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Low Temperature Thermal Atomic Layer Deposition of Aluminum Nitride Using Hydrazine As the Nitrogen Source

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Low Temperature Thermal Atomic Layer Deposition of Aluminum Nitride Using Hydrazine As the Nitrogen Source materials Article Low Temperature Thermal Atomic Layer Deposition of Aluminum Nitride Using Hydrazine as the Nitrogen Source Yong Chan Jung 1, Su Min Hwang 1, Dan N. Le 1, Aswin L. N. Kondusamy 1, Jaidah Mohan 1, Sang Woo Kim 1,2, Jin Hyun Kim 1,2, Antonio T. Lucero 1, Arul Ravichandran 1 , Harrison Sejoon Kim 1 , Si Joon Kim 3 , Rino Choi 2, Jinho Ahn 4, Daniel Alvarez 5, Jeff Spiegelman 5 and Jiyoung Kim 1,* 1 Department of Materials Science and Engineering, The University of Texas at Dallas, 800 West Campbell Road, Richardson, TX 75080, USA; [email protected] (Y.C.J.); [email protected] (S.M.H.); [email protected] (D.N.L.); [email protected] (A.L.N.K.); [email protected] (J.M.); [email protected] (S.W.K.); [email protected] (J.H.K.); [email protected] (A.T.L.); [email protected] (A.R.); [email protected] (H.S.K.) 2 Department of Materials Science and Engineering, Inha University, 100 Inha-ro, Michuhol-gu, Incheon 22212, Korea; [email protected] 3 Department of Electrical and Electronics Engineering, Kangwon National University, 1 Gangwondaehakgil, Chuncheon, Gangwon-do 24341, Korea; [email protected] 4 Division of Materials Science and Engineering, Hanyang University, 222 Wangsimni-ro, Seongdong-gu, Seoul 04763, Korea; [email protected] 5 RASIRC Inc., 7815 Silverton Avenue, San Diego, CA 92126, USA; [email protected] (D.A.); [email protected] (J.S.) * Correspondence: [email protected] Received: 20 June 2020; Accepted: 28 July 2020; Published: 31 July 2020 Abstract: Aluminum nitride (AlN) thin films were grown using thermal atomic layer deposition in the temperature range of 175–350 ◦C. The thin films were deposited using trimethyl aluminum (TMA) and hydrazine (N2H4) as a metal precursor and nitrogen source, respectively. Highly reactive N2H4, compared to its conventionally used counterpart, ammonia (NH3), provides a higher growth per cycle (GPC), which is approximately 2.3 times higher at a deposition temperature of 300 ◦C and, also exhibits a low impurity concentration in as-deposited films. Low temperature AlN films deposited at 225 ◦C with a capping layer had an Al to N composition ratio of 1:1.1, a close to ideal composition ratio, with a low oxygen content (7.5%) while exhibiting a GPC of 0.16 nm/cycle. We suggest that N2H4 as a replacement for NH3 is a good alternative due to its stringent thermal budget. Keywords: atomic layer deposition (ALD); aluminum nitride; hydrazine; trimethyl aluminum (TMA) 1. Introduction Aluminum nitride (AlN) is one of the promising materials for electronic and optoelectronic devices due to its wide band gap structure (6.2 eV), high thermal conductivity (2.85 W/cm K at 300 K), · melting point (2750 ◦C), and large critical electric field (12 MV/cm) [1–3]. Additionally, using a highly thermal conductive material like AlN as a thermal spreader can result in enhanced thermal dissipation, which is highly beneficial in scaled devices [4–6]. These nitride deposition processes should be compatible with the thermal budget of back-end-of-line (BEOL) processes in conventional complementary metal-oxide-semiconductor (CMOS) fabrication. A lower deposition temperature (<300 ◦C) is preferred and conformality over high-aspect ratio structures, commonly found in novel, Materials 2020, 13, 3387; doi:10.3390/ma13153387 www.mdpi.com/journal/materials Materials 2020, 13, 3387 2 of 10 Materials 2020, 13, x FOR PEER REVIEW 2 of 11 complex device structures, is also desirable. Hence, the atomic layer deposition (ALD) technique is a forerunnercomplex device among structures, other deposition is also desirable. techniques Hence, that meets the atomic these specifications layer deposition while (ALD) providing technique excellent is a thicknessforerunner controllability. among other Plasma-enhanced deposition techniques ALD (PEALD)that meets provides these thespecifications plasma radicals while required providing to pushexcellent the boundariesthickness controllability. of ALD reactions Plasma-enhanced towards a lower temperatureALD (PEALD) but provides sensitive substratesthe plasma can radicals suffer fromrequired plasma-induced to push the damage boundaries [7]. PEALD of ALD has reactions a relatively towards poor conformal a lower temperature deposition on but complicated sensitive 3Dsubstrates nano-structures can suffer compared from plasma-induced to thermal ALD. damage [7]. PEALD has a relatively poor conformal depositionCurrently, on complicated AlN ALD using3D nano-structures ammonia (NH compared3) and trimethyl to thermal aluminum ALD. (TMA) results in an incompleteCurrently, reaction AlN at temperaturesALD using ammonia below 300 (NH◦C[83)]. and High-temperature trimethyl aluminum ALD above (TMA) 450 ◦resultsC