Covalent carbon nitride has been produced for the first time. Binary carbon-nitrogen solids are an important synthetic goal, since although β-C3N4, has been predicted to have a hardness comparable to or greater than diamond, it cannot be produced by traditional solid-state chemistry methods. The novel approach described here combines pulsed laser ablation with a high-flux atomic beam. From comparisons with calculated diffraction patterns, it is inferred that crystalline β-C3N4, has been synthesized, although in an impure form.