CN106001979B - A kind of graphene ZnOw Tin Composite Material and preparation method thereof - Google Patents
A kind of graphene ZnOw Tin Composite Material and preparation method thereof Download PDFInfo
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- CN106001979B CN106001979B CN201610332022.7A CN201610332022A CN106001979B CN 106001979 B CN106001979 B CN 106001979B CN 201610332022 A CN201610332022 A CN 201610332022A CN 106001979 B CN106001979 B CN 106001979B
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- 239000002131 composite material Substances 0.000 title claims abstract description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 38
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 68
- 238000005245 sintering Methods 0.000 claims description 67
- 239000011812 mixed powder Substances 0.000 claims description 35
- 238000000498 ball milling Methods 0.000 claims description 34
- 238000001125 extrusion Methods 0.000 claims description 34
- 239000011521 glass Substances 0.000 claims description 34
- 229910052757 nitrogen Inorganic materials 0.000 claims description 34
- 239000000843 powder Substances 0.000 claims description 34
- 238000002156 mixing Methods 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 21
- 230000008569 process Effects 0.000 claims description 19
- 229910000831 Steel Inorganic materials 0.000 claims description 18
- 239000010959 steel Substances 0.000 claims description 18
- 229910052804 chromium Inorganic materials 0.000 claims description 17
- 239000011651 chromium Substances 0.000 claims description 17
- 239000011261 inert gas Substances 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 17
- 239000000758 substrate Substances 0.000 claims description 17
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims 2
- 238000007731 hot pressing Methods 0.000 claims 2
- 238000007493 shaping process Methods 0.000 claims 1
- 239000011787 zinc oxide Substances 0.000 claims 1
- 229910000679 solder Inorganic materials 0.000 abstract description 24
- 238000011161 development Methods 0.000 abstract description 7
- 230000005802 health problem Effects 0.000 abstract description 2
- 230000010354 integration Effects 0.000 abstract description 2
- LQBJWKCYZGMFEV-UHFFFAOYSA-N lead tin Chemical compound [Sn].[Pb] LQBJWKCYZGMFEV-UHFFFAOYSA-N 0.000 abstract 2
- 238000012545 processing Methods 0.000 description 16
- 239000000203 mixture Substances 0.000 description 8
- 238000004100 electronic packaging Methods 0.000 description 4
- 238000003466 welding Methods 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005476 soldering Methods 0.000 description 2
- 230000005355 Hall effect Effects 0.000 description 1
- PQIJHIWFHSVPMH-UHFFFAOYSA-N [Cu].[Ag].[Sn] Chemical compound [Cu].[Ag].[Sn] PQIJHIWFHSVPMH-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000005219 brazing Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000021615 conjugation Effects 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- -1 graphite Alkene Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- GZCWPZJOEIAXRU-UHFFFAOYSA-N tin zinc Chemical compound [Zn].[Sn] GZCWPZJOEIAXRU-UHFFFAOYSA-N 0.000 description 1
- 229910001174 tin-lead alloy Inorganic materials 0.000 description 1
- 229910000969 tin-silver-copper Inorganic materials 0.000 description 1
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
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a kind of graphene ZnOw Tin Composite Material and preparation method thereof, and its is raw materials used including graphene, ZnOw and tin, and each raw material weight ratio is 1 ~ 4：0.5~1.5：94.5~98.5.Connecting material of the alternative traditional tin-lead solder of graphene ZnOw Tin Composite Material provided by the invention as super large-scale integration, overcome the environment and health problem that lead element is brought in conventional tin-lead solders, and there is mechanical property higher than existing lead-free solder, more reliable, it is a kind of composite for meeting modern electronics industry development trend.
Description
Technical field
The invention belongs to technical field of welding materials, and in particular to a kind of graphene-ZnOw-Tin Composite Material
And preparation method thereof.
Background technology
With the arrival of information age, electronics industry has obtained the fast of the product such as swift and violent development, computer, mobile phone
Speed popularization, makes electronic industry become one of most noticeable and most potential industry.The prosperous also band of electronic industry
The development of electronics manufacturing closely related therewith is moved, as the key links during electronic manufacture, Electronic Packaging
Importance it is also increasingly notable.And soldering becomes the desirable technique for ensuring conductive interconnection between Electronic Packaging component.Solder is made
For a kind of connecting material, it is responsible for during Electronic Packaging and realizes appointing for the functions such as mechanical connection, electrical equipment connection and heat exchange
Business.
