WO2015001593A1 - シリカガラスルツボ - Google Patents
シリカガラスルツボ Download PDFInfo
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- WO2015001593A1 WO2015001593A1 PCT/JP2013/067948 JP2013067948W WO2015001593A1 WO 2015001593 A1 WO2015001593 A1 WO 2015001593A1 JP 2013067948 W JP2013067948 W JP 2013067948W WO 2015001593 A1 WO2015001593 A1 WO 2015001593A1
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- Prior art keywords
- crucible
- silica glass
- glass crucible
- silicon
- single crystal
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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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/09—Other methods of shaping glass by fusing powdered glass in a shaping mould
- C03B19/095—Other methods of shaping glass by fusing powdered glass in a shaping mould by centrifuging, e.g. arc discharge in rotating mould
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/10—Crucibles or containers for supporting the melt
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- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Definitions
- the present invention relates to a silica glass crucible having an uneven structure on the inner surface of the crucible.
- the single crystal can be pulled by pulling the seed crystal that has been deposited in the silicon melt.
- an outer carbon heater is heated to a temperature of about 1450 to 1600 ° C.
- a silicon melt obtained by melting a silicon polycrystal raw material is stored inside a silica glass crucible, and a silicon single crystal seed crystal is melted at a melting temperature of about
- the silicon single crystal is brought into contact with the surface of the silicon melt at 1420 ° C., gradually pulled while rotating, and grown using the seed crystal of the silicon single crystal as a nucleus, and the silicon single crystal is gradually manufactured while controlling the pulling rate and the melt temperature.
- the temperature of the silica glass crucible is as high as 1450 to 1600 ° C. in order to keep the solid-liquid interface at the center of the silicon melt surface where the silicon melt is in contact with the single crystal at around 1420 ° C. which is the melting point of silicon. .
- the amount of deformation of the rim of the silica glass crucible may be 5 cm or more.
- a silicon single crystal In pulling up a silicon single crystal, first, the crystal is expanded to the center of the seed crystal until a desired diameter is reached (formation of a shoulder). Next, the cylindrical ingot-shaped single crystal is pulled up by pulling up the trunk. Finally, the single crystal is pulled up by narrowing the bottom.
- a silica glass crucible having a diameter of 610 to 1015 mm silicon ingot diameter: 200 mm, 300 mm, 450 mm
- a large single crystal silicon ingot having a length of 2 m or more is manufactured.
- a single crystal silicon wafer manufactured from such a large ingot is preferably used for manufacturing a flash memory and a DRAM.
- the cause of the hot water surface vibration is considered as follows.
- a reaction of SiO 2 (solid) ⁇ Si (liquid) + 2O occurs at the interface between the silicon melt and silica glass, and the silica glass is dissolved.
- a reaction of Si (liquid) + O ⁇ SiO (gas) occurs due to an increase in pulling temperature or a decrease in atmospheric pressure, and the surface of the melt vibrates when this SiO gas floats from the melt.
- the large silica glass crucible has a longer distance from the outer carbon heater to the center of the silicon melt (previously it was about 300 mm but over 500 mm), and the temperature of the carbon heater during the pulling can be avoided. Absent.
- the vibration of the molten metal surface of the silicon melt becomes intense with the temperature rise at the time of pulling up, and it is necessary to suppress it. Therefore, in order to improve the single crystallization rate of the silicon single crystal, it is necessary to suppress the surface vibration generated in the silicon melt.
- Patent Document 1 a glass surface made of silica sand of the first component is formed on the inner surface of a quartz crucible having an opaque layer and a transparent layer, and then A crucible is described in which glass is scattered and fused with silica sand of the second component, and glass formed of synthetic quartz sand is formed on the inner surfaces of the corner and bottom.
- a technique for adjusting the bubble content of the inner peripheral surface layer of the crucible in the vicinity of the hot water surface at the start of pulling up to a certain range is disclosed. This is because it has been found that the micro unevenness suppresses the molten-metal surface vibration of the silicon melt based on the same principle that the boiling stone prevents bumping.
- Patent Document 2 discloses a technique in which a minute recess is provided in the inner surface layer of the crucible in order to suppress the melt surface vibration of the silicon melt filled in the silica glass crucible. This is because it has been found that the minute concave portion suppresses the vibration of the melt surface of the silicon melt based on the same principle as the boiling stone prevents bumping.
