WO2014129123A1 - シリコン単結晶棒の製造方法 - Google Patents
シリコン単結晶棒の製造方法 Download PDFInfo
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- WO2014129123A1 WO2014129123A1 PCT/JP2014/000505 JP2014000505W WO2014129123A1 WO 2014129123 A1 WO2014129123 A1 WO 2014129123A1 JP 2014000505 W JP2014000505 W JP 2014000505W WO 2014129123 A1 WO2014129123 A1 WO 2014129123A1
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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
- C30B15/20—Controlling or regulating
- C30B15/203—Controlling or regulating the relationship of pull rate (v) to axial thermal gradient (G)
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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
- C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
- C30B15/04—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt adding doping materials, e.g. for n-p-junction
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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
- C30B15/14—Heating of the melt or the crystallised materials
-
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/322—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to modify their internal properties, e.g. to produce internal imperfections
- H01L21/3221—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to modify their internal properties, e.g. to produce internal imperfections of silicon bodies, e.g. for gettering
- H01L21/3225—Thermally inducing defects using oxygen present in the silicon body for intrinsic gettering
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
- H01L22/10—Measuring as part of the manufacturing process
- H01L22/12—Measuring as part of the manufacturing process for structural parameters, e.g. thickness, line width, refractive index, temperature, warp, bond strength, defects, optical inspection, electrical measurement of structural dimensions, metallurgic measurement of diffusions
Definitions
- the present invention relates to a method of pulling up and manufacturing a silicon single crystal rod by the Czochralski method (CZ method), and particularly to a method of pulling up and manufacturing an N region silicon single crystal rod by the CZ method.
- CZ method Czochralski method
- This COP-free region is a portion that does not include giant dislocation clusters (I region), COP (V region), defects detected by Cu deposition, and OSF regions.
- This guarantee method includes confirmation of a large dislocation cluster by etching called LEP in the crystal inspection process and EOSF (Enhanced-OSF) inspection (see Patent Document 1, Patent Document 2, etc.). Is possible.
- Manufacture of an N region silicon single crystal rod by the CZ method is realized when manufacturing at a certain growth rate under the condition that the temperature gradient in the vicinity of the growth interface is kept constant in the plane.
- the crystal temperature gradient in the vicinity of the growth interface is G and the crystal growth rate (pull-up rate) is F
- F / G is required to be within the N region regardless of where in the plane.
- Such a range is narrow, and when F or G exceeds a desired required range, it does not become an N region and is rejected as a product. Therefore, this product has a narrow manufacturing margin and constantly monitors in which defect region the V region, OSF region, N region (Nv region, Ni region), and I region are manufactured, and if necessary,
- the pulling conditions need to be tuned (adjusted). This is because the temperature distribution in the furnace changes with time based on changes in the furnace parts such as heaters and heat insulating materials used, and tuning of this pulling condition is indispensable for stable production of N-region crystals. It is because it becomes.
- the present invention has been made in view of the above problems, and a manufacturing method capable of adjusting the pulling condition of the N region silicon single crystal by the CZ method from the inspection result of the sample wafer even if no defect appears.
- the purpose is to provide.
- the present invention provides a method for manufacturing a silicon single crystal rod in which a pulling condition is controlled by a Czochralski method to pull up an N region silicon single crystal rod, wherein the pulled N region silicon single crystal
- the sample wafer cut out from the rod is subjected to a heat treatment for revealing oxygen precipitates, subjected to selective etching, and subjected to EOSF inspection to measure the density of Enhanced-OSF.
- the defect region of the sample wafer is determined by performing a shallow pit inspection to investigate the defect region.
- Nv region when the defect region is N region
- Provided is a method for producing a silicon single crystal rod, wherein it is also determined which part or which part is in the Ni region, and the pulling condition is adjusted according to the result of the determination. .
- the portion is close to the boundary with the V region (the portion on the V region side in the Nv region) or the portion close to the boundary with the I region (the portion on the I region side in the Ni region). Then, when the next pull-up is performed under the same conditions, the pull-up conditions are appropriately adjusted so as to prevent the fluctuation of the process and the unscheduled defect region being shifted to become the V region or the I region. It is possible. Therefore, it becomes possible to manufacture the N region silicon single crystal rod more reliably and stably.
- the first stage heat treatment is performed at 900 to 1050 ° C. for 30 to 300 minutes, and then the second stage heat treatment is performed at 1100 to 1200 ° C. for 30 to 200 minutes. it can.
