WO2002006569A1 - Produit cristallin a surface libre en cristal epitaxial et procede de production - Google Patents

Produit cristallin a surface libre en cristal epitaxial et procede de production Download PDF

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Publication number
WO2002006569A1
WO2002006569A1 PCT/JP2001/004633 JP0104633W WO0206569A1 WO 2002006569 A1 WO2002006569 A1 WO 2002006569A1 JP 0104633 W JP0104633 W JP 0104633W WO 0206569 A1 WO0206569 A1 WO 0206569A1
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WIPO (PCT)
Prior art keywords
crystal
product
melt
inorganic material
liquid
Prior art date
Application number
PCT/JP2001/004633
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English (en)
Japanese (ja)
Inventor
Shiro Sakuragi
Original Assignee
Shikoku Instrumentation Co.,Ltd.
Union Material, Inc.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shikoku Instrumentation Co.,Ltd., Union Material, Inc. filed Critical Shikoku Instrumentation Co.,Ltd.
Publication of WO2002006569A1 publication Critical patent/WO2002006569A1/fr

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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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/002—Crucibles or containers for supporting 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
    • 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
    • C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi

Definitions

  • the present invention relates to a crystal product having a crystal growth free surface of an inorganic material and a method for producing the same.
  • crystal product means a product that has been processed by cutting or the like into a product shape that does not cause processing loss of expensive and valuable raw material. Devices are polished, deposited, and plated.
  • liquid-repellent state means that the inorganic material melt is completely wettable with contact surfaces such as a support substrate, a mold surface, and a container surface that come into contact with the inorganic material melt. This is because, when viewed microscopically, a gas or vacuum space exists at the interface between the melt and the support substrate, mold surface, and container surface that comes into contact with the melt. The entire surface of the melt forms a free surface. Therefore, “free surface of crystal growth” means that the melt of the inorganic material in the lyophobic state has grown while maintaining the free surface.
  • the present invention provides a crystal product of an inorganic material manufactured by an environment-adaptive technology in which the processing loss unavoidable in the conventional method of obtaining a crystal product by processing such as cutting from an intermediate material and the number of steps involved are reduced. It is intended to be.
  • Another object of the present invention is to provide a crystal of an inorganic material that can be reduced in cost by mass production and has good performance, that is, a crystal product of an inorganic material having a crystal growth free surface.
  • the gist of the present invention is a product-shaped crystal characterized by having a smooth crystal growth free surface of an inorganic material.
  • the crystal growth free surface is a single crystal growth surface, preferably a single crystal growth surface obtained by providing a seed crystal portion at a lower end of a melt of an inorganic material in a liquid repellent state and single crystallizing the crystal.
  • a product shape characterized by having a smooth single crystal growth surface of an inorganic material, preferably having a seed crystal portion at the lower end of the melt in a liquid repellent state of the inorganic material and having a single crystal growth surface. It is a crystal.
  • the free surface for crystal growth is a polycrystal growth surface, and in this case, the present invention relates to a product having a smooth polycrystal growth surface made of an inorganic material. It is crystalline.
  • the present invention provides a crystal product manufacturing method characterized in that a liquid-repellent inorganic material melt is defined in a product shape and solidified and crystallized as it is into a product-shaped crystal having a free surface for crystal growth. And The crystal is grown in an atmosphere that maintains the liquid repellent state of the inorganic material melt.
  • the present invention defines the liquid repellent inorganic material melt in a product shape and maintains the liquid repellent state of the inorganic material melt
  • a crystal product manufacturing method characterized by solidifying and crystallizing as it is in an atmosphere and growing the crystal to obtain a product-shaped crystal having a free surface for crystal growth. The above atmosphere is maintained so that there is no contamination.
  • the present invention defines the liquid-repellent inorganic material melt in a product shape, and controls the liquid-repellent state of the inorganic material melt without contamination.
