Liquid flow rate estimation and verification by direct liquid measurement

• US 5,866,795 A
• Filed: 03/17/1997
• Issued: 02/02/1999
• Est. Priority Date: 03/17/1997
• Status: Expired due to Term

• Current Assignee: Applied Materials Incorporated
• Original Assignee: Applied Materials Incorporated
• Inventors: Plante, Jeff, Pham, Thanh, Wang, Yen-Kun, Chang, Fong
• Primary Examiner(s): RAEVIS, ROBERT R
• Application Number:
  US08/819,593
• Time in Patent Office: 687 Days
• Field of Search: 73/1.36, 73/1.16, 427/8
• US Class Current: 73/1.36
• CPC Class Codes: C23C 16/4481 by evaporation using carrier gas in contact with the source material C23C16/4486 takes precedence
• CPC Class Codes: G01F 1/007 by measuring the level variations of storage tanks relative to the time
• CPC Class Codes: G01F 1/708 Measuring the time taken to traverse a fixed distance
• CPC Class Codes: G01F 25/10 of flowmeters
• CPC Class Codes: G01F 25/13 using a reference counter
• CPC Class Codes: G01F 25/17 using calibrated reservoirs

Abstract

An apparatus for controlling the flow of a liquid precursor into a deposition chamber comprises a liquid injection system having a liquid injection outlet connected to a chamber inlet line upstream of the deposition chamber. The liquid injection system includes a liquid precursor supply, a purge gas supply, a carrier gas supply, a liquid flow meter, and a controller managing flows of the liquid precursor and carrier gas to the chamber. A purge line is connected between the purge gas supply and the liquid flow meter and is used to trap a known mass of liquid precursor. To calibrate the flow of the liquid precursor, the purge gas is used to push the trapped liquid precursor through the liquid flow meter at a steady rate. The elapsed time for evacuating the trapped liquid precursor from the purge line is measured. Calibration information is computed using the mass of the trapped liquid precursor and the measured elapsed time based on the direct liquid measurement approach. The calibration information is used to calibrate the controller to correct deviations in the liquid flow rate and achieve a target liquid precursor flow rate for improving wafer uniformity.

Claims

1. A method for calibrating a liquid flow controller, comprising the steps of:

measuring an expected elapsed time for draining a mass of liquid through an inlet line connected to an inlet of a pre-calibrated liquid flow controller at an expected flow rate;

measuring an actual elapsed time for draining said mass of liquid through said inlet line connected to an inlet of a liquid flow controller set at said expected flow rate;

computing calibration information using said expected elapsed time and said actual elapsed time; and

calibrating said liquid flow controller using said calibration information to achieve said expected flow rate of said liquid.

2. The method of claim 1, wherein said step of computing calibration information comprises calculating a correction factor for said liquid flow controller by dividing said expected elapsed time by said actual elapsed time.

3. The method of claim 2, wherein said step of calibrating said liquid flow controller comprises adjusting a flow rate setting of said liquid flow controller if said correction factor deviates from 1 by more than a desired preset percentage.

4. The method of claim 3, wherein said step of adjusting a flow rate setting of said liquid flow controller comprises resetting said liquid flow controller from said expected flow rate to a reset flow rate equal to said expected flow rate divided by said correction factor.

5. The method of claim 1, wherein said step of measuring said expected elapsed time comprises recording an expected start time for draining said mass of liquid, recording measured mass flow rate data sensed in said pre-calibrated liquid flow controller as a function of time, and observing a sudden drop in said measured mass flow rate at an expected end time, said expected elapsed time being equal to said expected end time minus said expected start time.

6. The method of claim 1, wherein said step of measuring an actual elapsed time comprises recording a start time for draining said mass of liquid, recording measured mass flow rate data sensed in said liquid flow controller as a function of time, and observing a sudden drop in said measured mass flow rate at an end time, said actual elapsed time being equal to said end time minus said start time.

7. The method of claim 1, wherein said step of measuring an expected elapsed time is performed with a control module which releases said mass of liquid into said inlet line and traps said liquid in said inlet line, directs an inert gas flow to drive said mass of liquid from said inlet line through said pre-calibrated liquid flow controller at an expected start time until said mass of liquid completely exits said inlet line at an expected end time, said expected elapsed time being equal to said expected end time minus said expected start time.

8. The method of claim 1, wherein said step of measuring an actual elapsed time is performed with a control module which releases said mass of liquid into said inlet line and traps said liquid in said inlet line, directs an inert gas flow to drive said mass of liquid from said inlet line at a start time through said liquid flow controller at a start time until said mass of liquid completely exits said inlet line at an end time, said actual elapsed time being equal to said end time minus said start time.

