CN109262159B - Low-temperature magnetic solder and preparation method thereof - Google Patents

Low-temperature magnetic solder and preparation method thereof Download PDF

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CN109262159B
CN109262159B CN201811030255.7A CN201811030255A CN109262159B CN 109262159 B CN109262159 B CN 109262159B CN 201811030255 A CN201811030255 A CN 201811030255A CN 109262159 B CN109262159 B CN 109262159B
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solder
solution
phase particles
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magnetic phase
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CN109262159A (en
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郭文波
耿家维
张俊
蔡昌礼
邓中山
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Yunnan Zhongxuan Liquid Metal Technology Co ltd
Yunnan Kewei Liquid Metal Valley R&D Co Ltd
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Yunnan Kewei Liquid Metal Valley R&D Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24Selection of soldering or welding materials proper
    • B23K35/26Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/40Making wire or rods for soldering or welding

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  • Mechanical Engineering (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention relates to a low-temperature magnetic solder and a preparation method thereof; heating a solder matrix to be completely melted, cooling and placing the solder matrix in a closed environment, adding a covering solution into the closed environment, immersing the solder matrix in the covering solution, heating the solder matrix to be completely melted, adding magnetic phase particles into an obtained melting system until the magnetic phase particles are completely melted, and cooling to obtain the magnetic phase-free solder; the magnetic phase particles are selected from one or more of iron powder, cobalt powder, nickel powder and iron-cobalt-nickel alloy powder; the dosage of the magnetic phase particles accounts for 0.1-15% of the total weight of the low-temperature magnetic solder. The preparation method of the invention effectively reduces the secondary oxidation of the alloy caused by the stirring of the melting machine; not limited to iron powder, nickel powder and the like which are commonly used at present; most of the magnetic particles can be mixed into the molten alloy and can be effectively and uniformly distributed, so that the utilization rate of the magnetic phase particles is improved; the mixed solution can be reused, so that the cost is effectively reduced; the mixing reaction is rapid, and the production efficiency is greatly improved.

Description

Low-temperature magnetic solder and preparation method thereof
Technical Field
The invention relates to the field of electronic device welding and surface packaging materials, in particular to a low-temperature magnetic solder and a preparation method thereof.
Background
The traditional solder for electronic products is tin-lead solder (melting point about 183 ℃), and has a long history due to good welding performance and service performance. In recent years, electronic manufacturing industry has been rapidly developed, and lead pollution has become serious, and thus, lead pollution has become a public nuisance affecting human health. Therefore, the implementation of the overall lead-free process in the electronic manufacturing industry is a necessary measure for reducing environmental pollution and improving the competitiveness of green manufacturing. In addition, the excessive soldering temperature of the conventional solder may cause damage to the chip and the electronic device.
For example, semiconductor elements having a semiconductor refrigeration element or the like have lower heat resistance than general electronic components having a heat resistance temperature of 130 ℃ or lower, and when soldering such electronic components having low heat resistance (hereinafter referred to as low heat resistance components), the soldering temperature must be lower than 130 ℃. The brazing temperature is preferably + 20-40 ℃ of the liquidus temperature of the used solder, so that the liquidus temperature of the low-temperature solder for brazing the low-heat-resistant parts is required to be about 90 ℃, namely 80-100 ℃, and the key point for solving the problem is to adopt a low-temperature welding material.
Chinese patent CN 201110361214.8 discloses a magnetic particle tin-zinc based composite solder and a preparation method thereof. The magnetic solder is prepared by mixing nickel-plated iron powder particles into tin-zinc-based solder powder, wherein the iron powder particles are plated with a nickel layer with the thickness of 1-3 mu m by adopting a chemical nickel plating mode, and then the tin-zinc-based solder powder and the nickel-plated iron powder are proportionally added into a smelting furnace to be uniformly mixed. The method has complex processing technology, the thickness of the nickel layer can not be ensured to be uniform in the manufacturing process, and the nickel layer is manufactured by using welding powder, so the cost is increased.
Chinese patent CN 201310002553.6 discloses a low-temperature solder-based composite solder for in-situ synthesis of magnetic phase particles and a preparation method thereof. The magnetic solder is prepared by adding manganese and bismuth to form a manganese-bismuth phase as a magnetic material, preparing a tin-manganese intermediate alloy, smelting the tin-manganese intermediate alloy and a tin-bismuth-based solder together, and cooling according to certain conditions during cooling. This method has a complicated production process and the magnetic particles are not necessarily mixed uniformly.
