JP5978722B2 - Silicon seed crystal manufacturing method, silicon single crystal manufacturing method - Google Patents

Description

  The present invention relates to a silicon seed crystal manufacturing method used when a silicon single crystal is manufactured by a CZ (Czochralski) method and a technique suitable for use in a silicon single crystal manufacturing method using the seed crystal.

  In silicon single crystal production by the Czochralski method, a single crystal is produced by a pulling process in which a silicon seed crystal is immersed in a silicon melt in a crystal growth furnace and then grown to a target size. Usually, when a silicon seed crystal is immersed in a silicon melt, dislocations that are crystal defects are generated around the immersed portion. The main cause of dislocation generation is considered to be thermal stress caused by the temperature difference between the seed crystal and the silicon melt before and after being immersed in the melt. In the production of silicon single crystals, it is essential to prevent the occurrence of dislocations or to eliminate dislocations. Conventionally, as a means of removing dislocations generated during immersion, the seed crystal diameter is reduced after immersion to reduce the crystal diameter. Dash necking that forms the aperture is performed. By this dash necking, the diameter of the aperture that can be made dislocation-free is about 4 mm. If the diameter is larger than that, it becomes difficult to completely remove the dislocation.

  Considering the strength of silicon that supports a single crystal that has become heavier with the increase in the diameter of a silicon single crystal in recent years, there is a risk of fracture when the diameter of the aperture is 4 mm. Therefore, in order to manufacture a single crystal without forming a narrowed portion due to necking, which is a problem in terms of silicon strength, the treatment state of the landing surface of the silicon seed crystal is controlled to enable dislocations during the growth of the silicon single crystal. A technique for preventing and enlarging the aperture diameter is described in Patent Document 1.

  Similarly, Patent Documents 2 and 3 describe techniques for enlarging the diameter of the diaphragm by defining the etching amount of the liquid landing surface of the seed crystal and by regulating the boron concentration in the seed crystal.

Japanese Patent Laid-Open No. 2002-187795 JP 2003-192488 A Japanese Patent Laid-Open No. 07-265643

  However, the seed crystal may break at a position above the liquid landing part, that is, at the position where the original seed crystal diameter is maintained, rather than the reduced diameter part of the dash neck that is a problem in the prior art. As a result, high-frequency crystals with a diameter of 300 mm or more have been pulled up, and the frequency of breakage has increased. Judging from the fracture position, this is considered to be caused by other causes regardless of the lack of strength due to the reduced diameter for dislocation elimination. Therefore, there has been a demand to prevent such seed crystal breakage that occurs even when the narrowed portion is not formed.

  The present invention has been made in view of the above circumstances, and intends to achieve the object of preventing breakage of a silicon seed crystal in response to an increase in the weight of a single crystal to be pulled up.

A seed crystal for pulling a silicon single crystal by the Czochralski method is produced by cutting out an ingot pulled by a single crystal.
As shown in FIG. 1, the seed crystal T has a quadrangular prism shape or a cylindrical shape, and is attached to the seed chuck 5 with a diameter-expanding portion T1 for attachment to the seed chuck 5 described later. It consists of a columnar portion T2 extending downward from the attached enlarged diameter portion T1 and a liquid landing portion T3 located at the lower end opposite to the attached enlarged diameter portion T1 of the columnar portion T2. A single crystal pulled from the liquid landing part T3 is grown. In the figure, the neck portion N is also shown as a single crystal grown state.
The surface of the seed crystal T is subjected to a surface cleaning process such as etching in order to remove attached contaminants before being attached to the seed chuck 5 for lifting.

  Originally, when a single crystal to be pulled up to support large diameters of φ300 mm or more and φ450 mm or more becomes heavy, if the seed crystal diameter is reduced in the necking process, it may not be able to withstand the weight. Has been made. For example, it is conceivable to carry out a dislocation-free liquid deposition method for crystals having a weight that can be handled by a dash neck.

  Up to now, there has been a case where a fracture has occurred even if the weight is within a range that does not cause a problem in strength against the load. For example, it may be broken at the neck portion N, and it was confirmed that the breakage occurred due to the foreign matter attached in the subsequent inspection. In addition, there was an example in which stress was applied at the contact portion between the seed chuck 5 and the seed crystal T, and breakage was caused by a slip that entered the inside of the attachment enlarged diameter portion T1. Then, at the first stage of pulling up the single crystal, the work of “soaking” the seed crystal in silicon melt is carried out, but if the work is insufficient, it breaks due to the slip generated in the liquid landing part T3. There was a case to do. These three points could occur even if they were not heavy and could be expected to some extent. However, there has been a case where the columnar portion T2 that is not the neck portion N is broken after the weight is increased.

  Therefore, the inventors of the present application investigate and prevent the cause of the breakage occurring at the columnar part T2 processed and formed as the seed crystal 5 side where the breakage occurs from the liquid landing part T3, that is, the corresponding seed crystal T. It was decided to take measures.