9. A method for calibrating a liquid flow meter in a precursor liquid injection system, said method comprising the steps of:

trapping a liquid precursor with a mass in a tube having an outlet connected to an inlet of a liquid flow meter;

supplying a purge gas to an inlet of said tube, said purge gas and said liquid precursor forming a liquid-gas boundary therebetween;

setting said liquid flow meter at an expected liquid precursor mass flow rate to release said trapped liquid precursor from said tube to flow through said inlet of said liquid flow meter with said liquid-gas boundary moving across said tube;

measuring an elapsed time for said liquid-gas boundary to reach said inlet of said liquid flow meter;

computing calibration information using said elapsed time; and

calibrating said liquid flow meter using said calibration information.

10. The method of claim 9, wherein said step of computing calibration information comprises calculating an actual liquid precursor mass flow rate by dividing said mass by said elapsed time and computing a calibration factor for said liquid flow meter by dividing said actual liquid precursor mass flow rate by said expected liquid precursor mass flow rate.

11. The method of claim 10, wherein said step of calibrating said liquid flow meter comprises adjusting said liquid flow meter if said calibration factor deviates from 1 by more than a preset tolerance.

12. The method of claim 11, wherein said step of adjusting said liquid flow meter comprises resetting said liquid flow meter from said expected liquid precursor mass flow rate to a reset liquid precursor mass flow rate equal to said expected liquid precursor mass flow rate divided by said calibration factor.

13. The method of claim 9, wherein said step of trapping said liquid precursor comprises opening a liquid precursor inlet valve disposed between a liquid precursor supply and said tube, and said step of supplying said purge gas comprises closing said liquid precursor inlet valve and opening a purge valve disposed between a purge gas supply and said inlet of said tube.

14. The method of claim 9, wherein said step of measuring an elapsed time comprises monitoring measured liquid precursor mass flow rate in said liquid flow meter and observing a sudden drop of said measured liquid precursor mass flow rate at said elapsed time.

15. A method for controlling the flow of a liquid precursor into a deposition process chamber, said method comprising the steps of:

accumulating a liquid precursor in a line connected upstream to a liquid precursor controller;

directing a purge gas at a start time t₀ to drive said liquid precursor from said line through said liquid precursor controller at a liquid precursor flow rate, said liquid precursor drained from said line at an end time t₁ ;

generating control data from said start time and said end time; and

controlling said liquid precursor flow rate to achieve an intended liquid precursor flow rate in response to said control data.

16. The method of claim 15, further comprising the step of determining an expected elapsed time prior to performing the aforementioned steps, said step of determining an expected elapsed time comprising:

accumulating said liquid precursor in said line connected upstream to a pre-calibrated liquid precursor controller;

directing a purge gas at an expected start time t_e0 to drive said liquid precursor from said line through said pre-calibrated liquid precursor controller at said intended liquid precursor flow rate, said liquid precursor drained from said line at an expected end time t_e1 ; and

computing said expected elapsed time t_e =t_e1 -t_e0.

17. The method of claim 16, wherein said step of determining an expected elapsed time is repeated for a plurality of intended liquid precursor flow rates to generate a plot of t_e as a function of intended liquid precursor flow rate.

18. The method of claim 16, wherein said step of generating control data comprises computing a correction factor C=(t₁ -t₀)/t_e.

19. The method of claim 18, wherein said step of controlling said liquid precursor flow rate comprises adjusting said liquid precursor flow rate if C deviates from 1 by more than a preset percentage.

20. The method of claim 19, wherein said step of controlling said liquid precursor flow rate comprises resetting said liquid precursor flow rate to a reset liquid precursor flow rate which is equal to the intended liquid precursor flow rate divided by C.

21. The method of claim 15, wherein said step of directing said purge gas comprises setting said liquid precursor controller at said intended liquid precursor flow rate and opening a purge valve connected between a purge gas supply and an inlet of said line.

22. The method of claim 21, wherein said step of generating control data comprises calculating an actual liquid precursor flow rate by dividing the mass of said liquid precursor accumulated in said line by an elapsed time equal to said end time minus said start time, and computing a control factor for said liquid precursor controller by dividing said actual liquid precursor flow rate by said intended liquid precursor flow rate.

23. The method of claim 22, wherein said step of controlling said liquid precursor flow rate comprises adjusting said liquid precursor flow rate if said control factor deviates from 1 by more than a preset percentage.

24. The method of claim 23, wherein said step of adjusting said liquid precursor flow rate comprises resetting said liquid precursor flow rate of said liquid precursor controller from said intended liquid precursor flow rate to a reset liquid precursor flow rate equal to said intended liquid precursor flow rate divided by said control factor.