US3809584A - Method for continuously growing epitaxial layers of semiconductors from liquid phase - Google Patents

Method for continuously growing epitaxial layers of semiconductors from liquid phase Download PDF

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Publication number
US3809584A
US3809584A US00324887A US32488773A US3809584A US 3809584 A US3809584 A US 3809584A US 00324887 A US00324887 A US 00324887A US 32488773 A US32488773 A US 32488773A US 3809584 A US3809584 A US 3809584A
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epitaxial layers
semiconductors
furnace
liquid phase
substrates
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US00324887A
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English (en)
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N Takahashi
S Iguchi
S Akai
H Mori
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Sumitomo Electric Industries Ltd
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Sumitomo Electric Industries Ltd
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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
    • C30B19/00—Liquid-phase epitaxial-layer growth
    • C30B19/06—Reaction chambers; Boats for supporting the melt; Substrate holders
    • C30B19/063—Sliding boat system
    • 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
    • Y10S148/006—Apparatus
    • 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
    • Y10S148/107—Melt
    • 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
    • Y10S148/119—Phosphides of gallium or indium

Definitions

  • the substrates are moved consecutively on a plurality of lvessels in a reaction furnace from a high temperature regionto a low temperature region maintained within the reaction furnace, which is provided with a temperature gradient in the longitudinal direction, all the while the substrates are kept in contact-with the liquid solution containing a source material of the epitaxial layers, whereby the epitaxial layers are grown successively and on a continuous basis.
  • the present invention relates to a method for successively growing liquid phase epitaxial layers which enables the epitaxial growth of semiconductors on a commercial basis.
  • the present invention relates to an improvement in or relating to said slowly-cooling liquid phase epitaxial growth method.
  • epitaxial layers of the following various semiconductors can be grown successively on suitable substrates: Group III- V compound semiconductors such as GaAs, GaP, InP,
  • Group III-V mixed semiconductors such as Ga1 xAlXAs, InAsLXSb,' In'xGalQxP, In ⁇ Ga1 ,Sb, InxAl1 XP, GaxAl1 XP and In1 xAlXAs (0 x ⁇ 1 in the foregoing semiconductors); Group II-VI compound semiconductors such as CdTe, CdS, ZnSe, ZnTe, ZnOy and BeTe; mixed crystals of Group II-VI semiconductors such as ZnSe1 xTex, Cd1 ZnXS and Hg1 XCd,Te (0 x 1 in the foregoing semiconductors) and other compound semiconductors such as (ZnS)1 X(GaP)X, (ZnSe)1 (GaAs)x (0 x 1 in thev foregoing semiconductors) and ZnSip2.
  • Group III-V mixed semiconductors such as Ga1 xAlXAs, InA
  • a suitable substrate consisting of a single crystal of a semiconductor is moved through a reaction furnace having a temperature gradient from a high temperature region to a low temperature region within the reaction furnace, all
  • the principal object of this invention is ⁇ to provide a method of growing liquid phase epitaxial ⁇ layers of semiconductors successively, as well as continuously, on many suitable substrates from the liquid phase.
  • a feature of thisinvention resides in a method'of grow ⁇ ing epitaxial layers of semiconductors on suitable singlecrystal substrates from the liquid phase, wherein the single-crystal substrates are moved through a reaction furnace from a high temperature region to a low temperature region within the reaction furnace, which is provided to have a temperature gradient in the longitudinal direction thereof, all the while the substrates are kept in contact with the liquid solution containing a source material of the semiconductor, thereby growing epitaxial layers of said semiconductors on said single-crystal substrates.
  • Another feature of this invention resides in a method of growing epitaxial layers of semiconductors on suitable single-crystal substrates from the liquid phase wherein substrate-supporting vessels are employed with each containing at the bottom of the vessel the single-crystal substrate and a liquid solution containing a source material of the semiconductor is supplied onto the substrate in the substrate-'supporting vessels from a main container of liquid solution having at least five times as much Volume as the vessel.
  • the vessels are moved through a reaction furnace from a high temperature region to a low temperature region within the reaction furnace, which is provided to have a temperature gradient in the longitudinal direction of the furnace, all the while the single-crystal substrates are kept in contact with the liquid solution, thereby growing epitaxial layers of the semiconductors on the single-crystal substrates.
  • Still another feature of this invention resides in a method of forming epitaxial growth layers of semiconductors on suitable single-crystal substrates from the liquid phase wherein substrate-supporting vessels are employed with each containing at the bottom of the vessel the single-crystal substrate and these vessels are vertically moved in a vertically elongated reaction furnace having a vertical temperature gradient, from a high temperature region to a low temperature region within the reaction furnace, all the while the single-crystal substrates are kept in contact with a liquid solution containing a source material of the semiconductor so that the single-crystal substrates in the vessel are positioned on the low temperature side of the reaction furnace and the solution is positioned on the high temperature side of the furnace.
