US4368098A — Epitaxial composite and method of making

Claim 1

Independent Claim 96 words

An organo-metallic process for producing an epitaxial film of Group III-V semiconductor disposed on a single crystal substrate, said process employing an open reactor and comprising the steps of: heating said substrate in said open reactor, introducing into said open reactor a fist material containing a hydride or halide-free alkyl compound of at least one Group V constituent of said semiconductor, and, as a second material, at least one halide-free alkyl compound containing at least one of the Group III constituents of said semiconductor, and exhausting said open reactor to pressure not greater than one atmosphere.

Claim 2

Dependent Claim 96 words

An organo-metallic process for producing an epitaxial film of Group III-V semiconductor disposed on a single crystal substrate, said process employing an open reactor and comprising the steps of: heating said substrate in said open reactor, introducing into said open reactor a fist material containing a hydride or halide-free alkyl compound of at least one Group V constituent of said semiconductor, and, as a second material, at least one halide-free alkyl compound containing at least one of the Group III constituents of said semiconductor, and exhausting said open reactor to pressure not greater than one atmosphere.

Claim 3

Dependent Claim 130 words

A process for producing an epitaxial film of a Group III-V semiconductor disposed on a single crystal substrate, said process employing an open reactor having exterior walls defining an interior chamber and comprising the steps of: providing a single heated zone within said interior chamber of said open reactor without substantially heating said exterior walls of said reactor, heating said substrate in said single, heated zone of said interior chamber of said open reactor, and introducing into said reactor a first halide-free material containing at least one Group V constituent of said semiconductor, and, as a second material, at least one halide-free organic alkyl compound containing at least one of the Group III constituents of said semiconductor, and exhausting said open reactor to a pressure not greater than one atmosphere.

Claim 4

Dependent Claim 130 words

A process for producing an epitaxial film of a Group III-V semiconductor disposed on a single crystal substrate, said process employing an open reactor having exterior walls defining an interior chamber and comprising the steps of: providing a single heated zone within said interior chamber of said open reactor without substantially heating said exterior walls of said reactor, heating said substrate in said single, heated zone of said interior chamber of said open reactor, and introducing into said reactor a first halide-free material containing at least one Group V constituent of said semiconductor, and, as a second material, at least one halide-free organic alkyl compound containing at least one of the Group III constituents of said semiconductor, and exhausting said open reactor to a pressure not greater than one atmosphere.

Claim 5

Dependent Claim 139 words

An organo-metallic process for producing an epitaxial film of a Group III-V semiconductor directly on a single crystal substrate, said process comprising the steps of: providing a first material containing a hydride or alkyl of at least one Group V constituent of said semiconductor, providing a second, metal-organic source material comprising at least one organic alkyl compound containing at least one of the Group III constituents of said semiconductor, disposing said substrate in an open reactor, providing a controlled, elevated temperature zone within only the interior of said reactor for heating said substrate to a required temperature for deposition of said film thereon, introducing said first and second materials into said reactor and heating said substrate in accordance with said controlled temperature zone to effect the deposition of an epitaxial film of the Group III-V semiconductor on said substrate.

Claim 6

Dependent Claim 139 words

An organo-metallic process for producing an epitaxial film of a Group III-V semiconductor directly on a single crystal substrate, said process comprising the steps of: providing a first material containing a hydride or alkyl of at least one Group V constituent of said semiconductor, providing a second, metal-organic source material comprising at least one organic alkyl compound containing at least one of the Group III constituents of said semiconductor, disposing said substrate in an open reactor, providing a controlled, elevated temperature zone within only the interior of said reactor for heating said substrate to a required temperature for deposition of said film thereon, introducing said first and second materials into said reactor and heating said substrate in accordance with said controlled temperature zone to effect the deposition of an epitaxial film of the Group III-V semiconductor on said substrate.

Claim 7

Dependent Claim 25 words

The process according to claim 1 in which a single heated zone is provided in the interior of the reactor without substantially heating said reactor.

Claim 8

Dependent Claim 36 words

The process according to claim 1 in which said first and second materials are introduced under reduced pressure conditions in the reactor and the source of the constituents consists of substantially pure forms of said materials.

Claim 9

Dependent Claim 18 words

The process according to claim 1, 2, or 3 in which said materials are introduced in flowing hydrogen.

Claim 10

Dependent Claim 18 words

The process according to claim 1, 2, or 3 in which said materials are introduced in flowing nitrogen.

Claim 11

Dependent Claim 14 words

The process according to claim 1 in which said first material comprises a hydride.

