WO1998041670A1 - Internally heated pyrolysis zone and a method wherein use is made of this zone - Google Patents
Internally heated pyrolysis zone and a method wherein use is made of this zone Download PDFInfo
- Publication number
- WO1998041670A1 WO1998041670A1 PCT/US1998/003657 US9803657W WO9841670A1 WO 1998041670 A1 WO1998041670 A1 WO 1998041670A1 US 9803657 W US9803657 W US 9803657W WO 9841670 A1 WO9841670 A1 WO 9841670A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- tube
- zone
- gas
- heating element
- centerline
- Prior art date
Links
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45563—Gas nozzles
- C23C16/4557—Heated nozzles
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4488—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by in situ generation of reactive gas by chemical or electrochemical reaction
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/452—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by activating reactive gas streams before their introduction into the reaction chamber, e.g. by ionisation or addition of reactive species
Definitions
- the present invention relates generally to an internally heated pyrolysis zone, and more specifically to such an apparatus that can be used in the vacuum deposition of parylene monomer.
- Conformal coatings having low dielectric constants and high melting temperatures are desirable for many applications, including the medical, electronics and automotive industries.
- Parylene polymers are poly-p-xylylenes which may be prepared with a parylene dimer. Parylene polymers generally have a structure:
- parylene dimers wherein X is typically a hydrogen atom or a halogen atom.
- parylene dimers include the following:
- parylene polymer layers are formed by a vapor deposition method that is performed using a vacuum apparatus 10 as shown in Fig. 1, such as disclosed in U.S. Patent No. 5,538,758 which is herein incorporated by reference.
- Apparatus 10 includes a vaporization zone 12, a pyrolysis zone 14, a post-pyrolysis zone 16 and a deposition chamber 18.
- the parylene dimer is vaporized in vaporization zone 12 and the dimer bond is then cleaved by pyrolysis in pyrolysis zone 14 to form parylene monomer having the structure:
- the parylene monomer passes through post-pyrolysis zone 16 which removes a substantial amount of undesired chemical species.
- the parylene monomer is then deposited onto the surface of a substrate 19 disposed within deposition chamber 18. Polymerization of the deposited parylene monomer occurs spontaneously to form the parylene polymer layer coating on the surface of substrate 19.
- Fig. 2 shows a pyrolysis zone 14 which includes a tube 20 with one or more electric tube heaters 22 disposed along the outer surface 24 of wall 26 of tube 20.
- Heaters 22 increase the temperature of tube 20 to heat the parylene dimer disposed within the interior of tube 20, resulting in cleavage of the parylene dimer bond and formation of the parylene monomer. Due to the arrangement of heaters 22, parylene dimer disposed adjacent the inner surface 28 of wall 26 of tube 20 is maintained at a higher temperature than parylene dimer disposed adjacent the centerline 29 of tube 20.
- tube 20 may not be effective in heating the parylene dimer flowing adjacent centerline 29 to a temperature high enough to pyrolyze the parylene dimer and form parylene monomer.
- overpyrolysis of parylene dimer adjacent inner surface 28 can occur, causing a carbonaceous residue to build up on surface 28.
- greater than about 1 weight percent of the vaporized parylene dimer results in carbonaceous buildup on inner surface 28.
- the present invention provides a deposition apparatus that comprises a deposition chamber, a tube and a heating element.
- the tube is in fluid communication with the deposition chamber, and the heating element is constructed and arranged so that the heating element preferentially heats the centerline of the tube relative to the inner surface of the tube.
- the present invention provides an apparatus for depositing a gas that comprises a deposition chamber, a tube and means for preferentially heating the centerline of the tube relative to the inner surface of the tube.
- the tube is in fluid communication with the deposition chamber.
- the present invention provides an apparatus for depositing parylene monomer.
- the apparatus comprises a first zone for providing parylene dimer, a pyrolysis zone, a heating element and a deposition chamber.
- the pyrolysis zone is designed to pyrolyze the parylene dimer to form the parylene monomer.
- the pyrolysis zone comprises a tube and a heating element.
- the tube is in fluid communication with the first zone and the deposition chamber.
- the heating element is constructed and arranged so that the heating element preferentially heats the centerline of the tube relative to the inner surface of the tube.
- the present invention provides an apparatus for depositing parylene monomer.
- the apparatus comprises a first zone for providing parylene dimer, a pyrolysis zone and a deposition chamber.
- the pyrolysis zone is designed to pyrolyze the parylene dimer to form parylene monomer.
- the pyrolysis zone comprises a tube and means for preferentially heating the centerline of the tube relative to the inner surface of the tube.
- the tube is in fluid communication with the first zone and the deposition chamber.
- the present invention provides a method of depositing a product gas onto a surface.
- the method comprises placing a first gas into a tube; heating first and second portions of the first gas to first and second temperatures, respectively, to form the product gas, the first portion of the first gas being adjacent the centerline of the tube, the second portion of the first gas being adjacent the inner surface of the tube, the first temperature being greater than the second temperature; and depositing the product gas onto the surface.
- FIG. 1 is a cross-sectional view of a deposition apparatus according to the related art
- Fig. 2 is a cross-sectional view of a pyrolysis zone according to the related art
- Fig. 3 is a cross-sectional view of a deposition apparatus according to one embodiment the present invention.
- Fig. 4 is a cross-sectional view of a pyrolysis zone according to one embodiment of the present invention.
- Fig. 3 shows one embodiment of a deposition apparatus 20 which includes a vaporization zone 12, a pyrolysis zone 40, a post-pyrolysis zone 16 and a deposition chamber 18.