  • This is a method of manufacturing a crystal product characterized by solidifying and crystallizing as it is in an atmosphere to be maintained and growing the crystal to form a crystal having a product shape having a free surface for crystal growth.
  • a liquid-repellent inorganic material melt obtained by removing a wettability-promoting substance from an inorganic material melt is used.
  • the present invention provides a liquid-repellent liquid obtained by removing a wettability-promoting substance from an inorganic material melt.
  • the inorganic material melt is specified in the product shape, and solidified as it is in an atmosphere that maintains the liquid repellency of the inorganic material melt, preferably in an atmosphere that maintains the liquid repellency of the inorganic material melt without contamination.
  • ⁇ This is a method of manufacturing a crystal product characterized by crystallizing and growing the crystal to obtain a product-shaped crystal having a free surface for crystal growth.
  • the product shape is defined using a crystal growth type of a material suitable for realizing the liquid repellent state of the inorganic material.
  • the present invention provides a liquid repellent inorganic material melt, preferably an inorganic material melt.
  • the liquid-repellent inorganic material melt obtained by removing the wettability promoting substance is defined in the product shape using a crystal growth mold of a material suitable for realizing the liquid-repellent state of the inorganic material.
  • a crystal growth mold of a material suitable for realizing the liquid-repellent state of the inorganic material Under an atmosphere where the liquid repellent state is maintained, preferably in an atmosphere where the liquid repellent state of the inorganic material melt is kept free of contamination, the product is solidified and crystallized as it is and the crystal grows, and the product shape has a free surface for crystal growth And a method for producing a crystal product characterized by being a crystalline body. Crystallization is performed in a single crystal growth atmosphere.
  • the present invention provides a liquid-repellent inorganic material melt, preferably a liquid-repellent inorganic material melt obtained by removing a wettability promoting substance from the inorganic material melt, Defined in the product shape, preferably in a product shape using a crystal growth type of a material suitable for realizing the liquid repellent state of the inorganic material, under an atmosphere in which the liquid repellent state of the inorganic material melt is maintained, Preferably, the product is solidified and crystallized as it is in an atmosphere in which the liquid repellent state of the inorganic material melt is kept free of contamination and in a single crystal growth atmosphere, and crystal growth is performed, and a crystal growth free surface is provided.
  • a single crystal is formed by providing a seed crystal portion at the lower end of the liquid-repellent inorganic material melt.
  • the present invention removes the wettability promoting substance from the liquid-repellent inorganic material melt, preferably from the inorganic material melt.
  • the liquid-repellent inorganic material melt obtained as described above is defined in the product shape, preferably the crystal shape of a material suitable for realizing the liquid-repellent state of the inorganic material is specified in the product shape.
  • the liquid repellency of the inorganic material melt is preferably maintained so as not to cause contamination.
  • a seed crystal part is provided at the lower end of the liquid-repellent inorganic material melt under a single atmosphere and solidified and crystallized as it is in a single crystal growth atmosphere, and the crystal is grown to form a product-shaped crystal having a free crystal growth surface This is a method for producing a crystal product.
  • the present invention provides a liquid-repellent inorganic material S4 liquid, preferably a liquid-repellent inorganic material melt obtained by removing a wettability promoting substance from an inorganic material melt, Defined in the product shape, preferably in a product shape using a crystal growth type of a material suitable for realizing the liquid repellent state of the inorganic material, under an atmosphere in which the liquid repellent state of the inorganic material melt is maintained, Preferably, the product is solidified and crystallized as it is in an atmosphere in which the inorganic material melt is kept liquid-repellent without contamination and in a polycrystalline growth atmosphere, and the crystal is free from crystal growth.
  • a liquid-repellent inorganic material S4 liquid preferably a liquid-repellent inorganic material melt obtained by removing a wettability promoting substance from an inorganic material melt, Defined in the product shape, preferably in a product shape using a crystal growth type of a material suitable for realizing the liquid repellent state of the
  • the inorganic material melt be completely wettable with contact surfaces such as a support substrate and a container surface that come into contact with the inorganic material melt, that is, a liquid repellent state.
