US3788890A - Method of preparing dislocation-free crystals - Google Patents

Method of preparing dislocation-free crystals Download PDF

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US3788890A
US3788890A US00231695A US3788890DA US3788890A US 3788890 A US3788890 A US 3788890A US 00231695 A US00231695 A US 00231695A US 3788890D A US3788890D A US 3788890DA US 3788890 A US3788890 A US 3788890A
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crystal
crystals
dislocation
substrate
dislocations
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S Mader
J Matthews
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International Business Machines Corp
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International Business Machines Corp
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    • 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
    • C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
    • C30B13/34—Single-crystal growth by zone-melting; Refining by zone-melting characterised by the seed, e.g. by its crystallographic orientation
    • 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
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/36—Single-crystal growth by pulling from a melt, e.g. Czochralski method characterised by the seed, e.g. its crystallographic orientation
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10S117/901—Levitation, reduced gravity, microgravity, space
    • Y10S117/902—Specified orientation, shape, crystallography, or size of seed or substrate
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S148/00—Metal treatment
    • Y10S148/025—Deposition multi-step
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S148/00—Metal treatment
    • Y10S148/115—Orientation

Definitions

  • FIG.2 Sheets-Sheet l Filed March 5, 1972 SLIP PLANE FIGJa FIG.2
  • the invention includes a method of selecting suitable seed or substrate crystals which permit the growth of dislocation-free crystals, a method of selecting the optimum plane on which to grow the crystal as well as approximating a large number of suitable planes, and then growing the crystal to a minimum thickness at which all dislocations are removed from the growing crystal.
  • This invention is particularly applicable to the growth of dislocation-free thin film crystals since the minimum thickness can be readily calculated and is often quite small.
  • This invention relates to a crystal growth process, and is particularly directed to the growth of dislocation-free crystals useful in semiconductor applications.
  • Dislocation-free crystals are most desirable in the manufacture of semiconductors.
  • Dislocation lines on semiconductors may act as electron acceptor Cites in addition to being areas for the accumulation of gross impurities. If the impurities accumulated are electrically active, which is often the case, the electrical behavior in the vicinity of the dislocation lines may be substantially different from the electrical behavior in other areas of the semiconductor.
  • doped semiconductor crystals where impurity atoms are diffused into the semiconductor crystal the depth and concentration of the impurity atoms in the vicinity of the dislocations may substantially differ from the rest of the crystal, causing erratic electrical behavior of the device. In certain cases where electrically conductive impurities have accumulated, shorting of the device may occur.
  • FIGS. la1d show cross-sectional views following the growth of a dislocation-free crystal upon a dislocation containing substrate.
  • FIG. 2 depicts the relationship of the slip plane to the crystal growth interface so as to show the Burgers vector and the angles A and FIG. 3 demonstrates constructing a stereographic projection.
  • FIG. 4 is the standard (001) stereo-graphic projection for an fcc. crystal.
  • FIG. 5 shows the family of planes in an fcc. crystal in which cos A and cos 5 are equal to zero.
  • FIGS. 6-9 show the suitable interfaces upon which to grow dislocation free crystals for various crystalline structures.
  • FIG. 10 shows a dislocation-free crystal upon a substantially identical substrate made in accordance with the process of this invention.
  • FIG. 1 shows the growth of a dislocation-free crystal B upon a seed or substrate crystal A which contains dislocation lines.
  • FIG. 1a shows the growth of crystal B in which dislocations contained in A extend into the growing crystal B. Since the lattice parameters of A and B differ, an elastic strain is produced which, upon further growth, exerts a force on the dislocation lines of B forcing them to bow out as shown in FIG. 1b. As the thickness of B is increased, the force on the dislocation lines in B also increases until a critical thickness is obtained in which the dislocation lines in B glide to the edge of the specimen as shown in FIG. and finally escape as shown in FIG. 1d. This process leaves dislocation lines at the interface between A and B but removes the dislocations from B.
  • the difference in lattice parameters between A and B creates an elastic strain or misfit.
  • the magnitude of the misfit between the unstrained lattice parameters of A and B must be large enough to remove all dislocations from B but less than that which would spontaneously create new dislocations. We have found the minimum misfit needed to remove dislocations, which is dependent upon the materials employed.
  • p is the dislocation density
  • b is the Burgers vector of misfit dislocation
  • L is the diameter across the AB interface and is the angle between the Burgers vector of the dislocations and that direction in the AB interface which is perpendicular to the line of intersection of the slip plane and the interface as shown in FIG. 2.
  • the maximum number of dislocations allowable in the seed or substrate crystal can be calculated by using the equation:
  • L bL cos A can thus be obtained from the lattice parameters of the crystal.
  • Table I gives the lattice parameters of some common crystalline materials.
  • Lattice parameter (s) A. Aluminum 4.0496 Gold 4.0788 Germanium 5.6570 Silicon 5.4305 Silver 4.0857 Gallium arsenide 5.6530 Chromium 2.8846 Iron 2.8664
  • lattice parameters of other crystals can be readily obtained from standard texts, such as The International Tables for X-Ray Crystallography, vol. 3, Kynoch, England, 1962, and Handbook of Lattice Spacings o Metals and Alloys, Pergamon Press: New York, 1958.
  • N and N are the number of dopant and Si atoms/cc. while r and m are their bond radii.
  • Table III gives the slip plane and slip direction of common crystalline structures.
  • GaP, InSb 111 Boc metals e.g., Fe, Nb, Cr, W, Ta
  • 123 111 Alkali halides structure 110 110 PbS, PbSe, PbTe structure 001 110
  • the minimum misfit or the maximum dislocation density of the substrate can be calculated for any crystal whose lattice parameters and slip system are known.
  • dislocations moving to the edge may meet obstacles which they can overcome only if the force per unit length of each dislocation is large.
  • the condition that the force per unit length be large is that be large for all the dislocations present in the crystal.
  • cos A not be equal to 0 as before, but in addition, cos should not be equal to 0.
  • the magnitude of e is determined by the misfit and thickness. Cos A and cos depend upon the orientation of the interface, on the slip direction (i.e., the direction of the Burgers vector), and on the orientation of the slip plane. The orientation in which cost. and cos are both large for all possible dislocations can be determined by using standard projection of the crystal and knowledge of its slip system.
  • the dots can be projected onto a planar surface 16. If the planar surface is placed so that its plane is perpendicular to the diameter of the sphere that touches the light source then the array of dots on the paper is a stereographic projection 17.
