A study on microstructural evolution and age hardening behavior of a new metastable beta titanium alloy Ti–2Al–9.2Mo–2Fe was undertaken by microscopic observation, Vickers hardness and tensile tests in this research. The result showed that the athermal ω phase was formed in the beta matrix after solution treatment and followed by water quench, but it seemed that the athermal ω phase did not result in a considerable hardening (300HV in hardness and 670MPa in YS in ST condition). However, the isothermal ω phases with 10–40nm and nano-scaled α platelets with 30–100nm were observed in the alloy aged at lower temperatures (300–450°C). The nano-scaled ω and α phase led to an attractive hardening effect (400–500HV in hardness and above 1500MPa in YS). However, micro-scaled α phase with 0.5–3μm obtained in the samples aged at temperatures (500–600°C) showed a moderate hardening (350–450HV in hardness and 1100–1500MPa in YS). The hardening went through an under-aging, peak-aging and over-aging due to the continuation of nucleation and growth of the α phases and subsequent coarsening. The coarsen α phases (3–5μm) and grain boundary α layers (0.1–0.5μm in thickness) obtained at high temperatures aging (650–750°C) showed a poor hardening or even a softening (around 300HV in hardness and below 1000MPa in YS). The Ti–2Al–9.2Mo–2Fe alloy had a fast aging response, and can be age hardened to high hardness above 400HV within 30min at a broad aging temperature region. The age hardening curves can also provide a basic criterion for selecting aging treatment for a given stress level.