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Democritus (460-370 B.C.) is the one who stated th every idea of atoms in the fifth century B.C. Although he performed no experiment and had very weak evidence to support this hypothesis, his theory was kept alive by Roman poet Lucretius, who survived the Dark Ages to be discovered in the 1400s.
Skip ahead about a millenium to John Dalton in 1803. Dalton made several suggestions, which included that atoms are indivisible, identical, and are neither created, nor destroyed. Several of these theories were proven wrong later.
In 1897, J.J. Thompson discovered how cathode rays could be deflected by an electric field, and how they really weren't "rays" at all, but particles.
Robert Millikan used an oil drop experiment to test whether or not electrons were negatively charged. He also tested protons and found their charge to be positive.
Ernest Rutherford studied the absorption of redioactivity. He updated Thomson's plum pudding model and discovered neutrons that had no charge.