CN111601916A - Quality determination method of silicon ingot, quality determination program of silicon ingot, and manufacturing method of single crystal silicon - Google Patents
Quality determination method of silicon ingot, quality determination program of silicon ingot, and manufacturing method of single crystal silicon Download PDFInfo
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Abstract
Description
技术领域technical field
本发明涉及一种硅块的品质判定方法、硅块的品质判定程序及单晶硅的制造方法。The invention relates to a method for judging the quality of a silicon block, a program for judging the quality of a silicon block and a method for producing single crystal silicon.
背景技术Background technique
以往,在制造硅晶片等半导体晶片时,例如在对利用提拉法提拉的单晶硅锭进行外周磨削后,切掉不能作为产品而使用的顶部与尾部。之后,利用线锯等切断装置,将单晶硅锭切成多个硅块。Conventionally, when manufacturing semiconductor wafers, such as a silicon wafer, after grinding the outer periphery of the single crystal silicon ingot pulled by the pulling method, for example, the top part and the tail part which cannot be used as a product are cut off. After that, the single crystal silicon ingot is cut into a plurality of silicon ingots using a cutting device such as a wire saw.
此时,从硅块的端部切出样品晶片,通过评价电阻率、氧浓度、OSF(OxidationInduced Stacking Fault ring,氧化诱导层错环)、Void缺陷、L/DL缺陷(LargeDislocation Loop,大位错环)等Grown-in(原生)缺陷等,进行硅块的品质评价。At this time, a sample wafer was cut out from the end of the silicon block, and the resistivity, oxygen concentration, OSF (Oxidation Induced Stacking Fault ring, oxidation induced stacking fault ring), Void defect, L/DL defect (Large Dislocation Loop, large dislocation ring) were evaluated by evaluating Ring) and other Grown-in (original) defects, etc., to evaluate the quality of the silicon block.
另外,近年来,强烈地需求在晶片的整个表面中没有原生缺陷或只有极低密度的原生缺陷的晶片,伴随于此,还强烈地需求没有原生缺陷或只有极低密度的原生缺陷的单晶硅。In addition, in recent years, there has been a strong demand for wafers having no primary defects or only an extremely low density of primary defects in the entire surface of the wafer, and along with this, there is also a strong demand for single crystals with no primary defects or only an extremely low density of primary defects. silicon.
作为提拉这种单晶硅的方法,例如有改善提拉装置的炉内温度分布,一边调整提拉速度,一边提拉单晶硅的方法。As a method of pulling such single crystal silicon, for example, there is a method of pulling the single crystal silicon while improving the temperature distribution in the furnace of the pulling device and adjusting the pulling speed.
然而,提拉速度的管理范围非常狭小,因此即使硅块端部的晶体品质合格,若在块中间部提拉速度发生变动,则会有在硅块中产生原生缺陷的情况,因此存在下一个工序中发生不良的问题。However, the management range of the pulling speed is very narrow, so even if the crystal quality at the end of the silicon block is acceptable, if the pulling speed varies in the middle part of the block, there may be cases where primary defects are generated in the silicon block, so there is a next A defect occurred in the process.
在此,在不良中,将基于L/DL缺陷的检测结果的不良称为L/DL不良,将基于Void缺陷的检测结果的不良称为Void不良。Here, among the defects, the defect based on the detection result of the L/DL defect is referred to as the L/DL defect, and the defect based on the detection result of the Void defect is referred to as the Void defect.
专利文献1中公开有如下技术:沿着单晶硅锭的生长轴将提拉数据读取到计算机中,当提拉数据与目标值之差成为规定值以上时,在成为规定位置以上的位置切断单晶硅锭,获得没有原生缺陷的硅块。Patent Document 1 discloses a technique in which pulling data is read into a computer along the growth axis of a single crystal silicon ingot, and when the difference between the pulling data and a target value becomes a predetermined value or more, the position becomes a predetermined position or more. A single crystal silicon ingot is cut to obtain a silicon ingot without primary defects.
现有技术文献prior art literature
专利文献Patent Literature
专利文献1:日本特开2007-99556号公报Patent Document 1: Japanese Patent Laid-Open No. 2007-99556
发明内容SUMMARY OF THE INVENTION
发明所要解决的技术问题The technical problem to be solved by the invention
然而,专利文献1中公开的技术中,由于以使提拉数据与目标值之差成为规定值的方式进行管理,因此不一定与实际的样品晶片的品质评价结果一致。因此,在下一个工序中,排除被判定为不良品的硅块并切断硅块,并且再次进行品质评价的情况下,不知道在哪一个部分发生了不良,因此存在导致品质确认频度增加的问题。However, in the technique disclosed in Patent Document 1, since the difference between the pulling data and the target value is managed so that the difference between the target value becomes a predetermined value, it does not necessarily agree with the quality evaluation result of the actual sample wafer. Therefore, in the next step, when the silicon block determined to be defective is excluded, the silicon block is cut, and the quality evaluation is performed again, it is not known in which part the defect has occurred, so there is a problem that the frequency of quality confirmation increases. .
本发明的目的在于提供一种能够降低下一个工序中的品质确认频度的硅块的品质判定方法、硅块的品质判定程序及单晶硅的制造方法。An object of the present invention is to provide a method for judging the quality of a silicon ingot, a program for judging the quality of a silicon ingot, and a method for producing single crystal silicon, which can reduce the frequency of quality confirmation in the next step.
