WO2005121416A1 - 結晶製造方法および装置 - Google Patents
結晶製造方法および装置 Download PDFInfo
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- WO2005121416A1 WO2005121416A1 PCT/JP2005/010719 JP2005010719W WO2005121416A1 WO 2005121416 A1 WO2005121416 A1 WO 2005121416A1 JP 2005010719 W JP2005010719 W JP 2005010719W WO 2005121416 A1 WO2005121416 A1 WO 2005121416A1
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- crystal
- raw material
- crucible
- temperature
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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
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/136—Liquid crystal cells structurally associated with a semi-conducting layer or substrate, e.g. cells forming part of an integrated circuit
-
- 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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/001—Continuous 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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/04—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method adding crystallising materials or reactants forming it in situ to the melt
-
- 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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/04—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method adding crystallising materials or reactants forming it in situ to the melt
- C30B11/08—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method adding crystallising materials or reactants forming it in situ to the melt every component of the crystal composition being added during the crystallisation
-
- 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
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/30—Niobates; Vanadates; Tantalates
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
-
- 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
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
- Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
-
- 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
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
- Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
- Y10T117/1032—Seed pulling
- Y10T117/1052—Seed pulling including a sectioned crucible [e.g., double crucible, baffle]
-
- 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
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
- Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
- Y10T117/1032—Seed pulling
- Y10T117/1056—Seed pulling including details of precursor replenishment
-
- 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
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
- Y10T117/10—Apparatus
- Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
- Y10T117/1092—Shape defined by a solid member other than seed or product [e.g., Bridgman-Stockbarger]
Definitions
- the present invention relates to a method and an apparatus for producing a crystal, and more particularly to a method and an apparatus for producing a large-sized and high-quality crystal by a vertical Bridgman method, a vertical temperature gradient solidification method, or the like.
- a method for producing a crystal there is known a method in which a seed crystal is brought into contact with a surface of a raw material that has been liquefied in advance, and the temperature of the raw material that has been liquefied is lowered to grow the crystal using the seed crystal as a nucleus.
- Such a method includes a “TSSG (Top-Seed-Solution-Growth) method” for growing a crystal with a solution force (see, for example, Patent Document 1) and a “pulling method” for growing a crystal from a melt (eg, And Patent Document 2).
- the first problem is that the growth rate during growth changes for each part of the crystal, and as a result, the crystal quality of the crystal fluctuates.
- a vertical Bridgman method for example, see Patent Document 3
- a vertical temperature gradient solidification method for example, see Patent Document 4
- the vertical Bridgman method places a crucible vertically and gives a temperature gradient.
- the output of the heater is adjusted so that the lower part of the crucible is a low-temperature region lower than the crystallization temperature and the upper part of the crucible is a high-temperature region higher than the crystallization temperature.
- the heater output kept constant, the crucible is moved to a low-temperature region and cooled to grow crystals.
- the vertical temperature gradient solidification method fixes the crucible vertically.
- the output of the heater is adjusted so that the lower portion is a low-temperature region lower than the crystallization temperature and the upper portion is a high-temperature region higher than the crystallization temperature. While maintaining this temperature gradient, the output of the heater is changed and the crystal is grown by cooling from below the crucible.
- the raw material is filled in the crucible 1 and heated and liquefied to obtain a liquid raw material 2.
- the crystal production furnace has a temperature distribution 5 in which a region below the crucible 1 is a low-temperature region lower than the crystallization temperature and a region above the crucible 1 is a high-temperature region higher than the crystallization temperature.
- the liquid raw material 2 is cooled by moving the crucible 1 at a constant speed to a low-temperature region, that is, a lower portion, while keeping the output of the heater constant.
- the crystal 3 that has reached the crystallization temperature grows with the seed crystal 4 as a nucleus.
- the raw material is filled in the crucible 1 and liquefied by heating to form a liquid raw material 2.
- the crystal production furnace has a temperature distribution 5 in which a region below the crucible 1 is a low-temperature region lower than the crystallization temperature and a region above the crucible 1 is a high-temperature region higher than the crystallization temperature. With the furnace position of the crucible 1 fixed, the temperature of the crucible 1 is lowered at a constant speed by changing the output of the heater while maintaining the temperature gradient as shown in the figure. By changing the temperature distribution, the crystal 3 which has reached the crystallization temperature grows with the seed crystal 4 as a nucleus.
