ExperimentalSynthesis Protocol: Polystyrene-b-poly(ethylene oxide) [P1503-SEO, M n : PS (2300) -PEO (3100), M w /M n : 1.08, PEO volume fraction: 0.56, calculated using known densities of polystyrene and poly(ethylene oxide) at room temperature (r PS = 1.05 g cm ±3 , r PEO = 1.13 g cm ±3 )[11] Polymer Source, Inc.], liquid scintillation mixture containing 1,4-bis-2-(5-phenyloxazolyl)-benzene (POPOP) and 2,5-diphenyloxazole (PPO) in toluene (Aldrich, 1 L contains 1.25 g POPOP and 100 g PPO in toluene), 6 LiOH . H 2 O (95 %), HCl (12.2 M, EM Science), toluene (Aldrich, anhydrous, 99.8 %), and methyl alcohol (MeOH, Burdick & Jackson, HPLC grade) were used as received. The liquid scintillation mixture (600 lL) was diluted (to 2500 lL) with toluene beforehand. In a typical synthesis, 40.6 mg of P1503-SEO was dissolved in 500 lL of MeOH with varying amounts (1, 2.4 mg; 2, 4.7 mg; 3, 9.4 mg; 4,14.1 mg; 5,18.8 mg; 6, 28.3 mg) of 6 LiCl. Subsequently, 20 lL of the diluted PPO/POPOP solution was added to each solution. The control samples (C1 and C2) were prepared with P1503-SEO (40.6 mg) in MeOH (500 lL) for C1 and P1503-SEO (40.6 mg) in MeOH (500 lL) containing diluted PPO/POPOP (20 lL) for C2. Each precursor solution was sonicated for about 10 min. The viscous solutions were then applied to 1 in. (1 in. = 2.54cm) diameter quartz discs to give thick monolithic films. After drying for one week at room-temperature, these monolithic films were tested for neutron detection capabilities.Characterization: The pulse-height analysis system consisted of a one-inch-diameter PMT (Hamamatsu R1924A), amplifiers (Ortec 113 preamplifier and 575A shaping main amplifier), and a computerinterfaced multichannel analyzer (Spectrum Techniques UCS-20). The procedure for neutron measurements involved placing a specific scintillator near a neutron source storage drum containing a 3 Ci AmBe neutron source and a 3 mCi 252 Cf spontaneous fission neutron source. The drum uses a thick neutron moderator/absorber shield, so that thermal neutrons predominate in the energy distribution outside the drum. The scintillator and PMT were shielded from fission gamma radiation by 5 cm lead bricks, and an additional 3 cm of high-density polyethylene moderator was interposed between the bricks and the source drum. Pulse-height spectra were accumulated over 1.5 10 4 s for each neutron detector sample.Fluorescence emission and excitation spectra were recorded on a SPEX Fluorolog spectrofluorometer Model FL3-22, equipped with two double-grating monochromators and a 450 W xenon lamp as an excitation source.