用于解决技术问题的方案Solutions for Technical Problems
本发明的硅块的品质判定方法是判定从利用提拉法提拉的单晶硅中切出的多个硅块的品质的硅块的品质判定方法,所述硅块的品质判定方法的特征在于执行:取得从多个硅块各自的端部切出的样品晶片的品质评价结果的步骤;取得所述单晶硅的提拉实际数据的步骤;根据各样品晶片的品质评价结果,设定各硅块的提拉管理范围的步骤;以及对照所取得的所述提拉实际数据和所设定的提拉管理范围,判定各硅块的品质的步骤。The quality judging method of a silicon ingot of the present invention is a quality judging method of a silicon ingot for judging the quality of a plurality of silicon ingots cut out from single crystal silicon pulled by the pulling method, and the characteristics of the quality judging method of the silicon ingot It is to perform: the step of obtaining the quality evaluation results of the sample wafers cut out from the respective ends of the plurality of silicon blocks; the step of obtaining the actual data of the pulling of the single crystal silicon; according to the quality evaluation results of each sample wafer, setting The step of pulling management range of each silicon block; and the step of judging the quality of each silicon block by comparing the obtained actual data of pulling and the set pulling management range.
在此,样品晶片的品质评价是指在不存在原生缺陷的单晶硅的Pv区域、Pv区域及Pi区域混合存在的区域以及Pi区域中的品质评价。Here, the quality evaluation of the sample wafer refers to the quality evaluation in the Pv region, the region where the Pv region and the Pi region coexist, and the Pi region of the single crystal silicon without primary defects.
并且,提拉管理范围是指相对于提拉目标值能够允许的实际值的范围,其根据样品晶片的品质评价结果来设定。In addition, the pull-up management range refers to a range of allowable actual values with respect to the pull-up target value, and is set based on the quality evaluation result of the sample wafer.
根据本发明,根据样品晶片的品质评价结果,设定各硅块的提拉管理范围,对照每个硅块的提拉管理范围以及提拉实际数据。因此,能够高精度地判定超出提拉管理范围的提拉实际数据,并能够降低下一个工序中的品质确认频度。According to the present invention, according to the quality evaluation result of the sample wafer, the pulling management range of each silicon block is set, and the pulling management range and actual pulling data of each silicon block are compared. Therefore, the actual pulling data beyond the pulling management range can be determined with high accuracy, and the frequency of quality confirmation in the next process can be reduced.
本发明中,优选在设定所述提拉管理范围的步骤之前,在所述样品晶片的品质评价结果中,若取得显示L/DL(Large Dislocation Loop)不良的结果,则执行排除显示该结果的硅块的步骤。In the present invention, before the step of setting the pull-up management range, if a result showing L/DL (Large Dislocation Loop) failure is obtained in the quality evaluation result of the sample wafer, it is preferable to execute the exclusion and display the result. steps of the silicon block.
根据本发明,若样品晶片显示出L/DL不良,则切出该样品晶片的所有硅块都是L/DL不良的可能性高,因此能够预先排除不良品来更加降低下一个工序中的品质确认频度。According to the present invention, if a sample wafer exhibits L/DL failure, it is highly likely that all silicon blocks from which the sample wafer is cut out have L/DL failure. Therefore, it is possible to preliminarily exclude defective products and further reduce the quality in the next process. Confirm the frequency.
本发明中,优选在设定所述提拉管理范围的步骤之前,在所述样品晶片的品质评价结果中,若取得显示Void不良的结果,则执行排除显示该结果的硅块的步骤。In the present invention, before the step of setting the pull-up management range, if a result showing void failure is obtained in the quality evaluation result of the sample wafer, the step of excluding the silicon block showing the result is preferably performed.
根据本发明,与L/DL不良的情况相同地,能够排除Void不良的硅块,而更加降低下一个工序中的品质确认频度。According to the present invention, similarly to the case of L/DL failure, it is possible to exclude a silicon block with a Void failure, and to further reduce the frequency of quality confirmation in the next process.
本发明的硅块的品质判定程序的特征在于,使计算机执行前述的硅块的品质判定方法。The quality judging program of a silicon block of the present invention is characterized by causing a computer to execute the above-mentioned method for judging the quality of a silicon block.
根据本发明,通过使计算机执行,能够促进自动化,因此能够减轻品质管理工序本身的负担。According to the present invention, since automation can be promoted by executing the computer, the burden of the quality control process itself can be reduced.
本发明的单晶硅的制造方法的特征在于,使计算机执行前述的硅块的品质判定程序,计算出提拉单晶硅时的提拉管理范围,并根据计算出的提拉管理范围,控制所述单晶硅的提拉。The method for producing single crystal silicon of the present invention is characterized in that a computer executes the quality determination program of the silicon block, calculates a pulling control range when pulling the single crystal silicon, and controls the pulling control range based on the calculated pulling control range. The pulling of the single crystal silicon.
根据本发明,根据对每个硅块设定的提拉管理范围,控制单晶硅的提拉,由此能够防止产生品质不合格的硅块来减少不合格品的产生。According to the present invention, by controlling the pulling of single crystal silicon according to the pulling management range set for each silicon block, it is possible to prevent the generation of defective silicon blocks and reduce the generation of defective products.
附图说明Description of drawings
图1是表示本发明的实施方式所涉及的单晶硅的提拉装置的示意图。FIG. 1 is a schematic view showing a pulling apparatus for single crystal silicon according to an embodiment of the present invention.
图2是表示所述实施方式的单晶硅的品质判定方法的流程图。FIG. 2 is a flowchart showing the quality determination method of single crystal silicon according to the embodiment.
图3是用于说明所述实施方式的管理范围的示意图。FIG. 3 is a schematic diagram for explaining the management range of the embodiment.