- the OSF can be forcibly generated, and a highly accurate inspection (EOSF inspection) can be performed.
- EOSF inspection highly accurate inspection
- the relationship between the V region and the N region and the density of the Enhanced-OSF is investigated in advance, and based on the relationship and the density of the Enhanced-OSF measured by the EOSF inspection, The determination of the V region and the N region can be performed.
- the position of the oxygen precipitate formation area formed at the boundary between the I area and the N area is determined from the occurrence pattern of the shallow pit investigated by the shallow pit inspection, and the I area and the The determination of the N region can be performed.
- the pulling speed F of the N-region silicon single crystal rod when adjusting the pulling conditions, the pulling speed F of the N-region silicon single crystal rod, the distance D between the raw material melt surface and the bottom of the heat shield member, the position P H of the heater for heating the raw material, and the raw material melt are accommodated. It can be performed by adjusting one or more of the positions P C of the crucible.
- V / G can be adjusted, and the pulling conditions of the N region silicon single crystal can be adjusted more appropriately.
- the pulling speed F is decreased or the distance D is increased, and the I region side in the Ni region is increased.
- the pulling speed F can be increased or the distance D can be decreased.
- the defect region can be pulled up to be a portion further away from the V region in the Nv region, or can be pulled to be a portion further away from the I region in the Ni region. Even if the fluctuation of the defect occurs and the defect area shifts, it can be made difficult to become the V area or the I area. Therefore, an N region silicon single crystal rod can be manufactured more reliably.
- an N region silicon single crystal rod can be manufactured with high accuracy. Therefore, the N region crystal can be manufactured stably, and productivity and yield can be improved.
- FIG. 2 shows an example of a CZ single crystal pulling apparatus that can be used in the method for producing a silicon single crystal rod of the present invention.
- CZ single crystal pulling apparatus 1 shown in FIG. 2 is a crucible 4 (here for accommodating the raw material melt 2, although the crucible position P C is set to the height position relative to the bottom of the main chamber, this criterion particularly not limited to), a polycrystalline silicon material to heat to heater 5 (here for melting, but the heater position P H is the bottom height position relative to the main chamber, this criterion is not specifically limited), etc.
- Is provided in the main chamber 6.
- a pulling mechanism (not shown) for pulling up the grown single crystal is provided on the upper portion of the pulling chamber 7 connected to the main chamber 6.
- a pulling wire 8 is unwound from a pulling mechanism attached to the upper part of the pulling chamber 7, and a seed crystal 9 supported by a seed holder is attached to the tip of the pulling wire 8.
- the single crystal rod 10 is formed below the seed crystal 9 by dipping in the liquid 2 and winding the pulling wire 8 at a pulling speed F by a pulling mechanism.
- the crucible 4 is supported by a crucible rotating shaft 17 that can be rotated and raised by a rotary drive mechanism (not shown) attached to the lower part of the CZ single crystal pulling apparatus 1. Further, a heat insulating member 11 is provided outside the heater 5 disposed around the crucible 4.
- the chambers 6 and 7 are provided with a gas inlet 12 and a gas outlet 13, so that argon gas or the like can be introduced into the chambers 6 and 7 and discharged.
- the gas rectifying cylinder 14 extends from at least the ceiling of the main chamber 6 toward the raw material melt surface 3 so as to surround the single crystal rod 10 being pulled up. Further, a heat shield member 15 is provided to cool the single crystal rod 10 by blocking the radiant heat from the heater 5 between the vicinity of the raw material melt surface 3 and the gas flow straightening cylinder 14. The heat shield member 15 is provided such that the lower end thereof is spaced from the raw material melt surface 3 by a distance D.
- a magnetic field application device 16 can be further installed outside the main chamber 6 in the horizontal direction, thereby suppressing the convection of the raw material melt by applying a magnetic field in the horizontal direction or the vertical direction to the raw material melt 2.
- a CZ single crystal pulling apparatus based on the so-called MCZ method for achieving stable growth of a single crystal can also be used.
- FIG. 1 is a flowchart showing an example of a method for producing a silicon single crystal rod according to the present invention.
- (Process 1) Sample wafer preparation, (Process 2) EOSF inspection, (Process 3) Shallow pit inspection, (Process 4) Defect area determination (Nv, Ni area determination) (Step 5) adjustment of the pulling conditions, and (step 6) pulling up the N-region silicon single crystal rod.
- Process 1 Preparation of sample wafer
- An N region silicon single crystal rod pulled up by the CZ method is cut into a wafer shape by, for example, a wire saw.
