Method of passivating a gas vessel or component of a gas transfer system using a silicon overlay coating

• US 6,511,760 B1
• Filed: 02/26/1999
• Issued: 01/28/2003
• Est. Priority Date: 02/27/1998
• Status: Expired due to Term

• Current Assignee: SilcoTek Corporation
• Original Assignee: Restek Corporation
• Inventors: Barone, Gary A., Stauffer, Joseph, Schuyler, Andy S.
• Primary Examiner(s): Jones, Deborah
• Assistant Examiner(s): STEIN, STEPHEN J
• Application Number:
  US09/259,656
• Time in Patent Office: 1,432 Days
• Field of Search: 427/452, 427/255, 427/248.1, 427/230, 427/237, 427/238, 423/348, 423/349, 118/715, 118/50, 206/0.6, 148/279, 148/508, 428/450, 428/446, 428/641, 428/336, 428/212
• US Class Current: 428/641
• CPC Class Codes: C23C 16/0254 Physical treatment to alter the texture of the surface, e.g. scratching or polishing
• CPC Class Codes: C23C 16/045 Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates
• CPC Class Codes: C23C 16/24 Deposition of silicon only
• CPC Class Codes: C23C 16/4408 by purging residual gases from the reaction chamber or gas lines
• CPC Class Codes: C23C 16/45523 Pulsed gas flow or change of composition over time
• CPC Class Codes: F17C 1/10 with provision for protection against corrosion, e.g. due to gaseous acid F17C1/14, F17C1/16 take precedence; inhibiting corrosion of metallic material or incrustation in general C23F
• CPC Class Codes: F17C 2203/0604 Liners
• CPC Class Codes: F17C 2203/0607 Coatings
• CPC Class Codes: F17C 2203/0619 with two layers
• CPC Class Codes: F17C 2203/0636 Metals
• CPC Class Codes: F17C 2209/232 of walls
• CPC Class Codes: F17C 2221/037 Containing pollutant, e.g. H2S, Cl
• CPC Class Codes: F17C 2223/0123 gaseous, e.g. CNG, GNC
• CPC Class Codes: F17C 2223/036 Very high pressure (>80 bar)
• CPC Class Codes: F17C 2260/053 Reducing corrosion
• CPC Class Codes: F17C 3/12 with provision for protection against corrosion, e.g. due to gaseous acid protection against corrosion in general C23F
• CPC Class Codes: Y10T 428/12674 Ge- or Si-base component
• CPC Class Codes: Y10T 428/24942 including components having same physical characteristic in differing degree
• CPC Class Codes: Y10T 428/265 1 mil or less

Abstract

A method of passivating the interior surface of a gas storage vessel to protect the surface against corrosion. The interior surface of the vessel is first dehydrated and then evacuated. A silicon hydride gas is introduced into the vessel. The vessel and silicon hydride gas contained therein are heated and pressurized to decompose the gase. A layer of silicon is deposited on the interior surface of the vessel. The duration of the silicon depositing step is controlled to prevent the formation of silicon dust in the vessel. The vessel is then purged with an inert gas to remove the silicon hydride gas. The vessel is cycled through the silicon depositing step until the entire interior surface of the vessel is covered with a layer of silicon. The vessel is then evacuated and cooled to room temperature.

Claims

1. A method of passivating the interior surface of a gas storage vessel to protect the surface against corrosion, comprising the steps of:

a) dehydrating the interior surface of the vessel;

b) evacuating the interior of the vessel;

c) introducing a silicon hydride gas into the vessel;

d) heating and pressurizing the silicon hydride gas in the vessel;

e) depositing a layer of silicon on the interior surface of the vessel;

f) controlling the duration of the silicon depositing step to prevent the formation of silicon dust in the vessel;

g) purging the vessel with an inert gas to remove the silicon hydride gas;

h) cycling the vessel through steps b-g until the entire interior surface of the vessel is covered with a layer of silicon;

i) evacuating the vessel; and

,

j) cooling the vessel to room temperature.

2. The method recited in claim 1, said dehydration step comprising heating the storage vessel to a temperature in the range of 360°

to 600°

C. for 30 to 240 minutes.

3. The method recited in claim 2, including the step of heating the storage vessel in an inert gas or in a vacuum.

4. The method recited in claim 1, said silicon hydride gas being selected from the group comprising SiH₄ and SinHn⁺².

5. The method recited in claim 1, said silicon hydride gas being heated to a temperature approximately equal to the gas'"'"'s decomposition temperature.

6. The method recited in claim 5, said silicon hydride gas being heated to a temperature in the range of 360°

to 600°

C.

7. The method recited in claim 1, said silicon hydride gas being pressurized to a pressure in the range of 2 to 45 p.s.i.a.

8. The method recited in claim 1, said layer of silicon being deposited on the interior surface of the vessel for a period in the range of 30 to 240 minutes.

9. The method recited in claim 1, including the step of measuring the average surface roughness (RA) of the interior surface of the vessel before dehydrating the vessel.

10. The method recited in claim 9, including cycling the vessel 1 to 2 times if the surface RA is less than about 20 microinches, and cycling the vessel 2 to 5 times if the surface RA is greater than about 20 microinches.

11. The method recited in claim 9, including cycling the vessel until the silicon passivation layer is 120 to 500 angstroms in thickness if the vessel RA is less than about 20 microinches.

12. The method recited in claim 9, including cycling the vessel until the silicon passivation layer is 501 to 50,000 angstroms if the surface R,A is greater than about 20 microinches.

13. A corrosion resistant gas storage vessel having a passive interior surface, comprising:

a) a metallic interior surface having an average surface roughness RA;

b) a silicon layer formed over the entire interior surface, said silicon layer being formed from a plurality of sublayers of silicon which are substantially free of silicon dust;

said interior surface having an average roughness RA less than about 20 microinches, and said silicon layer having a thickness in the range of 120 to 500 angstroms.

