CN111872600B - MOFs carbonized product, preparation method and application in lead-free solder modification - Google Patents
MOFs carbonized product, preparation method and application in lead-free solder modification Download PDFInfo
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- CN111872600B CN111872600B CN202010649384.5A CN202010649384A CN111872600B CN 111872600 B CN111872600 B CN 111872600B CN 202010649384 A CN202010649384 A CN 202010649384A CN 111872600 B CN111872600 B CN 111872600B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
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Abstract
The invention discloses an MOFs carbonized product, a preparation method and application in lead-free solder modification, wherein the preparation method of the MOFs carbonized product comprises the following steps: step 1, mixing nitrate serving as a metal particle source, an organic ligand and liquid serving as reaction conditions, and carrying out ultrasonic stirring reaction on the mixed solution; putting the mixed solution into a reaction kettle, putting the reaction kettle into a drying oven for reaction, centrifuging and filtering the obtained precipitate by using absolute ethyl alcohol, and finally drying to obtain dodecahedron, lamellar or flaky MOFs powder; and 2, putting the MOFs powder obtained in the step 1 into a tubular furnace for carbonization to obtain a carbonized product of the MOFs. The MOFs carbonized product can be applied to lead-free solder modification. According to the invention, the carbon material organic ligand is used for coating the nano Ni particles or Co particles to obtain the modifier with a special appearance, and the modifier is greatly reduced or avoided from agglomeration after being fused with the lead-free solder, so that the modification effect is fully exerted.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method and application of a lead-free solder modifier based on MOFs carbonized products.
Background
In the production process of electronic products, the realization of the connection between an electronic component and a substrate is an indispensable link, and the microelectronic welding technology is a core component of the electronic packaging and assembling technology. Lead-containing solder and lead alloy coating have been widely used as basic materials for interconnection of electronic products for a long time, but the toxicity generated by lead and lead compounds brings serious harm to the environment and human bodies. Therefore, the development and application of the lead-free solder become hot topics in the industry, and have great application prospects in electronic packaging.
During the brazing process, intermetallic compounds are generated between the substrate and the brazing filler metal, wherein Sn — Cu compounds are mainly used on the conventional copper substrate. However, since Cu atoms are rapidly dissolved in the liquid solder and have high solubility, Sn — Cu compounds are rapidly formed and grown, and their growth morphology greatly affects the service life of the joint due to their brittleness. With the rapid development of the lead-free solder, various means are available for modifying the lead-free solder to regulate and control the interface behavior, such as adding nano metal particles of Co, Ni and the like or adding carbon materials of graphene, carbon nano tubes and the like into the lead-free solder. Although the added phase can improve the comprehensive performance of the composite solder to a certain extent, the addition of the nano particles is an unstable process, the nano particles are easy to float on the surface of the solder and agglomerate, so that the defects of the composite solder are increased, and the modification effect is limited and even can influence the performance of the matrix solder.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a preparation method of a modifier based on MOFs carbonized products and application of the modifier in lead-free solder. In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of MOFs carbonized products comprises the following steps:
step 1, mixing nitrate serving as a metal particle source, an organic ligand and liquid serving as reaction conditions, and ultrasonically stirring the mixed solution; putting the mixed solution into a reaction kettle, putting the reaction kettle into a drying oven for reaction, centrifuging and filtering the obtained precipitate by using absolute ethyl alcohol, and finally drying to obtain dodecahedron, lamellar or flaky MOFs powder;
and 2, putting the MOFs powder obtained in the step 1 into a tubular furnace for carbonization to obtain a carbonized product of the MOFs.
In the step 1, the nitrate is cobalt nitrate or nickel nitrate, the organic ligand is one or more of 2-methylimidazole and terephthalic acid, and the alkaline liquid is one or more of triethylamine, tripropylamine and diethylamine; the molar ratio of the nitrate to the organic ligand to the alkaline liquid is 1: (4-16): (4-16); the ultrasonic stirring reaction is carried out at room temperature for 10-20 min.
In the step 1, the temperature of the oven is 100-.
In the step 1, the drying temperature is 70-100 ℃ and the time is 12-24 h.
In the step 2, the carbonization process is as follows: heating the tube furnace at 3-6 deg.C/min under the protection of argon atmosphere, and maintaining at 600-1000 deg.C for 2-8 h.
A MOFs carbonized product prepared by the method.
The MOFs carbonized product can be applied to lead-free solder modification. The carbonization product of the MOFs accounts for 0.01-1.0% of the total mass of the lead-free solder, and the lead-free solder is one of Sn-Cu, Sn-Ag and Sn-Zn solder.
