TPIR apparatus for monitoring tungsten hexafluoride processing to detect gas phase nucleation, and method and system utilizing same

• US 9,340,878 B2
• Filed: 05/28/2010
• Issued: 05/17/2016
• Est. Priority Date: 05/29/2009
• Status: Active Grant

• Current Assignee: Entegris Incorporated
• Original Assignee: Entegris Incorporated
• Inventors: Arno, Jose I., Despres, Joseph R., Letaj, Shkelqim, Lurcott, Steven M., Baum, Thomas H., Zou, Peng
• Primary Examiner(s): WIECZOREK, MICHAEL P
• Application Number:
  US13/375,053
• Publication Number:
  US 20120114836A1
• Time in Patent Office: 2,181 Days
• Field of Search: 427/8, 702/24, 702/28, 702/30
• US Class Current: 1/1
• CPC Class Codes: C23C 16/14 Deposition of only one other metal element
• CPC Class Codes: C23C 16/455 characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
• CPC Class Codes: C23C 16/52 Controlling or regulating the coating process C23C16/45557, C23C16/279 take precedence
• CPC Class Codes: G01N 21/3504 for analysing gases, e.g. multi-gas analysis

Abstract

Apparatus and method for monitoring a vapor deposition installation in which a gas mixture can undergo gas phase nucleation (GPN) and/or chemically attack the product device, under process conditions supportive of such behavior. The apparatus includes a radiation source arranged to transmit source radiation through a sample of the gas mixture, and a thermopile detector assembly arranged to receive output radiation resulting from interaction of the source radiation with the gas mixture sample, and to responsively generate an output indicative of onset of the gas phase nucleation and/or chemical attack when such onset occurs. Such monitoring apparatus and methodology is useful in tungsten CVD processing to achieve high rate tungsten film growth without GPN or chemical attack.

Claims

1. An apparatus for monitoring and control of a vapor deposition installation wherein a gas mixture containing gas species can cause gas phase nucleation and/or chemical attack under process conditions supportive of such behavior, the monitoring and control apparatus comprising:

a radiation source arranged to transmit source radiation through a sample of said gas mixture;

a detector arranged to receive output radiation resulting from interaction of the source radiation with the gas mixture sample, and to responsively generate a detector output; and

a processor and control assembly, comprising an algorithmic program for determining incipient occurrence of gas phase nucleation and/or chemical attack, the processor being configured to receive the detector output, algorithmically process same according to the algorithmic program to determine incipient occurrence of said gas phase nucleation and/or chemical attack in the vapor deposition installation, and responsively generate an output to control the vapor deposition installation so as to avoid gas phase nucleation and/or chemical attack therein, and maintain the vapor deposition installation in non-gas phase nucleation and/or non-chemical attack operation throughout vapor deposition in the vapor deposition installation.

2. The apparatus of claim 1, wherein the processor is adapted to determine incipient occurrence of said gas phase nucleation and/or chemical attack in the vapor deposition installation, by operation according to the algorithmic program including at least one of the following:

(i) determination of peak heights of one or more gas species of the gas mixture;

(ii) determination of differences in peak heights between two or more of the gas species of the gas mixture;

(iii) determination of ratios of peak heights of two or more of the gas species of the gas mixture;

(iv) determination of AUC of a spectral portion of the output radiation for one or more gas species of the gas mixture;

(v) determination of differences of AUC for spectral portions of the output radiation for two or more gas species of the gas mixture;

(vi) determination of ratios of AUC for spectral portions of the output radiation for two or more gas species of the gas mixture;

(vii) determination of slope of a spectral curve in a spectral portion of the output radiation of one or more gas species of the gas mixture;

(viii) determination of differences of slopes of spectral curves in spectral portions of the output radiation of two or more gas species of the gas mixture;

(ix) determination of ratios of slopes of spectral curves in spectral portions of the output radiation of two or more gas species of the gas mixture;

(x) determination of peak heights of the output radiation of one or more gas species of the gas mixture at a predetermined point in time;

(xi) determination of differences in peak heights of the output radiation between two or more of the gas species of the gas mixture at a predetermined point in time;

(xii) determination of ratios of peak heights of the output radiation of two or more of the gas species of the gas mixture at a predetermined point in time; and

(xiii) monitoring of a gas species reactant that is consumed during vapor deposition, as an indicator of onset of gas phase nucleation and/or chemical attack.

