JP2011029578A - Heat treating method for silicon wafer, and silicon wafer - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a heat treating method for silicon wafers suppressing formation of an oxygen precipitate large in size, increasing the density of an oxygen precipitate of appropriate size and effectively suppressing plastic deformation of the wafers, and silicon wafers. <P>SOLUTION: The silicon wafer is heat-treated to pass through: a first heating process S1a of carrying the silicon wafer in a treatment chamber kept at a first temperature T<SB>1</SB>below 600°C, and thereafter heating the silicon wafer at a heating rate of 3.1°C/min or less from T1 to a second temperature T<SB>2</SB>of 700-800°C (T<SB>1</SB><T<SB>2</SB>); a second heating process S1b including a process of heating the silicon wafer from T<SB>2</SB>to the highest achieving temperature T<SB>3</SB>(T<SB>2</SB><T<SB>3</SB>) and keeping the silicon wafer for 30-240 min at a certain temperature T4 in a range of 800-1,100°C between T<SB>2</SB>and T<SB>3</SB>; a highest achieving temperature keeping process S2 of keeping the silicon wafer at T<SB>3</SB>for a certain period; and a cooling process S3 of cooling the silicon wafer from T<SB>3</SB>to a temperature for carrying out the silicon wafer to the outside of the treatment chamber. <P>COPYRIGHT: (C)2011,JPO&INPIT

Description

  The present invention relates to a heat treatment method applied in a silicon wafer manufacturing process and a silicon wafer manufactured thereby.

  In recent years, with the high integration of semiconductor elements, high quality silicon wafers, which are semiconductor substrate materials, have been demanded. Therefore, high-temperature heat treatment such as hydrogen annealing, Ar annealing, ammonia annealing, and annealing in an oxidizing gas atmosphere is performed in the silicon wafer manufacturing process. Also in a device formation process using a silicon wafer, high-temperature heat treatment such as activation annealing treatment and oxidation treatment after impurity introduction is performed.

  A vertical diffusion furnace is generally used for the high-temperature heat treatment performed in the above-described silicon wafer manufacturing process or device forming process. This vertical diffusion furnace has the advantage that a plurality of silicon wafers can be processed at the same time. Particularly, in order to obtain a desired effect such as reduction of crystal defects, a long-time heat treatment is required. In this case, it is much more advantageous in terms of throughput than the single wafer heat treatment apparatus.

The heat treatment by the vertical diffusion furnace is performed by loading a plurality of silicon wafers on a holder called a boat and heat-treating at a high temperature of several hundred to several hundreds of degrees by external heater heating.
In such a heat treatment using a vertical diffusion furnace, thermal stress caused by an in-plane temperature difference of the silicon wafer and self-weight stress at the boat support position are applied in combination, and the silicon wafer is likely to be plastically deformed. In particular, when a silicon wafer is heat-treated in a non-oxidizing atmosphere in a vertical diffusion furnace, oxygen having a dislocation fixing action contained in the silicon wafer is diffused outwardly, and the strength of the wafer is reduced, so that plastic deformation occurs. It is further accelerated.

  In addition, in the heat treatment of a silicon wafer in a non-oxidizing atmosphere, even if no plastic deformation occurs in the heat treatment in the silicon wafer manufacturing process, the strength of the wafer is reduced by this heat treatment. Plastic deformation tends to occur during heat treatment in the forming process. When such plastic deformation occurs, there is a problem that device characteristics are deteriorated.

Therefore, as a measure for suppressing the plastic deformation as described above, for example, means for improving the density of oxygen precipitates having an action of inhibiting the movement of dislocations has been studied (for example, Patent Document 1).
However, oxygen precipitates are deposited with distortion in the periphery, and when the size of the oxygen precipitates is large, conversely, dislocations are easily introduced at a high density, which causes a problem of causing plastic deformation. is there.

As other countermeasures, means for raising the temperature at a low speed in the temperature range of 1100 ° C. to 1300 ° C. (for example, Patent Document 2) and means for optimizing the boat shape (for example, Patent Document 3) have been studied. Yes.
However, the means for raising the temperature at a low speed in the temperature range of 1100 ° C. to 1300 ° C. has a problem that oxygen precipitates having a large size may remain and become a source of plastic deformation. In addition, regarding the optimization of the boat shape and the like, it is often difficult to put it into practical use in terms of development time and cost.

  On the other hand, in the initial step of heat treatment, the temperature range of 700 to 1000 ° C. is heated at a rate of 15 ° C./min or higher to control the density of ultrafine oxygen precipitates, and 850 to 980. Means for growing the precipitation nuclei while maintaining the temperature in the temperature range of 0.5 ° C. for 0.5 to 60 minutes has been studied (for example, Patent Document 4).