- JP 2006-169084 A International Publication 2011/0774568 JP 2004-250304 A
- Patent Document 1 it is difficult to produce a crucible in which silica sand as the second component is evenly scattered, and there is a problem in quality, such as the vibration of the molten metal surface cannot be suppressed by the produced silica glass crucible. There is. There is also a problem that the manufacturing process is complicated and expensive. Furthermore, Patent Document 1 describes that a 24 inch crucible was effective, but there is a problem that the effect of suppressing melt surface vibration cannot be obtained when pulling up a silicon single crystal having a larger diameter.
- At least one minute concave portion is provided for each annular inner surface portion that is partitioned at regular intervals in the height direction of the silica glass crucible, and the silicon melt and the silica glass crucible are provided.
- the effect of the minute recesses cannot be exhibited in all the contact areas on the inner surface, and it is difficult to completely suppress the molten metal vibration of the silicon melt.
- the present inventors are a silica glass crucible that is easy to manufacture and that can suppress the surface vibration from seeding, which is the initial stage of pulling up a silicon single crystal, to during the growth of the silicon single crystal.
- the purpose is to provide.
- the present inventors have made extensive studies and suppressed the melt surface vibration of the silicon melt by analyzing in detail the relationship between the structure of the crucible inner surface and the melt surface vibration.
- a silica glass crucible that can be used.
- the present inventors have analyzed the relationship between the fine structure of the inner surface of the crucible and the molten metal surface vibration.
- a silica glass crucible in which a wavefront having a fine concavo-convex structure is formed on the inner surface in the direction from the edge of the straight body portion to the corner portion, has been found to suppress the melt surface vibration of the silicon melt when pulling up the silicon single crystal, Based on this, the present invention has been completed.
- such a silica glass crucible can stably suppress molten metal surface vibration. is there. Further, unlike the silica glass crucible described in Patent Document 3, even if the fine uneven structure on the inner surface of the crucible is provided in a portion other than the vicinity of the silicon liquid surface at the start of pulling up the silicon single crystal, The seed crystal can be stably deposited and, of course, the transition during the growth of the silicon single crystal hardly occurs.
- the present invention has a substantially cylindrical straight body portion that is open at the top and extends in the vertical direction, a curved bottom portion, and a corner portion that connects the straight body portion and the bottom portion and has a larger curvature than the bottom portion.
- a silica glass crucible wherein the inner surface of the crucible has a concave-convex structure in which a groove-shaped valley is sandwiched between ridges and ridges, and an average interval between the ridges and ridges is 5 to 100 ⁇ m. It is. Further, the present invention has a substantially cylindrical straight body portion that is open at the top and extends in the vertical direction, a curved bottom portion, and a corner portion that connects the straight body portion and the bottom portion and has a larger curvature than the bottom portion.
- the crucible has an uneven structure in which an inner surface of the crucible is sandwiched between a ridge and a ridge, and the center line average roughness Ra of the uneven structure is 0.02 to 0.5 ⁇ m.
- This is a silica glass crucible.
- the silica glass crucible 12 includes, for example, a substantially cylindrical straight body portion 15 that is open at the upper end and extends in the vertical direction, as shown in the cross-sectional view of FIG. 15 and the bottom portion 16 are connected, and a corner portion 17 having a larger curvature than the bottom portion 16 is provided.
- Silica glass preferably includes a transparent layer 20 on the inner side and a bubble layer 14 on the outer side.
- the transparent layer 20 is a layer formed inside the silica glass crucible and substantially does not contain bubbles. “Substantially free of bubbles” means that the bubble content and bubble diameter are such that the single crystallization rate does not decrease due to bubbles.
- the bubble content is the volume of bubbles in the unit volume of the crucible.
- the bubble layer 14 has, for example, a bubble content of 0.2% to 1% and an average bubble diameter of 20 ⁇ m to 200 ⁇ m.
- the inner surface of the silica crucible has a grooved uneven structure in which a grooved valley is sandwiched between ridges.
- the inner surface of the crucible is provided with a fine uneven structure, not only the silicon melt is prevented from bumping and the molten metal surface vibration is suppressed, but also the contact area between the silicon melt and the inner surface of the crucible increases. The frictional resistance between the two increases, and the molten metal surface vibration is suppressed.
- a fine groove-like concavo-convex structure is provided on the inner surface of the crucible, even if SiO gas is generated, minute turbulence is caused in the concavo-convex portion, energy is attenuated, and hot water surface vibration is less likely to occur. Become.