图4是用于说明所述实施方式的管理范围的示意图。FIG. 4 is a schematic diagram for explaining the management range of the embodiment.
图5是表示实施例的品质判定结果的图表。FIG. 5 is a graph showing the quality judgment results of the example.
图6是表示实施例的品质判定结果的图表。FIG. 6 is a graph showing the quality judgment result of the example.
具体实施方式Detailed ways
[1]单晶硅的提拉装置1的结构[1] Structure of the pulling device 1 for single crystal silicon
图1中示出表示能够适用本发明的实施方式所涉及的单晶硅10的制造方法的单晶硅的提拉装置1的结构的一例的示意图。提拉装置1是利用提拉法提拉单晶硅10的装置,其具备构成外壳的腔室2以及配置于腔室2的中心部的坩埚3。FIG. 1 is a schematic diagram showing an example of the configuration of a single crystal silicon pulling device 1 to which the method for producing single crystal silicon 10 according to the embodiment of the present invention can be applied. The pulling apparatus 1 is an apparatus for pulling up the single crystal silicon 10 by the pulling method, and includes a
坩埚3是由内侧的石英坩埚3A以及外侧的石墨坩埚3B构成的双层结构,被固定于能够旋转及升降的支承轴4的上端部。The
在坩埚3的外侧设置有包围坩埚3的阻抗加热式加热器5A、5B,在其外侧沿着腔室2的内表面设置有绝热材料6。
在坩埚3的上方,在与支承轴4相同的轴上设置有朝向反方向或相同方向以规定速度旋转的线等提拉轴7。在该提拉轴7的下端安装有籽晶8。Above the
在腔室2内配置有筒状的热屏蔽体12。A cylindrical heat shield 12 is arranged in the
热屏蔽体12发挥如下作用:对于培育中的单晶硅10,切断来自坩埚3内的硅熔液9或加热器5A、5B或坩埚3的侧壁的高温的辐射热,同时对于晶体生长界面即固液界面的附近,抑制热向外部扩散,担当控制单晶中心部及单晶外周部的提拉轴方向的温度梯度的功能。The heat shield 12 functions to cut off the high-temperature radiant heat from the silicon melt 9 in the
热屏蔽体12还发挥利用从炉上方导入的非活性气体将来自硅熔液9的蒸发部分排到炉外的整流筒的功能。The heat shield 12 also functions as a rectifying cylinder for discharging the evaporated part from the silicon melt 9 to the outside of the furnace by the inert gas introduced from above the furnace.
在腔室2的上部设置有气体导入口13,所述气体导入口13将氩气(以下称为Ar气)等非活性气体导入到腔室2内。在腔室2的下部设置有排气口14,所述排气口14通过驱动未图示的真空泵来吸引腔室2内的气体并将其排出。The upper part of the
从气体导入口13导入到腔室2内的非活性气体,下降到培育中的单晶硅10与热屏蔽体12之间,经过热屏蔽体12的下端与硅熔液9的液面之间的间隙后,朝向热屏蔽体12的外侧,甚至是坩埚3的外侧流出,之后在坩埚3的外侧下降,从排气口14排出。The inert gas introduced into the
在使用这种提拉装置1来制造单晶硅10时,将腔室2内维持为减压下的非活性气体的状态下,通过加热器5A、5B的加热使填充于坩埚3的多晶硅等固体原料熔融,形成硅熔液9。当坩埚3内形成硅熔液9时,使提拉轴7下降,将籽晶8浸渍到硅熔液9中,一边使坩埚3及提拉轴7朝规定方向旋转,一边慢慢地提拉提拉轴7,从而培育出与籽晶8相连的单晶硅10。When the single crystal silicon 10 is produced using the pulling apparatus 1, the polycrystalline silicon or the like filled in the
[2]产生于单晶硅10内的晶体缺陷[2] Crystal defects generated in the single crystal silicon 10
已知在利用提拉法提拉的单晶硅10中,存在在晶体生长时形成的晶体缺陷(原生缺陷)。It is known that in the single crystal silicon 10 pulled by the pulling method, there are crystal defects (primary defects) formed during crystal growth.
通常在单晶硅10中存在真性的点缺陷即Vacancy(空位)以及Interstitial(侵入型)硅。Generally, there are real point defects in the single crystal silicon 10 , namely, Vacancy (vacancy) and Interstitial (invading) silicon.
这些真性的点缺陷的饱和浓度是温度的函数,伴随着晶体培育中的急速的温度的下降而产生点缺陷的过饱和状态。The saturation concentration of these genuine point defects is a function of temperature, and a supersaturated state of point defects occurs with the rapid temperature drop during crystal growth.
过饱和的点缺陷会因成对消灭、外扩散·斜坡扩散等而朝向缓和过饱和状态的方向进行。通常无法完全消除该过饱和状态,最终作为空位或侵入型硅中的任意一者占优势的过饱和的点缺陷而存留。The supersaturated point defects progress in the direction of alleviating the supersaturated state due to pair extinction, out-diffusion, slope diffusion, and the like. Usually, the supersaturation state cannot be completely eliminated, and eventually it remains as a supersaturated point defect in which either vacancies or intrusive silicon predominate.
已知当晶体生长速度快时,空位容易成为过饱和状态,相反地,当晶体生长速度慢时,侵入型硅容易成为过饱和状态。It is known that when the crystal growth rate is high, vacancies tend to be in a supersaturated state, and conversely, when the crystal growth rate is slow, intrusive silicon tends to be in a supersaturated state.
当该过饱和状态的浓度达到一定值以上时,这些凝聚,并在晶体生长过程中形成晶体缺陷(原生缺陷)。When the concentration of this supersaturated state reaches a certain value or more, these aggregate and form crystal defects (primary defects) during crystal growth.