JP 2008-160069 A JP-A-8-264549 JP 2005-511187 A Japanese Patent No. 3172389

  However, in the heat treatment as described in Patent Document 4, since the initial rate of temperature rise is large, the thermal stress resulting from the in-plane temperature difference of the silicon wafer becomes large and it is difficult to suppress plastic deformation of the wafer. Further, even with such means, there is a possibility that large-sized oxygen precipitates may remain, which causes a source of plastic deformation.

  The present invention has been made to solve the above technical problem, suppresses the formation of large-sized oxygen precipitates, increases the density of oxygen precipitates of an appropriate size, and increases the plasticity of the wafer. An object of the present invention is to provide a silicon wafer heat treatment method and a silicon wafer capable of effectively suppressing deformation.

The silicon wafer heat treatment method according to the present invention is a method of heat treating a silicon wafer obtained by slicing a silicon single crystal ingot grown by the Czochralski method, and at a first temperature T ₁ of 600 ° C. or lower. After carrying the silicon wafer into the processing chamber held, the temperature rise rate is 3.1 ° C. from the first temperature T ₁ to a second temperature T ₂ (T ₁ <T ₂ ) of 700 ° C. or more and 800 ° C. or less. First temperature rising process in which the temperature is increased at a rate of less than / minute, the temperature is increased from the second temperature T ₂ to the maximum temperature T ₃ (T ₂ <T ₃ ), and the second temperature T ₂ and the A second temperature raising process including a process of holding at a constant temperature T ₄ in a temperature range of 800 ° C. to 1100 ° C. between the maximum temperature T ₃ and 30 minutes to 240 minutes, and the maximum temperature T ₃ Maximum temperature maintained for a certain time And extent, characterized in that it includes a cooling step of cooling from the highest temperature T ₃ to a temperature at which unloading the silicon wafer to the processing chamber.
By performing such a heat treatment, it is possible to suppress the formation of oxygen precipitates having a large size, increase the density of oxygen precipitates of an appropriate size, and effectively suppress plastic deformation of the wafer. .

The constant temperature T ₄ is preferably 850 ° C. or higher and 950 ° C. or lower.
By maintaining at a constant temperature within such a range, it is possible to easily grow the oxygen precipitation nuclei formed in the first temperature raising process to a size larger than the annihilation critical size at a temperature exceeding T ₄ .

In the heat treatment method, it is preferable that the temperature increase rate when the temperature is increased from the second temperature T ₂ to the maximum temperature T ₃ (T ₂ <T ₃ ) is 1 ° C./min or more. Moreover, it is preferable that the cooling rate in the cooling process is 1 ° C./min or more.
By shortening the heat treatment time as such a temperature increasing / decreasing rate, when the temperature is increased from the second temperature T ₂ to the maximum temperature T ₃ or when the temperature is decreased from the maximum temperature T ₃ , The disappearance of oxygen precipitates formed in the first temperature raising process can be suppressed.

Further, the silicon single crystal ingot for slicing a silicon wafer was grown by passing through a temperature range from 1100 ° C. to 900 ° C. within 40 minutes in the cooling process during pulling by the Czochralski method. It is preferable.
By growing the silicon single crystal ingot under such conditions, oxygen precipitate nuclei can be formed at a high density during the growth of the silicon single crystal ingot. Therefore, the size of the oxygen precipitate after the heat treatment is further reduced. be able to.

Further, in the heat treatment method, it is preferable that the maximum temperature T ₃ is 1150 ° C. or higher and 1300 ° C. or lower, and the holding time in the maximum temperature holding step is 1 minute or longer and 180 minutes or shorter.
By setting it as such conditions, effects, such as a crystal defect reduction in the surface layer part from the wafer surface to a depth of 5 micrometers, can be acquired efficiently.

The silicon wafer according to the present invention has a defect density of less than 1 piece / cm ² in the surface layer portion from the wafer surface to a depth of 5 μm, and an oxygen concentration within a depth of 1 μm from the wafer surface has a depth of 1 μm from the wafer surface. The wafer bulk portion having a depth lower than the above oxygen concentration and a depth of 5 μm or more from the wafer surface has a scattered light intensity of 5000 a. u. Less than oxygen precipitates having a density of 1 × 10 ⁹ pieces / cm ³ or more are formed.
The silicon wafer having such a configuration is a high-quality silicon wafer that can suppress plastic deformation in a heat treatment performed in a subsequent device formation process.