- the silica glass on the inner surface of the crucible is dissolved by the reaction between the inner surface of the crucible and the silicon melt.
- oxygen is supplied into the silicon melt, and this oxygen is mixed into the silicon single crystal and used to form a gettering site.
- the reaction between the inner surface of the crucible and the silicon melt is likely to occur, and oxygen is efficiently supplied into the silicon melt. Can prevent problems caused by lack of oxygen.
- the concave-convex structure is preferably provided on the entire inner surface of the straight body of the crucible from the viewpoint of preventing molten metal surface vibration.
- the crucible is preferably provided at a position lower than the entire crucible, particularly the initial liquid level at the time of pulling up the silicon single crystal.
- the groove-shaped valley substantially extends in the circumferential direction of the straight body portion of the crucible.
- the valley may be formed to be slightly inclined toward the upper end or the lower end of the straight body portion, or may be formed to meander.
- the valley extends in the circumferential direction, the contact resistance between the silicon melt and the inner surface of the crucible becomes particularly large, and the molten metal surface vibration is effectively suppressed.
- the average interval between the ridges is 5 to 100 ⁇ m, preferably 20 to 60 ⁇ m, and more preferably 15 to 50 ⁇ m.
- the interval between ridges is the distance from the vertex of the ridge to the vertex. More specifically, the average interval is, for example, 5, 10, 20, 30, 40, 50, 60, 70, 80, 90, 100 ⁇ m, and is within a range between any two of the numerical values exemplified here. It may be. When the average distance is small, the contact area between the silicon melt and the inner surface of the crucible is too large, and the frictional resistance between the two is too large, and the molten metal surface vibration may not be effectively suppressed.
- the distance between the ridge and the ridge is preferably approximately equal.
- the distance between the ridge and the ridge is 15 to 50 ⁇ m, preferably 20 to 30 ⁇ m.
- the concavo-convex structure is formed in a non-contact manner using an optical detection device including a light emitting unit that irradiates light on the inner surface of the silica glass crucible and a light receiving unit that receives reflection of light irradiated on the inner surface of the silica glass crucible. It is possible to measure.
- the irradiation light for example, visible light, ultraviolet light, infrared light, laser light, or the like can be used, and any light can be used as long as the uneven structure on the inner surface of the crucible can be detected.
- the light-emitting part may be built in the optical detection device, and in that case, it is preferable to use a light-emitting part that can be rotated along the inner surface of the silica glass crucible.
- the light receiving unit can be appropriately selected according to the type of irradiation light, and for example, an optical camera including a light receiving lens and an image unit can be used.
- an optical camera including a light receiving lens and an image unit can be used.
- it is preferable that only the light generated at the condensing point is received by the light receiving unit.
- it is preferable to provide a pinhole in front of the light receiving unit for example, the photodetector.
- the objective lens 10 is arranged in a non-contact manner on the inner surface 11 of the crucible 12.
- the concavo-convex structure can be measured by scanning in the scanning direction 13.
- Examples of other scanning methods include a sample scanning method and a laser scanning method.
- the sample scanning method is a method of acquiring a two-dimensional image by driving a stage on which a sample is placed in the XY directions.
- the laser scanning method is a method in which a sample is two-dimensionally scanned by applying a laser in the XY directions. Any scanning method may be adopted.
- the scanning direction include the vertical direction 18 and the horizontal direction 19 of the straight body portion 15. Further, only a part of the inner surface of the crucible may be scanned. For example, the periphery of the molten metal surface where the seed crystal is deposited may be intensively scanned.
- the condensing point is scanned to obtain a two-dimensional image of the inner surface of the crucible. Further, by scanning in the thickness direction of the crucible, a three-dimensional fine concavo-convex structure image can be acquired (see FIG. 5). From the acquired image, the direction of the groove-shaped valley can be confirmed. It is also possible to scan the condensing point two-dimensionally, measure the ridge and the ridge from the brightness of the reflection, and quantify the pitch (average interval). Furthermore, the Z position information at the time of focusing is recorded on the sample while scanning the condensing point in the XY directions, and the height information of the sample can be captured by digitizing the sample (FIG. 6). reference). These methods are preferable in that the scanning time can be shortened.
- the average interval between the ridge and the ridge is a value obtained by dividing the sum of the intervals between the ridge and the ridge by the number of intervals between the ridge and the ridge.
