CN111996403A - Preparation method of lead-free indium tin-based solder alloy and prepared solder alloy - Google Patents
Preparation method of lead-free indium tin-based solder alloy and prepared solder alloy Download PDFInfo
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- CN111996403A CN111996403A CN202010849822.2A CN202010849822A CN111996403A CN 111996403 A CN111996403 A CN 111996403A CN 202010849822 A CN202010849822 A CN 202010849822A CN 111996403 A CN111996403 A CN 111996403A
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- powder
- solder alloy
- lead
- based solder
- indium tin
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0483—Alloys based on the low melting point metals Zn, Pb, Sn, Cd, In or Ga
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C13/00—Alloys based on tin
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
Abstract
The invention discloses a preparation method of a lead-free indium tin-based solder alloy, which comprises the following steps: (1) milling: mixing the following raw materials in percentage by weight: 45-50% of In powder, 45-50% of Sn powder, 3.5-6.1% of Bi powder, 0.02-0.08% of Tb powder, 0.1-0.7% of Zr powder, 0.7% of Fe powder and the balance of Se powder; (2) and (3) sintering: and (2) putting the powder mixed in the step (1) into a graphite mould, then putting the mould into a discharge plasma sintering furnace, vacuumizing, heating to 520 ℃ at a temperature rate of 50 ℃/min under a sintering pressure not higher than 50Mpa, keeping the temperature for 5min, and cooling along with the furnace to obtain the lead-free indium-tin-based solder alloy. The invention also provides the solder alloy prepared by the preparation method. The invention has the beneficial effects that: the lead-free indium tin-based solder alloy prepared by the preparation method has a low melting point and good wetting property.
Description
Technical Field
The invention relates to the technical field of solder alloys, in particular to a preparation method of a lead-free indium tin base solder alloy and the prepared solder alloy.
Background
The soldering technique is widely applied in the whole industrial field, particularly in the field of electronic product manufacturing, various soldering methods are needed, one common method is soldering, the soldering technique is that a solder and a soldering part are heated to the melting temperature of the solder, the solder is melted below the melting point of the soldering part so as to wet a soldering surface, and new alloy is formed between the solder and the soldering part through interatomic diffusion, so that the whole soldering process is completed. The most common of brazing is soldering.
As a soldering material which is very commonly used, lead-tin alloy, in which lead has toxicity and causes great harm to human body and natural environment, has attracted much attention as a lead-free solder research. Several major requirements for lead-free solders are: 1. the lead content is lower than 0.1%; 2. the conductive and heat-conducting performance is good; 3. the mechanical processability is good; 4. low cost, 5. the added components are not excessively complex and difficult to recover. Such as patent application publication No. CN101257995A, which discloses a solder composition comprising tin, indium, silver and bismuth, and comprising about 30% to 85% tin and about 15% to 65% indium, and may further comprise copper. And further limiting the content of silver to be 1% to 10%, the content of bismuth to be 0.25% to 6%, and the content of copper to be 0.25% to 0.75%.
However, in the subsequent studies, many problems were found, and other solders have poor wettability and higher melting points than the conventionally used lead-tin solder, which indicates that the electronic components may be damaged by raising the temperature at the time of soldering.
Disclosure of Invention
The invention aims to solve the technical problems that the solder alloy in the prior art has higher melting point and is easy to damage electronic elements in the welding process, and provides a preparation method of the lead-free indium tin-based solder alloy.
The invention solves the technical problems through the following technical means:
a preparation method of a lead-free indium tin-based solder alloy comprises the following steps:
(1) milling: mixing the following raw materials in percentage by weight: 45-50% of In powder, 45-50% of Sn powder, 3.5-6.1% of Bi powder, 0.02-0.08% of Tb powder, 0.1-0.7% of Zr powder, 0.7% of Fe powder and the balance of Se powder;
(2) and (3) sintering: and (2) putting the powder mixed in the step (1) into a graphite mould, then putting the mould into a discharge plasma sintering furnace, vacuumizing, sintering, and cooling along with the furnace to obtain the lead-free indium-tin-based solder alloy.
Has the advantages that: the lead-free indium tin-based solder alloy prepared by the preparation method has a low melting point and good wetting property.
The preparation method is simple, and has the advantages of low energy consumption, time saving and high efficiency.
Preferably, the following raw materials in percentage by weight are mixed in the step (1): 45% of In powder, 45% of Sn powder, 6.1% of Bi powder, 0.02% of Tb powder, 0.1% of Zr powder, 0.7% of Fe powder and the balance of Se powder.