- FIG. 3 shows a phase diagram of a solid solution crystal of ABC power.
- the three components A, B, and C may be composed of a plurality of components.
- Solid solution crystals ABC generally have a liquidus line 6 and a solidus line 7 is off.
- a crystal having the composition at the point b of the solidus line 7 grows. Since more component B is incorporated into the solid phase, component B in the liquid phase is reduced. Therefore, in proportion to the progress of crystal growth, the composition of the liquid phase changes from the a-point force to the composition at point c along the liquidus line 6, and the composition of the grown crystal also changes at the d point along the solidus line 7. Changes in composition.
- the produced crystal gradually changes to the composition at the point d at the composition force at the point b over the length direction.
- this method has a third problem that the additional supply of the replenishment raw material 9 causes a deterioration in crystal quality and a decrease in yield due to frequent occurrence of polycrystallization.
- the processing temperature higher than the crystallization temperature to 20% or more by the processing temperature (hereinafter referred to as the soaking temperature) with a high LOO degree. It is necessary to perform a soaking process to decompose and grow crystals. If crystals are grown without soaking treatment, the crystal quality will deteriorate and polycrystallization will occur.
- the replenishment material cannot be supplied in a state where the soaking process has been performed, and the third problem described above has occurred.
- replenishment raw material 9 is supplied as a liquid near the powder or crystallization temperature, the temperature of the liquid raw material 2 is changed, and the crystal growth rate is changed. There was also a fourth problem that the crystal quality fluctuated depending on the crystal position due to the fluctuation of the growth rate.
- Patent Document 1 US Pat. No. 5,858,898
- Patent Document 2 US Pat. No. 5,290,395
- Patent Document 3 US Pat. No. 5,342,475
- Patent Document 4 U.S. Pat.No. 4,404,172
- Patent Document 5 US Pat. No. 5,787,784
- Patent Document 6 US Pat. No. 6,733,330
- An object of the present invention is to provide a crystal manufacturing method and apparatus capable of maintaining crystal quality and making a crystal composition uniform from an early growth stage to a late growth stage.
- the present invention heats and liquefies a raw material in a crucible held in a furnace, and gradually cools the raw material upward from below the crucible to grow the crystal.
- the temperature distribution in the vertical direction in the furnace holding the crucible includes a low-temperature region below the crystallization temperature below and a high-temperature region above the crystallization temperature above it.
- the heater is adjusted so that the replenishing raw material supplied from the raw material supply device installed above the crucible is heated to the same temperature as the high temperature region and supplied to the crucible.
- the replenishment raw material corresponding to the amount of the crystal grown is supplied at the same temperature as the liquid raw material obtained by liquefying the initial filling raw material. Crystal can be grown.
- the replenishment raw material becomes a liquid raw material that is sufficiently high and decomposed at the temperature. Can be additionally supplied.
- a crystal production apparatus that is powerful in the present invention is a raw material supply device that supplies a supplementary material, and a crucible that is installed above the crucible and liquefies the supplementary material supplied from the material supply device to serve as a liquid material. And a reflecting plate for dropping the reflecting plate.
- the replenishment raw material for crystal growth can be liquefied by the reflector provided above the crucible, and can be dropped into the crucible as a liquid raw material.
- FIG. 1 is a diagram for explaining a conventional method for producing a crystal by a vertical Bridgman method.
- FIG. 2 is a diagram showing a conventional method for producing a crystal by a vertical temperature gradient solidification method.
- FIG. 3 is a phase diagram of a solid solution crystal composed of AB x Cix ,
- FIG. 4 is a diagram for explaining a method for suppressing a change in composition by additionally supplying a raw material during crystal growth.
- FIG. 5 is a view showing a configuration of a crystal production apparatus according to a first embodiment of the present invention.
- FIG. 6 is a view showing a configuration of a crystal production apparatus provided with a plurality of raw material supply devices.
- FIG. 7 is a view showing a configuration of a crystal crystal manufacturing apparatus according to a second embodiment of the present invention.
