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Atmospheric Pressure Chemical Vapor Deposition of Tin from Tetrakis(Dimethylamido)Titanium and Ammonia Joshua N

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Atmospheric Pressure Chemical Vapor Deposition of Tin from Tetrakis(Dimethylamido)Titanium and Ammonia Joshua N Journal of MATERIALS RESEARCH Welcome Comments Help Atmospheric pressure chemical vapor deposition of TiN from tetrakis(dimethylamido)titanium and ammonia Joshua N. Musher and Roy G. Gordon Department of Chemistry, Harvard University, Cambridge, Massachusetts 02138 (Received 15 December 1994; accepted 28 October 1995) Near stoichiometric titanium nitride (TiN) was deposited from tetrakis(dimethylamido)titanium (TDMAT) and ammonia using atmospheric pressure chemical vapor deposition. Experiments were conducted in a belt furnace; static experiments provided kinetic data and continuous operation uniformly coated 150-mm substrates. Growth rate, stoichiometry, and resistivity are examined as functions of deposition temperature (190–420 ±C), ammonia flow relative to TDMAT (0–30), and total gas-flow rate (residence time 0.3–0.6 s). Films were characterized by sheet resistance measurements, Rutherford Backscattering Spectrometry, and X-Ray Photoelectron Spectrometry. Films deposited without ammonia were substoichiometric (NyTi , 0.6–0.75), contained high levels of carbon (CyTi ­ 0.25–0.40) and oxygen (OyTi ­ 0.6–0.9), and grew slowly. Small amounts of ammonia (NH3yTDMAT > 1) brought impurity levels down to CyTi , 0.1 and OyTi ­ 0.3–0.5. Ammonia increased the growth rates by a factor of 4–12 at temperatures below 400 ±C. Films 500 A˚ thick had resistivities as low as 1600 mV-cm when deposited at 280 ±C and 1500 mV-cm when deposited at 370 ±C. Scanning electron micrographs indicate a smooth surface and poor step coverage for films deposited with high ammonia concentrations. I. INTRODUCTION Three problems are associated with this process: Nitrides are technologically important materials be- chlorine contamination, HCl by-products, and high sub- cause of their hardness, stability at high temperatures, strate temperatures. Incorporation of chlorine into the chemical inertness, and electrical and optical proper- film is detrimental to film properties, such as conduc- ties. Transition metal nitrides comprise an important tivity, and causes delamination from steel substrates. subclass, with applications in wear-resistant, electronic, Chlorine corrosion of aluminum over layers is possible. and optical coatings. Titanium nitride, in particular, is Ammonium chloride by-products form particulates and used for tool coating, solar-control films, and micro- can cause problems with vacuum pumps and exhaust electronic applications. Optically similar to gold, it is systems. Lastly, the temperature is still too high for harder than alumina and thermally stable to 3000 ±C. metallized wafers and plastics. TiN is chemically stable with respect to most etching The use of low-temperature physical vapor deposi- solutions, has a low resistivity, and provides an excel- tion (PVD) techniques allowed the deposition of TiN lent diffusion barrier against metals. These properties on metallized wafers. Reactive sputtering of titanium make TiN useful in integrated circuit manufacturing, in a nitrogen atmosphere forms TiN with only a slight in which TiN is used as a glue layer for tungsten dependence on substrate temperature. This process al- lows for film growth at room temperature.2 More often, deposition, and as a diffusion barrier between silicon and ± 3 metals. substrate temperatures of 300 C are used, low enough Early chemical vapor deposition (CVD) techniques for metallized silicon wafers. Deposition methods are severely tested when coated tools by the reaction of TiCl4 1 N2 1 H2 at temperatures above 1000 ±C. Many substrates cannot be microelectronic circuit dimensions decrease and aspect subjected to such high temperatures. Kurtz and Gordon1 ratio (depthywidth) of interconnect vias increase. PVD demonstrated that the deposition temperature could be is a line-of-sight process, with sticking coefficients of lowered by introducing preheated ammonia into the gas highly reactive ions close to 1; deposition occurs on stream. Reaction (1) allows some less thermally sensitive the first encountered surface. Material that enters a substrates to be coated, such as glass or unmetallized narrow via will probably hit a wall before reaching silicon wafers. the bottom. Voids form as sidewalls thicken and cause failure of devices. A diffusion barrier must coat the 500–700± 6TiCl4 1 8NH3 °°°°°°°°! 