  • FIG. 1 illustrates in cross section a horizontal reaction furnace or apparatus for continuously growing the epitaxial layers on suitable substrates from the liquid phase together with a graphic illustration of the longitudinal temperature profile of the reaction furnace.
  • FIG. 2 is a perspective view of a portion of the apparatus shown in FIG. 1.
  • FIG. 3 illustrates in cross section a vertical reaction furnace r apparatus for continuously growing the epitaxial layers on suitable substrates from the liquid phase together with a graphic illustration of the vertical temperature profile of the reaction furnace.
  • FIG. 1 is a cross sectional View of a liquid phase epitaxial growth reaction furnace apparatus for carrying out the continuous liquid phase epitaxial growth used in this example together with an illustration of the temperature profile in the reaction furnace.
  • FIG. 2 is a perspective view of a portion of the inside of the reaction furnace shown in FIG. 1.
  • a main container 2 of a liquid solution 1 containing a source material is supported from within the reaction tube S and is kept at a temperature T1 by an electric heater 9.
  • the liquid solution 1 in which a source material consisting of constituent elements or the semiconductor has been dissolved is contained.
  • a frame 4 for supporting the liquid solution is positioned upon a slider or carrier 3 to provide a plurality of substrate-supporting vessels 20.
  • a single-crystal substrate 5 is positioned.
  • the substrate-supporting vessels 20 containing the single-crystal substrate 5 are continuously moved in the direction of an arrow 19 into the reaction furnace heated by an electric furnace and thereafter introduced into the lower portion or area of the main container 2.
  • An opening 11 is provided in the bottom of the main container 2 through which the liquid solution is supplied into each vessel 2t) passing therebeneath.
  • the main container 2 is provided with at least tive times as much volu-me as a single vessel in order to feed the liquid solution successively into a plurality of vessels 20 on a continuous basis.
  • a temperature gradient of 0.1-15 C./cm. is provided horizontally through the furnace by an electric heater 12 as depicted in the temperature profile curve at 21. The temperature gradient through the furnace is controlled depending upon the desired conditions of the epitaxial growth and moving rate of the vessels 20 through the furnace.
  • each vessel 20 It is desirable to select the value of the product GV C./min.) of the temperature gradient G C./cm.) and the moving rate V (cm/min.) in the range of 0.1-10 C./min. Temperature gradient in the vertical direction through each vessel 20 is not necessarily required but preferably the temperature of the singlecrystal substrate 5 is lower than that of the solution. While each vessel 20 containing the single-crystal substrate 5 and the deposited liquid solution is moved through a remainder of the furnace, an epitaxial layer is grown on the single-crystal substrate 5. The right side or area of the reaction tube 8 is kept at a predetermined temperature T2 by an electric heater 13.
  • FIG. 2 illustrates an embodiment for separation of the frame 4 from the slider 3.
  • the frame 4 for supporting the liquidsolution is caused to slide by a xed arm member 14 in therdirection of an arrow 22 which is substantially perpendicular to the direction of vessel movement depicted by Varrow 19, so that the liquid solution is separated by member 14 from the surface of the epitaxial layer grown on'the single-crystal substrate 5.
  • a solid or integral substrate-supporting vessel 20 may also be used.
  • the liquid solution is .removed after the entire vessel has been taken out from the reaction tube.
  • hydrogen gas or an inert gas such as nitrogen gas is introduced through a gas inlet 6 of the tube 8, and the gas is exhausted through a gas outlet 15.
  • Hydrogen gas or an inert gas such as nitrogen is introduced at outlets 7 and 16 and exhausted, respectively, through outlet 17 and outlet 18 of the reaction tube 8.
  • a semicontinuous liquid phase growth method is also contemplated within the scope of this invention wherein the temperature region of T1 is longer than that shown in FIG. 1 because the quartz reaction tube 8 is longer than that shown in FIG. 1. Also, the main container 2 would be positioned at the left end of the tube to supply the liquid solution into each vessel 20 which are fixed so that the reaction furnace itself is moved-in a direction toward the container 2, that is, toward the left of FIG. l.
  • GaP epitaxial layers were grown successively on GaP single-crystal substrates from the liquid phase.
  • the liquid solution 1 comprises about 30 g. of Ga and 1.0 g. of GaP.
  • Temperature T1 of the solution was kept at 1050 C. ⁇ In the formation of nepitaxial growth layers, Te or S was doped as impurity.
  • the single-crystal substrates 6 wafers obtained from GaP single crystals grown bythe liquid encapsulated Czochralski process were used. Surface area of the'wafer was about 2 cm?.
  • the single-crystal substrate 5v was coveredk 'withmthe liquid solution to a depth of about 2 mrn. as supported within the frame 4 which is about 2 mm. in'height'for supporting the liquid solution.
  • the substrate Sand the liquid solution were moved in this state in the 'reaction tube 8 having a temperature gradient of 2 C./cm. at a rate of 3 cm./min. in the direction of arrow 19.
  • T 2 950 C.
  • ⁇ frame 4 is separated from the moving slider 3 by means of the xed arm member 14.
  • the height of the frame may be selected inthe range of 0.5"- 5 mm.
