WO1992003204A1 - Procede de croissance de corps cristallins tubulaires et cylindriques - Google Patents

Procede de croissance de corps cristallins tubulaires et cylindriques Download PDF

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Publication number
WO1992003204A1
WO1992003204A1 PCT/US1991/005676 US9105676W WO9203204A1 WO 1992003204 A1 WO1992003204 A1 WO 1992003204A1 US 9105676 W US9105676 W US 9105676W WO 9203204 A1 WO9203204 A1 WO 9203204A1
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WO
WIPO (PCT)
Prior art keywords
seed
melt
rate
crystalline body
growing
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Ceased
Application number
PCT/US1991/005676
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English (en)
Inventor
Juris P. Kalejs
Richard W. Stormont
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Schott Solar CSP Inc
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Mobil Solar Energy Corp
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Publication date
Application filed by Mobil Solar Energy Corp filed Critical Mobil Solar Energy Corp
Publication of WO1992003204A1 publication Critical patent/WO1992003204A1/fr
Anticipated expiration legal-status Critical
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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
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/34—Edge-defined film-fed crystal-growth using dies or slits

Definitions

  • This invention pertains to methods of growing crystals, and more particularly to methods of growing cylindrical tubular crystalline bodies by the EFG process.
  • Silicon sheet used in the fabrication of photovoltaic devices is frequently formed from the flat sides of tubular crystalline bodies of the type having a polygonal cross section, e.g., a nonagon crystal.
  • Apparatus of the type described in U.S. Patent No. 4,544,528 have been used to manufacture these crystalline bodies according to the edge-defined, film-fed growth process (the EFG process) .
  • these apparatus comprise a crucible for containing a melt of the material to be grown (e.g., silicon), a capillary die for controlling the form and shape of the grown crystal, a heater for controlling the temperature of the die and melt, a seed support assembly for supporting the seed used in growing the crystal, and a pulling mechanism coupled to the seed support assembly for drawing the tubular crystalline body out of the melt.
  • a melt of the material to be grown e.g., silicon
  • a capillary die for controlling the form and shape of the grown crystal
  • a heater for controlling the temperature of the die and melt
  • a seed support assembly for supporting the seed used in growing the crystal
  • a pulling mechanism coupled to the seed support assembly for drawing the tubular crystalline body out of the melt.
  • Taylor et al. grew tubular crystalline bodies up to 9 cm in diameter, with wall thicknesses ranging from 0.015 to 0.071 cm. The crystalline bodies were not rotated during the growth thereof. It was intended that solar cell substrates would be fabricated by flattening rectangular portions of the wall of the tubular body.
  • Crystalline bodies grown with the apparatus of U.S. Patent No. 4,544,528 are not rotated about their long axes during the growth thereof. It is known, however, to rotate elongate, hollow crystalline bodies during the growth thereof by the EFG process, as illustrated in U.S. Patent No. 3,846,082 to LaBelle, Jr. et al. and in the article "The Tubular Solar Cell - A New Concept for Photovoltaic Power Generation", by Mlavsky et al., published in Proceedings of the Twelfth IEEE Photovoltaic Specialists Conference, 1976. Crystalline bodies grown by the apparatus of U.S. Patent No. 3,846,082 have spirally-shaped interior and/or exterior surfaces. Unlike the crystalline bodies grown with the apparatus developed by LaBelle Jr. et al., the crystalline bodies grown by Mlavsky et al. were tubular, i.e. they had parallel interior and exterior walls that were substantially straight along the length thereof.
  • the Mlavsky et al. process for growing a crystalline body involves rotating the body only during the initial formation thereof. As soon as the pulling mechanism begins to pull the crystalline body away from the die, rotation of the body is stopped.
  • the tubular bodies grown by Mlavsky et al. were about 0.375 inches in diameter and were mounted whole in the collector of a photovoltaic-solar thermal energy system.
  • Tubular crystalline bodies grown by the Mlavsky et al. process tend to have one or more regions extending along the length of the body in which the impurity concentration is much higher than in the remainder of the body.
  • Conventional solar cell substrates cannot be cut from tubular crystalline bodies grown by the Mlavsky et al. process due to the small diameter of the bodies.
  • the impurity "rashes" present in the crystalline bodies grown by Mlavsky et al. would render the Mlavsky et al. process unsuitable as a method of growing crystalline bodies from which solar cell substrates could be fabricated.
  • a primary object of the present invention is to provide a method of growing by the EFG process tubular crystalline bodies having parallel cylindrical interior and exterior surfaces and improved uniformity of distribution of the impurities disposed therein as compared to the uniformity of distribution of impurities in a tubular crystalline body of polygonal cross-section grown by the EFG process.
