A method of preparing a conductive metallic layer or pattern
A conductive metal layer, metal layer technology, applied in the formation of conductive patterns, improvement of metal adhesion of insulating substrates, conductive coatings, etc.
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Embodiment 1
[0192] Preparation of silver nanoparticle dispersion NPD-01
[0193] 576.0 g of 2-pyrrolidone, 576.0 g of ethanol and 1728.0 g of YTZ beads were added to a 2 liter PE container. To this mixture was added 320.0 g of silver oxide (from Umicore). The closed container was then placed on a "roller mill" for 24 hours. After removal of the YTZ beads, a predispersion was obtained.
[0194] 44.26 ml of formic acid was added to the predispersion at 22°C (1.25 mL / min). The mixture was then stirred overnight at 22°C. The mixture was then filtered using a 60 μm filter cloth. The filtrate was then concentrated at 40° C., first at 110 mbar for 60 minutes and then at 60 mbar for 30 minutes.
[0195] The resulting silver nanoparticle dispersion NPD-01 had ± 20% by weight of silver relative to the total weight of the dispersion.
Embodiment 2
[0197] The silver nanoparticle dispersion NPD-01 and the dispersion obtained by first diluting the dispersion with a 50 / 50% by weight mixture of 2-phenoxyethanol / 2-methylpyrrolidone were subsequently coated on polyester ( Blade coater, the coating thickness is 10 μm), to obtain coating layers CL-01 and CL-02.
[0198] CL-01 and CL-02 were subsequently subjected to multiple treatments: drying, application of an overcoat of 1% HCl solution on top of the coating, and curing in the order shown in Table 2.
[0199] The surface resistance (SER) of the coatings after different treatments of the coatings was measured using a four-point collinear probe. The surface or sheet resistance is calculated by the following formula:
[0200] SER=(π / ln2)*(V / I)
[0201] in:
[0202] SER is the surface resistance of the layer, expressed in Ω / □;
[0203] π is a mathematical constant, approximately equal to 3.14;
[0204] ln2 is a mathematical constant equal to the natural logarithm of the valu...
Embodiment 3
[0218] Preparation of Silver Nanoparticle Dispersion NPD-02
[0219] While stirring, 78.0 g of silver oxide was slowly added to the 1 L reactor containing 275.0 g of valeric acid and 401.0 g of 2-pyrrolidone. The temperature of the mixture was maintained at 25°C.
[0220] After the silver oxide addition was complete, the suspension was stirred overnight at 25°C.
[0221] Subsequently, 300.0 g of N,N-diethylhydroxylamine were added to the suspension over a time span of 1.5 hours. The temperature of the reaction mixture was maintained at 25 °C. When all the reducing agent had been added, the reaction was kept at 25°C while stirring for an additional 1 hour.
[0222]The reaction mixture was then fed into a settling vessel where it was kept overnight without stirring. Carefully remove the supernatant from the pellet.
[0223] The resulting sediment was washed four times: with DowanolPM TM (547g) washed twice and with butylcellosolve TM (547g) was washed twice. In each wash...
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