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1.
ACS Mater Lett ; 2(5): 511-518, 2020 May 04.
Artigo em Inglês | MEDLINE | ID: mdl-32421046

RESUMO

With downscaling of device dimensions, two-dimensional (2D) semiconducting transition metal dichalcogenides (TMDs) such as WS2 are being considered as promising materials for future applications in nanoelectronics. However, at these nanoscale regimes, incorporating TMD layers in the device architecture with precise control of critical features is challenging using current top-down processing techniques. In this contribution, we pioneer the combination of two key avenues in atomic-scale processing: area-selective atomic layer deposition (AS-ALD) and growth of 2D materials, and demonstrate bottom-up processing of 2D WS2 nanolayers. Area-selective deposition of WS2 nanolayers is enabled using an ABC-type plasma-enhanced ALD process involving acetylacetone (Hacac) as inhibitor (A), bis(tert-butylimido)-bis(dimethylamido)-tungsten as precursor (B), and H2S plasma as the co-reactant (C) at a low deposition temperature of 250 °C. The developed AS-ALD process results in the immediate growth of WS2 on SiO2 while effectively blocking growth on Al2O3 as confirmed by in situ spectroscopic ellipsometry and ex situ X-ray photoelectron spectroscopy measurements. As a proof of concept, the AS-ALD process is demonstrated on patterned Al2O3/SiO2 surfaces. The AS-ALD WS2 films exhibited sharp Raman (E 2g 1 and A 1g) peaks on SiO2, a fingerprint of crystalline WS2 layers, upon annealing at temperatures within the thermal budget of semiconductor back-end-of-line processing (≤450 °C). Our AS-ALD process also allows selective growth on various TMDs and transition metal oxides while blocking growth on HfO2 and TiO2. It is expected that this work will lay the foundation for area-selective ALD of other 2D materials.

2.
ACS Appl Mater Interfaces ; 12(3): 3873-3885, 2020 Jan 22.
Artigo em Inglês | MEDLINE | ID: mdl-31880425

RESUMO

Two-dimensional (2D) layered transition metal dichalcogenides (TMDs) such as WS2 are promising materials for nanoelectronic applications. However, growth of the desired horizontal basal-plane oriented 2D TMD layers is often accompanied by the growth of vertical nanostructures that can hinder charge transport and, consequently, hamper device application. In this work, we discuss both the formation and suppression of vertical nanostructures during plasma-enhanced atomic layer deposition (PEALD) of WS2. Using scanning transmission electron microscopy studies, formation pathways of vertical nanostructures are established for a two-step (AB-type) PEALD process. Grain boundaries are identified as the principal formation centers of vertical nanostructures. Based on the obtained insights, we introduce an approach to suppress the growth of vertical nanostructures, wherein an additional step (C)-a chemically inert Ar plasma or a reactive H2 plasma-is added to the original two-step (AB-type) PEALD process. This approach reduces the vertical nanostructure density by 80%. It was confirmed that suppression of vertical nanostructures goes hand in hand with grain size enhancement. The vertical nanostructure density reduction consequently lowers film resistivity by an order of magnitude. Insights obtained in this work can contribute toward devising additional pathways, besides plasma treatments, for suppressing the growth of vertical nanostructures and improving the material properties of 2D TMDs that are relevant for nanoelectronic device applications.