Traditional tin-kupper solder alloy is long with its cheap cost, good electric conductivity and excellent soldering processes performance
It has been widely used in since phase in component package and printed circuit board (PCB) assembling, it is extremely important in electronic-packaging processes so as to become
Brazing material.But lead can cause potential hazard to health and natural environment.With the development of electronics industry, super large rule
Solder joint is less and less in vlsi die, and be subject to mechanics, attack a vital point and calorifics load is increasingly heavier, the requirement to solder is more next
It is higher.The creep-resistant property of traditional tin-lead alloy is poor, it is impossible to meets the requirement of modern electronics industry.Therefore, lead-free solder
Development and application, it is responsible for environmental protection and improves the dual role of Quality of electronic products.
There are the series alloys such as tin-copper, tin-silver-copper, tin-zinc than more typical in the lead-free solder of prior art.But
Up to the present, a kind of lead-free solder that can replace traditional tin-kupper solder completely is not still developed.Strengthen solder performance
Possible ways be that the second phase is introduced in general solder, become composite solder.
Graphene, at present by the carbon material of extensive concern, is the most thin two-dimentional material that the current mankind are had found as a kind of
Material, its microstructure is with sp by carbon atom2What hybrid form was formed by connecting.Because graphene has stable conjugation electricity in itself
Subsystem, thus many excellent physical characteristics can be shown.Such as：The intensity of graphene is more than 100 times of steel, is reached
130GPa, it is the material of the maximum intensity obtained at present；The thermal conductivity of graphene is 5 × 103 Wm-1K-1, it is the 3 of diamond
Times；Graphene has known highest carrier mobility, is 1.5 × 104 cm2·V-1S-1；In addition, graphene also has
There are some other special nature, the ferromagnetism and room-temperature quantum Hall effect of such as room temperature.Just because of the property of these protrusions, graphite
Alkene it is novel for development, high performance polymer composite material provide possible approach.
The content of the invention
It is an object of the invention to provide a kind of graphene-ZnOw-Tin Composite Material and preparation method thereof, its
Connecting material of the alternative traditional tin-kupper solder as super large-scale integration, overcomes lead element in traditional tin-kupper solder
The environment and health problem brought, and there is mechanical property higher than existing lead-free solder, more reliable, it is that one kind meets the modern times
The composite of electronics industry development trend.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of graphene-ZnOw-Tin Composite Material, it is raw materials used including graphene, ZnOw and tin,
Its weight ratio is 1 ~ 4：0.5~1.5：94.5~98.5.Wherein, the purity of the tin is 99.9%.
The preparation method of the graphene-ZnOw-Tin Composite Material comprises the following steps：
1）In a nitrogen environment, the glass putty by tin ultrasonic atomizatio into 200 mesh；
2）Gained glass putty, graphene, ZnOw are taken in proportion, is mixed in V-type and 2h is mixed in powder machine, and mixing rotating speed is
10r/min；
3）By step 2）Gained mixed powder, which is put into VC high efficient mixers, mixes 10min, and mixing rotating speed is 100r/min；
4）By step 3）Gained mixed powder is placed in stirring ball mill simultaneously with high-carbon-chromium bearing steel matter abrading-ball, ball material
Weight ratio be 5：1, liquid nitrogen is then charged with to after being totally submerged abrading-ball, low temperature ball milling 2h；
5）Powder after ball milling is taken out, is placed in inert gas shielding case and is cooled to room temperature, is then charged into mould hot
Pressure sintering, the pressure of sintering are 50MPa, 600 DEG C of temperature, sintering time 2h；
6）Base substrate extrusion process after hot pressed sintering is molded, processing temperature is 350 DEG C, extrusion ratio 20：1, institute is made
State graphene-ZnOw-Tin Composite Material.
The remarkable advantage of the present invention is：
（1）Graphene has good mechanics, electrically and thermally property, can turn into the excellent enhancing phase of conventional solder.
