Ultra-High Purity Hydrazine Delivery for Low Temperature Metal Nitride ALD

Álvarez, Daniel; Spiegelman, Jeffrey; Holmes, Russell J.; Andachi, Keisuke; Raynor, Mark W.; Shimizu, Hank

doi:10.1149/07705.0219ecst

Cited by 3 publications

(3 citation statements)

References 4 publications

(4 reference statements)

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“…Samples were exposed to 200 ms pulses of TiCl 4 (Hi-k grade, Air Products) and 13 s pulses of N 2 H 4 in a hot wall ALD reactor on the UHV cluster at approximately 1 mbar and 20 sccm between 523 K (250 °C) and 623 K (350 °C) for multiple cycles to grow a film. Anhydrous N 2 H 4 in a non-volatile solvent was purchased from RASIRC Technologies pre-filled in a BRUTE style ALD source bottle to minimize safety hazards [6,7]. Hydrazine is a base and strong reducing agent that is commonly used as a rocket propellant.…”

Section: Methodsmentioning

confidence: 99%

“…An alternative is to use a more reactive N precursor such as hydrazine, dimethylhydrazine, or NH 3 activated using a plasma. Hydrazine (N 2 H 4 ) has recently been used as a substitute for NH 3 in ALD processes to grow TiN and TaN [6,7]. Hydrazine is generally more reactive than NH 3 and could reduce the number of Ti-Cl bonds and the Cl concentration in the film in addition to lowering the thermal budget of the process.…”

Section: Introductionmentioning

confidence: 99%

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Atomic Layer Deposition of TiN below 600 K Using N2H4

Hinckley

Muscat²

2018

SSP

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Atomic layer deposition (ALD) was used to grow titanium nitride (TiN) on SiO2with TiCl4and N2H4. X-ray photoelectron spectroscopy (XPS) and ellipsometry were used to characterize film growth. A hydrogen-terminated Si (Si-H) surface was used as a reference to understand the reaction steps on SPM cleaned SiO2. The growth rate of TiN at 573 K doubled on Si-H compared to SiO2because of the formation of Si-N bonds. When the temperature was raised to 623 K, O transferred from Ti to Si to form Si-N when exposed to N2H4. Oxygen and Ti could be removed at 623 K by TiCl4producing volatile species. The added surface reactions reduce the Cl in the film below detection limits.

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Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Atomic Layer Deposition of TiN below 600 K Using N2H4

Hinckley

Muscat²

2018

SSP

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“…Usually, NH 3 is used as N-source for thermal ALD process [20][21][22][23] . Hydrazine is presented as highly reactive alternative but it is also highly hazardous 24 .…”

Section: Introductionmentioning

confidence: 99%

Conductive TiN thin films grown by plasma-enhanced atomic layer deposition: Effects of N-sources and thermal treatments

Badie

Tissot

Sciacca

et al. 2023

Journal of Vacuum Science &Amp; Technology A

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This work consists of optimizing TiN plasma-enhanced atomic layer deposition using two different N-sources: NH[Formula: see text] and N[Formula: see text]. In addition to maximizing the growth per cycle (GPC) and to shorten the deposition duration, comprehensive in situ and ex situ physicochemical characterizations give valuable information about the influence of the N-source nature, their dilution in Ar, and the plasma power on layer’s final properties. N[Formula: see text] and NH[Formula: see text] dilutions within Ar are extensively investigated since they are critical to decreasing the mean free path ([Formula: see text]) of plasma-activated species. A 1:1 gas ratio for the N-sources:Ar mixture associated with low flows (20 sccm) is optimal values for achieving highest GPCs (0.8 Å/cycle). Due to lower reactivity and shorter [Formula: see text] of the excited species, N[Formula: see text] plasma is more sensitive to power and generator-to-sample distance, and this contributes to lower conformality than with NH[Formula: see text] plasma. The resistivity of the initial amorphous films was high ([Formula: see text] cm) and was significantly reduced after thermal treatment ([Formula: see text] cm). This demonstrates clearly the beneficial effect of the crystallinity of the film conductivity. Though N[Formula: see text] process appears slightly slower than the NH[Formula: see text] one, it leads to an acceptable film quality. It should be considered since it is nonharmful, and the process could be further improved by using a reactor exhibiting optimized geometry.

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