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Article

Atomic Layer Deposition of Y2O3 Thin Films Using Y(MeCp)2(iPr-nPrAMD) Precursor and H2O, and Their Erosion Resistance in CF4-Based Plasma

by
Seong Lee
1,
Hyunchang Kim
2 and
Sehun Kwon
1,*
1
School of Materials Science and Engineering, Pusan National University, Busan 46241, Republic of Korea
2
iChems Co., Ltd., 73, Banjeong-ro 204beon-gil, Hwaseong-si 18374, Republic of Korea
*
Author to whom correspondence should be addressed.
Coatings 2025, 15(1), 22; https://doi.org/10.3390/coatings15010022
Submission received: 12 December 2024 / Revised: 24 December 2024 / Accepted: 26 December 2024 / Published: 30 December 2024
(This article belongs to the Special Issue Anti-Corrosion and Anti-Wear Coatings: Fundamentals, Technologies, and Applications)
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Abstract

:
Atomic layer deposition (ALD) of Y2O3 thin films was investigated using Y(MeCp)2(iPr-nPrAMD) precursor and H2O reactant. The self-limiting reaction mechanism of ALD-Y2O3 thin films was confirmed at a growth temperature of 260 °C. And, the saturated growth rate was confirmed to be ~0.11 nm/cycle. Also, it was demonstrated that a wide ALD temperature window from 150 °C to 290 °C maintains a consistent growth rate. ALD-Y2O3 thin films were found to have a typical cubic polycrystalline structure, independent of growth temperature, which can be attributed to their stoichiometric composition of Y2O3, negligible carbon impurity, and high film density, analogous to the Y2O3 bulk. Even at a low growth temperature of 150 °C, ALD-Y2O3 exhibited a markedly lower plasma etching rate (~0.77 nm/min) than that (~4.6 nm/min) of ALD-Al2O3 when using RIE at a plasma power of 400 W with a mixed gas of Ar/CF4/O2. Furthermore, the growth temperature of Y2O3 thin films had minimal impact on the etching rate.