Chinese patent CN 201410406921.8 discloses a method for preparing magnetic solder. The method simply describes the melt mixing of the magnetic particles, flux and solder, and the specific information is not clear.
Disclosure of Invention
At present, no matter the magnetic solder is manufactured by adopting an external compounding, powder remelting or in-situ compounding mode in the research field of the magnetic solder, the problems of more complex manufacturing process, higher cost and limited material quality of used magnetic phase particles exist.
In order to solve the above problems, the present invention aims to provide a method for preparing a low-temperature environment-friendly magnetic solder with simple process, uniform mixing of magnetic particles, and capability of mixing a large number of types of magnetic phase particles.
Heating a solder matrix to be completely melted, cooling and placing the solder matrix into a closed container, adding a covering solution into the closed container, immersing the solder matrix into the covering solution, heating the solder matrix until the solder matrix is completely melted, adding magnetic phase particles into the obtained melting system until no magnetic phase particles exist in the solution, and cooling to obtain the low-temperature magnetic solder;
the magnetic phase particles are selected from one or more of iron powder, cobalt powder, nickel powder, iron-cobalt-nickel alloy powder, iron-silicon-aluminum alloy powder, aluminum-nickel-cobalt alloy powder and molybdenum permalloy powder; cobalt powder is more preferred. The dosage of the magnetic phase particles accounts for 0.1-15% of the total weight of the magnetic phase particles and the solder matrix.
Preferably, the amount of the magnetic phase particles is 0.5-10.0% of the total weight of the low-temperature magnetic solder.
The method provided by the invention adopts a solution endocytosis method, which is similar to the endocytosis effect of outside particles phagocytosed by cells, and when a molten system in a solution environment is acted by an electric field or chemical substances, the molten system can efficiently swallow surrounding particles into a body, thereby effectively reducing the problem of secondary oxidation of the alloy caused by mechanical stirring of the molten system. And can endocytose a plurality of magnetic phase particles, not only being limited to iron powder, nickel powder and the like which are commonly used at present.
According to the preparation method, the particle size of the magnetic phase particles is 0.1-50 microns; preferably 10-30 μm.
In the preparation method of the present invention, preferably, the covering solution is an acidic solution with a pH value of less than 6; it will be understood by those skilled in the art that when the magnetic phase particles are added to the resulting molten system, the molten system is continuously stirred to increase the speed of phagocytosis of the magnetic phase particles until the non-magnetic phase particles are present in the solution.
More preferably, the acidic solution is 0.1 to 2.0mol/L HCl solution and 0.1 to 2.0mol/L H2SO4Solution, 0.1 mol/L-2.0 mol/L of H3PO4One or more mixtures of solutions. Most preferably, the acidic solution is a 1.0mol/L HCl solution, or 0.5mol/L H2SO4Solution and 1.0mol/L of H3PO4The solution was prepared as follows 2: (1-3) mixing the components in proportion.
The acidic solution is used as the covering solution, so that the method has the advantages of fast reaction of phagocytizing magnetic phase particles and easy removal of a molten system and an oxide layer on the surface of the magnetic phase particles. The coating solution is preferably one in which the magnetic phase particles are selected from easily oxidizable magnetic phase particles such as iron powder and cobalt powder.
Or the like, or, alternatively,
preferably, the covering solution is a neutral solution with a pH equal to 7; preferably, when the magnetic phase particles are added into the obtained molten system, 2-30V of direct current voltage is applied to the molten system; the electric field is formed by applying voltage in the solution, because the wettability of the molten system is enhanced by the electrowetting effect, so that the phagocytosis speed of the molten system to the external magnetic phase particles is enhanced.
More preferably, the neutral solution is 0.1-2.0 mol/L NaCl solution;
the neutral solution is used as the covering solution, and the method has the advantages of convenient manufacture, convenient transportation and capability of phagocytosing magnetic phase particles with oxide layers difficult to remove. When the pH is 7, the magnetic phase particles are preferably selected from cobalt powder, nickel powder, iron-cobalt-nickel alloy powder, and the like.