The modification method is any one of the following two methods:
the first modification method comprises the following steps: weighing MOFs carbonized products and lead-free solder raw material particles, cleaning the MOFs carbonized products and the lead-free solder raw material particles by using hydrochloric acid alcohol, drying the MOFs carbonized products and the lead-free solder raw material particles by using a vacuum drying oven, smelting the MOFs carbonized products and the lead-free solder raw material particles in a vacuum furnace under the protection of high-purity argon atmosphere, wherein the heating rate is 8 ℃/min, the temperature is kept at 210-400 ℃ for 3-5h, and the whole smelting process is.
And a second modification method comprises the following steps: weighing carbonized products of MOFs and lead-free solder raw material powder, pouring the carbonized products and the lead-free solder raw material powder into ethanol, carrying out ultrasonic treatment for 5-10min to obtain a mixed solution, pouring the mixed solution into a ball milling tank for wet milling, wherein the ball-material ratio is about 6:1, the ball milling rotation speed is 200r/min, rotating forwards for 5min, stopping for 5min, rotating backwards for 5min, and carrying out ball milling for 240 min; and (3) placing the obtained ball-milling slurry in a drying box at 40-60 ℃ for heat preservation for 2-4h for drying, pressing the dried mixed powder into a block by using a grinding tool, placing the block into a porcelain boat, sintering in a tubular furnace under the protection of high-purity argon atmosphere at the heating rate of 8 ℃/min, preserving heat at 180 ℃ and 200 ℃ for 2-3h, and then overturning the composite solder block for sintering again.
Has the advantages that: according to the invention, the carbon material organic ligand is used for coating the nano Ni particles or Co particles to obtain the novel modifier with a special appearance, and the novel modifier can greatly reduce or avoid the agglomeration phenomenon after being fused with the lead-free solder, so that the modification effect is fully exerted.
Detailed Description
The invention relates to a preparation method of a lead-free solder modifier based on MOFs carbonized products, which comprises the following steps:
(1) preparing MOFs;
nitrate serving as a metal particle source, an organic ligand and liquid serving as reaction conditions are mixed according to a molar ratio of 1: (4-16): (4-16) mixing, and carrying out ultrasonic stirring reaction on the mixed solution at room temperature for 10-20 min; and then putting the solution into a reaction kettle, putting the reaction kettle into an oven with the temperature of 100-150 ℃ for reaction for 12-24h, centrifuging and filtering the obtained precipitate by using absolute ethyl alcohol, and finally drying the precipitate for 12-24h at the temperature of 70-100 ℃ to obtain the dodecahedral, lamellar or flaky MOFs powder with the particle size of 100nm-1 mu m.
(2) Carbonizing treatment:
and (2) placing the MOFs powder obtained in the step (1) in a tubular furnace, setting a temperature-raising curve, enabling the tubular furnace to carry out a temperature-raising process at the speed of 3-6 ℃/min under the protection condition of argon atmosphere, and preserving heat for 2-8h at the temperature of 600-1000 ℃ to obtain the MOFs carbonized product.
(3) Modification of the lead-free solder:
modifying the lead-free solder by using the MOFs carbonized product obtained in the step (2) to obtain the lead-free solder modified based on the MOFs carbonized product; wherein the MOFs carbonized product accounts for 0.01-1.0% of the total mass of the lead-free solder, and the lead-free solder is one of Sn-Cu, Sn-Ag and Sn-Zn solder.
The modification step is any one of the following two methods:
the first modification method comprises the following steps: according to the mass ratio, the MOFs carbonized product and the lead-free solder raw material particles are weighed by a high-precision balance for later use, hydrochloric acid spirit with the concentration of 4 vol.% is used for cleaning oxide films possibly remained on the surfaces of the metal particles, then a vacuum drying oven is used for drying, then smelting is carried out in a vacuum furnace under the protection of high-purity argon (Ar is more than or equal to 99.999%) atmosphere, the heating rate is 8 ℃/min, the heat is preserved for 3-5h at the temperature of 400 ℃, and the whole smelting process is repeated for 3-5 times.
And a second modification method comprises the following steps: according to the mass ratio, the carbonized MOFs and the lead-free solder raw material powder are weighed by a high-precision balance, and poured into ethanol for ultrasonic treatment for 5-10min to obtain a mixed solution. Pouring the mixture into a ball milling tank for wet milling, wherein the ball-material ratio is about 6:1, the ball milling rotation speed is 200r/min, rotating forwards for 5min, stopping for 5min, rotating backwards for 5min, and ball milling for 240 min. And (2) placing the obtained ball-milling slurry in a drying box at 40-60 ℃ for heat preservation for 2-4h for drying, pressing the dried mixed powder into blocks by using a grinding tool with the inner diameter of 16mm, placing the obtained blocks into a porcelain boat, sintering in a tubular furnace under the protection of high-purity argon (Ar is more than or equal to 99.999%) at the heating rate of 8 ℃/min at the temperature of 180 ℃ plus 200 ℃ for 2-3h, and turning over the composite brazing filler metal blocks for sintering again in order to ensure uniform sintering.