- Pyrolysis zone 40 (Fig. 4) includes a tube 42, a heating element 44 disposed substantially along centerline
- tube 48 and a power supply 50 in electrical communication with element 44 via electrical connectors 51 and 53.
- Tube 42 is designed to be in fluid communication with vaporization zone 12 and post- pyrolysis zone 16 such that vaporized dimer can exit zone 12, be pyrolyzed to parylene monomer within tube 42 and pass to post-pyrolysis zone 16. Since pyrolysis occurs at temperatures of about 1000°C or less, inner surface 52 of wall 54 of tube 42 should be chemically inert to parylene dimer and parylene monomer within this temperature range.
- materials appropriate for use as wall 54 of tube 42 include, but are not limited to, quartz, stainless steel with a quartz inner surface, inconel with a quartz inner surface, monel with a quartz inner surface. Alternatively, the quartz may be partially or entirely replaced with certain ceramics, such as aluminum oxide, or beryllium oxide. Other such materials are known to those skilled in the art and are intended to be within the scope of the present invention.
- Tube 42 may have any dimensions that allow tube 42 to be used according to the Gorham process, such as described in U.S. Patent No. 5,538,758. Typically, tube 42 is from about three feet to about four feet long with a diameter of from about 32 millimeters to about 50 millimeters.
- Heating element 44 is designed to heat parylene dimer disposed within tube 42 to form parylene monomer.
- Element 44 may be heated using ohmic heating produced by applying a potential across element 44 using power supply 50. Therefore, element 44 should be formed from a material which is chemically inert to parylene dimer and parylene monomer at temperature of about 1000°C or less.
- An illustrative and nonlimiting list of such materials includes nichrome, platinum, platinum-iridium alloys, tungsten and other such materials which are known to those skilled in the art.
- element 44 may be in the shape of a coil with varying diameter.
- the largest diameter portions of element 44 should have a diameter that is about the same as the inner diameter of tube 44 such that the largest diameter portions of element 44 provide mechanical support for element 44 within tube 42.
- element 44 may be have a substantially constant diameter along its entire length within tube 42.
- mechanical support for element 44 may be provided by, for example, ceramic spacers, or perforated washers. While certain types of mechanical supports have been disclosed herein, it is to be understood that other supports may also be used so long as they are capable of supporting element 44 in its preferred position. It should be noted that such mechanical supports should not substantially reduce the throughput or flow rate of gas through tube 42.
- Element 44 is limited only in that it should be capable of preferentially heating a gas disposed along centerline 46 relative to inner surface 52 of tube 42 without substantially reducing the throughput or flow rate of gas through tube 42. Accordingly, in some embodiments, element 44 may be in the form of a mesh, a ribbon wire, a rounded wire, a rod with heat conducting fins or other such arrangements as will be apparent to those skilled in the art.
- parylene deposition may be carried out without substantial carbonaceous buildup on inner surface 52 of pyrolysis tube 42.
- less than about 1 weight percent of the vaporized parylene dimer forms carbonaceous material on inner surface 52, more preferably less than about 0.5 weight percent, and most preferably less than about 0.1 weight percent.
- pyrolysis tube 42 may include one or more components formed of pyrex, quartz or similar materials that are bent and disposed within the interior of tube 42 such that a gas flowing through tube 42 can follow a tortuous path. Such devices, often referred to as static mixers, are known to those skilled in the art.
- heating element 44 may also be disposed within the interior of tube 42 as described herein.
- tube 48 should be in fluid communication with both vaporization zone 12 and deposition zone 18.
- tube 48 may include heating element 44 within the interior of tube 48 and one or more heaters 22 disposed along the outer surface of wall 54.
Abstract
Description
Claims
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU61855/98A AU6185598A (en) | 1997-03-14 | 1998-02-25 | Internally heated pyrolysis zone and a method wherein use is made of this zone |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US08/818,537 | 1997-03-14 | ||
US08/818,537 US6051276A (en) | 1997-03-14 | 1997-03-14 | Internally heated pyrolysis zone |
Publications (1)
Publication Number | Publication Date |
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WO1998041670A1 true WO1998041670A1 (en) | 1998-09-24 |
Family
ID=25225776
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/US1998/003657 WO1998041670A1 (en) | 1997-03-14 | 1998-02-25 | Internally heated pyrolysis zone and a method wherein use is made of this zone |
Country Status (4)
Country | Link |
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US (1) | US6051276A (en) |
AU (1) | AU6185598A (en) |
TW (1) | TW561194B (en) |
WO (1) | WO1998041670A1 (en) |
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US20030050692A1 (en) * | 2000-12-22 | 2003-03-13 | Avantec Vascular Corporation | Delivery of therapeutic capable agents |
US20050125054A1 (en) * | 2000-12-22 | 2005-06-09 | Avantec Vascular Corporation | Devices delivering therapeutic agents and methods regarding the same |
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US20020082679A1 (en) * | 2000-12-22 | 2002-06-27 | Avantec Vascular Corporation | Delivery or therapeutic capable agents |
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1997
- 1997-03-14 US US08/818,537 patent/US6051276A/en not_active Expired - Lifetime
-
1998
- 1998-02-25 WO PCT/US1998/003657 patent/WO1998041670A1/en active Application Filing
- 1998-02-25 AU AU61855/98A patent/AU6185598A/en not_active Abandoned
- 1998-04-04 TW TW087103732A patent/TW561194B/en not_active IP Right Cessation
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Also Published As
Publication number | Publication date |
---|---|
AU6185598A (en) | 1998-10-12 |
TW561194B (en) | 2003-11-11 |
US6051276A (en) | 2000-04-18 |
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