作为空位占优势的区域(V区域)的情况下的原生缺陷,已知OSF核或Void缺陷。OSF核是,在湿氧气氛中以1100℃左右的高温对从晶体切出的样品进行热处理时,从表面注入侵入型硅,在OSF核周围生长出堆垛层错(SF),在选择蚀刻液内一边摇动该样品,一边对其进行选择蚀刻时作为堆垛层错而被观察到的缺陷。As a native defect in the case of a vacancy-dominated region (V region), an OSF core or a void defect is known. The OSF core is that when a sample cut from a crystal is heat-treated at a high temperature of about 1100°C in a humid oxygen atmosphere, intrusive silicon is implanted from the surface, and stacking faults (SF) are grown around the OSF core. Defects observed as stacking faults when the sample was selectively etched while being shaken in the liquid.
由于通过氧化处理而生长出堆垛层错,所以被称为OSF(Oxygen induced StackingFault,氧致层错)。Since stacking faults are grown by oxidation treatment, they are called OSFs (Oxygen induced Stacking Faults).
Void缺陷是空位聚集而成的空洞状的缺陷,已知在内部的壁上形成有被称为内壁氧化膜的氧化膜。该缺陷根据检测方法而有几个名称。Void defects are void-like defects in which vacancies are aggregated, and it is known that an oxide film called an inner wall oxide film is formed on the inner wall. This defect has several names depending on the detection method.
对晶片表面照射激光光线,并通过检测其反射光·散射光等的粒子计数器而观察到的情况下,被称为COP(Crystal Originated Pattern Defect,晶源图案缺陷)。When the surface of the wafer is irradiated with laser light and observed by a particle counter that detects reflected light, scattered light, etc., it is called COP (Crystal Originated Pattern Defect).
在选择蚀刻液内不摇动样品而将其放置比较长时间后,作为流动模样而被观察到的情况下,被称为FPD(Flow Pattern Defect,流体图案缺陷)。When the sample is left to stand for a relatively long period of time without shaking the sample in the selected etching solution, when a flow pattern is observed, it is called FPD (Flow Pattern Defect).
从晶片的表面入射红外光激光,并通过检测其散射光的红外散射断层扫描仪观察到的情况下,被称为LSTD(Laser Scattering Tomography Defect,激光散射层析缺陷)。这些虽然检测方法都不同,但都被认为是Void缺陷。When an infrared light laser is incident from the surface of the wafer and observed by an infrared scattering tomography scanner that detects the scattered light, it is called LSTD (Laser Scattering Tomography Defect). Although these detection methods are different, they are all considered Void defects.
DSOD(Direct Surface Oxide Defect,直接表面氧化缺陷)也是Void缺陷中的一个。DSOD是微小的Void缺陷,存在于OSF区域。由于是微小的Void缺陷,因此无法通过选择蚀刻等而被观测到。DSOD (Direct Surface Oxide Defect, Direct Surface Oxide Defect) is also one of the Void defects. DSODs are tiny void defects that exist in the OSF region. Since it is a minute void defect, it cannot be observed by selective etching or the like.
DSOD评价通过使氧化膜生长在晶片上并在其上进行Cu装饰来检测出缺陷。DSOD evaluation detects defects by growing an oxide film on a wafer and performing Cu decoration on it.
另一方面,在侵入型硅占优势的情况下,形成凝聚有侵入型硅的晶体缺陷。其真面目虽不明确但认为是位错环等,巨大缺陷作为位错环团簇而被TEM(TransmissionElectron Microscopy,透射电子显微镜技术)观察到。On the other hand, when the intrusive silicon is dominant, a crystal defect in which the intrusive silicon is aggregated is formed. Although its true identity is not clear, it is considered to be a dislocation loop or the like, and the huge defect is observed by TEM (Transmission Electron Microscopy, transmission electron microscopy) as a cluster of dislocation loops.
该侵入型硅的原生缺陷,是通过与FPD相同的蚀刻法,即通过在选择蚀刻液内不摇动样品而将其放置比较长时间,作为贝壳状的大凹坑而被观察到的。这被称为LEP(Large EtchPit,大腐蚀陷斑)。The primary defects of the intrusive silicon were observed as large conchoidal pits by the same etching method as that of FPD, that is, by leaving the sample in a selective etching solution for a relatively long period of time without shaking it. This is called LEP (Large EtchPit).
将这些位错环、位错环团簇以及LEP统称为L/DL(Large Dislocation Loop,大位错环)。These dislocation loops, dislocation loop clusters and LEPs are collectively referred to as L/DL (Large Dislocation Loop, large dislocation loop).
[3]硅块的品质判定方法[3] Quality judgment method of silicon block
根据图2所示的流程图对本实施方式的硅块的品质判定方法进行说明。本实施方式的硅块的品质判定程序能够通过将硅块的品质判定程序安装到计算机中来执行。The quality determination method of the silicon block of the present embodiment will be described with reference to the flowchart shown in FIG. 2 . The quality determination program of the silicon block of the present embodiment can be executed by installing the quality determination program of the silicon block in a computer.
