The content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of circuit board conductive liquid and preparation method thereof and
Using.
To reach this goal of the invention, the present invention uses following technical scheme:
On the one hand, the present invention provides a kind of circuit board conductive liquid, and the circuit board conductive liquid includes blank hole liquid and silver nanoparticle
Line.
In the present invention, nano silver wire is added in blank hole liquid, built-up circuit plate conduction liquid.Nano silver wire is led with height
The characteristic of electric rate, the resistance of blank hole liquid is greatly reduced, make conduction liquid that integrally there is more preferable electric conductivity on hole wall;Separately
Outside, because nano silver wire has preferable pliability and special linear structure, bridging action can be played in entirety, is shortened
Conductive path, macroscopically also show to drop low-resistance characteristic, in the later stage electroplates flow, stable performance, the obtained product back of the body
Light grade is high.
In the present invention, the blank hole liquid includes the component of following mass percentage content:
Preferably, the conductive black mass percentage content is 1%-5%, for example, can be 1%, 1.5%, 2%,
2.5%th, 3%, 3.5%, 4%, 4.5% or 5%.
Preferably, the surfactant is neopelex, lauryl sodium sulfate, aliphatic alcohol polyethenoxy
Ether or one kind in nonyl phenol polyethenoxy ether or at least two combination, mass percent can be 0.5%, 1%,
1.5%th, 2%, 2.5% or 3%.
Preferably, the dispersant is aliphatic alcohol polyethenoxy sulfuric ester, 1-isobutyl-3,5-dimethylhexylphosphoric acid potassium, polyethylene glycol or poly-
One kind or at least two combination in vinylpyrrolidone, mass percent can be 1%, 1.5%, 2%, 2.5%, 3%,
3.5%th, 4%, 4.5% or 5%.
Preferably, the pH adjusting agent is one kind in potassium carbonate, saleratus, ammoniacal liquor or monoethanolamine or at least two
Combination, mass percent can be 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5% or 5%.
Preferably, the binding agent is one kind or extremely in polyvinyl alcohol, Sodium Polyacrylate, polyacrylamide or potassium silicate
Few two kinds of combination, mass percent can be 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%,
0.9% or 1%.
Preferably, the decentralized medium be water, ethylene glycol, isopropanol or acetone in one kind or at least two combination,
Mass percent can be 81%, 83%, 85%, 88%, 90%, 92%, 94% or 96.4%.
In the present invention, the blank hole liquid is prepared by the following method:
(1) conductive black, surfactant, dispersant, pH adjusting agent, binding agent and decentralized medium are well mixed;
(2) mixture obtained in step (1) is fully ground, obtains the blank hole liquid.
Preferably, the time of step (1) described mixing is 1-2 hours, for example, can be 1 hour, 1.2 hours, it is 1.4 small
When, 1.5 hours, 1.7 hours, 1.8 hours or 2 hours.
Preferably, the time of step (2) described grinding is 2-10 hours, for example, can be 2 hours, 3 hours, 4 hours, 5
Hour, 6 hours, 7 hours, 8 hours, 9 hours or 10 hours.
The preparation method of blank hole liquid of the present invention is simple, and technique is excellent.
In the present invention, the preparing raw material of the nano silver wire includes aqueous surfactant solution and is dissolved in reduction point
Silver nitrate, dispersant and crystal seed in dispersion media.
Preferably, the mass percent concentration of the aqueous surfactant solution is 0.4%-4%, such as can be
0.4%th, 0.6%, 0.9%, 1.5%, 2%, 2.2%, 2.5%, 3%, 3.5% or 4%.
Preferably, the mass percent concentration of silver nitrate, dispersant and crystal seed is as follows in the reduction decentralized medium:
0.2%-2% silver nitrates (such as can be 0.2%, 0.8%, 1.1%, 1.4%, 1.6%, 1.8% or 2%);0.4%-4%
Dispersant (such as can be 0.4%, 0.8%, 1%, 1.5%, 2%, 2.2%, 2.5%, 3%, 3.5% or 4%);
0.01%-0.1% crystal seeds (such as can be 0.01%, 0.03%, 0.05%, 0.06%, 0.08%, 0.09% or 0.1%).
Preferably, the reduction decentralized medium is one kind or at least in glycerine, propane diols, ethylene glycol or diethylene glycol
Two kinds of combination.
In the present invention, reduction decentralized medium not only acts as the effect of reducing agent, the silver ion in reducing solution, also simultaneously
With peptizaiton so that solution has good stability.
Preferably, the dispersant is one kind or extremely in polyacrylamide, Sodium Polyacrylate or polyvinylpyrrolidone
Few two kinds combination.