- Prepare a sample wafer by extracting a part of it.
- the number of sample wafers to be prepared and the location to be taken out are not particularly limited, and can be determined as appropriate.
- EOSF inspection is performed on the sample wafer.
- a heat treatment for revealing oxygen precipitates is performed. Any heat treatment that can reveal Enhanced-OSF (hereinafter sometimes simply referred to as EOSF) may be used, and specific heat treatment conditions are not particularly limited.
- the first stage heat treatment can be performed at 900 to 1050 ° C. for 30 to 300 minutes, and then the second stage heat treatment can be performed at 1100 to 1200 ° C. for 30 to 200 minutes.
- the atmosphere of the heat treatment is not particularly limited, and dry oxygen (dry O 2 ) or wet O 2 containing water vapor in O 2 gas can be used for both the first stage and the second stage heat treatment.
- the temperature raising rate and the temperature lowering rate in the heat treatment step are not particularly limited, and may be set to 2 ° C./min or more. By performing such two-stage heat treatment, OSF can be detected with higher sensitivity than conventional OSF heat treatment (for example, one-stage oxidation heat treatment at 1100 to 1200 ° C.).
- the etched surface is observed with an optical microscope and the EOSF density (number of large particle size OSF generated per unit area) is measured.
- Step 4 Determination of defect area
- the defective area of the sample wafer is determined.
- the determined defect area is the N area, it is further determined which part in the Nv area or which part in the Ni area.
- FIG. 3 shows the distribution of crystal defects in the pulling axis direction when the CZ silicon single crystal bar is grown from a high speed by gradually decreasing the pulling speed.
- the right side of FIG. The in-plane defect distribution of the wafer cut out from each of the positions is shown.
- the N region is closer to the V region. That is, it is a portion on the V region side even in the Nv region.
- the density of EOSF is small where the Nv region and the Ni region are mixed. As described above, it is also determined which part in the Nv region. Note that EOSF is not detected in the Ni region or the I region.
- the sample wafer defect area is set to the V area, and is smaller than the upper limit value and 1 ⁇ 2 or more of the upper limit value (high density) ) In the Nv region, and when it is smaller than 1/2 of the upper limit value and larger than zero (low density), the Nv region and the Ni region are mixed, and when it is zero, it can be determined as the Ni region or the I region.
- FIG. 3 shows an example where the upper limit value is exceeded, the upper limit value is high, and the density is high.
- the determination criteria such as the upper limit value can be appropriately determined and are not particularly limited.
- the defect density in the EOSF inspection is an inspection in which the oxygen precipitation region is observed, and depends on the oxygen concentration and the defect level.
- shallow pits are not detected in the V region and the Nv region.
- heat treatment of EOSF natural contamination due to impurities is slightly caused from the heat treatment furnace. By this heat treatment, oxygen precipitates are formed in the V region and the Nv region and have gettering ability. Shallow pits are not observed.
- shallow pits are generated in the Ni region and the generated pattern can be detected. Therefore, when the Nv region and the Ni region are mixed, the shallow pits are generated in a ring shape.
- the portion where the Nv region and the Ni region are mixed as shown in FIG. 3 there is no Nv region in the in-plane center portion and the outer peripheral portion, and no shallow pit is generated.
- Ni region exists in the vicinity of / 2 and shallow pits are generated in a ring shape.
- shallow pits are generated on the entire surface. Therefore, even in the Ni region, it is possible to determine whether it is a portion on the Nv region side mixed with the Nv region or a portion on the I region side without mixing.
- An oxygen precipitate formation region also exists in the boundary region between the I region and the Ni region, but this oxygen precipitate formation region cannot be detected by the EOSF inspection, but can be detected only by the shallow pit inspection. Since shallow pits are not detected in this oxygen precipitate formation region, they are detected in a ring shape (no shallow pits) between the Ni region and the I region where the shallow pits are detected. For example, in the radial direction, there is no ring-shaped shallow pit in the vicinity of 1 ⁇ 2 of the radius R. Therefore, it is possible to determine the position of the oxygen precipitate formation region from the occurrence pattern of the shallow pits and determine whether or not it is closer to the I region even in the Ni region. As described above, it is also determined which part in the Ni region.
- the pulling conditions of the N region silicon single crystal to be pulled next are adjusted according to the determination result of the defect region in step 4.
- adjustment of the temperature gradient G of the crystal growth interface vicinity may be carried out by adjusting the raw material melt distance D between the shielding member lower end, the position P H of the heater, and the position P C of the crucible.