According to the silicon wafer heat treatment method of the present invention, the formation of large-sized oxygen precipitates is suppressed, the density of oxygen precipitates of an appropriate size is increased, and the plastic deformation of the wafer is effectively suppressed. can do.
In addition, since the silicon wafer according to the present invention can suppress plastic deformation in a heat treatment performed in a subsequent device formation process, it can greatly contribute to yield improvement in the device formation process.

It is a schematic diagram of the heat processing sequence for demonstrating the heat processing method of the silicon wafer which concerns on this invention. It is a schematic diagram of the heat processing sequence for demonstrating the other aspect of the heat processing method of the silicon wafer which concerns on this invention. It is the plot figure which showed the relationship between the temperature increase rate in Examples 3-8 and the comparative example 3, and the oxygen precipitate density in the wafer bulk part of the silicon wafer after heat processing. It is the plot figure which showed the relationship between the temperature increase rate in Examples 3-8 and the comparative example 3, and the size of the oxygen precipitate in the wafer bulk part of the silicon wafer after heat processing.

Hereinafter, the present invention will be described in more detail with reference to the drawings.
FIG. 1 shows a schematic diagram of a heat treatment sequence for explaining a silicon wafer heat treatment method according to the present invention.

In the silicon wafer heat treatment method according to the present invention, a silicon wafer obtained by slicing a silicon single crystal ingot grown by the Czochralski method is placed in a processing chamber held at a _first temperature T ₁ of 600 ° C. or lower. After carrying in, heat treatment is performed by a heat treatment sequence as shown in FIG.

  As shown in FIG. 1, the heat treatment sequence in the heat treatment method according to the present invention is roughly divided into a temperature rising process S1, a maximum temperature maintaining process S2, and a temperature decreasing process S3. The temperature raising process S1 includes a first temperature raising process S1a and a second temperature raising process S1b.

In the first temperature raising step S1a, the temperature raising rate is 3.1 ° C./min or less from the first temperature T ₁ to the second temperature T ₂ (T ₁ <T ₂ ) of 700 ° C. to 800 ° C. Raise the temperature.
Next, in the second temperature raising step S1b, the temperature is raised from the second temperature T ₂ to the maximum temperature T ₃ (T ₂ <T ₃ ), and the second temperature T ₂ and the maximum temperature are reached. Including a process of maintaining at a constant temperature T ₄ in a temperature range between 800 ° C. and 1100 ° C. between the temperature T ₃ and 30 minutes or more and 240 minutes or less.
Then, in the maximum temperature holding step S2, held for a given time the maximum temperature T _3.
Further, in the cooling process S3, the temperature is decreased from the highest temperature T ₃ to a temperature at which unloading the silicon wafer to the processing chamber.

  According to the heat treatment method for a silicon wafer according to the present invention including the temperature raising process as described above, the oxygen precipitate density can be increased with an appropriate size even when the oxygen concentration is reduced in the high temperature heat treatment. Therefore, it becomes possible to effectively suppress plastic deformation of the wafer.

In the heat treatment method according to the present invention, in particular, in the first temperature rising step S1a, the temperature rising rate in the temperature region of 800 ° C. or lower where oxygen precipitation nuclei are formed is set to 3.1 ° C./min or lower. The size of oxygen precipitation nuclei can be formed with high density.
When the heating rate in the temperature range of 800 ° C. or less exceeds 3.1 ° C./min, the size of the oxygen precipitation nuclei increases, and it is difficult to effectively suppress the plastic deformation of the wafer.

The temperature increase rate from the first temperature T ₁ to the second temperature T ₂ (T ₁ <T ₂ ) between 700 ° C. and 800 ° C. in the first temperature increase process S1a is smaller than the oxygen precipitation nuclei. From the viewpoint of obtaining a higher density, it is more preferably 2.0 ° C./min or less. More preferably, it is 0.7 ° C./min or less.
Note that the lower limit of the rate of temperature increase from the first temperature T ₁ to the second temperature T ₂ (T ₁ <T ₂ ) of 700 ° C. or more and 800 ° C. or less is 0.2 ° C. / It is preferable that it is more than minutes.

In addition, by setting the first temperature T ₁ to 600 ° C. or less, it is possible to prevent problems such as cracking, plastic deformation, and particle adhesion of the silicon wafer when it is carried into the processing chamber.
The lower limit value of the first temperature T ₁ is preferably 300 ° C. or higher from the viewpoint of productivity.

