Method for coating inner surfaces of equipment

• US 6,416,577 B1
• Filed: 06/07/2000
• Issued: 07/09/2002
• Est. Priority Date: 12/09/1997
• Status: Expired due to Term

• Current Assignee: ASM International NV
• Original Assignee: ASM Microchemistry Ltd. (ASM International NV)
• Inventors: Suntoloa, Tuomo, Leskelä, Markku, Ritala, Mikko
• Primary Examiner(s): Beck, Shrive P.
• Assistant Examiner(s): FLETCHER III, WILLIAM P
• Application Number:
  US09/581,020
• Time in Patent Office: 762 Days
• Field of Search: 117/84, 117/88, 117/104, 117/109, 117/200, 427/237, 427/38, 427/255.23, 427/255.28, 427/255.7, 427/230, 118/723, 118/715
• US Class Current: 117/88
• CPC Class Codes: C23C 16/045 Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates
• CPC Class Codes: C23C 16/45525 Atomic layer deposition [ALD]
• CPC Class Codes: C23C 16/46 characterised by the method used for heating the substrate C23C16/48, C23C16/50 take precedence
• CPC Class Codes: C30B 35/00 Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
• CPC Class Codes: Y10T 117/10 Apparatus

Abstract

This invention concerns a method for coating the inner surfaces of equipment with a layer of material. According to the invention, of the inner space of the equipment limited by the surfaces to be coated is at least partly closed, to said inner space pulses of at least two different reagents in gaseous phase are fed alternately and repeatedly and a layer of material is grown on the surfaces of the inner space according to ALE-technique by exposing the surfaces to the alternating surface reactions of the reagents. With the aid of the invention it is possible to coat pipes and tanks of desired size without using a separate growing equipment.

Claims

1. A method for coating the inner surfaces of equipment with a layer of material using atomic layer deposition, said method comprising:

closing at least a part of an inner space limited by the inner surfaces of the equipment;

alternately and repeatedly feeding vapor phase pulses of at least two different reagents into said inner space; and

growing a layer of material on the inner surfaces of the equipment by exposing the inner surfaces of the equipment to alternating surface reactions of the reagents.

2. The method according to claim 1, further comprising the following steps in sequence:

a. emptying the space limited by the inner surfaces from gases with a pump, wherein said inner surfaces have surface bond sites;

b. bringing said inner surfaces to a temperature required for the surface reactions used in the coating process;

c. feeding a first reagent (A) to the space limited by the inner surfaces in at least an amount that is sufficient for occupying the surface bond sites on said inner surfaces;

d. removing any excess first reagent (A) from said space;

e. feeding a second reagent (B) to the space limited by the inner surfaces in at least an amount that is sufficient for occupying the surface bond sites created by the first reagent (A) on said inner surfaces;

f. removing any excess second reagent (B) from said inner space; and

g. repeating steps c. to f. in sequence in cycles until the layer reaches a desired thickness.

3. The method according to claim 2, wherein the inner surfaces to be coated are brought to the temperature required for the surface reactions used in the coating process with space limited by the inner surfaces.

4. The method according to claim 2, wherein the inner surfaces to be coated are brought to the temperature required for the surface reactions used in the coating process by feeding heat-transfer liquid or gas into the space limited by the inner surfaces to be coated before steps a. to f.

5. The method according to claim 4, wherein said heat-transfer liquid or gas is fed more than once to the space limited by the inner surfaces to be coated after the cycle c. to f.

6. The method according to claim 2, further comprising flowing protective gas into the space limited by the inner surfaces in steps d and f, whereby the removal of excess amounts of reagents (A,B) is made more efficient.

7. The method according to claim 2, further comprising feeding at least one other reagent in addition to said first reagent and said second reagent to the space limited by the surfaces to be coated to facilitate the surface reactions caused by the first and the second reagent.

8. The method according to claim 1, wherein said at least a part of the inner space limited by the inner surfaces is closed with the aid of valve gears.

9. The method according to claim 8, wherein at least one of the valve gears is used in feeding the reagents.

10. The method according to claim 8, wherein at least one valve gear is used for removing excess gas.

11. The method according to claim 1, wherein the inner surface of process equipment is coated.

12. The method according to claim 1, wherein coating improves at least one of the stress, corrosion endurance optical, electrical and friction properties of the inner surface of equipment.

13. The method according to claim 1, wherein at least one layer is selected from the group consisting of an oxide layer, a nitride layer, and a chalcogenide layer is grown on the inner surface.

14. The method according to claim 1, wherein said reagents are selected from the group consisting of the inorganic compounds of metals, metalorganic compounds, pure metals, water, hydrogen peroxide, oxygen, ozone, alcohols, ammonia, and organic nitrogen compounds.

15. The method according to claim 9, wherein at least two sources of reagent are connected to said valve gear.

16. The method according to claim 11, wherein said process equipment is piping or a tank.

17. A method for coating inner surfaces of a workpiece using atomic layer deposition, comprising a plurality of cycles, wherein each cycle comprises:

providing a workpiece defining an enclosed space having an inlet and an outlet therein;

providing a first reagent to the enclosed space via the inlet;

forming no more than a monolayer by providing the first reagent on the workpiece;

removing any excess amount of the first reagent from the enclosed space via the outlet;

providing a second reagent to the enclosed space via the inlet after removing any excess amount of the first reagent;

allowing the second reagent to react or absorb with the monolayer from the first reagent; and

removing any excess amount of the second reagent from the enclosed space via the outlet.

18. The method of claim 17, wherein the workpiece comprises a conduit.

19. The method of claim 17, wherein the workpiece comprises a container.

20. The method of claim 17, further comprising closing off flow through the outlet while providing the first reagent.

21. The method of claim 17, wherein the inlet and outlet define an open flow path through the enclosed space during provision of the first reagent and the second reagent.

22. The method of claim 17, wherein at least a portion of the first reagent adsorbs upon the inner surface of the workpiece, and the second reagent reacts with the portion of the first reagent adsorbed upon the inner surface.

23. The method of claim 17, further comprising externally heating the workpiece.

24. A deposition apparatus for coating only interior surfaces of a workpiece using atomic layer deposition, comprising:

a first collar configured to seal one opening of the workpiece;

a feed line communicating through the first collar, the feed line communicating with a gaseous source of deposition reagents, a second feed line communicating with a second gaseous source of deposition reagents, the first and second feed lines configured such that the first and second gaseous sources can be alternately and exclusively fed into the work piece;

a second collar configured to seal another opening of the workpiece; and

an exhaust line communicating through the second collar.

25. The apparatus of claim 24, further comprising a heat source for externally heating the workpiece.

26. The apparatus of claim 24, further comprising a valve along the exhaust line for selectively closing exhaust flow.

27. The apparatus of claim 24, further comprising a second feed line communicating a second gaseous source of deposition reactants.

28. The apparatus of claim 24, wherein the exhaust line extends from the second collar to a pump.