WO1992009108A1 - Oxydation d'arseniure de gallium - Google Patents

Oxydation d'arseniure de gallium Download PDF

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Publication number
WO1992009108A1
WO1992009108A1 PCT/US1991/007941 US9107941W WO9209108A1 WO 1992009108 A1 WO1992009108 A1 WO 1992009108A1 US 9107941 W US9107941 W US 9107941W WO 9209108 A1 WO9209108 A1 WO 9209108A1
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Prior art keywords
gaas
oxide
substrate
layer
oxidation
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English (en)
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Mark A. Hoffbauer
Jon B. Cross
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United States Department of Energy
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United States Department of Energy
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
    • H10P14/60—Formation of materials, e.g. in the shape of layers or pillars of insulating materials
    • H10P14/63—Formation of materials, e.g. in the shape of layers or pillars of insulating materials characterised by the formation processes
    • H10P14/6302—Non-deposition formation processes
    • H10P14/6304—Formation by oxidation, e.g. oxidation of the substrate
    • H10P14/6306—Formation by oxidation, e.g. oxidation of the substrate of the semiconductor materials
    • H10P14/6312—Formation by oxidation, e.g. oxidation of the substrate of the semiconductor materials of Group III-V semiconductors
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
    • H10P14/60—Formation of materials, e.g. in the shape of layers or pillars of insulating materials
    • H10P14/63—Formation of materials, e.g. in the shape of layers or pillars of insulating materials characterised by the formation processes
    • H10P14/6302—Non-deposition formation processes
    • H10P14/6304—Formation by oxidation, e.g. oxidation of the substrate
    • H10P14/6314—Formation by oxidation, e.g. oxidation of the substrate of a metallic layer
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
    • H10P14/60—Formation of materials, e.g. in the shape of layers or pillars of insulating materials
    • H10P14/69—Inorganic materials
    • H10P14/692—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses
    • H10P14/6938—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses the material containing at least one metal element, e.g. metal oxides, metal oxynitrides or metal oxycarbides
    • H10P14/6939—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses the material containing at least one metal element, e.g. metal oxides, metal oxynitrides or metal oxycarbides characterised by the metal
    • H10P14/69391—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses the material containing at least one metal element, e.g. metal oxides, metal oxynitrides or metal oxycarbides characterised by the metal the material containing aluminium, e.g. Al2O3