1. Introduction

In the semiconductor industry, semiconductor devices with smaller feature sizes are more sensitive to particle and metal contamination, making this an important area of focus. For example, three-dimensional vertical NAND(3D V NAND) technology is being used to stack circuits in multiple layers by reducing the integrated circuit line width directly on the wafer. Therefore, the dry etching process uses fluorocarbon-based high-density plasma performed repeatedly in the chamber and at the same time, ceramic equipment components are exposed to plasma atmosphere [1]. Furthermore, fluorocarbon plasma bombards and erodes the inner-wall materials of the equipment parts [2,3,4,5,6]. In particular, the showerhead facing the wafer can undergo significant etching in a harsh, high-density plasma flux. This erosion of equipment components and the generation of contaminant particles causes serious problems, such as reducing the yield in mass production [6]. Thus, the development of advanced protective coating materials, along with proper deposition techniques, has recently become the focus of intensive efforts to minimize equipment component erosion and contaminant particle generation. A core requirement for coatings on equipment components is that the coating itself should not release particles and should not contain metal contaminants. Therefore, it must exhibit high resistance to corrosion and erosion under various chemical and plasma conditions. Corrosion can be mitigated through the use of ceramic coatings, which offer exceptional resistance to fluorine plasma.
To protect semiconductor components from plasma erosion and the formation of particle contaminants, oxide ceramics such as Al2O3 and SiO2 are commonly used as plasma-resistant materials. However, the performance of Al2O3 and SiO2 coatings has become increasingly problematic due to the higher power levels in fluorine-based plasma equipment. Additionally, these materials are shown to be vulnerable to the fluorine-based plasma etching process when subjected to repeated cycles in a chamber. To address this issue, yttrium oxide (Y2O3) has increasingly been proposed as a widely used protective coating material because of its significantly lower etching rate and low chemical reactivity [1,7,8,9,10]. Y2O3 has many favorable properties making it highly attractive for various industrial applications. These properties include a wide energy band gap (5.5 eV~5.8 eV) and band offset (2.3 eV), a relatively high dielectric constant (14~18), a high refractive index (1.9), a high melting point (2430 °C) that ensures excellent thermal stability, and good thermal conductivity (κ = 0.33 W cm−1 K−1) [11,12]. Notably, Y2O3 possesses impressive wear resistance, and high mechanical and dielectric strength, as well as superior corrosion and chemical resistance, making it an ideal choice for a protective coating in fluorine-based plasma equipment components [11,12,13,14,15].
Up to now, Y2O3 protective coating has been extensively studied using various deposition techniques, such as atmosphere plasma spray (APS) [16], vacuum plasma spray (VPS) [17], physical vapor deposition (PVD) [18], and chemical vapor deposition (CVD) [19]. However, defects such as pore generation, impurities, and poor conformality still need to be addressed in order to improve their protective performance and reduce the coating thickness. In this regard, the atomic layer deposition (ALD) technique has recently attracted attention as a feasible method for forming Y2O3 protective coatings. In this process, precursor molecules in the gaseous state are introduced into a chamber, where they react with the substrate surface to grow thin films in a layer-by-layer fashion. The key advantage of ALD lies in its atomic-scale deposition and inherently self-limiting growth mechanism, offering several benefits, including precise atomic-scale thickness control, completely conformal and pinhole-free coatings, and excellent step coverage in highly complex structures [20,21,22]. Moreover, a recent development of batch-type ALD equipment [23] is accelerating the application of the ALD protective layer in large-scale components. ALD-Y2O3 has been demonstrated by using various precursors including Y(MeCp)3 [24], Y(EtCp)3 [25], Y(iPrCp)3 [26], Y(thd)3 [27,28,29,30], and Y(EtCp)2(iPr2-amd) [31], and oxidants such as H2O and O3. However, most ALD-Y2O3 studies have primarily focused on high-k dielectric applications, with only a few studies [31] reporting its anti-corrosion properties against fluorine-based plasma. Additionally, the relatively narrow ALD temperature window of some precursors [24,25,26] needs further improvement, as it may restrict its potential for a broader range of industrial applications. For example, the ALD temperature window for Y(MeCp)3 was 250–300 °C [24]. Y(EtCp)3 and Y(iPrCp)3 also exhibited narrow ALD temperature windows (250–280 °C for Y(EtCp)3 and 245–300 °C for Y(iPrCp)3) [25,26]. For the Y(EtCp)2(iPr2-amd) precursor, the ALD temperature window was 300–450 °C, which may restrict low-temperature applications. On the other hand, Y(thd)3 showed a relatively wide ALD temperature window from 250 to 375 °C. However, high carbon and hydrogen impurities were also reported for Y(thd)3 [27,28,29,30].
Therefore, herein, we investigated ALD-Y2O3 thin films using Bis(methylcyclopentadienyl)(N’-isopropyl-N-n-propylacetamidinate)Yttrium (Y(MeCp)2(iPr-nPrAMD)). ALD growth kinetics of Y(MeCp)2(iPr-nPrAMD) were carefully examined. Also, the dependence of the growth rate and physical properties of Y2O3 thin films on the growth temperature was systematically analyzed. Finally, the etching resistance properties of ALD-Y2O3 thin films were thoroughly discussed in the context of fluorine-based plasma.