  • the melt of the inorganic material completely loses wettability with the supporting substrate and the surface of the container in contact with it, that is, there is no physical or chemical bond with each other.
  • the basic principle of the present invention is that the material melt and the contact surface such as the support substrate and the container surface Is to realize a completely non-wetting state, that is, a liquid-repellent state. Therefore, the "wetting property" will be described first.
  • Wettability '' originally targets water, oil, etc. at around room temperature, and the form of contact with the supporting substrate depends on the value of the contact angle as shown in Fig. 5. Is described in Where A: completely wet when contact angle ⁇ is 0 °; partially wet when contact angle 0 is between 0 ° and 90 °, and C: when contact angle 0 is close to 180 ° Is not wet at all, that is, it is described as being "water repellent.”
  • wettability is determined by parameters such as temperature and vapor pressure, the surface structure and surface tension of a liquid, the structure and chemical components of a liquid-solid interface, and the physical structure and chemical components of a solid surface. This may be due to the complex correlation that requires a rigorous discussion of the relationship.
  • the single crystal material is in a molten state (liquid state) at a temperature higher than room temperature and the contact angle ⁇ between the single crystal material and the supporting substrate is close to 180 °, the melt and the solid do not wet. In other words, it is said to be in a "lyophobic state".
  • liquid-repellent state is used to refer to the phenomenon that the temperature of the melt is not limited to room temperature, but is generally higher than the melting point of the material, and is distinguished from the “water-repellent state”. It was done.
  • liquids tend to have as small a surface area as possible due to surface energy, and parts of the surface are attracted to each other along the plane. As a sum of these forces, the liquid tends to be essentially spherical. However, there is a force that antagonizes this surface tension, that is, affinity, and it is presumed that the presence or absence and magnitude of wettability are determined by the magnitude relationship between these two forces.
  • the background that led to the present invention is that while dealing with melts of many kinds of inorganic materials for many years, the cause of this affinity is the liquid existing at the solid-liquid interface or the solid wetting promoting substance. It came to the conclusion that it was in existence. Presence and degree of wettability are determined by the presence and amount of the wetting promoting substance. Conversely, by preparing an environment in which no wetting promoting substance is generated, a state of no wetting and a “lyophobic state” can be achieved. Will be realized. In order to produce the crystal product of the present invention, it is essential to prevent the generation of the above-mentioned wetting promoting substance, realize a “liquid-repellent state”, and maintain that state for a long time.
  • semiconductors Ge, GaAs, GaSb, HgCdTe, InAs, InSb, PbTe, BiTe, SbTe, C d T e, Z n
  • the oxides on the surface and inside of these materials are partly taken into the melt or floated on the surface of the melt when the material is made into a melt, and the rest chemically reacts with the material of the container, and the above-mentioned wetting promoting substances are formed. Will be generated.
  • the last wetting-promoting substance wets the melt and the container, and proceeds with crystallization in this state, which enters the space between the crystal and the container and acts as an adhesive, and the crystal and the container are fixed and the crystal is fixed.
  • the product cannot be manufactured.
  • the following describes a method for obtaining a purified inorganic raw material by removing effectively the wetting promoting substance mainly from oxides from metals and semiconductor materials.
  • a commercially available inorganic material melt 2 containing oxides is heated and stored in a heater 7 in a graphite container 1 shown in FIG. 7, and all these members are placed in a high-purity argon atmosphere. is there.
  • This inorganic material melt 2 is wet with the container 1, and the contact angle is 90 degrees or less as shown in FIG.
  • a number of small holes 3 are opened in the lower part of the container 1, and are tightly fixed on the receiver 5.
  • the pressure in the upper space A of the inorganic material melt 2 is gradually increased to apply a pressure difference between the lower space B and the receiver 5.
