CN107009044B - A kind of lead-free solder and preparation method thereof - Google Patents
A kind of lead-free solder and preparation method thereof Download PDFInfo
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- CN107009044B CN107009044B CN201710329209.6A CN201710329209A CN107009044B CN 107009044 B CN107009044 B CN 107009044B CN 201710329209 A CN201710329209 A CN 201710329209A CN 107009044 B CN107009044 B CN 107009044B
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- lead
- free solder
- alloy
- mxene
- matrix
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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
- 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
- B23K35/406—Filled tubular wire or rods
Abstract
The invention discloses a kind of lead-free solder and preparation method thereof, which includes lead-free solder matrix and reinforced phase, and reinforced phase accounts for the 0.1%~1% of lead-free solder substrate quality；Wherein the lead-free solder matrix is one of Sn-Ag-Cu alloy, Sn-Sb alloy, Sn-In alloy, Sn-Cu alloy or Sn-Ag alloy, and the reinforced phase is two-dimentional transition metal carbide or carbonitride (MXene) material.The lead-free solder disperses through ultrasonic vibration, is uniformly mixed according to a certain percentage with lead-free solder matrix later, is pressed into green body the preparation method is as follows: MXene is placed in dehydrated alcohol；Finally, being sintered under inert atmosphere protection, a kind of new solder than existing lead-free solder with more Gao Lixue, electricity, thermal property is made, this method is environmentally protective, meets the development trend of modern electronics industry.
Description
Technical field
The present invention relates to a kind of lead-free solders and preparation method thereof, belong to field of material preparation.
Background technique
Conventional tin-lead solders are widely applied in past industrial production because having excellent welding performance.
But lead is a kind of noxious material, causes and seriously threatens to the health of human body.2006, related decree was promulgated in Europe first,
Forbid the use of lead in commercial electronic products, hereafter various countries also launch respectively corresponding policy.Therefore in recent years lead-free solder by
Gradually replace plumber's solder, is applied widely.With the development of science and technology, electronic circuit integrated level increasingly changes, solder joint also phase
Becoming for answering is smaller and smaller, and new challenge is proposed to the performance of its mechanics, electricity, calorifics etc..Traditional lead-free solder
The demand of current industrial, therefore the development and application to New Lead-free Solder are had been unable to meet, becomes very urgent.
There are many lead-free solders on the market at present, and relatively common has the series such as Sn-Cu, Sn-Ag-Cu, Sn-Zn.But
It is until currently, still traditional tin-lead solder can be replaced completely without a solder.In conventional, lead-free solder, the is introduced
Two-phase reinforced phase becomes composite solder, is a kind of possible ways for enhancing solder performance.
Two-dimentional transition metal carbide or carbonitride, i.e. MXene are a kind of New Two Dimensional structural woods of similar graphene
Material has high-specific surface area, high conductivity；Currently, MXene has shown huge dive in fields such as energy storage, absorption, enhancings
Power.The present invention introduces MXene as the second phase reinforced phase, prepares MXene enhancing Pb-free coating in traditional lead-free solder
Material.More traditional lead-free solder, MXene enhance the mechanics of lead-free solder, calorifics etc. performance and are obviously improved.
Summary of the invention
Technical problem: the object of the present invention is to provide a kind of lead-free solder and preparation method thereof, which is introduced
MXene enhances conventional, lead-free solder as the second phase, obtains a kind of having more Gao Lixue, electricity, calorifics than existing lead-free solder
Performance more meets the composite brazing material of modern electronics industry development trend.
Technical solution: the present invention provides a kind of lead-free solder, which includes lead-free solder matrix and reinforced phase, and is increased
The 0.1%~1% of Qiang Xiangzhan lead-free solder substrate quality；Wherein the lead-free solder matrix is Sn-Ag-Cu alloy, Sn-Sb conjunction
One of gold, Sn-In alloy, Sn-Cu alloy or Sn-Ag alloy, the reinforced phase are MXene material.
