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(1) Background: The high-voltage anodic-plasma (HVAP) coating technique has a series of specificities that are not simultaneously met in other deposition methods. This paper aimed at assessing the potential of HVAP to synthesize quality multilayers for X-ray optics. (2) Methods: Nanolayers of W, Ta, B, and Si were deposited as mono-, bi-, and multilayers onto very smooth glass substrates by HVAP, and their thickness and density were analyzed by X-ray reflectometry. The minimal film thickness needed to obtain continuous nanolayers was also investigated. (3) Results: Nanolayer roughness did not increase with layer thickness, and could be lowered via deposition rate, with values as low as 0.6 for the W nanolayer. Minimal film thickness for continuous films for the studied metals was 4 nm (W), 6 nm (Ta), 2.5 nm (B), and 6 nm (Si). (4) Conclusions: The investigation revealed the range of parameters to be used for obtaining quality nanolayers and multilayers by HVAP. Advantages and possible improvements are discussed. This deposition technique can be tailored for demanding applications such as X-ray mirrors.