CN201611231422.5A CN106695158A (en) | 2016-12-28 | 2016-12-28 | Soft solder containing graphene and preparation method of soft solder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611231422.5A CN106695158A (en) | 2016-12-28 | 2016-12-28 | Soft solder containing graphene and preparation method of soft solder |
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| Publication Number | Publication Date |
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| CN106695158A true CN106695158A (en) | 2017-05-24 |
Family
ID=58902793
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| CN201611231422.5A Pending CN106695158A (en) | 2016-12-28 | 2016-12-28 | Soft solder containing graphene and preparation method of soft solder |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107350656A (en) * | 2017-07-14 | 2017-11-17 | 苏州海旭新材料科技有限公司 | welding wire coated with graphene and preparation method thereof |
| CN107433402A (en) * | 2017-08-30 | 2017-12-05 | 桂林电子科技大学 | A kind of preparation method and applications of graphene nano silver paste |
| CN107695567A (en) * | 2017-09-08 | 2018-02-16 | 如皋市下原科技创业服务有限公司 | A kind of stamp-mounting-paper diode welds the preparation method of special solder(ing) paste |
| CN108857149A (en) * | 2018-08-29 | 2018-11-23 | 佛山朝鸿新材料科技有限公司 | A kind of preparation method of aluminum welding tin paste |
| CN109014661A (en) * | 2018-09-27 | 2018-12-18 | 华北水利水电大学 | A kind of high nitrogen steel soldering solder additive |
| CN109396720A (en) * | 2018-11-29 | 2019-03-01 | 中国工程物理研究院机械制造工艺研究所 | A kind of multistation vacuum welding is consecutive |
| CN112122825A (en) * | 2020-08-17 | 2020-12-25 | 深圳市兴鸿泰锡业有限公司 | Preparation method of 5G communication tin base band coating halogen-free preformed soldering lug |
| CN112570929A (en) * | 2019-09-29 | 2021-03-30 | 金华三合新材料有限公司 | Aluminothermic welding powder and preparation method thereof |
| CN114850732A (en) * | 2022-06-21 | 2022-08-05 | 齐齐哈尔大学 | Preparation method of graphene-reinforced tin-based composite solder |
| US20230199949A1 (en) * | 2021-12-16 | 2023-06-22 | Dell Products L.P. | Solder composition for use in solder joints of printed circuit boards |
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| CN107350656A (en) * | 2017-07-14 | 2017-11-17 | 苏州海旭新材料科技有限公司 | welding wire coated with graphene and preparation method thereof |
| CN107433402B (en) * | 2017-08-30 | 2019-08-16 | 桂林电子科技大学 | A kind of preparation method and applications of graphene-nano mattisolda |
| CN107433402A (en) * | 2017-08-30 | 2017-12-05 | 桂林电子科技大学 | A kind of preparation method and applications of graphene nano silver paste |
| CN107695567A (en) * | 2017-09-08 | 2018-02-16 | 如皋市下原科技创业服务有限公司 | A kind of stamp-mounting-paper diode welds the preparation method of special solder(ing) paste |
| CN108857149A (en) * | 2018-08-29 | 2018-11-23 | 佛山朝鸿新材料科技有限公司 | A kind of preparation method of aluminum welding tin paste |
| CN109014661A (en) * | 2018-09-27 | 2018-12-18 | 华北水利水电大学 | A kind of high nitrogen steel soldering solder additive |
| CN109396720A (en) * | 2018-11-29 | 2019-03-01 | 中国工程物理研究院机械制造工艺研究所 | A kind of multistation vacuum welding is consecutive |
| CN112570929A (en) * | 2019-09-29 | 2021-03-30 | 金华三合新材料有限公司 | Aluminothermic welding powder and preparation method thereof |
| CN112122825A (en) * | 2020-08-17 | 2020-12-25 | 深圳市兴鸿泰锡业有限公司 | Preparation method of 5G communication tin base band coating halogen-free preformed soldering lug |
| CN112122825B (en) * | 2020-08-17 | 2022-03-18 | 深圳市兴鸿泰锡业有限公司 | Preparation method of 5G communication tin base band coating halogen-free preformed soldering lug |
| US20230199949A1 (en) * | 2021-12-16 | 2023-06-22 | Dell Products L.P. | Solder composition for use in solder joints of printed circuit boards |
| US11832386B2 (en) * | 2021-12-16 | 2023-11-28 | Dell Products L.P. | Solder composition for use in solder joints of printed circuit boards |
| CN114850732A (en) * | 2022-06-21 | 2022-08-05 | 齐齐哈尔大学 | Preparation method of graphene-reinforced tin-based composite solder |
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Application publication date: 20170524 |