In the Sn-Ag-Cu alloy, the mass percent of each element is as follows: Sn 85%-98%, Ag 0.5%-
5%, Cu 0.5%-10%；In the Sn-Sb alloy, the mass percent of each element is as follows: Sb 1%-5%, remaining
For Sn；In the Sn-In alloy, the mass percent of each element is as follows: In 0.1%-50%, remaining is Sn；Described
In Sn-Cu alloy, the mass percent of each element is as follows: Cu 0.5%-3.5%, remaining is Sn；The Sn-Ag alloy
In, the mass percent of each element is as follows: Ag 1%-5%, remaining is Sn.
The present invention also provides a kind of preparation methods of lead-free solder, method includes the following steps:
1) after, mixing MXene and dehydrated alcohol, ultrasonic disperse is uniform, and drying obtains microcosmic finely dispersed later
MXene material, obtains reinforced phase；
2), the enhancing in proportion obtaining step 1) is added in lead-free solder matrix and mixes, and obtains a homogeneous mixture；
3), the homogeneous mixture for obtaining step 2) is put into mold, and pressing mold forms to obtain green body；
4), under protective atmosphere, by green body 150 DEG C -200 DEG C sintering 2~5h (its is recommended that interval value) obtain described in
Lead-free solder.
Wherein:
The mass volume ratio of MXene described in step 1) and dehydrated alcohol is 0.75mg/ml~1.75mg/ml, described
Ultrasonic disperse, which refers to, shakes dispersion 30~60min, supersonic frequency 20-40kHz with ultrasonic oscillation instrument.
Enhancing mixing in lead-free solder matrix is added to described in step 2) to refer to reinforced phase and lead-free solder base
Body is put into mixed powder machine, is mixed 6~12h, is uniformly dispersed in MXene in lead-free solder matrix, obtains a homogeneous mixture.
The molding of pressing mold described in step 4) refers to the homogeneous mixture list in mold under the pressure of 500~1000MPa
Axis is compacted into green body cylinders.
The diameter of the green body cylinders is 8~16mm.
The protective atmosphere refers to high-purity argon gas.
The utility model has the advantages that compared with prior art, present invention has the advantage that
1, the present invention with Sn-Ag-Cu, Sn-Ag, Sn-In, Sn-Cu, Sn-Ag-Cu-Bi, Sn-In-Ag powder and
MXene powder is initial feed, and the second phase reinforced phase MXene is introduced into conventional, lead-free solder, is compared compared with conventional, lead-free solder,
MXene enhance lead-free solder mechanics, in terms of performance be obviously improved.
2, the method for powder metallurgy of the invention improves dispersibility of the MXene in lead-free solder matrix.
3,100-200 DEG C is heated under protective atmosphere, rapid synthesis MXene enhances lead-free solder, uses equipment letter
It is single, it is suitble to large-scale production.
Specific embodiment
Embodiment 1:
0.005gMXene is weighed, is placed in 3.75ml dehydrated alcohol, ultrasonic vibration 30min obtains good dispersion after drying
MXene；MXene is added in 5g lead-free solder matrix Sn-5Ag-10Cu (SAC) alloy later, is put into mixed powder machine and mixes
6 hours are closed, MXene is evenly distributed in lead-free solder matrix, obtains a homogeneous mixture；Homogeneous mixture is put into mould
In tool, under the pressure of 500MPa, it is pressed into the green body cylinders that diameter is 16mm；Later by green body high-purity argon gas protection gas
Under atmosphere, 200 DEG C of sintering keep the temperature 2h, obtain MXene enhancing lead-free solder.
Embodiment 2:
0.01gMXene is weighed, is placed in 17.5ml dehydrated alcohol, ultrasonic vibration 60min obtains good dispersion after drying
MXene；MXene is added in 5g lead-free solder matrix Sn-1Ag-1Cu (SAC) alloy later, is put into mixed powder machine and mixes
It 11 hours, is evenly distributed in MXene in lead-free solder matrix, obtains a homogeneous mixture；Homogeneous mixture is put into mould
In tool, under the pressure of 600MPa, it is pressed into the green body cylinders that diameter is 9mm；Later by green body high-purity argon gas protection gas
Under atmosphere, 160 DEG C of sintering keep the temperature 3.5h, obtain MXene enhancing lead-free solder.
