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Atomic Layer Deposition of Tio2 Using Titanium Isopropoxide and H2O: Operational Principle of Equipment and Parameter Setting

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Atomic Layer Deposition of Tio2 Using Titanium Isopropoxide and H2O: Operational Principle of Equipment and Parameter Setting JOURNAL OF SEMICONDUCTOR TECHNOLOGY AND SCIENCE, VOL.16, NO.3, JUNE, 2016 ISSN(Print) 1598-1657 http://dx.doi.org/10.5573/JSTS.2016.16.3.346 ISSN(Online) 2233-4866 Atomic Layer Deposition of TiO2 using Titanium Isopropoxide and H2O: Operational Principle of Equipment and Parameter Setting Karam Cho1, Jung-Dong Park2, and Changhwan Shin1 Abstract—Titanium dioxide (TiO2) films are deposited control. ALD is a modification of the chemical vapor by atomic layer deposition (ALD) using titanium deposition (CVD) technique, and it involves the separate isopropoxide (TTIP) and H2O as precursors. The chemical injection of gaseous phases. Since ALD is operating instructions for the ALD equipment are performed at low temperatures (< 400°C), performance described in detail, along with the settings for degradation of nanometer-scale devices due to thermal relevant parameters. The thickness of the TiO2 film is diffusion is prevented. Moreover, there are many measured, and thereby, the deposition rate is advantages associated with ALD, such as low impurity quantitatively estimated to verify the linearity of the content, high aspect ratio, and step coverage close to deposition rate. 100%. Titanium dioxide (TiO2) thin films can be deposited Index Terms—Atomic layer deposition, TiO2, titanium using the ALD technique. TiO2 is a material that has been isopropoxide, H2O widely investigated for use in diverse applications such as photocatalysts [1], optical coatings [2], and high I. INTRODUCTION permittivity dielectric layers for gate oxides [3]. In addition, TiO2 is used for applications such as dynamic For the upcoming era of nanometer-scale technology, random access memory (DRAM) [4, 5] and ferroelectric atomic layer deposition (ALD) has attracted much random access memory (FeRAM) [6]. attention because it can achieve atomic level film From a range of titanium precursors, which include deposition with excellent conformality and precise titanium tetrachloride (TiCl4) [7], tetrakis(dimethyl- amido) titanium (TDMAT) [8], and titanium isopro- poxide (TTIP), TTIP is the most appropriate precursor Manuscript received Nov. 25, 2015; accepted Jan. 5, 2016 for the deposition of TiO2 thin films using the ALD This work was supported by the National Research Foundation of Korea (NRF) grant funded by the Korean government (MSIP) (No. technique. TTIP, which is an alkoxide of titanium having 2014R1A2A1A11050637). Also, this work was supported by the NRF a chemical formula of Ti(OCH(CH3)2)4, is considered the of Korea funded by the MSIP under Grant NRF-2015046617 (Fundamental Technology Program). Also, this research was supported most appropriate precursor for TiO2 films because it has by Nano·Material Technology Development Program through the the highest vapor pressure [9], exhibits non-corrosive and National Research Foundation of Korea(NRF) funded by the Ministry of Science, ICT and Future Planning.(2009-0082580). Also, this work self-limiting growth, and thus produces films of high was supported by IDEC(EDA Tool, MPW). Also, this work is purity, whereas the by-products of TiCl are corrosive, financially supported by the Ministry of Trade, Industry and Energy 4 through the fostering project of the Innovation for Engineering and TDMAT is primarily used to deposit TiN with NH3 Education. 1 School of Electrical and Computer Engineering, University of Seoul, [8]. Korea In this paper, we describe the operation of the ALD 2 Division of Electronics and Electrical Engineering, Dongguk University, Korea ([email protected]) equipment for the deposition of TiO2 thin films in detail, E-mail : [email protected] JOURNAL OF SEMICONDUCTOR TECHNOLOGY AND SCIENCE, VOL.16, NO.3, JUNE, 2016 347 and provide a method to determine the parameters. The layers, the HF cleaning process that is normally working principle of the ALD technique is first explained, conducted prior to the TiO2 deposition process was and subsequently, how to operate the equipment and omitted. Alternatively, the silicon surface was blown off deposit the TiO2 thin films using TTIP as the Ti precursor by N2 gas to remove all the particles. As shown in Fig. and H2O as the other precursor (known as the reactant or 1(a), the temperatures of the precursor, line, reactor, oxidant) is minutely described, and finally, the results substrate, and furnace were set at 50°C, 90°C, 100°C, regarding the TiO2 film thickness and estimated 250°C, and 350°C, respectively. This is an essential step, deposition rate are presented and discussed. This paper which is conducted prior to the TiO2 deposition process. should be instructive to the researchers who will use the As TTIP