JP2016074574A - Measuring method of distance between lower end surface of heat-shielding member and surface of raw material melt and manufacturing method of silicon single crystal - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a measuring method capable of stably and accurately measuring the DPM at lower cost.SOLUTION: Provided is a measuring method of distance between the lower end surface of a heat-shielding member and the surface of raw material melt in pulling of a silicon single crystal using the Czochralski method, in which: before pulling of the silicon single crystal, a tool having a virtual surface of the raw material melt is provided, a position of a mirror image of a reference reflector reflected on the virtual surface of the raw material melt is measured, and a relationship between the distance between the mirror image and the reference reflector and the distance between the lower end surface of the heat-shielding member and the virtual surface of the raw material melt, is obtained; and during pulling of the silicon single crystal, a position of the mirror image of the reference reflector reflected on the surface of the raw material melt is measured, and on the basis of the relationship between the distance between the mirror image of the reference reflector and the reference reflector and the distance between the lower end surface of the heat-shielding member and the virtual surface of the raw material melt, the distance between the lower end surface of the heat-shielding member and the surface of the raw material melt is calculated.SELECTED DRAWING: Figure 1

Description

  The present invention relates to a method for measuring a distance between a lower surface of a heat shield member disposed above a raw material melt surface and a raw material melt surface when pulling up a silicon single crystal from the raw material melt in a crucible by the Czochralski method. And a silicon single crystal manufacturing method for pulling up the silicon single crystal by controlling the distance.

  As a method for producing a silicon single crystal used for a semiconductor substrate, the Czochralski method (CZ method) in which the silicon single crystal is pulled up while growing from a raw material melt in a quartz crucible is widely adopted. Further, for the purpose of reducing the oxygen concentration of a silicon single crystal and easily manufacturing a large-diameter crystal, the MCZ method is widely known in which a silicon single crystal is pulled up by a CZ method while applying a magnetic field.

  In the CZ method, a seed crystal is immersed in a raw material melt (silicon melt) in a quartz crucible under an inert gas atmosphere, and a silicon single crystal having a desired diameter is grown by pulling up the quartz crucible and the seed crystal while rotating. In the MCZ method, a silicon single crystal is grown by the CZ method while applying a magnetic field to the raw material melt in the quartz crucible.

  In recent years, with the progress of high integration of semiconductor devices and the accompanying miniaturization, growth defects (grown-in defects) in silicon wafers have become a problem as a cause of deterioration in characteristics of semiconductor devices. As such grown-in defects, octahedral void-like defects, which are aggregates of vacancies in a silicon single crystal by the CZ method, and dislocation clusters formed as aggregates of interstitial silicon are known. .

  It is known that the amount of these grown-in defects is determined by the crystal temperature gradient at the growth interface of the silicon single crystal and the growth rate of the silicon single crystal, and by controlling these with high precision, There is known a manufacturing method for obtaining a defect-free crystal over the entire surface in the radial direction.

  Specifically, as a means for suppressing the grown-in defects, a structure (shielding) that blocks the cylindrical or inverted conical radiant heat around the silicon single crystal grown above the raw material melt surface for controlling the crystal temperature gradient. A heat member is provided. Furthermore, in order to obtain defect-free crystals, it is necessary to control the temperature gradient of the crystal with high precision. For this purpose, the heat shielding member located above the liquid surface of the raw material melt (raw material melt surface) and the raw material melt surface. It is necessary to control the distance (hereinafter also referred to as DPM) to the predetermined distance with a very high accuracy.

JP 2007-290906 A JP 2008-195545 A

  However, in recent years, as the diameter of the silicon single crystal to be grown increases, the position of the raw material melt surface changes greatly due to the thickness error of the quartz crucible, deformation during operation, etc. There is a problem that it changes every growing batch and during crystal growing. For this reason, it is increasingly difficult to control the DPM so as to be a predetermined distance with high accuracy.

  In order to solve this problem, for example, in Patent Document 1, a reference reflector is disposed in a furnace, and the relative position of the mirror image reflected on the reference reflector and the raw material melt surface is measured. The distance between the raw material melt surfaces is measured. In this measurement, a real image of the reference reflector and a mirror image of the reference reflector reflected on the raw material melt surface are captured by a detection means such as an optical camera, and the captured real image of the reference reflector and the reflected image on the raw material melt surface are reflected. The brightness of the mirror image of the reference reflector is determined by determining a certain threshold value (binarization level threshold value) and quantizing it into two output values (binarization process).

  By the way, it is the distance between the heat shield member lower end surface and the raw material melt surface that greatly affects the grown-in defect of the silicon single crystal. In the conventional measurement method described above, the position of the raw material melt surface is the same. Even if the temperature can be measured with high accuracy, the distance between the bottom surface of the heat shield member and the melt surface of the material is the heat generated by the manufacturing dimension error of the heat shield member and the difference in thermal expansion coefficient of the material used for the heat shield member Since there is a difference in expansion, it can be measured only with the relative value for each batch of pulling silicon single crystals. For this reason, the distance between the heat shield member lower end surface and the raw material melt surface cannot be accurately controlled to be a desired distance. As a result, it becomes impossible to manufacture a silicon single crystal of desired quality with high productivity.