Embodiment 3:
0.025gMXene is weighed, is placed in 31.25ml dehydrated alcohol, ultrasonic vibration 30min obtains dispersibility after drying
Good MXene；MXene is added in 5g lead-free solder matrix Sn-5Ag-0.5Cu (SAC) alloy later, is put into mixed powder machine
9 hours are mixed, MXene is evenly distributed in lead-free solder matrix, obtains a homogeneous mixture；Homogeneous mixture is put into
In mold, under the pressure of 800MPa, it is pressed into the green body cylinders that diameter is 10mm；Later by green body high-purity argon gas protection
Under atmosphere, 180 DEG C of sintering keep the temperature 4h, obtain MXene enhancing lead-free solder.
Embodiment 4:
0.05gMXene is weighed, is placed in 37.5ml dehydrated alcohol, ultrasonic vibration 30min obtains good dispersion after drying
MXene；MXene is added in 5g lead-free solder matrix Sn-0.5Ag-10Cu (SAC) alloy later, is put into mixed powder machine
11 hours are mixed, MXene is evenly distributed in lead-free solder matrix, obtains a homogeneous mixture；Homogeneous mixture is put
Enter in mold, under the pressure of 900MPa, is pressed into the green body cylinders that diameter is 14mm；Later by green body high-purity argon gas guarantor
It protects under atmosphere, 190 DEG C of sintering keep the temperature 3h, obtain MXene enhancing lead-free solder.
Embodiment 5:
0.01gMXene is weighed, is placed in 17.5ml dehydrated alcohol, ultrasonic vibration 60min obtains good dispersion after drying
MXene；MXene is added in 5g lead-free solder matrix 49Sn-51In alloy later, it is 12 small to be put into mixing in mixed powder machine
When, it is evenly distributed in MXene in lead-free solder matrix, obtains a homogeneous mixture；Homogeneous mixture is put into mold,
Under the pressure of 700MPa, it is pressed into the green body cylinders that diameter is 8mm；Later by green body under the protective atmosphere of high-purity argon gas, 150
DEG C sintering, keep the temperature 5h, obtain MXene enhancing lead-free solder.
Embodiment 6:
0.01gMXene is weighed, is placed in 17.5ml dehydrated alcohol, ultrasonic vibration 60min obtains good dispersion after drying
MXene；MXene is added in 5g lead-free solder matrix Sn-0.1In alloy later, it is 12 small to be put into mixing in mixed powder machine
When, it is evenly distributed in MXene in lead-free solder matrix, obtains a homogeneous mixture；Homogeneous mixture is put into mold,
Under the pressure of 700MPa, it is pressed into the green body cylinders that diameter is 8mm；Later by green body under the protective atmosphere of high-purity argon gas, 150
DEG C sintering, keep the temperature 5h, obtain MXene enhancing lead-free solder.
Embodiment 7:
0.025gMXene is weighed, is placed in 31.25ml dehydrated alcohol, ultrasonic vibration 30min obtains dispersibility after drying
Good MXene；MXene is added in 5g lead-free solder matrix Sn-1Sb alloy later, it is 8 small to be put into mixing in mixed powder machine
When, it is evenly distributed in MXene in lead-free solder matrix, obtains a homogeneous mixture；Homogeneous mixture is put into mold,
Under the pressure of 1000MPa, it is pressed into the green body cylinders that diameter is 11mm；Later by green body under the protective atmosphere of high-purity argon gas,
170 DEG C of sintering, keep the temperature 3h, obtain MXene enhancing lead-free solder.
Embodiment 8:
0.025gMXene is weighed, is placed in 31.25ml dehydrated alcohol, ultrasonic vibration 30min obtains dispersibility after drying
Good MXene；MXene is added in 5g lead-free solder matrix Sn-5Sb alloy later, it is 8 small to be put into mixing in mixed powder machine
When, it is evenly distributed in MXene in lead-free solder matrix, obtains a homogeneous mixture；Homogeneous mixture is put into mold,
Under the pressure of 1000MPa, it is pressed into the green body cylinders that diameter is 11mm；Later by green body under the protective atmosphere of high-purity argon gas,