  • the inorganic material melt 2 enters the gap 4 from the small hole 3 by the force of the differential pressure and drops into the space B of the lower receiver 5 while touching the oxide adsorbent 8.
  • the oxides in the inorganic material melt 2 are combined with the oxide adsorbent 8 while passing through the gap 4 or chemically reacted to form a composite oxide, and are removed from the inorganic material melt 2.
  • a liquid-repellent melt 6 is obtained in the lower space B of the receiver 5.
  • the liquid-repellent melt 6 solidifies in its initial rounded shape, and is cooled to room temperature to obtain a purified inorganic material.
  • the inorganic material melt 2 is brought into contact with the oxide adsorbent 8, thereby adsorbing harmful oxides or forming a complex compound of the harmful oxides and the oxide adsorbent.
  • This is the most important point in the present invention in the purification step of obtaining the inorganic material.
  • the container material There are combinations depending on the inorganic raw materials. Therefore, what should be considered is that when the inorganic raw material is melted, it does not form a solid solution with the container material, does not chemically react with each other, and the container is made of a substance having a higher melting point than the material melt.
  • Quartz glass Ga, Se, Cd, In, Sb, Te, Hg, Tl, Pb, Bi,
  • Alumina Ga, Se, Cd, In, Sb, Te, Hg, Tl, Pb, Bi Graphite: Ga, Se, Cd, In, Sb, Te, Hg, Tl, Pb, Bi, Insb, PbTe, BiTe, SbTe
  • the container material must be subjected to vacuum heating immediately before use at a temperature higher than the melting point of the applied material, so that water and oxygen are not released during the lyophobic process.
  • the atmosphere surrounding the melt / container material will be described. Many inorganic materials become chemically reactive when they become molten, and are oxidized quickly when there is oxygen or water around them, leading to a deterioration in their quality. In particular, if oxidation of the melt occurs during the liquid repellency process, the liquid repellency of the melt will no longer be maintained. Production of crystal products becomes impossible.
  • the atmosphere gas during the lyophobic process is ultra-high-purity, reducing the amount of impurities that cause a chemical reaction with the melt, such as moisture, oxygen, carbon monoxide, etc., to the ppb (parts per billion) level.
  • Argon or helm is suitable.
  • ultra-high-purity nitrogen or hydrogen may be used depending on the material.
  • fluoride a high vacuum atmosphere of 10-6 Torr level is required. In this way, if sufficient attention is paid to the three factors of raw material, container material, and crystallization in the container in the atmosphere, the melt will show a “lyophobic state” and its appearance will be rounded and will not wet the supporting substrate at all. . At this time, the wetting promoting substance is on the melt surface
  • the raw material, the container material, and the crystallization of the atmosphere are firstly removed from the inorganic raw material by removing the oxide-based wetting promoting substance from the inorganic raw material, and then purifying the inorganic raw material. It is most important to get Next, selection of container materials and pretreatment, use of ultra-high-purity atmospheric gas and supply method Is important. This series of operations is the “liquid repellent process technology”. By finding the conditions for achieving liquid repellency for each specific material, the inorganic material melt can be completely wettable with the supporting substrate (container surface). That is, the liquid repellent state is set.
  • the melt When the melt is in the “lyophobic state”, it becomes rounded due to its self-shape holding force due to its surface tension, and the one with a size of 1-2 mm becomes a perfect sphere. Therefore, by applying force to the melt in the “lyophobic state”, the shape is defined as a disk or square plate, and the temperature is reduced as it is to solidify and crystallize, allowing free crystal growth without going through the cutting process It is possible to obtain a crystal product in the shape of a final product having a surface.
  • the crystal and the support substrate do not adhere at all, and the crystal product can be easily taken out, and the support substrate can be used repeatedly.