Definitions

  • This invention relates to gallium arsenide semiconductors and, more particularly, to the oxidation of surface layers of gallium arsenide semiconductors for semiconductor device fabrication. This invention is the result of a contract with the Department of Energy (Contract No. W-7405-ENG-36) .
  • Gallium arsenide is a semiconductor material that has properties complementary to silicon in many applications. Electrons move more readily through..GaAs than through Si, producing less waste heat than in Si. GaAs materials also have faster switching speeds and lower noise operating characteristics than Si materials. Yet another advantage is the capability to engineer the separation between its electronic bands, or energy levels, to obtain design flexibility in providing opto-electronic capabilities and transistor designs. See, e.g. , Brodsky, "Progress in Gallium Arsenide Semiconductors," Sci. Am., pp. 68-75 (February 1990) , incorporated herein by reference. As noted by Brodsky, a major problem in fabricating GaAs components is the lack of a usable native oxide for insulating adjacent components on chips.
  • Patent 4,474,829 issued October 2, 1984, to Peters, describes a process for forming a layer of native oxide on a substrate of a selected material, which might be selected from a group consisting of HgCdTe, GaAlAs, InP, InGaP, InSb, GaAs, GaSb, GaP, S, and Ge.
  • Atomic oxygen is formed in a chamber including the substrate and reacts on the surface to form a "native oxide" layer (defined to be a layer 10-100 A thick) on the substrate surface at temperatures from about 30-300°C.
  • a "native oxide” layer defined to be a layer 10-100 A thick
  • insulators and masking structures have been formed on GaAs substrates by other methods.
  • a gate-like structure is formed from a metal placed in contact with the GaAs to form a Shottky barrier gate.
  • Thin crystalline layers of aluminum gallium arsenide have been grown as insulators.
  • One other object of the present invention is to form a uniform layer of oxidized GaAs that is uniform throughout in stoichiometry and chemical composition.
  • the method of this invention may comprise fully oxidizing the surface of a compound material.
  • the surface of the material is established at a selected temperature.
  • the surface is then exposed to a beam of high kinetic energy atomic oxygen for a time effective to fully oxidize the compound material to a predetermined thickness on said surface.
  • the substrate material is GaAs.
  • the surface of a compound semiconductor material is passivated by establishing the material surface at a selected temperature and then exposing the material to a beam of high energy kinetic atomic oxygen for a time effective to fully oxidize the compound material to a predetermined thickness on the surface.
  • an electronic component is formed from a compound semiconductor material, where at least a portion of the compound material is fully oxidized by exposure of the material to a high kinetic energy beam of atomic oxygen and has a thickness of at least 100 A.
  • FIGURE 1 is a schematic representation in cross-section of apparatus for forming an oxide layer of GaAs according to the present invention.
  • FIGURES 2A and 2B depict Ga and As 3d core-level XPS (Al K excitation) for three regions of the GaAs surface at various exposures to a beam of 2.8 eV atomic oxygen.
  • FIGURES 3A and 3B depict Ar + -ion sputter profiling results showing the Ga 3d, As3d, O Is and C Is intensities vs. sputtering time for the regions exposed in Figure 1.
  • FIGURE 5 is a cross-sectional illustration of a GaAs device having a fully oxidized layer of GaAs.
  • a GaAs substrate layer is exposed to a high kinetic energy atomic oxygen beam source, i.e., greater than 0.5 eV.
  • a high kinetic energy atomic oxygen beam source i.e., greater than 0.5 eV.
  • the reacted layer is chemically uniform in composition, having a well-defined stoichiometry with a Ga/As atomic ratio equal to that of GaAs, and to be relatively thick, i.e., greater than 100 A to provide passivation or insulation from adjacent semiconductor materials.
  • FIG. 1 A suitable system for generating a high kinetic energy beam of atomic oxygen is shown in Figure 1, and more particularly described in U.S. Patent Number 4,780,608, issued October 25, 1988, to Cross, and incorporated herein by reference.
  • Light from a high_ power cw laser 10. is focused by lens .12 into a region 14. of an appropriate gas mixture in which a continuous optical discharge is to be generated.
  • Light from pulsed laser __ ⁇ is directed by beam mirror 18. through lens .12. and focused into substantially the same volume .14. as cw laser .10.
  • the continuous optical discharge in region .14. is then expanded through a nozzle 20 having a throat 2__ into region 2__ that is maintained at a low pressure by conventional pumps.
  • Beam skimmer 30 collimates the emerging atoms into a well-defined atomic beam . 32 . that impinges upon a GaAs substrate target 34.
  • an atomic O beam was generated with a kinetic energy of 2.8 eV (FWHM of about l.OeV) at a flux of about 10 17 atoms/cm 2 (i.e., about 100 ⁇ nolayers/sec) .
  • the GaAs samples were (110)- or - 0)-oriented wafers that were semi-insulating or Si-doped (n - 2xl0 18 /cm 3 ) , and were repolished in a freshly prepared 1% Br 2 /methanol solution prior to use.
  • the samples were exposed to the atomic O beam over an area of about 5x7 mm for periods of from 1 to 5 hours, during which time the sample temperature was held constant at 50°C.
  • the samples were then subjected to x-ray photoe ission (XPS) and Raman spectroscopy analyses to determine the stoichiometry and uniformity of the resulting oxide layer.
  • XPS x-ray photoe ission
  • the oxide thickness was estimated to be at least 300-500 _A. It is tentatively concluded that the oxide layer is gallium arsenate (GaAs0 4 ) and is chemically uniform.
  • Figures 2A and 2B respectively, show the Ga and As 3d core-level XPS data taken on an unexposed part of a sample, an area at the edge of the O-atoms exposed area and at the center of that area.
  • the As 3d binding energy (BE) shift, relative to that of unexposed GaAs, is about 3.2 eV at the edge of the irradiated area and about 4.2 eV at the center.
  • Reference to standard compounds shows that a 3.2 eV BE shift corresponds to As 2 0 3 , while a shift of 4.2 eV is intermediate between those of As 2 0 3 (3.2-3.4 eV) and As 2 0 5 (4.7-4.9 eV) .
  • Oxidation-induced BE shifts are generally smaller for Ga than for As 3d.
  • the Ga 3d BE shift of 1.0 eV corresponds to that of Ga 2 0 3 (0.9-1.4 eV)
  • the smaller shift at the edge indicates a species in which the Ga is less than fully oxidized.