- the average interval can be obtained by processing the image of the fine concavo-convex structure obtained by the measurement method as described above, for example, with software.
- the inner surface of the silica crucible has a grooved uneven structure, and the center line average roughness Ra is preferably 0.02 to 0.5 ⁇ m, more preferably 0.05 to 0.4 ⁇ m, and 0 More preferably, it is 2 to 0.4 ⁇ m.
- the center line average roughness Ra is, for example, 0.02, 0.05, 0.1, 0.15, 0.2, 0.25, 0.3, 0.35, 0.4. 0.45, 0.5 ⁇ m, and may be in a range between any two of the numerical values exemplified here.
- the center line average roughness Ra can be calculated from a value obtained by folding the measured roughness curve from the center line and dividing the area obtained by the roughness curve and the center line by the length L.
- the roughness curve and the like can be calculated by measuring in the same manner as the groove-shaped uneven structure and by software processing.
- the silica crucible according to the present invention has a groove-like uneven structure, and as described above, even if the center line average roughness Ra has a fine uneven structure within a predetermined range, the molten metal surface vibration is effectively suppressed. be able to.
- Silica powder used for the production of silica glass crucible includes crystalline natural silica powder and amorphous synthetic silica powder produced by chemical synthesis.
- Natural silica powder is a silica powder produced by pulverizing a natural mineral mainly composed of ⁇ -quartz.
- Synthetic silica powder can be produced by chemical synthesis techniques such as gas phase oxidation of silicon tetrachloride (SiCl4) (dry synthesis method) and hydrolysis of silicon alkoxide (Si (OR4)) (sol-gel method). it can.
- natural silica powder is supplied to the silica glass crucible mold.
- Natural silica powder can be produced by pulverizing a natural mineral mainly composed of ⁇ -quartz.
- the synthetic silica powder is supplied onto the natural silica powder, and the silica powder is melted by Joule heat of arc discharge, and then cooled to cool the inner silica layer (synthetic layer) and natural silica.
- a silica glass crucible composed of an outer surface layer (natural layer) that is vitrified from powder is produced.
- the silica powder layer is strongly depressurized to remove bubbles to form a transparent silica glass layer (transparent layer), and then the bubble is contained in the bubble-containing silica glass layer by decreasing the depressurization. (Bubble layer) is formed.
- the inner surface layer and the transparent layer formed from the synthetic silica powder do not necessarily coincide with each other.
- the outer surface layer and bubble layer formed from natural silica powder do not necessarily coincide.
- the silica powder is preferably melted so that the maximum temperature reached on the inner surface of the rotary mold is 2000 to 2600 ° C. If the maximum temperature reached is lower than 2000 ° C., the gas remaining as bubbles in the structure of the silica glass or in the silica glass cannot be exhausted, and the crucible may swell violently during pulling in the silicon single crystal. On the other hand, if the maximum temperature reached is higher than 2600 ° C., the viscosity of the silica glass may be lowered and shape collapse may occur.
- Arc melting is performed, for example, by arc discharge of alternating current three phases (R phase, S phase, T phase). Therefore, in the case of AC three-phase, the silica powder layer is melted by generating arc discharge using three carbon electrodes. Arc melting starts arc discharge at the point where the tip of the carbon electrode is located above the mold opening. Thereby, the silica powder layer in the mold opening vicinity is preferentially melted. Thereafter, the carbon electrode is lowered to melt the silica powder layer of the mold body part, the corner part and the bottom part.
- a grooved concavo-convex structure in which a grooved valley is sandwiched between ridges on the inner surface of the crucible can be formed by lowering the carbon electrode stepwise.
- the descending speed of the carbon electrode can be 10 to 35 mm / min, specifically, for example, 10, 13, 15, 17, 18, 20, 23, 25, 28, 30 or 35 mm / min per minute. Any two of the numerical values shown here may be used.
- the descending speed may be an average value.
- Lowering stepwise means lowering while repeating lowering and stopping. For example, pulse driving that repeats lowering and stopping of the arc electrode may be used.
- the pulse width is, for example, 5, 10, 20, 30, 40, 50, 60, 70, 80, 90, 100 ms, and may be in the range of any two numerical values shown here.
- the pulse width may be between 50 and 250 ms.
- the duty cycle can be, for example, 30 to 70%, specifically 30, 40, 45, 50, 55, 60, 70%, and any two of the two shown here It may be a numerical range.
