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The NiCo layers with various Ni/Co atomic ratio have been successfully electroless deposited on PZT layers by varying the bath composition. As the cobalt atomic ratio in the deposited layer increases from 17.2 to 54.8 wt%, the magnetostrictive coefficient decreases. The magnetoelectric effect depends strongly on the magnetostrictive properties of magnetostrictive phase. The magnetoelectric coefficient of NiCo/PZT/NiCo trilayers increases with Ni/Co atomic ratio of the deposited NiCo layers increasing from 45:55 to 83:17. A maximum ME voltage coefficient of αE,31 = 2.8 V ⋅ cm−1 ⋅ Oe−1 is obtained at a frequency of about 88 kHz, which makes these trilayers suitable for applications in actuators, transducers and sensors.