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We developed a method for measuring signal enhancement produced by high-Z nanofilm electrodes in parallel plate ionization chambers with variable thickness microgaps.We used a laboratory-made variable gap parallel plate ionization chamber with nanofilm electrodes made of aluminum–aluminum (Al–Al) and aluminum–tantalum (Al–Ta). The electrodes were evaporated on 1 mm thick glass substrates. The interelectrode air gap was varied from 3 μm to 1 cm. The gap size was measured using a digital micrometer and it was confirmed by capacitance measurements. The electric field in the chamber was kept between 0.1 kV/cm and 1 kV/cm for all the gap sizes by applying appropriate compensating voltages. The chamber was exposed to 120 kVp X-rays. The current was measured using a commercial data acquisition system with temporal resolution of 600 Hz. In addition, radiation transport simulations were carried out to characterize the dose, D(x), high-energy electron current, J(x), and deposited charge, Q(x), as a function of distance, x, from the electrodes. A deterministic method was selected over Monte Carlo due to its ability to produce results with 10 nm spatial resolution without stochastic uncertainties. Experimental signal enhancement ratio, SER(G) which we defined as the ratio of signal for Al–air–Ta to signal for Al–air–Al for each gap size, was compared to computations. The individual contributions of dose, electron current, and charge deposition to the signal enhancement were determined.Experimental signals matched computed data for all gap sizes after accounting for several contributions to the signal: (a) charge carrier generated via ionization due to the energy deposited in the air gap, D(x); (b) high-energy electron current, J(x), leaking from high-Z electrode (Ta) toward low-Z electrode (Al); (c) deposited charge in the air gap, Q(x); and (d) the decreased collection efficiency for large gaps (>˜500 μm). Q(x) accounts for the electrons below 100 eV, which are regarded as stopped by the radiation transport code but which can move and form electron current in small gaps (<100 μm). While the total energy deposited in the air gap increases with gap size for both samples, the average high-energy current and deposited charge are moderately decreasing with the air gap. When gap sizes are smaller than ˜20 μm, the contribution to signal from dose approaches zero while contributions from high-energy current and deposited charges give rise to an offset signal. The measured signal enhancement ratio (SER) was 40.0 ± 5.0 for the 3 μm gap and rapidly decreasing with gap size down to 9.9 ± 1.2 for the 21 μm gap and to 6.6 ± 0.3 for the 100 μm gap. The uncertainties in SER were mostly due to uncertainties in gap size and data acquisition system.We developed an experimental method to determine the signal enhancement due to high-Z nanolayers in parallel plate ionization chambers with micrometer spatial resolution. As the water-equivalent thicknesses of these air gaps are 3 nm to 10 μm, the method may also be applicable for nanoscopic spatial resolution of other gap materials. The method may be extended to solid insulator materials with low Z.