  Of these seed crystals, the one that was broken in the crystal extraction step after the end of the pulling was analyzed, and the fracture surface was a brittle fracture type fracture surface of the shell pattern, and the origin was not the center of the cross section of the seed crystal, but the edge of the cross section. It was on the columnar side. Further, it was found that the seed (seed crystal) was not simply broken into two parts from this starting point but was complicatedly broken into more than three parts. Since the fracture starting point was in the vicinity of the surface of the columnar portion T2, it is considered that the possibility of fracture from a defect in the seed (seed crystal) base material is low.

  In addition, other seeds cut out from the same block as the seed base material were used in a plurality of crystal growth furnaces, but none of them caused breakage. If there is a cause in the single crystal that is the base material from which the seed crystal is cut out, it is possible that other seed crystals cut out in the same way may break, so that is not the case. The possibility of destruction from defects in the base metal is considered low.

  From the above fracture pattern, it was found that the fracture starting point was a single point near the surface of the columnar portion T2, and as a possible possibility, the melt attached to the seed (seed crystal) surface was splashed or oxidized near the surface. The case where there was a precipitate such as a material and these were the starting points of the breakage was examined. However, there was no evidence of splashing of the melt, and no precipitated oxide was detected at the break starting point.

  Next, the possibility that the breakage occurred due to the heat shock at the time of landing was considered. However, the starting point of the break is on the upper side (seed chuck 5 side) of the liquid landing part T3 that is the range where the slip enters from the liquid landing surface that is the end surface of the seed (seed crystal), and is caused by heat shock. It is unlikely that breakage occurred. Further, since the break starting point is on the seed chuck 5 side of the columnar portion T2, even if a slip due to a heat shock exists in the vicinity of the break starting point, the density is considered to be quite low. For this reason, if breakage occurs due to heat shock, the starting point is the liquid landing part T3, and it was determined that the breakage at the columnar part T2 targeted this time is not related.

In addition, for verification, the longitudinal cross section near the fracture starting point was confirmed by X-ray.
As a result, there were no defects such as dislocations and precipitates in the vicinity of the starting point where the fracture occurred. On the other hand, although dislocation occurred in the mounting enlarged diameter portion T1 that is in contact with the seed chuck 5 above the break starting point, this dislocation did not propagate to the break portion of the columnar portion T2. It is considered that the dislocation caused by contact with the seed chuck 5 does not lead to the cause of this breakage.

Next, the possibility of breakage due to scratches on the seed surface was considered.
Although the processed surface of the seed was observed, it was in a beautiful (mirror surface) state, and scratches could not be confirmed visually. Therefore, it is considered that there is a low possibility that scratches that can be visually observed exist. In addition, the fracture starting point is not caused by the scratch caused by the contact with the seed chuck 5, but not by the mounting enlarged diameter portion T <b> 1 whose diameter is increased to be held by the seed chuck 5.

However, silicon is a brittle material, and even scratches that are not visible can be the starting point of destruction. Therefore, fine surface processing scratches and grinding damage that are not visible to be introduced to the columnar side surface during seed (seed crystal) production are considered as one of the causes of breakage. Before attaching the seed crystal T to the seed chuck (holder) 5, it is visually confirmed that there are cracks, cracks, etc. However, since fine scratches etc. cannot be confirmed, it is attached as it is and the possibility of becoming the starting point of destruction Judged that there is.
Therefore, it came to the view that it was important to prepare seeds so that they would not remain.

  Based on this knowledge, the processing damage layer generated by grinding and grinding introduced into the columnar side surface during seed (seed crystal) production is quantified, and the damage layer is removed / reduced based on the information to prevent the occurrence of breakage. For the purpose of avoiding this, the present invention has been completed.