3.
Chem Mater ; 31(22): 9354-9362, 2019 Nov 26.
Artigo em Inglês | MEDLINE | ID: mdl-31806923

RESUMO

Phase-controlled synthesis of two-dimensional (2D) transition-metal chalcogenides (TMCs) at low temperatures with a precise thickness control has to date been rarely reported. Here, we report on a process for the phase-controlled synthesis of TiS2 (metallic) and TiS3 (semiconducting) nanolayers by atomic layer deposition (ALD) with precise thickness control. The phase control has been obtained by carefully tuning the deposition temperature and coreactant composition during ALD. In all cases, characteristic self-limiting ALD growth behavior with a growth per cycle (GPC) of ∼0.16 nm per cycle was observed. TiS2 was prepared at 100 °C using H2S gas as coreactant and was also observed using H2S plasma as a coreactant at growth temperatures between 150 and 200 °C. TiS3 was synthesized only at 100 °C using H2S plasma as the coreactant. The S2 species in the H2S plasma, as observed by optical emission spectroscopy, has been speculated to lead to the formation of the TiS3 phase at low temperatures. The control between the synthesis of TiS2 and TiS3 was elucidated by Raman spectroscopy, X-ray photoelectron spectroscopy, high-resolution electron microscopy, and Rutherford backscattering study. Electrical transport measurements showed the low resistive nature of ALD grown 2D-TiS2 (1T-phase). Postdeposition annealing of the TiS3 layers at 400 °C in a sulfur-rich atmosphere improved the crystallinity of the film and yielded photoluminescence at ∼0.9 eV, indicating the semiconducting (direct band gap) nature of TiS3. The current study opens up a new ALD-based synthesis route for controlled, scalable growth of transition-metal di- and tri-chalcogenides at low temperatures.

4.
Chem Mater ; 31(14): 5104-5115, 2019 Jul 23.
Artigo em Inglês | MEDLINE | ID: mdl-31371869

RESUMO

Edge-enriched transition metal dichalcogenides, such as WS2, are promising electrocatalysts for sustainable production of H2 through the electrochemical hydrogen evolution reaction (HER). The reliable and controlled growth of such edge-enriched electrocatalysts at low temperatures has, however, remained elusive. In this work, we demonstrate how plasma-enhanced atomic layer deposition (PEALD) can be used as a new approach to nanoengineer and enhance the HER performance of WS2 by maximizing the density of reactive edge sites at a low temperature of 300 °C. By altering the plasma gas composition from H2S to H2 + H2S during PEALD, we could precisely control the morphology and composition and, consequently, the edge-site density as well as chemistry in our WS2 films. The precise control over edge-site density was verified by evaluating the number of exposed edge sites using electrochemical copper underpotential depositions. Subsequently, we demonstrate the HER performance of the edge-enriched WS2 electrocatalyst, and a clear correlation among plasma conditions, edge-site density, and the HER performance is obtained. Additionally, using density functional theory calculations we provide insights and explain how the addition of H2 to the H2S plasma impacts the PEALD growth behavior and, consequently, the material properties, when compared to only H2S plasma.

5.
Dalton Trans ; 48(10): 3496-3505, 2019 Mar 14.
Artigo em Inglês | MEDLINE | ID: mdl-30801097

RESUMO

Atomic/molecular layer deposited (ALD/MLD) inorganic-organic thin films form a novel class of materials with tunable properties. In selected cases, hybrid materials are reported to show environmental instability, specifically towards moisture. In this article, we focus on zinc oxide/zincone multi-layers with the theoretical formula of (ZnO)a(Zn-O-C6H4-O)b. We show by means of ellipsometric porosimetry that micro-porosity in the range of 0.42 and 2 nm in the pristine zincone layer is responsible for its environmental degradation. During degradation, it is found that a relative micro-porosity content of 1.2 ± 0.1 vol% in the pristine zincone films evolves into micro-mesoporosity with a relative content of 39 ± 1 vol%. We also show that the micro-porosity in the zincone layer can be gradually suppressed when few cycles (a = 1-10) of ZnO are introduced. The resulting (ZnO)a(Zn-O-C6H4-O)b = 1 periodic multilayer is an environmentally stable film with a = 10. It is found that the suppressed micro-porosity is due to the development of continuous ZnO layers with a≥ 10.