170 DEG C of sintering, keep the temperature 3h, obtain MXene enhancing lead-free solder.
Embodiment 9:
0.05gMXene is weighed, is placed in 37.5ml dehydrated alcohol, ultrasonic vibration 30min obtains good dispersion after drying
MXene；MXene is added in 5g lead-free solder matrix Sn-1Ag alloy later, is put into 10 hours of mixing in mixed powder machine,
It is evenly distributed in MXene in lead-free solder matrix, obtains a homogeneous mixture；Homogeneous mixture is put into mold,
Under the pressure of 900MPa, it is pressed into the green body cylinders that diameter is 14mm；Later by green body under the protective atmosphere of high-purity argon gas,
180 DEG C of sintering, keep the temperature 4h, obtain MXene enhancing lead-free solder.
Embodiment 10:
0.05gMXene is weighed, is placed in 37.5ml dehydrated alcohol, ultrasonic vibration 30min obtains good dispersion after drying
MXene；MXene is added in 5g lead-free solder matrix Sn-5Ag alloy later, is put into 10 hours of mixing in mixed powder machine,
It is evenly distributed in MXene in lead-free solder matrix, obtains a homogeneous mixture；Homogeneous mixture is put into mold,
Under the pressure of 900MPa, it is pressed into the green body cylinders that diameter is 14mm；Later by green body under the protective atmosphere of high-purity argon gas,
180 DEG C of sintering, keep the temperature 4h, obtain MXene enhancing lead-free solder.
Embodiment 11:
0.05gMXene is weighed, is placed in 37.5ml dehydrated alcohol, ultrasonic vibration 30min obtains good dispersion after drying
MXene；MXene is added in 5g lead-free solder matrix Sn-0.5Cu alloy later, it is 10 small to be put into mixing in mixed powder machine
When, it is evenly distributed in MXene in lead-free solder matrix, obtains a homogeneous mixture；Homogeneous mixture is put into mold,
Under the pressure of 900MPa, it is pressed into the green body cylinders that diameter is 14mm；Later by green body under the protective atmosphere of high-purity argon gas,
180 DEG C of sintering, keep the temperature 4h, obtain MXene enhancing lead-free solder.
Embodiment 12:
0.05gMXene is weighed, is placed in 37.5ml dehydrated alcohol, ultrasonic vibration 30min obtains good dispersion after drying
MXene；Two-dimentional titanium carbide is added in 5g lead-free solder matrix Sn-3.5Cu alloy later, is put into mixed powder machine and mixes 10
A hour is evenly distributed in MXene in lead-free solder matrix, obtains a homogeneous mixture；Homogeneous mixture is put into mold
In, under the pressure of 900MPa, it is pressed into the green body cylinders that diameter is 14mm；Later by green body high-purity argon gas protective atmosphere
Under, 180 DEG C of sintering keep the temperature 4h, obtain MXene enhancing lead-free solder.
Table 1 is density, hardness, the test result of fusing point of SAC solder and MXene enhancing lead-free solder,；
Table 2 is the thermal diffusion coefficient of SAC solder and MXene enhancing lead-free solder at different temperatures；
By table 1 and table 2, it can be seen that, after MXene is added in SAC lead-free solder, fusing point is reduced, and hardness highest is promoted
7%, thermal diffusion coefficient highest can promote 68%, and mechanics, the thermal property of lead-free solder are significantly improved.
