FIB-SEM tomography for porosity characterization of inkjet printed nanoparticle gold ink

Abstract

Inkjet printing is a versatile technology for the manufacturing of electronic devices to be used in various applications [1,2]. Common inks to create conductive layers are suspensions of a solvent with metal nanoparticles such as gold or silver [3]. After the deposition and solidification of an ink on a substrate, the metal nanoparticles are sintered to realize the conductivity of the printed layer. A porous, solid metal matrix remains, whereby the conductivity of the metal layer tends to be dependent on the porosity. To characterize the porosity of inkjet printed conductive layers, focused ion beam-scanning electron microscope (FIB-SEM) tomography is suggested as a potential characterization method in the presented study. For the experiment, a wafer diced silicon substrate with size of 10 x 10 mm² was used, onto which a 1.2 µm thin layer of commercially available nanoparticle gold ink was inkjet printed and then sintered. Subsequently, a four-step procedure for the FIB-SEM tomography-based porosity characterization was performed: 1) FIB preparation of the volume of interest (VOI), 2) serial sectioning including image acquisition, 3) image processing and 4) 3D-reconstruction and porosity analysis. The steps 1) and 2) were conducted using a FIB-SEM dual beam system ZEISS AURIGA 40 (Carl Zeiss Microscopy Deutschland GmbH, Germany). Prior to serial sectioning, a thin platinum layer was FIB induced deposited on top of the inkjet printed gold layer. A cube-shaped VOI with the size 5000 x 6000 x 5000 nm³ was then prepared by FIB milling. The surface to be sectioned was end face polished and a line trench serving as a reference marker for the image processing was milled along the VOI. The prepared VOI prior to FIB sectioning is shown in Figure 1. a). Next, the serial sectioning was conducted. The ion acceleration voltage was set to 30 kV. The aperture current was set to 50 pA, resulting in an ion beam spot size of 12.5 nm, which corresponds to the section slice thickness. No melting and re-sintering of the solid metal structure could be observed during sectioning. SEM images of the revealing surface areas were acquired with 1024 x 768 pixels image resolution and a pixel size of 5.82 nm. Both a secondary electron (SE) detector as well as a backscattered electron (BSE) detector were used for imaging. In total, a 2D stack of 368 SEM images was recorded. For comparison of individual sections, Figure 1. b) and c) show BSE detector images of the cross-sectioned VOI after slice 70 and slice 140. One can clearly see that the size and distribution of sintered metal particles varies along the VOI, forming a porosity network within the solid gold. Since the images acquired with the BSE detector presented a higher contrast and thus, a better distinction between the pores and the metal structure, these images were used for the image processing and final porosity analysis, for which the software AVIZO (Thermo Fisher Scientific Inc., USA) was used. First, the 2D images were aligned to correct for the shifts which occurred during the serial sectioning. Then, a sub-VOI was cropped out to exclude the reference line. The new 3D VOI was of a size of 3026 x 1164 x 2750 nm³, representing a stack of BSE detector images ranging from slice 30 to 250. Noise interference was minimized by applying a Gaussian filter. Afterwards, thresholding was applied as a segmentation technique to differentiate between pores and the solid gold as well as erosion as morphological operation. As a result, a reconstructed 3D model of the pores located in the solid gold was obtained, as shown in Figure 2. a). Using this 3D pore model, the number of pores and their diameters within the VOI could be determined. For the calculation of the pore diameters, each pore was considered to be of a spherical shape. A total of 1509 pores was counted. The pore diameter distribution is shown in the box plot in Figure 2. b). As it can be obtained from Figure 2. b), a pore size of 23 nm represents the lower quartile, while a pore size of 112 nm represents the upper quartile. The median pore size is 44 nm, while the mean is 63 nm, which indicates a trend towards smaller pores surrounded by larger pores. Based on the obtained results, FIB-SEM tomography with subsequent image processing is assessed by the authors to be a proper method to characterize the porosity of inkjet printed conductive layers, which was tested by means of a nanoparticle gold ink.