  • a liquid-repellent process technology is applied to various inorganic materials, conditions are set, and the product shape of the melt in a liquid-repellent state is adjusted to have a free-growing crystal surface, that is, a crystal is formed without relying on cutting. The product is obtained.
  • the crystal product and its manufacturing method using the “liquid-repellent process technology” of the present invention described above are characterized as environmentally compliant technologies that solve many problems in conventional processes, and will become increasingly important in the future. It seems to be.
  • the advantages and features of the present invention include the following. 1. Material loss can be drastically reduced because there is no crystal cutting.
  • gallium antimony for thermophotovoltaic power generation does not require surface addition and becomes a substrate product as it is.
  • This crystal product has no distortion or rupture layer due to the cutting process on the surface.
  • the adhesion of the plating is good and the quality of the device can be improved.
  • FIG. 1 is a drawing for explaining the production of a plano-convex lens crystal product of Example 1.
  • FIG. 2 is a view for explaining extraction of a plano-convex lenticular single crystal of Example 1.
  • FIG. 3 is a drawing for explaining the production of the plate-shaped crystal product of Example 2.
  • FIG. 4 is a drawing for explaining removal of the plate-shaped crystal product of Example 2.
  • FIG. 5 is a drawing for explaining a liquid-repellent state.
  • FIG. 6 is a view for explaining realization of a liquid-repellent state.
  • FIG. 7 is a drawing explaining a liquid repellent process technology using a liquid repellent inorganic material melt obtained by removing a wettability promoting substance from the inorganic material melt.
  • Example 1 In Example 1, a plano-convex lens crystal product of fluoride (MgF 2 , CaF 2 , BaF 2 , SrF 2 ) is taken up, and an example of a manufacturing method thereof will be described with reference to FIG. .
  • MgF 2 , CaF 2 , BaF 2 , SrF 2 plano-convex lens crystal product of fluoride
  • Tsu fluoride melt 2 which is Tokasa by the heater 7 in the container 1 in FIG (manufactured by graph I g) (e.g., the melting point of C a F 2; 1 3 9 6 ° C) is held All the components (made of Graphite) necessary for the production of these crystal products are in a high vacuum atmosphere in a vacuum chamber 18.
  • the upper part of the fluoride melt 2 is sealed with a plug 12, which is connected to a discharge rate control shaft 13.
  • a lot of small holes 3 are opened at the bottom of the container 1 and graphite fiber 4 is filled under it, and a melt introduction frame 9 with a hole at the center is fixed at the bottom. .
  • the crystal product container 5 is shown in detail in the cross-sectional view a on the right side of the figure and in the top view b below it.
  • the melt receiver 10 has the curvature R of the convex part of the plano-convex lens and has a center in the lower part.
  • the c- crystal product container 5 in which the small hole of the seed crystal generating part 11 is opened is incorporated into the melt introduction frame 9 from below.
  • the fluoride melt 2 falls downward while rotating the discharge amount control shaft 13 and moving the plug 12 downward, applying force to the plug 12 and passing through the small hole 3 and touching the graphite fiber 4. To go.
  • the fluoride melt 2 is purified by reacting or adsorbing the wetting promoting substances such as oxides therein with the graphite fiber 4, and the melt which has become a liquid repellent state is melted.
  • Liquid introduction frame 9 Drops downward from the center hole.
  • the amount of the purified melt stored in the crystal product container 5 is set in advance by the movement distance of the plug 12 with the rotation of the discharge amount control shaft 13, and a predetermined amount of the purified melt is performed by one discharge operation. It becomes 6.
  • the crystal product container 5 containing a predetermined amount of melt is moved to the pull-down shaft 16 and heated by the crystallization heater 14 to keep the melt repellent state.
  • the product container 5 is incorporated in the melt introduction frame 9.
  • the first crystal product container 5 is moved downward at a constant speed of about 1 mm per minute by the pull-down shaft 16 to promote crystallization.