Or the like, or, alternatively,
preferably, the covering solution is an alkaline solution having a pH greater than 7; preferably, when the magnetic phase particles are added to the obtained molten system, aluminum particles are further added in an amount of 0.1 to 5% by weight based on the weight of the solder base. The selection of the aluminum particles can be arbitrarily selected by those skilled in the art within the conventional range.
More preferably, the alkaline solution is a NaOH solution of 0.1mol/L to 2.0 mol/L.
The alkaline solution is used as the covering solution, so that the method has the advantages of easily removing an oxide layer or impurities on the surface of the melting system and enhancing the surface activity of the melting system and the magnetic phase.
When the pH value is more than 7, it is more preferable that the magnetic phase particles are selected from the group consisting of cobalt powder, iron-silicon-aluminum alloy powder, aluminum-nickel-cobalt alloy powder, and molybdenum permalloy powder.
In the preparation method, the solder matrix is selected from one or more of bismuth base, indium base and tin base, and the solder matrix acceptable in the field is selected.
The preparation method comprises the steps of adding low-temperature solder into a smelting furnace, mixing and heating until the low-temperature solder is completely melted, mixing and stirring, keeping the temperature for 30-60min, cooling to room temperature, taking out and placing in a container.
According to the preparation method, the cooled low-temperature magnetic solder is cleaned by clear water.
The preparation method provided by the invention adopts a solution endocytosis method, so that the problem of secondary oxidation of the alloy caused by mechanical stirring of melting is effectively reduced; can endocytose a plurality of magnetic phase particles, not only being limited to iron powder, nickel powder and the like which are commonly used at present; most of the magnetic particles can be mixed into the molten alloy and can be effectively and uniformly dispersed and distributed, so that the utilization rate of the magnetic phase particles is improved; the mixed solution can be reused, so that the cost is effectively reduced; the mixing reaction is rapid, the magnetic phase particles can be mixed within 5 seconds under the stirring condition, and the production efficiency is greatly improved.
The invention also provides the magnetic solder prepared by any one of the technical schemes.
Preferably, the melting point of the magnetic solder provided by the invention is in the range of 60-150 ℃ (preferably the melting point is above 74 ℃), and/or the magnetic induction intensity is above 0.05T (preferably the magnetic induction intensity is above 0.4T).
The low-temperature environment-friendly magnetic solder comprises a low-temperature environment-friendly solder matrix and magnetic phase particles, wherein the low-temperature environment-friendly solder matrix comprises a bismuth base, an indium base, a tin base and the like. The magnetic phase particles are micron-sized particles which are dispersed in the low-temperature environment-friendly solder matrix, wherein the magnetic phase particles account for 0.1-15% of the low-temperature magnetic solder by weight percent, and the balance is the low-temperature environment-friendly solder matrix. The preferable content is 0.1-10.0%.
The magnetic phase particles are magnetic material powder, such as iron powder, cobalt powder, nickel powder, iron-cobalt-nickel alloy powder, iron-silicon-aluminum alloy powder, aluminum-nickel-cobalt alloy powder, molybdenum permalloy powder and the like, and the particle size of the magnetic phase particles is 0.1-50 mu m; in the prior art, the particle size of the magnetic phase particles is required to be between 10 and 35um during preparation, but according to the preparation method provided by the application, the application range of the particle size can be greatly widened, and the limitation of the prior art is removed.
The invention also provides the application of the low-temperature solder in the fields of welding technology and semiconductor welding.
Magnetic solder as a new solder has many possible new uses, such as three-dimensional controlled soldering by an alternating magnetic field, and selectively heating the solder to melt only the solder itself, while the surrounding materials can be at a safe temperature; in addition, remote soldering can be controlled by an applied magnetic field so that it can access hard to reach locations, such as narrow vertical channels, meaning that a magnetic field can be applied to melt the solder and connect the terminals, thereby repairing a broken connection within the device; moreover, the solder can be easily extracted by using the magnetic tweezers, which brings great convenience to the clamping of the solder, especially in the field of welding of tiny devices in the semiconductor industry.
