CN114850732A - Preparation method of graphene-reinforced tin-based composite solder - Google Patents
Preparation method of graphene-reinforced tin-based composite solder Download PDFInfo
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- CN114850732A CN114850732A CN202210702831.8A CN202210702831A CN114850732A CN 114850732 A CN114850732 A CN 114850732A CN 202210702831 A CN202210702831 A CN 202210702831A CN 114850732 A CN114850732 A CN 114850732A
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- 239000002131 composite material Substances 0.000 title claims abstract description 65
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910000679 solder Inorganic materials 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 74
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 73
- 238000000034 method Methods 0.000 claims abstract description 36
- 239000011812 mixed powder Substances 0.000 claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000013329 compounding Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 239000011159 matrix material Substances 0.000 claims abstract description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 5
- 230000002776 aggregation Effects 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000005054 agglomeration Methods 0.000 claims description 2
- 238000007781 pre-processing Methods 0.000 claims description 2
- 230000003014 reinforcing effect Effects 0.000 claims description 2
- 238000005219 brazing Methods 0.000 abstract description 26
- 239000002184 metal Substances 0.000 abstract description 21
- 230000000694 effects Effects 0.000 abstract description 13
- 238000000748 compression moulding Methods 0.000 abstract description 8
- 238000003756 stirring Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 5
- 239000006185 dispersion Substances 0.000 abstract description 4
- 238000007906 compression Methods 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000004377 microelectronic Methods 0.000 abstract description 2
- 239000000945 filler Substances 0.000 description 19
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 12
- 238000011068 loading method Methods 0.000 description 12
- 238000000498 ball milling Methods 0.000 description 8
- 238000002844 melting Methods 0.000 description 7
- 230000008018 melting Effects 0.000 description 7
- 238000005303 weighing Methods 0.000 description 5
- 239000011521 glass Substances 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000004100 electronic packaging Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 229910020830 Sn-Bi Inorganic materials 0.000 description 1
- 229910018728 Sn—Bi Inorganic materials 0.000 description 1
- 229910018956 Sn—In Inorganic materials 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Images
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
- B23K35/40—Making wire or rods for soldering or welding
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention belongs to the field of composite materials, and discloses a preparation method of a graphene reinforced tin-based composite solder. The preparation process of the composite solder comprises the steps of putting graphene into a proper amount of alcohol for ultrasonic treatment, mixing and stirring the graphene and tin powder after ultrasonic treatment, putting the obtained mixed powder into a die for compression molding, wherein metal tin generates plastic flow in the compression process, and the graphene is uniformly dispersed in a matrix by virtue of the plastic flow of the metal tin, so that the composite solder with a better composite effect is finally obtained. The composite solder prepared by the process method realizes the uniform dispersion of graphene due to the plastic flow of the material in the pressurizing process. The graphene after compounding has good dispersibility, simple and efficient process, low equipment requirement and low energy consumption, is easy for industrial production, and can be used in the field of microelectronic brazing.
Description
The technical field is as follows:
the invention belongs to the field of composite materials, and relates to a preparation method of a graphene reinforced tin-based brazing filler metal.
Background art:
with the rapid development of the electronic industry, brazing is a main welding method for connecting lead connectors in the electronic industry field. Since the lead-free implementation of the electronic packaging field, the development of the lead-free solder with low cost, good wettability, good conductivity and comprehensive mechanical properties has become the focus of attention of enterprises and various large research units.
The graphene is a novel material, has good electrical conductivity, thermal conductivity and mechanical properties, and can be added into the tin-based solder as a reinforcing phase to improve the performance of the solder. The problem that composite brazing filler metal with more excellent performance than the traditional brazing filler metal is prepared by compounding the traditional brazing filler metal and graphene is now concerned is solved.
At present, lead-free solders for electronic packaging are all tin-based solders, and the mass percentage of tin In common tin-based solders is over 90% except for low-temperature series of Sn-Bi and Sn-In solders. Therefore, the key point of the preparation of the tin-based graphene composite solder lies in the composition of tin and graphene.