The method for producing a silicon seed crystal of the present invention is a method for producing a silicon seed crystal used by being attached to a seed chuck when producing a silicon single crystal by the Czochralski method,
A processing step of cutting out from a silicon single crystal to form a columnar silicon seed crystal;
The weight of the silicon single crystal to be pulled up by eliminating the remaining surface scratches and the surface processing damage layer on the columnar side surface of the columnar portion on the seed chuck side with respect to the liquid landing portion located on the lower end portion of the silicon seed crystal In order to maintain the strength that can maintain the surface processing damage layer removal step,
In the silicon seed crystal side surface, a measurement step of measuring whether a scratch on the processing surface or a surface processing damage layer is removed,
By solving this problem, the above-mentioned problems were solved.
In the present invention, it is more preferable that the damaged layer removing step includes an etching process.
The damaged layer removing step of the present invention can include two or more grinding processes having different grinding conditions before the etching process.
Further, in the present invention, as different grinding conditions in the grinding process, means having different grinding wheel roughness or means having different grinding wheel pressing conditions (abrasion amount) may be employed.
In the present invention, it is desirable that the measurement step includes an angle polishing process and a light etching process.
Furthermore, the measurement step may include a measurement process using high-energy radiated light (white X-ray topograph) that is an X-ray having a wavelength of 0.001 nm to 0.25 nm .
Further, the silicon single crystal to be pulled may be φ300 mm or more, or may be a silicon seed crystal in which the amount of raw material charge at the time of pulling is 300 kg or more.
In the present invention, when producing a silicon single crystal by the Czochralski method, a method for producing a silicon seed crystal used by being attached to a seed chuck,
A processing step of cutting out from a silicon single crystal to form a columnar silicon seed crystal;
The weight of the silicon single crystal to be pulled up by eliminating the remaining surface scratches and the surface processing damage layer on the columnar side surface of the columnar portion on the seed chuck side with respect to the liquid landing portion located on the lower end portion of the silicon seed crystal In order to maintain the strength that can maintain the surface processing damage layer removal step,
Can have.
In the method for producing a silicon single crystal of the present invention, it is preferable to pull up the silicon single crystal using a seed crystal for producing a silicon single crystal produced by any one of the production methods described above.
In the method for producing a silicon single crystal of the present invention, a damage layer removal determining step for determining whether the damaged layer is removed and having a required strength from the result measured in the measurement step;
A pulling step of pulling up the silicon single crystal using the seed crystal for silicon single crystal production produced by any one of the production methods described above;
Have
In the damage layer removal determining step, when it is determined that the surface processing damaged layer is removed, the silicon single crystal is pulled up as the pulling step, and it is determined that the surface processing damaged layer is not removed. In this case, it is possible to return to the surface processing damaged layer removal step.

The method for producing a silicon seed crystal of the present invention is a method for producing a silicon seed crystal used when producing a silicon single crystal by the Czochralski method,
A processing step of cutting out from a silicon single crystal to form a columnar silicon seed crystal;
Damage layer removing step for maintaining the strength capable of retaining the weight of the silicon single crystal to be pulled up by eliminating the scratches on the columnar side surface of the silicon seed crystal and the surface processing damage layer,
In the silicon seed crystal side surface, a measurement step of measuring whether a scratch on the processing surface or a surface processing damage layer is removed,
By removing the processing scratches and processing damage layer, the fine scratches that can be the starting point of the fracture are completely removed, the seed crystal is prevented from breaking and the weight of the silicon single crystal to be pulled up is maintained. Seed crystals can be produced that maintain the possible strength.

  In the present invention, the damage layer removing step includes an etching process, so that at the final stage of the damaged layer removing step, the processing scratch and the processing damage layer existing on the seed crystal surface without generating a new processing damage layer Can be removed.

  When the damaged layer removing step of the present invention includes two or more grinding processes having different grinding conditions before the etching process, the processing damaged layer can be removed in a short time and the final grinding process can be performed. It is possible to shorten the processing time of the etching process, which is a subsequent process for completely removing the necessary processing damage layer by changing the grinding conditions so as to reduce the generation of the processing damage layer at a stage. That is, it is possible to reduce grinding damage by changing the grinding wheel count under the grinding conditions in the seed forming process, and to measure the etching amount reduction after grinding accordingly. Specifically, the thickness of the processing damage layer existing before the etching treatment can be 50 μm or less, preferably 10 μm or less.

  Further, in the present invention, as the different grinding conditions in the grinding process, by adopting means having different grinding wheel roughness or means having different grinding wheel pressing conditions (cutting amount), grinding on the start side of the grinding process is performed. The processing conditions are such that the thickness that can be removed by the grinding process is given priority to allow the generation of a processing damage layer to some extent, and on the end side of the grinding process, there is a condition that reduces the generation of a new processing damage layer. can do. For this reason, the grinding wheel and the roughness of the stone are changed so as to increase from the processing start to the end side, or the grinding wheel pressing condition (cutting amount) is changed so as to decrease from the processing start to the end side. Means are possible. Specifically, when setting two grinding conditions, the grindstone count is set to start at # 140 and end at # 800, and the grinding stone pressing condition (shaving amount) starts at 5 mm. It can be set to end at 0.05 mm.

  Moreover, in this invention, a seed surface layer state evaluation can be performed by having the measurement process which measures whether the flaw of a processing surface or the surface processing damage layer is removed in the said silicon seed crystal side surface.

In the present invention, it is desirable that the measurement step includes an angle polishing process and a light etching process, and the angle polishing + light etching evaluation method performed in the wafer evaluation is performed as the seed surface layer evaluation.
Here, as shown in FIG. 2A, the sample is prepared by cutting out the surface layer portion of the columnar portion T2 so as to extend in the axial direction from the seed to be measured, as shown in FIGS. As shown in Fig. 4, the cut sample piece is angle-polished. At this time, the polishing angle can be set to 5 ° 44 ′. Thereafter, light etching with a 2HF: 2CH ₃ COOH: 1HNO ₃ : 1CrO ₃ [400 g / l] aqueous solution is performed to about 2 μm to emphasize the processing damage layer portion. This emphasized processing damage layer portion is observed with an optical microscope, and the depth of the processing damage layer is evaluated by measuring the range where damage exists.