2. Materials and Methods

Y2O3 thin films were deposited on p-type Si (100) wafer by ALD at a growth temperature ranging from 150 to 290 °C. Bis(methylcyclopentadienyl)(N’-isopropyl-N-n-propylacetamidinate)Yttrium (Y(MeCp)2(iPr-nPrAMD), iChems Co., Ltd., Hwaseong-si, Republic of Korea) precursor was used as the precursor for Y, and H2O was used as a reactant. It is noted that Y(MeCp)2(iPr-nPrAMD) and H2O were kept in separate individual canisters and maintained at 120 °C and room temperature, respectively, to provide a sufficient vapor pressure. One ALD cycle of Y2O3 consisted of Y(MeCp)2(iPr-nPrAMD) injection with 50 sccm Ar for 3 s, a purge injection with 50 sccm Ar for 20 s, an injection of H2O reactant with 50 sccm for 2 s, and another 50 sccm Ar purge injection for 20 s. And, the chamber working pressure was maintained at 1.2 × 10−1 Torr. A set of ALD-Y2O3 thin films was deposited by changing the growth temperature from 150 to 290 °C. And, the Y2O3 thin films deposited at 150, 180, 220, 260, and 290 °C were designated as Y2O3-150, Y2O3-180, Y2O3-220, Y2O3-260, and Y2O3-290, respectively. The number of the repeated ALD cycles was intentionally controlled to have a similar film thickness of ~ 30 nm, regardless of the growth temperatures, in order to diminish the effect of the film thickness on the physical and chemical properties of Y2O3 thin films.
The film thickness as well as the corresponding refractive index was analyzed using spectroscopic ellipsometry (α-SE, J. A. Woollam Co., Inc., Lincoln, NE, USA). The crystal structure and thin film density were determined by X-ray diffraction (XRD) and X-ray reflectometry (XRR) using a Rigaku Smartlab diffractometer (D/MAX-2500V, Tokyo, Japan) with a Cu-kα1 radiation. And, depth profile of the composition was studied by Auger electron spectroscopy (AES, PHI-710, ULVAC-PHI, Chigasaki, Japan). The surface was checked by atomic force microscopy (AFM). The high-density plasma resistance was studied using reactive ion etching (RIE, LABStar, TTL, Pyeongtaek, Gyeonggi-do, Korea) at a plasma power of 400 W and a pressure of 50 mTorr for 15 min, employing a mixed gas of Ar (50 sccm), CF4 (45 sccm), and O2 (5 sccm).