Claim 12

Dependent Claim 20 words

The process according to claim 1 in which at least one of said alkyl compounds comprises more than one alkyl.

Claim 13

Dependent Claim 22 words

The process according to claim 1 in which the first material comprises more than one alkyl compound containing a Group V constituent.

Claim 14

Dependent Claim 41 words

The process according to claim 1 in which said semiconductor comprises gallium arsenide, said first material comprises arsine, said second material is selected from the class consisting of trimethylgallium and triethylgallium, and said process is carried out in a hydrogen atmosphere.

Claim 15

Dependent Claim 41 words

The process according to claim 1 in which said semiconductor comprises gallium arsenide, said first compound comprises arsine, said second material is selected from the class consisting of trimethylgallium and triethylgallium, and said process is carried out in a nitrogen atmosphere.

Claim 16

Dependent Claim 41 words

The process according to claim 1 in which said semiconductor comprises gallium phosphide, said first compound comprises phosphine, said second material is selected from the class consisting of trimethylgallium and triethylgallium, and said process is carried out in a hydrogen atmosphere.

Claim 17

Dependent Claim 41 words

The process according to claim 1 in which said semiconductor comprises gallium phosphide, said first material comprises phosphine, said second material is selected from the class consisting of trimethylgallium and triethylgallium, and said process is carried out in a nitrogen atmosphere.

Claim 18

Dependent Claim 29 words

The process according to claim 1 in which said Group III constituent is selected from the class consisting of gallium, aluminum, indium and combinations of more than one thereof.

Claim 19

Dependent Claim 15 words

The process according to claim 1 further comprising: introducing a dopant-containing gas in said reactor.

Claim 20

Dependent Claim 18 words

The process according to claim 1 in which said first material is introduced before introducing said second material.

Claim 21

Dependent Claim 24 words

The process according to claim 17 in which said first material comprises a hydride and wherein said second material comprises at least one alkyl.

Claim 22

Dependent Claim 27 words

The process according to claim 18 in which said second material is selected from the class consisting of trimethylgallium and triethylgallium; trimethylaluminum and triethylaluminum; trimethylindium and triethylindium.

Claim 23

Dependent Claim 19 words

The process according to claim 17 further comprising: providing a small amount of gas phase etchant in said reactor.

Claim 24

Dependent Claim 13 words

The process according to claim 20 in which said etchant comprises hydrogen halide.

Claim 25

Dependent Claim 24 words

The process according to claim 20 in which said Group V constituent comprises arsenic and said etchant is provided from arsenic halide and hydrogen.

Claim 26

Dependent Claim 25 words

The process according to claim 20 in which said Group V constituent comprises phosphorus and said etchant is provided from a phosphorus halide and hydrogen.

Claim 27

Dependent Claim 23 words

The process according to claim 1 in which the amount of said first material introduced exceeds that stoichiometrically required to form said film.

Claim 28

Dependent Claim 23 words

The process according to claim 24 in which the first material comprises more than one of the alkyls including the Group V constituent.

Claim 29

Dependent Claim 16 words

The process according to claim 1 in which said compounds are introduced in flowing inert gas.

Claim 30

Dependent Claim 22 words

The process according to claim 26 in which said inert gas is one selected from the group consisting of helium and argon.

Claim 31

Dependent Claim 25 words

The process according to claim 1 in which said first material comprises a hydride and wherein said second material comprises more than one alkyl compound.

Claim 32

Dependent Claim 38 words

The process according to claim 28 in which at least one of said more than one alkyl compound comprising said second material is selected from the class consisting of trimethylgallium and triethylgallium; trimethylaluminum and triethylaluminum; trimethylindium and triethylindium.

Claim 33

Dependent Claim 21 words

The process according to claim 29 in which said hydride is selected from the class consisting of arsine, phosphine and stibine.

Claim 34

Dependent Claim 44 words

The process according to claim 1 in which said semiconductor comprises gallium arsenide, said first material comprises arsine, and said second material is selected from the class consisting of trimethylgallium and triethylgallium and said process is carried out in an atmosphere of inert gas.

Claim 35

Dependent Claim 14 words

The process of claim 31 in which said inert gas is helium or argon.

Claim 36

Dependent Claim 42 words

The process according to claim 1 in which said semiconductor comprises gallium phosphide, said first material comprises phosphine, said second material is selected from the class consisting of trimethylgallium and triethylgallium, and said process is carried out in an inert gas atmosphere.

Claim 37

Dependent Claim 14 words

The process of claim 33 in which said inert gas is helium or argon.