14. A corrosion resistant gas storage vessel having a passive interior surface, comprising:

a) a metallic interior surface having an average surface roughness RA;

b) a silicon layer formed over the entire interior surface, said silicon layer being formed from a plurality of sublayers of silicon which are substantially free of silicon dust;

said interior surface having an average roughness RA greater than about 20 microinches and said silicon layer having a thickness in the range of 501 to 50,000 angstroms.

15. A corrosion resistant gas storage vessel having a passive interior surface, comprising:

a) a metallic interior surface having an average surface roughness RA;

b) a silicon passivation layer formed over the entire interior surface;

said interior surface having an average roughness RA less than about 20 microinches, and said silicon layer having a thickness in the range of 120 to 500 angstroms,

said silicon passivation layer being substantially free of silicon dust and having been formed according to the following steps;

a) dehydrating the interior surface of the vessel;

b) evacuating the interior of the vessel;

c) introducing a silicon hydride gas into the vessel;

d) heating and pressurizing the silicon hydride gas in the vessel;

e) depositing a layer of silicon on the interior surface of the vessel;

f) controlling the duration of the silicon depositing step to prevent the formation of silicon dust in the vessel;

g) purging the vessel with an inert gas to remove the silicon hydride gas;

h) cycling the vessel through steps b-g until the entire interior surface of the vessel is covered with a layer of silicon;

i) evacuating the vessel; and

j) cooling the vessel to room temperature.

16. A method of passivating the interior surface of a gas storage vessel to protect the surface against corrosion, comprising the steps of:

a) dehydrating the interior surface of the vessel;

b) evacuating the interior of the vessel;

c) introducing a silicon hydride gas into the vessel;

d) heating and pressurizing the silicon hydride gas in the vessel;

e) depositing a passivation layer of silicon on the interior surface of the vessel;

f) controlling the duration of the silicon depositing step to prevent the formation silicon dust in the vessel;

g) purging the vessel with an inert gas to remove the silicon hydride gas;

h) cycling the vessel through steps b-g until the entire interior surface of the vessel is covered with a layer of silicon;

i) evacuating the vessel; and

,

j) cooling the vessel to room temperature;

said dehydration step comprising heating the storage vessel to a temperature in the range of 360°

to 600°

C. for 30 to 240 minutes;

including the step of heating the storage vessel in an inert gas or in a vacuum;

said silicon hydride gas being selected from the group comprising SiH₄ and SinHn<sup>−

2</sup>;

said silicon hydride gas being heated to a temperature approximately equal to the gas'"'"'s decomposition temperature;

said silicon hydride gas being heated to a temperature in the range of 360°

to 600°

C.

said silicon hydride gas being pressurized to a pressure in the range of 2 to 45 p.s.i.a.;

said layer of silicon being deposited on the interior surface for a period in the range of 30 to 240 minutes;

including the step of measuring the average roughness RA of the interior surface of the vessel before dehydrating the vessel;

including cycling the vessel 1 to 2 times if the surface RA is less than about 20 microinches;

including cycling the vessel until the silicon layer is 120 to 500 angstroms in thickness if the surface RA is less than about 20 microinches;

including cycling the vessel 2 to 5 times if the surface RA is greater than about 20 microinches;

including cycling the vessel until the silicon layer is 501 to 50,000 angstroms if the surface RA is greater than about 20 microinches.

17. A method of passivating the interior surface of a gas storage vessel to protect the surface against corrosion, comprising the steps of:

a) measuring the average surface roughness (RA) of the interior surface of the vessel and then dehydrating the interior surface of the vessel;

b) evacuating the interior of the vessel;

c) introducing a silicon hydride gas into the vessel;

d) heating and pressurizing the silicon hydride gas in the vessel;

e) depositing a layer of silicon on the interior surface of the vessel;

f) controlling the duration of the silicon depositing step to prevent the formation of silicon dust in the vessel;

g) purging the vessel with an inert gas to remove the silicon hydride gas;

h) cycling the vessel through steps b-g until the entire interior surface of the vessel is covered with a layer of silicon;

i) evacuating the vessel; and

,

j) cooling the vessel to room temperature,

including cycling the vessel 1 to 2 times if the surface RA is less than about 20 microinches and cycling the vessel 2 to 5 times if the surface RA is greater than about 20 microinches.

18. The method recited in claim 17, including cycling the vessel until the silicon passivation layer is 501 to 50,000 angstroms if the surface RA is greater than about 20 microinches.

19. The method recited in claim 17, including cycling the vessel until the silicon passivation layer is 120 to 500 angstroms in thickness if the vessel RA is less than about 20 microinches.

20. A corrosion resistant gas storage vessel having a passive interior surface, comprising:

a) a metallic interior surface having an average surface roughness RA;

b) a silicon passivation layer formed over the entire interior surface;

said interior surface having an average roughness RA greater than about 20 microinches, and said silicon layer having a thickness in the range of 501 to 50,000 angstroms,

said silicon passivation layer being substantially free of silicon dust and having been formed according to the following steps;

a) dehydrating the interior surface of the vessel;

b) evacuating the interior of the vessel;

c) introducing a silicon hydride gas into the vessel;

d) heating and pressurizing the silicon hydride gas in the vessel;

e) depositing a layer of silicon on the interior surface of the vessel;

f) controlling the duration of the silicon depositing step to prevent the formation of silicon dust in the vessel;

g) purging the vessel with an inert gas to remove the silicon hydride gas;

h) cycling the vessel through steps b-g until the entire interior surface of the vessel is covered with a layer of silicon;

i) evacuating the vessel; and

j) cooling the vessel to room temperature.