CN110121576B - Method for determining defective region of silicon single crystal wafer - Google Patents
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Abstract
The present invention provides a defect region determination method for a silicon single crystal wafer, which determines a defect region of a silicon single crystal wafer, characterized in that a Void defect distribution on the surface of the silicon single crystal wafer is measured by size using LST without heat treatment of the silicon single crystal wafer, and the defect region is determined based on the Void defect density distribution obtained by the measurement. Thus, a method for determining a defective region of a single-crystal silicon wafer is provided, which can determine a defective region of a wafer by an easy method without depending on the initial oxygen concentration.
Description
Technical Field
The present invention relates to a method for determining a defective region of a silicon single crystal wafer.
Background
In recent years, low oxidation and low defect of a wafer have been required according to the requirements of device design, and the demand for NPC (near Perfect Crystal) has been high. The NPC is defined as a region where Void defects and LEPs (Large Etch Pit) are not generated, and may be divided into a Ni region and an Nv region. The Void defect is formed by aggregation of point defects called Vacanty (empty hole) in which Si atoms of lattice points are lost.
When pulling a crystal while changing the pulling rate by the Czochralski (CZ) method, the defect distributions are arranged in the order of V-rich/OSF/Nv/Ni/I-rich from the high-speed side according to the crystal pulling conditions. Here, the V-rich region (hereinafter also referred to as V region) is a region where many Void(s) are generated due to insufficient silicon atoms on the high speed side under the pulling condition, and the I-rich region (hereinafter also referred to as I region) is a region where many dislocations and excessive blocks of silicon atoms are generated due to the presence of extra silicon atoms, i.e., Interstitial-Si, on the low speed side under the pulling condition. The OSF region is a region closer to the low-speed side than the V-rich region, and is a region in which defects called OSFs (Oxidation Induced Stacking faults) are distributed in a ring shape when viewed in a cross section (in a wafer plane) perpendicular to the crystal growth axis. The Ni region and the Nv region are as described above.
When a silicon single crystal having a relatively high oxygen concentration is used, the relationship between the OSF region, Nv region, Ni region, and I region and the silicon single crystal wafer in the As-Grown state (state in which the silicon single crystal rod is pulled and then heat treatment is not performed at all) and the relationship between the silicon single crystal wafer after heat treatment are summarized As shown in table 1 below.
[ TABLE 1 ]
| As-Grown | After heat treatment | |
| OSF area | With Void and without LEP | Little BMD and OSF production |
| Nv region | No VoidNo LEP | With BMD generation, NPC zone |
| Ni region | No VoidNo LEP | No BMD, NPC zone was generated |
| I region | Void-free and LEP-free | BMD was not produced |
Void is generally measured by infrared Laser Scattering Tomography (LST), and conventionally used devices such as LST (MO441) can measure Void having a diameter of more than 25 nm.
As a method for determining NPC, Enhanced-OSF inspection can be performed (patent document 1, patent document 2), but this method measures OSF generated by discharging i-Si due to BMD generated by heat treatment. In this case, since OSF cannot be generated even when BMD is not generated, it is difficult to measure a low oxygen concentration product of 12ppma (jeida) or less, and it is necessary to change the heat treatment conditions depending on the initial oxygen concentration, for example, to treat the product for a longer time in the case of low oxygen concentration crystallization. Setting conditions and setting density determination for this purpose are labor-intensive.
NPC is divided into Nv areas and Ni areas, and generally, there is no Void in an Nv area, although Void may be generated in a part of an Nv area. The Nv region and the Ni region in NPC are determined by whether or not BMD is generated (whether or not oxygen is precipitated) by performing heat treatment. This determination also requires changing the heat treatment conditions in accordance with the initial oxygen concentration.
On the other hand, there is a method of determining NPC by directly measuring Void with LST, which is independent of the initial oxygen concentration and can be determined as not being NPC as long as Void is present. However, since most of Nv regions and Ni regions do not have Void, Nv regions and Ni regions cannot be determined by this method.
When a low-oxygen crystal (12ppma or less) is used, the relationship between the OSF region, the Nv region, the Ni region, and the I region, the As-Grown single crystal silicon wafer, and the heat-treated wafer is summarized As shown in Table 2 below.