Theoretical calculation shows that graphene mechanical property is substantially better than other crystal whisker materials, has very high rigidity；And graphene is low close
Degree and good structural stability, make it have tempting application prospect in composite solder field.The present invention is appropriate by adding
The graphene of ratio, the contact resistance of contact can be reduced, improve the performances such as resistance fusion welding, make its enhancing as lead-free solder
Phase, reach green, the reliable requirement of welding, instead of traditional tin-kupper solder, improve the performance of lead-free solder；
（2）ZnOw stable performance, mechanical performance are superior, can be used as supporting material, increase the machinery of composite solder
Intensity and tensile modulus of elasticity.Importantly, ZnOw is mixed with graphene, both can be made effectively and uniformly to disperse
In tin, solves the problem that graphene can not be effectively and uniformly dispersed in tin.
（3）Graphene, ZnOw and tin are directly mixed powder by the present invention, using the process of powder metallurgy, not
Destroy on the basis of graphene original structure, improve dispersiveness of the graphene in matrix solder, technique is simple, is adapted to big rule
Mould produces.
Embodiment
In order that content of the present invention easily facilitates understanding, with reference to embodiment to of the present invention
Technical scheme is described further, but the present invention is not limited only to this.
Embodiment 1
1）In a nitrogen environment, the glass putty by the tin ultrasonic atomizatio of purity 99.9% into 200 mesh；
2）By weight 95.5：4：0.5 weighs gained glass putty, graphene, ZnOw, mixes in powder machine and mixes in V-type
2h, mixing rotating speed are 10r/min；
3）By step 2）Gained mixed powder, which is put into VC high efficient mixers, mixes 10min, and mixing rotating speed is 100r/min；
4）By step 3）Gained mixed powder is placed in stirring ball mill simultaneously with high-carbon-chromium bearing steel matter abrading-ball, ball material
Weight ratio be 5：1, liquid nitrogen is then charged with to after being totally submerged abrading-ball, low temperature ball milling 2h；
5）Powder after ball milling is taken out, is placed in inert gas shielding case and is cooled to room temperature, is then charged into mould hot
Pressure sintering, the pressure of sintering are 50MPa, 600 DEG C of temperature, sintering time 2h；
6）Base substrate extrusion process after hot pressed sintering is molded, processing temperature is 350 DEG C, extrusion ratio 20：1, institute is made
State graphene-ZnOw-Tin Composite Material.
Embodiment 2
1）In a nitrogen environment, the glass putty by the tin ultrasonic atomizatio of purity 99.9% into 200 mesh；
2）By weight 95：4：1 weighs gained glass putty, graphene, ZnOw, is mixed in V-type in powder machine and mixes 2h, mixed
Conjunction rotating speed is 10r/min；
3）By step 2）Gained mixed powder, which is put into VC high efficient mixers, mixes 10min, and mixing rotating speed is 100r/min；
4）By step 3）Gained mixed powder is placed in stirring ball mill simultaneously with high-carbon-chromium bearing steel matter abrading-ball, ball material
Weight ratio be 5：1, liquid nitrogen is then charged with to after being totally submerged abrading-ball, low temperature ball milling 2h；
5）Powder after ball milling is taken out, is placed in inert gas shielding case and is cooled to room temperature, is then charged into mould hot
Pressure sintering, the pressure of sintering are 50MPa, 600 DEG C of temperature, sintering time 2h；
6）Base substrate extrusion process after hot pressed sintering is molded, processing temperature is 350 DEG C, extrusion ratio 20：1, institute is made
State graphene-ZnOw-Tin Composite Material.
Embodiment 3
1）In a nitrogen environment, the glass putty by the tin ultrasonic atomizatio of purity 99.9% into 200 mesh；
2）By weight 94.5：4：1.5 weigh gained glass putty, graphene, ZnOw, mix in powder machine and mix in V-type
2h, mixing rotating speed are 10r/min；
3）By step 2）Gained mixed powder, which is put into VC high efficient mixers, mixes 10min, and mixing rotating speed is 100r/min；
4）By step 3）Gained mixed powder is placed in stirring ball mill simultaneously with high-carbon-chromium bearing steel matter abrading-ball, ball material
Weight ratio be 5：1, liquid nitrogen is then charged with to after being totally submerged abrading-ball, low temperature ball milling 2h；
5）Powder after ball milling is taken out, is placed in inert gas shielding case and is cooled to room temperature, is then charged into mould hot
Pressure sintering, the pressure of sintering are 50MPa, 600 DEG C of temperature, sintering time 2h；
6）Base substrate extrusion process after hot pressed sintering is molded, processing temperature is 350 DEG C, extrusion ratio 20：1, institute is made
State graphene-ZnOw-Tin Composite Material.