Preferably, the crystal seed is one kind or at least two group in copper chloride, sodium chloride, iron chloride or palladium bichloride
Close.
In the present invention, it is crystal seed to add good crystal structure material, can accelerate into brilliant speed, better beneficial to being formed
Good crystal formation.
Preferably, the surfactant is polyoxyethylene alkyl ether sulfate, 1-isobutyl-3,5-dimethylhexylphosphoric acid potassium, dodecane
One kind or at least two combination in base benzene sulfonic acid sodium salt or lauryl sodium sulfate.
In the present invention, the suspension of described nano silver wire is prepared by the following method:
(1) silver nitrate is dissolved in reduction decentralized medium, obtains silver nitrate solution A;
(2) dispersant, crystal seed are dissolved in reduction decentralized medium, obtain dispersant seed-solution B;
(3) surfactant is soluble in water, stirring obtains clear solution C;
(4) by solution B described in step (2) stirring, heating, the solution B after will heat up add to step (1) obtain it is molten
Reacted in liquid A, be incubated after reaction, then reaction solution is centrifuged, washs to obtain nano silver wire;
(5) step (4) described nano silver wire is scattered in aqueous surfactant solution C, that is, obtains the nano silver wire
Suspension.
Preferably, the concentration of solution A described in step (1) is 0.2%-2%, for example, can be 0.2%, 0.4%,
0.6%th, 0.9%, 1.1%, 1.4%, 1.7%, 1.8% or 2%.
Preferably, the concentration of solution B described in step (2) is 0.41%-4.1%, for example, can be 0.41%, 0.7%,
1.2%th, 1.6%, 1.9%, 2.2%, 2.7%, 3.1%, 3.5%, 4% or 4.1%.
Preferably, relative to the dosage of 10g surfactants, water consumption described in step (3) is 240g-2490g, such as
Can be 240g, 300g, 500g, 1000g, 1200g, 1500g, 1900g, 2200g or 2490g.
Preferably, the stir speed (S.S.) stirred described in step (4) is that 1000-2000 turns/min, such as can be 1000 turns/
Min, 1200 turns/min, 1400 turns/min, 1500 turns/min, 1700 turns/min, 1900 turns/min or 2000 turn/min.
Preferably, heating described in step (4) is is warming up to 150-200 DEG C, for example, can be 150 DEG C, 155 DEG C, 160
DEG C, 170 DEG C, 175 DEG C, 180 DEG C, 185 DEG C, 190 DEG C, 195 DEG C or 200 DEG C.
Preferably, solution B is incubated after being heated up in step (4), the time of the insulation is 10-60min, such as can
To be 10min, 20min, 30min, 40min, 50min or 60min.
Preferably, the method added described in step (4) is dropwise addition.
Preferably, the speed of the dropwise addition is 0.1mL/min-1mL/min, such as can be 0.1mL/min, 0.2mL/
Min, 0.3mL/min, 0.4mL/min, 0.5mL/min, 0.6mL/min, 0.7mL/min, 0.8mL/min, 0.9mL/min or
1mL/min。
Preferably, the time being incubated described in step (4) is 30min-180min, for example, can be 30min, 50min,
80min, 100min, 120min, 140min, 160min or 180min.
On the other hand, the present invention provides a kind of preparation method of described circuit board conductive liquid, and methods described is:By black holes
Liquid mixes with nano silver wire suspension, stirs, and obtains the circuit board conductive liquid.
Preferably, nano silver wire suspension mass fraction in blank hole liquid is 10%-30%, such as can be
10%th, 12%, 15%, 18%, 20%, 24%, 26%, 29% or 30%.
Preferably, the mixing speed be 500-1000 turn/min, such as can be 500 turns/min, 600 turns/min, 700
Turn/min, 800 turns/min, 900 turns/min or 1000 turn/min.
The preparation method of conduction liquid of the present invention is very simple, easy to operate, is easy to produce, reduces cost.
In the present invention, there is provided a kind of application of described circuit board conductive liquid in electroplating printed circuit board.
Relative to prior art, the invention has the advantages that:
Nano silver wire is added to the circuit board conductive liquid obtained in blank hole liquid by the present invention, has the characteristic of high conductivity,
Resistance is greatly reduced, another aspect nano silver wire has special linear structure, and bridging action can be played in conduction liquid,
Shorten conductive path, macroscopically also show excellent reduction resistive performance.
Nano silver wire and conductive black reduce the resistance of blank hole liquid, make it on hole wall as conductive materials in the present invention
With more preferable through hole ability.Conduction liquid with preferable flexible nano silver wire with blank hole liquid composition, electric conductivity are excellent
Good, price is relatively low, applies in routinely flow is electroplated, and can electroplate the product backlight after flow through heat-shock, stable performance
Grade is high, compared to conductive materials such as other Nano silver grains, golden nanometer particle and graphenes, has larger advantage.