- the pulling speed F when it is determined that the portion is on the V region side in the Nv region, the pulling speed F can be decreased or the distance D can be increased.
- the defect region can be pulled up to be a part further away from the V region. That is, it is possible to prevent the crystal to be grown from shifting to the V region due to process variations due to various factors as described above.
- the adjustment can be performed in the same manner when it is determined that the region is the V region, but in this case, the adjustment width may be increased so as to shift from the V region to the N region.
- the pulling speed F can be increased or the distance D can be decreased.
- the defect region can be pulled up so as to be a portion further away from the I region. That is, it is possible to prevent a shift to the I region due to process variations.
- An example of the relationship between the pulling speed and the defect area is shown in FIG. Note that the adjustment can be performed in the same manner when it is determined that the region is the I region, but in this case, the adjustment width may be increased so as to shift from the I region to the N region. By these methods, the N region silicon single crystal can be pulled up more reliably and stably.
- the position P H of the heater may be to adjust the position P C of the crucible. That is, a high relative heater position P H, when to lower the position P C of the crucible, to be able to obtain the same effect as increasing the pulling speed, a relatively heater reversed position P the H low, if to be higher the position P C of the crucible, it is possible to obtain the same effect as reducing the pulling rate.
- These parameters may be adjusted independently, but a plurality of parameters may be adjusted simultaneously in accordance with other single crystal quality conveniences.
- Step 6 Pulling up the N region silicon single crystal rod
- a polycrystalline raw material is put into a crucible 4 of a CZ single crystal pulling apparatus 1 shown in FIG. 2 and heated and melted by a heater 5 to obtain a raw material melt 2.
- the seed crystal 9 is immersed in the raw material melt 2 and then pulled, and an N region silicon single crystal rod 10 is manufactured by the CZ method.
- the specific pulling conditions at this time are the pulling conditions adjusted in step 5.
- the EOSF inspection or the like is only for pass / fail judgment, and the pulling conditions are adjusted only after the failure occurs.
- the failure is not limited to the occurrence of the failure. Even if it does not occur (in the N region), it is determined whether or not it is in the vicinity of the V region or the I region, and even if a process fluctuation occurs, it shifts to the V region or the I region and does not fail.
- the pulling conditions can be adjusted as follows. Therefore, the N region silicon single crystal can be manufactured more reliably than the conventional method.
- Example 1 The manufacturing method of the silicon single crystal rod of the present invention shown in FIG. 1 was carried out. A plurality of sample wafers from an N region silicon single crystal rod by the CZ method were subjected to EOSF inspection and shallow pit inspection to determine a defect region. Based on the determination result, the pulling conditions were adjusted so that the pulling can be performed more reliably in the N region. Further, the following N-region silicon single crystal rod was manufactured based on the adjusted pulling conditions.
- first stage heat treatment was performed at 900 ° C. for 60 minutes under dry O 2
- second stage heat treatment was performed for 100 minutes at 1200 ° C. under wet O 2 .
- a mixed solution of 49% concentration dilute hydrofluoric acid and 0.15 mol% concentration potassium dichromate aqueous solution that is, Seco solution [composition: HF 100 cc, K 2 Cr 2 O 7 aqueous solution. (0.15 mol%) 50 cc] for 10 minutes, the ⁇ 100> plane was selectively etched, the etched plane was observed with an optical microscope, and the EOSF density was measured.
- the shallow pit inspection the sample wafer on which the EOSF was measured was visually observed under the light collection, and the pattern of the shallow pit was investigated by confirming the pattern of minute defects.
- the upper limit value of the EOSF density (the boundary between the V region and the N region) is set to 1.3X 2 -10X (pieces / cm 2 ) as in Patent Document 2 (where X is the initial oxygen concentration).
- the concentration was set to ppma (ASTM '79).
- Table 1 shows the result of the EOSF inspection, the result of the shallow pit inspection, the determination of the defective area, and the adjustment method of the lifting conditions (in this case, the adjustment of the lifting speed).
- the speed at which OSF appears in the wafer surface is F 1
- the speed at which LEP appears or the above-mentioned special shallow pit pattern is detected is F 2
- F 1 -F 2 is F 0 .
- the density (upper limit value) of EOSF that is a criterion for acceptance / rejection is assumed to be EOSF 1 .
- Example 2 The pulling speed is adjusted in the same manner as in Example 1, and the in-plane distribution is adjusted from the results of the EOSF inspection and the shallow pit inspection so that the margin for pulling up in the N region is optimized, and the N region silicon single unit is adjusted. A crystal rod was produced.