  • Another object of the present invention is to provide a method of growing by the EFG process tubular cylindrical crystalline bodies having thinner walls, reduced dislocation density and increased minority carrier diffusion lengths, as compared to tubular crystalline bodies of polygonal cross-section grown by the EFG process using known apparatus and methods.
  • Yet another object of the present invention is to provide a solar cell substrate having improved microstructural characteristics, as compared to solar cell substrates fabricated from crystalline bodies grown by known processes.
  • a method of growing by the EFG process tubular cylindrical crystalline bodies having an improved evenness of distribution of impurities relative to tubular crystalline bodies of polygonal cross-section grown by the EFG process without rotation using known apparatus or methods is accomplished using an apparatus comprising a crucible for containing a melt of the material, e.g., silicon, from which the crystalline body is grown, a heater for maintaining the melt at selected temperature, a die for forming and determining the shape of the crystalline body, a seed, a seed holder, a pulling mechanism coupleable to the seed holder for pulling the crystalline body away from the die, and a rotation mechanism coupled to the pulling mechanism for rotating the crystalline body about its growth axis while the body is being pulled away from the die.
  • a melt of the material e.g., silicon
  • the method involves rotating the seed holder, seed and crystalline body relative to the die at about 50 revolutions per minute during the entire time the crystalline body is being pulled away from the die.
  • the temperature of the melt, pull speed and other control variables are similar to those used in known methods of growing tubular crystalline bodies of polygonal cross-section by the EFG process.
  • Fig. 1 is a schematic elevation view, partially broken away, of the present invention
  • Fig. 2 is a photograph presenting a front elevational view of a portion of a cylindrical tubular crystalline body grown from a melt doped with aluminum, with the upper portion of the body being grown without rotation and the bottom portion of the body being grown with rotation;
  • Fig. 3 is a photograph presenting a front elevational view of a portion of a cylindrical tubular crystalline body grown from a melt doped with iron and aluminum, with the upper portion of the body being grown without rotation and the bottom portion of the body being grown with rotation.
  • the present invention is a method of growing cylindrical tubular crystalline bodies by the EFG process from molten silicon.
  • Ethyl silicon of the 'type manufactured by Ethyl Corporation, Electronic Materials Division, of Baton Rouge, Louisiana, is used as the feed stock for the melt.
  • Ethyl silicon is silicon in a high purity, spherical, free-flowing particulate form.
  • Ethyl silicon has an average statistical impurity concentration of 0.12 ppba of boron, 0.11 ppba of phosphorous, 0.11 ppba of arsenic, and 0.25 ppma of carbon.
  • the method of the present invention is accomplished using an EFG crystal growing apparatus 20 for growing cylindrical tubular crystalline bodies.
  • the apparatus comprises a furnace enclosure 22 having an aperture 23 extending through the top surface thereof.
  • Apparatus 20 includes -8-
  • Enclosure 22, crucible 24, capillary die 26, seed holder 28 and graphite seed 30 are substantially identical to the corresponding elements in the crystal forming device disclosed in U.S. Patent No. 4,544,528 (the '528 patent), which is incorporated herein by reference. Attention is directed to this patent for a more detailed description of the structure and function of elements 22-30 of the present invention.
  • the capillary die 26 has a circular cross-sectional configuration (since cylindrical crystalline bodies are grown by the present apparatus) rather than the nonagon cross-sectional configuration of the capillary die of the crystal growing apparatus of the 528 patent.
  • die 26 has a diameter selected so that crystalline bodies grown therefrom have an outside diameter ranging about 10 to 30 cm, with smaller and larger diameter dies also being within the scope of the present invention.
  • capillary die 26 is substantially identical to the capillary die of the '528 patent.
  • Seed holder 28 comprises an elongate shaft 32 having a flat, circular stop plate 34 secured to the lower end thereof. Seed holder 28 also comprises a top plate 35 having a central bore 36 extending therethrough. The bottom end of bore 36 comprises a counterbore 37. Stop plate 34 is positioned in counterbore 37 of top plate 35, and seed 30 attached thereto, hang down from the stop plate. Stop plate 34 and counterbore 37 are sized so that the peripheral edge of stop plate 34 frictionally engages the sidewall of counterbore 37 such that top plate 35 rotates with stop plate 34 and shaft 32 attached thereto, except when a sufficient resistive force is applied to top plate 35. Such a resistive force is generated when, for instance, the growing crystal freezes to the die. When such a resistive force is applied to top plate 35, stop plate 34 will rotate within counterbore 37. This slip-fit connection is provided so that the growing crystal does not shatter in the event of a freeze-up.
  • Furnace enclosure 22 is surrounded by a heating coil 44 which is coupled to a controllable power supply (not shown) of conventional construction.
  • Heating coil 44 is provided for maintaining the melt supported within crucible 24 at a predetermined temperature.