3. Results and Discussion

First, the self-limiting growth of the ALD-Y2O3 thin films was studied. Figure 1a shows the growth rate of Y2O3 thin films as a function of Y(MeCp)2(iPr-nPrAMD) pulse time to confirm the ALD reaction mechanism at a constant growth temperature of 260 °C. Other pulses in one ALD cycle, except for the Y(MeCp)2(iPr-nPrAMD) precursor pulse time, were fixed to a 20 s purge, H2O reactant for 10 s, and another 20 s purge. By increasing the Y(MeCp)2(iPr-nPrAMD) pulse time from 2 s to 5 s, the growth rate increased and then saturated to 0.11 nm/cycle above 3 s. And, this result indicates that Y(MeCp)2(iPr-nPrAMD) was chemisorbed in a self-limiting manner. Figure 1b shows the growth rate of Y2O3 thin films depending on the H2O pulse time at 260 °C. In this case, the pulses for Y(MeCp)2(iPr-nPrAMD), precursor purge, and reactant purge were fixed at 3 s, 20 s, and 20 s, respectively. As shown in Figure 1b, the growth rate of Y2O3 thin films was saturated to ~0.11 nm/cycle above 2 s, confirming that 2 s of H2O pulse was enough to completely react with chemisorbed Y(MeCp)2(iPr-nPrAMD) precursor. Thus, the saturated growth rate of Y2O3 thin films was confirmed to be ~0.11 nm/cycle at 260 °C. Another important aspect of ALD is that the film thickness can be digitally controlled by the repeated ALD cycles. Therefore, we investigated the dependence of Y2O3 film thickness as a function of the repeated ALD cycles, as shown in Figure 1c. As shown in Figure 1c, the thicknesses of Y2O3 were increased linearly with increasing ALD-Y2O3 cycles from 300 to 900. Also, the extrapolated line shows a negligible growth delay, indicating a rapid nucleation of Y2O3 by ALD. Next, we investigated the effect of growth temperatures on the growth rate and refractive index of Y2O3 thin films as shown in Figure 1d. With increasing the growth temperatures from 150 to 290 °C, the growth rate of Y2O3 exhibited a nearly constant growth rate and did not exhibit CVD growth, suggesting a wide ALD temperature window of Y2O3. Additionally, an almost similar refractive index of ~1.87, with consideration to that (1.9) of bulk Y2O3 [12], was obtained within the ALD temperature window. Since the refractive index of a film generally depends on the film density [32], it was expected that a similar film density can be obtained from 150 to 290 °C. Also, it needs to be mentioned that the self-decomposition temperature of Y(MeCp)2(iPr-nPrAMD) precursor could be higher than 290 °C, potentially extending the upper limit of the ALD temperature window, although this could not be confirmed due to the temperature limitation of the ALD equipment used.
The microstructures of Y2O3 thin films depending on the growth temperature were investigated by XRD, as shown in Figure 2a. It is worth mentioning that XRD patterns were obtained from the Y2O3 thin films having similar thicknesses of ~30 nm by controlling ALD cycles considering the obtained growth rate at each temperature shown in Figure 1d. As shown in Figure 2a, all the Y2O3 thin films exhibited a typical cubic polycrystalline phase of Y2O3 (JCPDS 31-1105) with (222), (400), (431), and (440) planes, regardless of the growth temperatures. These characteristic phases were observed even at a low growth temperature of 150 °C, likely due to the highly dense and pure Y2O3 film formation. However, as the growth temperature increases, the amount of Y2O3 (222) planes becomes dominant due to the higher thermal energy, which is consistent with previous reports [24,30]. Therefore, the effect of growth temperature on the film density was investigated by XRR analysis, as shown in Figure 2b. The film densities were extracted from the location of the critical angles shown in Figure 2b. And, the film densities of Y2O3-150, Y2O3-180, Y2O3-220, Y2O3-260, and Y2O3-290 samples were revealed to be 4.88 g/cm3, 4.95 g/cm3, 5.0 g/cm3, 4.94 g/cm3, and 4.98 g/cm3, respectively. Regardless of the growth temperatures, the film densities of all the Y2O3 thin films were close to the bulk density (5.03 g/cm3) of Y2O3, supporting the well-crystallized phases even for the films grown at 150 °C in the XRD observation. Similarly, it can explain the similar value (~1.87) of refractive indexes within the ALD temperature window.
An AES depth profile study was also performed to investigate the effect of growth temperature on the compositions and impurities of the Y2O3 thin films, as shown in Figure 3. For this, ALD-Y2O3 thin films grown at 150 and 290 °C were selected. As shown in Figure 3a,b, it showed that a stoichiometric Y2O3 thin film was successfully formed by ALD. Also, carbon impurities were below the detection limit of AES, which implies the ligands of Y(MeCp)2(iPr-nPrAMD) precursor were completely removed even at a low temperature of 150 °C by an optimized ALD process. Thus, ALD-Y2O3 thin film resulted in high purity and high density, analogous to the Y2O3 bulk, and is a promising film for various applications including a protective coating against CF4 based plasma.
The plasma etching rate of ALD-Y2O3 thin films prepared at growth temperatures ranging from 150 to 290 °C was investigated using RIE at a plasma power of 400 W and a pressure of 50 mTorr, employing a mixed gas of Ar (50 sccm), CF4 (45 sccm), and O2 (5 sccm), as shown in Figure 4. Among the etching gases used, Ar induces only physical etching due to its chemical stability. CF4 is generally known to influence both chemical and physical etching, while O2 is employed to remove carbon from the film or Si by forming CO2 gas, as carbon is generated by the decomposition of CF4. For the plasma etching process, ~30 nm thick-Y2O3 thin films were used. And, Al2O3 thin film with a thickness of ~110 nm was prepared at 150 °C by ALD in order to compare its etching behavior with that of ALD-Y2O3 thin films. After performing the RIE process for 15 min, the plasma etching rate was calculated based on the thickness difference of the films before and after RIE. As shown in Figure 4, Y2O3 thin films prepared at 150 °C exhibited a low plasma etching rate of 0.77 nm/min, while Al2O3 thin films prepared at the same temperature exhibited a very high plasma etching rate of 4.6 nm/min, which is approximately 6 times higher than that of the Y2O3 thin films.
The disparity in the plasma etching rate between the two materials indicates that the Y2O3 thin film exhibits greater resistance to Ar/CF4/O2 plasma compared to the Al2O3 thin film. Also, it is noteworthy that the growth temperature had minimal impact on the dry etching gas conditions for Y2O3 thin films. This is attributed to the high purity and high density of ALD-Y2O3 thin films using Y(MeCp)2(iPr-nPrAMD) precursor and H2O, regardless of the growth temperature.
These results can be explained by the fluorination plasma chemical etching reactions of Y2O3 and Al2O3 thin films:
Y2O3 (s) + 3/2 CF4 (g) → 2 YF3 (s) + 3/2 CO2 (g)
Al2O3 (s) + 3/2 CF4 (g) → 2 AlF3 (s) + 3/2 CO2 (g)
According to the fluorination reaction formulas described above, Y2O3 and Al2O3 thin films are generally fluorinated from the surface, forming YF3 and AlF3 surface layers, while CO2 is removed by a vacuum system. During this process, YF3 and AlF3 surface layers are spontaneously formed due to the negative values of the standard enthalpy of formation and the standard Gibbs free energy of fluorination reactions [33]. In our case, therefore, similar YF3 and AlF3 thin films could be formed on Y2O3 and Al2O3 thin films, when Y2O3 and Al2O3 thin films were exposed to Ar/CF4/O2 plasma during the RIE. The formation of a YF3 surface layer can reduce the erosion rate of Y2O3 thin films due to its high boiling temperature (2230 °C), while the AlF3 surface layer can similarly reduce the erosion rate of Al2O3. However, the lower boiling temperature of AlF3 (1291 °C) indicates that YF3 is less prone to evaporation. Moreover, it was reported that the physical etching rate of AlF3 is much faster than YF3, while the physical etching rates are almost similar between Al2O3 and Y2O3 [34]. Therefore, the high difference in the plasma etching rate of Y2O3 and Al2O3 can be explained by a continuous surface fluorination reaction and its physical etching rates. Consequently, Y2O3 experiences less plasma erosion than Al2O3, suggesting that ALD-Y2O3 using Y(MeCp)2(iPr-nPrAMD) precursor and H2O is a promising protective coating compared to ALD-Al2O3.

