EP0417190A1 - Films de dioxyde de silicium sur diamant - Google Patents

Films de dioxyde de silicium sur diamant

Info

Publication number
EP0417190A1
EP0417190A1 EP89906913A EP89906913A EP0417190A1 EP 0417190 A1 EP0417190 A1 EP 0417190A1 EP 89906913 A EP89906913 A EP 89906913A EP 89906913 A EP89906913 A EP 89906913A EP 0417190 A1 EP0417190 A1 EP 0417190A1
Authority
EP
European Patent Office
Prior art keywords
substrate
diamond
crystals
seed crystals
slurry
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP89906913A
Other languages
German (de)
English (en)
Inventor
Michael W. Geis
Nikolay N. Efremow
Henry I. Smith
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Massachusetts Institute of Technology
Original Assignee
Massachusetts Institute of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Massachusetts Institute of Technology filed Critical Massachusetts Institute of Technology
Publication of EP0417190A1 publication Critical patent/EP0417190A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
    • 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
    • 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
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions

Definitions

  • This invention relates to the fabrication of semiconductor material for use in electronic devices, and more particularly, to the fabrication of diamond semiconductor films.
  • Diamond is a material with semiconductor properties that are superior to Silicon (Si), Germanium (Ge) or Gallium Arsenide (GaAs), which are now commonly used.
  • Si Silicon
  • Ge Germanium
  • GaAs Gallium Arsenide
  • diamond provides a higher band gap, a higher breakdown voltage and a greater saturation velocity which produces a substantial increase in its projected cutoff frequency and maximum operating voltage compared to devices fabricated from Si, Ge, or GaAs.
  • diamond has the highest thermal conductivity of any solid at room temperature and excellent conductivity over a temperature range up to and beyond 500°k. Diamond therefore holds the potential Unfortunately, however, the advantages of diamond as a semiconductor have not been exploited because of the difficulty in forming electrical contacts on diamond surfaces which allow access to and contol of diamond semiconductor devices..
  • natural diamonds may be of device quality, they are of limited supply and size.
  • Carbon radical reactions produce diamond crystals on the substrate, while the hydrogen present is converted to atomic hydrogen which preferentially etches away graphite and thereby leaves a film which is predominately diamond.
  • This method also allows for the possibility of doping by introducing electrically active impurities into the environment above the substrate which are then trapped in the diamond lattices so synthesized.
  • the quality and growth rate of diamond films produced by CVD on substrates has been found in the past to be dependent on the nature of the substrate. In fact, it had been thought that only when the substrate is diamond itself may device quality films be grown. In this technique, known as homoepitaxy, the orientation of newly deposited diamond is coincident with that of the substrate.
  • These seed crystals may be diamond, boron nitride, or like material.
  • Yet another object of the present invention is to provide a crystal film on a substrate which is a mosaic of single crystal diamonds whose (111) planes are substantially parallel.
  • Fig. 1 is a flow diagram showing four preferred steps of the oriented diamond crystal process of the present invention
  • Fig. 2 is a perspective view of a diamond crystal seeded onto a flat substrate in practice of process steps 1-3 of Fig. 1, showing a preferred crystal orientation on the substrate;
  • Fig. 3 is a graphic representation of an X-ray diffraction intensity pattern obtained from diamond crystals oriented on a quartz substrate according to the present invention, where X-ray intensity is plotted on the Y-axis against the Bragg angle 2 ⁇ ;
  • Fig. 4 is a graphic representation of the distribution of the orientations of the crystals' (111) plane relative to the substrate plane, before (dotted line) and after (solid line) step 3 of Fig. 1, where diffraction intensity is plotted on the Y-axis in arbitrary units and degree of tilt of crystals' (111) plane relative to the substrate plane is plotted along the X-axis;
  • Fig. 5a is a schematic view of seed crystals on a substrate surface before step 4 of the present invention;
  • Fig. 5b is a schematic view showing growth of the seed crystals during the early stage of step 4 of the present invention.
  • Fig. 5c is a schematic view showing formation of a crystal film after step 4 of the present invention