The invention has the beneficial effects that: the introduction method of the magnetic particles is an endocytosis method, and has great advantages compared with the mechanical stirring and mixing of common solders and the low-temperature magnetic solder prepared by adopting the melting and mixing of the intermediate magnetic alloy:
1. the invention adopts a solution endocytosis method, thereby effectively reducing the problem of secondary oxidation of the alloy caused by the stirring of a melting machine;
2. because the solution endocytosis method is adopted, a plurality of magnetic phase particles can be endocytosed, and the method is not limited to iron powder, nickel powder and the like which are commonly used at present;
3. due to the adoption of the solution endocytosis method, most of the magnetic particles can be mixed into the molten alloy and can be effectively and uniformly dispersed and distributed, so that the utilization rate of the magnetic phase particles is improved;
4. the mixed solution can be reused, so that the cost is effectively reduced;
5. the mixing reaction is rapid, the magnetic phase particles can be mixed within 5 seconds under the stirring condition, and the production efficiency is greatly improved.
Drawings
FIG. 1 shows example 1 of the present invention: manufacturing a structural schematic diagram of the solder of the acid covering solution;
FIG. 2 is example 2 of the present invention: manufacturing a structural schematic diagram of neutral covering solution solder;
FIG. 3 shows example 3 of the present invention: manufacturing a structural schematic diagram of the alkaline covering solution solder;
fig. 4 is a scanning electron microscope image of the low-temperature environment-friendly magnetic solder prepared in example 1 of the present invention.
Reference numerals:
closing the crucible 1; closing the crucible cover 2; a covering solution 3; stirring 4; 5, cobalt powder; a low-temperature magnetic solder 6; direct current 7; aluminum particles 8.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
Referring to FIG. 1, the present embodiment uses an acidic coating solution 3, and the selected acidic coating solution 3 is 0.5mol/L H2SO4The solution, the magnetic phase particles selected were 23 μm cobalt powder 5. The solder matrix of the selected low temperature solder is Sn46-In12-Bi 42.
The preparation method comprises the following steps:
weighing components of low-temperature environment-friendly solder with the weight of 99.5% according to a ratio, adding the components into a smelting furnace, mixing and heating the components until the components are completely melted, mixing and stirring the components, preserving heat for 30min, cooling the components to room temperature, taking out the components and putting the components into a sealed crucible 1;
preparing 0.5mol/L H2SO4 A covering solution 3;
thirdly, mixing 0.5mol/L of H2SO4The covering solution 3 is added into the closed crucible 1, and the H of 0.5mol/L2SO4The covering solution 3 is added to the thickness of 10 mm;
fourthly, heating the closed crucible 1 filled with the low-temperature environment-friendly solder matrix and the covering solution 3 until the solder matrix is completely melted;
weighing 0.5 wt% of cobalt powder 5 according to the ratio, placing the cobalt powder 5 into the heating sealed crucible 1, and continuously stirring and mixing until no cobalt powder 5 remains;
sixthly, cooling the mixed low-temperature magnetic solder 6, taking out the low-temperature magnetic solder 6, and washing the low-temperature magnetic solder with clear water to obtain the required low-temperature environment-friendly magnetic solder.
Example 2
Referring to FIG. 2, the present embodiment uses a neutral covering solution 3, the selected neutral covering solution 3 is 0.1mol/L NaCl solution, and the selected magnetic phase particles are 23 μm cobalt powder 5. The solder base of the selected low temperature solder is In-Bi 33.
The preparation method comprises the following steps:
weighing a solder matrix of 98 wt% of low-temperature environment-friendly solder according to a ratio, adding the solder matrix into a smelting furnace, mixing and heating the solder matrix until the solder matrix is completely melted, mixing and stirring the solder matrix, preserving heat for 30min, cooling the solder matrix to room temperature, taking out the solder matrix and putting the solder matrix into a sealed crucible 1;
preparing 0.1mol/L NaCl covering solution 3;
thirdly, 0.1mol/L of NaCl covering solution 3 is added into the closed crucible 1, and the thickness of the added 0.1mol/L of NaCl covering solution 3 is 20 mm;
fourthly, heating the closed crucible 1 containing the low-temperature environment-friendly solder matrix and 0.1mol/L of NaCl covering solution 3 until the solder matrix is completely melted;
fifthly, weighing 1.0 wt% of cobalt powder 5 according to the ratio, placing the cobalt powder 5 into the sealed heating crucible 1, applying 3V direct current 7 to 0.1mol/L of NaCl covering solution 3, continuously stirring and mixing until no cobalt powder 5 remains, and disconnecting the 3V direct current 7;
sixthly, cooling the mixed low-temperature magnetic solder 6, taking out the low-temperature magnetic solder 6, and washing the low-temperature magnetic solder with clear water to obtain the required low-temperature environment-friendly magnetic solder.