  • Desirable growth directions, or orientations for the interface between the two crystals, should be away from all the lines shown in FIG. 5.
  • FIG. 4 contains 24 triangles each of which have indices of the type and (111) at their comers. All of these triangles are essentially the same.
  • any interface AB of FIG. 1 can be represented by a point on one of these triangles.
  • the most desirable AB interface in fee. materials like Si, GaAs, Au, Al, Cu is shown by the hatched area in FIG. 6, tlieptiiaangle of which is obtained from the hatched portion 0 5.
  • FIG. 7 shows suitable interfaces for growing alkali halide (NaCl) type crystals while FIG. 8 shows areas for body centered cubic (bcc.) crystals and FIG. 9 for PbS type crystals.
  • NaCl alkali halide
  • bcc. body centered cubic
  • b is the magnitude of the Burgers vector of the dislocation
  • v is Poissons ratio
  • 1 is the misfit between the equilibrium lattice parameters of A and B
  • )t is the angle between the slip direction and that direction in the film plane which is perpendicular to the line of intersection of the slip plane and specimen surface as shown in FIG. 2.
  • Suitable interfaces are those in which h is always finite, so, cos A must eirceed zero for all dislocations.
  • the lattice parameters of the substrate or seed crystal must be different than the crystal to be grown. Thus, the two materials cannot be identical.
  • the same material for the substrate and the perfect crystal is required.
  • the critical thickness of B must be greater than 2h to ensure that dislocations will be' removed from B during the growth of B, and will not be drawn back into B when A is grown.
  • a suitable plane on which to grow the dislocation-free crystal is determined using the stereographicprojections discussed above. By placing the substrate or seed crystal on a goniometer and taking X-ray laue photographs of the crystals, or by any other known method, the suitable plane and orientation is marked and the crystal is 'cut along these lines.
  • the dislocation-free crystal can be grown on the substrate, by a variety of techniques, to a thickness greater than the critical thickness discussed above.
  • Well known single crystal growth methods from a melt or solution including the Czochralski crystal pulling technique, floating-zone technique, the gradient-freeze technique, the Horizontal-Bridgman method and the horizontal zone melt technique may be employed.
  • vapor-growth methods including vacuum evaporation, sputtering, and chemical vapor deposition can be used.
  • other methods such as molecular beam techniques and electro-deposition may be employed.
  • the vapor-growth methods are particularly applicable to the manufacture of thin films, and are fully discussed in references on that subject such as Handbook of Thin Film Technology, Maissel, L. I. and Glang, R. (McGraw Hill, New York), 1970, and Thin Film Technology, Berry, Hall & Harns (D. van Nostrand, 00., Princeton), 1968.
  • Germanium is grown on gallium arsenide. Since the lattice parameters are known, the misfit between the unstrained lattice parameters are calculated;
  • the dislocations of the specimen are less than the maximum which can be removed, a dislocation. free crystal is assured if it is grown to a critical height. It should be noted that if the number of dislocations in .the specimen is greater than the maximum to be removed, then the size of the specimen substrate (L). must be decreased so that p is equal to or less than the dislocation density of the specimen.
  • a thin film of 1500 A. may be grown in which all the dislocations of the substrate are removed.
  • Single-crystal films of germanium is grown on gallium arsenide by the process described in US. Pat. 3,345,209 and assigned to the same assignee as the present invention.
  • the method includes thepassage of GeI- over the substrate material which is maintained at 350 C.
  • EXAMPLE II A silicon ingot 1 cm. in diameter, is cut to expose a suitable plane at the interface. Since silicon is an fcc. crystal, a suitable plane is the (210) plane, as shown in FIG. 6. The maximum density of dislocation which can be removed is calculated from the equation:
  • the misfit is calculated using Vegards law, the results of which for a boron concentration of 10 atoms/cc. is shown in Table II.
  • the maximum dislocation density removable is 4x10
  • the dislocation density of the silicon ingot interface is then measured using X-ray techniques. For silicon ingot specimens the dislocation density is generally 'lessthan about 1X10. Thus, all of the dislocations can be removed from silicon doped with 10 atoms/ cc. of boron on a 1 cm. diameter substrate.
  • the boron' doped silicon is then grown on the silicon substrate by introducing a boron containing gas with a gaseous stream of 'Si which is formed by the reduction of SiCl
  • the gaseous mixture is then allowed 'to flow across the silicon substrate until a critical thickness of 500 A. is obtained at which height all dislocations are removed.
  • This method of chemical vapor deposition is discussed in Thin Films Technology, supra, p. 269 and in US. Pats. 3,184,348 and 3,361,600, assigned to the same assignee as the present invention.
  • EXAMPLE III A pure, silicon dislocation-free crystal may be grown on a silicon substrate using an intermediate layer as shown in FIG. 10.
  • the boron-doped silicon is grown to twice the critical thickness of 1000 A., as in Example II.
  • Pure. silicon may then be vapor grown on the boron doped silicon by discontinuing the flow of boron-supplying gas to yield a dislocation-free silicon crystal on a silicon substrate with a boron doped silicon intermediate layer.
  • Dislocation-free chromium films can be grown on iron substrates. Since these materials have bcc. crystalline structures the iron substrate is cut and oriented on some plane within the shaded area" of FIG. 8 such as the (001) or (111') plane. The misfit is first determined from the difference in lattice parameters, so
  • chromium is vapor deposited onto the iron crystal to a thickness of 50 A. or more.
  • a method of preparing dislocation free crystals from a dislocation containing substrate crystal comprising the steps of: I
  • a suitable substrate crystal such that the percentage misfit between the lattice parameters of said seed crystal and the crystal to be grown is at least equal to bL cos A wherein p is the dislocation density, b is the magnitude of Burgers vector of'the misfit dislocation, L is the diameter at the interface of the substrate crystal and the crystal to be grown and A is the angle between the Burgers vector and that direction in said interface which is perpendicular to the line of intersection of the slip plane and the interface, but less than .7%.
  • said substrate crystals are selected from the group of fcc. crystals, consisting of Al, Ni, Cu, Au, P'd, Ag, Pt, Si, Ge, GaAs, GaP, and InSb.
  • said substrate crystals are selected from the group of bcc. crystals, consisting of Fe, Nb, Cr, W, Ta and Mo.
  • said substrate crystals are selected from the group consisting of PbS, PbSe and PbTe.
  • a method of growing a dislocation free germanium crystal on a gallium arsenide monocrystalline substrate comprising the steps of:
  • a method of growing dislocation free doped silicon crystals on a monocrystalline silicon substrate comprising the steps of:
  • b is the magnitude of the Burgers vector
  • 1 is Poissons ratio
  • f is the percentage misfit
  • A is said angle measured from the Burgers vector the cosine of A not equaling zero.
  • a method of growing dislocation free chromium filrns on a monocrystalline iron substrate comprising the steps of:

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3976535A (en) * 1975-05-27 1976-08-24 Bell Telephone Laboratories, Incorporated Screening seeds for quartz growth
US4174422A (en) * 1977-12-30 1979-11-13 International Business Machines Corporation Growing epitaxial films when the misfit between film and substrate is large
US4710259A (en) * 1983-09-23 1987-12-01 Howe Stephen H Setting the orientation of crystals
US4776917A (en) * 1984-12-24 1988-10-11 Shin-Etsu Chemical Co., Ltd. Single crystal wafer of lithium tantalate
US4857415A (en) * 1987-05-29 1989-08-15 Raytheon Company Method of producing single crystalline magnetic film having bi-axial anisotropy
US4865659A (en) * 1986-11-27 1989-09-12 Sharp Kabushiki Kaisha Heteroepitaxial growth of SiC on Si
US4908074A (en) * 1986-02-28 1990-03-13 Kyocera Corporation Gallium arsenide on sapphire heterostructure
US5156995A (en) * 1988-04-01 1992-10-20 Cornell Research Foundation, Inc. Method for reducing or eliminating interface defects in mismatched semiconductor epilayers
US20030047795A1 (en) * 2001-09-10 2003-03-13 Showa Denko K.K. Compound semiconductor device, production method thereof, light-emitting device and transistor
WO2007144557A1 (en) * 2006-06-16 2007-12-21 Rolls-Royce Plc Friction welding of a single crystal component to a second component with minimisation of in plane friction and forge forces
US11614378B2 (en) 2017-01-06 2023-03-28 Direct-C Limited Polymeric nanocomposite based sensor and coating systems and their applications