[ TABLE 2 ]
| As-Grown | After heat treatment | |
| OSF area | With Void and without LEP | BMD and OSF are not produced |
| Nv region | Void and LEP free | Is not generatedBMD, NPC zone |
| Ni region | Void and LEP free | No BMD, NPC zone was generated |
| I region | Void-free and LEP-free | BMD was not produced |
As described above, even in the case of low-oxygen crystals, the Nv region and the Ni region cannot be determined by a conventionally used apparatus such as LST (MO 441). Further, since BMD does not occur after the heat treatment, the OSF region, Nv region, and Ni region cannot be determined by the Enhanced-OSF inspection described above.
Paragraph [0025] of patent document 3 describes that Void in a low-oxygen crystal can be measured by LST (MO441), and in this case, the OSF region and Nv and Ni regions (together, NPC) can be discriminated. The Nv region and the Ni region were determined by measuring BMD after the heat treatment. At this time, in the case of low-oxygen crystals of 12ppma or less, since BMD does not occur after heat treatment, Nv region and Ni region cannot be discriminated.
Documents of the prior art
Patent document
Patent document 1: japanese patent laid-open publication No. 6-97251
Patent document 2: international publication WO2014/129123 pamphlet
Patent document 3: japanese patent laid-open publication No. 2012-79932
Disclosure of Invention
Technical problem to be solved
The present invention has been made in view of the above problems, and an object thereof is to provide a method for determining a defective region of a single crystal silicon wafer, which can determine a defective region of a wafer by an easy method without depending on an initial oxygen concentration.
(II) technical scheme
In order to achieve the above object, the present invention provides a defect region determination method for a silicon single crystal wafer, which determines a defect region of a silicon single crystal wafer, characterized in that a Void defect distribution on a surface of the silicon single crystal wafer is measured by size using LST without heat treatment of the silicon single crystal wafer, and the defect region is determined based on the Void defect density distribution obtained by the measurement.
According to the method for determining a defective region in a single crystal silicon wafer, a defective region in a wafer can be determined by an easy method without depending on the initial oxygen concentration.
In addition, the determined defective region is preferably set to be one or more of a V region, an OSF region, an Nv region, and a Ni region.
According to the present invention, these defective regions can be easily determined.
In addition, it is preferable that the size of the Void defect distribution measured by size using the LST is set to a size exceeding 25nm and a size of 12 to 25 nm.
Therefore, the OSF region, the Nv region, and the Ni region can be particularly easily determined.
(III) advantageous effects
Conventionally, NPC is determined by performing heat treatment + selective etching + microscopic observation and measurement of OSF density in order to determine NPC, but according to the present invention, NPC can be determined only by an easy method such as measurement using LST. In the conventional method, it is necessary to change the OSF density and the heat treatment conditions in accordance with the initial oxygen concentration, and to set the conditions, and in some cases, it is necessary to change the measurement conditions in accordance with the measured value of the oxygen concentration. However, in the present invention, the measurement conditions need not be changed. In addition, in the conventional measurement method using LST, the Nv region and the Ni region cannot be determined, but are determined as the NPC region together.
Drawings
FIG. 1 is a graph showing the lifetime after heat treatment of a silicon single crystal wafer sliced in the axial direction from a silicon single crystal ingot obtained by gradually changing the pulling rate of the crystal in example 1 and the LST measurement result of the silicon single crystal wafer in the As-Grown state.
FIG. 2 is a graph showing the results of LST measurement in a silicon single crystal wafer in the As-Grown state and the lifetime after heat treatment of a silicon single crystal wafer sliced in the axial direction from a silicon single crystal ingot obtained by gradually changing the pulling rate of the crystal in example 2.
FIG. 3 is a view schematically showing a method of detecting crystal defects in a silicon single crystal wafer by an infrared laser scattering tomography method.
Detailed Description
The present invention will be described in more detail below.
As described above, there is a need for a defect region determination method for a single-crystal silicon wafer, which can determine a defect region of a wafer by an easy method without depending on the initial oxygen concentration.