Embodiment 4
1）In a nitrogen environment, the glass putty by the tin ultrasonic atomizatio of purity 99.9% into 200 mesh；
2）By weight 96：3.5：0.5 weighs gained glass putty, graphene, ZnOw, mixes in powder machine and mixes in V-type
2h, mixing rotating speed are 10r/min；
3）By step 2）Gained mixed powder, which is put into VC high efficient mixers, mixes 10min, and mixing rotating speed is 100r/min；
4）By step 3）Gained mixed powder is placed in stirring ball mill simultaneously with high-carbon-chromium bearing steel matter abrading-ball, ball material
Weight ratio be 5：1, liquid nitrogen is then charged with to after being totally submerged abrading-ball, low temperature ball milling 2h；
5）Powder after ball milling is taken out, is placed in inert gas shielding case and is cooled to room temperature, is then charged into mould hot
Pressure sintering, the pressure of sintering are 50MPa, 600 DEG C of temperature, sintering time 2h；
6）Base substrate extrusion process after hot pressed sintering is molded, processing temperature is 350 DEG C, extrusion ratio 20：1, institute is made
State graphene-ZnOw-Tin Composite Material.
Embodiment 5
1）In a nitrogen environment, the glass putty by the tin ultrasonic atomizatio of purity 99.9% into 200 mesh；
2）By weight 95.5：3.5：1 weighs gained glass putty, graphene, ZnOw, mixes in powder machine and mixes in V-type
2h, mixing rotating speed are 10r/min；
3）By step 2）Gained mixed powder, which is put into VC high efficient mixers, mixes 10min, and mixing rotating speed is 100r/min；
4）By step 3）Gained mixed powder is placed in stirring ball mill simultaneously with high-carbon-chromium bearing steel matter abrading-ball, ball material
Weight ratio be 5：1, liquid nitrogen is then charged with to after being totally submerged abrading-ball, low temperature ball milling 2h；
5）Powder after ball milling is taken out, is placed in inert gas shielding case and is cooled to room temperature, is then charged into mould hot
Pressure sintering, the pressure of sintering are 50MPa, 600 DEG C of temperature, sintering time 2h；
6）Base substrate extrusion process after hot pressed sintering is molded, processing temperature is 350 DEG C, extrusion ratio 20：1, institute is made
State graphene-ZnOw-Tin Composite Material.
Embodiment 6
1）In a nitrogen environment, the glass putty by the tin ultrasonic atomizatio of purity 99.9% into 200 mesh；
2）By weight 95：3.5：1.5 weigh gained glass putty, graphene, ZnOw, mix in powder machine and mix in V-type
2h, mixing rotating speed are 10r/min；
3）By step 2）Gained mixed powder, which is put into VC high efficient mixers, mixes 10min, and mixing rotating speed is 100r/min；
4）By step 3）Gained mixed powder is placed in stirring ball mill simultaneously with high-carbon-chromium bearing steel matter abrading-ball, ball material
Weight ratio be 5：1, liquid nitrogen is then charged with to after being totally submerged abrading-ball, low temperature ball milling 2h；
5）Powder after ball milling is taken out, is placed in inert gas shielding case and is cooled to room temperature, is then charged into mould hot
Pressure sintering, the pressure of sintering are 50MPa, 600 DEG C of temperature, sintering time 2h；
6）Base substrate extrusion process after hot pressed sintering is molded, processing temperature is 350 DEG C, extrusion ratio 20：1, institute is made
State graphene-ZnOw-Tin Composite Material.
Embodiment 7
1）In a nitrogen environment, the glass putty by the tin ultrasonic atomizatio of purity 99.9% into 200 mesh；
2）By weight 96.5：3：0.5 weighs gained glass putty, graphene, ZnOw, mixes in powder machine and mixes in V-type
2h, mixing rotating speed are 10r/min；
3）By step 2）Gained mixed powder, which is put into VC high efficient mixers, mixes 10min, and mixing rotating speed is 100r/min；
4）By step 3）Gained mixed powder is placed in stirring ball mill simultaneously with high-carbon-chromium bearing steel matter abrading-ball, ball material
Weight ratio be 5：1, liquid nitrogen is then charged with to after being totally submerged abrading-ball, low temperature ball milling 2h；
5）Powder after ball milling is taken out, is placed in inert gas shielding case and is cooled to room temperature, is then charged into mould hot
Pressure sintering, the pressure of sintering are 50MPa, 600 DEG C of temperature, sintering time 2h；
6）Base substrate extrusion process after hot pressed sintering is molded, processing temperature is 350 DEG C, extrusion ratio 20：1, institute is made
State graphene-ZnOw-Tin Composite Material.