Furthermore, the measurement process can include a measurement process using high-energy synchrotron radiation (white X-ray topograph) at a large synchrotron radiation facility (SPring-8), and thereby, whether there is a large strain on the order of 100 μm. Can be revealed.
As the high energy radiation for measurement at this time, it is preferable to use white X-ray topography by white X-rays. In particular, as white X-rays, 30 keV to 1 MeV having a continuous spectrum, about 40 to 100 keV, 50 The number of photons obtained through a slit of 1 mm × 1 mm at a position of a distance of 44 m from the light source has a distribution as shown in FIG. 1 at about 60 keV or X-ray having a wavelength of about 0.001 nm to 0.25 nm. It is supposed to be. FIG. 3 (a) shows an X-ray state as an example of the high-energy radiated light in the present invention, and shows the distribution of the number of photons with respect to the energy of the X-ray. FIG. 3 (a) Fig. 2 shows X-rays as an example of high-energy radiated light in the present invention, and shows the distribution of the number of photons with respect to wavelength.

  In addition, the silicon single crystal to be pulled is φ300 mm or more, or a silicon seed crystal whose raw material charge amount at the time of pulling is set to 300 kg or more, so that even if such a large load is applied, the columnar portion It can be set as the seed crystal which does not fracture | rupture from T2.

Furthermore, in the present invention, when it is determined that sufficient damage removal has been made based on the measurement data accumulated in the measurement process, the measurement process is omitted,
A processing step of cutting out from a silicon single crystal to form a columnar silicon seed crystal;
Damage layer removal step for maintaining the strength capable of retaining the weight of the silicon single crystal pulled up by eliminating the scratches on the columnar side surface of the silicon seed crystal and the surface processing damage layer,
By removing the processing scratches and processing damage layer, the fine scratches that can be the starting point of the fracture are completely removed, the seed crystal is prevented from breaking and the weight of the silicon single crystal to be pulled up is maintained. Seed crystals can be produced that maintain the possible strength.

  In the method for producing a silicon single crystal according to the present invention, the silicon single crystal is pulled up using the seed crystal for producing a silicon single crystal produced by any one of the production methods described above, so that the crystal falls due to the fracture of the seed crystal. Occurrence can be prevented.

  According to the present invention, it is possible to completely remove a processing scratch or a processing damage layer on the surface of a seed (seed crystal) to be used before growing a silicon single crystal. There is an effect that can be prevented.

It is a model front view which shows the silicon seed crystal used for manufacture of a silicon single crystal. The perspective view (a) which shows the cutting | disconnection of the sample (sample piece) in the case of angle polishing in one Embodiment of the manufacturing method of the silicon seed crystal based on this invention, (b) (c) is a model which shows the sample which carried out angle polishing FIG. It is a graph which shows the characteristic of high energy radiation light irradiation in 1st Embodiment of the manufacturing method of the silicon single crystal which concerns on this invention. It is a flowchart which shows one Embodiment of the manufacturing method of the silicon seed crystal which concerns on this invention. It is a schematic diagram which shows the pulling furnace in one Embodiment of the manufacturing method of the silicon single crystal which concerns on this invention. It is an image which shows the result of angle grinding concerning one embodiment of a manufacturing method of a silicon seed crystal concerning the present invention. It is an image which shows the result of angle grinding concerning one embodiment of a manufacturing method of a silicon seed crystal concerning the present invention.

Hereinafter, an embodiment of a method for producing a silicon seed crystal and a method for producing a silicon single crystal according to the present invention will be described with reference to the drawings.
FIG. 4 is a flowchart showing a method for producing a silicon seed crystal in the present embodiment.

  As shown in FIG. 4, the method for producing a silicon seed crystal in this embodiment includes a seed crystal formation processing step (processing step) S00 for cutting out from a silicon single crystal to form a rough shape as a seed crystal, and the silicon seed crystal. A damage layer removing step S10 for maintaining the strength capable of maintaining the weight of the silicon single crystal to be pulled up by eliminating the surface scratches and surface processing damage layers remaining on the columnar side surfaces of the substrate.

  In the single crystal formation processing step (processing step) S00, as shown in FIG. 1, a columnar portion T2 that is a substantially cylindrical or substantially polygonal column, and one end that is larger in diameter than the columnar portion T2, is a seed chuck 5 A process such as a grinding process is performed so as to obtain a shape having an attachment diameter-increased portion T1 for mounting and supporting, and a liquid landing portion T3 at the other end of the columnar portion T2. Therefore, a processing damage layer is formed on these surfaces.

