Method and apparatus to help promote contact of gas with vaporized material

• US 7,828,274 B2
• Filed: 01/23/2009
• Issued: 11/09/2010
• Est. Priority Date: 07/23/2002
• Status: Expired due to Term

• Current Assignee: Entegris Incorporated
• Original Assignee: Advanced Technology Materials, Inc. (Entegris Incorporated)
• Inventors: Naito, Donn K., Laxman, Ravi, Banton, Jeffrey I., Gregg, John N., Battle, Scott L.
• Primary Examiner(s): BUSHEY, CHARLES S
• Application Number:
  US12/358,723
• Publication Number:
  US 20090136668A1
• Time in Patent Office: 655 Days
• Field of Search: 261/21, 261/22, 261/23.1, 261/74, 261/121.1, 261/124, 261/142, 261/147, 261/DIG.65, 261/DIG.89, 118/726, 342/09, 342/11, 343/59, 343/80, 344/93, 344/97, 345/10
• US Class Current: 261/142
• CPC Class Codes: C23C 16/4408 by purging residual gases from the reaction chamber or gas lines
• CPC Class Codes: C23C 16/4481 by evaporation using carrier gas in contact with the source material C23C16/4486 takes precedence
• CPC Class Codes: C23C 16/4483 using a porous body
• CPC Class Codes: C23C 16/45544 characterized by the apparatus
• CPC Class Codes: C23C 16/50 using electric discharges generation and control of plasma in discharge tubes for surface treatment H01J37/32, H01J37/34
• CPC Class Codes: F17C 11/00 Use of gas-solvents or gas-sorbents in vessels absorbing compositions for acetylene C10L3/04; absorbing compositions for hydrogen C01B3/0005
• CPC Class Codes: F17C 2203/03 Thermal insulations
• CPC Class Codes: F17C 3/00 Vessels not under pressure
• CPC Class Codes: F17C 3/02 with provision for thermal insulation thermal insulation in general F16L59/00 ; refrigerators F25D; insulation specially adapted for cryogenic vessels F17C13/001; tank vehicles B60P3/22; railway tank wagons B61D5/00
• CPC Class Codes: Y02E 60/32 Hydrogen storage
• CPC Class Codes: Y10S 261/65 Vaporizers

Abstract

Vaporizable material is supported within a vessel to promote contact of an introduced gas with the vaporizable material, and produce a product gas including vaporized material. A heating element supplies heat to a wall of the vessel to heat vaporizable material disposed therein. The vessel may comprise an amoule having a removable top. Multiple containers defining multiple material support surfaces may be stacked disposed within a vessel in thermal communication with the vessel. A tube may be disposed within the vessel and coupled to a gas inlet. Filters, flow meters, and level sensors may be further provided. Product gas resulting from contact of introduced gas with vaporized material may be delivered to atomic layer deposition (ALD) or similar process equipment. At least a portion of source material including a solid may be dissolved in a solvent, followed by removal of solvent to yield source material (e.g., a metal complex) disposed within the vaporizer.

Claims

1. A method utilizing a vaporizer that includes a vaporizer ampoule wall defining an internal compartment;

and a plurality of solid source material holders disposed at different levels within the internal compartment;

wherein at least one solid source material holder has a solid source material support surface and a thermally conductive holder sidewall extending above the solid source material support surface; and

wherein each holder sidewall is adapted to be in substantial thermal contact with the vaporizer ampoule wall at an ampoule operating temperature, and the ampoule wall is adapted to transfer heat to the thermally conductive holder sidewall, the method comprising;

introducing source material comprising a solid into at least one solid source material holder of the plurality of solid source material holders;

dissolving at least a portion of the source material in a solvent;

removing said solvent from said source material; and

stacking said plurality of solid source material holders in the vaporizer ampoule.

2. The method of claim 1, further comprising heating the source material.

3. The method of claim 1, further comprising heating the vaporizer ampoule to vaporize at least a portion of the source material.

4. The method of claim 1, wherein the step of removing said solvent from said source material comprises use of reduced pressure.

5. The method of claim 1, further comprising flowing a first gas to the vaporizer ampoule to contact said source material.

6. The method of claim 1, wherein said source material comprises a metal complex.

7. The method of claim 1, wherein said source material comprises at least one of:

boron (B), phosphorous (P), copper (Cu), gallium (Ga), arsenic (As), ruthenium (Ru), indium (In), antimony (Sb), lanthanum (La), tantalum (Ta), iridium (Ir), decaborane (B₁₀H₁₄), hafnium tetrachloride (HfCl₄), zirconium tetrachloride (ZrCl₄), indium trichloride (InCl₃), a metal organic β

-diketonate complex, cyclopentadienyl cycloheptatrienyl titanium (CpTiChT), aluminum trichloride (AlCl₃), titanium iodide (Ti_xI_y), cyclooctatetraene cyclopentadienyl titanium ((Cot)(Cp)Ti), bis(cyclopentadienyl)titanium diazide, tungsten carbonyl (W_x(CO)_y), bis(cyclopentadienyl)ruthenium (II) (Ru(Cp)₂), and ruthenium trichloride (RuCl₃).

8. The method of claim 1, wherein the at least a portion of the source material is dissolved in the solvent before the source material is introduced into at least one solid source material holder.

9. The method of claim 1, further comprising vaporizing at least a portion of the source material to form vaporized source material, and flowing the vaporized source material through a porous frit.

10. The method of claim 1, wherein each solid source material holder is placed in the vaporizer ampoule prior to the removing of said solvent.

11. A vaporizer comprising:

a vaporizer ampoule wall defining an internal compartment;

a plurality of solid source material holders disposed at different levels within the internal compartment; and

a solid source material disposed within the internal compartment, the solid source material comprising a material processed by dissolution in a solvent followed by removal of the solvent;

wherein at least one solid source material holder has a solid source material support surface and a thermally conductive holder sidewall extending above the solid source material support surface; and

wherein each holder sidewall is adapted to be in substantial thermal contact with the vaporizer ampoule wall at an ampoule operating temperature, and the ampoule wall is adapted to transfer heat to the thermally conductive holder sidewall.

12. The vaporizer of claim 11, further comprising a heating element adapted to supply heat to any of (i) the ampoule wall, (ii) the sidewall, and (iii) the solid source material.

13. The vaporizer of claim 11, wherein each solid source material holder includes a solid source material support surface defining a plurality of gas flow passages.

14. The vaporizer of claim 11, wherein the vaporizer includes a gas inlet that is connectable to a first gas source and is adapted to supply a first gas to the internal compartment.

15. The vaporizer of claim 11, comprising an outlet and a porous frit arranged to receive a flow of vaporized source material delivered to or through the outlet.

16. The vaporizer of claim 11, coupled in vapor delivery relationship to a process tool adapted to perform at least one step in the manufacture of a semiconductor device.

17. The vaporizer of claim 11, wherein the solid source material comprises a metal complex.