The common preparation method of the tin-based graphene composite solder is a powder metallurgy method, and the process flow comprises ultrasonic pretreatment, ball milling and mixing, pressurization and sintering. The preparation process requires that the tin powder has small granularity, the ultrasonic pretreatment and ball milling consumes long time, the technological parameters (ball milling time and ball milling speed) of the ball milling are not well controlled, the preparation process is complex and the like.
The invention content is as follows:
in order to solve the defects and shortcomings of the existing preparation technology of the tin-based solder and graphene composite solder, the graphene reinforced tin-based solder with more excellent performance is obtained. The invention aims to provide a preparation process of a tin-based brazing filler metal and graphene composite brazing filler metal, which is low in cost, high in production efficiency, simple in process and good in composite effect. Microscopic structure analysis of the pressed composite solder shows that the graphene of the composite material prepared by the process is uniformly dispersed, and microscopic structure observation of the melted composite solder sheet shows that the graphene and tin composite effect is good.
In order to solve the technical problem, the invention provides a preparation method of a graphene reinforced tin-based composite solder, which comprises the following steps:
step 1, weighing: weighing a certain amount of graphene and tin powder by using an electronic balance with the precision of 0.0001, wherein the particle size of the tin powder is less than 100 micrometers (the mesh number is more than 150 meshes), the selected graphene is multilayer graphene, and the preferable numerical value range of the graphene in the tin powder is 0.01-0.1%;
step 2, preprocessing graphene: and (2) putting the graphene weighed in the step (1) into alcohol (the volume ratio of the graphene to the alcohol is 1:1-1:2), and carrying out ultrasonic treatment for 2min by adopting ultrasonic equipment. Forming a graphene alcohol suspension after treatment, and uniformly dispersing graphene in alcohol;
step 3, mixing powder: adding the tin powder weighed in the step 1 into the graphene alcohol suspension obtained in the step 2, stirring by using a glass rod for 50-100 times, primarily mixing the tin powder, and volatilizing alcohol to obtain mixed powder;
step 4, compression molding: placing the mixed powder obtained in step 3 into a die, loading to a first pressure at a first rate and pressing the mixed powder at a first hold time. The first pressure is 200-500MPa, the first speed is 0.2-1MPa/s, and the first pressure-retaining time is 0.1-10 min;
and 5, repeating the step four 2-3 times by properly stacking the materials and putting the materials into a mould to improve the compounding effect because the compounding effect of the composite solder obtained in the step 4 is not ideal due to insufficient plastic flow.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention greatly shortens the ultrasonic treatment time in the conventional composite process;
(2) the invention replaces the ball milling process (the ball milling time is generally more than 2 hours) of the conventional composite method with a simple stirring process (the stirring time is about 2 min), and greatly shortens the process time. In addition, the process also avoids the influence of improper selection of ball milling process parameters on the powder mixing effect and the composite effect;
(3) the invention provides a preparation method of a graphene-reinforced tin-based lead-free solder. The method has the advantages of low cost, high production efficiency, good compounding effect, simple steps, low equipment requirement, low energy consumption and easy industrial production, and can be used for the field of microelectronic brazing and compounding other metal materials and graphene.
Drawings
FIG. 1 is an SEM photograph of tin powder used in examples;
FIG. 2 is a low magnification SEM image of multi-layer graphene used in the examples;
FIG. 3 is a photomicrograph of the composite powder of example 1 after press molding;
FIG. 4 is a metallographic structure photograph of a composite solder sheet after compression molding, in example 1, of a tin-graphene composite material with a graphene content of 0.02%;
FIG. 5 is a metallographic micrograph of a solder structure of the composite material after press molding in example 1, which was obtained after remelting the composite material with glycerol as a medium in a tin pot.
Fig. 6 is a macro photograph of the mixed powder of tin and graphene in example 2 after compression molding, wherein the content of graphene is 0.02%;
fig. 7 is a metallographic micrograph of a composite material sheet after press molding in example 2.
Fig. 8 is a metallographic micrograph of a solder structure obtained after the composite material sheet was press-molded in example 2 and was remelted with glycerol as a medium by heating in a tin pot.