6.
Chem Mater ; 31(1): 2-12, 2019 Jan 08.
Artigo em Inglês | MEDLINE | ID: mdl-30774194

RESUMO

Bottom-up nanofabrication by area-selective atomic layer deposition (ALD) is currently gaining momentum in semiconductor processing, because of the increasing need for eliminating the edge placement errors of top-down processing. Moreover, area-selective ALD offers new opportunities in many other areas such as the synthesis of catalysts with atomic-level control. This Perspective provides an overview of the current developments in the field of area-selective ALD, discusses the challenge of achieving a high selectivity, and provides a vision for how area-selective ALD processes can be improved. A general cause for the loss of selectivity during deposition is that the character of surfaces on which no deposition should take place changes when it is exposed to the ALD chemistry. A solution is to implement correction steps during ALD involving for example surface functionalization or selective etching. This leads to the development of advanced ALD cycles by combining conventional two-step ALD cycles with correction steps in multistep cycle and/or supercycle recipes.

7.
ACS Appl Mater Interfaces ; 11(5): 5526-5535, 2019 Feb 06.
Artigo em Inglês | MEDLINE | ID: mdl-30624886

RESUMO

Ultrathin metal oxides prepared by atomic layer deposition (ALD) have gained utmost attention as moisture and thermal stress barrier layers in perovskite solar cells (PSCs). We have recently shown that 10 cycles of ALD Al2O3 deposited directly on top of the CH3NH3PbI3- xCl x perovskite material, are effective in delivering a superior PSC performance with 18% efficiency (compared to 15% of the Al2O3-free cell) with a long-term humidity-stability of more than 60 days. Motivated by these results, the present contribution focuses on the chemical modification which the CH3NH3PbI3- xCl x perovskite undergoes upon growth of ALD Al2O3. Specifically, we combine in situ Infrared (IR) spectroscopy studies during film growth, together with X-ray photoelectron spectroscopy (XPS) analysis of the ALD Al2O3/perovskite interface. The IR-active signature of the NH3+ stretching mode of the perovskite undergoes minimal changes upon exposure to ALD cycles, suggesting no diffusion of ALD precursor and co-reactant (Al(CH3)3 and H2O) into the bulk of the perovskite. However, by analyzing the difference between the IR spectra associated with the Al2O3 coated perovskite and the pristine perovskite, respectively, changes occurring at the surface of perovskite are monitored. The abstraction of either NH3 or CH3NH2 from the perovskite surface is observed as deduced by the development of negative N-H bands associated with its stretching and bending modes. The IR investigations are corroborated by XPS study, confirming the abstraction of CH3NH2 from the perovskite surface, whereas no oxidation of its inorganic framework is observed within the ALD window process investigated in this work. In parallel, the growth of ALD Al2O3 on perovskite is witnessed by the appearance of characteristic IR-active Al-O-Al phonon and (OH)-Al═O stretching modes. Based on the IR and XPS investigations, a plausible growth mechanism of ALD Al2O3 on top of perovskite is presented.

8.
ACS Appl Mater Interfaces ; 10(36): 30367-30378, 2018 Sep 12.
Artigo em Inglês | MEDLINE | ID: mdl-30113160

RESUMO

In this work, we present an extensive characterization of plasma-assisted atomic-layer-deposited SnO2 layers, with the aim of identifying key material properties of SnO2 to serve as an efficient electron transport layer in perovskite solar cells (PSCs). Electrically resistive SnO2 films are fabricated at 50 °C, while a SnO2 film with a low electrical resistivity of 1.8 × 10-3 Ω cm, a carrier density of 9.6 × 1019 cm-3, and a high mobility of 36.0 cm2/V s is deposited at 200 °C. Ultraviolet photoelectron spectroscopy indicates a conduction band offset of ∼0.69 eV at the 50 °C SnO2/Cs0.05(MA0.17FA0.83)0.95Pb(I2.7Br0.3) interface. In contrast, a negligible conduction band offset is found between the 200 °C SnO2 and the perovskite. Surprisingly, comparable initial power conversion efficiencies (PCEs) of 17.5 and 17.8% are demonstrated for the champion cells using 15 nm thick SnO2 deposited at 50 and 200 °C, respectively. The latter gains in fill factor but loses in open-circuit voltage. Markedly, PSCs using the 200 °C compact SnO2 retain their initial performance at the maximum power point over 16 h under continuous one-sun illumination in inert atmosphere. Instead, the cell with the 50 °C SnO2 shows a decrease in PCE of approximately 50%.

