Development of a scanning probe microscopy integrated atomic layer deposition system for in situ successive monitoring of thin film growth

Abstract

A dual chamber system integrated with atomic layer deposition (ALD) and atomic force microscopy (AFM) was developed for the successive monitoring of nanoparticles to thin film growth process. The samples were fabricated in the ALD chamber. A magnetic transmission rod enabled sample transferring between the ALD and the AFM test chambers without breaking the vacuum, avoiding possible surface morphology change when frequently varying the growth condition and oxidation under ambient condition. The sample transmission also avoids deposition and contamination on the AFM tip during the successive testing. The sample stage has machined a group of accurate location pinholes, ensuring the 10 μm2 measurement consistency. As a demonstration, the platinum thin films with different thickness were fabricated by varying ALD cycles. The surface morphology was monitored successively during the deposition. Under vacuum with controlled oxygen partial pressure, the aging and sintering phenomenon of particles has been studied in the AFM testing chamber after high temperature treatment. The integrated AFM/ALD instrument is potentially a powerful system for monitoring the thin film preparation and characterization.

Two-Step Hybrid Passivation Strategy for Ultrastable Photoluminescence Perovskite Nanocrystals

“…Previous studies reported that the optical properties of NCs are influenced by the surface chemical reaction between the ALD precursors and the NCs’ ligands. , Accordingly, a specially designed ALD reactor integrated with an FTIR spectrometer is exploited, which enables in situ characterizations to investigate ligand exchange and evolution during deposition after each precursor dosing (Figure c,d). The position and separation of ν­(COO – ) bands, Δ, can be used to deduce the carboxylate coordination mode. , Only after one pulse of the TMA precursor, the intensity of the COO – group associated with the Pb-bridged oleate ligands decreases (Δ = 156 cm –1 ) and it increases for the oleate ligands coordinated to Al (Figure c), which indicates the reorganization of OA ligands from Pb to Al atoms (Δ = 119 cm –1 ) .…”

“…Previous studies reported that the optical properties of NCs are influenced by the surface chemical reaction between the ALD precursors and the NCs' ligands. 22,33 Accordingly, a specially designed ALD reactor integrated with an FTIR spectrometer is exploited, 37 which enables in situ characterizations to investigate ligand exchange and evolution during deposition after each precursor dosing (Figure 4c,d). The position and separation of ν(COO − ) bands, Δ, can be used to deduce the carboxylate coordination mode.…”

“…35,36 1 H NMR measurements were recorded on a Bruker Ascend Spectrometer operating at a 1H frequency of 600 MHz and equipped with a BBFO-Z probe. The testing temperature was set to 298.2 K. For the quantitative 1D 1H measurements, 64k data points were sampled with the spectral width set to 20 ppm and a relaxation delay of 30 s. Infrared spectra were collected in a specially designed ALD reactor integrated with a Fourier transform infrared (FTIR) spectrometer (Nicolet iS50), 37 which enabled in situ characterizations during the ALD process.…”

In Situ Kinetic Observations on Crystal Nucleation and Growth

“…AFM was invented in 1986, and thereafter, a number of different imaging modes have been developed to date, such as the contact mode (CM), noncontact mode (NCM), and tapping mode (TM), with vacuum, gas, or liquid environments. − ,− The main advantages of CM are the scanning speed, the simplicity of implementation, as well as the possibility of simultaneously measuring mechanical or electrical properties. However, its notable drawbacks are the possible damage to fragile samples, the rapid wear of certain tip coatings, as well as the inconvenience linked to the presence of contamination on the surfaces.…”

Ambient pressure x-ray photoelectron spectroscopy setup for synchrotron-based in situ and operando atomic layer deposition research

“…Some of the most common in situ tools that are used to obtain information on ALD processes are quartz crystal microbalance (QCM), 6,7 mass spectrometry, 8,9 spectroscopic ellipsometry, 10 and, recently also, atomic force microscopy. 11 To study surface components and termination of the substrate, infrared spectroscopy, in particular, Fourier transform infrared spectroscopy (FTIR), [12][13][14][15][16] has seen interest. These techniques provide information on the ALD reaction mechanism through measurement of various quantities either in the gas phase or more directly on the surface.…”