We developed a technique to dope electrodeposited Ni with B to produce ductile bulk electrodeposits of Ni–B alloys. The conventional method, in which TMAB is added as a source for B-doping to the deposition bath before electrodeposition, affected only the first layer, producing two layers of Ni–B alloys and pure Ni in the bulk electrodeposits. These inhomogeneous specimens showed poor tensile properties, because of processing-defects presented in the layer of Ni–B alloys. These defects were produced because TMAB immediately decomposes during electrodeposition, generating hydrogen gas. In contrast, the developed technique for B-doping, in which TMAB is added intermittently during electrodeposition, produced a more-uniform B content of 0.04 at.% in the growth direction. This B distribution resulted in a uniform nanocrystalline structure with a grain size of ~28 nm. The sample of bulk nanocrystalline Ni–B alloys exhibited a good tensile elongation of 7.6% with a high tensile strength of 1.45 GPa. The developed B-doping technique avoids the harmful effects of the hydrolysis of boron compounds, and it can produce electrodeposited bulk nanocrystalline Ni–B alloys with good ductility.
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