9.
ACS Appl Mater Interfaces ; 10(15): 13158-13180, 2018 Apr 18.
Artigo em Inglês | MEDLINE | ID: mdl-29554799

RESUMO

Oxide and nitride thin-films of Ti, Hf, and Si serve numerous applications owing to the diverse range of their material properties. It is therefore imperative to have proper control over these properties during materials processing. Ion-surface interactions during plasma processing techniques can influence the properties of a growing film. In this work, we investigated the effects of controlling ion characteristics (energy, dose) on the properties of the aforementioned materials during plasma-enhanced atomic layer deposition (PEALD) on planar and 3D substrate topographies. We used a 200 mm remote PEALD system equipped with substrate biasing to control the energy and dose of ions by varying the magnitude and duration of the applied bias, respectively, during plasma exposure. Implementing substrate biasing in these forms enhanced PEALD process capability by providing two additional parameters for tuning a wide range of material properties. Below the regimes of ion-induced degradation, enhancing ion energies with substrate biasing during PEALD increased the refractive index and mass density of TiO x and HfO x and enabled control over their crystalline properties. PEALD of these oxides with substrate biasing at 150 °C led to the formation of crystalline material at the low temperature, which would otherwise yield amorphous films for deposition without biasing. Enhanced ion energies drastically reduced the resistivity of conductive TiN x and HfN x films. Furthermore, biasing during PEALD enabled the residual stress of these materials to be altered from tensile to compressive. The properties of SiO x were slightly improved whereas those of SiN x were degraded as a function of substrate biasing. PEALD on 3D trench nanostructures with biasing induced differing film properties at different regions of the 3D substrate. On the basis of the results presented herein, prospects afforded by the implementation of this technique during PEALD, such as enabling new routes for topographically selective deposition on 3D substrates, are discussed.

10.
Chem Mater ; 30(4): 1209-1217, 2018 Feb 27.
Artigo em Inglês | MEDLINE | ID: mdl-29515290

RESUMO

The maximum conductivity achievable in Al-doped ZnO thin films prepared by atomic layer deposition (ALD) is limited by the low doping efficiency of Al. To better understand the limiting factors for the doping efficiency, the three-dimensional distribution of Al atoms in the ZnO host material matrix has been examined on the atomic scale using a combination of high-resolution transmission electron microscopy (TEM) and atom probe tomography (APT). Although the Al distribution in ZnO films prepared by so-called "ALD supercycles" is often presented as atomically flat δ-doped layers, in reality a broadening of the Al-dopant layers is observed with a full-width-half-maximum of ∼2 nm. In addition, an enrichment of the Al at grain boundaries is observed. The low doping efficiency for local Al densities > ∼1 nm-3 can be ascribed to the Al solubility limit in ZnO and to the suppression of the ionization of Al dopants from adjacent Al donors.

11.
Chem Mater ; 30(3): 663-670, 2018 Feb 13.
Artigo em Inglês | MEDLINE | ID: mdl-29503508

RESUMO

Area-selective atomic layer deposition (ALD) is envisioned to play a key role in next-generation semiconductor processing and can also provide new opportunities in the field of catalysis. In this work, we developed an approach for the area-selective deposition of metal oxides on noble metals. Using O2 gas as co-reactant, area-selective ALD has been achieved by relying on the catalytic dissociation of the oxygen molecules on the noble metal surface, while no deposition takes place on inert surfaces that do not dissociate oxygen (i.e., SiO2, Al2O3, Au). The process is demonstrated for selective deposition of iron oxide and nickel oxide on platinum and iridium substrates. Characterization by in situ spectroscopic ellipsometry, transmission electron microscopy, scanning Auger electron spectroscopy, and X-ray photoelectron spectroscopy confirms a very high degree of selectivity, with a constant ALD growth rate on the catalytic metal substrates and no deposition on inert substrates, even after 300 ALD cycles. We demonstrate the area-selective ALD approach on planar and patterned substrates and use it to prepare Pt/Fe2O3 core/shell nanoparticles. Finally, the approach is proposed to be extendable beyond the materials presented here, specifically to other metal oxide ALD processes for which the precursor requires a strong oxidizing agent for growth.

