© 2019 Wiley-VCH Verlag GmbH & Co. KGaA, WeinheimAt present, CNT supported catalysts were prepared by two different methods as NaBH4 reduction and dendrimer templated NaBH4 reduction method to observe the effect of preparation method on the sensitivity and activity of H2O2 reduction. Then, CNT supported PdxAuy bimetallic nanocatalysts having various atomic ratio were synthesized via novel dendrimer templated NaBH4 reduction method. The resulting materials were characterized employing XRD and TEM. Crystallite size of 10 %Pd0.7Au0.3/CNTdendrimer was obtained from XRD 17.1 nm and mean particle size obtained from TEM is about 15 nm. Moreover, the electrochemical behavior of these catalysts was characterized by cyclic voltammetry (CV) and chronoamperometry (CA) techniques. PdxAuy bimetallic nanocatalysts have excellent electrocatalytic properties and great potential for applications in electrochemical detection. The sensitivity and the limit of detection values for the prepared sensor with monometallic 10 % Pd/CNTdendrimer catalysts are 219.78 μA mM−1cm−2 and 2.6 μM, respectively. However, the sensor constructed with 10 %Pd0.7Au0.3/CNTdendrimer modified electrode has a very high sensitivity of 316.89 μA mM−1 cm−2 with a quick response time of 2 s and a wide linear range of 0.001–19.0 mM. In addition, the interference experiment indicated that the 10 % Pd0.7Au0.3/CNTdendrimer nanoparticles have good selectivity toward H2O2.