4. Conclusions

The ALD-Y2O3 process using the Y(MeCp)2(iPr-nPrAMD) precursor and H2O as the reactant demonstrated a wide ALD temperature window from 150 to 290 °C, with a consistent growth rate and refractive index. Additionally, ALD Y2O3 thin films exhibited a typical cubic polycrystalline phase, regardless of the growth temperature, primarily due to their high purity and density, similar to bulk Y2O3. The plasma etching rate of ALD-Y2O3 thin films grown at various temperatures was investigated using RIE at a plasma power of 400 W with a mixed gas of Ar/CF4/O2. For comparison, the plasma etching rate of ALD-Al2O3 thin films was also studied. When a growth temperature of 150 °C was applied to both ALD-Al2O3 and Y2O3 thin films, ALD-Y2O3 exhibited a significantly lower plasma etching rate compared to ALD-Al2O3. The difference in plasma etching rates between Y2O3 and Al2O3 was explained in detail based on continuous surface fluorination reactions and physical etching rates. Furthermore, it was observed that the growth temperature had minimal impact on the dry etching behavior of Y2O3 thin films. Based on these results, ALD-Y2O3 using the Y(MeCp)2(iPr-nPrAMD) precursor and H2O can be considered a promising protective coating for semiconductor components, outperforming Al2O3 in this regard.