Has the advantages that: when there is no lead indiumWhen the raw materials of the tin-based solder alloy are the percentage, the solidus temperature of the prepared solder alloy is 220 ℃, the liquidus temperature is 228 ℃, and the shearing strength is 38N/mm2。
Preferably, the following raw materials in percentage by weight are mixed in the step (1): 46% of In powder, 47% of Sn powder, 4.5% of Bi powder, 0.05% of Tb powder, 0.4% of Zr powder, 0.7% of Fe powder and the balance of Se powder.
Has the advantages that: when the raw materials of the lead-free indium tin-based solder alloy are the percentage, the solidus temperature of the prepared solder alloy is 222 ℃, the liquidus temperature is 230 ℃, and the shearing strength is 34N/mm2Under the condition of low temperature of-25 ℃, the elongation of the indium-tin-based solder is 55.374%, the breaking strength is 9.832Mpa, and the tensile strength is 19.323 Mpa.
Preferably, the following raw materials in percentage by weight are mixed in the step (1): 47% of In powder, 48% of Sn powder, 3.5% of Bi powder, 0.05% of Tb powder, 0.4% of Zr powder, 0.7% of Fe powder and the balance of Se powder.
Has the advantages that: when the raw materials of the lead-free indium tin-based solder alloy are the percentage, the solidus temperature of the prepared solder alloy is 225 ℃, the liquidus temperature is 236 ℃, and the shearing strength is 33N/mm2。
Preferably, all the raw materials in the step (1) are mixed and then placed in a vacuum ball milling tank, and are mixed and stirred for 2 hours under the condition of 300 r/min.
Preferably, in the step (2), the sintering pressure is not more than 50Mpa, the heating rate is 50 ℃/min, and the temperature is kept for 5min after being increased to 520 ℃.
The invention aims to solve the technical problems that the solder alloy in the prior art has higher melting point and is easy to damage electronic elements in the welding process, and provides the lead-free indium tin-based solder alloy prepared by the preparation method.
Has the advantages that: compared with the prior art, the preparation method mainly shows the advantages of SPS, such as high temperature rise rate, relatively complicated heating time period, and the like, for example, the patent with the publication number of CN 106862795A.
The components of the solder alloy prepared by the invention are mutually diffused, mutually influenced and interacted, the wettability of the solder alloy is improved, and the solder alloy has a lower melting point.
The invention has the advantages that: the lead-free indium tin-based solder alloy prepared by the preparation method has a low melting point and good wetting property.
The preparation method is simple, and has the advantages of low energy consumption, time saving and high efficiency.
Drawings
FIG. 1 is a scanning electron micrograph of a solder alloy according to example 1 of the present invention;
FIG. 2 is a graph of the true stress-strain curve obtained by stretching the solder alloy at-25 ℃ in example 2 of the present invention;
FIG. 3 is a graph of the true stress-strain curve obtained by stretching the solder alloy at 25 ℃ in example 2 of the present invention;
fig. 4 is a graph of the true stress-strain curve obtained by stretching the solder alloy at 100 c in example 2 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The specific techniques or conditions not specified in the examples can be performed according to the techniques or conditions described in the literature in the field or according to the product specification.
Example 1
Method for preparing lead-free indium tin-based solder alloy by spark plasma sintering
(1) Milling: mixing the following raw materials in percentage by weight: putting 45% of In powder, 45% of Sn powder, 6.1% of Bi powder, 0.02% of Tb powder, 0.1% of Zr powder, 0.7% of Fe powder and the balance of Se powder into a vacuum ball milling tank, and stirring and mixing for 2 hours at 300 r/min;
(2) and (3) sintering: putting the powder mixed in the step (1) into a graphite mould, then putting the mould into a spark plasma sintering furnace, and vacuumizing the furnace chamber to 10 ℃ at room temperature-1Pa, sintering pressure of 50Mpa, heating rate of 45 ℃/min, keeping the temperature for 5min after the temperature is raised to 520 ℃, and cooling along with the furnace to obtain the lead-free indium tin-based solder alloy, wherein figure 1 is a scanning electron microscope image of the solder alloy prepared in the embodiment, and can be seen that the prepared sample is uniform and compact.