  • the depth of th'e liquid solution over the substrate 5 may be 0.5-5 mm., depending upon the height of the frame 4. If the depth is too small, the epitaxialgrwth is diflicult. Too large of a'depth is undesirable from 'an economicalviewpoint. It is desirable to provide a solid cover (not shown in the figure) on the'liquid solution jso that the depth of the liquid solution is uniform.
  • volatile components of the semiconductorsor volatile doping impurities may be evaporated out of the solutions.
  • the loss from the solution by evaporation may be covered up by putting a lid on the top of container 2 and also each vessel 20 to prevent the evaporation or may be compensated by introducing the volatile compound into the reaction tube 8 together with the carrier gas through the inlet 6.
  • FIG. 3 illustrates in cross section a vertical reaction furnace for continuously growing the epitaxial layers used in this particular example together with the temperature profile vertically through the reaction furnace.
  • This process in which the vertical reaction furnace is used is superior to that in Example 1 wherein the horizontal furnace is used for ⁇ the following reasons:
  • the temperature gradient is also produced on the surface of the semiconductor substrateand convection of the solution is produced since the semiconductor substrate is placed horizontally in the substrate-supporting vessel and is in contact with the solution in the reaction furnace having a horizontal temperature gradient. Therefore, the temperature across the deposited solution in the vessel is notuniform.
  • the direction of the temperature gradient is perpendicular to the surface of the semiconductor substrate and the temperature on the surface of the semiconductor substrate is uniform and, therefore, more uniform epitaxial growth layer :can be obtained.
  • the substrate is cooled with a special cooling device.
  • a special cooling device it is not desirable that temperatures of the semiconductor substrate and the saturated lsolution be the same.
  • the conditions can be satisfied by l(3) In effecting the successive epitaxial growth, the
  • a substrate-supporting vessel 25 made of carbon, quartz or BN is provided for containing a semiconductor substrate 23 and a solution 24 saturated Withthesource material.
  • An elevator conveyor is provided to have many shelves for lowering the individual vessels 25 to the lower portion of the vertical furnace 43.
  • Heaters 27 through 41 and 52 are provided in the furnace 43.
  • the T-shaped quartz tube 42 is housed within the internal area of the furnace 43.
  • the overall length of the furnace 43 is about 1 m.
  • the temperature gradient is produced so that high temperature (T1 C.) region is :positioned in the upper portion of the furnace 43 and low temperature (T2 C.) region is positioned in the lower portion thereof, with the middle portion adapted to have nearly a straight temperature gradient (see temperature profile 51 on the left of FIG. 3).
  • the temperature gradient, T1 and T2 can be changed selectively depending upon variety ofthe compound semiconductor to be epitaxilly grown, and thickness of theepitaxial layer to be grown.
  • Each vessel 25 having a frame for supporting the liquid solution 24 and containing the GaP semiconductor substrate 23 is introduced in the direction of an arrow 44 beneath the lower or bottom inlet 47 of a main container 46 containing a Ga solution saturated with GaP source material.
  • the Ga solution 24 saturated with GaP is fed into the frame of the vessel 25 and then introduced into the conveyor 26.
  • the GaP semiconductor substrate 23 had a thickness of 450 am. and the surface area on which the epitaxial layer is to be grown was about 2 om?.
  • the liquid solution 45 comprised about 30 g. of Ga and 1.8 g. of GaP.
  • the solution 45 was kept at a temperature T1 of 1050 C.
  • Te or Ga2S2 was added as impurity.
  • Temperature gradient in the furnace 43 was about 2 C./ cm.
  • the low temperature region in the lower portion of the furnace was kept at about 950 C
  • Each vessel 25 was lowered at a rate of 3 cm./min. from the high temperature region to the low temperature region in the furnace 43, which took about 20 minutes.
  • the vessel 25 lowered to the low temperature region was then moved in the direction of an arrow 48 by means of a push bar 49.
  • the frame for supporting the solution of the vessel 25 was removed by a jig bar 50 having the same structure as the arm member 14 in FIG. 2. Thickness of the resulting epitaxial growth layer was about 30 nm.
  • the temperature profile may be produced so that the temperature gradient in a high temperature region changes slowly and the temperature gradient in a low temperature region changes sharply.
  • the middle part of the temperature prole may be kept at a temperature l0-50 C. higher than the high temperature region and then the temperature may be made gradually lower thereafter in order to dissolve 1-5 um. thickness of the surface of the semiconductor substrate 23 in the solution 24 and bring about epitaxial growth.
  • the method of continuously growing epitaxial layers of semiconductors on single-crystal substrates from the liquid phase comprising the steps of moving a plurality of consecutively arranged vessels through a reaction furnace provided with a high temperature region and a low temperature region, each of said vessels including a single-crystal substrate, depositing the liquid solution containing a source material of the semiconductor within each of said vessels on the surface of the substrate as they proceed through the furnace within the high temperature region, and thereafter continuously moving each of said vessels from the high temperature regionv through a decreasing temperature gradient region and thence into the low temperature region of the furnace while said substrates are maintained in contact with the liquid solution thereby growing epitaxial layers of said semiconductors consecutively on said substrates.