Example 3
Referring to FIG. 3, this embodiment uses an alkaline coating solution 3, the selected alkaline coating solution 3 is a 1mol/L NaOH solution, and the selected magnetic phase particles are cobalt powder 5 with a particle size of 23 μm. The solder base of the selected low temperature solder is Sn-In51-Bi 33.
The preparation method comprises the following steps:
weighing a solder matrix of 95 wt% of low-temperature environment-friendly solder according to a ratio, adding the solder matrix into a smelting furnace, mixing and heating the solder matrix until the solder matrix is completely melted, mixing and stirring the solder matrix, preserving heat for 30min, cooling the solder matrix to room temperature, taking out the solder matrix and putting the solder matrix into a sealed crucible 1;
preparing 1mol/L NaOH covering solution 3;
thirdly, adding 1mol/L of NaOH covering solution 3 into the closed crucible 1, wherein the thickness of the 1mol/L of NaOH covering solution 3 is 15 mm;
fourthly, heating the closed crucible 1 containing the low-temperature environment-friendly solder matrix and 1mol/L NaOH covering solution 3 until the solder matrix is completely melted;
weighing 5.0 wt% of cobalt powder 5 according to the ratio, placing the cobalt powder into the heating sealed crucible 1, weighing and adding 0.5 wt% of aluminum particles 8, and continuously stirring and mixing until no cobalt powder 5 remains;
sixthly, cooling the mixed low-temperature magnetic solder 6, taking out the low-temperature magnetic solder 6, and washing the low-temperature magnetic solder with clear water to obtain the required low-temperature environment-friendly magnetic solder.
Example 4
Referring to fig. 1, the present embodiment uses an acidic coating solution 3, where the acidic coating solution 3 is selected according to the following formula 2: 1 proportion of 0.5mol/L H2SO4Solution and 1.0mol/L of H3PO4The solution, the magnetic phase particles selected were 23 μm cobalt powder 5. The solder matrix of the selected low temperature solder is Sn46-In12-Bi 42.
The preparation method comprises the following steps:
weighing components of low-temperature environment-friendly solder with the weight of 99.5% according to a ratio, adding the components into a smelting furnace, mixing and heating the components until the components are completely melted, mixing and stirring the components, preserving heat for 30min, cooling the components to room temperature, taking out the components and putting the components into a sealed crucible 1;
preparing to press 2: 1 proportion of 0.5mol/L H2SO4Solution and 1.0mol/L of H3PO4The solution is used as a covering solution 3;
the ratio of the three to the three is as follows 2: 1 proportion of 0.5mol/L H2SO4Solution and 1.0mol/L of H3PO4The solution covering solution 3 is added into the closed crucible 1, and the H of 0.5mol/L2SO4The covering solution 3 is added to the thickness of 10 mm;
fourthly, heating the closed crucible 1 filled with the low-temperature environment-friendly solder matrix and the covering solution 3 until the solder matrix is completely melted;
weighing 0.5 wt% of cobalt powder 5 according to the ratio, placing the cobalt powder 5 into the heating sealed crucible 1, and continuously stirring and mixing until no cobalt powder 5 remains; sixthly, cooling the mixed low-temperature magnetic solder 6, taking out the low-temperature magnetic solder 6, and washing the low-temperature magnetic solder with clear water to obtain the required low-temperature environment-friendly magnetic solder.
Comparative example 1
This comparative example provides a low-temperature magnetic solder and a method for preparing the same, differing from example 1 only in that 0.5mol/L of H is added2SO4And replacing by 1mol/L nitric acid.
Comparative example 2
This comparative example provides a low-temperature magnetic solder and a method for manufacturing the same, differing from example 2 only in that the 0.1mol/L NaCl was replaced with 0.1mol/L potassium chloride.
Comparative example 3
This comparative example provides a low-temperature magnetic solder and a method for preparing the same, differing from example 3 only in that the 1mol/L NaOH solution is replaced with a 1mol/L KOH solution.
Test example 1
The results of measuring the spreading areas of examples 1, 2, 3 and 4 are shown in Table 1 (the wettability of the solder was measured in an oven, the sample mass was 0.2g, the test temperature was 150 ℃, the holding time was 60s, and the spreading test pieces were prepared in accordance with GB/T11364-2008.)