  In order to solve such a problem, in Patent Document 2, a protrusion whose length has been measured is disposed on the lower end surface of the heat shield member, and the crucible containing the raw material melt is raised to raise the raw material melt surface. A method is disclosed in which the protrusion is brought into contact with the protrusion and the contact is electrically detected instantaneously. According to this method, the distance between the lower end surface of the heat shield member and the raw material melt surface at the time of contact detection is equal to the length of the protrusion measured in advance. The distance between the actual heat shield member lower end surface and the raw material melt surface can be accurately measured. And by calibrating the measurement result of the relative position of the above-described real image of the reference reflector and the mirror image reflected on the raw material melt surface by the distance between the heat shield member lower end surface and the raw material melt surface at this time, It can eliminate the influence of thermal expansion difference caused by manufacturing dimensional error of heat shield member and difference of thermal expansion coefficient of the material used for heat shield member. The distance between the liquid level can be measured. As a result, it is possible to accurately control a desired distance between the lower end surface of the heat shield member and the raw material melt surface, and to produce a silicon single crystal having a desired quality with high productivity.

  However, this method requires an apparatus that electrically detects contact between the protrusions disposed at the lower end of the heat shield member and the raw material melt surface for each single crystal manufacturing apparatus. Generally, a single crystal manufacturing apparatus is constituted by a water-cooled stainless steel chamber, and an in-furnace member disposed in the chamber is constituted by a graphite member. Since these are conductors, in order to electrically detect the contact between the projections arranged at the lower end of the heat shield member and the raw material melt surface, it is necessary to insulate the circuit constituting them from other in-furnace members and chambers. There is. Therefore, in order to perform this method, a contact detection device is installed for each manufacturing device, a circuit for detecting contact between the protrusion disposed at the lower end of the heat shield member and the raw material melt surface, other in-furnace members, and Large-scale modifications to insulate the chamber or new introduction of a single crystal manufacturing apparatus having an insulating structure are required, resulting in a very high apparatus cost.

  In addition, after starting the pulling of the silicon single crystal, when the raw material silicon polycrystal and the protrusions arranged at the lower end of the heat shield member unexpectedly contact with each other during the melting of the raw material silicon polycrystal, the protrusions were damaged or dissolved. When the raw material melt scatters and adheres to the projection, the length of the projection changes from the actually measured value. In this case, this method makes it impossible to accurately measure the distance between the lower end of the heat shield member and the raw material melt surface. As a result, the distance between the real image of the reference reflector disposed on the heat shield member and the mirror image of the reference reflector reflected on the raw material melt surface is the distance between the lower end surface of the heat shield member and the raw material melt surface. Since it cannot be calibrated with actual measurement values and cannot be controlled to have a desired distance with high accuracy, a silicon single crystal having a desired quality cannot be manufactured with high productivity.

  The present invention has been made in view of the above-described problems, and an object thereof is to provide a measurement method capable of measuring DPM stably and accurately at a lower cost. In addition, the present invention is based on the DPM measured by such a measurement method, and by appropriately controlling the DPM during pulling of the silicon single crystal, the silicon single crystal that can reliably obtain a defect-free crystal entirely. Another object is to provide a manufacturing method.

  In order to achieve the above object, the present invention provides a reference reflector at the lower end of the heat shield member located above the raw material melt surface when pulling up the silicon single crystal from the raw material melt in the crucible by the Czochralski method. And a method of measuring a distance between the lower end surface of the heat shield member and the raw material melt surface, wherein the mirror image of the reference reflector can be reflected before starting to pull up the silicon single crystal. A jig provided with a raw material melt surface is provided so that the virtual raw material melt surface is located below the heat shield member, and the position of the mirror image of the reference reflector reflected on the virtual raw material melt surface is a fixed point measuring machine The distance between the mirror image of the reference reflector and the reference reflector is calculated from the measured position of the mirror image of the reference reflector, and the mirror image of the reference reflector and the reference reflector are calculated. The distance between the heat shield member lower end surface and the virtual raw material melt surface In the measurement of the distance between the lower end surface of the heat shield part and the raw material melt surface during pulling of the silicon single crystal, the fixed point measuring machine is used to obtain the raw material melt surface. Measuring the position of the mirror image of the reference reflector reflected in the above, the distance between the determined mirror image of the reference reflector and the reference reflector, the bottom surface of the heat shield member, and the virtual raw material melt surface Calculating the distance between the bottom surface of the heat shield member and the raw material melt surface from the position of the mirror image of the reference reflector reflected on the raw material melt surface Provided is a method for measuring a distance between a heat shield member lower end surface and a raw material melt surface.