The present invention will be further described with reference to the following examples.
Example 1
(1) Synthesis of ZIF-67
Weighing 0.5g Co (NO)3)2·6H2Dissolving O in 50mL of deionized water to form solution A; weighing 2-methylimidazole and Triethylamine (TEA) and dissolving in 50mL of deionized water to form a solution B; respectively ultrasonically stirring A, B solutions for 10min, and mixing; wherein, Co (NO)3)2·6H2The molar ratio of O, 2-methylimidazole to Triethylamine (TEA) was 1: 16: 16; and (3) carrying out ultrasonic stirring reaction on the mixed solution at room temperature for 10min, then putting the solution into a reaction kettle, putting the reaction kettle into an oven with the temperature of 120 ℃ for reaction for 24h, centrifuging and filtering the obtained precipitate by using absolute ethyl alcohol, and finally drying the precipitate in the oven with the temperature of 70 ℃ for 12h to obtain ZIF-67 powder.
(2) Carbonization treatment
And (2) placing the ZIF-67 powder obtained in the step (1) into a tube furnace, heating the tube furnace at the speed of 5 ℃/min under the protection of argon atmosphere, and keeping the temperature at 800 ℃ for 6 h.
(3) Modification of lead-free solder
Respectively weighing and placing Sn, Cu particles and ZIF-67 carbonized powder with different mass fractions by using a high-precision balance according to the proportion of Sn-0.7Cu-0.15 carbonized ZIF-67 for later use, cleaning the Sn and Cu particles by using hydrochloric acid alcohol with the concentration of 4 vol.% before smelting to form an oxide film possibly remained on the surfaces of the metal particles, drying by using a vacuum drying box, then smelting in a vacuum furnace under the protection of high-purity argon (Ar is more than or equal to 99.999%) atmosphere, wherein the heating rate is 8 ℃/min, the heat preservation is carried out for 3h at 230 ℃, and the whole smelting process is repeated for 4 times in order to obtain the brazing filler alloy with uniform components.
Example 2
(1) Synthesis of ZIF-67
Weighing 0.5g Co (NO)3)2·6H2Dissolving O in 50mL of deionized water to form solution A; weighing 2-methylimidazole and Triethylamine (TEA) and dissolving in 50mL of deionized water to form a solution B; respectively ultrasonically stirring A, B solutions for 10min, and mixing; wherein, Co (NO)3)2·6H2The molar ratio of O, 2-methylimidazole to Triethylamine (TEA) was 1: 16: 16; and ultrasonically stirring the mixed solution at room temperature for reaction for 10min, washing with deionized water for 2-3 times, putting the solution into a reaction kettle, placing the reaction kettle in an oven with the temperature of 100 ℃ for reaction for 18h, centrifuging and filtering the obtained precipitate with absolute ethyl alcohol, and finally placing the obtained precipitate in the oven with the temperature of 70 ℃ for drying for 12h to obtain ZIF-67 powder.
(2) Carbonization treatment
And (2) placing the ZIF-67 powder obtained in the step (1) into a tube furnace, heating the tube furnace at the speed of 5 ℃/min under the protection of argon atmosphere, and keeping the temperature at 800 ℃ for 6 h.
(3) Modification of lead-free solder
And weighing tin powder, copper powder and ZIF-67 carbonized powder with different mass fractions by using a high-precision balance according to the proportion of Sn-0.7Cu-0.15 carbonized ZIF-67, and pouring the weighed materials into ethanol for ultrasonic treatment for 10min to obtain a mixed solution. Pouring the mixture into a ball milling tank for wet milling, wherein the ball-material ratio is about 6:1, the ball milling rotation speed is 200r/min, rotating forwards for 5min, stopping for 5min, rotating backwards for 5min, and ball milling for 240 min. And (3) placing the obtained ball-milling slurry in a drying box at 50 ℃ for heat preservation for 4h for drying, pressing the dried mixed powder into blocks by using a grinding tool with the inner diameter of 16mm, placing the obtained blocks into a porcelain boat, sintering in a tubular furnace under the protection of high-purity argon (Ar is more than or equal to 99.999%) atmosphere at the heating rate of 8 ℃/min, preserving heat at 180 ℃ for 2h, and turning the composite solder blocks for sintering again in order to ensure uniform sintering.