  In the damaged layer removing step S10, a grinding step S11 for removing the damaged layer, a finish grinding step S12 for removing the damaged layer generated in the grinding step S11, and a damaged layer from at least the columnar portion T2 surface. And an etching process step S13 for removal.

  In the grinding step S11 and the finish grinding step S12, these grinding conditions are set to be different so that the thickness of the damaged layer is different. Specifically, in the grinding step S11, the main condition is to remove the surface of the seed crystal T in order to remove the damaged layer generated in the seed crystal formation processing step S00 which is the previous step. The finish grinding step S12 is set as a condition for simultaneously removing that the damaged layer generated in the grinding step S11 is removed and that a new damaged layer is not generated as much as possible.

  Specifically, as different grinding conditions in the grinding step S11 and the finish grinding step S12, the roughness of the grinding wheel can be different. For example, the grindstone count is # 140 in the grinding step S11, A higher count, # 400, # 800, etc. can be set.

Alternatively, as different grinding conditions in the grinding step S11 and the finish grinding step S12, the pressing condition (shaving amount) of the grinding wheel of the grinding wheel, that is, the cutting amount can be different. For example, the pressing condition of the grinding wheel is different in the grinding step S11. In the grinding amount 5 mm and the finish grinding step S12, a smaller grinding amount 0.5 mm, a grinding amount 0.05 mm or the like can be set.
Further, the grinding treatment step S11 can be performed a plurality of times regardless of whether or not the grinding conditions are changed.

  In the etching process S13, the columnar portion T2 can maintain the strength to support the pulled silicon single crystal that may be 300 kg or more by removing the processing damage layer remaining in the finish grinding process S12. Therefore, the etching conditions are set so as to remove at least the thickness of the columnar portion T2 surface that exceeds the thickness of the processing damage layer generated in the finish grinding step S12. Specifically, when the processing damage layer remaining after finishing the finishing grinding step S12 is about 10 μm, it is at least equal to or more than this thickness, specifically about 15 μm (± 4 μm), which is 50% higher. To about 500 μm, which is 50 times larger, the columnar bT2 surface is set to be removed by etching.

  Furthermore, in the method for producing a silicon seed crystal according to the present embodiment, in order to check whether the strength in the columnar portion T2 is maintained, as shown in FIG. It is possible to have a measurement step S20 for confirming that it does not remain on the surface of the columnar portion T2.

  The measurement step S20 is to measure whether the scratch on the processed surface or the surface processed damage layer has been removed. As shown in FIG. 4, the sample collection step S21 for angle polishing, the angle polishing process S22, and the light etching process S23 are performed. The damage layer measurement step S24 is included.

In the sample collection step S21 for angle polishing, as shown in FIG. 2A, the side surface of the columnar portion T2 is cut along a plane that tends to be an axis, and the thickness dimension t2 is formed on the radially outer side of the original columnar portion T2. However, sample T2a which is a thin piece which has curved surface T2b so that it may become 0.5-3 mm in the thickest part is extract | collected.
The axial length t1 in the original columnar portion T2 of the sample may be any length that allows angle polishing in a subsequent process, but is about 5 to 50 mm, preferably about 10 to 16 mm.

  Next, in the angle polishing process S22, as shown in FIGS. 2B and 2C, the monopolar surface T2b that is the outer peripheral surface of the columnar portion T2 is polished with a plane having an angle inclined in the axial direction from the cut surface. Thus, a polished surface T2c having a curved contour T2e such as a parabola is formed. At this time, the polishing angle can be about 5 °, for example, 5 ° 44 '.

Next, a region including the curved surface contour T2e in the vicinity of the center of the polishing surface Tc in the axial direction is defined as a measurement region T2d. Then, the depth distribution (whether or not it remains) of the processing damage layer due to grinding is measured by light etching the portion including the measurement region to emphasize the processing damage and observing the distribution state of the portion. . At this time, in the measurement region T2d, the maximum depth position (thickness) can be measured depending on the position in the axial direction from the curved contour T2e side.

Etchant in light _{etching, 2HF: 2CH 3 COOH: 1HNO} 3: as 1CrO 3 [400g / l] solution, as the etching conditions, the process preferably performed about 2μm to.

In addition, X-ray topograph measurement process S25 which is a measurement process by high energy radiation light can also be performed as a process damage layer presence / absence confirmation.
At this time, white X-rays having the energy distribution shown in FIG. 3 are irradiated as high-energy radiated light, and the diffracted X-rays are measured by, for example, a detection unit including a CCD having a predetermined performance.
In particular, the white X-ray is an X-ray having a continuous spectrum of 30 keV to 1 MeV, about 40 to 100 keV, about 50 to 60 keV, or a wavelength of about 0.001 nm to 0.25 nm, and a distance of 44 m from the light source. The number of photons obtained through a 1 mm × 1 mm slit at the position of FIG. 3 has a distribution as shown in FIG. FIG. 3A shows an X-ray state as an example of high-energy radiation in the present embodiment, and shows a distribution of the number of photons with respect to the energy of the X-ray. FIG. FIG. 2 shows X-rays as an example of high-energy radiation in the present embodiment, and shows the distribution of the number of photons with respect to wavelength.