  • Heating coil 44 is substantially identical to and functions in the same manner as the heating coil surrounding the furnace enclosure of the crystal-growing apparatus disclosed in the '528 patent.
  • Apparatus 20 further comprises a rotation mechanism 52 coupled with shaft 32 for imparting rotational movement to the latter.
  • Rotation mechanism 52 includes support arm 54 and bearing assembly 56 attached to the underside of one end of the support arm.
  • Bearing assembly 56 is adapted to receive the upper end of shaft 32 and to rotatably support the shaft and prevent the shaft from moving radially or axially relative to support arm 54.
  • Rotation mechanism 52 further comprises rotational drive motor 64 which is attached via bracket 66 to the opposite end of support arm 54.
  • Rotational drive motor 64 has an output shaft 68 to which a drive sprocket 70 is attached.
  • a similar driven sprocket 72 is attached to shaft 32 substantially in alignment with drive sprocket 70.
  • Sprockets 70 and 72 are rotationally coupled by a flexible endless drive member 74.
  • member 74 is a flexible chain and sprockets 70 and 72 are suitably toothed to' engage the chain so that rotational drive can be transmitted from drive sprocket 70 to driven sprocket 72.
  • member 74 may be a flexible V-belt and sprockets 70 and 72 may have a circumferential groove for receiving the V-belt.
  • Apparatus 20 also comprises a pulling mechanism 80 coupled to rotation mechanism 52 and attached to a fixed surface 82 above the apparatus 20.
  • Pulling mechanism 80 is substantially identical to the pulling mechanism disclosed in U.S. Patent No. 4,544,528.
  • Pulling mechanism 80 is coupled to rotation mechanism 52 so that upon actuation of the former the entire rotation mechanism, as well as seed holder 28 which is attached to the rotation mechanism, will be pulled away from die 26.
  • Heating coil 44, rotation mechanism 52 and pulling mechanism 80 may be individually operated so as to achieve the operating characteristics required to grow a cylindrical tubular crystalline body with apparatus -11-
  • heating coil 44, rotation mechanism 52 and pulling mechanism 80 may be coupled to a conventional control unit (not shown) which automatically controls these elements 44, 52 and 80 so as to achieve the operating characteristics required to grow a cylindrical tubular crystalline body with apparatus 20.
  • pulling mechanism 80 is operated to lower rotation mechanism 52, and seed holder 28 and seed 30 attached to the rotation mechanism, so that seed 30 will just contact the end face of die 26.
  • Apparatus 20 is now in condition to grow a cylindrical tubular crystalline body.
  • Heating coil 44 is operated to heat die 26 above the melting point of seed 30 to cause the portion of the latter contacting the die to melt so as to wet the die.
  • Pulling mechanism 80 is now activated to raise rotation mechanism 52, and seed holder 28 and seed 30 attached thereto, away from die 26.
  • the melted seed material wetting the die is drawn out, by surface tension, into a thin film between the seed and the die end face.
  • the previously charged melt of Ethyl silicon in crucible 24 rises, by capillary action, to replenish the material wetting the die end face.
  • the portion of liquid film nearest seed 30 is at a lower temperature than that at the end face of die 32, and begins to solidify as its temperature • 12-
  • Pulling mechanism 80 is operated so as to continue to pull seed 30 away from die 26 until a cylindrical, tubular crystalline body of suitable length hangs from the seed. Pulling mechanism 80 is operated so as to pull seed 30 away from die 26 at substantially the same rate of speed as that of the pulling mechanism of the device of U.S. Patent No. 4,544,528, i.e. about 2.5 cm/min. Pull speed may be satisfactorily controlled using apparatus of the type disclosed in U.S. Patent No. 4,267,151 to Yates et al.
  • rotation mechanism 52 is actuated so as to rotate seed 30 relative to die 26. More specifically, rotational drive motor 64 is actuated causing its output shaft 68 and drive sprocket 70 attached thereto to rotate. This rotation is transmitted via chain or belt 74 to driven sprocket 72. The latter, via its coupling with shaft 32, transmits rotational drive to the shaft. As shaft 32 and stop plate 34 attached thereto rotate, rotational drive is transmitted to top plate 35, seed 30 and the growing crystalline body attached to the seed by virtue of the frictional engagement of stop plate 34 with the sidewall of counterbore 37. Rotational drive motor 64 is preferably operated so that its output shaft 68 rotates at about 35-65, preferably about 50, rotations per minute, although higher rates of rotation, e.g. 100-200 -13 -
  • apparatus 20 may be used if apparatus 20 comprises sufficient mechanical vibrational dampening to prevent breakage or irregular formation of the growing crystalline body.
  • a hollow tubular crystalline body 100 (Fig. 2) having a circular cross section was grown using crystal growing apparatus 20.
  • Ethyl silicon as described above, was used as the feed material. After being converted to a molten state in crucible 24 of apparatus 20, the Ethyl silicon was doped with aluminum to a concentration of about 400ppm.
  • Crystalline body 100 was then grown following the method described above, except that the upper portion 100a (i.e., the first grown portion) of body 100 was grown without rotation. After the growing crystalline body 100 reached a predetermined length, rotation mechanism 52 was activated with the result that the lower portion 100b of the crystalline body was rotated during the growth thereof at a speed of 48 revolutions per minute. Line 102 in Fig. 2 indicates the interface of the non-rotated and rotated portions of crystalline body 100.
