CA2515196A1 - Free-standing diamond structures and methods - Google Patents
Free-standing diamond structures and methods Download PDFInfo
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- CA2515196A1 CA2515196A1 CA002515196A CA2515196A CA2515196A1 CA 2515196 A1 CA2515196 A1 CA 2515196A1 CA 002515196 A CA002515196 A CA 002515196A CA 2515196 A CA2515196 A CA 2515196A CA 2515196 A1 CA2515196 A1 CA 2515196A1
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 82
- 239000010432 diamond Substances 0.000 title claims abstract description 82
- 238000000034 method Methods 0.000 title claims abstract description 57
- 239000000758 substrate Substances 0.000 claims abstract description 41
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 14
- 229910052710 silicon Inorganic materials 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000010899 nucleation Methods 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 125000004432 carbon atom Chemical group C* 0.000 claims description 5
- 238000003486 chemical etching Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 238000000151 deposition Methods 0.000 claims description 2
- 239000000446 fuel Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims 5
- 239000004215 Carbon black (E152) Substances 0.000 claims 1
- 238000005530 etching Methods 0.000 claims 1
- 229930195733 hydrocarbon Natural products 0.000 claims 1
- 150000002430 hydrocarbons Chemical class 0.000 claims 1
- 239000000463 material Substances 0.000 description 6
- 230000006911 nucleation Effects 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000004050 hot filament vapor deposition Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000615 nonconductor Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- 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
- C23C16/22—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 deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
-
- 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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
-
- 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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0254—Physical treatment to alter the texture of the surface, e.g. scratching or polishing
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/10—Heating of the reaction chamber or the substrate
- C30B25/105—Heating of the reaction chamber or the substrate by irradiation or electric discharge
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/04—Diamond
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The present invention is directed in one aspect to methods of making free-standing, internally-supported, three-dimensional objects having an outer surface comprising a plurality of intersecting facets wherein a sub-set of the intersecting facets have a diamond layer of substantially uniform thickness.
The diamond layer may be formed by chemical vapor deposition (CVD) over the surface of a substrate that has been fabricated to form a mold defining the sub-set of intersecting facets. A backing layer may be formed over at least a portion of the exposed diamond layer to enhance the rigidity of the layer when the substrate is removed.
The diamond layer may be formed by chemical vapor deposition (CVD) over the surface of a substrate that has been fabricated to form a mold defining the sub-set of intersecting facets. A backing layer may be formed over at least a portion of the exposed diamond layer to enhance the rigidity of the layer when the substrate is removed.
Description
FREE-STANDING DIAMOND STRUCTURES AND METHODS
CLAIM OF PRIORITY
[0001] This application claims the benefit of the filing date priority of U.S.
Provisional Application No. 601445,237 :fled February 6, 2003; No. 60/494,089 filed August 12, 2003; and No. 60/494,095 filed August 12, 1003.
BACKGR~UND ~F THE INVENTI~N
CLAIM OF PRIORITY
[0001] This application claims the benefit of the filing date priority of U.S.
Provisional Application No. 601445,237 :fled February 6, 2003; No. 60/494,089 filed August 12, 2003; and No. 60/494,095 filed August 12, 1003.
BACKGR~UND ~F THE INVENTI~N
[0002] The present invention relates to free-standing objects having laboratory grown diamond surfaces and methods f~r fabricating such objects. fore parhicularly, the present invention is directed to such objects and methods wherein the outer surface of the object includes a plurality of intersecting facets having a diamond layer.
[0~03] hiamond is one of the host ~;echnologically and scientifically valuable materials found in nature due to its combination of high resistance to thermal shocks e~~treme hardness, excellent infrared transparency, and excellent semiconductor , proper ties.
[~004] Diamond has the highest l~nown isotropic thermal c~r~ductivity and a relatively low expansion coefficient thus providing it with desirable resistance to thermal shock. Because of these pxoperties, diamond has found increasing use as a thermal management material in electronic packaging of devices such as high power laser diodes, ultichip anodules, and other microelectronic devices.
