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Described experimental conditions, reproducibility and optimization for the nonlinear optical effects (SHG, THG) for the diagnostic of functionalization of vertically aligned mesoporous silica thin films activated by silver and copper ions. The samples synthesis procedure are described in details. The dependence sof the seonc dhamroni genriaotn (SHG) and third harmonic genriaotn (THG) verus the fundamental energy density are presetned. The diffences between the SHG and THG energy power dependences are observed.

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