Detailed Description
According to the invention, multilayer graphene is used as a reinforcement, tin is used as a substrate, a powder metallurgy technology is used as a composite process, and plastic flow of materials in a pressurizing process is utilized to realize uniform dispersion of graphene and thinning of multilayer graphene so as to achieve a good composite effect. The invention aims to provide a preparation process of a tin-based graphene composite material, which has high production efficiency, simple process and good composite effect. Microscopic structure analysis of the pressed composite material shows that the graphene of the composite material prepared by the process is uniformly dispersed, and microscopic structure observation of the melted composite solder shows that the graphene and tin composite effect is good.
The technical solutions of the present invention are further described in detail below with reference to the accompanying drawings and specific embodiments, which are only illustrative and not limiting of the present invention.
Example 1 a single compression molding method is adopted to prepare a Sn + 0.02% graphene composite solder, and the steps are as follows:
(1) weighing: and weighing 0.8mg of graphene and 4g of tin powder by using an electronic balance. The number of the used graphene layers is 6-9, SEM pictures are shown in figure 1, and the maximum grain size of tin powder is 30 μm, which is shown in figure 2;
(2) graphene pretreatment: and (3) putting the multilayer graphene weighed in the step (1) into a beaker, and adding alcohol, wherein the volume ratio of the graphene to the alcohol is about 1: 2. And (3) putting the beaker filled with the graphene and the alcohol into a small ultrasonic device for ultrasonic treatment for 2min to form graphene alcohol turbid liquid. Stirring and observing by using a glass rod after ultrasonic treatment, and observing until no graphene agglomeration is observed visually;
(3) mixing powder: and (3) pouring the tin powder weighed in the step (1) into the graphene alcohol turbid liquid obtained in the step (2). And stirring the mixed powder by using a glass rod for about 1-2min to preliminarily mix the graphene and the tin powder. And (3) placing the mixed powder in a room temperature environment for about 0.5h to volatilize alcohol in the mixed powder. In order to accelerate the volatilization of alcohol, a glass rod is used for stirring for 5-10 times every 10min during the standing process to promote the volatilization of alcohol. After the preliminary mixing, the mixed powder can also be placed in a vacuum drying oven, the temperature is set to be 50-60 ℃, and the standing time is 10 min. After the alcohol is completely volatilized, mixed powder is obtained.
(4) And (3) pressing and forming: and (3) loading the mixed powder obtained in the step (3) into a die with the inner diameter of 15mm, loading under a press machine, wherein the loading pressure is increased from 0 to 240MPa, the loading rate is 0.6MPa/s, and the pressure maintaining time after loading is 5 min. The composite solder sheet after press forming was taken out of the mold, thereby obtaining a Sn + graphene composite sheet, as shown in fig. 3. And cutting the middle circular area of the obtained brazing filler metal sheet into 9 parts, and carrying out subsequent composite effect detection.
(5) Observing a microstructure after molding: taking the area of the cut composite brazing filler metal sheet obtained in the step 4 to be about 0.25cm 2 And (3) size, inlaying the denture base powder, polishing the inlaid sample, and observing the microstructure by using a metallographic microscope. The microstructure of the composite brazing sheet was obtained as shown in FIG. 4. The graphene is uniformly dispersed in the matrix, and only a small amount of graphene aggregation exists in a partial area.
(6) Observation of microstructure after melting: taking the area of the cut composite brazing filler metal sheet obtained in the step 4 to be about 0.25cm 2 And (5) putting the mixture into a tin melting furnace, and melting by using glycerol as a medium. The microstructure of the molten composite solder ball is shown in fig. 5, and the graphene is well combined with the Sn matrix. Graphene particles are uniformly dispersed in the tin matrix after melting.
Example 2 a Sn + 0.02% graphene composite solder was prepared by the following steps:
(1) step 1, weighing;
(2) step 2, graphene pretreatment;
(3) step 3, mixing the powder;
the above three steps are carried out in the same manner as in example 1.