- the adjustment method as shown in FIG. 5, if the shallow pit is generated in the EOSF defect generation, or peripheral portion in the center, increasing the distance D, or raised heater position P H. In the opposite case, the reverse adjustment was performed. As for the value to be changed, the distance D was adjusted at a rate of 5%, and in the case of the heat generation position, the limit was 10% of the melt depth.
- this pattern is derived from the manufacturing method. Therefore, when the pulling speed and the appearance pattern of the crystal defect are different, it is necessary to set a determination criterion according to that.
- LEP inspection, OSF inspection, and Cu deposition inspection were performed on a plurality of sample wafers from an N region silicon single crystal rod by the CZ method, and pass / fail was determined.
- LEP is a Seco solution or a chemical solution disclosed in JP-A-2003-209150 (hydrofluoric acid, nitric acid, acetic acid and water in the etching solution are (400) :( 2-4) :( 10-50) :( 80 )
- a defect observed by selective etching with iodine or iodide containing 0.03 g or more per liter of the total amount of the etching solution If it fails, it will be rejected.
- the OSF is rejected if ring defects are observed when oxidized at 1100-1200 ° C.
- Cu deposition was a method in which a voltage was applied to a wafer with an oxide film in a solution containing Cu ions, and copper was deposited on the crystal defect portion to observe the defects. Ring defects were confirmed. In this case, it is rejected (see Japanese Patent Application Laid-Open No. 2002-201093).
- the pass / fail result was fed back to the pulling conditions to produce the next N-region silicon single crystal rod.
- the pulling rate was increased by 1/2 of the margin
- the pulling rate was decreased by 1/2 of the margin.
- Comparative Example 2 EOSF inspection similar to Example 1 and LEP inspection similar to Comparative Example 1 were performed on a plurality of sample wafers from an N region silicon single crystal rod by the CZ method, and pass / fail was determined.
- the pulling speed was adjusted. In the case of LEP failure, the pulling speed was increased by 1/2 of the margin, and when the upper limit of EOSF was exceeded, it was decreased by 1/2 of the margin.
- Table 2 shows the pass rate of defects in the N-region silicon single crystal rod pulled up in Examples 1 and 2 and Comparative Examples 1 and 2. It shows the ratio of the number of crystals in which no defects occurred with respect to the number of crystals produced.
- Example 1 and Example 2 in which the present invention is implemented are much higher than those of Comparative Examples 1 and 2 according to the conventional method, and an N-region silicon single crystal rod can be manufactured reliably.
- an N-region silicon single crystal rod can be manufactured more stably than before, and the number of quality defects can be reduced. Therefore, the yield can be improved and the manufacturing cost can be reduced.
- the present invention is not limited to the above embodiment.
- the above-described embodiment is an exemplification, and the present invention has substantially the same configuration as the technical idea described in the claims of the present invention, and any device that exhibits the same function and effect is the present invention. It is included in the technical scope of the invention.
- the sample wafer is exemplified not only in the N region but also in the sample wafer including a portion where a defect such as the V region and the I region occurs. Even if not, it is possible to adjust the pulling condition to a more appropriate numerical value from the EOSF density and the generation pattern of the shallow pits, and to manufacture the N region silicon single crystal rod more reliably.
