Although modern analytical instruments such as gas chromatograph, high-performance liquid chromatograph, and inductively coupled plasma mass spectrometer have improved detection limit and can simultaneously analyze several target compounds in complex sample matrices, they possess certain limitations such as the high cost of procurement, significant recurring cost for routine maintenance, large space demand, incapability of field deployment for in-situ analysis, and requirement of thorough training for the operators. As a result, there has been a strong need for the development of a cheap, fast, sensitive, and field deployable device for analytical purposes. Sensor fabrication has attracted a huge attention as an alternative to the sophisticated analytical instruments due to their competitive advantages in terms of cost, simplicity, ease of operation, and sensitivity and minimal environmental impact. The quality of a sensor’s performance is dependent on the selectivity of the sensing layer of the device. In comparison with a single nanomaterial and bulk material, hybrid nanomaterials obtained by combining two or more sensing materials at a nanoscale have been reported to exhibit more fascinating characteristics and possess competitive advantages in the construction of sensing devices due to their large surface area, uniformity, and porosity. The combination of multiple sensing material may synergistically improve the sensing performance of the sensor. This chapter briefly presents the overview, advantages, limitations of nanomaterials from the hybrid sources, their synthesis methods, and different applications of the sensing materials for analytical sensors design.