[0005] Diamond is also the hardest known material and has desirable resistance to abrasion. Thus diamond components and coatings have found increasing use as wear resistance elements in various mechanical devices and in cutting and grinding tools.
Diamond is also highly resistant to corrosion.
[0006] Diamond is also a good electrical insulator, but can be synthesized to be electrically conducting by the addition of certain elements such as boron to the growth SUBSTITUTE SHEET (R,ULE 26) atmosphere. Diamond is also used in many semiconductor devices including high-power transistors, resistors, capacitors, FET's, and integrated circuits.
[0007] The scarcity and high cost of natural diamond has prohibited its widespread commercial use. However, the development of various methods for synthesizing diamond has made the widespread commercial use of diamond possible. The most commercially promising method for synthesizing diamond includes the growth of diamond by chemical vapor deposition (CVD).
(000] Diamond synthesis by CVD has become a well established art. It is known that diamond coatings on various objects may be synthesized, as well as free-standing objects. Typically, the free-standing objects have been fabricated by deposition of diamond on planar substrates or substrates having relatively simple cavities formed therein. For example, LT.S. Patent l~To. 69132,27 discloses forming solid generally pyramidal or conical diamond microchip emitters by plasma enhanced CVD by growing diamond to fill cavities formed in the silicon substrate. However, there remains a need for methods of making free-standing, internally-supported, three-dimensional obj acts having an outer surface comprising a plurality of intersecting facets (planar or non-planar), wherein at least a sub-set of the intersecting facets have a diamond layer.
[0009] Accordingly, it is an object of the present invention to obviate many of the deficiencies in the prior art and to provide novel methods of making free-standing structures having diamond surfaces.
[0010] It is another object of the present invention to provide novel methods of making structures using diamond CVD.
[0011] It is yet another object of the present invention to provide novel structures formed by diamond CVD.
[0012] It is still another object of the present invention to provide novel methods of making free-standing structures having an exposed diamond surface.
[0013] It is a further object of the present invention to provide novel methods of making internally-supported structures having an exposed diamond surface.
[0014] These and many other objects and advantages of the present invention will be readily apparent to one skilled in the art to which the invention pertains from a perusal of the claims, the appended drawings, and the following detailed description of the preferred embodiments.
DETAILED DESCRIPTI~N ~F THE DRAWINGS
[0015] Figure 1 is an illustration showing the steps of the preferred embodiment of the present invention.
DESCRIPTI~II~TT ~F PI~FEI~ED EMS~DIMENTS
[001] In one aspect, the present invention is directed to methods ofmaking free-standing, internally-supported, three-dimensional objects having a diamond layer on at least a portion of the outer surface of the object. The diamond layer may be formed by any method of synthesizing diamond such as high-pressure, high-temperature (IiPI-IT) methods or CAD. In accordance with the preferred embodiment of the present invention, the diamond is synthesized by CVD.
[0017] In the diamond CVD methods according to the present invention, a mixture of hydrogen and carbon-containing gases is activated to obtain a region of gas-phase non-equilibl-ium adjacent the substrate on which the diamond will be grown. The carbon-containing gas may be selected from a large variety of gases including methane, aliphatic and aromatic hydrocarbons, alcohols, ketones, amines, esters, carbon monoxide, carbon dioxide, and halogens. Methane is used according to the preferred embodiment of the invention.
[0018] The mixture of gases is energized to obtain a region of gas-phase non-equilibrium adjacent the substrate on which the diamond will be grown. A
variety of gas-phase activation techniques may be used and these techniques may be categorized as either hot-filament CVD, plasma-assisted CVD, or flame CVD. In plasma-assisted CVD
the plasma may be generated by a number of energy sources including microwave, radio-frequency, or direct current electric fields.
[0019] The substrate may be any material suitable for nucleating and growing diamond such as semiconductor, metal, and insulator materials. Generally, the nucleation rates are much higher on carbide forming substrates (e.g., Si, Mo, and ~ than on substrates that do not form carbides. According to the preferred embodiment of the present invention, silicon substrates are used in view of the desirable nucleation rates and well known fabrication techniques of silicon.