The beam diameter is preferably 0.01 to 1 times the neck diameter of the object to be measured.
X-ray topography, also called X-ray diffraction microscopy, is a non-destructive method for observing the spatial distribution of defects. When continuous X-rays are incident on a single crystal, a plurality of diffraction images called diffraction spots are observed. Will be analyzed.

  Here, the two-dimensional detector used for observing the diffraction image includes a fluorescent plate, an X-ray film, a nuclear dry plate, an imaging plate using a photostimulable luminescence phenomenon of a stimulable phosphor (BaFBr: Eu2 +), and an X-ray. An X-ray television using an imaging tube having a PbO film or an amorphous Se-As film having a photoconductive surface as a photoconductive surface, a CCD X-ray detector using a charge coupled device CCD, or the like can also be used. For the X-ray detector of this embodiment, it is preferable to consider the following characteristics as the spatial resolution and dynamic range.

Detection quantum efficiency dynamic range
Intensity linearity region
Dead time and counting off
Photosensitive area and position resolution
Sensitivity non-uniformity Non-linearity (or image distortion)
Energy resolution Time resolution Real-time measurement capability Operational stability

  In the X-ray topograph measurement step S25, if no large strain of the order of 100 μm is observed by irradiation with synchrotron radiation (Spring-8), it can be determined that there is no processing damage layer.

  As shown in FIG. 4, the silicon seed crystal manufacturing method in the present embodiment determines whether or not the damaged layer is removed and has the required strength from the result measured in the measurement step S20. When it is determined in step S30 that the damaged layer has been removed, a pulling step S40 is performed in which the silicon single crystal is pulled using the corresponding silicon seed crystal T. If it is determined in the damaged layer removal determination step S30 that the damaged layer has not been removed, the process returns to the damaged layer removal step S10. In particular, if the remaining damage layer is thick enough to require grinding, the process returns to the grinding process S11. If the remaining damage layer is thick enough to require some grinding, the process returns to the finish grinding process S12, and the remaining damage If the layer does not require grinding, the process returns to the etching process step S13.

Thereby, the silicon seed crystal T having the columnar portion T2 having a required load strength without having a processing damage layer can be manufactured.
In addition, the surface treatment of the attachment enlarged diameter part T1 and the liquid landing part T3 can be appropriately performed according to the specifications. The damage layer removing step S10 for removing the processing damage layer for giving the load strength described in the present embodiment can be applied to these surfaces.

  In addition, after the preferable conditions in the damaged layer removal step S10 are set by adopting specific manufacturing conditions in the damaged layer removal determination step S30, the pulling step is performed without performing the measurement step S20 and the damaged layer removal determination step S30. It is also possible to pull a single crystal at S40.

Hereinafter, an embodiment of a method for producing a silicon single crystal according to the present invention will be described with reference to the drawings.
FIG. 5 is a schematic front view showing an apparatus for producing a silicon single crystal in the present embodiment. In the figure, reference numeral 1 denotes a quartz crucible.

The CZ furnace shown in FIG. 5 includes a crucible 1 disposed in the center of the chamber, a heater 2 disposed outside the crucible 1, and a magnetic field supply device 9 disposed outside the heater 2. . The crucible 1 has a double structure in which a quartz crucible 1a containing a silicon melt 3 inside is held by an outer graphite crucible 1b, and is rotated and moved up and down by a support shaft 1c called a pedestal.
A cylindrical heat shield 7 is provided above the crucible 1. The heat shield 7 has a structure in which an outer shell is made of graphite and the inside thereof is filled with graphite felt. The inner surface of the heat shield 7 is a tapered surface whose inner diameter gradually decreases from the upper end to the lower end. The upper outer surface of the heat shield 7 is a tapered surface corresponding to the inner surface, and the lower outer surface is formed in a substantially straight surface so as to gradually increase the thickness of the heat shield 7 downward.
Then, the silicon single crystal 6 can be formed by immersing the seed crystal T attached to the seed chuck 5 in the silicon melt 3 and pulling up the seed crystal T while rotating the crucible 1 and the pulling shaft 4. .

