Exploiting　efficient　and　stable　noble　metal-free　hydrogen　evolution　catalysts　for　water　splitting　is　of　great　importance.　In　this　work,　NixCo1-xO@C/CdS　hybrid　is　successfully　fabricated　through　an　electrostatic　interaction　of　oppositely　charged　nanoparticles　on　their　surfaces.　The　resulting　NixCo1-xO@C　nanoboxes　cocatalysts　which　were　derived　from　NiCo-LDH@ZIF-67　with　Ni–Co　layered　double　hydroxides　(LDH)　decorated　with　ZIF-67　precursor　exhibited　improved　hydrogen　production　rate　compared　with　bare　CdS　semiconductor　from　0.7　mmol　g−1　h−1　to　56　mmol　g−1　h−1.　It　is　demonstrated　that　the　electrostatic　interaction　between　the　two　surface　charged　nanoparticles　of　NixCo1-xO@C　and　CdS　play　an　important　role　in　migrating　and　separating　of　photogenerated　charge　carriers.　The　synthesized　NixCo1-xO@C　as　excellent　candidates　for　cost-effective　cocatalysts　is　aimed　to　substitute　for　noble　metals　in　photocatalytic　H2　evolution.　©　2020　Hydrogen　Energy　Publications　LLC