Introduction Nowadays, high-density interconnect (HDI) printed circuit board (PCB) substrates have been widely applied to high-end electronics to meet the increasing input and output (I/O) density and small footprint area. Micro-via, a tiny structure buried among build-up layers that provide electrical interconnection is a key component in the HDI substrate. However, the preparation of micro-via is facing new challenges. It is not only required that the size of the micro-via scales down to meet the increased interconnect density, but also that the micro-via should withstand severe operating conditions in different scenarios. Therefore, it is of great importance to improve the quality of micro-vias during processing and manufacturing. The micro-via structure is a sandwich structure that is processed by electroless Cu plating and Cu electrolyte plating sequentially, and thus the quality of the electroless Cu layer can significantly affect the reliability of micro-via. In this work, we mainly focused on the electroless Cu plating process and investigated the effect of the electroless Cu deposition speed on the quality of the micro-via structure. SIM and HR-TEM characterizations were employed to investigate the micro-structure inside the electroless Cu layer. Materials and Method In this study, we used the common alkaline ion catalyst method to prepare the electroless Cu layer. The electroless Cu plating and electrolyte Cu plating was conducted on a PCB Resin Coated Copper (RCC) substrate that was cleaned by soft etching in an acid condition. The surface is then pre-dipped in an anionic solution, and palladium ions were adsorbed using an alkaline ion catalyst. The electroless Cu processes adopted in a reaction bath that consists of Cu resource (CuSO4·5H2O), complexing agent (KNaC4H4O6·4H2O) and reductant (HCHO). The whole reaction was conducted in the alkaline condition with a PH of 12.5, and the thickness of the electroless Cu deposition was controlled at around 0.20 µm. NiSO4 is selected as the Ni precursor to alter the Ni concentration in the reation bath. The contents of Ni addition were selected as 50 %, 100 %, 200 % and 300% of a conventional process at a bath temperature of 27 ºC. The thickness of the plated Cu layer was measured by a gravimetric method. Results and discussion TEM observation was used to identify the structure at the interface. Fig. 1 shows the TEM observation of the sample with 50 % and 200 % Ni concentrate. There are some nanovoids found at the interface between the Cu substrate and electroless Cu, which is arguably due to hydrogen generated during electroless Cu plating. The sample with a higher reaction speed has more nanovoids. It can be due to that the higher reaction speed can generate more hydrogen bubbles in the bath that can attach to the electroless Cu layer, leading to nanovoids as shown in Fig. 1. The samples prepared at different bath temperatures are under investigation to illustrate that the reaction speed can significantly affect the Cu electroless layer quality. Conclusions In this work, we investigated the Ni effect in electroless Cu on the RCC substrate. It is found that the higher Ni incorporation can lead to massive nanovoids generation and fine Cu grains in the electroless layer, which is a potential risk for the reliability of the HDI substrate. By reducing the Ni incorporation content, the number of nanovoids can be effectively reduced. Figure 1