- FIG. 8 is a configuration of a crystal crystal manufacturing apparatus according to a third embodiment of the present invention.
- FIG. 9A is a top view showing a funnel-type reflecting plate according to an embodiment of the present invention.
- FIG. 9B is a side view showing a funnel-type reflecting plate according to an embodiment of the present invention.
- FIG. 9C is a top view showing another form of the funnel reflection.
- FIG. 9D is a top view showing another form of the funnel reflection.
- FIG. 9E is a top view showing another form of the funnel reflection.
- FIG. 10A is a top view showing a trumpet-type reflecting plate according to an embodiment of the present invention.
- FIG. 10B is a side view showing a trumpet-type reflecting plate according to an embodiment of the present invention.
- FIG. 10C is a top view showing another embodiment of the trumpet-type reflector.
- FIG. 10D is a top view showing another embodiment of the trumpet-type reflector.
- FIG. 10E is a top view showing another form of the trumpet-type reflector.
- FIG. 5 shows a crystal manufacturing apparatus according to the first embodiment of the present invention.
- the case of producing large KTa Nb ⁇ (0 ⁇ 1) crystal by the vertical Bridgman method is shown.
- the crystal manufacturing apparatus liquefies the replenishing raw material 19 supplied from the raw material supply device 18, performs a soaking process, and then places a funnel-shaped reflector 20 that is dropped into the crucible 11 as a liquid raw material 21 above the crucible 11.
- Example 1 the crystallization temperature was 1180 ° C., the soaking temperature was 1280 ° C., and the temperature was maintained for 10 hours.
- the crucible 11 is slowly lowered at a speed of 2 mmZ days, and the replenishment material 19 is dropped from the material supply device 18 onto the heated funnel-type reflector 20.
- the funnel-type reflector 20 is made of, for example, platinum. Since the funnel-type reflector 20 is heated by the radiant heat from the crucible 11 and the heat convection in the furnace, the replenishment raw material 19 is converted into a liquid without requiring a heating mechanism for heating the funnel-type reflector 20. I can do it.
- the vertical position of the funnel-type reflector 20 is adjusted so that the surface temperature thereof becomes a soaking temperature of 1280 degrees.
- the funnel-type reflection plate 20 may be provided with a heating mechanism such as a heater, for example, so that the temperature of the liquid raw material 21 matches the temperature of the upper portion of the crucible 11 described above.
- the position of the funnel-type reflection plate 20 may be moved in conjunction with the crucible 11 if it is installed above the crucible 11, or may be used to adjust the supply temperature of the liquid raw material 21. Alternatively, it may be made to move independently of the crucible 11. It is desirable that the surface area of the funnel-type reflector 20 be sufficiently large so as to be heated to the soaking temperature by radiant heat from the crucible 11 and heat convection in the furnace. Also, it is desirable that sufficient heat capacity is provided so that temperature fluctuations are reduced even if the replenishment material 19 falls.
- the supply amount of the raw material is made to match the amount consumed by the crystal growth. 2 inches used In the diameter crucible, the 2 mm thick crystal in the constant diameter part weighs 13 g, so the supply rate of the replenishment material 19 is 13 gZ days. This supply rate is converted into minutes, and the supply material 19 is supplied at a rate of 9 mgZ.
- the arrangement of the raw material supply device 18 is shifted relative to the funnel-type reflector 20 so that the supply material 19 falls on the inner surface of the funnel-type reflector 20. As a result, the replenishment raw material 19 drips while falling on the inner surface of the funnel type reflection plate 20.
- the angle of the inclined surface of the funnel-type reflecting plate 20 was adjusted such that the liquid-reacted raw material stayed on the inclined surface for one hour.
- the replenishing raw material 19 becomes a soaked liquid raw material 21 while falling on the inner surface of the funnel-type reflector 20, and is supplied stably into the crucible 11 through the funnel-type reflector 20.
- the raw material corresponding to the amount of the crystal grown is subjected to the soaking process, and is supplied as the liquid raw material 21 having the same temperature as the liquid raw material 12 obtained by liquefying the initial filling raw material.
