A novel solvent controlled precipitation (SCP) process based on microfluidization was assessed to produce solid dispersions of carbamazepine, a poorly water-soluble drug with dissolution-rate limited absorption. A half-factorial design (23–1 + 2 central points) was conducted to study the effect of different formulation variables (viz. polymer type, drug load, and feed solids' concentration) on the particle size and morphology, drug's solid state and drug's molecular distribution within the carrier of the co-precipitated materials produced. Co-precipitated powders were isolated via spray drying (SD). Nano-composite aggregated particles were obtained among all the tests. The particle size of the aggregates was dependent on the feed solids' concentration, while the level of aggregation between nanoparticles was dependent on the drug-polymer ratio. Both amorphous and crystalline nano-solid dispersions were produced using the proposed SCP process. The solid dispersion produced was dependent on both the type of polymeric stabilizer chosen and the drug load. Controls of amorphous and crystalline nano-solid dispersions produced by SCP and an amorphous micro-solid dispersion produced by SD were tested for: in vitro dissolution, in vivo pharmacokinetics in mice, and long-term storage physical stability. Both nano-amorphous and nano-crystalline presented faster dissolution rates and enhanced bioavailabilities than the micro-sized amorphous powder. The reduction of particle size to the nano-scale was found to be more important than the amorphization of the drug. The long-term physical stability of the amorphous nano-solid dispersion and the amorphous micro-solid dispersion were comparable.