3. The apparatus of claim 1, wherein the processor and control assembly includes a database of spectra or spectral characteristics of gas species of interest in the gas mixture, and the processor is arranged to process the detector output against the database to determine incipient occurrence of said gas phase nucleation and/or chemical attack throughout the vapor deposition in the vapor deposition installation.

4. The apparatus of claim 1, as operatively coupled with a chemical vapor deposition system arranged for deposition of tungsten from a source gas mixture including silane and tungsten hexafluoride.

5. The apparatus of claim 4, wherein the chemical vapor deposition system comprises a chemical vapor deposition chamber having one or more windows, wherein the radiation source comprises an infrared radiation diode laser arranged to transmit IR radiation through a window into the chamber for interaction with vapor of the gas mixture therein during chemical vapor deposition in the chamber to generate the output radiation from such interaction, and the detector comprises a photodiode detector arranged to receive said output radiation transmitted through a same or different window of the chamber and to responsively generate the detector output.

6. The apparatus of claim 5, wherein the chemical vapor deposition chamber is arranged in an arrangement in which:

(A) the chemical vapor deposition chamber comprises a single window, and the photodiode detector is arranged for detecting back-scatter IR radiation;

or

(B) the chemical vapor deposition chamber comprises two windows in opposing registration with one another, with the infrared radiation diode laser being arranged for transmitting IR radiation through a first one of said windows, and the photodiode detector being arranged for detecting output radiation transmitted through a second one of said windows.

7. The apparatus of claim 1, as adapted for monitoring of at least one of WF₆, SiF₄ and SiH₄, wherein the radiation source is arranged to transmit infrared radiation, and the detector comprises a TPIR detector.

8. The apparatus of claim 1, comprising:

a monitoring cell adapted to receive the sample of said gas mixture for monitoring;

and wherein;

the radiation source comprises an infrared source that transmits infrared radiation through the sample of said gas mixture in the monitoring cell;

the detector comprises a TPIR detector; and

the algorithmic program of the processor and control assembly is configured so that the processor in determining incipient occurrence of said gas phase nucleation and/or chemical attack in the vapor deposition installation, performs an algorithmic process comprising

removing ambient radio frequency noise spikes from the TPIR detector output to produce a first refined data output;

smoothing the first refined data output using a binomial smoothing algorithm to produce a second refined data output;

calculating slope and offset values for signals of gas mixture components monitored in the monitoring cell;

utilizing the slopes and offsets for the monitored gas mixture components to temperature correct the second refined output and produce a third refined output;

conducting a peak search algorithm of the third refined output and calculating peak heights of the monitored gas mixture components, to generate peak heights of such monitored gas mixture components, and determining from peak height differences of such monitored gas mixture components whether incipient occurrence of said gas phase nucleation and/or chemical attack in the vapor deposition installation is identified, as predictive of actual occurrence of said gas phase nucleation and/or chemical attack in the vapor deposition installation in the absence of modulation of the vapor deposition installation; and

the processor and control assembly comprises a controller coupled with the processor for correspondingly modulating the vapor deposition installation to avoid gas phase nucleation and/or chemical attack therein, and maintain the vapor deposition installation in non-gas phase nucleation and/or non-chemical attack operation throughout the vapor deposition in the vapor deposition installation.

9. The apparatus of claim 8, wherein the processor and control assembly comprises a memory unit in which the algorithmic program and associated monitoring and control operational instructions are stored, and the processor is arranged to access and execute said instructions.