- the temperature and composition of 2 can always be kept constant. Further, since the replenished liquid raw material 21 has been soaked and sufficiently decomposed, it is possible to stably grow a highly uniform growth crystal 13 having no composition change.
- FIG. 6 shows a configuration of a crystal manufacturing apparatus provided with a plurality of raw material supply apparatuses.
- FIG. 7 shows a crystal manufacturing apparatus according to a second embodiment of the present invention.
- the case of producing a long KTa Nb ⁇ (0 ⁇ 1) crystal by the vertical Bridgman method is shown.
- the crystal manufacturing apparatus liquefies the replenishing raw material 19 supplied from the raw material supply device 18, performs a soaking process, and then places a funnel-shaped reflector 20 that is dropped into the crucible 11 as a liquid raw material 21 above the crucible 11. Provided.
- the temperature at the lower part of the crucible 11 is lower than the crystallization temperature determined by the raw material composition, and the temperature at the upper part of the crucible 11 is a soaking temperature higher than the crystallization temperature. At this time, it goes without saying that the seed crystal 14 is not melted.
- the crystallization temperature was 1180 ° C.
- the soaking temperature was 1280 ° C.
- the temperature was maintained for 10 hours.
- the crucible 11 is slowly lowered at the speed of ImmZ days, and the replenishing material 19 is dropped from the material supply device 18 to the heated funnel-type reflector 20.
- the funnel-type reflector 20 is made of, for example, platinum. Since the funnel-type reflector 20 is heated by the radiant heat from the crucible 11 and the heat convection in the furnace, the replenishment raw material 19 is converted into a liquid without requiring a heating mechanism for heating the funnel-type reflector 20. I can do it.
- the vertical position of the funnel-type reflector 20 is adjusted so that the surface temperature thereof becomes a soaking temperature of 1280 degrees.
- the supply amount of the raw material is made to match the amount consumed by the crystal growth.
- the crystal with lmm thickness in the constant diameter part weighs 7 g, so the supply speed of replenishment material 19 is 7 gZ days. This supply rate is converted into minutes, and the supply material 19 is supplied at a rate of 5 mgZ.
- the arrangement of the raw material supply device 18 is such that the replenishment raw material 19 is It is shifted relative to the funnel-type reflector 20 so that it falls on the inner surface. Thereby, the replenishment raw material 19 is liquefied while falling on the inner surface of the funnel-type reflector 20.
- the angle of the inclined surface of the funnel type reflection plate 20 was adjusted such that the liquid-reacted raw material stayed on the inclined surface for one hour.
- the replenishing raw material 19 becomes a soaked liquid raw material 21 while falling on the inner surface of the funnel-shaped reflector 20, and is supplied stably into the crucible 11 through the funnel-shaped reflector 20.
- the distance between the crucible 11 and the funnel-shaped reflector 20 increases as the crystal grows. For this reason, the liquid raw material 21 that has been liquid-dried has a higher falling speed due to gravity and scatters in a milk crown shape. Therefore, the distance between the crucible 11 and the funnel-type reflector 20 is kept constant by lowering the funnel-type reflector 20 at the same speed as the crucible 11. By keeping the distance constant, scattering of the solution composition 12 can be suppressed.
- the raw material corresponding to the amount of the crystal grown is subjected to the soaking process, and is supplied as the liquid raw material 21 having the same temperature as the liquid raw material 12 obtained by liquefying the initial filling raw material.
- the temperature and composition of 2 can always be kept constant.
- the liquid raw material 21 since the liquid raw material 21 has been soaked and sufficiently decomposed, it is possible to stably grow the highly uniform grown crystal 13 having no composition change.
- FIG. 8 shows a crystal manufacturing apparatus according to a third embodiment of the present invention.
- the case of fabricating a KTa Nb ⁇ (0 ⁇ 1) crystal by the vertical Bridgman method is shown.
- the crystal manufacturing apparatus performs a soaking process on the replenishing raw material 19 supplied from the raw material supply device 18, performs a soaking process on the replenishing raw material 19, and then drops a trumpet-type reflector 22 which is dropped into the crucible 11 as a liquid raw material 21, above the crucible 11. Is provided.
- the temperature of the lower part of the crucible 11 is lower than the crystallization temperature determined by the raw material composition.
