Copper electroplating leveler, preparation method thereof, and electroplating solution
A leveling agent and electroplating copper technology, which is applied in the field of applied electrochemistry, can solve the problems of high price, and achieve the effects of simple equipment, reduced complexity, and good adaptability
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[0050] The preparation method of the electroplating copper leveling agent according to the embodiment of the present invention comprises the following steps:
[0051] Step 1: Weigh the imidazole compound and dichloromethyl ether, put them into a flask of a rotary evaporator, and heat through a water bath while rotating to obtain intermediate 1.
[0052] The structural formula of the intermediate 1 is shown in (2) below:
[0053]
[0054] Its chemical reaction formula is as shown in following formula (5):
[0055]
[0056] Wherein, the imidazole compound may be selected from 1-vinylimidazole, N-ethylimidazole, 1,2-dimethylimidazole, 1-n-butylimidazole, or a mixture thereof.
[0057] Specifically, put the imidazole compound and dichloromethyl ether into the flask of a rotary evaporator with a molar ratio of 1:(0.8-1.2), heat it to 50-60° C. in a water bath, and carry out the process while rotating. After 2-4 hours of reaction, Intermediate 1 was obtained.
[0058] Step ...
Embodiment 1
[0083] First, 1-vinylimidazole and dichloromethyl ether were put into a flask of a rotary evaporator with a molar ratio of 1:1, heated to 50°C in a water bath, and reacted for 4 hours to generate intermediate 1.
[0084] Next, continue to add liquid bromine into the reaction system, the mole fraction of which is half of the mole fraction of 1-vinylimidazole, continue to heat up to 70°C, continue to rotate and stir, and fully react for 5 hours to generate intermediate 2.
[0085] Thereafter, continue to add phenylhydrazine to the reaction system, the mole fraction of which is the same as that of 1-vinylimidazole, maintain the temperature at 70°C, continue to rotate and stir, and fully react for 6 hours to generate intermediate 3.
[0086] Thereafter, feed high-purity oxygen into the rotary evaporator, maintain the temperature at 70°C, continue to rotate and stir, and fully react for 2 hours to obtain the target product, namely polyheterocyclic ammonium salt.
[0087] Finally, t...
Embodiment 2
[0089] The electroplating solution was prepared by using the polyheterocyclic ammonium salt obtained in Example 1.
[0090] First, prepare a base solution based on a mixed solution of copper sulfate pentahydrate and sulfuric acid, wherein the concentration of copper sulfate pentahydrate in the base solution is 100g / L, the concentration of sulfuric acid in the base solution is 200g / L, and the chloride ion The concentration in the base solution is 60mg / L.
[0091] Thereafter, the polyheterocyclic ammonium salt obtained in Example 1, sodium polydipropylenesulfonate disulfide as an accelerator, and tridecyl alcohol polyoxyethylene propylene ether as an inhibitor were added to the base solution.
[0092] Wherein, the concentration of the polyheterocyclic ammonium salt in the whole plating solution is 30ppm, the concentration of the accelerator in the whole plating solution is 10ppm, and the concentration of the inhibitor in the whole plating solution is 600ppm.
[0093] After mixi...
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