12.
Ultramicroscopy ; 182: 233-242, 2017 11.
Artigo em Inglês | MEDLINE | ID: mdl-28734230

RESUMO

A combined X-ray and scanning tunneling microscopy (STM) instrument is presented that enables the local detection of X-ray absorption on surfaces in a gas environment. To suppress the collection of ion currents generated in the gas phase, coaxially shielded STM tips were used. The conductive outer shield of the coaxial tips can be biased to deflect ions away from the tip core. When tunneling, the X-ray-induced current is separated from the regular, 'topographic' tunneling current using a novel high-speed separation scheme. We demonstrate the capabilities of the instrument by measuring the local X-ray-induced current on Au(1 1 1) in 800 mbar Ar.

14.
ACS Appl Mater Interfaces ; 9(2): 1858-1869, 2017 Jan 18.
Artigo em Inglês | MEDLINE | ID: mdl-28059494

RESUMO

The advent of three-dimensional (3D) finFET transistors and emergence of novel memory technologies place stringent requirements on the processing of silicon nitride (SiNx) films used for a variety of applications in device manufacturing. In many cases, a low temperature (<400 °C) deposition process is desired that yields high quality SiNx films that are etch resistant and also conformal when grown on 3D substrate topographies. In this work, we developed a novel plasma-enhanced atomic layer deposition (PEALD) process for SiNx using a mono-aminosilane precursor, di(sec-butylamino)silane (DSBAS, SiH3N(sBu)2), and N2 plasma. Material properties have been analyzed over a wide stage temperature range (100-500 °C) and compared with those obtained in our previous work for SiNx deposited using a bis-aminosilane precursor, bis(tert-butylamino)silane (BTBAS, SiH2(NHtBu)2), and N2 plasma. Dense films (∼3.1 g/cm3) with low C, O, and H contents at low substrate temperatures (<400 °C) were obtained on planar substrates for this process when compared to other processes reported in the literature. The developed process was also used for depositing SiNx films on high aspect ratio (4.5:1) 3D trench nanostructures to investigate film conformality and wet-etch resistance (in dilute hydrofluoric acid, HF/H2O = 1:100) relevant for state-of-the-art device architectures. Film conformality was below the desired levels of >95% and attributed to the combined role played by nitrogen plasma soft saturation, radical species recombination, and ion directionality during SiNx deposition on 3D substrates. Yet, very low wet-etch rates (WER ≤ 2 nm/min) were observed at the top, sidewall, and bottom trench regions of the most conformal film deposited at low substrate temperature (<400 °C), which confirmed that the process is applicable for depositing high quality SiNx films on both planar and 3D substrate topographies.