Density, the hardness, fusing point of 1 SAC lead-free solder of table and MXene enhancing lead-free solder
The thermal diffusion coefficient of 2 SAC lead-free solder of table and MXene enhancing lead-free solder at different temperatures
Claims (6)
1. a kind of lead-free solder, it is characterised in that: the solder includes lead-free solder matrix and reinforced phase, and reinforced phase accounts for Pb-free coating
Expect the 0.1%~1% of substrate quality；Wherein the lead-free solder matrix is Sn-Ag-Cu alloy, Sn-Sb alloy, Sn-In conjunction
One of gold, Sn-Cu alloy or Sn-Ag alloy, the reinforced phase are two-dimentional transition metal carbide or carbonitride；
Wherein in the Sn-Ag-Cu alloy, the mass percent of each element is as follows: Sn 85%-98%, Ag 0.5%-
5%, Cu 0.5%-10%；In the Sn-Sb alloy, the mass percent of each element is as follows: Sb 1%-5%, remaining
For Sn；In the Sn-In alloy, the mass percent of each element is as follows: In 0.1%-50%, remaining is Sn；Described
In Sn-Cu alloy, the mass percent of each element is as follows: Cu 0.5%-3.5%, remaining is Sn；The Sn-Ag alloy
In, the mass percent of each element is as follows: Ag 1%-5%, remaining is Sn.
2. a kind of preparation method of lead-free solder as described in claim 1, it is characterised in that: method includes the following steps:
1) after, mixing two-dimentional transition metal carbide or carbonitride and dehydrated alcohol, ultrasonic disperse is uniform, dries later
To microcosmic finely dispersed two-dimentional transition metal carbide or carbon nitride material, reinforced phase is obtained；
2), the enhancing in proportion obtaining step 1) is added in lead-free solder matrix and mixes, and obtains a homogeneous mixture；
3), the homogeneous mixture for obtaining step 2) is put into mold, and pressing mold forms to obtain green body；
4), under protective atmosphere, by green body in 150 DEG C of -200 DEG C of 2~5h of sintering, the lead-free solder is obtained；
Wherein the mass volume ratio of two-dimentional transition metal carbide or carbonitride and dehydrated alcohol described in step 1) is
0.75mg/ml~1.75mg/ml, the ultrasonic disperse, which refers to, shakes 30~60min of dispersion, supersonic frequency with ultrasonic oscillation instrument
Rate is 20-40kHz.
3. a kind of preparation method of lead-free solder as claimed in claim 2, it is characterised in that: by reinforced phase described in step 2)
It is added in lead-free solder matrix mixing and refers to and reinforced phase and lead-free solder matrix are put into mixed powder machine, mix 6~12h, make
Two-dimentional transition metal carbide or carbonitride are uniformly dispersed in lead-free solder matrix, are obtained a homogeneous mixture.
4. a kind of preparation method of lead-free solder as claimed in claim 2, it is characterised in that: the molding of pressing mold described in step 4)
Refer to and the homogeneous mixture single shaft in mold is compacted into green body cylinders under the pressure of 500~1000MPa.
5. a kind of preparation method of lead-free solder as claimed in claim 4, it is characterised in that: the green body cylinders it is straight
Diameter is 8~16mm.
6. a kind of preparation method of lead-free solder as claimed in claim 2, it is characterised in that: the protective atmosphere refers to height
Pure argon.
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| CN107009044B true CN107009044B (en) | 2019-06-18 |
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| WO2020062200A1 (en) * | 2018-09-30 | 2020-04-02 | 苏州优诺电子材料科技有限公司 | High-strength low-temperature lead-free solder and preparation method therefor |
| CN112108789B (en) * | 2020-08-21 | 2021-11-30 | 西南交通大学 | Composite brazing filler metal suitable for high-silicon aluminum alloy brazing connection and application thereof |
| CN112935615A (en) * | 2021-03-26 | 2021-06-11 | 云南锡业集团（控股）有限责任公司研发中心 | Low-temperature soldering paste added with anti-falling particles |
| CN114227059B (en) * | 2022-01-06 | 2023-03-21 | 南京工程学院 | Bi @ MAX core-shell structure, high-reliability lead-free solder and preparation method thereof |
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| CN104842089A (en) * | 2015-06-02 | 2015-08-19 | 哈尔滨工业大学 | Composite high-strength lead-free brazing filler metal for electronic packaging and preparation method thereof |
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| WO2017044262A1 (en) * | 2015-09-08 | 2017-03-16 | Drexel University | Improved routes to mx-ene carbides |
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