  • a high-impurity concentration region 104 was formed in the upper portion 100a during the growth thereof.
  • the region 104 was characterized by vertical ⁇ triations or rashes extending parallel to the axis of the crystalline body 100 and extending across about a 15° segment of the entire circumference of the body.
  • the portions 106 of the upper portion 100a adjacent region 104 did not contain such striations.
  • the aluminum impurity concentration of region 104 was determined to be 846 pp and the aluminum impurity concentration of region 106 was found to be 59ppm.
  • the aluminum impurity concentration of region 108 in lower portion 100b which is positioned directly below region 104 in upper portion 100a, was found to be 506ppm.
  • the aluminum impurity concentration of region 110 adjacent region 108 was found to be 425ppm.
  • This change in impurity concentration between upper portion 100a and lower portion 100b confirms that the method of the present invention improves the evenness of distribution of impurities in a crystalline body grown according to the method of the present invention.
  • the melt used to grow crystalline body 100 was doped with aluminum to a much greater concentration than is typical for a melt from which crystalline bodies used to make solar cell substrates are grown. However, it is believed that similar improvement in the uniformity of distribution of impurities will be achieved with the method of the present invention for crystalline bodies grown from a silicon melt having an impurity mix and concentration consistent with that used to grow crystalline bodies from which solar cell substrates are fabricated.
  • impurity concentrations may increase precipitously at the end of the growth run, particularly when feedstock having a higher impurity concentration than that of ethyl silicon is used.
  • the method of the present invention has important application as a process for improving the evenness of distribution of impurities in a crystalline body.
  • the wall thickness of crystalline body 100 was 5 mils, plus or minus 0.5 mils.
  • tubular crystalline bodies having a polygonal cross section grown by the EFG process without rotation using state-of-the art crystal growth apparatus typically have a wall thickness of 16 mils, plus or minus 8 mils.
  • a second experiment was conducted to verify that the method of the present invention improves the evenness of distribution of impurities in a crystalline body.
  • the second experiment was substantially identical to the first experiment described above, except that both iron and aluminum were added as impurities to the silicon melt from which crystalline body 200 was grown.
  • upper portion 200a was not rotated, while lower portion 200b was rotated during the growth thereof at a speed of 48 revolutions per minute.
  • Line 202 represents the interface between the upper and lower portions.
  • a high-impurity concentration region 204 was formed having an impurity concentration of 235ppm for iron and 367 for aluminum.
  • the adjacent low-impurity concentration region 206 in upper portion 200a had an impurity concentration of 7ppm for iron and 4ppm for aluminum.
  • region 208 of lower portion 200b of body'200 which lower portion was rotated during the growth thereof, was 118ppm for iron and 162ppm for aluminum.
  • Region 208 is positioned directly below high-impurity region 204 in upper portion 200a.
  • the impurity concentration of region 210, which is adjacent region 208 in lower portion 200b, is 126ppm for iron and 164pp ⁇ for aluminum.
  • the wall thickness of crystalline body 200 was 5 mils, plus or minus 0.5 mils.
  • the wall thickness of a crystalline body having improved uniformity of impurity distribution as measured about a circumference thereof.
  • the apparatus of the present invention it is possible to grow a tubular crystalline body having wall thickness variations of less than + 0.5 mils as measured about a selected circumferential band of the body.
  • the ability to more precisely control wall thickness comes the ability to grow crystalline bodies with the present method having relatively thin walls, e.g. about 5 mils thick.
  • a second advantage occurs in connection with improving the uniformity of impurity distribution.
  • Substrates cut from tubular crystalline bodies grown with the apparatus of the present invention have reduced dislocation density and greater as-grown minority carrier diffusion lengths.
  • solar cell performance typically decreases as dislocation density increases and increases as minority carrier diffusion lengths increase.
  • the method of the present invention is also advantageous inasmuch as the crystalline bodies grown according to the method have a circular cross section. As compared to crystalline bodies having polygon cross sections, crystalline bodies having circular cross sections have fewer internal stresses and hence less propensity to crack.
  • Ethyl silicon be used as the feed stock in the present method
  • the above-described advantages of the present invention are also achieved when other, lower grade silicon stock is used.
  • Ethyl silicon shall mean silicon of the type manufactured by Ethyl Corporation, Electronic Materials Division, of Baton Rouge, Louisiana and described above in greater detail.