[0020] The surface of the substrate on which the diamond will be grown may be pretreated by ~rarious techniques to enhance diamond nucleation and improve the nucleation density of diamond on the surface. Such methods may include (i) scratching, abrading, or blasting the surface with diamond particles or paste, (ii) seeding the surface with submicron powders such as diamond, silicon, or c~llT, (iii) biasing the substrate, (iv) carburi~ation, (v) pulsed laser irradiation, and (vi) ion implantation.
[0021] In accordance with the preferred embodiment of the present invention, a free-standing, internally-supported, three-dimensional object is provided having an outer surface comprising a plurality of intersecting facets wherein at least a sub-set of the intersecting facets have a diamond layer of substantially uniform depth. The teen "facet"
as used herein, includes a surface or face that is either planar or non-planar.
[0022] Figure 1 illustrates the various steps of the preferred embodiment of the present invention. With reference to Figure 1, a silicon substrate 10 is fabricated using conventional fabrication techniques to form a mold having an exposed surface defining the sub-set of intersecting facets. A diamond layer 14 of generally uniform thickness is grown over the exposed surface 12 of the substrate 10 by any suitable method such as hot-filament CVD or plasma-assisted CVD.
[0~03] hiamond is one of the host ~;echnologically and scientifically valuable materials found in nature due to its combination of high resistance to thermal shocks e~~treme hardness, excellent infrared transparency, and excellent semiconductor , proper ties.
[~004] Diamond has the highest l~nown isotropic thermal c~r~ductivity and a relatively low expansion coefficient thus providing it with desirable resistance to thermal shock. Because of these pxoperties, diamond has found increasing use as a thermal management material in electronic packaging of devices such as high power laser diodes, ultichip anodules, and other microelectronic devices.
[0005] Diamond is also the hardest known material and has desirable resistance to abrasion. Thus diamond components and coatings have found increasing use as wear resistance elements in various mechanical devices and in cutting and grinding tools.
Diamond is also highly resistant to corrosion.
[0006] Diamond is also a good electrical insulator, but can be synthesized to be electrically conducting by the addition of certain elements such as boron to the growth SUBSTITUTE SHEET (R,ULE 26) atmosphere. Diamond is also used in many semiconductor devices including high-power transistors, resistors, capacitors, FET's, and integrated circuits.
[0007] The scarcity and high cost of natural diamond has prohibited its widespread commercial use. However, the development of various methods for synthesizing diamond has made the widespread commercial use of diamond possible. The most commercially promising method for synthesizing diamond includes the growth of diamond by chemical vapor deposition (CVD).
(000] Diamond synthesis by CVD has become a well established art. It is known that diamond coatings on various objects may be synthesized, as well as free-standing objects. Typically, the free-standing objects have been fabricated by deposition of diamond on planar substrates or substrates having relatively simple cavities formed therein. For example, LT.S. Patent l~To. 69132,27 discloses forming solid generally pyramidal or conical diamond microchip emitters by plasma enhanced CVD by growing diamond to fill cavities formed in the silicon substrate. However, there remains a need for methods of making free-standing, internally-supported, three-dimensional obj acts having an outer surface comprising a plurality of intersecting facets (planar or non-planar), wherein at least a sub-set of the intersecting facets have a diamond layer.
[0009] Accordingly, it is an object of the present invention to obviate many of the deficiencies in the prior art and to provide novel methods of making free-standing structures having diamond surfaces.
[0010] It is another object of the present invention to provide novel methods of making structures using diamond CVD.
[0011] It is yet another object of the present invention to provide novel structures formed by diamond CVD.
[0012] It is still another object of the present invention to provide novel methods of making free-standing structures having an exposed diamond surface.
[0013] It is a further object of the present invention to provide novel methods of making internally-supported structures having an exposed diamond surface.
[0014] These and many other objects and advantages of the present invention will be readily apparent to one skilled in the art to which the invention pertains from a perusal of the claims, the appended drawings, and the following detailed description of the preferred embodiments.