Claim 38

Dependent Claim 46 words

The process according to claim 1 in which said semiconductor is selected from a group consisting of III-V semiconductor alloys containing at least one of the Group III constituents Ga, Al and In and at least one of the Group V constituents As, P, and Sb.

Claim 39

Dependent Claim 42 words

The process according to claim 35 in which said second material is selected from a group of trialkyl Ga, Al, or In compounds and said process is carried out in an atmosphere selected from the class consisting of hydrogen, nitrogen, and helium.

Claim 40

Dependent Claim 38 words

The process according to claim 35 in which the composition of the Group V constituent is controlled by adjusting the relative concentration of more than one of the group consisting of arsine, phosphine and stibine in said reactor.

Claim 41

Dependent Claim 15 words

The process according to claim 1 in which said single crystal substrate is non-electrically insulating.

Claim 42

Dependent Claim 18 words

The process according to claim 38, 2 or 3 in which said single crystal substrate is a semiconductor.

Claim 43

Dependent Claim 15 words

The process according to claim 38, 2 or 3 in which the substrate is germanium.

Claim 44

Dependent Claim 13 words

The process according to claim 39 in which the substrate is silicon carbide.

Claim 45

Dependent Claim 15 words

The process according to claim 39 in which said substrate possesses a zinc blend structure.

Claim 46

Dependent Claim 22 words

The process according to claim 42 in which said substrate is selected from the class consisting of III-V semiconductors and semiconductor alloys.

Claim 47

Dependent Claim 30 words

The process according to claim 43 in which said substrate is selected from the class of III-V semiconductors consisting of GaAs, GaP, GaSb, AlAS, AlP. AlSb, InAs, InP, and InSb.

Claim 48

Dependent Claim 46 words

The process according to claim 43 in which said substrate is selected from a group consisting of III-V semiconductor alloys containing at least one of the Group III constituents Ga, Al or In and at least one of the Group III constituents As, P or Sb.

Claim 49

Dependent Claim 15 words

The process according to claim 1 in which said single crystal substrate is electrically insulating.

Claim 50

Dependent Claim 32 words

The process according to claim 46 in which said substrate is selected from the class consisting of sapphire, spinel, chrysoberyl, beryllium oxide, thorium oxide, calcium fluoride, barium fluoride and gadolinium gallium garnet.

Claim 51

Dependent Claim 29 words

The process according to claim 1 in which said Group V constituent is selected from the class consisting of arsenic, phosphorus, antimony and combinations of more than one thereof.

Claim 52

Dependent Claim 29 words

The process according to claim 48 in which said Group III constituent is selected from a class consisting of In, Ga, Al and mixtures of more than one thereof.

Claim 53

Dependent Claim 23 words

The process according to claim 1, 4 or 2 in which the single heated zone is about 650° C. to about 800° C.

Claim 54

Dependent Claim 37 words

A process according to claim 1, 4 or 2, further comprising the step of: controlling the introduction of said first and second materials into said open reactor to maintain a pressure therewithin of less than one atmosphere.

Claim 55

Dependent Claim 29 words

A process according to claim 1, 4 or 2, further comprising the step of: evacuating said open reactor to maintain a reduced pressure of less than one atmosphere therewithin.

Claim 56

Dependent Claim 95 words

A process for producing an epitaxial film of a Group III-V semiconductor disposed on a single crystal sapphire (α-aluminum oxide) substrate which process comprises: heating a substrate in a reactor with the orientation of the exposed surfaces of the substrate being the (0001), (1123) (0112), (1125), or (1126) crystallographic plane or being about 10° from the (0112) crystallographic plane and introducing into the reactor one or more gaseous hydrides or alkyls of As, Sb and P as Group V constituent and one or more gaseous alkyls of Ga, Al or In as Group III constituent.

Claim 57

Dependent Claim 95 words

A process for producing an epitaxial film of a Group III-V semiconductor disposed on a single crystal sapphire (α-aluminum oxide) substrate which process comprises: heating a substrate in a reactor with the orientation of the exposed surfaces of the substrate being the (0001), (1123) (0112), (1125), or (1126) crystallographic plane or being about 10° from the (0112) crystallographic plane and introducing into the reactor one or more gaseous hydrides or alkyls of As, Sb and P as Group V constituent and one or more gaseous alkyls of Ga, Al or In as Group III constituent.

Claim 58

Dependent Claim 100 words

A process for producing an epitaxial film of a Group III-V semiconductor disposed on a single crystal spinel substrate, which process comprises heating the substrate in a reactor with the orientation of the exposed surface of the substrate being the (110) crystallographic plane, and introducing into the reactor one or more gaseous hydrides or alkyls of As, Sb and P as Group V constituent, and one or more gaseous alkyls of Ga, Al or In as Group III constituent of the semiconductor, the (100) crystallographic plane of the film thereby deposited being parallel to the exposed plane of the spinel.