  With such a measuring method, accurate measurement is possible without being affected by the manufacturing dimension error of the heat shield member and the change in DPM due to thermal expansion. In addition, since the present invention calibrates the DPM based on the measured value measured using a jig provided with a virtual raw material melt surface that is regarded as the raw material melt surface before pulling up the silicon single crystal, the silicon single crystal is not necessarily used. There is no need to arrange a measuring device or the like for DPM calibration in the apparatus being pulled up. Accordingly, there is almost no risk of deformation or damage due to contact with the raw material melt of these measuring devices, and stable measurement can be performed. Furthermore, since it is not necessary to significantly modify the single crystal manufacturing apparatus, accurate measurement can be performed at low cost. Here, the “reference reflector” in the present invention reflects a mirror image on the raw material melt surface, and the distance between the heat shield member lower end surface and the raw material melt surface is observed by observing this mirror image. And the position of the raw material melt surface can be controlled.

  At this time, as a jig provided with the virtual raw material melt surface, a measuring instrument for measuring a distance between the virtual raw material melt surface and the lower surface of the heat shield member is used. It is preferable to actually measure the distance between the heat shield member lower end surface and the virtual raw material melt surface.

  In this way, the measuring instrument provided in the above jig can efficiently calculate the distance between the mirror image of the reference reflector and the reference reflector and the distance between the lower surface of the heat shield member and the virtual raw material melt surface simultaneously. Can measure well.

  At this time, a mirror can be used as the virtual raw material melt surface.

  In the present invention, it is preferable to use a mirror to project a mirror image of the reference reflector.

  At this time, the reference reflector can be made of any one of high-purity quartz, silicon, and carbon.

  If any of these is used as the reference reflector, the heat resistance is high, and even if the reference reflector comes into contact with the raw material melt, the contamination of the raw material melt is suppressed. Can do.

  At this time, the relationship between the distance between the mirror image of the reference reflector and the reference reflector and the distance between the lower surface of the heat shield member and the virtual raw material melt surface is two different heights. It can obtain | require by measuring the position of the mirror image of the said reference | standard reflector in the said virtual raw material melt surface.

  In the present invention, between the virtual raw material melt surfaces of two different levels of height, the position of the mirror image of the reference reflector reflected on each virtual raw material melt surface is used to determine the gap between the mirror image of the reference reflector and the reference reflector. By obtaining the relationship between the distance between the heat shield member lower end surface and the distance between the virtual raw material melt surface, accurate DPM can be reliably measured when the silicon single crystal is pulled up. .

  Further, the present invention provides the heat shield member lower end surface and the raw material melt based on the distance between the heat shield member lower end surface and the raw material melt surface measured by any one of the methods described above. Provided is a method for producing a silicon single crystal characterized by pulling up the silicon single crystal by the Czochralski method while controlling the distance between the surfaces.

  With such a manufacturing method, based on the highly accurate DPM measured by the DPM measuring method of the present invention, the DPM during pulling of the silicon single crystal can be appropriately controlled, and a defect-free crystal can be obtained with certainty. it can. In addition, the silicon single crystal manufacturing apparatus does not need to be significantly modified, and the apparatus cost can be reduced as compared with the conventional apparatus. Therefore, a high-quality silicon single crystal can be manufactured at low cost.

  With the DPM measuring method of the present invention, accurate measurement is possible without being affected by the manufacturing dimension error of the heat shield member and the DPM change due to thermal expansion. Further, the present invention calibrates the DPM using a jig having a virtual material melt surface before pulling up the silicon single crystal. There is no need to provide a measuring device or the like, and there is almost no risk of deformation or breakage due to contact with the raw material melt of these measuring devices, so that stable measurement can be performed. Furthermore, since it is not necessary to significantly modify the single crystal manufacturing apparatus, accurate measurement can be performed at low cost. Moreover, the silicon single crystal manufacturing method of the present invention can reliably manufacture a high-quality silicon single crystal at a low cost.

In this invention, it is a figure explaining the measuring method between a thermal-insulation member lower end surface and a virtual raw material melt surface with the jig | tool provided with the virtual raw material melt surface, (a) is a 1st level virtual raw material The figure which shows the measurement state of melt surface height, (b) is the schematic of the image obtained with the fixed point measuring device at that time, (c) is the figure which shows the measurement state of the virtual raw material melt surface of the 2nd level, ( d) is a schematic view of an image obtained by the fixed point measuring machine at that time. In Example 1, it is the schematic at the time of pulling up a silicon single crystal, using the measuring method of DPM of the present invention. 1 is a schematic view of a silicon single crystal produced in Example 1. FIG. In the comparative example 1, it is the schematic at the time of pulling up a silicon single crystal, using the measuring method of the conventional DPM. 2 is a schematic view of a silicon single crystal manufactured in Comparative Example 1. FIG.

  Hereinafter, although an embodiment is described about the present invention, the present invention is not limited to this.

  As described above, in the conventional DPM measurement method, the measurement of DPM is not affected by the difference in thermal expansion caused by the manufacturing dimension error of the heat shield member or the difference in thermal expansion coefficient of the material used for the heat shield member. In order to accurately perform the above, there is a problem that the manufacturing apparatus needs to be greatly modified, resulting in high costs. Furthermore, in the conventional method, it is necessary to arrange a measuring device for calibrating the DPM in the device during the pulling of the silicon single crystal, and deformation or breakage due to contact with the raw material melt of the measuring device occurs. Therefore, there is a problem that measurement cannot be performed stably.

