A Comparative Study of Reactor Designs for the Production of Graded Films with Applications to Combinatorial CVD

Segmented CVD reactor designs enabling spatial control of across-wafer gas phase composition were evaluated for depositing graded films suitable for combinatorial studies. Specifically two reactor designs were constructed and evaluated with experiments and response surface model (RSM) based analysis to quantify the reactor performance in terms of film thickness uniformity, sensitivity to adjustable reactor operating conditions, range of thickness over which uniformity could be achieved and each reactor ability to control the thickness gradient across the wafer surface. Design features distinguishing the two reactor systems and their influence on gradient control versus deposition rate performance are summarized. RS models relating wafer state properties to process recipes are shown to be effective tools to quantify, qualify and compare different reactor designs

Real-time acoustic sensing and control of metalorganic chemical vapor deposition precursor concentrations delivered from solid phase sources

We have investigated the performance and potential benefit of acoustic sensing for real-time monitoring and closed loop control of binary gas mixture compositions delivered from low vapor pressure metalorganic sources. Two solid phase sources were investigated in the presence of H 2 as a carrier gas: (1) trimethylindium (TMI) and (2) bis(cyclopentadienyl) magnesium ͑Cp 2 Mg͒, which have room temperature ͑25°C͒ vapor pressures of 2.5 and 0.04 Torr, respectively. An acoustic sensor was implemented on the gas feed line to measure the concentration-dependent speed of sound in the gas mixture. This enabled sensitivity and control at precursor levels as low as 0.6 ppm in H 2 . Closed loop process control was implemented to maintain TMI and Cp 2 Mg concentration target in the presence of intentionally introduced long term temperature drifts. Despite induced variations of the precursor vapor pressure up to 50%, the delivered composition was controlled to within ±0.15% for TMI (at 0.5 mol% set point) and ±0.3% for Cp 2 Mg (at 0.01 mol% set point). Short term variability could also be substantially reduced by the control scheme. This work demonstrates the feasibility of sensor-driven control systems for stable delivery of low vapor pressure, normally problematic precursor materials. In turn, this opens the door to utilization of a broader range of species which can be synthesized as chemical precursors

Real-time acoustic sensing and control of metalorganic chemical vapor deposition precursor concentrations delivered from solid phase sources

We have investigated the performance and potential benefit of acoustic sensing for real-time monitoring and closed loop control of binary gas mixture compositions delivered from low vapor pressure metalorganic sources. Two solid phase sources were investigated in the presence of H 2 as a carrier gas: (1) trimethylindium (TMI) and (2) bis(cyclopentadienyl) magnesium ͑Cp 2 Mg͒, which have room temperature ͑25°C͒ vapor pressures of 2.5 and 0.04 Torr, respectively. An acoustic sensor was implemented on the gas feed line to measure the concentration-dependent speed of sound in the gas mixture. This enabled sensitivity and control at precursor levels as low as 0.6 ppm in H 2 . Closed loop process control was implemented to maintain TMI and Cp 2 Mg concentration target in the presence of intentionally introduced long term temperature drifts. Despite induced variations of the precursor vapor pressure up to 50%, the delivered composition was controlled to within ±0.15% for TMI (at 0.5 mol% set point) and ±0.3% for Cp 2 Mg (at 0.01 mol% set point). Short term variability could also be substantially reduced by the control scheme. This work demonstrates the feasibility of sensor-driven control systems for stable delivery of low vapor pressure, normally problematic precursor materials. In turn, this opens the door to utilization of a broader range of species which can be synthesized as chemical precursors

Crystal structure of mixed fluorites Ca(1-x)Sr(x)F(2) and Sr(1-x)Ba(x)F(2) and luminescence of Eu(2+) in the crystals

Within the framework of the virtual crystal method implemented in the shell model and pair potential approximation the crystal structure of mixed fluorites Ca(1-x)Sr(x)F(2) and Sr(1-x)Ba(x)F(2) has been calculated. The impurity center Eu(2+) and the distance Eu(2+)-F in this crystals have been also calculated. The low level position of excited 4f65d configuration of the Eu(2+) ion has been expressed using phenomenological dependence on distance E(2+)-F. The dependences of Stokes shift and Huang-Rhys factor on concentration x have been received for yellow luminescence in Sr(1-x)Ba(x)F(2):Eu(2+). The value x, for which the eg -level of Eu(2+) ion will be in conduction band in Sr(1-x)Ba(x)F(2):Eu(2+) has been calculated.Comment: 8 pages, 3 figures. The manuscript is sent to journal 'Physics of the solid state'. The results will be submitted on inernational conference SCINTMAT'2002 in oral session (june,20-22,2002,Ekaterinburg,Russia). Corresponding author e-mail: [email protected]