The heat shield 7 blocks the radiation heat from the heater 2 and the silicon melt 3 surface to the side surface of the silicon single crystal 6, surrounds the side surface of the growing silicon single crystal 6, and the silicon melt 3. It surrounds the surface. An example of the specification of the heat shield 7 is as follows.
The width W in the radial direction is, for example, 50 mm, the inclination θ with respect to the vertical direction of the inner surface that is the inverted truncated cone surface is, for example, 21 °, and the height H1 from the melt surface at the lower end of the heat shield 7 is 10-250 mm, for example, 50 mm, 100 mm. Moreover, the height dimension H1 can be set in each step described later.

  Moreover, a horizontal magnetic field, a cusp magnetic field, etc. can be employ | adopted for the magnetic field supplied from the magnetic field supply apparatus 9, For example, as intensity | strength of a horizontal magnetic field, 2000-5000G (0.2T-0.5T), 3000-4000G ( 0.3T to 0.4T), more preferably 3000 to 3500G (0.30T to 0.35T), and the magnetic field center height is -150 to +100 mm, more preferably -75 to the melt surface. It can be set to be within a range of +50 mm, and it is possible not to apply a magnetic field.

  Next, a method for producing a silicon single crystal using the CZ furnace shown in FIG. 5 will be described.

  As shown in FIG. 4, the manufacturing method of this embodiment uses a silicon seed crystal T that has undergone a single crystal formation processing step (processing step) S00, a damage layer removal step S10, a measurement step S20, and a damage layer removal determination step S30. Thus, it has a pulling step S40 for pulling up the silicon single makeup.

In the pulling step S40 shown in FIG. 4, a high-purity silicon polycrystal, for example, 100 to 400 kg is charged into the crucible 1, and at the same time, p-type or n-type is used so that the concentration in the silicon crystal becomes a predetermined concentration. Further, the dopant for setting the resistivity is adjusted, and the concentration of dopant such as carbon and nitrogen for setting or adjusting the resistivity or gettering ability is adjusted. Alternatively, no dopant can be added.
Next, the seed crystal T is attached to the seed chuck 5.

Next, the inside of the CZ furnace is set to an inert gas atmosphere, and the atmospheric pressure is adjusted to be 1.3 to 13.3 kPa (10 to 100 torr). A technique such as a hydrogen gas-containing atmosphere can also be employed.
Next, a horizontal magnetic field of, for example, 3000 G (0.3 T) is applied from the magnetic field supply device 9 so that the center height of the magnetic field is −75 to +50 mm with respect to the melt liquid surface. Heat to make silicon melt 3.

  The seed crystal T attached to the seed chuck 5 is lowered while rotating, and the tip thereof is immersed in the silicon melt 3. After the tip of the seed crystal T is immersed and acclimated, the descent of the seed crystal T is stopped, and the crystal pulling is started while the crucible 1 and the pulling shaft 4 are rotated. At this time, the respective temperatures are set so that the temperature state of the seed crystal T and the silicon melt 3 falls within a predetermined range. Specifically, the melt surface temperature is adjusted by adjusting the heater power so that a meniscus having a predetermined shape is formed around the tip of the seed crystal T.

Thus, in the dipping process in which the seed crystal T is made to conform to the silicon melt 3, the holding time for immersing and holding the seed crystal T that sets the temperature of the seed crystal T in the silicon melt 3, the silicon melt 3 and the heat shield. It is possible to set the height H1, which is the distance from the body 7, the seed rotation speed at the time of pulling up, the crucible rotation speed, and the like.
When applying the MCZ method in which a magnetic field is applied, it is desirable that the transverse magnetic field applied to the silicon melt 3 be in the range of 2000 to 4000 G.

After removing the dash neck or other dislocations, as a diameter expansion process, the pulling speed, the seed crystal / crucible rotation speed, and the heater power are controlled to expand the diameter to increase the diameter compared to the neck portion N. A shoulder portion (expanded diameter portion) is formed and pulled up.
Next, as a straight body process, a predetermined dimension such as φ300 mm or φ450 mm defined by a silicon wafer or the like to be a product is maintained, and the straight body portion 6b is pulled up to a predetermined crystal length. Following the straight body process, the diameter is reduced as a tail process, and the pulled silicon single crystal 6 is separated from the silicon melt 3.

  In the present embodiment, by removing the damage layer on the surface of the columnar portion T2 of the silicon seed crystal T, the strength of the columnar portion T2 is maintained, the occurrence of breakage in the columnar portion T2 is prevented, and safe pulling is performed. It becomes possible.

  Examples of the present invention will be described below.

The damage layer was measured in the seed crystal that had undergone the seed crystal formation processing step (processing step) S00 and the damage layer removal step S10 described in the embodiment.
In addition, as grinding process S11 and finish grinding process S12, the grinding wheel count was # 140, and the pressing condition (shaving amount) was 0.05 mm in the finish grinding process S12.

In the angle polishing sample collecting step S21, a sample T2a having a length of about 10 to 16 mm and a maximum thickness of about 1 mm was sampled and subjected to 5 ° 44 ′ angle polishing. FIG. 6 shows an image near the apex of the curved contour T2e after the light etching process of 2 μm as the measurement region T2d.
In the figure, three types of samples are taken as R, C, and L, and the result of polishing twice is shown as levels (1) and (2), and the results are shown as images and numerical values of damage depth. .