is a metal source, it can solidify as it is ALD equipment for the first time. transported through the pipelines of the ALD equipment. Therefore, it is mandatory to maintain a high temperature II. EXPERIMENTS along the pipelines to prevent the metal source from solidifying. Specifically, the TTIP in the source reservoir 1. Operational Principle of ALD [i.e., the blue box shown in Fig. 1(b)] is heated to 50°C to achieve the correct pressure for its release. ALD is a chemical deposition technique that enables Subsequently, at a temperature of 90°C, the TTIP is the formation of an atomic-scale thin film using the transported through the pipelines by a flow of ultrapure sequential reactions of separately injected chemicals. (99.999%) N2 at 200 sccm (standard cubic centimeters During the ALD deposition process, chemicals in their per minute). At the entrance of the chamber (or at the gaseous phases, known as precursors, are injected reactor), the metal source is heated to a temperature of separately into the chamber of the ALD equipment. 100°C, which also facilitates the heating of the chamber. Subsequently, each of them interacts with and is The substrate temperature is set at 250°C to promote a adsorbed onto the substrate surface, on which thin films chemical reaction between the reactants. The by-product are grown layer-by-layer. Specifically, two precursors are of the chemical reaction is toxic, and thus it is removed used (denoted as A and B). Initially, precursor A is in the furnace by burning at a temperature of 350°C or injected into the chamber. It reacts with the substrate greater. surface, and then, by supplying a sufficient amount of Once the temperature of each pipeline in the ALD inert gas, such as N2 or Ar, the precursor is degassed equipment reaches its targeted value, the TiO2 deposition from the chamber (so called ‘purging’). Subsequently, process can commence. Any remaining air in the precursor B is injected, and an identical method to that of pipelines can affect the chemical reaction of the reactants precursor A is followed. Herein, it is important to and thus has to be removed. When the equipment has not separate the supply of precursor A from that of precursor been used for 24 h, the pump should be switched on and B by degassing (purging) the remnant reactants for a the isolation valves (ISV), V1, V6, and V4, should be specific period of time to prevent the reactants from opened in succession and remain open for a period of 4 h interacting. This mechanism is known as a self-limiting [see Fig. 1(a)]. If the equipment has been used in the reaction, which is characteristic of the ALD process. It is previous 24 h, it is sufficient to pump the pipelines for 10 noteworthy that the sequential process involving the min to remove any existing air. To clean the pipeline for injection and purging of precursor A/precursor B is the metal source, the V6 valve should be closed and the performed in a cycle, and this cycle is repeated as many V5 valve should be opened in succession. Subsequently, times as required to deposit an atomistic thin film. the V3 valve should be opened for 3 s and then closed; this step should be repeated three times. Once the 2. Deposition of TiO2 Thin Film pipeline for the metal source is clean, the V5 valve should be closed and the V4 valve should be opened. The A. Preparatory Steps and Considerations precursor is highly reactive to ambient air and it can be To preserve the native silicon dioxide layer on the easily transmuted. Therefore, to ensure safety it is silicon substrate, which aids the deposition of the TiO2 essential to entirely fill the pipelines with N2 gas by 348 KARAM CHO et al : ATOMIC LAYER DEPOSITION OF TIO2 USING TITANIUM ISOPROPOXIDE AND H2O: OPERATIONAL … (a) (b) (c) Fig. 1. (a) Schematic illustrating the configuration of valves (V1 to V6 and ISV) along the pipelines and the temperature settings for the precursor, line, reactor, substrate, and furnace, (b) The reservoirs of H2O and TTIP are shown by the red and blue boxes, respectively, (c) in/out-manual valves of the TTIP source reservoir. setting the N2 flow rate at 200 sccm for at least 1 min. should be open and all the other valves should be closed. When all the pipelines are filled with N2 gas, the out- It is necessary to feed N2 gas through the pipeline at 200 manual valve of the TTIP source reservoir [shown in Fig. sccm and ensure that the pressure in the chamber is the 1(c)] can be opened, and then the V6 and V5 valves same as the ambient air pressure (i.e., ~8.7E+2 Torr). The should be closed and opened, respectively. Subsequently, chamber can then be opened for a sample to be loaded. the V3 valve should be opened for 3 s and then closed; When a sample is loaded into the chamber, it is necessary this step should be repeated three times. Finally, by to close/degas the chamber again by opening the ISV opening the manual valve of the H2O reservoir [shown in valve.
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