The primary goals of this study were to demonstrate and fully characterize a microscale ionization source (i.e. micro-ion source) and to determine the validity of impact ionization theory for microscale devices and pressures up to 100 mTorr. The field emission properties of carbon nanotubes (CNTs) along with Micro-Electro-Mechanical Systems (MEMS) design processes were used to achieve these goals. Microwave Plasma-enhanced CVD was used to grow vertically aligned Multi-Walled Carbon Nanotubes (MWNTs) on the microscale devices. A 4-dimensional parametric study focusing on CNT growth parameters confirmed that Fe catalyst thickness had a strong effect on MWNT diameter. The MWNT growth rate was seen to be a strong function of the methane-to-ammonia gas ratio during MWNT growth. A high methane-to-ammonia gas ratio was selected for MWNT growth on the MEMS devices in order to minimize growth time and ensure that the thermal budget of those devices was met. A CNT-enabled microtriode device was fabricated and characterized. A new aspect of this device was the inclusion of a 10 micron-thick silicon dioxide electrical isolation layer. This thick oxide layer enabled anode current saturation and performance improvements such as an increase in dc amplification factor from 27 to 600. The same 3-panel device was also used as an ionization source. Ion currents were measured in the 3-panel micro-ion source for helium, argon, nitrogen and xenon in the 0.1 to 100 mTorr pressure range. A linear increase in ion current was observed for an increase in pressure. However, simulations indicated that the 3-panel design could be modified to improve performance as well as better understand device behavior. Thus, simulations and literature reports on electron impact ionization sources were used to design a new 4-panel micro-ion source. The 4-panel micro-ion source showed an approximate 10-fold performance improvement compared to the 3-panel ion source device. The improvement was attributed to the increased electron current and improved ion collection efficiency of the 4-panel device. Further, the same device was also operated in a 3-panel mode and showed superior performance compared to the original 3-panel device, mainly because of increased ion collection efficiency. The effect of voltages applied to the different electrodes in the 4-panel micro-ion source on ion source performance was studied to better understand device behavior. The validity of the ion current equation (which was developed for macroscale ion sources operating at low pressures) in the 4-panel micro-ion source was studied. Experimental ion currents were measured for helium, argon and xenon in the 3 to 100 mTorr pressure range. For comparison, theoretical ion currents were calculated using the ion current equation for the 4-panel micro-ion source utilizing values calculated from SIMION simulations and measured electron currents. The measured ion current values in the 3 to 20 mTorr pressure range followed the calculated ion currents quite closely. A significant deviation was observed in the 20-100 mTorr pressure range. The experimental ion current values were used to develop a corrected empirical model for the 4-panel micro-ion source in this high pressure range (i.e., 3 to 100 mTorr). The role of secondary electrons and electron path lengths at higher pressures is discussed.