  • Fig. 6 is a perspective view of a flat surface, seeded with diamond crystals in practice of the present invention wherein the orientation pt the (ill) planes is depicted;
  • Fig. 7 is a perspective view of a grated surface, seeded with diamond crystals in practice of the present invention wherein certain planes and directions are depicted;
  • Fig. 8 is a side cross-sectional view of a vertical semiconductor device having a textured polycrystalline film grown in practice of the present invention on a conductive substrate.
  • FIG. 1 there is provided a flow diagram of the preferred method for oriented diamond crystal growth, including suspending seed crystals in a slurry, applying the slurry to the surface of a prepared substrate, heating the substrate and drawing off the slurry fluid, growing a film of diamond crystals on the treated substrate, by CVD.
  • a diamond crystal film can be grown on a substrate.
  • steps 1-3 of this procedure effect a desired orientation of seed crystals on the substrate surface.
  • These seed crystals may be, for example, diamond or boron nitride or any other crystal whose crystal structure and behavior is similar to diamond.
  • Step 4 a single crystal film is grown around these oriented seeds preferably by CVD. 5
  • synthetic or natural diamond grit is prepared for use, preferably by immersion in a bath of boiling sulfuric acid and ammonium persulfate at approximately 300°C for 10 minutes.
  • the grit is next rinsed with deionized water, concentrated hydrofloric acid and again with deionized water.
  • the grit is thus made ready for use in the first step of the present invention.
  • the first step of the present method is directed to separating or declumping, the seed crystals.
  • the washed seeds are suspended in a slurry, preferably by mixture of 0.l grams of grit per 10 ml of a 40,000:1 solution of water in soap, such
  • Alternate slurry solutions include silicone base diffusion pump oil in trichloroethylene. The slurry mixture is then subjected to an ultrasonic vibratory mixer to suspend the grit.
  • the substrate which may be, for example, a standard Si wafer, is preferably prepared by cleaning in an oxygen plasma asher. Other substrates having metal or quartz surfaces also may be used.
  • the substrate is then wetted across its surface by application of the slurry (step 2) in any conventional manner, such as by use of a dropper or the like.
  • step 3 the wafer is heated (step 3) until the solvent is removed and the surface is visually dry.
  • Such heating has been achieved by use of an ordinary laboratory hot plate, where the substrate is placed on the hot plate surface and is raised to approximately 200°C for approximately two minutes.
  • the diamond growth CVD process (step 4) involves heating the substrate to 900°C and passing a gaseous mixture of, for example, 99% hydrogen and 1% methane, through a 2.75 GHz discharge above the substrate surface to create a plasma. Since pure diamond is an insulator, it may be necessary to introduce or dope electrically active impurities to render the diamond useful as a semiconductor.
  • B 2 H g may be added to the gas during CVD at chosen concentrations in the parts per million range.
  • PH 3 may be added to the gas during CVD at chosen concentrations in the parts per million range.
  • Another CVD method of growing diamond is to flow a mixture of hydrogen and a hydrocarbon gas, such as methane, past a hot tungsten filament located in close proximity to the substrate surface.
  • This method of diamond CVD growth was described originally by S. Matsumoto et al. in the Japan Journal of Applied Physics, vol. 21, page L183, (1982), with recent elaborations by Hirose and Terasawa, in Japan. J. Appl. Phys. vol, 25, p. L519 (1986).
  • Fig. 2 a diamond crystal seeded onto a flat substrate in practice of process steps 1-3, and prior to step 4, is conceptually presented.
  • the desired orientaton of the (111) plane of the seed crystal is shown with respect to the substrate surface.
  • seeded crystals after the heating of step 3 and prior to the CVD of step 4 are oriented such that the (111) plane of the crystal (using the Miller indices referencing method) will lie parallel to the substrate plane.
  • FIG 3 a graphic representation of an X-ray diffraction pattern obtained from diamond crystals applied to a quartz substrate by the present method, and substantially as oriented in Fig. 2, is shown, where X-ray intensity is plotted in arbitrary units on the Y-axis and diffraction angle 2 ⁇ is plotted on the X-axis, where 2 ⁇ represents the Bragg angle.
  • X-ray intensity is plotted in arbitrary units on the Y-axis
  • diffraction angle 2 ⁇ is plotted on the X-axis, where 2 ⁇ represents the Bragg angle.
