Rutherford's Gold Foil Experiment (1911)
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Rutherford, with Geiger and Marsden, fired alpha particles at gold foil; most passed through, a few bounced back, leading him to propose the nuclear model in 1911.
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The rare, sharp deflections meant the particles struck something small, dense, and positively charged, hidden in mostly empty space.
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Rutherford expected no deflection under the "plum pudding" model; the rare bounce forced a new model.