Embodiment 8
1）In a nitrogen environment, the glass putty by the tin ultrasonic atomizatio of purity 99.9% into 200 mesh；
2）By weight 96：3：1 weighs gained glass putty, graphene, ZnOw, is mixed in V-type in powder machine and mixes 2h, mixed
Conjunction rotating speed is 10r/min；
3）By step 2）Gained mixed powder, which is put into VC high efficient mixers, mixes 10min, and mixing rotating speed is 100r/min；
4）By step 3）Gained mixed powder is placed in stirring ball mill simultaneously with high-carbon-chromium bearing steel matter abrading-ball, ball material
Weight ratio be 5：1, liquid nitrogen is then charged with to after being totally submerged abrading-ball, low temperature ball milling 2h；
5）Powder after ball milling is taken out, is placed in inert gas shielding case and is cooled to room temperature, is then charged into mould hot
Pressure sintering, the pressure of sintering are 50MPa, 600 DEG C of temperature, sintering time 2h；
6）Base substrate extrusion process after hot pressed sintering is molded, processing temperature is 350 DEG C, extrusion ratio 20：1, institute is made
State graphene-ZnOw-Tin Composite Material.
Embodiment 9
1）In a nitrogen environment, the glass putty by the tin ultrasonic atomizatio of purity 99.9% into 200 mesh；
2）By weight 95.5：3：1.5 weigh gained glass putty, graphene, ZnOw, mix in powder machine and mix in V-type
2h, mixing rotating speed are 10r/min；
3）By step 2）Gained mixed powder, which is put into VC high efficient mixers, mixes 10min, and mixing rotating speed is 100r/min；
4）By step 3）Gained mixed powder is placed in stirring ball mill simultaneously with high-carbon-chromium bearing steel matter abrading-ball, ball material
Weight ratio be 5：1, liquid nitrogen is then charged with to after being totally submerged abrading-ball, low temperature ball milling 2h；
5）Powder after ball milling is taken out, is placed in inert gas shielding case and is cooled to room temperature, is then charged into mould hot
Pressure sintering, the pressure of sintering are 50MPa, 600 DEG C of temperature, sintering time 2h；
6）Base substrate extrusion process after hot pressed sintering is molded, processing temperature is 350 DEG C, extrusion ratio 20：1, institute is made
State graphene-ZnOw-Tin Composite Material.
Embodiment 10
1）In a nitrogen environment, the glass putty by the tin ultrasonic atomizatio of purity 99.9% into 200 mesh；
2）By weight 97：2.5：0.5 weighs gained glass putty, graphene, ZnOw, mixes in powder machine and mixes in V-type
2h, mixing rotating speed are 10r/min；
3）By step 2）Gained mixed powder, which is put into VC high efficient mixers, mixes 10min, and mixing rotating speed is 100r/min；
4）By step 3）Gained mixed powder is placed in stirring ball mill simultaneously with high-carbon-chromium bearing steel matter abrading-ball, ball material
Weight ratio be 5：1, liquid nitrogen is then charged with to after being totally submerged abrading-ball, low temperature ball milling 2h；
5）Powder after ball milling is taken out, is placed in inert gas shielding case and is cooled to room temperature, is then charged into mould hot
Pressure sintering, the pressure of sintering are 50MPa, 600 DEG C of temperature, sintering time 2h；
6）Base substrate extrusion process after hot pressed sintering is molded, processing temperature is 350 DEG C, extrusion ratio 20：1, institute is made
State graphene-ZnOw-Tin Composite Material.
