Low-Temperature Organometallic Chemical Vapor Deposition of Transition Metals

1988 ◽  
Vol 131 ◽  
Author(s):  
Herbert D. Kaesz ◽  
R. Stanley Williams ◽  
Robert F. Hicks ◽  
Yea-Jer Arthur Chen ◽  
Ziling Xue ◽  
...  

ABSTRACTA variety of transition-metal films have been grown by organometallic chemical vapor deposition (OMCVD) at low temperatures using hydrocarbon or hydrido-carbonyl metal complexes as precursors. The vapors of the metal complexes are transported with argon as the carrier gas, adding H2 to the stream shortly before contact with a heated substrate.High-purity platinum films have been grown using (η5−C5H5)PtMe3 [1] or (η5−CH3C5H4)PtMe3 [2] at substrate temperatures of 180°C or 120°C, respectively. The incorporation of a methyl substituent on the cyclopentadienyl ligand decreases the melting point of the organoplatinum complex from 106°C [1] to 30°C [2] and increases the vapor pressure substantially. Film deposition also occurs at a lower substrate temperature. Analyses by X-ray diffraction (XRD), Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS) indicate that the films are well crystallized and do not contain any observable impurities after sputter cleaning.The substrate temperatures for the first appearance of other transition-metal films from organometallic precursors are as follows (°C): Rh(η3−C3H5)3 (120/Si), Ir(η3-C3H5)3 (100/Si), HRe(CO)5 (130/Si) and Ni(η5−CH3C5H4)2 (190/glass, 280/Si). These films are essentially amorphous and contain trace oxygen impurities (< 2%), except for the Re film, which was 10% oxygen and 20%carbon.

2005 ◽  
Vol 862 ◽  
Author(s):  
Kanji Yasui ◽  
Jyunpei Eto ◽  
Yuzuru Narita ◽  
Masasuke Takata ◽  
Tadashi Akahane

AbstractThe crystal growth of SiC films on (100) Si and thermally oxidized Si (SiO2/Si) substrates by hot-mesh chemical vapor deposition (HMCVD) using monomethylsilane as a source gas was investigated. A mesh structure of hot tungsten (W) wire was used as a catalyzer. At substrate temperatures above 750°C and at a mesh temperature of 1600°C, 3C-SiC crystal was epitaxially grown on (100) Si substrates. From the X-ray rocking curve spectra of the (311) peak, SiC was also epitaxially grown in the substrate plane. On the basis of the X-ray diffraction (XRD) measurements, on the other hand, the growth of (100)-oriented 3C-SiC films on SiO2/Si substrates was determined to be achieved at substrate temperatures of 750-800°C, while polycrystalline SiC films, at substrate temperatures above 850°C. From the dependence of growth rate on substrate temperature and W-mesh temperature, the growth mechanism of SiC crystal by HMCVD was discussed.


PLoS ONE ◽  
2021 ◽  
Vol 16 (10) ◽  
pp. e0259216
Author(s):  
Satoru Yoshimura ◽  
Satoshi Sugimoto ◽  
Takae Takeuchi ◽  
Kensuke Murai ◽  
Masato Kiuchi

We proposed an experimental methodology for producing films on substrates with an ion beam induced chemical vapor deposition (IBICVD) method using hexamethyldisilazane (HMDS) as a source material. In this study, both HMDS and ion beam were simultaneously injected onto a Si substrate. We selected Ar+ and N+ as the ion beam. The energy of the ion beam was 101 eV. Temperature of the Si substrate was set at 540 °C. After the experiments, films were found to be deposited on the substrates. The films were then analyzed by Fourier transform infrared (FTIR) spectroscopy, stylus profilometer, X-ray diffraction, atomic force microscopy, and X-ray photoelectron spectroscopy (XPS). The FTIR and XPS results showed that silicon carbide films containing small amount of nitrogen were formed when Ar+ ions were injected in conjunction with HMDS. On the other hand, in the cases of N+ ion beam irradiation, silicon nitride films involving small amount of carbon were formed. It was noted that no film deposition was observed when HMDS alone was supplied to the substrates without any ion beam injections.


MRS Advances ◽  
2020 ◽  
Vol 5 (31-32) ◽  
pp. 1681-1685
Author(s):  
Yoshiyuki Seki ◽  
Yutaka Sawada ◽  
Hiroshi Funakubo ◽  
Kazuhisa Kawano ◽  
Noriaki Oshima

AbstractMetal Ir films were prepared by spray chemical vapor deposition (CVD) in air from an Ir precursor, (1,3-cyclohexadiene)(ethylcyclopentadienyl)iridium, Ir(EtCp)(CHD). Film deposition was ascertained at 270–430°C on a SiO2/Si substrate and the deposition rate increased with the deposition temperature but was saturated above 330°C. The obtained films consisted of Ir metal without any iridium oxide impurity irrespective of the deposition temperature. Films tended to orient to (111) with increasing deposition temperature. Resistivity of these Ir films decreased with increasing film thickness and reached to values on the order of 10-6 Ω・cm, which was the same order of the values for bulk Ir metal. Good step coverage was observed for the Ir metal films deposited at 270°C and 330°C. This shows that the simple spray CVD process in air is a good candidate for depositing Ir metal films with good conductivity and step coverage.