  The present inventors have made studies in order to solve the above problems, and have come up with the following measurement method of the present invention. In the present invention, first, a single crystal provided with a virtual raw material melt surface below the heat shield member lower end surface when setting the in-furnace member in the chamber of the single crystal manufacturing apparatus before pulling up the silicon single crystal. Install a jig that is detachable from the manufacturing equipment. Then, at the same time as measuring the distance from the virtual raw material melt surface to the bottom surface of the heat shield member at the same time, the real image of the reference reflector disposed on the heat shield member and the mirror image of the reference reflector reflected on the virtual raw material melt surface The image is captured by a fixed point measuring machine equipped with detection means such as an optical camera. Thereby, the distance between the reference reflector and the virtual raw material melt surface is calculated. Then, the relationship between the distance between the mirror image of the reference reflector and the reference reflector and the distance between the lower surface of the heat shield member and the virtual raw material melt surface is obtained. In calculating the DPM at the time of actually pulling up the silicon single crystal, the DPM value is calibrated based on the previously obtained distance relationship with respect to the DPM value obtained by measurement with a fixed point measuring machine. .

  According to the present invention, a protrusion having a known length is disposed on the lower end surface of the heat shield member, and the distance between the heat shield member and the raw material melt surface is detected by detecting contact between the protrusion and the raw material melt surface. Is measured with the measured value, and the distance between the real image of the reference reflector arranged on the heat shield member and the mirror image of the reference reflector reflected on the raw material melt surface is calibrated with the same accuracy as the method of calibrating. The distance between the heat shield member lower end surface and the raw material melt surface during crystal pulling can be measured. Furthermore, it is not necessary to modify the insulation of the apparatus for electrically detecting the contact between the protrusion disposed at the lower end of the heat shield member for each single crystal manufacturing apparatus and the raw material melt surface and the single crystal manufacturing apparatus, and the apparatus cost can be reduced. In addition, after the start of the silicon single crystal pulling operation, the accidental phenomenon that the distance between the heat shield and the raw material melt surface cannot be measured accurately due to deformation or breakage of the measuring device (projection, etc.) is eliminated. it can.

  Hereinafter, embodiments of the present invention will be specifically described with reference to FIGS. FIG. 1 illustrates a method for measuring the distance between the lower end surface of the heat shield member 11 and the virtual raw material melt surface 22 by using a jig 21 having a virtual raw material melt surface in the present invention. It is a figure to do. FIG. 2 is a schematic diagram of a silicon single crystal manufacturing apparatus 30 when pulling up a silicon single crystal using the method for measuring the distance between the lower end surface of the heat shield member 11 and the raw material melt surface of the present invention. It is.

  As shown in FIG. 2, the single crystal manufacturing apparatus 30 includes a main chamber 1 that houses a member such as a quartz crucible 5, a pulling chamber 2 that is continuously fixed on the main chamber 1, and a temperature gradient of the silicon single crystal. And a cylindrical gas rectifying cylinder 10 having an opening through which the silicon single crystal 3 is conducted, and a heater 7 for heating and melting the raw material silicon polycrystal. Further, the single crystal manufacturing apparatus 30 is configured such that heat from the magnet 13 that applies a magnetic field to the raw material melt 4 during the pulling of the silicon single crystal, the graphite crucible 6 that supports the quartz crucible 5, and the heater 7 enters the main chamber 1. A heat insulating material 8 for preventing direct radiation, a pulling wire 18 and a seed crystal 9 for pulling up the silicon single crystal 3, a crucible shaft 12 for supporting the crucibles 5, 6, and the heights of the crucibles 5, 6 A position control device 17 is provided.

  In the DMP measuring method of the present invention, first, in the silicon single crystal manufacturing apparatus 30 as shown in FIG. 2, before the pulling of the silicon single crystal 3 from the raw material melt 4 in the crucibles 5 and 6 is started by the CZ method. When the in-furnace member is set in the silicon single crystal manufacturing apparatus 30 (at normal temperature and normal pressure), the reference reflector 14 is disposed at the lower end of the heat shield member 11 as shown in FIG.

  In the present invention, the reference reflector 14 can be made of any one of high-purity quartz, silicon, and carbon. If any of these is used as the reference reflector 14, even if the reference reflector 14 contacts the raw material melt 4, impurity contamination of the raw material melt 4 can be suppressed.

  Next, as shown in FIG. 1, a jig 21 having a virtual raw material melt surface 22 that can reflect a mirror image of the reference reflector 14 is positioned below the heat shield member 11. Provided.

  At this time, a mirror can be used as the virtual raw material melt surface 22. If a mirror is used as the virtual raw material melt surface 22, a simple configuration can be obtained.

  In the present invention, a jig 21 having a measuring instrument such as a depth gauge 23 for measuring the distance between the virtual raw material melt surface 22 and the lower end surface of the heat shielding member 11 is used, and the heat shielding is performed by the measuring instrument. The distance between the lower end surface of the member and the virtual raw material melt surface can be actually measured. In this way, the distance between the mirror image of the reference reflector 14 and the reference reflector 14 and the distance between the lower end surface of the heat shield member 11 and the virtual raw material melt surface 22 can be measured simultaneously.