Embodiment 11
1）In a nitrogen environment, the glass putty by the tin ultrasonic atomizatio of purity 99.9% into 200 mesh；
2）By weight 96.5：2.5：1 weighs gained glass putty, graphene, ZnOw, mixes in powder machine and mixes in V-type
2h, mixing rotating speed are 10r/min；
3）By step 2）Gained mixed powder, which is put into VC high efficient mixers, mixes 10min, and mixing rotating speed is 100r/min；
4）By step 3）Gained mixed powder is placed in stirring ball mill simultaneously with high-carbon-chromium bearing steel matter abrading-ball, ball material
Weight ratio be 5：1, liquid nitrogen is then charged with to after being totally submerged abrading-ball, low temperature ball milling 2h；
5）Powder after ball milling is taken out, is placed in inert gas shielding case and is cooled to room temperature, is then charged into mould hot
Pressure sintering, the pressure of sintering are 50MPa, 600 DEG C of temperature, sintering time 2h；
6）Base substrate extrusion process after hot pressed sintering is molded, processing temperature is 350 DEG C, extrusion ratio 20：1, institute is made
State graphene-ZnOw-Tin Composite Material.
Embodiment 12
1）In a nitrogen environment, the glass putty by the tin ultrasonic atomizatio of purity 99.9% into 200 mesh；
2）By weight 96：2.5：1.5 weigh gained glass putty, graphene, ZnOw, mix in powder machine and mix in V-type
2h, mixing rotating speed are 10r/min；
3）By step 2）Gained mixed powder, which is put into VC high efficient mixers, mixes 10min, and mixing rotating speed is 100r/min；
4）By step 3）Gained mixed powder is placed in stirring ball mill simultaneously with high-carbon-chromium bearing steel matter abrading-ball, ball material
Weight ratio be 5：1, liquid nitrogen is then charged with to after being totally submerged abrading-ball, low temperature ball milling 2h；
5）Powder after ball milling is taken out, is placed in inert gas shielding case and is cooled to room temperature, is then charged into mould hot
Pressure sintering, the pressure of sintering are 50MPa, 600 DEG C of temperature, sintering time 2h；
6）Base substrate extrusion process after hot pressed sintering is molded, processing temperature is 350 DEG C, extrusion ratio 20：1, institute is made
State graphene-ZnOw-Tin Composite Material.
Embodiment 13
1）In a nitrogen environment, the glass putty by the tin ultrasonic atomizatio of purity 99.9% into 200 mesh；
2）By weight 97.5：2：0.5 weighs gained glass putty, graphene, ZnOw, mixes in powder machine and mixes in V-type
2h, mixing rotating speed are 10r/min；
3）By step 2）Gained mixed powder, which is put into VC high efficient mixers, mixes 10min, and mixing rotating speed is 100r/min；
4）By step 3）Gained mixed powder is placed in stirring ball mill simultaneously with high-carbon-chromium bearing steel matter abrading-ball, ball material
Weight ratio be 5：1, liquid nitrogen is then charged with to after being totally submerged abrading-ball, low temperature ball milling 2h；
5）Powder after ball milling is taken out, is placed in inert gas shielding case and is cooled to room temperature, is then charged into mould hot
Pressure sintering, the pressure of sintering are 50MPa, 600 DEG C of temperature, sintering time 2h；
6）Base substrate extrusion process after hot pressed sintering is molded, processing temperature is 350 DEG C, extrusion ratio 20：1, institute is made
State graphene-ZnOw-Tin Composite Material.
Embodiment 14
1）In a nitrogen environment, the glass putty by the tin ultrasonic atomizatio of purity 99.9% into 200 mesh；
2）By weight 97：2：1 weighs gained glass putty, graphene, ZnOw, is mixed in V-type in powder machine and mixes 2h, mixed
Conjunction rotating speed is 10r/min；
3）By step 2）Gained mixed powder, which is put into VC high efficient mixers, mixes 10min, and mixing rotating speed is 100r/min；
4）By step 3）Gained mixed powder is placed in stirring ball mill simultaneously with high-carbon-chromium bearing steel matter abrading-ball, ball material
Weight ratio be 5：1, liquid nitrogen is then charged with to after being totally submerged abrading-ball, low temperature ball milling 2h；
5）Powder after ball milling is taken out, is placed in inert gas shielding case and is cooled to room temperature, is then charged into mould hot
Pressure sintering, the pressure of sintering are 50MPa, 600 DEG C of temperature, sintering time 2h；
6）Base substrate extrusion process after hot pressed sintering is molded, processing temperature is 350 DEG C, extrusion ratio 20：1, institute is made
State graphene-ZnOw-Tin Composite Material.