1986 ◽  
Vol 1 (3) ◽  
pp. 420-424 ◽  
Author(s):  
T.R. Jervis ◽  
L.R. Newkirk

Dielectric breakdown of gas mixtures can be used to deposit thin films by chemical vapor deposition with appropriate control of flow and pressure conditions to suppress gas-phase nucleation and particle formation. Using a pulsed CO2 laser operating at 10.6 μ where there is no significant resonant absorption in any of the source gases, homogeneous films from several gas-phase precursors have been sucessfully deposited by gas-phase laser pyrolysis. Nickel and molybdenum from the respective carbonyls representing decomposition chemistry and tungsten from the hexafluoride representing reduction chemistry have been demonstrated. In each case the gas precursor is buffered with argon to reduce the partial pressure of the reactants and to induce breakdown. Films have been characterized by Auger electron spectroscopy, x-ray diffraction, transmission electron microscopy, pull tests, and resistivity measurements. The highest quality films have resulted from the nickel depositions. Detailed x-ray diffraction analysis of these films yields a very small domain size consistent with the low temperature of the substrate and the formation of metastable nickel carbide. Transmission electron microscopy supports this analysis.


2002 ◽  
Vol 716 ◽  
Author(s):  
J.F. Conley ◽  
Y. Ono ◽  
D.J. Tweet ◽  
W. Zhuang ◽  
R. Solanki

AbstractHfO2 films have been deposited using anhydrous hafnium nitrate (Hf(NO3)4) as a precursor for atomic layer chemical vapor deposition (ALCVD). These films have been characterized using x-ray diffraction, x-ray reflectivity, atomic force microscopy, current vs. voltage, and capacitance vs. voltage measurements. An advantage of this precursor is that it produces smooth and uniform initiation of film deposition on H-terminated silicon surfaces. As deposited films remained amorphous at temperatures below ∼700°C. The effective dielectric constant of the film (neglecting quantum effects) for films less than ∼15 nm thick, was in the range of kfilm ∼ 10-11, while the HfO2 layer value was estimated to be kHfO2 ∼ 12-14. The lower than expected dielectric constant of the film stack is due in part to the presence of an interfacial layer such as HfSiOx. Excess oxygen may play a role in the lower than expected dielectric constant of the HfO2 layer. Breakdown of HfO2 films occurred at ∼5-7 MV/cm. Leakage current was lower than that of SiO2 films of comparable equivalent thickness.


1994 ◽  
Vol 363 ◽  
Author(s):  
Chongying Xu ◽  
Mark J. Hampden-Smith ◽  
Toivo T. Kodas

AbstractThe chemical vapor deposition (CVD) of Cu-Ag and Cu-Pd alloys using aerosol precursor delivery over a range of preheating temperatures, 70∼80 °C and substrate temperatures, 250∼300 °C is described. The precursors used include Cu(hfac)2, (hfac)Ag(Set2) and Pd(hfac)2 dissolved in toluene and 10% H2 in Ar as carrier gas. The films were characterized by SEM, EDS and X-ray diffraction (XRD). The X-ray diffraction results showed the Cu/Ag films were composed of α-and β-phases of Cu-Ag alloys, the Cu/Pd films were Cu-Pd alloy, solid solutions, under these conditions. Compositional variation studies in Cu-Pd and Pd-Ag alloy systems were also conducted by mixing Cu(hfac)2/Pd(hfac)2 and (hfac)Ag(SEt2)/Pd(hfac)2 in toluene solution in different ratios. The films were characterized by X-ray diffraction and the results showed the composition of films was affected by the solution stoichiometry.


2017 ◽  
Vol 8 ◽  
pp. 1266-1276 ◽  
Author(s):  
Yuriy Y Smolin ◽  
Masoud Soroush ◽  
Kenneth K S Lau

Polyaniline (PANI) is synthesized via oxidative chemical vapor deposition (oCVD) using aniline as monomer and antimony pentachloride as oxidant. Microscopy and spectroscopy indicate that oCVD processing conditions influence the PANI film chemistry, oxidation, and doping level. Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and X-ray photoelectron spectroscopy (XPS) indicate that a substrate temperature of 90 °C is needed to minimize the formation of oligomers during polymerization. Lower substrate temperatures, such as 25 °C, lead to a film that mostly includes oligomers. Increasing the oxidant flowrate to nearly match the monomer flowrate favors the deposition of PANI in the emeraldine state, and varying the oxidant flowrate can directly influence the oxidation state of PANI. Changing the reactor pressure from 700 to 35 mTorr does not have a significant effect on the deposited film chemistry, indicating that the oCVD PANI process is not concentration dependent. This work shows that oCVD can be used for depositing PANI and for effectively controlling the chemical state of PANI.


1993 ◽  
Vol 327 ◽  
Author(s):  
Matthew D. Healy ◽  
David C. Smith ◽  
Rodrigo R. Rubiano ◽  
Robert W. Springer ◽  
John E. Parmeter

AbstractThe organometallic chemical vapor deposition (OMCVD) of transition metal carbides (M = Ti, Zr, Hf, and Cr) from tetraneopentyl-metal precursors has been carried out. Metal carbides can be deposited on Si, A120 3, and stainless steel substrates from M[CH 2C(CH3)3]4 at temperatures in the range of 300 to 750 "C and pressures from 10-2 to 10-4 Torr. Thin films have also been grown using a carrier gas (Ar, H2). The effects of variation of the metal center, deposition conditions, and reactor design on the resulting material have been examined by SEM, XPS, XRD, ERD and AES. Hydrocarbon fragments generated in the deposition chamber have been studied by in-situ mass spectrometry. Complimentary studies examining the UHV surface decomposition of Zr[CH2C(CH3)3]4 have allowed for a better understanding of the mechanism leading to film growth.


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