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  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3884788A (en) * 1973-08-30 1975-05-20 Honeywell Inc Substrate preparation for liquid phase epitaxy of mercury cadmium telluride
US4026240A (en) * 1975-11-17 1977-05-31 Hewlett-Packard Company Liquid phase epitaxial reactor apparatus
US4063972A (en) * 1975-03-26 1977-12-20 Sumitomo Electric Industries, Ltd. Method for growing epitaxial layers on multiple semiconductor wafers from liquid phase
US4308820A (en) * 1973-05-01 1982-01-05 U.S. Philips Corporation Apparatus for epitaxial crystal growth from the liquid phase
US4347097A (en) * 1971-12-14 1982-08-31 Handotai Kenkyu Shinkokou Method and apparatus for producing a multilayer semiconductor device utilizing liquid growth
US4357620A (en) * 1980-11-18 1982-11-02 The United States Of America As Represented By The Secretary Of The Army Liquid-phase epitaxial growth of cdTe on HgCdTe
US4376663A (en) * 1980-11-18 1983-03-15 The United States Of America As Represented By The Secretary Of The Army Method for growing an epitaxial layer of CdTe on an epitaxial layer of HgCdTe grown on a CdTe substrate
US4516296A (en) * 1983-10-05 1985-05-14 Zsi, Inc. Tubing clamp and method of making the same
US20100102419A1 (en) * 2008-10-28 2010-04-29 Eric Ting-Shan Pan Epitaxy-Level Packaging (ELP) System
US20100105194A1 (en) * 2008-10-28 2010-04-29 Eric Ting-Shan Pan Method of Integrating Epitaxial Film onto Assembly Substrate
US20100101725A1 (en) * 2008-10-28 2010-04-29 Eric Ting-Shan Pan Apparatus for Making Epitaxial Film
ITRM20090074A1 (it) * 2009-02-19 2010-08-20 Bove Rafael Dalenz Forno con gradiente termico controllato per lavorazione di materiali mediante trattamenti termici cristallizzazione silico od altri mediante controllo del posizionamento del crogiolo all'interno del forno