Embodiment 15
1）In a nitrogen environment, the glass putty by the tin ultrasonic atomizatio of purity 99.9% into 200 mesh；
2）By weight 98.5：1：0.5 weighs gained glass putty, graphene, ZnOw, mixes in powder machine and mixes in V-type
2h, mixing rotating speed are 10r/min；
3）By step 2）Gained mixed powder, which is put into VC high efficient mixers, mixes 10min, and mixing rotating speed is 100r/min；
4）By step 3）Gained mixed powder is placed in stirring ball mill simultaneously with high-carbon-chromium bearing steel matter abrading-ball, ball material
Weight ratio be 5：1, liquid nitrogen is then charged with to after being totally submerged abrading-ball, low temperature ball milling 2h；
5）Powder after ball milling is taken out, is placed in inert gas shielding case and is cooled to room temperature, is then charged into mould hot
Pressure sintering, the pressure of sintering are 50MPa, 600 DEG C of temperature, sintering time 2h；
6）Base substrate extrusion process after hot pressed sintering is molded, processing temperature is 350 DEG C, extrusion ratio 20：1, institute is made
State graphene-ZnOw-Tin Composite Material.
After testing, the present invention gained graphene-ZnOw-Tin Composite Material tensile strength for 53.9MPa with
On, yield strength is more than 50.8MPa, and resistivity is less than 11.2 μ Ω cm-1。
The foregoing is only presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, it should all belong to the covering scope of the present invention.
Claims (7)
- A kind of 1. graphene-ZnOw-Tin Composite Material, it is characterised in that：It is raw materials used including graphene, zinc oxide Whisker and tin, its weight ratio are 1 ~ 4：0.5~1.5：94.5~98.5；The preparation method of the graphene-ZnOw-Tin Composite Material comprises the following steps：1）In a nitrogen environment, the glass putty by tin ultrasonic atomizatio into 200 mesh；2）Gained glass putty, graphene, ZnOw are taken in proportion, are mixed in V-type in powder machine and are mixed 2h；3）By step 2）Gained mixed powder is put into VC high efficient mixers and mixes 10min；4）By step 3）Gained mixed powder is placed in stirring ball mill simultaneously with high-carbon-chromium bearing steel matter abrading-ball, is filled with liquid nitrogen To after being totally submerged abrading-ball, low temperature ball milling 2h；5）Powder after ball milling is taken out, is placed in inert gas shielding case and is cooled to room temperature, hot pressing in mould is then charged into and burns Knot；6）Base substrate extrusion process after hot pressed sintering is molded, the graphene-ZnOw-Tin Composite Material is made.
- 2. graphene-ZnOw-Tin Composite Material according to claim 1, it is characterised in that：The purity of the tin For 99.9%.
- 3. graphene-ZnOw-Tin Composite Material according to claim 1, it is characterised in that：Step 2）Middle mixing Rotating speed is 10r/min.
- 4. graphene-ZnOw-Tin Composite Material according to claim 1, it is characterised in that：Step 3）Middle mixing Rotating speed is 100r/min.
- 5. graphene-ZnOw-Tin Composite Material according to claim 1, it is characterised in that：Step 4）Middle ball material Weight ratio be 5：1.
- 6. graphene-ZnOw-Tin Composite Material according to claim 1, it is characterised in that：Step 5）Middle hot pressing The pressure of sintering is 50MPa, 600 DEG C of temperature, sintering time 2h.
- 7. graphene-ZnOw-Tin Composite Material according to claim 1, it is characterised in that：Step 6）Middle extruding The temperature of machine-shaping is 350 DEG C, extrusion ratio 20：1.
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| CN106493483A (en) * | 2016-11-30 | 2017-03-15 | 安徽华众焊业有限公司 | Low-temperature lead-free tin cream |
| CN106624431A (en) * | 2016-11-30 | 2017-05-10 | 安徽华众焊业有限公司 | Tin-zinc lead-free solder and preparation method thereof |
| CN106624430A (en) * | 2016-11-30 | 2017-05-10 | 安徽华众焊业有限公司 | Tin soldering paste |
| CN107052613A (en) * | 2016-11-30 | 2017-08-18 | 安徽华众焊业有限公司 | Low-melting point leadless solder and preparation method thereof |
| CN107116318A (en) * | 2017-03-28 | 2017-09-01 | 常州大学 | A kind of preparation method of the low silver-colored hypoeutectic solder of high wettability |
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