Author Contributions

Conceptualization, H.K. and S.K.; methodology, S.K.; investigation, S.L.; data curation, S.L.; writing—original draft preparation, S.L.; writing—review and editing, S.K.; visualization, S.L.; supervision, S.K.; project administration, S.K.; funding acquisition, S.K. All authors have read and agreed to the published version of the manuscript.

Funding

This work was supported by the Korea Planning & Evaluation Institute of Industrial Technology (KEIT) grants funded by Ministry of Trade, Industry & Energy (MOTIE, Korea) (Technology Innovation Program, G01004064821 and K_G012001147505).

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

Data are contained within the article.

Conflicts of Interest

Hyunchang Kim is employed by iChems Co., Ltd. The remaining authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest.

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Figure 1. Growth rate of ALD-Y2O3 thin films depending on (a) the Y(MeCp)2(iPr-nPrAMD) pulse time and (b) H2O pulse time at a growth temperature of 260 °C. (c) thickness of ALD-Y2O3 thin films as a function of the number of ALD cycles at a growth temperature of 260 °C. And, (d) growth rate and refractive index of ALD-Y2O3 thin films depending on the growth temperature from 150 to 290 °C.
Figure 1. Growth rate of ALD-Y2O3 thin films depending on (a) the Y(MeCp)2(iPr-nPrAMD) pulse time and (b) H2O pulse time at a growth temperature of 260 °C. (c) thickness of ALD-Y2O3 thin films as a function of the number of ALD cycles at a growth temperature of 260 °C. And, (d) growth rate and refractive index of ALD-Y2O3 thin films depending on the growth temperature from 150 to 290 °C.
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Figure 2. (a) XRD and (b) XRR patterns of ALD-Y2O3 thin films depending on the deposition temperatures from 150 to 290 °C.
Figure 2. (a) XRD and (b) XRR patterns of ALD-Y2O3 thin films depending on the deposition temperatures from 150 to 290 °C.
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Figure 3. AES depth profiles of ALD-Y2O3 thin films prepared at a deposition temperature of (a) 150 °C and (b) 290 °C.
Figure 3. AES depth profiles of ALD-Y2O3 thin films prepared at a deposition temperature of (a) 150 °C and (b) 290 °C.
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Figure 4. Plasma etching rate of ALD-Al2O3 and ALD-Y2O3 thin films, which was calculated based on the thickness difference of the films before and after RIE for 15 min.
Figure 4. Plasma etching rate of ALD-Al2O3 and ALD-Y2O3 thin films, which was calculated based on the thickness difference of the films before and after RIE for 15 min.
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MDPI and ACS Style

Lee, S.; Kim, H.; Kwon, S. Atomic Layer Deposition of Y2O3 Thin Films Using Y(MeCp)2(iPr-nPrAMD) Precursor and H2O, and Their Erosion Resistance in CF4-Based Plasma. Coatings 2025, 15, 22. https://doi.org/10.3390/coatings15010022

AMA Style

Lee S, Kim H, Kwon S. Atomic Layer Deposition of Y2O3 Thin Films Using Y(MeCp)2(iPr-nPrAMD) Precursor and H2O, and Their Erosion Resistance in CF4-Based Plasma. Coatings. 2025; 15(1):22. https://doi.org/10.3390/coatings15010022

Chicago/Turabian Style

Lee, Seong, Hyunchang Kim, and Sehun Kwon. 2025. "Atomic Layer Deposition of Y2O3 Thin Films Using Y(MeCp)2(iPr-nPrAMD) Precursor and H2O, and Their Erosion Resistance in CF4-Based Plasma" Coatings 15, no. 1: 22. https://doi.org/10.3390/coatings15010022

APA Style

Lee, S., Kim, H., & Kwon, S. (2025). Atomic Layer Deposition of Y2O3 Thin Films Using Y(MeCp)2(iPr-nPrAMD) Precursor and H2O, and Their Erosion Resistance in CF4-Based Plasma. Coatings, 15(1), 22. https://doi.org/10.3390/coatings15010022

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