  Next, as shown in FIG. 1, the distance A between the virtual raw material melt surface 22 and the lower end surface of the heat shield member 11 is measured with a measuring instrument or the like provided in the jig 21.

  Next, as shown in FIG. 1B, the positions of the real image 24 of the reference reflector 14 and the mirror image 25 of the reference reflector 14 reflected on the virtual raw material melt surface 22 are shown in FIG. Measurement is performed by a fixed point measuring machine 15 such as an optical camera fixed to the main chamber 1 or the like shown in a). Then, as shown in FIG. 1 (b), from the measured position of the mirror image 25 of the reference reflector 14, for example, a measurement arithmetic unit 16 comprising the image processing device shown in FIG. 1 (a) is used. The distance B between the real image 24 of the reference reflector 14 and the mirror image 25 of the reference reflector 14 reflected on the virtual raw material melt surface 22 is calculated. These distance A and distance B are recorded.

  Then, the relationship between the distance B between the mirror image 25 of the reference reflector 14 and the reference reflector 14 obtained in this way and the distance A between the heat shield member lower end surface and the virtual raw material melt surface is obtained. .

  At this time, the relationship between the distance between the mirror image 25 of the reference reflector 14 and the reference reflector 14 and the distance between the lower end surface of the heat shield member 11 and the virtual raw material melt surface 22 is two different high levels. This can be obtained by measuring the position of the mirror image 25 of the reference reflector 14 on the virtual raw material melt surface 22.

  Specifically, the position of the virtual raw material melt surface 22 of the jig 21 in the height direction is changed as shown in FIG. 1C, and the virtual raw material melt surface is changed by the same method as described above. The distance A ′ between 22 and the lower end surface of the heat shield member 11 is measured. Next, as shown in FIG. 1 (d), between the real image 24 of the reference reflector 14 arranged at the lower end of the heat shield member 11 and the mirror image 25 of the reference reflector 14 reflected on the virtual raw material melt surface 22. The distance B ′ is measured by the same method as described above. These distances A ′ and B ′ are recorded.

And from the recorded distance A, distance A ′, distance B, distance B ′, for example, the lower end surface of the heat shield member 11 when the virtual raw material melt surface 22 changes to an arbitrary position in the height direction. The distance L1 between the virtual raw material melt surface 22 and the virtual raw material melt surface 22 is a real image 24 of the reference reflector 14 disposed at the lower end of the heat shield member 11 and a mirror image 25 of the reference reflector 14 reflected by the virtual raw material melt surface 22. If the distance L2 between is measured,
L1 = {(AA ′) / (BB ′)} × L2 Expression (1)
Can be obtained.

  Thereby, even if there is a dimensional individual difference due to a manufacturing error in the heat shield member 11, the method of the present invention obtains the distance between the lower end surface of the heat shield member 11 and the virtual raw material melt surface 22 by actual measurement. The influence of individual differences in the dimensions of the heat shield member 11 is eliminated. Therefore, even if there is a dimensional individual difference in the heat shield member 11, according to the method of the present invention, the distance L1 between the lower end surface of the heat shield member 11 and the virtual raw material melt surface 22 at an arbitrary height position is Accurately required.

  Next, a case where the present invention is used when actually pulling up a silicon single crystal from a raw material melt in a crucible by the CZ method as shown in FIG. 2 will be described. Hereinafter, the MCZ method in which the silicon single crystal is pulled up while applying a magnetic field to the raw material melt in the crucible will be described as an example.

  The silicon single crystal is pulled up by heating and melting the raw material silicon polycrystal filled in the quartz crucible 5 with a heater 7 disposed around it to form the raw material melt 4, and then immersing the seed crystal 9 in the raw material melt 4. The quartz single crystal 3 having a desired diameter is grown by pulling up the quartz crucible 5 and the seed crystal 9 while applying a magnetic field to the raw material melt 4 by the magnet 13. In the meantime, it is necessary to continuously heat the furnace of the silicon single crystal manufacturing apparatus 30 with the heater 7 so that the raw material melt 4 in the quartz crucible 5 does not re-solidify, and the furnace is usually kept at a high temperature of 1500 to 1600 ° C. Kept.

  As a result, the size of the heat shield member 11 disposed in the furnace of the silicon single crystal manufacturing apparatus 30 changes due to thermal expansion. In addition, changes in the dimensions of the heat shield member 11 due to thermal expansion are not uniform due to individual differences in the coefficient of thermal expansion of the material used for the heat shield member 11. Therefore, the position of the lower end surface of the heat shield member 11 in the height direction changes from the normal temperature and normal pressure before the silicon single crystal 3 is pulled up.

