Method for preparing composite grain size nano silver paste
A technology of nano-silver and nano-silver particles, which is applied in metal processing equipment, transportation and packaging, etc., can solve problems such as temperature increase, time extension, and thermal conductivity reduction, so as to improve thermal conductivity, reduce mean free path, crystallization, etc. The effect of small particle size
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[0042] The preparation method of composite particle size nano-silver paste provided by the invention, the preparation method comprises:
[0043] Step 1, preparing the first-size nano-silver particles, specifically comprising:
[0044] Step 1.1, uniformly mix the sodium citrate dihydrate solution with the ferrous sulfate heptahydrate solution to make a reducing solution; preferably, the sodium citrate dihydrate solution has a concentration of 1-2.5mol / L, and its volume fraction is 20 -50 parts; the concentration of ferrous sulfate heptahydrate solution is 1-2mol / L, and its parts by volume are 20-50 parts;
[0045] Step 1.2, adding the above-mentioned reducing solution dropwise to the silver nitrate solution that is strongly mechanically stirred to carry out the reduction reaction; preferably, the concentration of the silver nitrate solution is 0.5-1mol / L, and its volume fraction is 20-50 parts;
[0046] In step 1.3, the reduced and precipitated nano-silver particles are separa...
Embodiment 1
[0062] Evenly mix 35mL, 1.5mol / L sodium citrate dihydrate solution with 25mL, 1mol / L ferrous sulfate heptahydrate solution to make a reducing solution, and add dropwise to 25mL, 0.5mol / L in the silver nitrate solution. After the reaction is completed, the reduced and precipitated silver nanoparticles are separated from the solution by centrifugation at a speed of 4000 rpm for 3 minutes, and then the upper layer solution is removed. The nano-silver particles at the bottom of the centrifuge tube were redissolved in 20mL of ultrapure water, and ultrasonication was applied to disperse them evenly, forming a nano-silver sol. Then add 10mL, 1.5mol / L sodium citrate dihydrate solution for flocculation. After the nano-silver sol is added to the electrolyte solution, the ionization balance is destroyed and becomes unstable, and the nano-silver particles are re-precipitated and centrifuged again. This process was repeated three times to remove impurity ions in the nano-silver paste. F...
Embodiment 2
[0067] Evenly mix 50mL, 2mol / L sodium citrate dihydrate solution with 50mL, 2.5mol / L ferrous sulfate heptahydrate solution to make a reducing solution, and add dropwise to 50mL, 1mol / L in silver nitrate solution. After the reaction is completed, the reduced and precipitated silver nanoparticles are separated from the solution by centrifugation at a speed of 4000 rpm for 3 minutes, and then the upper layer solution is removed. Re-dissolve the nano-silver particles at the bottom of the centrifuge tube in 50mL of ultrapure water, and apply ultrasound to make them uniformly dispersed and become a nano-silver sol. Then add 30mL, 2.5mol / L sodium citrate dihydrate solution for flocculation. After the nano-silver sol is added to the electrolyte solution, the ionization balance is destroyed and becomes unstable, and the nano-silver particles are re-precipitated and centrifuged again. This process was repeated twice to remove impurity ions in the nano-silver paste. Finally, a single ...
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