Influence of Gas Composition on Wafer Temperature Control in a Tungsten Chemical Vapor Deposition Reactor

Experimental measurements of wafer temperature in a single-wafer,lamp-heated CVD system were used to study the wafer temperature responseto gas composition. A physically based simulation procedure for theprocess gas and wafer temperature was developed in which a subset ofparameter values were estimated using a nonlinear, iterative parameteridentification method, producing a validated model with true predictivecapabilities. With process heating lamp power held constant, wafertemperature variations of up to 160 degrees K were observed by varying feed gasH_2/N_2 ratio. Heat transfer between the wafer and susceptor wasstudied by shifting the instrumented wafer off the susceptor axis,exposing a portion of the wafer backside to the chamber floor. Modelpredictions and experimental observations both demonstrated that the gasvelocity field had little influence on the observed wafer and predictedgas temperatures

A NEW APPROACH TO SPATIALLY CONTROLLABLE CVD

This paper describes the continuing design evolution of a new approach to spatially controllable chemical vapor deposition for electronic materials manufacturing. Based on the success of a previous prototype reactor, we describe construction of a newer version of the prototype reactor system to assess its performance and identify its key operational characteristics. This new design includes a fully automated feed gas control system, allowing the reprogramming of reactor operation without hardware modifications and a time-shared gas sampling mass spectrometer for spatially resolved across-wafer gas composition analysis

Simulator Development for a Spatially Controllable Chemical Vapor Deposition System

Most conventional chemical vapor deposition systems do not have the spatial actuation and sensing capabilities necessary to control deposition uniformity, or to intentionally induce nonuniform deposition patterns for single-wafer combinatorial CVD experiments. In an effort to address this limitation, we began a research program at the University of Maryland focusing on the development of a novel CVD reactor system that can explicitly control the (2-dimensional) spatial profile of gas-phase chemical composition across the wafer surface. This reactor is based on a novel segmented showerhead design in which gas precursor composition can be individually controlled in the gas fed to each segment. Because the exhaust gas is recirculated up through the showerhead though the individual segments, the gas flow pattern created eliminates convective mass transfer between the segment regions. The effect of this design is a CVD system in which across-wafer composition gradients can be accurately predicted and controlled.This paper discusses the development of a simulator for a three-segment prototype that has recently been constructed as a modification to an Ulvac ERA1000 CVD cluster tool. A preliminary set of experiments has been performed to evaluate the performance of the prototype in depositing tungsten films for a range of wafer/showerhead spacing and segment gas compositions. We discuss the simulation approach taken to developing the simulator for this system focusing on a one-dimensional simulation of transport through the segments and exhaust mixing region, a model valid in the limit of close showerhead/wafer spacing. The use of simulation in the prototype system design, interpreting experimental data, and its ultimate use in controlling the CVD process to achieve true programmable CVD operation all will be discussed. Further information can be found at the project website, http://www.isr.umd.edu/Labs/CACSE/research/progrx

Real-Time Growth Rate Metrology for a Tungsten CVD Process by Acoustic Sensing

An acoustic sensor, the Leybold Inficon ComposerTM, was implemented downstream to a production-scale tungsten chemical vapor deposition (CVD) cluster tool for in-situ process sensing. Process gases were sampled at the outlet of the reactor chamber and compressed with a turbo-molecular pump and mechanical pump from the sub-Torr process pressure regime to above 50 Torr as required for gas sound velocity measurements in the acoustic cavity. The high molecular weight gas WF6 mixed with H2 provides a substantial molecular weight contrast so that the acoustic sensing method appears especially sensitive to WF6 concentration. By monitoring the resonant frequency of exhaust process gases, the depletion of WF6 resulting from the reduction by H2 was readily observed in the 0.5 Torr process for wafer temperatures ranging from 300 to 350 C. Despite WF6 depletion rates as low as 3-5%, in-situ wafer-state metrology was achieved with an error less than 6% over 17 processed wafers. This in-situ metrology capability combined with accurate sensor response modeling suggests an effective approach for acoustic process sensing in order to achieve run-to-run process control of the deposited tungsten film thickness