In particular, when low-oxygen crystals (12ppma or less) are used, as shown in table 2, although the evaluation before and after the heat treatment was performed by a conventional method such as Enhanced-OSF inspection, the difference between Nv region and Ni region could not be determined. The same applies to the case of using LST (MO 441).
As described above, in the conventional method, the measurement of Void is performed using LST (MO 441). As-GrownLEP is measured, for example, by selective etching. BMD is measured, for example, by performing a heat treatment at 800 ℃ for 4 hours and a heat treatment at 1000 ℃ for 16 hours followed by selective etching. OSF is measured, for example, by selective etching after a heat treatment at 1150 ℃ for 60 minutes.
As shown in table 2, since it was conventionally considered that Void is not detected in the Nv zone, a zone in which Void is not generated is referred to as NPC (in actuality, Void exists in a high-speed part of the NPC zone). This determination method is a determination method that does not depend on the initial oxygen concentration.
This time, when smaller Void was measured, it was confirmed that smaller Void (size of 12-25 nm) was generated in a considerable part of NPC, in other words, only the region where smaller Void was generated was NPC (especially Nv region). Thus, the present inventors found that: the above technical problems can be solved by measuring the Void defect distribution by size, particularly to a smaller Void, using LST, and the present invention has been completed.
That is, the present invention is a defect region determination method for a single crystal silicon wafer, which determines a defect region of a single crystal silicon wafer, characterized in that a Void defect distribution on a surface of the single crystal silicon wafer is measured by size using LST without heat treatment of the single crystal silicon wafer, and the defect region is determined based on the Void defect density distribution obtained by the measurement.
According to the present invention, defect region judgment, particularly NPC judgment can be performed based on the Void defect density and size of a single crystal silicon wafer in As-Grown state. Specifically, it can be determined that only an area in which a small-sized Void is generated is an NPC area (particularly, an Nv area). Such an NPC determination method can also be applied to the purpose of distinguishing Nv areas from Ni areas based on Void size information and the like. That is, NPC has been used as a general term for Nv regions and Ni regions up to now, but the method of the present invention is applicable to determination of Nv regions and Ni regions because only those with smaller voids are limited to Nv regions.
In the present invention, the Void defect distribution of the surface of a single-crystal silicon wafer is first measured in terms of size using LST. For example, it is preferable to set the size of the Void defect distribution measured in terms of size by LST to a size exceeding 25nm and a size of 12-25 nm. By measuring the defect distribution of Void (large Void) having a diameter exceeding 25nm and the defect distribution of Void (small Void) having a diameter of 12nm or more and 25nm or less, it is possible to easily determine the OSF region, the Nv region, and the Ni region in particular. The upper limit of the size of the large Void is not particularly limited, and may be 200nm, for example. Hereinafter, a method of measuring a small Void and a large Void using LST will be mainly described, but the present invention is not limited thereto.
Examples of devices capable of measuring small Void include LST having higher sensitivity than MO441, which is conventional LST, such as MO471 manufactured by Raytex corporation and LST300 manufactured by Semilab corporation. The large Void may be measured by MO441 as in the conventional case, or may be measured by MO471 as in the case of the small Void.
The method and the principle of measurement for measuring the size of Void defect to 12nm by using LST will be described below. As described above, MO471 and LST300 are examples of devices capable of measuring small Void. The measurement principle is the same as that of the MO441 or the like used in the related art. Is a 90 degree scattering LST. Since a camera with high sensitivity is developed and applied, it is possible to measure the Void defect distribution of the surface of the single crystal silicon wafer by size using LST as in the present invention. A specific example of a measurement method capable of measuring a Void size of 12nm is a method of measuring a region with less noise by MO 471.
More specifically, the Void defect distribution on the surface of the single-crystal silicon wafer can be measured in terms of size using LST as shown in fig. 3. FIG. 3 is a view schematically showing a method of detecting crystal defects in a silicon single crystal wafer by an infrared laser scattering tomography method. As shown in fig. 3, infrared rays 4 are made incident from the main surface 2 of the single-crystal silicon wafer 1, and scattered light 5 from the cleaved surface 3 is detected by a detector (CCD camera, CMOS image sensor, or the like) 6, whereby defects existing in the surface layer of the cleaved surface 3 are detected.
