Silver powder for low-temperature curing conductive silver paste and preparation method thereof
A technology for conductive silver paste and silver powder, which is applied in metal processing equipment, transportation and packaging, etc., can solve the problems of inability to meet the performance requirements of low-temperature cured conductive silver paste for silver powder, low tap density, and wide particle size distribution, and achieves a reduction in Cleaning difficulty, high tap density and good thixotropy
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[0027] The preparation method of silver powder for low-temperature curing conductive silver paste of the present invention specifically comprises the steps of: chemical reduction, ball milling, wherein:
[0028] The chemical reduction process includes: mixing the reducing agent solution and the silver salt solution for reaction, and controlling the pH of the system at 1-4, 4-7, and 7-14 sequentially through a pH adjusting solution; standing for sedimentation, washing, and obtaining a silver powder slurry ;
[0029] The ball milling process includes: adding ball milling solvent, lubricant, surfactant, ball milling medium and the above-mentioned silver powder slurry into ball milling equipment, ball milling, separating, filtering, drying, and sieving to obtain silver powder with high tap density; wherein, the surface active The agent contains amino and hydroxyl functional groups.
[0030] Preferably, during the chemical reduction process, the reaction process includes: adding t...
Embodiment 1
[0049] 1. Weigh 0.25kg of silver nitrate and dissolve it in 5L deionized water to make a silver salt solution; weigh 0.05kg of sodium carbonate or nitric acid and dissolve it in 0.5L of deionized water to make a pH adjustment solution; weigh 0.3kg of sodium phosphite Dissolve in 0.3L deionized water to make reducing agent solution.
[0050] 2. At 20°C, within 60 minutes, add the reducing agent solution into the silver salt solution by constant flow titration, and continue the reaction for 10 minutes; during the entire reaction process, control the pH of the system at 1-4 within the time period of 0-21 minutes, The pH of the system is controlled at 4-7 within the period of 22-63 minutes, and the pH of the system is controlled at 7-14 in the period of 64-70 minutes.
[0051] 3. Set aside to settle, after the powder settles, pour off the supernatant, wash with deionized water until the conductivity of the supernatant is less than 20μs / cm, and obtain a silver powder slurry;
[00...
Embodiment 2
[0054] 1. Weigh 1.25kg silver nitrate and dissolve in 5L deionized water to make a silver salt solution; weigh 0.2kg sodium hydroxide or nitric acid and dissolve it in 0.5L deionized water to make a pH adjustment solution; weigh 0.6kg tripropylene Dissolve triol in 0.3L deionized water to make reducing agent solution.
[0055] 2. At 50°C, within 120 minutes, add the reducing agent solution into the silver salt solution by constant flow titration, and continue to react for 30 minutes; during the whole reaction process, control the pH of the system at 1-4 within the time period of 0-60 minutes, The pH of the system is controlled at 4-7 within the period of 61-135 minutes, and the pH of the system is controlled at 7-14 in the period of 136-150 minutes.
[0056] 3. Set aside to settle, after the powder settles, pour off the supernatant, wash with deionized water until the conductivity of the supernatant is less than 20μs / cm, and obtain a silver powder slurry;
[0057] 4. Stir and...
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