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

Abstract

Procédé destiné à la croissance de corps cristallins tubulaires et cylindriques dans lesquels des impuretés sont réparties à des niveaux d'uniformité améliorés par rapport à la répartition d'impuretés dans des corps cristallins tubulaires non cylindriques et qui ne sont pas mis en rotation au cours du processus de croissance. Le procédé consiste à produire un corps cristallin cylindrique et tubulaire selon la méthode EFG et en mettant en rotation le corps cylindrique à une vitesse d'environ 35-65 tours/min pendant tout le temps où le corps est en train d'être tiré de la matrice de déformation. Des corps cristallins présentant une épaisseur de paroi de 5 millièmes de pouce, plus ou moins 0,5 millième, ont été obtenus selon ce procédé.
PCT/US1991/005676 1990-08-15 1991-08-09 Procede de croissance de corps cristallins tubulaires et cylindriques Ceased WO1992003204A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US56793890A 1990-08-15 1990-08-15
US567,938 1990-08-15

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WO1992003204A1 true WO1992003204A1 (fr) 1992-03-05

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3552931A (en) * 1967-07-14 1971-01-05 Little Inc A Apparatus for imparting translational and rotational motion
US3846082A (en) * 1971-11-08 1974-11-05 Tyco Laboratories Inc Production of crystalline bodies of complex geometries
US4544528A (en) * 1981-08-03 1985-10-01 Mobil Solar Energy Corporation Apparatus for growing tubular crystalline bodies

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3552931A (en) * 1967-07-14 1971-01-05 Little Inc A Apparatus for imparting translational and rotational motion
US3846082A (en) * 1971-11-08 1974-11-05 Tyco Laboratories Inc Production of crystalline bodies of complex geometries
US4544528A (en) * 1981-08-03 1985-10-01 Mobil Solar Energy Corporation Apparatus for growing tubular crystalline bodies

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"The Tubular Silicon Solar Cell-A New Concept For photovoltaic Power Generation", MLAUSKY et al., "MOBIL TYCO SOLAR ENERGY CORPORATION; p.p. 160-167. *

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Publication number Publication date
AU9034491A (en) 1992-03-17

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