6TiN 1 24HCl 1 N2 entire exposed surface, including hard-to-reach corners. (1) Precise control of incident material directionality can J. Mater. Res., Vol. 11, No. 4, Apr 1996 1996 Materials Research Society 989 J. N. Musher et al.: Atmospheric pressure CVD of TiN from tetrakis(dimethylamido)titanium and ammonia extend the usefulness of PVD processes. Collimators II. EXPERIMENTAL 4 allow the use of sputtering for 0.35 mm technologies Films were deposited in a prototype belt furnace at somewhat reduced growth rates. from the Watkins-Johnson Company, model WJ-956. PVD barriers fail at lower temperatures than their The 35-cm wide muffle would accommodate a 30-cm CVD counterparts because of their columnar structure. wide substrate without edge effects. An Inconel mesh A PVD barrier will fail at 350 ±CinanAuyTiNySi 5 belt, heated from below, delivered substrates to the depo- metallization scheme, while a CVD barrier can tolerate ± ± 6 sition zone at 190–480 C. Reactant gases were injected 550 C. Raaijmakers and co-workers showed that a into the deposition zone approximately 3 mm above the PVD barrier needs to be twice as thick as a CVD barrier ± 7 substrate. The injector head was cooled to 110–130 C, to provide the same degree of protection. providing a cold-wall reactor configuration. A series of Despite the higher temperatures required, CVD of- high-volume nitrogen curtains and exhausts prevented fers two distinct advantages over PVD for depositing laboratory air from reaching the deposition zone. thin films. First, process parameters are less sensitive to Precursor gases were injected in an ABA configu- fluctuations in CVD. During sputtering, a small shift in ration along lines perpendicular to the direction of the nitrogen partial pressure can result in a phase transition 2,8 motion of the belt (Fig. 1). Diluted ammonia passed in the deposited film. Reaction (1) deposits near stoi- through the center line (B) and diluted TDMAT vapor chiometric TiN (NyTi ­ 0.95–1.05) under a wide range 9 through the outer two lines. In the reverse configura- of conditions. Second, step coverage provided by CVD tion, only nonconductive orange films could be made. films is superior to that provided by PVD films. Laminar flow conditions were used (Reynolds number The TiCl4yNH3 reaction described earlier is reason- 1 , 30), though some turbulent mixing occurred near the ably robust to process irregularities and yields confor- inlets when dilution flows were high. Reactant flows mal films. A more reactive set of precursors would lower were controlled by mass-flow controllers (Tylan models the deposition temperature. Use of methyl-hydrazine in FC-260 and 2261, 61% stability) and by pressure place of ammonia9 can reduce the reaction temperature ± drops across small diameter tubing (1y8 inch o.d., 0.02 by 200 C, but the chlorine difficulties remain. inch i.d., from PhaseSep). Other nitrogen flows were An alternative is to replace TiCl4 with a more 10 controlled with rotameters from Porter Instruments. reactive dialkylamido complex. Bradley and Thomas TDMAT (99.999% purity, Schumacher corporation) demonstrated that transamination reactions of various was placed in a stainless steel bubbler heated with heat- amines with titanium dialkylamides [(2) and (3)] occur in ing tapes controlled by a Watlow 965 time proportional solution, which suggested that the reactions may occur temperature controller. A type K thermocouple placed in the in a well monitored the bubbler temperature of 80 ±C. Precursor vapor pressures were calculated according to M 2 NR 1 HNR0 °! M 2 NR0 1 HNR (2) 2 2 2 2 Eq. (4).14 With a temperature stability of 61 ±C, the vapor pressure (3.36 Torr) was kept constant at 65%. Carrier-gas flow rates were varied to change precursor MsNMe d 1 2RNH °! f M s ­ NRd g 1 4HNMe 2 4 2 2 2 flow rates; unless otherwise noted, the carrier flow was (3) 1000 standard cubic centimeters per minute (sccm). 11–13 The carrier gas was diluted with 4.4–14 standard liters gas phase with ammonia. Fix et al. demonstrated per minute (slm) of purified nitrogen after exiting the the potential of a low-temperature APCVD process bubbler. Delivery lines were heated to 100 ±C to prevent to deposit TiN from tetrakis(dimethylamido)titanium precursor condensation. [Ti(N(CH3)2)4 or TDMAT] and ammonia. Near- stoichiometric TiN was grown at 1000 A˚ymin at 2850 ± log P ­ 2 1 8.60 (4) 200–400 C, with low levels of oxygen and carbon TDMAT TsKd impurities. In addition to making lower deposition µ ∂ temperatures possible, chlorine and related corrosion Nitrogen was the boil-off from an in-house tank problems are avoided. of liquid nitrogen. Purity levels were comparable to APCVD, rather than LPCVD, was chosen because purchased UHP nitrogen (,0.5 ppm O2,H2O) as meas- of the inherent advantages of an atmospheric pressure ured by a Delta F Trace Oxygen Analyzer (Model system over a low pressure system. Atmospheric pres- FA30111SA) and Meeco Model W Moisture Analyzer. sure processes avoid costly vacuum equipment and allow Nitrogen delivered to the deposition zone was purified higher throughputs with a belt furnace. The present study using Oxiclear and Nanochem purifiers. Long purge was undertaken to examine the reaction kinetics of the times were required to reach the 5 ppb levels claimed TDMAT 1 NH3 system and determine the manufactur- achievable by the manufacturers. In practice, impu- ing feasibility of the process. rity concentrations were reduced to the 100 ppb level. 990 J. Mater. Res., Vol. 11, No. 4, Apr 1996 J. N. Musher et al.: Atmospheric pressure CVD of TiN from tetrakis(dimethylamido)titanium and ammonia ments. Crystal silicon substrates (p-type, k100l) from Silicon Sense were used for glancing angle and chan- neling RBS measurements.
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