(4) And (3) pressing and forming: and (3) loading the mixed powder obtained in the step (3) into a die with the inner diameter of 15mm, pressurizing under a press machine, wherein the loading pressure is increased from 0 to 300MPa, the loading rate is 1MPa/s, and the pressure maintaining time after loading is 5 min. And (3) taking out the composite brazing filler metal sheet after the press forming from the die to obtain a composite brazing filler metal sheet of tin and graphene, wherein the appearance of the composite brazing filler metal sheet after the press forming is similar to that of the composite brazing filler metal sheet obtained in the embodiment 1, and is shown in fig. 3.
(5) Secondary compression molding: and (4) taking out the composite brazing filler metal sheet obtained in the step (4), and filling the cut peripheral overflow part into a die again for secondary compression molding. The loading pressure, loading speed and pressure maintaining time of the secondary pressurization process are the same as those of the step 4.
(6) And (3) third-time compression molding: and (3) carrying out the press forming on the composite brazing filler metal sheet obtained in the step (5) again, wherein the specific process and parameters are the same as those in the step (5), and the composite brazing filler metal sheet obtained after the three press forming is shown in FIG. 6. And cutting the middle circular area of the obtained brazing filler metal sheet into 9 parts, and carrying out subsequent composite effect detection.
(7) Observing a microstructure after forming: taking the cut composite brazing filler metal sheet obtained in the step 6, wherein the area of the composite brazing filler metal sheet is about 0.25cm 2 The denture is embedded by denture powder, the embedded sample is polished, and a metallographic microscope is used for observing the microstructure. The microstructure of the composite brazing sheet was obtained as shown in FIG. 7. Compared with the composite brazing sheet (fig. 4) formed in the embodiment 1, the dispersion degree of graphene in a tin matrix is better after multiple compression forming,
(8) observation of microstructure after melting: taking the cut composite brazing sheet (area about 0.25 cm) obtained in step 6 2 ) And putting the solder into a tin pot, melting the solder under the protection of glycerol, wherein the microstructure of the composite solder ball after melting and forming is shown in figure 8. The graphene is dispersed in the tin matrix.
Example 2 demonstrates that by repeated multiple press forming, better composite results can be achieved, while uniform dispersion of GNSs can be achieved by plastic flow of the matrix material during the press forming process.
The technological process designed by the invention is not limited to compounding of the tin-based solder and the graphene/carbon nano tube, and is also suitable for compounding of other metal materials and the graphene/carbon nano tube.
Claims (8)
1. A preparation method of a graphene reinforced tin-based composite solder, wherein the composite solder takes tin as a main matrix and graphene as a reinforcing phase, and the method comprises the following steps:
pre-treating graphene powder to reduce graphene agglomeration and form a graphene alcohol suspension;
mixing the graphene alcohol suspension and tin powder, and obtaining mixed powder after alcohol volatilizes;
and pressing the mixed powder by a semi-open die.
2. The compounding method of claim 1, the pre-processing graphene powder comprising:
mixing the graphene powder and alcohol to form a graphene alcohol suspension;
and carrying out ultrasonic treatment on the graphene alcohol turbid liquid.
3. The compounding method of claim 1, the semi-open pressing the mixed powder comprising:
in a semi-open mold, the mixed powder is loaded to a first pressure at a first rate and pressed for a first hold time.
4. The compounding method of claim 3, the semi-open mold comprising:
a die block for applying a pressure to the mixed powder in a first direction when the mixed powder is pressed;
a top die for applying pressure to the mixed powder in a second direction during the pressing of the mixed powder, wherein the first direction and the second direction are opposite;
the bottom die is not absolutely closed in a third direction perpendicular to the first direction or the second direction, and can flow to the outside of the bottom die when plastic flow is generated after mixed powder is formed in the pressing process.
5. The compounding method of claim 3, the open mold comprising:
a die block for applying a pressure to the mixed powder in a first direction when the mixed powder is pressed;
a top die for applying pressure to the mixed powder in a second direction during the pressing of the mixed powder, wherein the first direction and the second direction are opposite;
wherein the pressing surface of the bottom mold and the pressing surface of the top mold are parallel to each other.
6. The method of claim 3, wherein the first pressure is 200-500 MPa.
7. The compounding method of claim 3, the first rate is 0.2 to 1 MPa/s.
8. The compounding method of claim 3, wherein the first hold pressure time is from 0.1 to 10 min.
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