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4142332B2 (ja) * 2002-04-19 2008-09-03 Ｓｕｍｃｏ Ｔｅｃｈｘｉｖ株式会社 単結晶シリコンの製造方法、単結晶シリコンウェーハの製造方法、単結晶シリコン製造用種結晶、単結晶シリコンインゴットおよび単結晶シリコンウェーハ

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3976535A (en) * 1975-05-27 1976-08-24 Bell Telephone Laboratories, Incorporated Screening seeds for quartz growth
US4174422A (en) * 1977-12-30 1979-11-13 International Business Machines Corporation Growing epitaxial films when the misfit between film and substrate is large
US4710259A (en) * 1983-09-23 1987-12-01 Howe Stephen H Setting the orientation of crystals
US4776917A (en) * 1984-12-24 1988-10-11 Shin-Etsu Chemical Co., Ltd. Single crystal wafer of lithium tantalate
US4898641A (en) * 1984-12-24 1990-02-06 Shin-Etsu Chemical Co., Ltd. Single crystal wafer of lithium tantalate
US4908074A (en) * 1986-02-28 1990-03-13 Kyocera Corporation Gallium arsenide on sapphire heterostructure
US4865659A (en) * 1986-11-27 1989-09-12 Sharp Kabushiki Kaisha Heteroepitaxial growth of SiC on Si
US4857415A (en) * 1987-05-29 1989-08-15 Raytheon Company Method of producing single crystalline magnetic film having bi-axial anisotropy
US5156995A (en) * 1988-04-01 1992-10-20 Cornell Research Foundation, Inc. Method for reducing or eliminating interface defects in mismatched semiconductor epilayers
US20030047795A1 (en) * 2001-09-10 2003-03-13 Showa Denko K.K. Compound semiconductor device, production method thereof, light-emitting device and transistor
US6730987B2 (en) * 2001-09-10 2004-05-04 Showa Denko K.K. Compound semiconductor device, production method thereof, light-emitting device and transistor
US20040169180A1 (en) * 2001-09-10 2004-09-02 Show A Denko K.K. Compound semiconductor device, production method thereof, light-emitting device and transistor
US7030003B2 (en) 2001-09-10 2006-04-18 Showa Denko Kabushiki Kaisha Compound semiconductor device, production method thereof, light-emitting device and transistor
WO2007144557A1 (en) * 2006-06-16 2007-12-21 Rolls-Royce Plc Friction welding of a single crystal component to a second component with minimisation of in plane friction and forge forces
US20090173769A1 (en) * 2006-06-16 2009-07-09 Rolls-Royce Plc Welding of Single Crystal Alloys
US7731075B2 (en) 2006-06-16 2010-06-08 Rolls-Royce Plc Welding of single crystal alloys
US11614378B2 (en) 2017-01-06 2023-03-28 Direct-C Limited Polymeric nanocomposite based sensor and coating systems and their applications

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