  • a graphic representation of Fig. 4 the distribution of crystals with (111) crystal planes oriented relative to the substrate plane is presented before and after the heating of step 3.
  • X-ray diffraction intensity is plotted along the Y-axis in arbitrary units, while the degree of tilt of the crystals' (111) plane relative to the substrate plane is plotted along the X-axis.
  • the mildly curvilinear dotted line represents diffraction intensity after the step 2 application of the seed crystals to a substrate but before the heating of step 3, and shows some amount of (111) plane orientation.
  • the sharply parabolic curve (in solid line) represents vastly improved diffraction intensity after the annealing of step 3, suggestive of vastly improved crystal orientation. It will thus be appreciated that the heating process of step 3 substantially improves the conformity of the seed crystal orientation on the substrate surface.
  • Fig. 5a is a schematic view of seed crystals on a substrate surface in practice of the invention, after step 3 but before step 4. These crystals, as seeded, obtain the preferred orientation shown in Fig. 2.
  • Fig. 5a the preferred orientation of the seed crystals is indicated by the horizontal hash marks drawn across the cross-section of the crystals.
  • Fig. 5b is a schematic representation of the early stage of the CVD process of step 4, where it will be seen that the seeded crystals become enlarged as new diamond material is deposited on the seed surface.
  • the new diamond material is also favorably oriented in coincidence with the orientation of the seed crystals, as indicated by the horizontal hash marks of Fig. 5b, coincident with the hash marks of 5a.
  • the resulting grown crystals merge and a crystalline film is formed upon completion of the CVD process.
  • This textured film is characterized by a multiplicity of crystals A, B, C grown from individual seeds a, b, c, all of whose (ill) planes are similarly oriented.
  • crystal defects may occur due to the differing rotational orientation of the seeds about their ⁇ 111> axis.
  • Fig. 6 a flat substrate surface, seeded with diamond crystals, is shown in perspective view. These crystals are indicated to have dissimilar orientations with respect to rotation about an axis perpendicular to the (111) plane. It will be appreciated that these crystals may have irregular shapes. However, regular tetrahedral crystal shapes are drawn in Figs. 6 and 7 for ease of indicating the orientations of the (111) planes. Growth of diamond films by CVD from such crystals may lead to crystal defects at the point at which film growth from adjacent crystals meet. This leads to a textured crystal film of many crystals (i.e., polycrystalline film) grown from adjacent seeds whose (111) planes are all similarly oriented.
  • a textured crystal film of many crystals i.e., polycrystalline film
  • An alternative embodiment of the present invention is to apply the method of steps 1-4 to a surface which has been previously patterned in the form of a grating, as disclosed in the perspective view of Figure 7.
  • Employing a grated substrate surface orients the seed crystals with respect to rotation relative to each other and thus reduces or eliminates the crystal defects arising from orientation mismatch between adjacent seed crystals. In this manner a polycrystalline film with fewer defect boundries may be formed.
  • the present invention may be favorably employed in the growth of vertical semiconductor devices. These devices are characterized by vertical current flow through the device. Turning now to Fig.
  • FIG. 8 there is shown a side cross-sectional view of a vertical semiconductor device having a textured polycrystalline film grown on an ungrated conductive substrate (such as of nickel or carbon) , created by the present method of crystal film growth.
  • a textured polycrystalline film grown on an ungrated conductive substrate (such as of nickel or carbon)
  • the now familiar grain boundaries of the textured film will be seen, where it will be appreciated that a grating ⁇ pattern has been etched into the surface of the prepared polycrystalline film, and where the device is provided with an emitter, base, and collector.
  • the vertical axes of the crystals of the textured film are within a few degrees of the substrate normal, where rotational orientations about the normal axis have not been controlled.
  • the film has been doped with boron sufficient to render it a suitable semiconductor. Ohmic contacts may be created by conventional means..
  • metal is evaporated on all horizontal grating surfaces without metallizing the vertical walls of the grating, thus creating a Schottky base and
  • This vertical device is only one of several devices which may be created in practice of the present invention.
  • the preferred process is as follows:

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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)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

On a mis point un procédé de production de films de diamant orientés sur un substrat. On suspend des germes de cristaux de diamant dans une bouillie (1) puis on les applique à la surface (2) du substrat. Le chauffage (3) du substrat élimine le fluide de la bouillie et produit des germes de cristaux dont les plans de cristaux (111) sont sensiblement parallèles au plan du substrat. On peut former par croissance un film de diamant polycristallin orienté autour des germes de cristaux par déposition chimique en phase vapeur (CVD) (4).
EP89906913A 1988-06-03 1989-06-02 Films de dioxyde de silicium sur diamant Withdrawn EP0417190A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US20287788A 1988-06-03 1988-06-03
US202877 1988-06-03

Publications (1)

Publication Number Publication Date
EP0417190A1 true EP0417190A1 (fr) 1991-03-20

Family

ID=22751602

Family Applications (1)

Application Number Title Priority Date Filing Date
EP89906913A Withdrawn EP0417190A1 (fr) 1988-06-03 1989-06-02 Films de dioxyde de silicium sur diamant

Country Status (3)

Country Link
EP (1) EP0417190A1 (fr)
JP (1) JPH03505861A (fr)
WO (1) WO1989011897A1 (fr)

Families Citing this family (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3941475A1 (de) * 1989-12-15 1991-06-20 Weidmueller C A Gmbh Co Bezeichnungstraeger fuer elektrische leiter
EP0459425A1 (fr) * 1990-05-30 1991-12-04 Idemitsu Petrochemical Company Limited Procédé pour la préparation de diamant
US5129850A (en) * 1991-08-20 1992-07-14 Motorola, Inc. Method of making a molded field emission electron emitter employing a diamond coating
US5141460A (en) * 1991-08-20 1992-08-25 Jaskie James E Method of making a field emission electron source employing a diamond coating
US5298286A (en) * 1992-11-09 1994-03-29 North Carolina State University Method for fabricating diamond films on nondiamond substrates and related structures
US5449531A (en) * 1992-11-09 1995-09-12 North Carolina State University Method of fabricating oriented diamond films on nondiamond substrates and related structures
US5455072A (en) * 1992-11-18 1995-10-03 Bension; Rouvain M. Initiation and bonding of diamond and other thin films
DE69417627T2 (de) * 1993-01-14 1999-09-09 Sumitomo Electric Industries Verfahren zur dampfphasendiamantsynthese
JP3549228B2 (ja) * 1993-05-14 2004-08-04 株式会社神戸製鋼所 高配向性ダイヤモンド放熱基板
US5488232A (en) * 1993-09-28 1996-01-30 North Carolina State University Oriented diamond film structures on non-diamond substrates
EP0659911A1 (fr) * 1993-12-23 1995-06-28 International Business Machines Corporation Procédé pour la formation d'un film polycristallin sur un substrat
EP0674028A3 (fr) * 1994-03-25 1996-04-03 Tokyo Gas Co Ltd Cristal de diamant et procédé de sa fabrication.
CN103787585B (zh) * 2014-02-10 2016-01-13 北京美顺达技术开发有限公司 在石英基片上沉积金刚石膜的方法
CN109371463A (zh) * 2018-11-27 2019-02-22 西安碳星半导体科技有限公司 一种cvd金刚石晶种的衬底选择方法
CN115181957B (zh) * 2022-08-25 2023-03-17 北京爱克瑞特金刚石工具有限公司 一种功能性金刚石微纳米粉体及复合体的制备和应用

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US3630679A (en) * 1968-06-26 1971-12-28 Univ Case Western Reserve Diamond growth process
US4045186A (en) * 1973-09-06 1977-08-30 General Electric Company Method for producing large soft hexagonal boron nitride particles
US4378629A (en) * 1979-08-10 1983-04-05 Massachusetts Institute Of Technology Semiconductor embedded layer technology including permeable base transistor, fabrication method
US4544540A (en) * 1982-06-25 1985-10-01 Sumitomo Electric Industries, Ltd. Diamond single crystals, a process of manufacturing and tools for using same
JPS60221395A (ja) * 1984-04-19 1985-11-06 Yoshio Imai ダイヤモンド薄膜の製造方法
US4551195A (en) * 1984-09-25 1985-11-05 Showa Denko Kabushiki Kaisha Method for growing boron nitride crystals of cubic system
US4547257A (en) * 1984-09-25 1985-10-15 Showa Denko Kabushiki Kaisha Method for growing diamond crystals
DE3674329D1 (de) * 1985-09-24 1990-10-25 Sumitomo Electric Industries Verfahren zur synthese von bornitrid des kubischen systems.
JPH0779958B2 (ja) * 1987-05-08 1995-08-30 住友電気工業株式会社 大型ダイヤモンドの合成方法

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Also Published As

Publication number Publication date
WO1989011897A1 (fr) 1989-12-14
JPH03505861A (ja) 1991-12-19

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