- the temperature above the low crucible 11 is a soaking temperature higher than the crystallization temperature. At this time, it goes without saying that the seed crystal 14 is not melted.
- the crystallization temperature was 1180 ° C.
- the soaking temperature was 1230 ° C.
- the temperature was maintained for 20 hours.
- the crucible 11 is slowly lowered at a speed of 2 mmZ days, and the replenishment material 19 is dropped from the material supply device 18 onto the heated flared reflector 22.
- the trumpet-type reflector 22 is made of, for example, platinum. Since the flapper-type reflector 22 is heated by the radiant heat from the crucible 11 and the heat convection in the furnace, the replenishment raw material 19 can be converted without using a heating mechanism for heating the flapper-type reflector 22. I can do it.
- the position of the flapper-type reflector 22 in the vertical direction is adjusted so that the surface temperature thereof becomes a soaking temperature of 1230 degrees.
- the wrapper-type reflection plate 22 may be provided with a heating mechanism such as a heater, for example, so that the temperature of the liquid raw material 21 matches the temperature of the upper portion of the crucible 11 described above.
- the position of the trumpet-type reflector 22 may be moved in conjunction with the crucible 11 if it is installed above the crucible 11, or may be used to adjust the supply temperature of the liquid raw material 21. Alternatively, it may be made to move independently of the crucible 11. It is desirable that the surface area of the flapper-type reflector 22 be sufficiently large so as to be heated to the soaking temperature by radiant heat from the crucible 11 and heat convection in the furnace. Also, it is desirable that sufficient heat capacity is provided so that temperature fluctuations are reduced even if the replenishment material 19 falls.
- the supply amount of the raw material is made to match the amount consumed by the crystal growth.
- the 2 mm thick crystal in the fixed diameter part weighs 55 g, so the supply rate of replenishment material 19 is 55 gZ days. This feed rate is converted into minutes and feedstock 19 is supplied at a rate of 38 mgZ.
- the arrangement of the raw material supply device 18 is such that the raw material supply device 18 can be positioned directly above the trumpet-type reflector 22 or the replenishment material 19 can be dropped on the inclined surface of the trumpet-type reflector 22. May be relatively shifted. If it is directly above, It is preferable that the tip of the P-type reflection plate 22 has a triangular pyramid shape.
- the replenishment raw material 19 is liquefied while falling on the inclined surface of the trumpet-type reflector 22.
- the angle of the inclined surface of the trumpet-type reflector 22 was adjusted such that the raw material after the liquid stayed on the inclined surface for one hour.
- the replenishing raw material 19 becomes a soaked liquid raw material 21 while falling on the inclined surface of the trumpet-type reflector 22, and is stably supplied into the crucible 11 through the trumpet-type reflector 22.
- the raw material corresponding to the amount of the crystal grown is subjected to the soaking process, and is supplied as the liquid raw material 21 having the same temperature as the liquid raw material 12 obtained by liquefying the initial filling raw material.
- the temperature and composition of 2 can always be kept constant.
- the liquid raw material 21 since the liquid raw material 21 has been soaked and sufficiently decomposed, it is possible to stably grow the highly uniform grown crystal 13 having no composition change.
- FIGS. 9A to 9E show a funnel-type reflecting plate according to an embodiment of the present invention.
- FIG. 9A shows a top view
- FIG. 9B shows a side view of a funnel-type reflector 20 applicable to the crystal manufacturing apparatus shown in FIGS. 5-7.
- the funnel-type reflection plate 20 has a funnel shape that narrows downward from above and has a drop port 31 at the bottom for dropping the liquid raw material 21 into the crucible 11.
- a spiral groove 32 and a radial groove 33 may be formed inside the funnel.
- the powdery replenishing raw material 19 dropped from the raw material supply device 18 drips on the funnel-shaped reflecting plate 20, flows through the grooves 32, 33, and flows from the falling port 31 to the crucible 11. Fall.
- the cross-sectional shapes of the grooves 32 and 33 are basically triangular, square, and semi-circular, and an optimum shape is selected based on the viscosity of the liquefied replenishment material 19.