  • the time for the crystal product container 5 is adjusted to move exactly by the height h and the time for the second melt to accumulate in the crystal product container, move it over the first crystal product container 5 Then, the crystallization can be continuously advanced by the lowering shaft 16.
  • the detailed melt 111-a at the lower end of the crystal product container 5 begins to solidify and crystallize as it moves downward, forming a seed crystal 111-b.
  • FIG. 2 shows a state in which the plano-convex lenticular single crystal 17 at room temperature is taken out of the crystal product container 5.
  • the plano-convex lens-shaped single crystal product 18 with the seed crystal 19 is easily removed from the crystal product container 5 because it has no wettability with the crystal product container 5, and its entire surface is a free-growing crystal plane. .
  • plano-convex lens-shaped single-crystal product 18 Since the plano-convex lens-shaped single-crystal product 18 has the required plano-convex lens shape as a whole, the seed crystal 19 is removed and the polishing process can be started immediately.
  • the right end of FIG. 2 shows a plano-convex lens single crystal final product 20 whose surface has been polished. From this, it is clear that the plano-convex lens crystal product in this example is a resource-saving, energy-saving, and labor-saving product that can produce a flat lens single crystal final product 20 without cutting.
  • Example 2 Example 2
  • G a S b has been developed for thermo-photovoltaic (TPV) It is attracting attention as a conductor material.
  • TPV thermo-photovoltaic
  • inexpensive plate-like G a S b is required, and the prospect of manufacturing using the current method of cutting ingots has not been possible. Therefore, a plate-shaped GaSb crystal product having a free-growing crystal plane, which can be expected to solve this problem, and a manufacturing method thereof will be described with reference to FIG.
  • a GaSb 'melt 2 melting point: 712 ° C
  • All components required for manufacture are in a high purity argon atmosphere in chamber-18.
  • the upper part of the G aS b melt 2 is sealed with a plug 12, which is connected to a discharge rate control shaft 13.
  • a number of small holes 3 are opened in the lower part of the container 1, and a quartz glass fiber 4 is filled under the small holes 3, and a melt introduction frame 9 having a hole in the center is fixed to the lower part.
  • the crystal product container 5 is shown on the right side of the figure in a cross-sectional view in which four sheets are stacked on the container table 23, and the melt receiving portion 10 has a thickness corresponding to the thickness of the required plate-shaped GaSb crystal. It is a blur.
  • the crystal product container 5 is continuously put on the moving rail 21 from right to left, and is moved by the lateral dimension L of the crystal product container 5 in one operation.
  • the top of the first crystal product container 5 is placed at a, and the vertical movement axis 22 is moved downward to create a space for receiving the crystal product container 5 on the melt introduction frame 9 and the lower movement rail 21. Therefore, the crystal product container 5 whose head is at a from the right is moved by L. At this position, the crystal product container 5 is moved upward by the distance H between the upper end b of the crystal product container 5 and the lower end c of the melt introduction frame 9 by the vertical movement axis 22. Assigned to introductory slot 9. The G a S b melt 2 falls downward while rotating the discharge amount control shaft 13 and moving the plug 12 downward, passing through the small hole 3 and touching the quartz glass fiber 4. Go.
  • the GaSb melt 2 is purified by reacting or adsorbing the wetting promoting substances such as oxides therein with the quartz glass fiber 4, and the melt which has become a liquid repellent state is melted.
  • Liquid introduction frame 9 Drops down from the center hole.
  • the amount of the purified melt 6 stored in the crystal product container 5 is set in advance by the moving distance of the plug 12 with the rotation of the discharge amount control shaft 13, and a predetermined amount of the purified melt is discharged by one discharge operation. It becomes liquid 6.
  • the crystal product container 5 in which a predetermined amount of melt is stored is moved downward by a distance H by a vertical moving shaft 22 and is placed on a moving rail 21.
  • the refined melt 6 in the crystal product container 5 on the moving rail 21 is heated by the lower heater 71 to keep the melt repellent.
