I've killed fish with DIY CO2, so yes, it's perfectly possible. If CO2 goes above a certain level, it will no longer diffuse out of the fishes' gills, so it kills them not by poisoning them, or replacing the oxygen, as some have thought, but simply by making it impossible for fish to unload their CO2 from their blood to replace it with O2.
This is because CO2 is lost from the blood by simple diffusion. If there's not a high enough difference between the CO2 concentration in the blood and the CO2 concentration in the water, this won't happen (remember diffusion gradients from chemistry?). It's like expecting a truck to spontaneously roll along the flat or even uphill. Ain't gonna happen.
In low light, CO2 will do no good at all. It's not the limiting factor for photosynthesis. Only where there is plenty of light and ferts, and therefore CO2 is the limiting factor, does it actually work. It's like making bread. If you've only got so much flour, it doesn't matter how much yeast you add, you won't get any more bread.