Fundamental Studies of TiN Film Growth by CVD From Ti(N M e2)4 and Ammonia

1992 ◽  
Vol 282 ◽  
Author(s):  
J. A. Prybyla ◽  
C.-M. Chiang ◽  
L. H. Dubois
Keyword(s):  
Mass Spectrometry ◽  
Gas Phase ◽  
Film Growth ◽  
High Vacuum ◽  
Reactant Ratio ◽  
Tin Films ◽  
Surface Mobility ◽  
Patterned Wafers ◽  
Elevated Pressures ◽  
Growth Properties

ABSTRACTTiN films were grown by CVD from Ti(N M e2)4 and ammonia using a novel gas delivery system which allowed the sample to be kept in high vacuum while the reactants were mixed at elevated pressures. The object was to study fundamental chemistries and growth properties. We obtained clean (<5% carbon), near-stoichiometric (Ti:N = 1.15+/-0.1) TiN films. The gas phase chemistry was studied by mass spectrometry while the films were analyzed in situ by Auger electron spectroscopy (AES), and then removed for Rutherford backscattering (RBS) analysis. Film quality was studied as a functionof reactant ratio, substrate temperature, and reactant gas pressure. We obtained definitive information on the growth mechanism. Isotopic substituiton experiments establish that a rapid transami-nation reaction occurs in the gas phase. Mass spectrometry experiments indicate that the reactive intermediate is polymeric, consisting of Ti, N, H, arid perhapscarbon. Growth on patterned wafers shows that this intermediate has a high sticking coefficient and a low surface mobility at 300°C. These findings are considered in terms ofthe potential of this precursor system to be used in manufacturing.

Direct STEM ADF imaging of gold on silicon (111)

1989 ◽  
Vol 47 ◽  
pp. 472-473
Author(s):  
P. Xu ◽  
E. J. Kirkland ◽  
J. Silcox
Keyword(s):  
Film Growth ◽  
Heavy Atom ◽  
High Vacuum ◽  
Dark Field ◽  
Thin Metal Film ◽  
Base Pressure ◽  
Ultra High Vacuum ◽  
Specimen Preparation ◽  
Dark Field Imaging ◽  
Wide Range

Many studies of thin metal film growth and the formation of metal-semiconductor contacts have been performed using a wide range of experimental methods. STEM annular dark field imaging could be an important complement since it may allow direct imaging of a single heavy atom on a thin silicon substrate. This would enable studies of the local atomic arrangements and defects in the initial stage of metal silicide formation.Preliminary experiments were performed in an ultra-high vacuum VG HB501A STEM with a base pressure of 1 × 10-10 mbar. An antechamber directly attached to the microscope for specimen preparation has a base pressure of 2×l0-10 mbar. A thin single crystal membrane was fabricated by anodic etching and subsequent reactive etching. The specimen was cleaned by the Shiraki method and had a very thin oxide layer left on the surface. 5 Å of gold was deposited on the specimen at room temperature from a tungsten filament coil monitored by a quartz crystal monitor.

Modifications of a JEOL 2000EX TEM for insSitu surface studies

1993 ◽  
Vol 51 ◽  
pp. 640-641
Author(s):  
Michael T. Marshall ◽  
Xianghong Tong ◽  
J. Murray Gibson
Keyword(s):  
Electron Diffraction ◽  
Surface Science ◽  
Film Growth ◽  
High Vacuum ◽  
High Energy ◽  
Energy Electron ◽  
Ultra High Vacuum ◽  
Transmission Electron ◽  
Fundamental Insight

We have modified a JEOL 2000EX Transmission Electron Microscope (TEM) to allow in-situ ultra-high vacuum (UHV) surface science experiments as well as transmission electron diffraction and imaging. Our goal is to support research in the areas of in-situ film growth, oxidation, and etching on semiconducter surfaces and, hence, gain fundamental insight of the structural components involved with these processes. The large volume chamber needed for such experiments limits the resolution to about 30 Å, primarily due to electron optics. Figure 1 shows the standard JEOL 2000EX TEM. The UHV chamber in figure 2 replaces the specimen area of the TEM, as shown in figure 3. The chamber is outfitted with Low Energy Electron Diffraction (LEED), Auger Electron Spectroscopy (AES), Residual Gas Analyzer (RGA), gas dosing, and evaporation sources. Reflection Electron Microscopy (REM) is also possible. This instrument is referred to as SHEBA (Surface High-energy Electron Beam Apparatus).The UHV chamber measures 800 mm in diameter and 400 mm in height. JEOL provided adapter flanges for the column.