Example 3
(1) Synthesis of Ni-MOF
0.1661g of terephthalic acid is added into 50ml of N, N-Dimethylformamide (DMF) to prepare solution A with the concentration of terephthalic acid (PTA) being 0.02 mol/L; 2.6173g of nickel nitrate is added into 100ml of deionized water to prepare a solution B with the concentration of the nickel nitrate being 0.09 mol/L; respectively ultrasonically stirring the A, B solutions for 10min, then mixing, and ultrasonically stirring the mixed solutions at room temperature for 10 min; and then putting the solution into a reaction kettle, putting the reaction kettle into an oven with the temperature of 150 ℃ for reaction for 12 hours, centrifuging and filtering the obtained precipitate by using absolute ethyl alcohol, and finally drying the precipitate at the temperature of 70 ℃ to obtain Ni-MOF powder.
(2) Carbonization treatment
And (2) placing the Ni-MOF powder obtained in the step (1) into a tube furnace, heating the tube furnace at the speed of 5 ℃/min under the protection of argon atmosphere, and keeping the temperature at 800 ℃ for 6 h.
(3) Solder preparation
The method comprises the steps of weighing and placing Sn, Cu particles and Ni-MOF carbides with different mass fractions by using a high-precision balance according to the proportion of Sn-0.7Cu-0.15Ni-MOF carbides for later use, cleaning oxidation films possibly remained on the surfaces of metal particles by using 4 vol.% hydrochloric acid alcohol before smelting, drying by using a vacuum drying oven, then smelting in a vacuum furnace under the protection of high-purity argon (Ar is more than or equal to 99.999%) atmosphere, wherein the heating rate is 8 ℃/min, keeping the temperature at 230 ℃ for 3h, and repeating the whole smelting process for 4 times in order to obtain the brazing filler alloy with uniform components.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (4)
1. A process for modifying lead-free solders with MOFs-carbonized products, prepared by:
step 1, mixing nitrate serving as a metal particle source, an organic ligand and liquid serving as reaction conditions, and ultrasonically stirring the mixed solution; putting the mixed solution into a reaction kettle, putting the reaction kettle into a drying oven for reaction, centrifuging and filtering the obtained precipitate by using absolute ethyl alcohol, and finally drying to obtain dodecahedron, lamellar or flaky MOFs powder;
and 2, putting the MOFs powder obtained in the step 1 into a tubular furnace for carbonization to obtain a carbonized product of the MOFs.
2. The process for the modification of lead-free solders of the carbonized products of MOFs according to claim 1, characterized in that: the carbonization product of the MOFs accounts for 0.01-1.0% of the total mass of the lead-free solder, and the lead-free solder is one of Sn-Cu, Sn-Ag and Sn-Zn solder.
3. Method for the modification of lead-free solders of the MOFs carbonized products according to claim 1 or 2, characterized in that: the modification steps are as follows: weighing MOFs carbonized products and lead-free solder raw material particles, cleaning the MOFs carbonized products and the lead-free solder raw material particles by using hydrochloric acid alcohol, drying the MOFs carbonized products and the lead-free solder raw material particles by using a vacuum drying oven, smelting the MOFs carbonized products and the lead-free solder raw material particles in a vacuum furnace under the protection of high-purity argon atmosphere, wherein the heating rate is 8 ℃/min, the temperature is kept at 210-400 ℃ for 3-5h, and the whole smelting process is.
4. Method for the modification of lead-free solders of the MOFs carbonized products according to claim 1 or 2, characterized in that: the modification steps are as follows: weighing carbonized products of MOFs and lead-free solder raw material powder, pouring the carbonized products and the lead-free solder raw material powder into ethanol, carrying out ultrasonic treatment for 5-10min to obtain a mixed solution, pouring the mixed solution into a ball milling tank for wet milling, wherein the ball-material ratio is 6:1, the ball milling rotation speed is 200r/min, rotating forwards for 5min, stopping for 5min, rotating backwards for 5min, and carrying out ball milling for 240 min; and (3) placing the obtained ball-milling slurry in a drying box at 40-60 ℃ for heat preservation for 2-4h for drying, pressing the dried mixed powder into a block by using a grinding tool, placing the block into a porcelain boat, sintering in a tubular furnace under the protection of high-purity argon atmosphere at the heating rate of 8 ℃/min, preserving heat at 180 ℃ and 200 ℃ for 2-3h, and then overturning the composite solder block for sintering again.
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| CN114632992B (en) * | 2022-01-26 | 2023-02-07 | 中国矿业大学 | A MOFs derivative interface modification layer and its preparation method and its application in the modification of lead-free solder |
| CN114425365B (en) * | 2022-01-29 | 2024-04-26 | 重庆交通大学 | Preparation method of defect-rich Mn-Co metal oxide catalyst |
| CN115893368A (en) * | 2022-11-04 | 2023-04-04 | 盱眙新远光学科技有限公司 | A kind of MOFs carbonization product and its preparation method and its application in electronic paste modification |
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