Method of negative tone development using a copolymer multilayer electrolyte and articles made therefrom
A technology of multi-layer products and block copolymers, applied in the direction of layered products, chemical instruments and methods, synthetic resin layered products, etc.
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example 1
[0136] This example details the synthesis of a first composition comprising a block copolymer comprising poly(N,N'-dimethylaminoethyl methacrylate)-block-poly(methacrylic acid tert-butyl ester) (PDMAEMA-b-PtBMA).
[0137] Dimethyl 2,2'-azobis(2-methylpropionate) (0.101 grams (g)), tert-butyl methacrylate (tBMA, 20.000 g), benzodithio 2-cyano A 250 milliliter (mL) glass vial was loaded with propan-2-yl ester (CPBD, 0.389 g), ethyl acetate (20 mL), and a magnetic stir bar. The mixture was deoxygenated with nitrogen for 1 hour (h) and then the flask was placed in a heat block at 70 °C for 24 hours. After the reaction, the flask was cooled by opening the bottle for 2 h and bubbling N 2 to evaporate the ethyl acetate. The reaction mixture was then dissolved in 60 mL THF and precipitated into 1 liter (L) of methanol / water mixture (9:1). The precipitate was collected and reprecipitated. The polymer poly-tert-butyl methacrylate (PtBMA) was harvested and dried overnight in a vacuu...
example 2
[0139]This example details poly(N,N'-dimethylaminoethyl methacrylate)-block-poly(adamantyl methacrylate)-block-poly(tert-butyl methacrylate) (PDMAEMA- Synthesis of b-PAdMA-b-PtBMA). Adamantyl methacrylate (AdMA) is the repeating unit used to form the neutral block. Thus, the neutral block comprises poly(1-adamantyl methacrylate). AdMA monomer was polymerized using a procedure similar to that set forth above, using PtBMA from Example 1 as the macroinitiator. Load 2.00 g of PtBMA, 13.3 g of AdMA, 0.014 g of dimethyl 2,2'-azobis(2-methylpropionate), PGMEA (15 mL), and a magnetic stir bar into a 50 mL air-free reactor . The mixture was freeze-pump-thaw three times, and then the flask was placed in a hot oil bath at 70°C for 16 hours. After the reaction, the flask was cooled, then the reaction mixture was dissolved in 10 mL of THF and precipitated into 1 L of acetonitrile. The precipitate was collected and reprecipitated. The polymer (PAdMA-b-PtBMA) was harvested and dried ov...
example 3
[0142] This example details poly(N,N'-dimethylaminoethyl methacrylate)-block-poly(adamantyl methacrylate-random-1,1-diphenylethyl methacrylate) Synthesis of (PDMAEMA-b-P(AdMA-r-PPMA)). Freeze-pump-thaw monomer and solvent three times to remove oxygen. All three monomers were activated with Al before use 2 o 3 Purified further and diluted with cyclohexane to about 50 vol% concentration. The amount of tetrahydrofuran (THF) required for a reaction concentration of about 7-10 wt% solids was transferred to the reactor containing pre-dried LiCl. The contents were cooled to -78°C in a dry ice / isopropanol bath. THF was titrated with 0.7M sec-butyllithium (SBL) initiator in cyclohexane until a green color was observed. The reaction bath was allowed to warm to room temperature until the green color completely disappeared. The reaction bath was again cooled to -78°C, followed by the addition of 0.442 g of diphenylethylene (DPE) and sec-butyllithium initiator (3.79 g, 0.43M in cyclo...
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