15.
ACS Appl Mater Interfaces ; 9(1): 592-601, 2017 Jan 11.
Artigo em Inglês | MEDLINE | ID: mdl-27977925

RESUMO

The atomic layer deposition (ALD) process of hydrogen-doped indium oxide (In2O3:H) using indium cyclopentadienyl (InCp) and both O2 and H2O as precursors is highly promising for the preparation of transparent conductive oxides. It yields a high growth per cycle (>0.1 nm), is viable at temperatures as low as 100 °C, and provides a record optoelectronic quality after postdeposition crystallization of the films ( ACS Appl. Mat. Interfaces , 2015 , 7 , 16723 - 16729 , DOI: 10.1021/acsami.5b04420 ) . Since both the dopant incorporation and the film microstructure play a key role in determining the optoelectronic properties, both the crystal growth and the incorporation of the hydrogen dopant during this ALD process are studied in this work. This has been done using transmission electron microscopy (TEM) and atom probe tomography (APT) in combination with deuterium isotope labeling. TEM studies show that an amorphous-to-crystalline phase transition occurs in the low-temperature regime (100-150 °C), which is accompanied by a strong decrease in carrier density and an increase in carrier mobility. At higher deposition temperatures (>200 °C), enhanced nucleation of crystals and the incorporation of carbon impurities lead to a reduced grain size and even an amorphous phase, respectively, resulting in a strong reduction in carrier mobility. APT studies on films grown with deuterated water show that the incorporated hydrogen mainly originates from the coreactant and not from the InCp precursor. In addition, it was established that the incorporation of hydrogen decreased from ∼4 atom % for amorphous growth to ∼2 atom % after the transition to crystalline film growth.

16.
Nanoscale ; 8(47): 19829-19845, 2016 Dec 01.
Artigo em Inglês | MEDLINE | ID: mdl-27878204

RESUMO

Integrating metals and metal oxides with graphene is key in utilizing its extraordinary material properties that are ideal for nanoelectronic and catalyst applications. Atomic layer deposition (ALD) has become a key technique for depositing ultrathin, conformal metal(oxide) films. ALD of metal(oxide) films on graphene, however, remains a genuine challenge due to the chemical inertness of graphene. In this study we address this issue by combining first-principles density functional theory (DFT) simulations with ALD experiments. The focus is on the Pt ALD on graphene, as this hybrid system is very promising for solar and fuel cells, hydrogen technologies, microreactors, and sensors. Here we elucidate the surface reactions underpinning the nucleation stage of Pt ALD on pristine, defective and functionalized graphenes. The employed reaction mechanism clearly depends on (a) the available surface groups on graphene, and (b) the ligands accompanying the metal centre in the precursor. DFT calculations also indicate that graphene oxide (GO) can afford a stronger adsorption of MeCpPtMe3, unlike Pt(acac)2, as compared to bare (non-functionalized) graphene, suggesting that GO monolayers are effective Pt ALD seed layers. Confirming the latter, we evince that wafer-scale, continuous Pt films can indeed be grown on GO monolayers using a thermal ALD process with MeCpPtMe3 and O2 gas. Besides, the current in-depth atomistic insights are of practical use for understanding similar ALD processes of other metals and metal oxides on graphene.

17.
ACS Appl Mater Interfaces ; 8(38): 25005-9, 2016 Sep 28.
Artigo em Inglês | MEDLINE | ID: mdl-27618251

RESUMO

The quality assessment of moisture permeation barrier layers needs to include both water permeation pathways, namely through bulk nanoporosity and local macroscale defects. Ellipsometric porosimetry (EP) has been already demonstrated a valuable tool for the identification of nanoporosity in inorganic thin film barriers, but the intrinsic lack of sensitivity toward the detection of macroscale defects prevents the overall barrier characterization. In this contribution, dynamic EP measurements are reported and shown to be sensitive to the detection of macroscale defects in SiO2 layers on polyethylene naphthalate substrate. In detail, the infiltration of probe molecules, leading to changes in optical properties of the polymeric substrate, is followed in time and related to permeation through macroscale defects.