- the time during which the replenishment raw material 19 stays on the funnel-type reflector 20 after it is liquefied can be adjusted.
- it is a semicircle having a width of 5 mm and a depth of 3 mm. This makes it possible to supply The liquid 19 can be stably liquid and supplied to the crucible 11 as a liquid raw material 21.
- FIG. 10A to FIG. 10E show a trumpet-type reflector that is useful in one embodiment of the present invention.
- FIG. 10A is a top view and
- FIG. 10B is a side view of a flapper-type reflector 22 applicable to the crystal manufacturing apparatus shown in FIG.
- the trumpet-type reflector 22 has a trumpet shape that spreads downward.
- a spiral groove 32 and a groove 33 formed radially from the center to the outer periphery may be formed outside the wrapper.
- the powdery replenishing material 19 dropped from the material supply device 18 can flow through the grooves 32 and 33 by squeezing on the flared reflector 22.
- the cross-sectional shapes of the grooves 32 and 33 are basically triangular, square, and semi-circular, and an optimum shape is selected for the viscous force of the liquefied replenishment material 19.
- the time during which the replenishing material 19 stays on the trumpet-type reflector 22 after the refilling can be adjusted.
- it is a semicircle having a width of 5 mm and a depth of 3 mm.
- the force described in the method for producing a KTaNbO crystal can be applied to the production of a crystal having another composition.
- the main component of the crystal is also composed of the periodicity table la group and Va group oxide or carbonate power, the la group is lithium and potassium, and the Va group is at least one of niobium and tantalum. Can be included.
- one or more of the la group of the periodic table, such as lithium, or the Ila group, may be included as an additive impurity.
- the solution In order to keep the dopant concentration constant in crystals that also produce melts, such as B-doped Si, P-doped Si, In-doped GaAs, Si-doped GaAs, and Fe-doped InP crystals, the solution must be mixed with the melt and soaked.
- the same effects as in the present embodiment can be obtained by replacing the treatment with the overheating treatment, the soaking temperature as the overheating treatment temperature, and the platinum as quartz glass or p-BN.
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- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Nonlinear Science (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Inorganic Chemistry (AREA)
- Mathematical Physics (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
Claims
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
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JP2006514595A JP4255972B2 (ja) | 2004-06-11 | 2005-06-10 | 結晶製造方法および装置 |
EP05749034.4A EP1757716B1 (en) | 2004-06-11 | 2005-06-10 | Method and apparatus for preparing crystal |
CNB2005800008661A CN100570018C (zh) | 2004-06-11 | 2005-06-10 | 结晶制造方法以及装置 |
KR1020067004839A KR100753322B1 (ko) | 2004-06-11 | 2005-06-10 | 결정 제조 방법 및 장치 |
US10/571,887 US7591895B2 (en) | 2004-06-11 | 2005-06-10 | Method and apparatus for producing crystals |
Applications Claiming Priority (2)
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JP2004-174699 | 2004-06-11 | ||
JP2004174699 | 2004-06-11 |
Publications (1)
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WO2005121416A1 true WO2005121416A1 (ja) | 2005-12-22 |