利用提拉装置1制造出单晶硅10(步骤S1)后,进行单晶硅10的外周磨削后,以线锯等切断成多个硅块10A、10B、10C(参考图4,例示了分割成3块的情况,但也可以是4块以上,也可以是2块以下)。此时,同时从硅块10A、10B、10C各自的两端切出样品晶片SW1、SW2、SW3、SW4,对样品晶片SW1、SW2、SW3、SW4各自进行品质评价。另外,样品晶片SW2是硅块10A与硅块10B的共通样品,样品晶片SW3是硅块10B与硅块10C的共通样品。After the single crystal silicon 10 is produced by the pulling device 1 (step S1 ), the outer periphery of the single crystal silicon 10 is ground, and then cut into a plurality of
品质评价结束后,将样品晶片SW1、SW2、SW3、SW4各自的品质评价结果读取到计算机中(步骤S2)。After the quality evaluation is completed, the quality evaluation results of each of the sample wafers SW1, SW2, SW3, and SW4 are read into the computer (step S2).
并且,将提拉单晶硅10时的制造实际数据也读取到计算机中(步骤S3)。In addition, the actual manufacturing data when the single crystal silicon 10 is pulled are also read into the computer (step S3).
计算机判定品质评价结果中是否存在显示L/DL不良或Void不良的样品晶片SW1、SW2、SW3、SW4(步骤S4)。关于L/DL不良的判定,在样品晶片SW1、SW2、SW3、SW4中,只要有一处产生L/DL,则判定为L/DL不良。并且,关于是否为Viod不良的判定,在样品晶片SW1、SW2、SW3、SW4中被检测出的Void缺陷为规定的数目以上,例如100个/片以上的情况下判定为不良。在L/DL不良或Void不良均未发生的情况下,进入到步骤S6。The computer determines whether or not there are sample wafers SW1 , SW2 , SW3 , and SW4 showing L/DL failure or Void failure in the quality evaluation results (step S4 ). Regarding the determination of L/DL failure, if L/DL occurred at one of the sample wafers SW1 , SW2 , SW3 , and SW4 , the L/DL failure was determined. In addition, regarding the determination of whether or not it is a Viod defect, when the number of Void defects detected in the sample wafers SW1 , SW2 , SW3 , and SW4 is a predetermined number or more, for example, 100 or more per wafer, it is determined to be a defect. When neither L/DL failure nor Void failure occurs, the process proceeds to step S6.
在存在显示L/DL不良或Void不良的样品晶片SW1、SW2、SW3、SW4的情况下,从送往下一个工序的硅块中排除切出该样品晶片SW1、SW2、SW3、SW4的硅块10A、10B、10C(步骤S5)。If there are sample wafers SW1, SW2, SW3, and SW4 showing L/DL failure or Void failure, the silicon ingot from which the sample wafers SW1, SW2, SW3, and SW4 are cut out is excluded from the silicon ingot to be sent to the next process. 10A, 10B, 10C (step S5).
计算机从品质评价结果中计算出能够取得目标品质的提拉管理范围(步骤S6)。在此,如图3所示,样品晶片SW1、SW2、SW3、SW4的品质根据提拉速度而发生变化。具体而言,在提拉速度快的情况下,产生空洞的凝聚体即Void。另一方面,在提拉速度慢的情况下,晶格间硅原子变得过剩,产生晶格间硅的凝聚体即L/DL。From the quality evaluation result, the computer calculates the pulling control range in which the target quality can be obtained (step S6 ). Here, as shown in FIG. 3 , the qualities of the sample wafers SW1 , SW2 , SW3 , and SW4 vary depending on the pulling speed. Specifically, when the pulling speed is high, a void, which is an aggregate of voids, is generated. On the other hand, when the pulling rate is slow, the amount of inter-lattice silicon atoms becomes excessive, and L/DL, which is an aggregate of inter-lattice silicon, is generated.
本实施方式的提拉速度是对提拉速度进行移动平均化而得的值,是指与图3的右图的缺陷分布具有最高相关性的移动平均速度。例如,能够采用50分钟至200分钟的范围内的时间移动平均速度。反过来说,在50分钟至200分钟的范围内,通常存在相关性最高的时间移动平均速度。The pulling speed of the present embodiment is a value obtained by performing a moving average of the pulling speed, and refers to a moving average speed having the highest correlation with the defect distribution in the right graph of FIG. 3 . For example, a time moving average speed in the range of 50 minutes to 200 minutes can be employed. Conversely, in the range of 50 minutes to 200 minutes, there is usually a time moving average speed with the highest correlation.
本实施方式中,虽然将提拉速度作为管理范围的指标,但并不限定于此,在检测出单晶硅10的直体直径并将其控制为一定的情况下,也可以适用本发明。In this embodiment, the pulling speed is used as an index of the management range, but it is not limited to this, and the present invention can also be applied when the diameter of the straight body of the single crystal silicon 10 is detected and controlled to be constant.
在产生Void的区域与产生L/DL的区域之间,存在Pv区域、Pi区域这两个无缺陷区域。There are two defect-free regions, the Pv region and the Pi region, between the Void region and the L/DL region.
Pv区域是指,在as-grown(生长)的状态下含有氧析出核,实施低温与高温(例如800℃与1000℃)的2阶段热处理时容易产生氧析出物的区域。Pi区域是指,在生长的状态下几乎不含有氧析出核,即使实施热处理也难以产生氧析出物的区域。The Pv region refers to a region that contains oxygen precipitation nuclei in an as-grown (grown) state and is prone to generate oxygen precipitates when a two-stage heat treatment of low temperature and high temperature (eg, 800° C. and 1000° C.) is performed. The Pi region refers to a region in which almost no oxygen precipitation nuclei are contained in the as-grown state, and it is difficult to generate oxygen precipitates even if heat treatment is performed.