DETAILED DESCRIPTI~N ~F THE DRAWINGS
[0015] Figure 1 is an illustration showing the steps of the preferred embodiment of the present invention.
DESCRIPTI~II~TT ~F PI~FEI~ED EMS~DIMENTS
[001] In one aspect, the present invention is directed to methods ofmaking free-standing, internally-supported, three-dimensional objects having a diamond layer on at least a portion of the outer surface of the object. The diamond layer may be formed by any method of synthesizing diamond such as high-pressure, high-temperature (IiPI-IT) methods or CAD. In accordance with the preferred embodiment of the present invention, the diamond is synthesized by CVD.
[0017] In the diamond CVD methods according to the present invention, a mixture of hydrogen and carbon-containing gases is activated to obtain a region of gas-phase non-equilibl-ium adjacent the substrate on which the diamond will be grown. The carbon-containing gas may be selected from a large variety of gases including methane, aliphatic and aromatic hydrocarbons, alcohols, ketones, amines, esters, carbon monoxide, carbon dioxide, and halogens. Methane is used according to the preferred embodiment of the invention.
[0018] The mixture of gases is energized to obtain a region of gas-phase non-equilibrium adjacent the substrate on which the diamond will be grown. A
variety of gas-phase activation techniques may be used and these techniques may be categorized as either hot-filament CVD, plasma-assisted CVD, or flame CVD. In plasma-assisted CVD
the plasma may be generated by a number of energy sources including microwave, radio-frequency, or direct current electric fields.
[0019] The substrate may be any material suitable for nucleating and growing diamond such as semiconductor, metal, and insulator materials. Generally, the nucleation rates are much higher on carbide forming substrates (e.g., Si, Mo, and ~ than on substrates that do not form carbides. According to the preferred embodiment of the present invention, silicon substrates are used in view of the desirable nucleation rates and well known fabrication techniques of silicon.
[0020] The surface of the substrate on which the diamond will be grown may be pretreated by ~rarious techniques to enhance diamond nucleation and improve the nucleation density of diamond on the surface. Such methods may include (i) scratching, abrading, or blasting the surface with diamond particles or paste, (ii) seeding the surface with submicron powders such as diamond, silicon, or c~llT, (iii) biasing the substrate, (iv) carburi~ation, (v) pulsed laser irradiation, and (vi) ion implantation.
[0021] In accordance with the preferred embodiment of the present invention, a free-standing, internally-supported, three-dimensional object is provided having an outer surface comprising a plurality of intersecting facets wherein at least a sub-set of the intersecting facets have a diamond layer of substantially uniform depth. The teen "facet"
as used herein, includes a surface or face that is either planar or non-planar.
[0022] Figure 1 illustrates the various steps of the preferred embodiment of the present invention. With reference to Figure 1, a silicon substrate 10 is fabricated using conventional fabrication techniques to form a mold having an exposed surface defining the sub-set of intersecting facets. A diamond layer 14 of generally uniform thickness is grown over the exposed surface 12 of the substrate 10 by any suitable method such as hot-filament CVD or plasma-assisted CVD.
[0023] The exposed surface 12 may be pretreated by any suitable technique to enhance the diamond nucleation and nucleation density on the exposed surface.
Typically, the exposed surface is pretreated by seeding the surface with carbon atoms 16.
The pretreatment of the exposed surface may be important in order to ensure growth of the diamond in the shape of the sub-set of facets which may be relatively complex.
[0024] In some instances, a backing layer 18 may be formed over at least portions of the exposed surface of the newly grown diamond layer to provide structural support to the diamond layer when the substrate is removed. Any material that will adhere to the exposed diamond and enhance the rigidity of the diamond layer 14 is suitable for the backing layer 1 ~ (e.g., epoxy, plastic, viscous polymers that harden, glass, etc.). The backing layer may be electrically conductive or non-conductive as desired.