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PCT/JP2005/010719 WO2005121416A1 (ja) | 2004-06-11 | 2005-06-10 | 結晶製造方法および装置 |
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US (1) | US7591895B2 (ja) |
EP (1) | EP1757716B1 (ja) |
JP (1) | JP4255972B2 (ja) |
KR (1) | KR100753322B1 (ja) |
CN (1) | CN100570018C (ja) |
WO (1) | WO2005121416A1 (ja) |
Cited By (4)
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JP2009137781A (ja) * | 2007-12-04 | 2009-06-25 | Nippon Telegr & Teleph Corp <Ntt> | 結晶成長方法およびその装置 |
JP2010143782A (ja) * | 2008-12-18 | 2010-07-01 | Shinshu Univ | 融液組成制御一方向凝固結晶成長装置および結晶成長方法 |
JP2012508153A (ja) * | 2008-11-10 | 2012-04-05 | エーエックスティー,インコーポレーテッド | 単結晶ゲルマニウムの結晶成長システム、方法および基板 |
JP2019006657A (ja) * | 2017-06-28 | 2019-01-17 | 日本電信電話株式会社 | 単結晶成長方法及び単結晶成長装置 |
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ATE544884T1 (de) † | 2007-12-19 | 2012-02-15 | Schott Ag | Verfahren zur herstellung eines monokristallinen oder polykristallinen halbleitermaterials |
CN102359926B (zh) * | 2011-09-09 | 2013-01-02 | 苏州浩波科技股份有限公司 | 安赛蜜结块周期的测算方法 |
KR101484961B1 (ko) * | 2014-08-08 | 2015-01-22 | 한국기계연구원 | 생체 영감의 표면 구조를 갖는 수지상 3차원 나노 구조체 및 그 제조 방법 |
CN109629003B (zh) * | 2018-12-29 | 2021-05-28 | 珠海鼎泰芯源晶体有限公司 | 一种低浓度p型磷化铟单晶的制备方法 |
Citations (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4404172A (en) | 1981-01-05 | 1983-09-13 | Western Electric Company, Inc. | Method and apparatus for forming and growing a single crystal of a semiconductor compound |
JPS61236681A (ja) * | 1985-04-13 | 1986-10-21 | Tohoku Metal Ind Ltd | 単結晶の製造方法及び製造装置 |
JPS6259593A (ja) * | 1985-09-09 | 1987-03-16 | Tohoku Metal Ind Ltd | 単結晶製造方法 |
JPS6296387A (ja) * | 1985-10-22 | 1987-05-02 | Tohoku Metal Ind Ltd | 単結晶の製造方法 |
JPS62191488A (ja) * | 1986-02-17 | 1987-08-21 | Sanyo Electric Co Ltd | 単結晶製造装置 |
US5290395A (en) | 1990-07-26 | 1994-03-01 | Sumitomo Electric Industries, Ltd. | Method of and apparatus for preparing single crystal |
JPH06157185A (ja) | 1992-09-25 | 1994-06-03 | Furukawa Electric Co Ltd:The | 化合物半導体単結晶の成長方法 |
US5342475A (en) | 1991-06-07 | 1994-08-30 | The Furukawa Electric Co., Ltd. | Method of growing single crystal of compound semiconductor |
JPH0867592A (ja) | 1994-08-31 | 1996-03-12 | Sony Corp | Mn−Zn系フェライト単結晶及びMn−Zn系フェライト単結晶の製造方法 |
US5785898A (en) | 1993-04-21 | 1998-07-28 | California Institute Of Technology | Potassium lithium tantalate niobate photorefractive crystals |
US5788764A (en) | 1995-01-19 | 1998-08-04 | Hoya Corporation | KTP solid solution single crystals and process for the production thereof |
JPH111388A (ja) | 1997-06-10 | 1999-01-06 | Kawatetsu Mining Co Ltd | 単結晶成長方法及び装置 |
WO1999063132A1 (fr) * | 1998-05-29 | 1999-12-09 | Toyo Communication Equipement Co., Ltd. | Dispositif et procede servant a fabriquer des monocristaux et monocristal |
US6673330B1 (en) | 1999-03-26 | 2004-01-06 | National Institute For Research In Inorganic Materials | Single crystal of lithium niobate or tantalate and its optical element, and process and apparatus for producing an oxide single crystal |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4521272A (en) | 1981-01-05 | 1985-06-04 | At&T Technologies, Inc. | Method for forming and growing a single crystal of a semiconductor compound |
JPH1111388A (ja) | 1997-06-23 | 1999-01-19 | Mitsubishi Heavy Ind Ltd | 電磁推進装置 |
JP4055362B2 (ja) * | 2000-12-28 | 2008-03-05 | 信越半導体株式会社 | 単結晶育成方法および単結晶育成装置 |