关于Pv区域或Pi区域的区域判定,由于评价热处理后的氧析出物的析出状态,因此Pv区域或Pi区域的判定结果受到氧浓度的影响。其结果,后述的无缺陷范围以及新管理线受到氧浓度的影响。Regarding the determination of the Pv region or the Pi region, since the precipitation state of the oxygen precipitates after the heat treatment is evaluated, the determination result of the Pv region or the Pi region is affected by the oxygen concentration. As a result, the defect-free range and the new management line described later are affected by the oxygen concentration.
无缺陷区域是以OSF区域支配的晶体生长速度及L/DL区域支配的晶体生长速度之间的晶体生长速度形成,由空洞优势区域(Pv区域)及晶格间硅优势区域(Pi区域)构成。The defect-free region is formed at a crystal growth rate between the crystal growth rate dominated by the OSF region and the crystal growth rate dominated by the L/DL region, and is composed of a cavity dominant region (Pv region) and an interlattice silicon dominant region (Pi region) .
以无缺陷区域的晶体生长速度提拉的无缺陷晶体可以说是COP或位错团簇等的原生缺陷不存在或者极少的良质的单晶硅。因此,利用无缺陷区域下的晶体生长速度进行单晶硅的提拉控制,在确保单晶硅的品质这点上相当重要。The defect-free crystal pulled at the crystal growth rate of the defect-free region can be said to be a good-quality single crystal silicon with no or very few primary defects such as COP and dislocation clusters. Therefore, it is important to control the pull-up of the single-crystal silicon using the crystal growth rate in the defect-free region in order to ensure the quality of the single-crystal silicon.
本实施方式中,如图3所示,在产生Void的区域与产生L/DL的区域之间,根据被采取的样品晶片SW1、SW2、SW3、SW4的Pv区域、Pi区域,即无缺陷区域的存在,设定成为提拉管理范围的提拉速度范围。In this embodiment, as shown in FIG. 3 , between the region where Void occurs and the region where L/DL occurs, there are Pv regions and Pi regions of sampled wafers SW1 , SW2 , SW3 , and SW4 , that is, defect-free regions. exists, and set the pull-up speed range that becomes the pull-up management range.
在图3的情况下,成为无缺陷区域的提拉速度范围,成为无缺陷区域中央的提拉速度(理想的提拉速度的目标值)的5%。In the case of FIG. 3 , the range of the pulling speed of the defect-free region is 5% of the pulling speed in the center of the defect-free region (target value of the ideal pulling speed).
具体而言,进行样品晶片SW1、SW2、SW3、SW4的缺陷分布评价,对照这些晶片面内的Pv区域及Pi区域所呈的图样与在图3左侧示出的缺陷分布及提拉速度的关系,由此能够掌握实际的提拉速度相对于无缺陷区域上限(OSF区域与Pv区域的边界)的提拉速度的范围(以下,称为上侧无缺陷范围)以及实际的提拉速度相对于无缺陷区域下限(Pi区域与L/DL区域的边界)的提拉速度的范围(以下,称为下侧无缺陷范围)。Specifically, the defect distribution evaluation of the sample wafers SW1, SW2, SW3, and SW4 was performed, and the pattern of the Pv region and Pi region in the wafer plane was compared with the defect distribution and the pulling speed shown on the left side of FIG. 3 . The relationship between the actual pulling speed and the upper limit of the defect-free region (the boundary between the OSF region and the Pv region) can be grasped (hereinafter, referred to as the upper defect-free range) and the actual pulling speed relative to the range of the pulling speed. The range of the pulling speed at the lower limit of the defect-free area (the boundary between the Pi area and the L/DL area) (hereinafter, referred to as the lower defect-free area).
即,在实际的提拉速度接近无缺陷区域上限(OSF区域与Pv区域的边界)的情况下,将上侧无缺陷范围设定为较小,将下侧无缺陷范围设定为较大。另一方面,在接近无缺陷区域下限(Pi区域与L/DL区域的边界)的情况下,将上侧无缺陷范围设定为较大,将下侧无缺陷范围设定为较小。That is, when the actual pulling speed is close to the upper limit of the defect-free region (the boundary between the OSF region and the Pv region), the upper defect-free range is set to be small, and the lower defect-free range is set to be larger. On the other hand, when approaching the lower limit of the defect-free region (the boundary between the Pi region and the L/DL region), the upper defect-free range is set larger, and the lower defect-free range is set smaller.
例如,本实施方式中,在只有Pv区域的样品晶片SW1的情况下,上侧无缺陷范围被设定为提拉速度的目标值的0.5%,下侧无缺陷范围被设定为提拉速度的目标值的4.5%。For example, in the present embodiment, in the case of the sample wafer SW1 having only the Pv region, the upper defect-free range is set to 0.5% of the target value of the pulling speed, and the lower defect-free range is set to the pulling speed 4.5% of the target value.
同样地,在样品晶片SW2的情况下,上侧无缺陷范围被设定为2.5%,下侧无缺陷范围被设定为2.5%,在样品晶片SW3的情况下,上侧无缺陷范围被设定为3%,下侧无缺陷范围被设定为2%,在样品晶片SW4的情况下,上侧无缺陷范围被设定为4.8%,下侧无缺陷范围被设定为0.2%。Similarly, in the case of the sample wafer SW2, the upper defect-free range is set to 2.5%, the lower defect-free range is set to 2.5%, and in the case of the sample wafer SW3, the upper defect-free range is set to 3%, the lower defect-free range was set to 2%, and in the case of the sample wafer SW4, the upper defect-free range was set to 4.8%, and the lower defect-free range was set to 0.2%.