[002] once the backing layer 1 ~ is formed as desired, the substrate 10 is removed to expose the surface 20 of the diamond layer 14 grown contiguous to the substrate which has been defined by the mold formed by the substrate. The substrate 10 may be removed by ally suitable means such as chemical etching. The diamond layer 14 may then be treated as desired.
[0026] The free-standing objects made according to the present invention may find utility in a variety of applications such as backward wave oscillators, bi-polar plates for fuel cells, traveling wave tubes, microchannel plates, and a multitude of other devices having a surface comprising a plurality of intersecting facets wherein a sub-set of intersecting facets have a diamond layer of substantially uniform thickness.
[0027] While preferred embodiments of the present invention have been described, it is to be understood that the embodiments described are illustrative only and that the scope of the invention is to be defined solely by the appended claims when accorded a full range of equivalence, many variations and modifications naturally occurring to those of skill in the art from a perusal hereof.
Typically, the exposed surface is pretreated by seeding the surface with carbon atoms 16.
The pretreatment of the exposed surface may be important in order to ensure growth of the diamond in the shape of the sub-set of facets which may be relatively complex.
[0024] In some instances, a backing layer 18 may be formed over at least portions of the exposed surface of the newly grown diamond layer to provide structural support to the diamond layer when the substrate is removed. Any material that will adhere to the exposed diamond and enhance the rigidity of the diamond layer 14 is suitable for the backing layer 1 ~ (e.g., epoxy, plastic, viscous polymers that harden, glass, etc.). The backing layer may be electrically conductive or non-conductive as desired.
[002] once the backing layer 1 ~ is formed as desired, the substrate 10 is removed to expose the surface 20 of the diamond layer 14 grown contiguous to the substrate which has been defined by the mold formed by the substrate. The substrate 10 may be removed by ally suitable means such as chemical etching. The diamond layer 14 may then be treated as desired.
[0026] The free-standing objects made according to the present invention may find utility in a variety of applications such as backward wave oscillators, bi-polar plates for fuel cells, traveling wave tubes, microchannel plates, and a multitude of other devices having a surface comprising a plurality of intersecting facets wherein a sub-set of intersecting facets have a diamond layer of substantially uniform thickness.
[0027] While preferred embodiments of the present invention have been described, it is to be understood that the embodiments described are illustrative only and that the scope of the invention is to be defined solely by the appended claims when accorded a full range of equivalence, many variations and modifications naturally occurring to those of skill in the art from a perusal hereof.
Claims (34)
1. A method of making a free-standing, internally-supported, three-dimensional object, the outer surface of the object comprising a plurality of intersecting facets, at least a sub-set of said intersecting facets having a diamond layer of substantially uniform depth, said method comprising the steps of:
(a) providing a mold having an exposed surface defining the sub-set of intersecting facets;
(b) growing a diamond layer of substantially uniform depth over the exposed surface;
(c) depositing a backing layer over at least a portion of the diamond layer;
and (d) removing the mold to expose the surface of the diamond layer grown immediately contiguous to the mold.
(a) providing a mold having an exposed surface defining the sub-set of intersecting facets;
(b) growing a diamond layer of substantially uniform depth over the exposed surface;
(c) depositing a backing layer over at least a portion of the diamond layer;
and (d) removing the mold to expose the surface of the diamond layer grown immediately contiguous to the mold.
2. The method of Claim 1 wherein the mold is a silicon substrate fabricated to define the sub-set of intersecting facets.
3. The method of Claim 2 wherein the mold is removed by chemical etching.
4. The method of Claim 1 further including the step of pretreating the exposed surface of the mold to enhance the growth of the diamond layer.
5. The method of Claim 4 wherein carbon atoms are deposited on the exposed surface of the mold to enhance the growth of the diamond layer.
6. The method of Claim 5 wherein the carbon atoms are deposited on the exposed surface of the mold by exposing the surface to a carbon containing plasma.