Abstract
Description
この保証方法としては、結晶検査工程でLEPというエッチングによる巨大転位クラスタの確認と、EOSF(Enhanced-OSF)検査(特許文献1、特許文献2等参照)が挙げられ、これらにより、判定することが可能である。
したがって、この製品は製造マージンが狭く、V領域、OSF領域、N領域(Nv領域、Ni領域)、I領域のどの欠陥領域で製造を行っているのか、常にモニタリングをし、必要に応じて、引き上げ条件をチューニング(調整)する必要がある。というのは、用いるヒータや断熱材等の炉内部品が経時変化することに基づき、炉内温度分布が経時変化するため、この引き上げ条件のチューニングがN領域結晶を安定して製造するのに不可欠となるためである。
しかしながら、これでは不良が出ないと引き上げ条件の調整が出来ないという問題があった。
しかしながら本発明の製造方法であれば、合格となるN領域(Nv領域、Ni領域)であっても、その領域内のどの部分であるかの判定も行い、該判定の結果に応じて次の引き上げ条件の調整を行う。したがって、本発明であれば、従来法とは異なり、上記のような欠陥領域のずれを予測し、不良が出ずとも引き上げ条件の適切な調整が可能である。
図2に本発明のシリコン単結晶棒の製造方法に使用することができるCZ単結晶引上げ装置の一例を示す。
図2に示したCZ単結晶引上げ装置1は、原料融液2を収容するルツボ4(ここで、ルツボ位置PCはメインチャンバの底部を基準とした高さ位置としているが、この基準は特に限定されない)、多結晶シリコン原料を加熱、溶融するための加熱ヒーター5(ここで、ヒーター位置PHはメインチャンバの底部を基準とした高さ位置としているが、この基準は特に限定されない)などがメインチャンバ6内に設けられている。また、該メインチャンバ6上に連設された引上げチャンバ7の上部には、育成された単結晶を引上げる引上げ機構(図示せず)が設けられている。
また、ルツボ4の周囲に配設された加熱ヒーター5の外側には、断熱部材11が設けられている。
また、チャンバ6、7には、ガス導入口12、ガス流出口13が設けられており、チャンバ6、7内部にアルゴンガス等を導入し、排出できるようになっている。
CZ法で引き上げたN領域シリコン単結晶棒を例えばワイヤソーによりウエーハ状に切り出す。この中から一部、サンプルウエーハを抜き取ることで用意する。用意するサンプルウエーハの枚数、取り出し箇所は特に限定されず、適宜決定することができる。
サンプルウエーハに対してEOSF検査を行う。まず、酸素析出物を顕在化させる熱処理を施す。Enhanced-OSF(以下、単にEOSFということがある)を顕在化できる熱処理であれば良く、具体的な熱処理条件は特に限定されない。
例えば、900~1050℃で30~300分間の第1段熱処理を施し、次いで1100~1200℃で30~200分間の第2段熱処理を施すことができる。
熱処理の雰囲気は特に限定されるものではなく、第1段、第2段熱処理のいずれも乾燥酸素(ドライO2)またはO2ガス中に水蒸気を含むウェットO2が使用できるが、第1段熱処理ではドライO2の方が操作が簡便で好ましく、第2段熱処理ではウェットO2の方が、OSFの長さがドライO2に比べて長くなり、後の光学顕微鏡による観察が容易となるので好ましい。熱処理工程における昇温速度、降温速度も特に限定されず、2℃/分以上に設定すればよい。
このような2段階の熱処理を行うことによって、従来のOSF熱処理(例えば、1100~1200℃での1段階の酸化熱処理)よりも、一層高感度にOSFを検出することができる。
次に、EOSFを測定したサンプルウエーハを、集光下、目視で観察し、微小欠陥のパターンを確認することによりシャローピット検査を行う。シャローピットが発生している部分は、表面がくすんだ状態になり、この部分をシャローピット有りとする。
工程2のEOSF検査および工程3のシャローピット検査の結果に基づいてサンプルウエーハの欠陥領域を判定する。なお、判定した欠陥領域がN領域の場合には、さらに、Nv領域内のどの部分であるか、またはNi領域内のどの部分であるかの判定も行う。
まず、EOSF検査の結果に関して、図3に示すように、V領域、OSF領域ではEOSFが非常に高密度で検出される。
また、COPフリー領域(N領域)はVacancyが優勢なNv領域とInterstitial Siが優勢なNi領域とに分類される。このNv領域は、酸素析出が起こりやすく、EOSF検査で欠陥が高密度で発生する。この値が大きければ大きいほど、V領域に近いN領域であることが確認できる。すなわち、Nv領域内でもV領域側の部分である。
また、Nv領域からNi領域にかけての製造で、このNv領域とNi領域が混在するところでは、EOSFの密度が少ない。
以上のように、Nv領域内のどの部分であるかの判定も行う。
なお、Ni領域、またはI領域ではEOSFが検出されない。
図3では、上限値超え、上限値、高密度の例を示してある。