is required in an inincomplete order to achievereaction a at vigorous temperatures reaction below with 300 methyl °C [8]. groups High-temperature (–CH3) and the ALD complete above removal 450 °C ofis by-productsrequired in order in the to ALD achieve process a vigorous using NHreaction3 and with TMA methyl [8]. One groups way (–CH of circumventing3) and the complete this issue removal is by introducingof by-products a more in the reactive ALD process nitrogen using source NH than3 and NH TMA3. From [8]. thisOne perspective,way of circumventing hydrazine (Nthis2H issue4) can is beby usedintroducing as a replacement a more reactive for NH nitrogen3 as the N–Nsource bond than in NH N23H. From4 (~167 this kJ/ mol)perspective, is weak hydrazine when compared (N2H4) tocan the be N–H used bondas a replacement (~386 kJ/mol) for in NH NH3 as3 [ the9]. TheN–N molecular bond in N structure2H4 (~167 ofkJ/mol) N2H4 isis weak as shown when in compared Figure1 usingto the aN–H ball-stick bond model.(~386 kJ/mol) Safety in was NH a3 key[9]. The concern molecular while structure handling of N 2NH24H,4 but is as the shown newly in available Figure 1 ultra-highusing a ball-stick purity anhydrousmodel. Safety N2 Hwas4 source a key concern is compliant while with handling the safety N2H standard4, but the requirementsnewly available and ultra- has alsohigh demonstrated purity anhydrous the deposition N2H4 source of metalis compliant nitrides with at low thetemperatures safety standard [10 requirements–12]. and has also demonstrated the deposition of metal nitrides at low temperatures [10–12]. Figure 1. Ball stick model of hydrazine (N H ) with N atoms and H atoms. Figure 1. Ball stick model of hydrazine (N22H44) with N atoms and H atoms. Abdulagatov et al. recently demonstrated AlN deposition by thermal ALD using tris(diethylamido) Abdulagatov et al. recently demonstrated AlN deposition by thermal ALD using aluminum (III) (TDEAA) and hydrazine in the deposition temperature range from 150 to 280 C[13]. tris(diethylamido)aluminum (III) (TDEAA) and hydrazine in the deposition temperature range◦ from Growth rates of 1.23, 1.16, and 1.72 Å/cycle were reported at 150, 200, and 280 C, respectively. 150 to 280 °C [13]. Growth rates of 1.23, 1.16, and 1.72 Å/cycle were reported at 150,◦ 200, and 280 °C, The higher growth rate observed at 280 C was mainly attributed to the organo-metallic precursor respectively. The higher growth rate observed◦ at 280 °C was mainly attributed to the organo-metallic decomposition and hence a chemical vapor deposition (CVD) reaction mechanism was suspected for precursor decomposition and hence a chemical vapor deposition (CVD) reaction mechanism was observing such a high growth rate. Additionally, it was also demonstrated that the impurity, such as suspected for observing such a high growth rate. Additionally, it was also demonstrated that the carbon and oxygen content, in nitride film deposited using hydrazine was comparable or lower when impurity, such as carbon and oxygen content, in nitride film deposited using hydrazine was compared to films deposited using NH3 [13,14]. comparable or lower when compared to films deposited using NH3 [13,14]. Previous studies revealed that the growth rate of AlN is less than 0.04 nm/cycle by thermal ALD Previous studies revealed that the growth rate of AlN is less than 0.04 nm/cycle by thermal ALD at temperatures below 400 ◦C using TMA and NH3 [13]. Furthermore, TMA starts to decompose at temperatures below 400 °C using TMA and NH3 [13]. Furthermore, TMA starts to decompose at at higher temperatures (above 377 C) [15] and reduces the film quality of AlN [16,17]. In order to higher temperatures (above 377 °C)◦ [15] and reduces the film quality of AlN [16,17]. In order to deposit high-quality AlN with a reasonable growth rate at low temperatures, it is essential to adopt deposit high-quality AlN with a reasonable growth rate at low temperatures, it is essential to adopt highly reactive precursors, such as hydrazine, into the ALD process. In this paper, we successfully highly reactive precursors, such as hydrazine, into the ALD process. In this paper, we successfully demonstrate AlN films deposition by thermal ALD at low temperatures. Ultra-pure anhydrous N2H4 demonstrate AlN films deposition by thermal ALD at low temperatures. Ultra-pure anhydrous N2H4 and TMA were used to deposit AlN thin films in the temperature range from 175 to 350 C, with the and TMA were used to deposit AlN thin films in the temperature range from 175 to 350 ◦°C, with the feasibility of AlN deposition using an Al ALD precursor of TMA. As a comparison, the growth rate and feasibility of AlN deposition using an Al ALD precursor of TMA. As a comparison, the growth rate surface roughness of AlN films deposited by thermal ALD using TMA and NH3 are also presented. and surface roughness of AlN films deposited by thermal ALD using TMA and NH3 are also presented. 2. Materials and Methods 2.1.
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