Time-domain Brillouin scattering (TDBS) is applied for the first time to perform the 3D imaging of polycrystalline water ice phases, VII and VI, coexisting at a pressure of 2.1 GPa in a diamond anvil cell (DAC) at room temperature. Materials and Methods The TDBS is a non-destructive opto-acousto-optic pump-probe technique [1] which allows the study of a variety of transparent materials [2]. In this method, an optical pump pulse from a femtosecond laser is absorbed by an optoacoustic transducer contacting the sample. As a result, a picosecond acoustic pulse is emitted into the sample. It scatters a time-delayed optical probe pulse from the same or another femtosecond laser. Thus, via detection of the changes of the transient optical reflectivity in time, the evolution of the acoustic pulse with its propagation distance can be probed when it traverses the sample. The TDBS signal contains information on the characteristics of the acoustic pulse and the parameters of the material in the current spatially localized position of the acoustic pulse. The length of this pulse is commonly at nanometers spatial scale. Therefore, the technique is suitable for imaging of materials along the pulse propagation path with a spatial resolution better than optical. Two-dimensional (lateral and depth) TDBS imaging has been earlier applied for revealing the texture of solid H2O [3] and Ar [4], the phase transitions [5] and the reliable pressure dependences of elastic moduli [6] in water ice. We report here the extension of the TDBS technique to the 3D imaging of samples compressed in a DAC. To accelerate the data acquisition and to make 3D imaging possible in reasonable time, we applied, for the first time, to a sample at high pressure in a DAC, an ultrafast laser technique called asynchronous optical sampling (ASOPS). In ASOPS technique, the time delay between the pump and the probe is controlled electronically by an offset of the repetition rate frequency of two lasers without the use of a slow mechanical delay line. The experiments were conducted on water ice in a DAC at 2.1 GPa. The opto-acoustic generator (iron plate of approximately 40 μm thickness [5]) inside the sample chamber has the diameter of ∼110 μm. The full width at half maximum of the laser beams at the surface of the generator is 1.4 μm. When irradiated by the pump optical pulses at 515 nm wavelength from our ASOPS-based picosecond acoustic microscope (JAX-M1, NETA, France), it emits picosecond acoustic pulses in 14.5 μm layer of water ice on the top of laser irradiated Fe surface [5]. The maximum analyzable time delay (1.9 ns) of the probe laser pulses at 532 nm wavelength provided opportunity for imaging the ice layers up to ∼10 μm distances from the generator. The image in the volume of 40x40x10 μm3 is obtained with the lateral step of 2 μm in 2 hours. Results Maps of the Brillouin frequencies in the moving time windows of the acoustic pulse propagation in the ice are presented in Fig.1. They were obtained using a time-frequency analysis based on the synchronous detection principle [6]. The delay times between the probe and the pump laser pulses inside the time windows are marked above each of the cross sectional maps (a)-(c) and, thus, correspond to different depth layers in the sample. The red line attracts the eyes to the variations of the Brillouin frequency with time in a selected lateral region. Note that, because acoustic waves propagate at different velocities in different lateral points, the same time window corresponds to different depth windows in different lateral points. The estimates demonstrate that the highest and the lowest detected Brillouin frequencies are the fingerprints of presence of the ice VII, while the intermediate frequencies in the lower half of the frequency spectrum could be due to the presence of ice VI. Fig.1. 2D maps of the Brillouin frequencies distribution in the 40x40 μm2 cross sections of the tested ice volume at 2.1 GPa for shifting time slices. The red line highlights one of the lateral regions with important variations of the Brillouin frequency as a function of the distance from the generator. Conclusions We demonstrated the ASOPS-based 3D TDBS imaging of water ice in a DAC. This 3D imaging allows us to visualize shapes of the crystallites formed in the sample volume and their transformation with increasing load. In perspective, the 3D imaging of the transient processes at high pressures with nanometers depth resolution could be possible. Acknowledgement This research is supported by the grant . References 1.C. 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