なお、予め、V領域およびN領域(特にはNv領域)と、EOSFの密度との関係を調査しておくと良い。そして調査によって得られた関係(上限値等)とEOSF検査で測定したEOSFの密度に基づき、V領域およびNv領域の判定を行うことができる。
また、全面Ni領域の場合には全面にシャローピットが発生する。
したがって、Ni領域内でも、Nv領域と混在するようなNv領域側の部分か、混在なしのI領域側の部分かの判定を行うことができる。
以上のように、Ni領域内のどの部分であるかの判定も行う。
工程4での欠陥領域の判定結果に応じて、次に引き上げるN領域シリコン単結晶の引き上げ条件の調整を行う。
N領域シリコン単結晶の引き上げのためには(引き上げ速度F)/(結晶成長界面近傍の温度勾配G)の値の制御が重要である。ここで、結晶成長界面近傍の温度勾配Gの調整は、原料融液と遮蔽部材下端との距離D、ヒーターの位置PH、ルツボの位置PCなどを調整することによって行うことができる。
なお、V領域であると判定された場合にも同様にして調整を行うことができるが、この場合はV領域からN領域へずれるように調整幅は大きくすると良い。
なお、I領域であると判定された場合にも同様にして調整を行うことができるが、この場合はI領域からN領域へずれるように調整幅は大きくすると良い。
これらの方法によって、N領域シリコン単結晶をより確実に安定して引き上げることが可能になる。
図2に示すCZ単結晶引上げ装置1のルツボ4内に多結晶原料を投入し、加熱ヒーター5で加熱溶融して原料融液2を得る。次に、該原料融液2に種結晶9を浸漬した後引上げ、CZ法により、N領域シリコン単結晶棒10を製造する。このときの具体的な引き上げ条件は、工程5で調整した引き上げ条件とする。
(実施例1)
図1に示す本発明のシリコン単結晶棒の製造方法を実施した。
CZ法によるN領域シリコン単結晶棒からの複数枚のサンプルウエーハにEOSF検査およびシャローピット検査を行って欠陥領域を判定した。そして該判定結果に基づいて、より確実にN領域で引き上げられるように引き上げ条件を調整した。さらに該調整した引き上げ条件に基づいて次のN領域シリコン単結晶棒を製造した。
また、表面の酸化膜を除去後、濃度49%の希フッ酸と濃度0.15モル%の重クロム酸カリウム水溶液との混合液、すなわちセコ液〔組成:HF100cc、K2Cr2O7水溶液(0.15モル%)50cc〕に10分間浸漬して、〈100〉面を選択的にエッチングし、光学顕微鏡によりエッチング面を観察し、EOSF密度を測定した。
前述したように、EOSFの値が酸素によって導き出された上限値に近い場合は、COPフリーのNv領域であっても、V領域に近い部分であり、次の単結晶棒の製造ではプロセスの変動でV領域にずれてしまう可能性がある。またEOSFがなく、シャローピットが全面で検出されるような場合、COPフリーのNi領域であっても、比較的I領域に近い部分であり、その場合は次の単結晶棒の製造ではプロセスの変動でI領域にずれてしまう可能性がある。そこで、Nv領域、Ni領域であっても引き上げ速度を調整した。
ウェーハ面内にOSFが出現する速度をF1、LEPが出現するもしくは上記の特殊なシャローピットパターンが検出される速度をF2とし、F1-F2をF0とする。また、合否判定基準となるEOSFの密度(上限値)をEOSF1とする。
実施例1と同様にして引き上げ速度の調整を行うとともに、EOSF検査、シャローピット検査の結果から、面内分布を調整し、N領域で引き上げるためのマージンが最適となるようにし、N領域シリコン単結晶棒を製造した。
調整方法としては、図5に示すように、中心部にEOSF欠陥が発生、または周辺部にシャローピットが発生している場合は、距離Dを広げる、またはヒーター位置PHを上げた。そして、その逆の場合は、逆の調整を行った。
変更する値は、距離Dは5%の割合で調整し、発熱位置の場合は、メルトの深さの10%を限度とした。
なお、ここでは上記のように設定したが、このパターンは、製造方法に由来するため、引き上げ速度と結晶欠陥の出現のパターンが違う場合は、それにあった判定基準を設定する必要がある。
CZ法によるN領域シリコン単結晶棒からの複数枚のサンプルウエーハにLEP検査、OSF検査、Cuデポジション検査を行って合否を判定した。
なお、LEPは、セコ液もしくは、特開2003-209150号公報の薬液(エッチング液中のフッ酸、硝酸、酢酸及び水が(400):(2~4):(10~50):(80)の容量比を有し、且つヨウ素又はヨウ化物がエッチング液の総液量1リットル当たり0.03g以上含有しているもの)で選択エッチングすることで観察される欠陥で、欠陥が確認された場合、不合格となる。
OSFは1100-1200℃で酸化処理されたときにリング状の欠陥が観測された場合、不合格となる。
また、Cuデポジションは、酸化膜をつけたウェーハをCuイオンを含有する溶液中で電圧を印加し、結晶欠陥部分に銅を析出させて欠陥を観察する方法で、リング状欠陥が確認された場合、不合格とする(特開2002-201093号公報参照)。