  • the same operation is repeated, but when the crystal product container 5 holding the first purified melt 6 comes to the position d, the weight 2 4 (quartz glass or graph Put one of them on the crystal product container 5.
  • the purified melt 6 spreads over the entire depression of the melt receiving portion 10 of the crystal product container 5, and a plate-like liquid-repellent melt 61 is formed.
  • the temperature starts dropping from the left end of the crystal product container 5, and the growth of the plate-like polycrystal 62 from the plate-like liquid-repellent melt 61 starts.
  • Fig. 4 shows a cold plate polycrystal 63 sandwiched between a crystal product container 5 and a weight 24. This shows how it is taken out.
  • the room-temperature plate-like polycrystal 6 3 has no wettability with the crystal product container 5 or the weight 24, so it can be easily removed therefrom. It has become.
  • the thickness of the G a S b plate-shaped polycrystal 6 3 is determined by the depth of the depression in the melt receiving portion 10, but the external shape should be pre-processed to the crystal product container 5 as required. become.
  • FIG. 4 10-a shows an example in which a rectangular plate-like polycrystal 27 can be obtained by making the melt receiving portion 10 into a square shape.
  • An example is shown in which a disk-shaped polycrystal 28 can be obtained by making it circular.
  • the G a S b plate-shaped polycrystalline crystal products 27 and 28 in this embodiment are processed only by etching these surfaces (operation of dissolving a very small portion of the surface with a strong acid), and the final polycrystalline products 29, 3 It is clear that 0 is a resource-, energy- and labor-saving product that can be manufactured.

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  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
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  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

La présente invention concerne un article en cristal de la forme d'un produit, caractérisé en ce qu'il présente une surface libre faite en matériau cristallin épitaxial de matière inorganique, la surface libre du matériau cristallin épitaxial est une surface d'un monocristal épitaxial ou d'une matière polycristalline épitaxiale. L'invention concerne également un procédé de production d'un produit cristallin impliquant l'obtention d'une fonte d'un matériau inorganique dans la forme d'un produit mais également répulsif par rapport à la paroi d'un récipient, puis la solidification ou la cristallisation de la fonde tout en maintenant l'état de répulsivité précédent, de façon à produire un article cristallin en forme d'un produit et disposant d'une surface libre en matériau cristallin épitaxial. Ce procédé permet la production d'un article cristallin et d'un produit cristallin étant capable de bonnes performances pour un coût réduit résultant d'une production à grande échelle.
PCT/JP2001/004633 2000-07-17 2001-06-01 Produit cristallin a surface libre en cristal epitaxial et procede de production WO2002006569A1 (fr)

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JP2000216319A JP4680354B2 (ja) 2000-07-17 2000-07-17 結晶成長自由表面を有する結晶製品の製造方法
JP2000/216319 2000-07-17

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JP2006001788A (ja) * 2004-06-17 2006-01-05 Hitachi Chem Co Ltd フッ化カルシウム結晶育成ルツボ、フッ化カルシウム結晶の製造方法及びフッ化カルシウム結晶
JP2006001787A (ja) * 2004-06-17 2006-01-05 Hitachi Chem Co Ltd フッ化カルシウム結晶育成ルツボ、フッ化カルシウム結晶の製造方法及びフッ化カルシウム結晶
JP2006001786A (ja) * 2004-06-17 2006-01-05 Hitachi Chem Co Ltd フッ化カルシウム結晶育成ルツボ、フッ化カルシウム結晶の製造方法及びフッ化カルシウム結晶
JP2008239438A (ja) * 2007-03-28 2008-10-09 National Institute Of Advanced Industrial & Technology 球状結晶の製造方法及び製造装置
JP5079151B1 (ja) * 2012-02-08 2012-11-21 ユニオンマテリアル株式会社 シリコン融液の絶対溌液化方法及びにその方法を使用した高品質シリコン結晶体用精密鋳造装置

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