Studies of Ge/Si(100) and Observation of Atomic Steps on Si(100) using Biassed Secondary Electron Imaging in a UHV STEM

1990 ◽  
Vol 48 (1) ◽  
pp. 308-309
Author(s):  
Mohan Krishnamurthy ◽  
Jeff S. Drucker ◽  
John A. Venablest
Keyword(s):  
Secondary Electron ◽  
Critical Thickness ◽  
Surface Defects ◽  
Film Growth ◽  
Growth Parameters ◽  
High Vacuum ◽  
Ultra High Vacuum ◽  
Surface Steps ◽  
Epitaxial Crystal Growth ◽  
Electron Imaging

Secondary Electron Imaging (SEI) has become a useful mode of studying surfaces in SEM[1] and STEM[2,3] instruments. Samples have been biassed (b-SEI) to provide increased sensitivity to topographic and thin film deposits in ultra high vacuum (UHV)-SEM[1,4]; but this has not generally been done in previous STEM studies. The recently developed UHV-STEM ( codenamed MIDAS) at ASU has efficient collection of secondary electrons using a 'parallelizer' and full sample preparation system[5]. Here we report in-situ deposition and annealing studies on the Ge/Si(100) epitaxial system, and the observation of surface steps on vicinal Si(100) using b-SEI under UHV conditions in MIDAS.Epitaxial crystal growth has previously been studied using SEM and SAM based experiments [4]. The influence of surface defects such as steps on epitaxial growth requires study with high spatial resolution, which we report for the Ge/Si(100) system. Ge grows on Si(100) in the Stranski-Krastonov growth mode wherein it forms pseudomorphic layers for the first 3-4 ML (critical thickness) and beyond which it clusters into islands[6]. In the present experiment, Ge was deposited onto clean Si(100) substrates misoriented 1° and 5° toward <110>. This was done using a mini MBE Knudsen cell at base pressure ~ 5×10-11 mbar and at typical rates of 0.1ML/min (1ML =0.14nm). Depositions just above the critical thickness were done for substrates kept at room temperature, 375°C and 525°C. The R T deposits were annealed at 375°C and 525°C for various times. Detailed studies were done of the initial stages of clustering into very fine (∼1nm) Ge islands and their subsequent coarsening and facetting with longer anneals. From the particle size distributions as a function of time and temperature, useful film growth parameters have been obtained. Fig. 1 shows a b-SE image of Ge island size distribution for a R T deposit and anneal at 525°C. Fig.2(a) shows the distribution for a deposition at 375°C and Fig.2(b) shows at a higher magnification a large facetted island of Ge. Fig.3 shows a distribution of very fine islands from a 525°C deposition. A strong contrast is obtained from these islands which are at most a few ML thick and mottled structure can be seen in the background between the islands, especially in Fig.2(a) and Fig.3.

Chemisorption of ethylene on nickel surfaces with preadsorbed oxygen

1981 ◽  
Vol 46 (2) ◽  
pp. 340-353
Author(s):  
Pavel Zachař ◽  
Zdeněk Bastl ◽  
Jakub Adámek
Keyword(s):  
Gas Phase ◽  
Phase Analysis ◽  
Oxygen Concentration ◽  
Electrical Resistance ◽  
High Vacuum ◽  
Volumetric Method ◽  
Surface Oxygen ◽  
Oxygen Chemisorption ◽  
Thin Polycrystalline ◽  
Total Adsorption

Chemisorption of ethylene was studied on thin polycrystalline layers of nickel prepared by metal deposition in high vacuum and modified by preadsorbed oxygen. The volumetric method combined with the gas-phase analysis and the measurement of the electrical resistance changes of these layers were used. Already small amounts of preadsorbed oxygen of the order of 10-2 of the monolayer affect rather substantially the extent of ethylene chemisorption. The extent of the initial irreversible chemisorption and also the total adsorption of ethylene as a function of the amount of preadsorbed oxygen have a maximum at the surface oxygen concentration of 3 . 1013 molecule cm-2. The adsorption accompanied by the extensive dissociation of ethylene C-H bonds proceeds predominantly on nickel atoms with lower coordination (atoms on the microcrystal edges, corner atoms, etc.), where also oxygen chemisorption proceeds preferentially.

Using Molecular-Beam Mass Spectrometry to Study the Pecvd of Diamondlike Carbon Films

1993 ◽  
Vol 334 ◽  
Author(s):  
I.B. Graff ◽  
R.A. Pugliese ◽  
P.R. Westmoreland
Keyword(s):  
Mass Spectrometry ◽  
Vapor Deposition ◽  
Molecular Beam ◽  
Film Growth ◽  
Chemical Vapor ◽  
Carbon Films ◽  
Total Flow ◽  
Measured Concentration ◽  
Molecular Beam Mass Spectrometry ◽  
Diamondlike Carbon

AbstractMolecular-beam mass spectrometry has been used to study plasma-enhanced chemical vapor deposition (PECVD) of diamondlike carbon films. A threshold-ionization technique was used to identify and quantify species in the plasma. Mole fractions of H, H2, CH4, C2H2, C2H6 and Ar were measured in an 83.3% CH4/Ar mixture at a pressure of 0.1 torr and a total flow of 30 sccm. Comparisons were made between mole fractions measured at plasma powers of 25W and 50W. These results were compared to measured concentration profiles and to film growth rates.

Mass Spectrometry and Gas-Phase Chemistry of Anilines

ChemInform ◽  
2007 ◽  
Vol 38 (30) ◽  
Author(s):  
Marcos N. Eberlin ◽  
Daniella Vasconcellos Augusti ◽  
Rodinei Augusti
Keyword(s):  
Mass Spectrometry ◽  
Gas Phase ◽  
Gas Phase Chemistry ◽  
Phase Chemistry
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