Then, according to the measurementAnd judging a defect area according to the obtained Void defect density distribution. First, the method shown in fig. 3 and the like described above is used, thereby obtaining the Void defect distribution by size. Thereby, the density distribution of the Void defect can be obtained by size. Then, the presence or absence of Void is determined from the obtained Void defect density distribution. When defect distributions of small Void and large Void are obtained, the presence or absence of small Void and the presence or absence of large Void can be determined. In this case, as shown in table 3 below, the defective region can be determined. Whether or not Void exists can be determined by, for example, setting the Void defect density to 1 × 106/cm3In the above case, it is determined that the Void defect density is 1 × 106/cm3The following case is determined to be none. The determination reference value of the Void density can be set as appropriate.
[ TABLE 3 ]
| As-Grown | After heat treatment | |
| OSF area | With large Void, small Void, no LEP | BMD and OSF are not produced |
| Nv region | There is no large Void,with a small VoidAbsence of LEP | No BMD, NPC zone was generated |
| Ni region | There is no large Void,no small VoidAbsence of LEP | No BMD, NPC zone was generated |
| I region | No big Void, No Small Void, LEP | BMD was not produced |
Small Void: void of 25-12nm in size
Large Void: void over 25nm in size
As shown in table 3, in the present invention, the Nv region, the Ni region, and the OSF region can be discriminated without depending on the initial oxygen concentration. In particular, by using a device such as MO471 or LST300, a crystal (wafer) in which only a small Void is generated can be specified as a crystal (wafer) in the Nv region of NPC. In addition, this determination method is a determination method that does not require adjustment of heat treatment or the like and does not depend on the initial oxygen concentration. In MO441, which is a conventional LST, small Void cannot be detected for both Nv areas and Ni areas because of low sensitivity of the camera, but by using MO471 and LST300 having a high-sensitivity camera, it is possible to determine the presence or absence of small Void and specify Nv areas and Ni areas.
In the present invention, it is preferable that the determined defect region is set to be any one or more of a V region, an OSF region, an Nv region, and an Ni region. According to the present invention, the V region, the OSF region, the Nv region, and the Ni region can be easily determined. The determination method of the OSF region, Nv region, and Ni region is shown in table 3. On the other hand, the defect density at Void of more than 25nm in size exceeds 1X 107/cm3In the case of (3), it can be determined that the region is a V region. In addition, in the case of LEP, it can be determined to be an I region, and As-growth LEP can be measured by selective etching, for example.
[ examples ] A method for producing a compound
The present invention will be described more specifically with reference to the following examples, but the present invention is not limited to the examples described below.
(example 1)
First, a single crystal silicon ingot is obtained by pulling a crystal while changing the pulling rate (specifically, gradually decreasing) by the CZ method. Next, the obtained single crystal silicon ingot is sliced in the axial direction. I.e., the single crystal silicon ingot is sliced longitudinally. After the longitudinal dicing, a shape processing treatment was performed to obtain a single-crystal silicon wafer in an As-Grown state As a sample. The diameter of the sample was 300mm and the oxygen concentration was 13.5 ppma. Next, the sample was cleaved as shown in fig. 3, and the Void defect distribution of the sample surface was measured by size using LST using the method shown in fig. 3. LST is measured with two sensitivities, a size exceeding 25nm and a size of 12-25 nm. MO441 and MO471 were used as measurement devices. The Void defect distribution over a size of 25nm was measured using MO 441. Void defect distributions of 12-25nm size were measured using MO 471. As for the measurement interval, MO441 is a 2mm interval, and MO471 is a 5mm interval. From this measurement, a Void defect density distribution as shown in fig. 1 was obtained as an in-plane distribution of Void before heat treatment. Next, in order to compare the above-described Void defect density distribution, the cleaved sample was subjected to heat treatment at 650 ℃ for 2 hours +800 ℃ for 4 hours +1000 ℃ for 16 hours, and the lifetime of the heat-treated sample was measured to obtain a lifetime map.