Embodiment 5
The present embodiment is prepared by the following method circuit board conductive liquid:
(1) preparation of blank hole liquid:
By conductive black, 2% lauryl sodium sulfate and the aliphatic alcohol polyethenoxy that mass percentage content is 2%
Ether, 2% 1-isobutyl-3,5-dimethylhexylphosphoric acid potassium and polyvinylpyrrolidone, 2% monoethanolamine and ammoniacal liquor, 0.7% polyvinyl alcohol and
91.3% water mixes 1.3 hours, then grinds uniform mixture 4 hours, obtains blank hole liquid.
(2) preparation of nano silver wire:
Silver nitrate is dissolved in propane diols and in glycerine, the silver nitrate for obtaining silver nitrate mass percent concentration 1.6% is molten
Liquid A;Polyacrylamide, Sodium Polyacrylate and copper chloride are dissolved in propane diols and glycerine, obtain dispersant mass percent
The dispersant seed-solution B that concentration is 3% and crystal seed mass percent concentration is 0.04%;By 10g lauryl sodium sulfate with
Neopelex is dissolved in 990g water, obtains the aqueous surfactant solution C that mass percent concentration is 1%.
Above-mentioned solution B is stirred with 1000 turns/min, 160 DEG C is warming up to, 20min is incubated after heating, then will be molten
Liquid B is added drop-wise in solution A with 0.7mL/min speed to be reacted, and is incubated 80min after reaction again, reaction solution centrifuged,
Washing obtains nano silver wire, and nano silver wire is scattered in solution C, obtains nano silver wire suspension.
(3) preparation of circuit board conductive liquid:
The blank hole liquid being prepared as described above is mixed with nano silver wire, is stirred, obtained with 600 turns/min speed
The circuit board conductive liquid that mass fraction is 22% in blank hole liquid to nano silver wire suspension.
Comparative example 1
This comparative example difference from Example 1 is, only containing the blank hole liquid prepared in embodiment 1, does not contain Yin Na
Rice noodles.
Comparative example 2
This comparative example and embodiment 1 only difference is that, mass fraction of the nano silver wire in blank hole liquid is 9%.
Comparative example 3
This comparative example and embodiment 1 only difference is that, mass fraction of the nano silver wire in blank hole liquid is 32%.
Above-described embodiment 1-5 and comparative example 1-3 is subjected to testing research, handled by carbon pores, test circuit plate hole resistance
Value, concrete outcome such as table 1 below:
Table 1
It can be concluded that by the experimental result of upper table 1, compared to like product, conduction liquid resistance of the invention is (small
In 2k Ω) it is significantly less than like product resistance;In the conduction liquid of nano silver wire is not contained, its resistance value differs with like product
Very few, effect is poor;When containing nano silver wire, but nano silver wire mass fraction is not in nano silver wire mass fraction of the present invention
When within 10%-30%, although resistance is still below like product, mass fraction is above as 10%-30% nano silver wires
Conduction liquid resistance.Therefore, the present invention contains the blank hole liquid circuit board conductive liquid that mass fraction is 10%-30% nano silver wires, tool
There is very excellent electric conductivity.
Above-described embodiment 1-5 and comparative example 1-3 is subjected to thermal shock experiment test, every group of experiment carries out 5 thermal shocks, tool
Body experimental result such as table 2 below:
Table 2
It can be concluded that by the experimental result of above-mentioned table 2, the present invention adds certain mass concentration in blank hole liquid
Nano silver wire, serve good stablizing effect, thermal shock can be withstood;And do not contain the conduction liquid of nano silver wire then without
Method is subjected to 5 thermal shock experiments, occurs and base material segregation phenomenon.
Above-described embodiment 1-5 and comparative example 1-3 is subjected to conventional plating, sample has been obtained and has been tested, as a result such as following table
3:
Table 3
It can be concluded that by the above-mentioned result of table 3, the circuit board conductive liquid prepared in the present invention is applied in conventional electricity
In plating, obtained product backlight level is high, stable performance.
Applicant states that the present invention illustrates a kind of circuit board conductive liquid of the present invention and its preparation by above-described embodiment
Methods and applications, but the invention is not limited in above-mentioned processing step, that is, do not mean that the present invention has to rely on above-mentioned technique step
Suddenly could implement.Person of ordinary skill in the field is it will be clearly understood that any improvement in the present invention, to former selected by the present invention
The equivalence replacement of material and the addition of auxiliary element, the selection of concrete mode etc., all fall within protection scope of the present invention and open model
Within enclosing.