  • the attenuation length for 1400 eV photoelectrons in GaAs is estimated to be about 27 A, giving an effective sampling depth of about 50 A for the spectra shown in Figures 2A and 2B.
  • the "parent" (i.e., unoxidized) Ga or As 3d peaks at the center of the O-irradiated area, i.e., the substrate has completely reacted to at least the depth sampled.
  • Figure 3 graphically depicts the results of Ar + -ion sputter profiling done to evaluate the thickness and composition of the oxide layer.
  • the C Is signal near the surface and the peak in O Is intensity are thought to arise from contamination incurred during transfer of the sample between chambers.
  • no accumulation of excess Ga or excess As was observed, and the Ga/As atomic ratio shows only a small variation as sputtering progresses through the oxide.
  • the apparent small excess of Ga at long sputter times is in agreement with the observed preferential sputtering of As from GaAs samples.
  • the As 3d oxide satellite showed only a slight change in BE shift (from 4.2 to 4.0 eV) as profiling progressed through the oxide and the "parent" peak gained intensity.
  • the oxide thickness is estimated to be at least 300-500 A, well over the thickness of 100 A that is desired for an electronic component device fabricated using the oxidized layer of GaAs.
  • Raman spectroscopy is a well established method used to detect oxidation-induced disorder and the accumulation of elemental column-V species at the oxide-substrate interface.
  • Figures 4A and 4B respectively, show Raman data for the semi-insulating (100) and n-type (110) samples with and without exposure to the O-beam.
  • the unoxidized area shows a strong GaAs LO (longitudinal optical) phonon peak at about 290 cm " , with only a very weak, if any, TO (transverse optical) phonon peak at about 270 cm " .
  • the symmetry-forbidden TO mode can be made observable by the presence of residual strain, roughness or disorder in the substrate.
  • Raman spectra of thermal oxides on GaAs also show strong peaks at about 257 and 200 cm -1 arising from the LO and TO phonons, respectively, of crystallizing As at the oxide/GaAs interface. Amorphous As, if present, produces a broad band from about 200 to 250 cm "1 . For the semi-insulating (100) samples, the O-exposed areas show none of these features. Although Raman spectroscopy of n-doped (110) samples routinely shows no signals indicative of elemental As, a single sample did show As signals, as shown in Figure 4B. This anomalous result is believed to have resulted from some sample contamination and is presented to show the type of signal that would be observed in the presence of elemental As.
  • GaAs substrates About 23 GaAs substrates have been prepared using the base-line process described above, and with modifications discussed below.
  • the GaAs substrate surfaces were of either (100) or (110) orientation; most were n-type doped, but at least three samples were semi-insulating (undoped) .
  • the results of the base-line process are graphically depicted in Figures 2A, 2B, 3, 4A, and 4B, and are summarized as follows: (1) Oxide layers greater than 100 A and at least 300-500 A thick have been grown on a variety of GaAs surfaces at or near room temperature using an atomic oxygen beam source with a kinetic energy of about 2.8 eV.
  • the Ga and As species formed are completely oxidized and in their highest oxidation states respectively, implying formation of Ga 2 0 3 and As 2 0 5 or GaAs0 4 (i.e., observed binding energy shifts are at least those observed in Figures 2A and 2B) ..
  • the oxide layer has a uniform stoichiometry and composition.
  • Raman spectroscopy indicates that the substrate is not disordered appreciably from the oxidation process.
  • N-type GaAs (110) and n-type GaAs (100) samples were oxidized under base-line conditions, except that the samples were exposed at 150°C with an O-atom beam kinetic energy of 1.0 eV.
  • the results were consistent with results (l)-(5), above, for both samples.
  • a kinetic energy of 1.0 eV did result in significant growth of a thick high-quality oxide layer.
  • oxidized samples in accordance with the present invention are quite stable in a laboratory environment without special precautions against moisture and further oxidation.
  • XPS analyses performed immediately after growing oxide layers and at long intervals, e.g., months, are very consistent.
  • the oxide layer is also very passivating on the GaAs surface and is chemically stable, unlike the thin native oxides normally found on the substrate.
  • one O-atom oxidized substrate was re-etched in the 1% Br 2 /Methanol solution in order to reuse the substrate in another oxidation experiment. Etching the sample resulted in the preferential removal of the unoxidized region of the sample, leaving the O-atom beam oxidized region largely intact.
  • a typical electronic component would include the layers shown in Figure 5, i.e., a substrate 52 of a compound semiconductor material with a layer 54. of the fully oxidized material.
  • the thickness t of layer 54. is at least 100 A for adequate passivation and insulation.
  • other material layers may be formed on surface ⁇ H for defining discrete electronic components.
  • Oxidized layer 5_4 is formed by exposing substrate 52 to a high energy beam of atomic oxygen at substrate temperatures below which thermal oxidation occurs.
  • the method of the present invention is not believed to be limited to the oxidation of GaAs.
  • Other compound semiconductor materials including InP, InSb, GaSb, HgCdTe, etc. , and other electronic device materials are difficult to oxidize using thermal and/or other established techniques.
  • the oxidation of high-temperature superconducting thin films has also been done with the high energy atomic O-beam.
  • the growth of high-quality oxide layers on a wide variety of materials will enable the development of new electronic devices.
  • the formation of passivating oxide layers on these and other materials will also provide increased applications for these materials, ranging from integrated circuits to infrared detectors.
  • thick, uniform, and fully oxidized layers of compound materials may be formed by exposure to high kinetic-energy atomic 0.
  • GaAs has been oxidized.
  • the reaction has minimal effect on the crystalline order of the substrate and has resulted in no detectable levels (by Raman spectroscopy) of either crystalline or amorphous elemental As at the oxide-GaAs interface.
  • the resulting oxide layer passivates the semiconductor surface to provide environmental stability for electronic component applications.
  • the layer is also insulating to permit layered semiconductor components to be formed.