- the duty cycle is preferably between 45 and 55%, more preferably 50% for the purpose of keeping the distance between the ridges constant.
- a fine concavo-convex structure having a center line average roughness Ra of 0.02 to 0.5 ⁇ m can be formed by lowering the carbon electrode while vibrating.
- the silica glass crucible according to the present invention can be used, for example, as follows.
- a silicon single crystal is obtained by melting polysilicon in a silica glass crucible to produce a silicon melt, and pulling up the seed crystal while rotating the seed crystal while the end of the silicon seed crystal is immersed in the silicon melt.
- the shape of the silicon single crystal is a cylindrical silicon seed crystal from the top, a conical silicon single crystal below it, a cylindrical silicon single crystal having the same diameter as the bottom surface of the upper cone, and a conical silicon with the apex facing downward Single crystal.
- the pulling of the silicon single crystal is usually performed at about 1420 ° C.
- the hot water surface vibration is particularly likely to occur. Since the silica glass crucible according to the present invention has a specific concavo-convex structure formed on the inner surface, it is possible to suppress the occurrence of molten metal surface vibration.
- Example 1 A silica glass crucible according to Example 1 was manufactured based on the rotational mold method.
- the diameter of the carbon mold was 32 inches (813 mm), the average thickness of the silica powder layer deposited on the inner surface of the mold was 15 mm, and arc discharge was performed with three three-phase alternating current three electrodes.
- the energization time in the arc melting step was 90 minutes, the output was 2500 kVA, and the silica powder layer was depressurized from atmospheric pressure to 90 kPa for 10 minutes from the start of energization.
- the carbon electrode was lowered stepwise.
- the average descent speed was 20 mm / min, the pulse width was 100 ms, and the duty cycle was 50%.
- Comparative Example 1 A silica glass crucible according to Comparative Example 1 was produced in the same manner as in Example 1 except that the carbon electrode was continuously lowered (falling speed: 20 mm / min) during arc melting.
- Comparative Example 2 A silica glass crucible according to Comparative Example 2 was produced in the same manner as in Example 1 except that the carbon electrode was lowered stepwise with an average descent rate of 35 mm / min, a pulse width of 100 ms, and a duty cycle of 50% during arc melting. .
- Comparative Example 3 A silica glass crucible according to Comparative Example 2 was produced in the same manner as in Example 1 except that the carbon electrode was lowered stepwise with an average descent rate of 10 mm / min, a pulse width of 100 ms, and a duty cycle of 50% during arc melting. .
- Table 1 shows part of the manufacturing conditions of Example 1 and Comparative Examples 1 to 3.
- FIG. 3 is a surface photograph taken with a confocal laser microscope on the inner surface of the silica glass crucible according to Comparative Example 1. As shown in FIG. 3, the uneven surface structure was not observed on the inner surface of the conventional silica glass crucible, and a non-uniform strain structure was observed.
- FIG. 4 is a surface photograph taken with a confocal laser microscope on the inner surface of the silica glass crucible according to the first embodiment. As shown in FIG. 4, a concavo-convex structure was formed on the inner surface of the silica glass crucible according to Example 1 in which a groove-like valley was sandwiched between the ridge and the ridge.
- FIG. 5 is an acquired three-dimensional image. As shown in FIG. 5, the concavo-convex structure was formed so as to be orthogonal to the points A and B. Point A is on the crucible opening side, and point B is on the crucible bottom side.
- FIG. 6 is a graph showing the height of the inner surface of the silica glass crucible from points A to B.
- Table 2 shows all the results of the average intervals obtained.
- Hot water surface vibration About 500 kg of polysilicon is added to each of the silica glass crucibles according to Example 1 and Comparative Examples 1 to 3, and heated to a temperature of about 1450 to 1600 ° C. using a carbon heater. While pulling up the crystals, the presence or absence of molten metal surface vibration was confirmed with an observation camera. In the silica glass crucibles according to Comparative Examples 1, 2, and 3, occurrence of hot water surface vibration was confirmed. On the other hand, in the silica glass crucible according to Example 1, suppression of hot water surface vibration was confirmed.
- the silica glass crucible according to the present invention is different from the silica glass crucible manufactured by a complicated and poorly reproducible method as in the prior art (for example, Patent Document 1), and the molten metal surface stably. It is possible to suppress vibration. Moreover, it is possible to stably suppress the molten metal surface vibration during the seeding which is the initial stage of the pulling process of the silicon single crystal and also during the growth of the silicon single crystal.