7. The method of Claim 1 wherein the sub-set of intersecting facets includes planar facets.
8. The method of Claim 1 wherein the sub-set of intersecting facets includes non-planar facets.
9. A method of fabricating a free-standing object comprising a three-dimensional structure covered by a diamond film having an exposed surface, said method comprising the steps of:
growing a diamond film on a preselected exposed surface of a substrate;
providing a backing on at least a portion of the grown diamond film; and removing the substrate to expose the diamond surface defined by the preselected surface of the substrate on which the diamond was grown.
growing a diamond film on a preselected exposed surface of a substrate;
providing a backing on at least a portion of the grown diamond film; and removing the substrate to expose the diamond surface defined by the preselected surface of the substrate on which the diamond was grown.
10. The method of Claim 9 wherein the substrate is silicon.
11. The method of Claim 9 including the further step of pretreating the preselected exposed surface to enhance the growth of diamond thereon.
12. The method of Claim 11 wherein a carbon seed layer is formed on the preselected exposed surface of the substrate.
13. The method of Claim 9 wherein the preselected surface of the substrate includes the intersection of two facets.
14. A method of fabricating a free-standing, internally-supported, three-dimensional object, the outer surface of the object comprising a plurality of intersecting facets, at least a sub-set of said intersecting facets having an exposed diamond surface, said method comprising the steps of:
growing a diamond film on a preselected exposed surface of a substrate;
providing a backing layer covering at least a portion of the grown diamond film;
and removing the substrate so that the exposed diamond surface is the surface grown immediately contiguous to the substrate.
growing a diamond film on a preselected exposed surface of a substrate;
providing a backing layer covering at least a portion of the grown diamond film;
and removing the substrate so that the exposed diamond surface is the surface grown immediately contiguous to the substrate.
15. The method of Claim 14 wherein the substrate is silicon.
16. The method of Claim 15 wherein the substrate is removed by chemical etching.
17. The method of Claim 14 wherein the backing layer covers the entire diamond film.
18. The method of Claim 14 wherein the backing layer is electrically conducting.
19. The method of Claim 14 wherein the backing layer is electrically non-conducting.
20. The method of Claim 19 wherein the backing layer is epoxy.
21. The method of Claim 14 including the further step of forming a carbon seed layer on the preselected exposed surface of the substrate to facilitate the growth of the diamond film thereon.
22. The method of Claim 21 wherein the diamond seed layer is formed by exposing the preselected exposed surface of the substrate to a carbon containing activated gas.
23. The method of Claim 22 wherein the diamond seed layer is formed by:
grounding the substrate;
providing ionized carbon atoms; and exposing the preselected exposed surface of the substrate to the ionized carbon atoms.
grounding the substrate;
providing ionized carbon atoms; and exposing the preselected exposed surface of the substrate to the ionized carbon atoms.
24. The method of Claim 22 wherein the activated gas is a plasma.
25. The method of Claim 24 wherein the plasma is formed by energizing a mixture of hydrogen and hydrocarbon gases.
26. The method of Claim 22 wherein the diamond seed layer is formed by chemical vapor deposition.
27. The method of Claim 14 wherein the diamond is grown by chemical vapor deposition.
28. The method of Claim 14 wherein the intersecting facets include planar facets.
29. The method of Claim 14 wherein the intersecting facets include non-planar facets.
30. The method of Claim 14 wherein the exposed diamond surface forms the surface of a waveguide.
31. The method of Claim 14 wherein the object is a bi-polar plate for a fuel cell.
32. A method of making a free-standing, internally-supported, three-dimensional object, the outer surface of the object comprising a plurality of intersecting facets, at least a sub-set of said intersecting facets having a diamond layer of substantially uniform depth, said method comprising the steps of:
(a) fabricating a silicon substrate to provide a molding surface defining the sub-set of intersecting facets;
(b) seeding the molding surface of the substrate with carbon;
(c) growing a diamond layer of substantially uniform depth over the molding surface of the substrate;
(d) forming an internally-supporting backing layer over the diamond layer; and (e) chemically etching the substrate to expose the surface of the diamond layer grown contiguous to the molding surface of the substrate.