在样品晶片SW1、SW2、SW3、SW4产生规定数目以上的Void的情况下、产生L/DL的情况下,不需要设定提拉管理范围,将产生的硅块10A、10B、10C作为不良品排除。When the sample wafers SW1, SW2, SW3, and SW4 generate a predetermined number or more of voids, or when L/DL occurs, it is not necessary to set a pull-up management range, and the generated
接着返回到图2中,根据提拉管理范围来设定新管理线(步骤S7)。具体而言,从硅块两端的硅晶片的缺陷分布评价结果,掌握实际的提拉速度下的上侧无缺陷范围以及下侧无缺陷范围。接着,掌握对应于无缺陷区域的中央的提拉速度(理想的速度的目标值)。Next, returning to FIG. 2, a new management line is set according to the pull-up management range (step S7). Specifically, from the evaluation result of the defect distribution of the silicon wafers at both ends of the silicon block, the upper defect-free range and the lower defect-free range at the actual pulling speed are grasped. Next, the pulling speed (target value of the ideal speed) corresponding to the center of the defect-free region is grasped.
关于硅块的内部,将连接硅块两端的无缺陷区域上限彼此的线设定为上侧的新管理线,将连接硅块两端的无缺陷区域下限彼此的线设定为下侧的新管理线。在图4(B)中,虽然以直线设定上限的新管理线以及下限的新管理线,但并不限定于此。With regard to the inside of the silicon block, the line connecting the upper limits of the defect-free areas at both ends of the silicon block is set as the new management line on the upper side, and the line connecting the lower limits of the defect-free areas at both ends of the silicon block is set as the new management line on the lower side. Wire. In FIG. 4(B) , the new management line of the upper limit and the new management line of the lower limit are set as straight lines, but it is not limited to this.
接着,返回到图2中,计算机进行提拉实际数据与提拉管理范围的对照(步骤S8)。Next, returning to FIG. 2, the computer compares the actual pulling data and the pulling management range (step S8).
如图4(A)所示,以往的提拉速度的管理线相对于提拉速度的目标值,均等地设定于Void侧区域及L/DL侧区域,在提拉速度实际值超过该以往管理线的情况下,判定该硅块10A、10B、10C为不良品。As shown in FIG. 4(A) , the management line of the conventional pulling speed is set equally in the Void side area and the L/DL side area with respect to the target value of the pulling speed, and the actual value of the pulling speed exceeds the conventional value. In the case of a management line, the silicon blocks 10A, 10B, and 10C are determined to be defective products.
相对于此,如图4(B)所示,关于本实施方式的提拉速度的新管理线,根据所取得的样品晶片SW1、SW2、SW3、SW4的评价结果变更提拉速度的管理线。On the other hand, as shown in FIG. 4(B) , regarding the new management line of the pulling speed of the present embodiment, the management line of the pulling speed is changed according to the evaluation results of the obtained sample wafers SW1 , SW2 , SW3 , and SW4 .
其结果,如图4(B)所示,在以往的管理线下被判定为良品的硅块10B,在本实施方式的提拉速度的新管理线下,被判定为有不良风险(步骤S9)。As a result, as shown in FIG. 4(B) , the
在被判定为有不良风险的情况下,排除硅块10B,在下一个工序中,将被排除的硅块10B分割为多个晶片,再进行评价(步骤S10)。另外,还可以直接废弃被判定为有不良风险的硅块10B。When it is judged that there is a risk of failure, the
在被判定为没有不良风险的情况下,将硅块10B排出到下一个工序中。When it is judged that there is no risk of failure, the
在利用计算机的硅块10A、10B、10C的品质判定方法结束的情况下,在进行下一个单晶硅10的提拉时,根据所计算出的提拉速度的新管理线,进行单晶硅10的提拉控制。When the method for judging the quality of the silicon blocks 10A, 10B, and 10C using the computer is completed, when the next pulling of the single crystal silicon 10 is performed, the single crystal silicon is subjected to a new management line based on the calculated pulling speed. 10 lift controls.
[4]实施方式的作用及效果[4] Action and effect of the embodiment
如此,根据本实施方式,根据已进行品质评价的样品晶片SW1、SW2、SW3、SW4计算出提拉速度的管理新线。因此,即使是以往被判定为非不良的硅块10B,也会被判定为有不良的风险,所以能够降低将不良的硅块10B送到下一个工序中的可能性,并能够降低下一个工序中的品质确认的频度。In this way, according to the present embodiment, a new line for managing the pull-up speed is calculated from the sample wafers SW1 , SW2 , SW3 , and SW4 that have been subjected to quality evaluation. Therefore, even if the
在计算提拉速度的管理新线之前,通过进行L/DL判定以及Void判定,能够预先排出明显不良的硅块10A、10B、10C,因此能够预先排除不良品来更加降低下一个工序中的品质确认频度。By performing L/DL judgment and Void judgment before calculating the new line of management of the pulling speed, obviously
将图2所示的连续的流程图所涉及的硅块的品质判定方法,作为计算机上的程序来执行,由此能够促进自动化,因此能够减轻品质管理工序本身的负担。By executing the quality determination method of the silicon block according to the continuous flow chart shown in FIG. 2 as a program on a computer, automation can be promoted, and the burden of the quality control process itself can be reduced.
根据对每个硅块10A、10B、10C设定的提拉速度的新管理线,控制单晶硅10的提拉,由此能够防止产生品质不合格的硅块10A、10B、10C来减少不合格品的产生。By controlling the pulling of the single crystal silicon 10 according to the new management line of the pulling speed set for each
实施例Example
接着,对本发明的实施例进行说明。另外,本发明并不限定于实施例。Next, the Example of this invention is demonstrated. In addition, this invention is not limited to an Example.