  However, the position change in the height direction of the reference reflector 14 during the actual pulling of the silicon single crystal is caused by the position change in the height direction of the heat shield member 11 because the reference reflector 14 is provided on the heat shield member 11. Is equal to

  Therefore, the distance between the real image of the reference reflector 14 captured by the fixed point measuring machine 15 and the mirror image of the reference reflector 14 reflected on the raw material melt surface is measured in advance at normal temperature and normal pressure before pulling the silicon single crystal. The crucibles 5 and 6 are moved so that the distance B is between the recorded real image 24 of the reference reflector 14 and the mirror image 25 of the reference reflector 14 reflected on the virtual raw material melt surface 22. If the surfaces are matched, the distance between the lower end surface of the heat shield member 11 and the raw material melt surface at that time is below the heat shield member 11 measured and recorded at normal temperature and normal pressure before pulling the silicon single crystal. It becomes equal to the distance A between the end surface and the virtual raw material melt surface 22.

  Similarly, the crucible is moved so that the distance between the real image of the reference reflector 14 and the mirror image of the reference reflector 14 reflected on the raw material melt surface becomes the distance B ′ described above, and the raw material melt surface is changed. If it puts together, the distance between the lower end surface of the thermal-insulation member 11 at that time and raw material melt surface will become equal to the distance A 'mentioned above.

This is because the actual image of the reference reflector 14 disposed at the lower end of the heat shield member 11 and the reference reflection reflected on the raw material melt surface even during the pulling of the actual silicon single crystal that continues to be exposed to high temperatures in the furnace. If the distance L2 ′ between the mirror image of the body 14 is measured, the distance L1 ′ between the end surface of the lower heat shield member 11 at that time and the raw material melt surface of the raw material melt 4 is expressed by the above formula (1). Similarly,
L1 ′ = (AA ′) / (BB ′) × L2 ′ Expression (1) ′
Means that it is required.

  Therefore, the distances A and A between the lower end surface of the heat shield member 11 and the virtual raw material melt surface 22 are obtained using a jig provided with the virtual raw material melt surface 22 at room temperature and normal pressure before pulling the silicon single crystal. Measurement and recording of 'and measurement of distances B and B' between the real image of the reference reflector 14 captured by the fixed point measuring instrument 15 and the mirror image of the reference reflector 14 reflected on the virtual raw material melt surface 22 From the measurement result of the distance L2 ′ between the actual image of the reference reflector 14 after starting the actual silicon single crystal pulling and the mirror image of the reference reflector reflected on the raw material melt surface by performing the recording. The distance L1 ′ between the lower end surface of the heat shield member 11 and the raw material melt surface at that time can be accurately obtained.

  In the present invention, based on the distance between the heat shield member lower end surface and the raw material melt surface measured by the method of the present invention as described above, the heat shield member lower end surface and the raw material melt surface The silicon single crystal can be pulled up by the Czochralski method while controlling the distance between them.

  By this silicon single crystal manufacturing method, the distance L2 ′ between the real image of the reference reflector captured by the fixed point measuring machine and the mirror image of the reference reflector reflected on the raw material melt surface is set to the height position of the crucibles 5 and 6. If the actual silicon single crystal pulling is performed while controlling to a desired distance by the control device 17 or the like, the distance L1 ′ between the lower end surface of the heat shield member and the raw material melt surface becomes a desired distance. Quality silicon single crystals can be manufactured with high productivity.

  EXAMPLES Hereinafter, the present invention will be described more specifically with reference to examples and comparative examples of the present invention, but the present invention is not limited to these examples.

Example 1
The reference reflector 14 was first attached to the lower end of the heat shield member 11 using the silicon single crystal manufacturing apparatus 30 shown in FIG. The reference reflector 14 was a transparent quartz rod with white quartz attached to the tip. Next, similarly to FIG. 1A, the pulling chamber 2 has a mirror-made virtual raw material melt surface 22 capable of changing the position in the height direction, and a heat shielding member is formed from the virtual raw material melt surface 22. A jig 21 equipped with a depth gauge 23 for measuring the distance to the lower end surface of 11 was attached.

  As a result of measuring the distance A between the virtual raw material melt surface 22 and the lower end surface of the heat shield member 11 with the depth gauge 23 at this time, it was 20 mm. At the same time, the reference reflection reflected on the real image 24 of the reference reflector 14 and the virtual raw material melt surface 22 by the fixed point measuring device 15 comprising an optical camera fixed to the pulling chamber 2 and the measurement arithmetic device 16 comprising an image processing device. It was 5 mm as a result of measuring the distance B with the mirror image 25 of the body 14.

  Next, similar to (c) of FIG. 1, the same measurement was performed with the height of the virtual raw material melt surface 22 lowered. At this time, the distance A ′ between the virtual raw material melt surface 22 and the lower end surface of the heat shield member 11 is 40 mm, and the real image 24 of the reference reflector 14 and the reference reflector 14 reflected by the virtual raw material melt surface 22 are reflected. The distance B ′ between the mirror image 25 was 10 mm.

From this result, the distance L1 between the lower end surface of the heat shield member 11 and the virtual raw material melt surface 22 is the reference reflector measured by the fixed point measuring machine 15 as in the above formulas (1) and (1) ′. From the distance L2 between the real image 24 of 14 and the mirror image 25 of the reference reflector 14 reflected on the virtual raw material melt surface 22,
L1 = 4 × L2
It is represented by Therefore, for example, in order to set the distance L1 ′ between the lower end surface of the heat shield member 11 and the raw material melt surface during actual pulling of the silicon single crystal to 30 mm, the reference reflector 14 measured with a fixed point measuring machine It was calculated that the distance L2 ′ between the mirror image of the reference reflector 14 reflected on the raw material melt surface may be set to 7.5 mm and controlled.

