This article explores the control of MXene electronic properties through termination and intercalation. MXenes are 2D materials with high electronic conductivity, used in applications such as electromagnetic interference shielding, chemical sensing, and energy storage. The study shows that surface de-functionalization and intercalation can significantly affect MXene conductivity. In situ vacuum annealing, electrical biasing, and spectroscopic analysis within the transmission electron microscope (TEM) were used to correlate surface de-functionalization with increased electronic conductivity. Intercalation was shown to induce transitions between metallic and semiconductor-like transport, with the transition from positive to negative temperature dependence of resistance. These findings suggest that intercalation- and termination-engineered MXenes could have improved electronic conductivity and potentially exhibit semiconducting, magnetic, and topologically insulating properties. MXenes are formed by etching MAX compounds to remove the A-group element. They have a general formula of Mₙ₊₁XₙTₓ, where M is a transition metal, X is carbon or nitrogen, and T is a surface termination. The study investigated three MXenes: Ti₃C₂Tₓ, Ti₃CNTₓ, and Mo₂TiC₂Tₓ. Ti₃C₂Tₓ is the most conductive MXene, while Ti₃CNTₓ and Mo₂TiC₂Tₓ have been less studied. The study found that de-intercalation and surface de-functionalization significantly increased the conductivity of all three MXenes. The effects of intercalation and surface termination on MXene electronic properties were analyzed using in situ and ex situ spectroscopic techniques. The results showed that intercalation can induce transitions between metallic and semiconductor-like transport, and that surface termination can significantly affect the electronic properties of MXenes. The study also found that the termination of MXenes can influence their electronic properties, with oxygen terminations being more stable than -F terminations. The findings suggest that MXenes can be engineered to have improved electronic properties, which could lead to new applications in electronics and materials science.This article explores the control of MXene electronic properties through termination and intercalation. MXenes are 2D materials with high electronic conductivity, used in applications such as electromagnetic interference shielding, chemical sensing, and energy storage. The study shows that surface de-functionalization and intercalation can significantly affect MXene conductivity. In situ vacuum annealing, electrical biasing, and spectroscopic analysis within the transmission electron microscope (TEM) were used to correlate surface de-functionalization with increased electronic conductivity. Intercalation was shown to induce transitions between metallic and semiconductor-like transport, with the transition from positive to negative temperature dependence of resistance. These findings suggest that intercalation- and termination-engineered MXenes could have improved electronic conductivity and potentially exhibit semiconducting, magnetic, and topologically insulating properties. MXenes are formed by etching MAX compounds to remove the A-group element. They have a general formula of Mₙ₊₁XₙTₓ, where M is a transition metal, X is carbon or nitrogen, and T is a surface termination. The study investigated three MXenes: Ti₃C₂Tₓ, Ti₃CNTₓ, and Mo₂TiC₂Tₓ. Ti₃C₂Tₓ is the most conductive MXene, while Ti₃CNTₓ and Mo₂TiC₂Tₓ have been less studied. The study found that de-intercalation and surface de-functionalization significantly increased the conductivity of all three MXenes. The effects of intercalation and surface termination on MXene electronic properties were analyzed using in situ and ex situ spectroscopic techniques. The results showed that intercalation can induce transitions between metallic and semiconductor-like transport, and that surface termination can significantly affect the electronic properties of MXenes. The study also found that the termination of MXenes can influence their electronic properties, with oxygen terminations being more stable than -F terminations. The findings suggest that MXenes can be engineered to have improved electronic properties, which could lead to new applications in electronics and materials science.