  From angle polishing, as shown by a broken line in the image, the length from the apex position in the measurement region T2d is observed as the damage depth, and this is shown as a scale in the figure from the angle polishing angle. In conversion, the numerical value of the damage layer thickness (depth) was calculated. In the image, a broken line indicates a vertex position and a damage depth position. Moreover, the vertical axis | shaft of a figure shows the depth of angle polishing.

  In the measurement of the seed crystal under the grinding condition # 140 finish, the average damage depth was about 30 μm. Although only one level of seed was measured this time, a comparison could not be made, but the prospect of quantitatively measuring the damage depth with this method was obtained.

Next, the grinding wheel count was started at # 140, and in the final finish grinding step, # 800 was set, and the pressing condition (shaving amount) was 0.05 mm in the finish grinding step S12.
FIG. 7 shows observation and measurement results of damage depth by angle polishing + light etching.

  From this result, it can be seen that even if the pressing conditions (the amount of cutting) are the same, the damage depth can be less than 10 μm on average if the grinding wheel count is # 800 in the finish grinding process.

Next, the grinding wheel count was not changed in # 140, and the pressing condition (shaving amount) was set to 0.5 mm in the final finish grinding step.
After removing 50 μm of the surface layer of this seed crystal by etching, the surface was observed to find irregularities.

  From this result, it was estimated that the damage depth was larger than 50 μm, and it was found that the damage was deeper when the finish grinding amount was 0.05 mm.

T ... Silicon seed crystal T1 ... Mounting diameter expansion part T2 ... Columnar part T3 ... Liquid landing part

Claims (11)

A method for producing a silicon seed crystal used by attaching to a seed chuck when producing a silicon single crystal by the Czochralski method,
A processing step of cutting out from a silicon single crystal to form a columnar silicon seed crystal;
The weight of the silicon single crystal to be pulled up by eliminating the remaining surface scratches and the surface processing damage layer on the columnar side surface of the columnar portion on the seed chuck side with respect to the liquid landing portion located on the lower end portion of the silicon seed crystal In order to maintain the strength that can maintain the surface processing damage layer removal step,
In the silicon seed crystal side surface, a measurement step of measuring whether a scratch on the processing surface or a surface processing damage layer is removed,
A method for producing a silicon seed crystal, comprising:   2. The method for producing a silicon seed crystal according to claim 1, wherein the damage layer removing step includes an etching process.   3. The method for producing a silicon seed crystal according to claim 2, wherein the damaged layer removing step includes two or more grinding processes having different grinding conditions before the etching process.   4. The method for producing a silicon seed crystal according to claim 3, wherein roughness of the grinding wheel is different as different grinding conditions in the grinding treatment.   4. The method for producing a silicon seed crystal according to claim 3, wherein pressing conditions of the grinding wheel are different as different grinding conditions in the grinding treatment.   2. The method for producing a silicon seed crystal according to claim 1, wherein the measuring step includes an angle polishing process and a light etching process. 2. The method for producing a silicon seed crystal according to claim 1, wherein the measurement step includes a measurement process using high-energy radiation that is an X-ray having a wavelength of 0.001 nm to 0.25 nm .   The silicon single crystal to be pulled is φ300 mm or more, or a silicon seed crystal having a raw material charge amount at the time of pulling of 300 kg or more. A method for producing a silicon seed crystal. A method for producing a silicon seed crystal used by attaching to a seed chuck when producing a silicon single crystal by the Czochralski method,
A processing step of cutting out from a silicon single crystal to form a columnar silicon seed crystal;
The weight of the silicon single crystal to be pulled up by eliminating the remaining surface scratches and the surface processing damage layer on the columnar side surface of the columnar portion on the seed chuck side with respect to the liquid landing portion located on the lower end portion of the silicon seed crystal In order to maintain the strength that can maintain the surface processing damage layer removal step,
A method for producing a silicon seed crystal, comprising:   A method for producing a silicon single crystal, comprising pulling up a silicon single crystal using a seed crystal for producing a silicon single crystal produced by the production method according to claim 1. Damage layer removal judgment step for judging whether the damage layer is removed and having the required strength from the result measured in the measurement step,
A pulling step of pulling up the silicon single crystal using the silicon single crystal manufacturing seed crystal manufactured by the manufacturing method according to any one of claims 1 to 8,
Have
  In the damage layer removal determining step, when it is determined that the surface processing damaged layer is removed, the silicon single crystal is pulled up as the pulling step, and it is determined that the surface processing damaged layer is not removed. If so, the method returns to the surface-processed damaged layer removing step, wherein the method for producing a silicon single crystal is characterized.