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  • Formation Of Insulating Films (AREA)

Abstract

On oxyde un matériau combiné (34) en exposant la surface du matériau à un faisceau (32) d'énergie cinétique élevée d'oxygène atomique. En particulier, l'on a oxygéné du GaAs à la température ambiante en l'exposant à un faisceau d'oxygène atomique de 2,8 eV. Des couches d'oxyde de 300 à 500 Å ont été produites sans que de l'As élémentaire ne soit apparent dans la couche d'oxyde ou de l'interface avec le substrat de GaAs. L'oxyde présente une stoichiométrie de Ga/As uniforme avec une oxydation complète du Ga et de l'As. Il a été démontré que la couche peut rendre la surface de GaAs passive, est isolante, et peut produire un condensateur pourvu d'une couche de recouvrement. Ces caractéristiques indiquent que des composants électroniques séparés peuvent être obtenus lorsqu'on utilise les caractéristiques de la couche d'oxyde de GaAs produite.
PCT/US1991/007941 1990-11-16 1991-11-01 Oxydation d'arseniure de gallium Ceased WO1992009108A1 (fr)

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US614,423 1990-11-16

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5241214A (en) * 1991-04-29 1993-08-31 Massachusetts Institute Of Technology Oxides and nitrides of metastabale group iv alloys and nitrides of group iv elements and semiconductor devices formed thereof

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US4469528A (en) * 1981-09-18 1984-09-04 U.S. Philips Corporation Method of manufacturing a semiconductor device of GaAs by two species ion implantation
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US4828812A (en) * 1987-12-29 1989-05-09 Mobil Oil Corporation Titanosilicates of enhanced ion exchange capacity and their preparation
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US4474829A (en) * 1981-11-23 1984-10-02 Hughes Aircraft Company Low-temperature charge-free process for forming native oxide layers
FR2529384A1 (fr) * 1982-06-25 1983-12-30 Thomson Csf Procede de reduction de compose en couche sur un substrat et son application a la fabrication de structure semi-conductrice a effet de champ
US4686022A (en) * 1985-09-25 1987-08-11 The Boeing Company Method and apparatus for producing a monatomic beam of ground-state atoms
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US4780608A (en) * 1987-08-24 1988-10-25 The United States Of America As Represented By The United States Department Of Energy Laser sustained discharge nozzle apparatus for the production of an intense beam of high kinetic energy atomic species
US4828812A (en) * 1987-12-29 1989-05-09 Mobil Oil Corporation Titanosilicates of enhanced ion exchange capacity and their preparation
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21 J. VAC. SCI. TECHNOL., No. 2, July/August, PETRO et al., "Effect of Low Intensity Laser radiation During Oxidation of the GaAs(110) Surface", pages 405-408. *
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ION IMPLANTATION IN SEMICONDUCTORS AND OTHER MATERIALS, CROWDER editor, PLENUM PRESS, 1972, FAVENNEC et al., "Compensation of GaAs by ion implantation", pages 621-630. *
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5241214A (en) * 1991-04-29 1993-08-31 Massachusetts Institute Of Technology Oxides and nitrides of metastabale group iv alloys and nitrides of group iv elements and semiconductor devices formed thereof

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