Claim 59

Dependent Claim 100 words

A process for producing an epitaxial film of a Group III-V semiconductor disposed on a single crystal spinel substrate, which process comprises heating the substrate in a reactor with the orientation of the exposed surface of the substrate being the (110) crystallographic plane, and introducing into the reactor one or more gaseous hydrides or alkyls of As, Sb and P as Group V constituent, and one or more gaseous alkyls of Ga, Al or In as Group III constituent of the semiconductor, the (100) crystallographic plane of the film thereby deposited being parallel to the exposed plane of the spinel.

Claim 60

Dependent Claim 26 words

A process according to claim 1, 2, 53 or 54 in which all of said materials, constituent compounds, hydrides and alkyls are introduced under reduced pressure.

Claim 61

Dependent Claim 33 words

A process according to claim 1, 2, 53 or 54 in which the Group V constituent hydride or alkyl is introduced into the reactor before the alkyl compound of the Group III constituent.

Claim 62

Dependent Claim 32 words

A process according to claim 1, 2, 53 or 54 in which the amount of the Group V constituent hydride or alkyl introduced exceeds that stoichiometrically required to form the said film.

Claim 63

Dependent Claim 28 words

A process according to claim 1, 2, 53 or 54 in which alkyl compounds of more than one of the Group V constituents are introduced into the reactor.

Claim 64

Dependent Claim 29 words

A process according to claim 1, 2, 53 or 54 in which the Ga, Al and In alkyl compounds are trimethylgallium or triethylgallium; trimethylaluminum or triethylaluminum; trimethylindium or triethylindium.

Claim 65

Dependent Claim 39 words

A process according to claim 1, 2, 53 or 54 in which the concentration of the Group V constituent is controlled by adjusting the relative concentration of more than one of arsine, phosphine and stibine present in the reactor.

Claim 66

Dependent Claim 22 words

A process according to claim 1, 2, 53 or 54 in which the constituent compounds are introduced in flowing Group O gas.

Claim 67

Dependent Claim 20 words

A process according to claim 1, 2, 53 or 54 in which the Group O gas is helium or argon.

Claim 68

Dependent Claim 22 words

A process according to any of claims 1, 2, 53 or 54 in which the constituent compounds are introduced in flowing nitrogen.

Claim 69

Dependent Claim 22 words

A process according to any of claims 1, 2, 53 or 54 in which the constituent compounds are introduced in flowing hydrogen.

Claim 70

Dependent Claim 20 words

A process as recited in claim 3 wherein there is provided a single controlled, elevated temperature zone in said reactor.

Claim 71

Dependent Claim 32 words

A process as recited in claim 3 or 65 wherein said substrate is heated to a temperature of from about 650° C. to about 800° C. in said controlled, elevated temperature zone.

Claim 72

Dependent Claim 17 words

A process as recited in claim 3 or 65 wherein said substrate comprises an electrically insulating material.

Claim 73

Dependent Claim 20 words

A process as recited in claim 3 or 65, performed in the absence of any halide material in said reactor.

Claim 74

Dependent Claim 51 words

A process as recited in claim 3 or 65, further comprising: providing a mixture of said first and second materials in the gaseous phases thereof within said temperature zone of said reactor with the amount of said first material introduced being in excess of that stoichiometrically required to form said film.

Claim 75

Dependent Claim 17 words

A process as recited in claim 3, further including: providing an inert gaseous atmosphere in said reactor.

Claim 76

Dependent Claim 55 words

A process as recited in claim 3, 65 or 70, wherein the step of introducing said materials comprises: introducing said first material at or prior to the time said substrate reaches the required temperature for achieving deposition, and introducing said metal-organic source material subsequently to said substrate being heated to said required temperature for deposition.

Claim 77

Dependent Claim 73 words

A process as recited in claim 3, 65 or 70, wherein the step of introducing said materials comprises: introducing said first material at or prior to the time said substrate reaches the required temperature for achieving deposition, and introducing said metal-organic source material subsequently to said substrate being heated to said required temperature for deposition, and introducing an amount of said first material in excess of that stoichiometrically required to form said film.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1986-01-10	1986-07-12	1987-01-11	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1990-01-10	1990-07-12	1991-01-11	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1994-01-10	1994-07-12	1995-01-11	$7700.00	Window Closed / Lapsed

Epitaxial composite and method of making

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