(a) fabricating a silicon substrate to provide a molding surface defining the sub-set of intersecting facets;
(b) seeding the molding surface of the substrate with carbon;
(c) growing a diamond layer of substantially uniform depth over the molding surface of the substrate;
(d) forming an internally-supporting backing layer over the diamond layer; and (e) chemically etching the substrate to expose the surface of the diamond layer grown contiguous to the molding surface of the substrate.
33. The method of Claim 32 wherein molding surface is seeded by chemical vapor deposition.
34. The method of Claim 32 wherein the diamond layer is grown by chemical vapor deposition.
Applications Claiming Priority (7)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US44523703P | 2003-02-06 | 2003-02-06 | |
| US60/445,237 | 2003-02-06 | ||
| US49409503P | 2003-08-12 | 2003-08-12 | |
| US49408903P | 2003-08-12 | 2003-08-12 | |
| US60/494,089 | 2003-08-12 | ||
| US60/494,095 | 2003-08-12 | ||
| PCT/US2004/003518 WO2004072319A2 (en) | 2003-02-06 | 2004-02-06 | Free-standing diamond structures and methods |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2515196A1 true CA2515196A1 (en) | 2004-08-26 |
Family
ID=32872752
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002515196A Abandoned CA2515196A1 (en) | 2003-02-06 | 2004-02-06 | Free-standing diamond structures and methods |
Country Status (6)
| Country | Link |
|---|---|
| EP (1) | EP1601807A4 (en) |
| JP (1) | JP2007524554A (en) |
| KR (1) | KR100700339B1 (en) |
| AU (1) | AU2004211648B2 (en) |
| CA (1) | CA2515196A1 (en) |
| WO (1) | WO2004072319A2 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB201209424D0 (en) | 2012-05-28 | 2012-07-11 | Element Six Ltd | Free-standing non-planar polycrystalline synthetic diamond components |
| KR101391179B1 (en) | 2012-10-05 | 2014-05-08 | 한국과학기술연구원 | Attenuated total reflection type waveguide mode resonance sensor using nanocrystalline diamond and method for manufacturing waveguide made of nanocrystalline diamond |
| JP6636239B2 (en) * | 2014-08-29 | 2020-01-29 | 国立大学法人電気通信大学 | Method for producing single crystal diamond, single crystal diamond, method for producing single crystal diamond substrate, single crystal diamond substrate and semiconductor device |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5514885A (en) * | 1986-10-09 | 1996-05-07 | Myrick; James J. | SOI methods and apparatus |
| JP3549227B2 (en) * | 1993-05-14 | 2004-08-04 | 株式会社神戸製鋼所 | Highly oriented diamond thin film |
| JPH11209194A (en) * | 1998-01-23 | 1999-08-03 | Sumitomo Electric Ind Ltd | Composition hard film, forming method of the film and wear resistant part |
| US6659161B1 (en) * | 2000-10-13 | 2003-12-09 | Chien-Min Sung | Molding process for making diamond tools |
-
2004
- 2004-02-06 CA CA002515196A patent/CA2515196A1/en not_active Abandoned
- 2004-02-06 KR KR1020057014525A patent/KR100700339B1/en not_active IP Right Cessation
- 2004-02-06 JP JP2006503393A patent/JP2007524554A/en active Pending
- 2004-02-06 WO PCT/US2004/003518 patent/WO2004072319A2/en active Search and Examination
- 2004-02-06 EP EP04709095A patent/EP1601807A4/en not_active Withdrawn
- 2004-02-06 AU AU2004211648A patent/AU2004211648B2/en not_active Ceased
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| EP1601807A4 (en) | 2008-01-23 |
| KR20060010718A (en) | 2006-02-02 |
| EP1601807A2 (en) | 2005-12-07 |
| KR100700339B1 (en) | 2007-03-29 |
| AU2004211648A1 (en) | 2004-08-26 |
| WO2004072319A2 (en) | 2004-08-26 |
| JP2007524554A (en) | 2007-08-30 |
| WO2004072319A3 (en) | 2006-08-17 |
| AU2004211648B2 (en) | 2008-10-02 |
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