18.
Nanotechnology ; 27(3): 034001, 2016 Jan 22.
Artigo em Inglês | MEDLINE | ID: mdl-26636744

RESUMO

The deposition of Pd and Pt nanoparticles by atomic layer deposition (ALD) has been studied extensively in recent years for the synthesis of nanoparticles for catalysis. For these applications, it is essential to synthesize nanoparticles with well-defined sizes and a high density on large-surface-area supports. Although the potential of ALD for synthesizing active nanocatalysts for various chemical reactions has been demonstrated, insight into how to control the nanoparticle properties (i.e. size, composition) by choosing suitable processing conditions is lacking. Furthermore, there is little understanding of the reaction mechanisms during the nucleation stage of metal ALD. In this work, nanoparticles synthesized with four different ALD processes (two for Pd and two for Pt) were extensively studied by transmission electron spectroscopy. Using these datasets as a starting point, the growth characteristics and reaction mechanisms of Pd and Pt ALD relevant for the synthesis of nanoparticles are discussed. The results reveal that ALD allows for the preparation of particles with control of the particle size, although it is also shown that the particle size distribution is strongly dependent on the processing conditions. Moreover, this paper discusses the opportunities and limitations of the use of ALD in the synthesis of nanocatalysts.

19.
ACS Appl Mater Interfaces ; 7(40): 22525-32, 2015 Oct 14.
Artigo em Inglês | MEDLINE | ID: mdl-26393381

RESUMO

Encapsulation of organic (opto-)electronic devices, such as organic light-emitting diodes (OLEDs), photovoltaic cells, and field-effect transistors, is required to minimize device degradation induced by moisture and oxygen ingress. SiNx moisture permeation barriers have been fabricated using a very recently developed low-temperature plasma-assisted atomic layer deposition (ALD) approach, consisting of half-reactions of the substrate with the precursor SiH2(NH(t)Bu)2 and with N2-fed plasma. The deposited films have been characterized in terms of their refractive index and chemical composition by spectroscopic ellipsometry (SE), X-ray photoelectron spectroscopy (XPS), and Fourier-transform infrared spectroscopy (FTIR). The SiNx thin-film refractive index ranges from 1.80 to 1.90 for films deposited at 80 °C up to 200 °C, respectively, and the C, O, and H impurity levels decrease when the deposition temperature increases. The relative open porosity content of the layers has been studied by means of multisolvent ellipsometric porosimetry (EP), adopting three solvents with different kinetic diameters: water (∼0.3 nm), ethanol (∼0.4 nm), and toluene (∼0.6 nm). Irrespective of the deposition temperature, and hence the impurity content in the SiNx films, no uptake of any adsorptive has been observed, pointing to the absence of open pores larger than 0.3 nm in diameter. Instead, multilayer development has been observed, leading to type II isotherms that, according to the IUPAC classification, are characteristic of nonporous layers. The calcium test has been performed in a climate chamber at 20 °C and 50% relative humidity to determine the intrinsic water vapor transmission rate (WVTR) of SiNx barriers deposited at 120 °C. Intrinsic WVTR values in the range of 10(-6) g/m2/day indicate excellent barrier properties for ALD SiNx layers as thin as 10 nm, competing with that of state-of-the-art plasma-enhanced chemical vapor-deposited SiNx layers of a few hundred nanometers in thickness.

20.
ACS Appl Mater Interfaces ; 7(35): 19857-62, 2015 Sep 09.
Artigo em Inglês | MEDLINE | ID: mdl-26305370

RESUMO

Atomic layer deposition (ALD) of silicon nitride (SiNx) is deemed essential for a variety of applications in nanoelectronics, such as gate spacer layers in transistors. In this work an ALD process using bis(tert-butylamino)silane (BTBAS) and N2 plasma was developed and studied. The process exhibited a wide temperature window starting from room temperature up to 500 °C. The material properties and wet-etch rates were investigated as a function of plasma exposure time, plasma pressure, and substrate table temperature. Table temperatures of 300-500 °C yielded a high material quality and a composition close to Si3N4 was obtained at 500 °C (N/Si=1.4±0.1, mass density=2.9±0.1 g/cm3, refractive index=1.96±0.03). Low wet-etch rates of ∼1 nm/min were obtained for films deposited at table temperatures of 400 °C and higher, similar to that achieved in the literature using low-pressure chemical vapor deposition of SiNx at >700 °C. For novel applications requiring significantly lower temperatures, the temperature window from room temperature to 200 °C can be a solution, where relatively high material quality was obtained when operating at low plasma pressures or long plasma exposure times.

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