  After the above measurement, an actual silicon single crystal pulling operation was performed. First, 340 kg of raw material silicon polycrystal was filled in a quartz crucible 5 having a diameter of 800 mm, which was heated and melted by a heater 7 to form a raw material melt 4, and then a horizontal magnetic field having a central magnetic field strength of 4000 G was applied by a magnet 13.

  Thereafter, the crucible shaft 12 is slowly raised, and the distance L2 ′ between the real image of the reference reflector 14 captured by the fixed point measuring machine 15 and the mirror image of the reference reflector 14 reflected on the raw material melt surface is 7.5 mm. Moved until.

  Thereafter, the silicon single crystal 3 was pulled up while controlling the distance L2 'between the real image of the reference reflector 14 and the mirror image of the reference reflector 14 reflected on the raw material melt surface to be 7.5 mm. As a result, as shown in FIG. 3, defect-free crystals were obtained over almost the entire region.

  From this result, using the measuring jig 21 provided with the virtual raw material melt surface 22, before the silicon single crystal pulling operation, the virtual raw material melt surface 22 having a two-level height and the lower end surface of the heat shield member 11 are obtained. And the actual image 24 of the reference reflector 14 disposed on the heat shield member 11 captured by the fixed point measuring instrument 15 at that time and the mirror image of the reference reflector 14 reflected on the raw material melt surface. The actual image of the reference reflector 14 captured by the fixed point measuring machine 15 during actual pulling of the silicon single crystal and the raw material melt The distance L1 ′ between the lower end surface of the heat shield member 11 and the raw material melt surface can be stably and accurately measured and controlled from the measurement result of the distance L2 ′ between the mirror image of the reference reflector 14 reflected on the surface. I understand that. Furthermore, with the measurement method of the present invention, it is not necessary to significantly modify the apparatus, and the apparatus cost can be kept low.

(Comparative Example 1)
A conventional DPM measurement method was used in pulling a silicon single crystal using the silicon single crystal manufacturing apparatus 130 shown in FIG. First, the protrusion 119 and the reference reflector 114 were attached to the lower end of the heat shield member 111. In order to use the conventional DPM measurement method, the silicon single crystal manufacturing apparatus 130 of FIG. 4 is in contact with the silicon single crystal manufacturing apparatus 30 of FIG. An electrically measuring instrument 120 and a part constituting an electric circuit from the heat shield member 111 of the silicon single crystal manufacturing apparatus to the measuring instrument 120 through the projection 119, the raw material melt 104, and the crucible shaft 112 are other parts. Remodeling was performed on the chamber of the silicon single crystal manufacturing equipment. As the reference reflector 114, a transparent quartz rod with white quartz attached to the tip was used. As the protrusion 119, a silicon single crystal cut into a conical shape and etched and washed with a mirror-like surface was used. Further, the protrusion 119 is set to be shorter than the set distance between the lower end surface of the heat shielding member 111 and the raw material melt surface during pulling up the silicon single crystal 103 and longer than the reference reflector 114, As a result of actually measuring the length of the protrusion 119 protruding from the lower end surface of the heat shield member 111, it was 20 mm.

  After the above measurement, an actual silicon single crystal pulling operation was performed. First, a quartz crucible 105 having a diameter of 800 mm was filled with 340 kg of raw material silicon polycrystal, heated and melted by a heater 107 to form a raw material melt 104, and then a horizontal magnetic field having a central magnetic field strength of 4000 G was applied by a magnet 113.

  Thereafter, the crucible shaft 112 was slowly raised and moved until the protrusion 119 attached to the lower end of the heat shield member 111 was in contact with the raw material melt surface. The contact between the raw material melt and the protrusion 119 was detected by the measuring instrument 120 that electricity flowed from the heat shield member 111 to the crucible shaft 112. At this time, the distance between the lower end surface of the heat shield member 111 and the raw material melt surface at the moment of sensing is the actually measured length of 20 mm of the portion of the protrusion 119 protruding from the lower end surface of the heat shield member 111. . Further, the distance between the real image of the reference reflector 114 at this time and the mirror image of the reference reflector 114 reflected on the raw material melt surface was measured by the fixed point measuring instrument 115, and the result was 5 mm.

  Next, the crucible shaft 112 was lowered by 10 mm, and the set distance L1 'between the lower end surface of the heat shield member 111 and the raw material melt surface at the time of pulling the silicon single crystal was adjusted to 30 mm. The distance L2 'between the real image of the reference reflector 114 at this time and the mirror image of the reference reflector 114 reflected on the raw material melt surface was measured by the fixed point measuring instrument 115, and the result was 7.5 mm.