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Abstract
Description
本発明に係るシリカガラスルツボ12は、例えば、図2の断面図に示されるような、上端が開口し鉛直方向に延びる略円筒形の直胴部15、湾曲した底部16、および前記直胴部15と前記底部16とを連結し且つ前記底部16よりも曲率が大きいコーナー部17を備える。
次に、本発明に係るシリカガラスルツボの製造方法の一実施形態について説明する。
本発明に係るシリカガラスルツボは、例えば、次のように用いることができる。
回転モールド法に基づいて、実施例1に係るシリカガラスルツボを製造した。カーボンモールド口径は、32インチ(813mm)、モールド内表面に堆積したシリカ粉層の平均厚さは15mmで、3相交流電流3本電極によりアーク放電を行った。アーク熔融工程の通電時間は90分、出力2500kVA、通電開始から10分間はシリカ粉層を大気圧から90kPa減圧した。アーク熔融中は、炭素電極を段階的に降下させた。平均降下速度は、20mm/分、パルス幅は、100ms、デューティーサイクルを50%とした。
アーク熔融中に炭素電極を連続的に降下(降下速度:20mm/分)させた以外は、実施例1と同様にして比較例1に係るシリカガラスルツボを製造した。
アーク熔融中に炭素電極を、平均降下速度35mm/分、パルス幅100ms、デューティーサイクル50%として段階的に降下させた以外は実施例1と同様にして比較例2に係るシリカガラスルツボを製造した。
アーク熔融中に炭素電極を、平均降下速度10mm/分、パルス幅100ms、デューティーサイクル50%として段階的に降下させた以外は実施例1と同様にして比較例2に係るシリカガラスルツボを製造した。
実施例1および比較例1~3に係るシリカガラスルツボにおいて、直胴部における透明層の表面を、共焦点レーザー顕微鏡を用いて観察した。走査方向は、シリカガラスルツボの縁から鉛直方向に走査した。走査面は、3cm×3cmの使用前シリカガラスルツボである。結果を図3および4に示す。
実施例1に係るシリカガラスルツボの内表面を、集光点をXY方向に走査しながら、焦点が合った時のZ位置情報を記録し、数値化して、サンプルの高さを測定した。数値処理ソフトウェアを用いて中心線平均粗さRaを演算したところ、0.37μmであった。
実施例1、および比較例1~3に係るシリカガラスルツボに、それぞれ約500kgのポリシリコンを加えて、カーボンヒーターを用いて温度約1450~1600℃まで加熱し、シリコン単結晶引き上げを行いつつ、湯面振動の有無を観測カメラにより確認した。比較例1、2、および3に係るシリカガラスルツボにおいては、湯面振動の発生が確認された。一方、実施例1に係るシリカガラスルツボにおいては、湯面振動の抑制が確認された。
Claims (4)
- 上端が開口し鉛直方向に延びる略円筒形の直胴部、湾曲した底部、および前記直胴部と前記底部とを連結し且つ前記底部よりも曲率が大きいコーナー部を有するルツボであって、
前記ルツボの内表面は、溝状の谷が尾根と尾根の間に挟まれた凹凸構造を有し、前記尾根と尾根との平均間隔が、5~100μmであることを特徴とするシリカガラスルツボ。 - 前記谷は、実質的に、前記直胴部の円周方向に延びる請求項1に記載のシリカガラスルツボ。
- 前記ルツボの内表面の中心線平均粗さRaが0.02~0.5μmである請求項1または2記載のシリカガラスルツボ。
- 上端が開口し鉛直方向に延びる略円筒形の直胴部、湾曲した底部、および前記直胴部と前記底部とを連結し且つ前記底部よりも曲率が大きいコーナー部を有するルツボであって、
前記ルツボの内表面は、溝状の谷が尾根と尾根の間に挟まれた凹凸構造を有し、前記凹凸構造の中心線平均粗さRaが0.02~0.5μmであることを特徴とするシリカガラスルツボ。
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US14/901,036 US9932692B2 (en) | 2013-06-30 | 2013-06-30 | Vitreous silica crucible |
PCT/JP2013/067948 WO2015001593A1 (ja) | 2013-06-30 | 2013-06-30 | シリカガラスルツボ |
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