-
2005
- 2005-06-10 EP EP05749034.4A patent/EP1757716B1/en not_active Ceased
- 2005-06-10 JP JP2006514595A patent/JP4255972B2/ja active Active
- 2005-06-10 KR KR1020067004839A patent/KR100753322B1/ko active IP Right Grant
- 2005-06-10 CN CNB2005800008661A patent/CN100570018C/zh not_active Expired - Fee Related
- 2005-06-10 US US10/571,887 patent/US7591895B2/en active Active
- 2005-06-10 WO PCT/JP2005/010719 patent/WO2005121416A1/ja not_active Application Discontinuation
Patent Citations (15)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4404172A (en) | 1981-01-05 | 1983-09-13 | Western Electric Company, Inc. | Method and apparatus for forming and growing a single crystal of a semiconductor compound |
JPS61236681A (ja) * | 1985-04-13 | 1986-10-21 | Tohoku Metal Ind Ltd | 単結晶の製造方法及び製造装置 |
JPS6259593A (ja) * | 1985-09-09 | 1987-03-16 | Tohoku Metal Ind Ltd | 単結晶製造方法 |
JPS6296387A (ja) * | 1985-10-22 | 1987-05-02 | Tohoku Metal Ind Ltd | 単結晶の製造方法 |
JPS62191488A (ja) * | 1986-02-17 | 1987-08-21 | Sanyo Electric Co Ltd | 単結晶製造装置 |
US5290395A (en) | 1990-07-26 | 1994-03-01 | Sumitomo Electric Industries, Ltd. | Method of and apparatus for preparing single crystal |
US5342475A (en) | 1991-06-07 | 1994-08-30 | The Furukawa Electric Co., Ltd. | Method of growing single crystal of compound semiconductor |
JPH06157185A (ja) | 1992-09-25 | 1994-06-03 | Furukawa Electric Co Ltd:The | 化合物半導体単結晶の成長方法 |
US5785898A (en) | 1993-04-21 | 1998-07-28 | California Institute Of Technology | Potassium lithium tantalate niobate photorefractive crystals |
JPH0867592A (ja) | 1994-08-31 | 1996-03-12 | Sony Corp | Mn−Zn系フェライト単結晶及びMn−Zn系フェライト単結晶の製造方法 |
US5788764A (en) | 1995-01-19 | 1998-08-04 | Hoya Corporation | KTP solid solution single crystals and process for the production thereof |
JPH111388A (ja) | 1997-06-10 | 1999-01-06 | Kawatetsu Mining Co Ltd | 単結晶成長方法及び装置 |
WO1999063132A1 (fr) * | 1998-05-29 | 1999-12-09 | Toyo Communication Equipement Co., Ltd. | Dispositif et procede servant a fabriquer des monocristaux et monocristal |
US6402834B1 (en) | 1998-05-29 | 2002-06-11 | Toyo Communication Equipment Co., Ltd. | Apparatus and method for manufacturing monocrystals |
US6673330B1 (en) | 1999-03-26 | 2004-01-06 | National Institute For Research In Inorganic Materials | Single crystal of lithium niobate or tantalate and its optical element, and process and apparatus for producing an oxide single crystal |
Non-Patent Citations (1)
Title |
---|
See also references of EP1757716A4 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2009137781A (ja) * | 2007-12-04 | 2009-06-25 | Nippon Telegr & Teleph Corp <Ntt> | 結晶成長方法およびその装置 |
JP2012508153A (ja) * | 2008-11-10 | 2012-04-05 | エーエックスティー,インコーポレーテッド | 単結晶ゲルマニウムの結晶成長システム、方法および基板 |
JP2010143782A (ja) * | 2008-12-18 | 2010-07-01 | Shinshu Univ | 融液組成制御一方向凝固結晶成長装置および結晶成長方法 |
JP2019006657A (ja) * | 2017-06-28 | 2019-01-17 | 日本電信電話株式会社 | 単結晶成長方法及び単結晶成長装置 |
Also Published As
Publication number | Publication date |
---|---|
US20080271666A1 (en) | 2008-11-06 |
CN100570018C (zh) | 2009-12-16 |
US7591895B2 (en) | 2009-09-22 |
JPWO2005121416A1 (ja) | 2008-04-10 |
EP1757716B1 (en) | 2016-08-17 |
EP1757716A4 (en) | 2010-09-15 |
EP1757716A1 (en) | 2007-02-28 |
CN1842619A (zh) | 2006-10-04 |
KR20060088538A (ko) | 2006-08-04 |
KR100753322B1 (ko) | 2007-08-29 |
JP4255972B2 (ja) | 2009-04-22 |
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