FIG. 1 shows the results of LST measurement of the lifetime after heat treatment and the As-Grown state of a silicon single crystal wafer sliced from a silicon single crystal ingot obtained by gradually changing the pulling rate of the crystal. The lifetime of the wafer after heat treatment is shown in the upper part of FIG. 1, and the Void defect density distribution of the single crystal silicon wafer in As-Grown state is shown in the lower part. In fig. 1, the lifetime map and the Void defect density distribution are arranged in a manner consistent with the measurement position. In the above-described Void defect density distribution diagram, the horizontal axis represents the wafer position (mm) when the wafer center is 0 (high-speed growth on the left side and low-speed growth on the right side), and the vertical axis represents the Void defect density. In addition, the solid figure in the Void defect density distribution diagram is a Void defect density distribution with the size of 12-25nm, and the open figure is a Void defect density distribution with the size exceeding 25 nm. In the upper part of the Void defect density distribution diagram, the determination result of the defect region based on the Void defect density distribution is shown. In addition, in the following table 4 and fig. 1, the following will be describedVoid defect density of 1 × 106/cm3The above conditions are set to have a Void defect density of 1 × 106/cm3The following case is set to none. As shown in fig. 1, the determination result and the lifetime map measured for comparison agree well. The B region sandwiched between the Ni region and the I region is referred to as a B-band, and is a region where a large amount of precipitates are generated by heat treatment.
If the lifetime map is compared with the distribution by size of As-Grown Void, there are no Void defects in the Nv region exceeding 25nm, but there are Void defects of 12-25 nm. In addition, As-Grown Void is not present in the Ni region, and BMD is small after heat treatment (estimated from lifetime map). From this, it is understood that the defect region can be determined from the Void defect density distribution as shown in table 4 below and fig. 1.
[ TABLE 4 ]
| As-Grown | After heat treatment | |
| OSF area | With large Void, small Void, no LEP | BMD and OSF are not produced |
| Nv region | There is no large Void,with a small VoidAbsence of LEP | No BMD, NPC zone was generated |
| Ni region | There is no large Void,no small VoidAbsence of LEP | No BMD, NPC zone was generated |
| I region | No big Void, No Small Void, LEP | BMD was not produced |
(example 2)
Lifetime graphs and LST measurement results in As-Grown state single crystal silicon wafers were obtained by the same method As in example 1, except that the oxygen concentration of the As-Grown state single crystal silicon wafer used As a sample was changed from medium oxygen concentration (13.5ppma) to low oxygen concentration (11.5 ppma). The results are shown in fig. 2. As shown in fig. 2, the method of the present invention can be applied to a single crystal silicon wafer in an As-growth state which is sliced from a low oxygen concentration crystal, and a defect region can be determined from the Void defect density distribution in example 2 As shown in table 4 and fig. 2. In particular, according to the method of the present invention, the Nv region, the Ni region, and the OSF region can be discriminated without depending on the initial oxygen concentration. Further, the boundary between the Nv region and the Ni region is a region where the V concentration is almost 0, that is, the Void size is also almost 0, and there is no device capable of measuring this. In the present invention, the vicinity of the boundary between the Nv region and the Ni region can be detected, and thus the Ni region and the Nv region can be determined.
The present invention is not limited to the above embodiments. The above-described embodiments are merely illustrative, and any embodiments having substantially the same configuration as the technical idea described in the claims of the present invention and achieving the same operational effects are included in the technical scope of the present invention.
Claims (3)
1. A method for judging a defective region of a silicon single crystal wafer, which judges a defective region of a silicon single crystal wafer,
without heat-treating the single crystal silicon wafer, Void defect distribution on the surface of the single crystal silicon wafer is measured by size using LST, and a defect region is determined based on Void defect density distribution obtained by the measurement.
2. The method of determining a defective region in a silicon single crystal wafer according to claim 1,
the determined defective region is set to be one or more of a V region, an OSF region, an Nv region, and a Ni region.
3. The method of determining a defective region in a silicon single crystal wafer according to claim 1 or claim 2,
the size of the Void defect distribution measured by size using the LST is set to a size exceeding 25nm and a size of 12-25 nm.
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