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5420944Y2 (ja) * 1973-11-09 1979-07-26
JPS5132488A (ja) * 1974-09-14 1976-03-19 Tokyo Shibaura Electric Co Ekisoseichohoho
JPS61251022A (ja) * 1985-04-27 1986-11-08 Junichi Nishizawa 化合物半導体の液相エピタキシヤル成長法及び成長装置

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5136448U (ja) * 1974-09-11 1976-03-18

Cited By (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4347097A (en) * 1971-12-14 1982-08-31 Handotai Kenkyu Shinkokou Method and apparatus for producing a multilayer semiconductor device utilizing liquid growth
US4308820A (en) * 1973-05-01 1982-01-05 U.S. Philips Corporation Apparatus for epitaxial crystal growth from the liquid phase
US3884788A (en) * 1973-08-30 1975-05-20 Honeywell Inc Substrate preparation for liquid phase epitaxy of mercury cadmium telluride
US4063972A (en) * 1975-03-26 1977-12-20 Sumitomo Electric Industries, Ltd. Method for growing epitaxial layers on multiple semiconductor wafers from liquid phase
US4026240A (en) * 1975-11-17 1977-05-31 Hewlett-Packard Company Liquid phase epitaxial reactor apparatus
US4357620A (en) * 1980-11-18 1982-11-02 The United States Of America As Represented By The Secretary Of The Army Liquid-phase epitaxial growth of cdTe on HgCdTe
US4376663A (en) * 1980-11-18 1983-03-15 The United States Of America As Represented By The Secretary Of The Army Method for growing an epitaxial layer of CdTe on an epitaxial layer of HgCdTe grown on a CdTe substrate
US4516296A (en) * 1983-10-05 1985-05-14 Zsi, Inc. Tubing clamp and method of making the same
US20100101725A1 (en) * 2008-10-28 2010-04-29 Eric Ting-Shan Pan Apparatus for Making Epitaxial Film
US20100105194A1 (en) * 2008-10-28 2010-04-29 Eric Ting-Shan Pan Method of Integrating Epitaxial Film onto Assembly Substrate
US20100102419A1 (en) * 2008-10-28 2010-04-29 Eric Ting-Shan Pan Epitaxy-Level Packaging (ELP) System
US7905197B2 (en) * 2008-10-28 2011-03-15 Athenaeum, Llc Apparatus for making epitaxial film
US20110247550A1 (en) * 2008-10-28 2011-10-13 Eric Ting-Shan Pan Apparatus for Making Epitaxial Film
US8193078B2 (en) 2008-10-28 2012-06-05 Athenaeum, Llc Method of integrating epitaxial film onto assembly substrate
US8430056B2 (en) * 2008-10-28 2013-04-30 Athenseum, LLC Apparatus for making epitaxial film
US8507371B2 (en) 2008-10-28 2013-08-13 Athenaeum Llc Method of forming epitaxial semiconductor structure
US8507370B2 (en) 2008-10-28 2013-08-13 Athenaeum Llc Method of transferring epitaxial film
US8530342B2 (en) 2008-10-28 2013-09-10 Athenaeum, Llc Method of integrating epitaxial film onto assembly substrate
US8541294B2 (en) 2008-10-28 2013-09-24 Athenaeum Llc Method of forming epitaxial film
US8673752B2 (en) 2008-10-28 2014-03-18 Athenaeum, Llc Method of forming epitaxial based integrated circuit
ITRM20090074A1 (it) * 2009-02-19 2010-08-20 Bove Rafael Dalenz Forno con gradiente termico controllato per lavorazione di materiali mediante trattamenti termici cristallizzazione silico od altri mediante controllo del posizionamento del crogiolo all'interno del forno

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