TABLE 1
Figure BDA0001789546420000091
At the same time, the spreading area of the conventional Sn46-In12-Bi42 solder was measured to be 47.52mm2It can be seen that the spreading area of the invention is greatly improved compared with the traditional Sn46-In12-Bi42 solder.
The average creep rupture life of examples 1-4 under a stress of 18.5MPa applied at 85 ℃ is shown in Table 2. The average creep life of the Sn46-In12-Bi42 solder was also determined to be 260 min.
It can be seen that the creep performance of the present invention is much better than that of the conventional bismuth indium tin solder.
TABLE 2
Figure BDA0001789546420000101
The solder joint shear strength test was performed on a LLOYD universal material tester with a loading rate of 0.01mm/s and a maximum tensile shear load of 2500N, and the average measurement results of examples 1, 2, 3, and 4 are shown in table 3. Meanwhile, the average shear strength of the Sn46-In12-Bi42 solder is measured to be 18 MPa. It can be seen that the shear strength of the present invention is much better than that of the conventional bismuth indium tin solder.
The melting points and the magnetic induction strengths of examples 1 to 4 and comparative examples 1 to 3 were found as shown in Table 4.
TABLE 3
Figure BDA0001789546420000102
TABLE 4
Figure BDA0001789546420000103
Test example 2
With reference to fig. 4, after the low-temperature environment-friendly magnetic solder prepared in example 1 is enlarged by 400 times, it can be seen that 23 μm cobalt powder is distributed in the low-temperature solder matrix more uniformly.
The cobalt powder of the low-temperature environment-friendly magnetic solder prepared in the embodiments 2 to 4 has a comparable distribution effect in the low-temperature solder matrix.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (3)

1. A method for preparing low-temperature magnetic solder is characterized in that a solder matrix is heated to be completely melted, cooled and placed in a closed environment, a covering solution is added into the closed environment, the solder matrix needs to be immersed by the covering solution, after the solder matrix is heated to be completely melted, magnetic phase particles are added into an obtained melting system until the magnetic phase particles are completely melted, and the low-temperature magnetic solder is obtained after cooling; when the magnetic phase particles are added into the obtained molten system, continuously stirring to enhance the speed of the molten system for phagocytosing the magnetic phase particles until no magnetic phase particles exist in the solution;
the using amount of the magnetic phase particles accounts for 0.1-15% of the total weight of the low-temperature magnetic solder; the solder matrix is selected from one or more of bismuth base, indium base and tin base;
the covering solution is an acid solution with the pH value less than 6, and the acid solution is 0.1-2.0 mol/L HCl solution and 0.1-2.0 mol/L H2SO4Solution, 0.1 mol/L-2.0 mol/L H3PO4One or more mixtures of solutions; the magnetic phase particles are selected from one or two of iron powder and cobalt powder;
alternatively, the first and second electrodes may be,
the covering solution is a neutral solution with pH equal to 7; the neutral solution is 0.1-2.0 mol/L NaCl solution; the magnetic phase particles are selected from cobalt powder, nickel powder and iron-cobalt-nickel alloy powder; when the magnetic phase particles are added into the obtained molten system, 2-30V of direct current voltage needs to be applied to the molten system;
alternatively, the first and second electrodes may be,
the covering solution is an alkaline solution with the pH value more than 7; the alkaline solution is 0.1-2.0 mol/L NaOH solution; the magnetic phase particles are selected from cobalt powder, iron-silicon-aluminum alloy powder, aluminum-nickel-cobalt alloy powder and molybdenum permalloy powder; when the magnetic phase particles are added into the obtained melting system, aluminum particles which are 0.1-5% of the weight ratio of the solder matrix need to be added.
2. The method according to claim 1, wherein the magnetic phase particles have a particle size of 0.1 to 50 μm;
the dosage of the magnetic phase particles accounts for 0.5-10.0% of the total weight of the low-temperature magnetic solder.
3. The method according to claim 2, wherein the magnetic phase particles have a particle size of 10 to 30 μm.
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JP4807637B2 (en) * 2008-06-11 2011-11-02 哲男 原田 Method and apparatus for producing liquid flux
CN102513719A (en) * 2011-11-17 2012-06-27 东南大学 Magnetic particle tin-zinc matrix composite solder and preparation method thereof
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