なお、LEP不良の場合、引き上げ速度をマージンの1/2の分だけプラスし、OSF不良及びCuデポジション不良の場合、引き上げ速度をマージンの1/2の分だけマイナスした。
CZ法によるN領域シリコン単結晶棒からの複数枚のサンプルウエーハに実施例1と同様のEOSF検査、比較例1と同様のLEP検査を行って合否を判定した。
EOSF上限及びLEPの不合格が発生した際に、引き上げ速度の調整を行った。
なお、LEP不良の場合、引き上げ速度をマージンの1/2の分だけプラスし、EOSFの上限を超えた場合、マージンの1/2の分だけマイナスした。
Claims (6)
- チョクラルスキー法により引き上げ条件を制御してN領域シリコン単結晶棒を引き上げるシリコン単結晶棒の製造方法であって、
前記引き上げたN領域シリコン単結晶棒から切り出したサンプルウエーハに、酸素析出物を顕在化させる熱処理を施し、選択エッチングを施してEnhanced-OSFの密度を測定するEOSF検査を行うとともに、該EOSF検査したサンプルウエーハにおけるシャローピットの発生パターンを調査するシャローピット検査を行うことにより、
前記サンプルウエーハの欠陥領域を判定し、該判定の結果に応じ、前記引き上げ条件を調整して次のN領域シリコン単結晶棒を引き上げるとき、
前記欠陥領域の判定において、前記欠陥領域がN領域の場合に、Nv領域内のどの部分であるか、またはNi領域内のどの部分であるかの判定も行い、該判定の結果に応じ、前記引き上げ条件の調整を行うことを特徴とするシリコン単結晶棒の製造方法。 - 前記酸素析出物を顕在化させる熱処理として、900~1050℃で30~300分間の第1段熱処理を施し、次いで1100~1200℃で30~200分間の第2段熱処理を施すことを特徴とする請求項1に記載のシリコン単結晶棒の製造方法。
- 前記欠陥領域の判定において、
予め、V領域およびN領域と、Enhanced-OSFの密度との関係を調査しておき、該関係と前記EOSF検査で測定したEnhanced-OSFの密度に基づき、前記V領域および前記N領域の判定を行うことを特徴とする請求項1または請求項2に記載のシリコン単結晶棒の製造方法。 - 前記欠陥領域の判定において、
前記シャローピット検査で調査したシャローピットの発生パターンから、I領域とN領域の境界に形成される酸素析出物形成領域の位置を判断し、前記I領域および前記N領域の判定を行うことを特徴とする請求項1から請求項3のいずれか一項に記載のシリコン単結晶棒の製造方法。 - 前記引き上げ条件を調整するとき、N領域シリコン単結晶棒の引き上げ速度F、原料融液面と遮熱部材下端との距離D、原料を加熱するヒーターの位置PH、原料融液を収容するルツボの位置PCのうち1つ以上を調整することにより行うことを特徴とする請求項1から請求項4のいずれか一項に記載のシリコン単結晶棒の製造方法。
- 前記欠陥領域の判定において、Nv領域内のV領域側の部分であると判定したときは前記引き上げ速度Fを小さくするか、前記距離Dを大きくし、Ni領域内のI領域側の部分であると判定したときは前記引き上げ速度Fを大きくするか、前記距離Dを小さくすることを特徴とする請求項5に記載のシリコン単結晶棒の製造方法。
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JP2021008388A (ja) * | 2019-07-02 | 2021-01-28 | 信越半導体株式会社 | 炭素ドープシリコン単結晶ウェーハ及びその製造方法 |
JP7188299B2 (ja) | 2019-07-02 | 2022-12-13 | 信越半導体株式会社 | 炭素ドープシリコン単結晶ウェーハ及びその製造方法 |
US11761118B2 (en) | 2019-07-02 | 2023-09-19 | Shin-Etsu Handotai Co., Ltd. | Carbon-doped silicon single crystal wafer and method for manufacturing the same |
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JP5946001B2 (ja) | 2016-07-05 |
JPWO2014129123A1 (ja) | 2017-02-02 |
KR20150120372A (ko) | 2015-10-27 |
KR101997561B1 (ko) | 2019-07-08 |
US20150354089A1 (en) | 2015-12-10 |
DE112014000431T5 (de) | 2015-10-15 |
DE112014000431B4 (de) | 2020-12-10 |
CN104995340A (zh) | 2015-10-21 |
US9777394B2 (en) | 2017-10-03 |
CN104995340B (zh) | 2018-02-06 |
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