  Thereafter, the silicon single crystal 103 was pulled up while controlling the distance L2 ′ between the real image of the reference reflector 114 and the mirror image of the reference reflector 114 reflected on the raw material melt surface to be 7.5 mm. . As a result, as shown in FIG. 5, a defect-free crystal was obtained over almost the entire region. As described above, in Comparative Example 1, defect-free crystals were obtained over almost the entire region as in Example 1. However, since the device needs to be remodeled, the device cost compared to Example 1 was increased. Will rise. Further, in the case of this method, the protrusion 119 is unexpectedly brought into contact with the raw material silicon polycrystal while the raw material silicon polycrystal is melted, and the protrusion is damaged, or the melted raw material melt is scattered to cause the protrusion. As a result, the length of the protrusion may change from the actually measured value, and accurate measurement may not be possible.

  Thus, when cost and the simplicity and stability of measurement are taken into consideration, it can be seen that the DPM measurement method of the present invention and the silicon single crystal manufacturing method using the same are superior.

  The present invention is not limited to the above embodiment. The above-described embodiment is an exemplification, and the present invention has any configuration that has substantially the same configuration as the technical idea described in the claims of the present invention and that exhibits the same effects. Are included in the technical scope.

1 ... main chamber, 2 ... pulling chamber, 3 ... silicon single crystal,
4 ... Raw material melt, 5 ... Quartz crucible, 6 ... Graphite crucible,
7 ... heater, 8 ... heat insulating material, 9 ... seed crystal,
10 ... Gas flow straightening cylinder, 11 ... Heat shield member, 12 ... Crucible shaft,
13 ... Magnet, 14 ... Reference reflector, 15 ... Fixed point measuring machine,
16 ... Measurement operation device, 17 ... Crucible position control device, 18 ... Pull-up wire,
21 ... Jig, 22 ... Virtual raw material melt surface, 23 ... Depth gauge,
24: Real image of a reference reflector obtained by a fixed point measuring machine,
25: Mirror image of a reference reflector obtained with a fixed point measuring machine,
30 ... Silicon single crystal production apparatus A ... Actual distance between heat shield member lower end surface and virtual raw material melt surface,
A ′: The measured distance between the bottom surface of the heat shield member and the virtual raw material melt surface after changing the height of the virtual raw material melt surface,
B: Distance between the real image and the mirror image of the reference reflector,
B ′: Distance between the real image and the mirror image of the reference reflector after changing the height of the virtual raw material melt surface

Claims (6)

When pulling up the silicon single crystal from the raw material melt in the crucible by the Czochralski method, a reference reflector is provided at the lower end of the heat shield member located above the raw material melt surface, and the lower surface of the heat shield member and the raw material melt A method for measuring the distance between surfaces,
Before starting the pulling of the silicon single crystal, a jig provided with a virtual raw material melt surface capable of reflecting a mirror image of the reference reflector is positioned below the heat shield member. So that
The position of the mirror image of the reference reflector reflected on the melt surface of the virtual raw material is measured with a fixed point measuring machine, and the mirror image of the reference reflector and the reference reflector are determined from the measured mirror image position of the reference reflector. Calculate the distance between
Obtain the relationship between the mirror image of the reference reflector and the reference reflector, and the distance between the heat shield member lower end surface and the virtual raw material melt surface,
In the measurement of the distance between the heat shield lower end surface and the raw material melt surface during the pulling of the silicon single crystal, the position of the mirror image of the reference reflector reflected on the raw material melt surface is measured by the fixed point measuring machine. Measure and
Based on the relationship between the determined distance between the mirror image of the reference reflector and the reference reflector and the distance between the lower surface of the heat shield member and the virtual raw material melt surface, the raw material melt is obtained. Calculating the distance between the lower end surface of the heat shield member and the raw material melt surface from the position of the mirror image of the reference reflector reflected on the liquid surface; How to measure the distance between.   As a jig provided with the virtual raw material melt surface, a jig provided with a measuring device for measuring the distance between the virtual raw material melt surface and the bottom surface of the heat shield member is used. The method for measuring the distance between the lower end surface of the heat shield member and the raw material melt surface according to claim 1, wherein the distance between the lower end surface of the heat member and the virtual raw material melt surface is actually measured.   The method for measuring the distance between the lower end surface of the heat shield member and the raw material melt surface according to claim 1 or 2, wherein a mirror is used as the virtual raw material melt surface.   4. The heat shield member lower end surface according to claim 1, wherein the reference reflector is made of any one of high-purity quartz, silicon, and carbon. 5. A method for measuring the distance between the raw material melt surface.   The relationship between the distance between the mirror image of the reference reflector and the reference reflector and the distance between the lower end surface of the heat shield member and the virtual material melt surface is two different levels of the virtual material. It calculates | requires by measuring the position of the mirror image of the said reference | standard reflector in a melt surface, The heat-shielding member lower end surface of any one of Claims 1-4, a raw material melt surface, How to measure the distance between.   The said heat shield member lower end surface and the said raw material based on the distance between the said heat shield member lower end surface and the said raw material melt surface measured by the method of any one of Claims 1-5. A method for producing a silicon single crystal, wherein the silicon single crystal is pulled up by a Czochralski method while controlling a distance from a melt surface.

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