Example 2
Method for preparing lead-free indium tin-based solder alloy by spark plasma sintering
(1) Milling: mixing the following raw materials in percentage by weight: putting 46% of In powder, 47% of Sn powder, 4.5% of Bi powder, 0.05% of Tb powder, 0.4% of Zr powder, 0.7% of Fe powder and the balance of Se powder into a vacuum ball milling tank, and stirring and mixing for 2 hours at 300 r/min;
(2) and (3) sintering: putting the powder mixed in the step (1) into a graphite mould, then putting the mould into a spark plasma sintering furnace, and vacuumizing the furnace chamber to 10 ℃ at room temperature-1Pa, sintering pressure of 50Mpa, heating rate of 45 ℃/min, keeping the temperature for 5min after the temperature is raised to 520 ℃, and cooling along with the furnace to obtain the lead-free indium tin-based solder alloy, wherein the graphs in figures 2-4 are real stress strain graphs obtained by stretching the lead-free indium tin-based solder alloy at-25 ℃, 25 ℃ and 100 ℃ respectively. It can be seen that the yield strength at-25 ℃ is 17.57MPa, the yield strength at 25 ℃ is 4.07MPa, and the yield strength at 100 ℃ is 11.93MPa)
Example 3
Method for preparing lead-free indium tin-based solder alloy by spark plasma sintering
(1) Milling: mixing the following raw materials in percentage by weight: putting 47% of In powder, 48% of Sn powder, 3.5% of Bi powder, 0.05% of Tb powder, 0.4% of Zr powder, 0.7% of Fe powder and the balance of Se powder into a vacuum ball milling tank, and stirring and mixing for 2 hours at 300 r/min;
(2) and (3) sintering: mixing in step (1)Placing the powder into a graphite mold, placing the mold in a spark plasma sintering furnace, and vacuumizing the furnace chamber to 10 deg.C at room temperature-1Pa, sintering pressure of 50Mpa, heating rate of 45 ℃/min, keeping the temperature for 5min after the temperature is raised to 520 ℃, and cooling along with the furnace to obtain the lead-free indium-tin-based solder alloy.
Example 4
The properties of the solder alloys obtained in examples 1 to 3 were measured by a conventional method, and the results are shown in Table 1.
TABLE 1 shows properties of the solder alloys of examples 1-3
| Group of | Solidus temperature (. degree.C.) | Liquidus temperature (. degree.C.) | Shear strength (N/mm)2) |
| Example 1 | 220 | 228 | 38 |
| Example 2 | 222 | 230 | 34 |
| Example 3 | 225 | 236 | 33 |
As can be seen from Table 1, the lead-free ITO-based solder alloy prepared by the invention has a lower melting point.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. A preparation method of a lead-free indium tin-based solder alloy is characterized by comprising the following steps: the method comprises the following steps:
(1) milling: mixing the following raw materials in percentage by weight: 45-50% of In powder, 45-50% of Sn powder, 3.5-6.1% of Bi powder, 0.02-0.08% of Tb powder, 0.1-0.7% of Zr powder, 0.7% of Fe powder and the balance of Se powder;
(2) and (3) sintering: and (2) putting the powder mixed in the step (1) into a graphite mould, then putting the mould into a discharge plasma sintering furnace, vacuumizing, sintering, and cooling along with the furnace to obtain the lead-free indium-tin-based solder alloy.
2. The method for preparing a lead-free indium tin-based solder alloy according to claim 1, characterized in that: in the step (1), the following raw materials in percentage by weight are mixed: 45% of In powder, 45% of Sn powder, 6.1% of Bi powder, 0.02% of Tb powder, 0.1% of Zr powder, 0.7% of Fe powder and the balance of Se powder.
3. The method for preparing a lead-free indium tin-based solder alloy according to claim 1, characterized in that: in the step (1), the following raw materials in percentage by weight are mixed: 46% of In powder, 47% of Sn powder, 4.5% of Bi powder, 0.05% of Tb powder, 0.4% of Zr powder, 0.7% of Fe powder and the balance of Se powder.
4. The method for preparing a lead-free indium tin-based solder alloy according to claim 1, characterized in that: in the step (1), the following raw materials in percentage by weight are mixed: 47% of In powder, 48% of Sn powder, 3.5% of Bi powder, 0.05% of Tb powder, 0.4% of Zr powder, 0.7% of Fe powder and the balance of Se powder.
5. The method for preparing a lead-free indium tin-based solder alloy according to claim 1, characterized in that: and (2) mixing all the raw materials in the step (1), putting the mixture into a vacuum ball-milling tank, and mixing and stirring for 2 hours under the condition of 300 r/min.
6. The method for preparing a lead-free indium tin-based solder alloy according to claim 1, characterized in that: in the step (2), the sintering pressure is not more than 50Mpa, the heating rate is 50 ℃/min, and the temperature is kept for 5min after being increased to 520 ℃.
7. The method for preparing a lead-free indium tin-based solder alloy according to claim 1, characterized in that: in the step (2), vacuumizing is carried out to 10-1Pa。
8. A lead-free indium tin-based solder alloy produced by the method for producing a lead-free indium tin-based solder alloy according to any one of claims 1 to 7.
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