关于被排出的硅块10B,将其分割为多个晶片并对每个晶片进行评价的结果得到图5所示的结果。The results shown in FIG. 5 were obtained as a result of dividing the discharged
在以以往管理线来进行管理的情况下,在提拉实际在Void侧取得峰值的情况以及在L/DL侧取得峰值的情况下,进行品质评价,并进行了良品、不良品的判定。In the case of managing with the conventional management line, when the lift actually obtained a peak value on the Void side and when the peak value was obtained on the L/DL side, quality evaluation was performed, and a good product and a bad product were judged.
另一方面,在以新管理线进行管理的情况下,进行了提拉实际超过新管理线的A1区域以及A2区域的晶片W1的良品、不良品的判定。On the other hand, when the new management line is used for management, the determination of the good and bad products of the wafer W1 actually pulled beyond the A1 area and the A2 area actually exceeds the new management line.
在A1区域的晶片W1的Void的分布图中,确认到在晶片W1的周围产生了环状的Void。In the Void distribution diagram of the wafer W1 in the A1 area, it was confirmed that a ring-shaped Void was generated around the wafer W1.
在A2区域的晶片W1的Void的分布图中,确认到在晶片W2的中央与周围产生了环状的Void。In the Void distribution diagram of the wafer W1 in the A2 area, it was confirmed that a ring-shaped void was generated in the center and the periphery of the wafer W2.
对其他部分进行判定的结果,如图6所示,在A3区域产生了L/DL,在A4区域及A5区域产生了Void。As a result of the determination of other parts, as shown in FIG. 6 , L/DL was generated in the A3 area, and Void was generated in the A4 area and the A5 area.
将硅块10B的品质评价的结果示于表1中。在以往方法的情况下,如果不评价取得提拉实际的峰值的所有晶片的品质,则无法抽出不良的部分。Table 1 shows the results of the quality evaluation of the
另一方面,在实施例的情况下,仅对提拉实际超过新管理线的A1区域至A5区域的晶片进行评价。将结果示于表1中。On the other hand, in the case of the example, only the wafers that were actually pulled beyond the new management line from the A1 area to the A5 area were evaluated. The results are shown in Table 1.
[表1][Table 1]
在以往方法中,对809片样品进行品质评价,发现了22片不良品。In the conventional method, 809 pieces of samples were evaluated for quality, and 22 pieces of defective products were found.
另一方面,在实施例中,376片样品进行品质评价,发现与以往方法相同的22片不良品。On the other hand, in the examples, 376 samples were evaluated for quality, and 22 defective samples were found to be the same as the conventional method.
从该结果能够确认到,通过执行基于本实施例的新管理线的品质判定方法,在已排出的硅块10B中,能够大幅地削减要再次进行品质评价的晶片的片数,能够降低下一个工序的品质评价频度。From this result, it was confirmed that by executing the quality determination method based on the new management line of the present example, the number of wafers to be re-evaluated for quality among the discharged silicon blocks 10B can be greatly reduced, and the next step can be reduced. The quality evaluation frequency of the process.
附图标记说明Description of reference numerals
1-提拉装置,2-腔室,3-坩埚,3A-石英坩埚,3B-石墨坩埚,4-支承轴,5A-加热器、5B-加热器,6-绝热材料,7-提拉轴,8-籽晶,9-硅熔液,10-单晶硅,10A-硅块、10B-硅块、10C-硅块,12-热屏蔽体,13-气体导入口,14-排气口,SW1-样品晶片、SW2-样品晶片、SW3-样品晶片、SW4-样品晶片,W1-晶片。1-pulling device, 2-chamber, 3-crucible, 3A-quartz crucible, 3B-graphite crucible, 4-support shaft, 5A-heater, 5B-heater, 6-insulation material, 7-pulling shaft , 8-seed crystal, 9-silicon melt, 10-single crystal silicon, 10A-silicon block, 10B-silicon block, 10C-silicon block, 12-heat shield, 13-gas inlet, 14-exhaust port , SW1-sample wafer, SW2-sample wafer, SW3-sample wafer, SW4-sample wafer, W1-wafer.
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| CN114897402A (en) * | 2022-05-26 | 2022-08-12 | 西安奕斯伟材料科技有限公司 | Crystal bar manufacturing management method and crystal bar manufacturing management system |
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| US11618971B2 (en) * | 2020-09-29 | 2023-04-04 | Sumco Corporation | Method and apparatus for manufacturing defect-free monocrystalline silicon crystal |
| JP7375716B2 (en) * | 2020-09-30 | 2023-11-08 | 株式会社Sumco | Quality evaluation method for crystal defects in single crystal silicon blocks, quality evaluation program for single crystal silicon blocks, method for manufacturing single crystal silicon blocks, and method for manufacturing silicon wafers |
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| JP5204415B2 (en) * | 2006-03-03 | 2013-06-05 | 国立大学法人 新潟大学 | Method for producing Si single crystal ingot by CZ method |
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| US20080302295A1 (en) * | 2004-08-04 | 2008-12-11 | Toshirou Kotooka | Method of Evaluating Quality of Silicon Single Crystal |
| CN101466876A (en) * | 2006-06-09 | 2009-06-24 | 上睦可株式会社 | COP Evaluation Method of Single Crystal Wafer |
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| CN114577757A (en) * | 2020-11-18 | 2022-06-03 | 苏州阿特斯阳光电力科技有限公司 | Method and system for evaluating quality of single crystal-like crystal |
| CN114897402A (en) * | 2022-05-26 | 2022-08-12 | 西安奕斯伟材料科技有限公司 | Crystal bar manufacturing management method and crystal bar manufacturing management system |
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