Further, in the heat treatment method according to the present invention, in the second temperature raising step S1b, a constant temperature T ₄ is maintained for 30 minutes to 240 minutes (t1) in a temperature range of 800 ° C. to 1100 ° C. in which oxygen precipitation nuclei grow. it allows the formed oxide precipitate nuclei can be grown over disappearance critical size, keep holding step at the maximum temperature T ₃ temperature-raising-period and the maximum temperature T ₃ up, the oxygen precipitation nuclei disappear to This can be suppressed.

The constant temperature T ₄ is preferably 850 ° C. or higher and 950 ° C. or lower.
By maintaining at a constant temperature within such a temperature range, the oxygen precipitation nuclei formed in the first temperature raising step S1a are likely to grow beyond the annihilation critical size at a temperature exceeding the constant temperature T ₄ .

When the holding time (t1) is less than 30 minutes, the small-sized oxygen precipitation nuclei formed in the first temperature raising step S1a are heated up to the highest temperature T ₃ and the highest temperature T because it may disappear in the holding process in _3, it is difficult to form a high density of oxygen precipitate nuclei of small size.
On the other hand, when the holding time (t1) exceeds 240 minutes, productivity is deteriorated and the size of oxygen precipitation nuclei grows large, which may be a source of plastic deformation.

Moreover, it is preferable that the rate of temperature increase when the temperature is increased from the second temperature T ₂ to the maximum temperature T ₃ (T ₂ <T ₃ ) is 1 ° C./min or more. Moreover, it is preferable that the cooling rate in the cooling process is 1 ° C./min or more.
By using such a temperature raising / lowering speed, the heat treatment time can be shortened, and when the temperature is increased from the second temperature T ₂ to the maximum temperature T ₃ or from the maximum temperature T ₃ . When the temperature is lowered, the disappearance of the oxygen precipitates formed in the first temperature raising process S1a can be suppressed.

It is preferable that the upper limit value of the temperature increase rate when the temperature is increased from the second temperature T ₂ to the maximum temperature T ₃ (T ₂ <T ₃ ) is 5.0 ° C./min or less. When the upper limit value of the heating rate exceeds 5.0 ° C./min, the thermal stress acting on the silicon wafer is greatly increased, and the plastic deformation of the wafer cannot be effectively suppressed.
Moreover, it is preferable that the upper limit of the temperature-fall rate in the said temperature-fall process is 6.0 degrees C / min or less. When the upper limit value of the temperature lowering rate exceeds 6.0 ° C./min, it is not preferable because the plastic deformation of the wafer cannot be effectively suppressed for the same reason as when the temperature is increased.

The maximum temperature T ₃ is preferably 1150 ° C. or more and 1300 ° C. or less, and the holding time (t2) in the maximum temperature holding process is preferably 1 minute or more and 180 minutes or less.
By setting it as such conditions, effects, such as reduction of the crystal defect in the surface layer part from the wafer surface to a depth of 5 micrometers, can be acquired efficiently.

When the maximum temperature T ₃ is less than 1150 ° C., crystal defects in the surface layer portion from the wafer surface to a depth of 5 μm are hardly eliminated, which is not preferable.
On the other hand, when the maximum temperature T ₃ exceeds 1300 ° C., the yield stress of the silicon wafer is lowered and slip is likely to occur, and quartz used as an apparatus member is deformed, which is not preferable.
Further, when the holding time (t2) in the maximum temperature holding process is less than 1 minute, it is not preferable because crystal defects in the surface layer portion from the wafer surface to a depth of 5 μm do not disappear.
On the other hand, when the holding time (t2) in the maximum temperature holding process exceeds 180 minutes, effects such as reduction of crystal defects have already been obtained, and productivity is deteriorated. Moreover, since the deformation amount of quartz used as a device member increases, it is not preferable.

Moreover, it is preferable that the temperature which carries out the said silicon wafer out of a process chamber after a temperature fall process is 700 degrees C or less.
By setting it as such a structure, the effect which relieve | moderates the temperature change of the silicon wafer at the time of carrying out is acquired.
In addition, it is preferable that the lower limit of the temperature which carries out the said silicon wafer out of a process chamber shall be 300 degreeC or more from a viewpoint of productivity.

FIG. 2 shows a schematic diagram of a heat treatment sequence for explaining another embodiment of the silicon wafer heat treatment method according to the present invention.
As shown in FIG. 2, in the silicon wafer heat treatment method according to the present invention, the rate of temperature increase from the first temperature T ₁ to the constant temperature T ₄ may be a constant rate of 3.1 ° C./min or less.
By adopting such a heat treatment sequence, small-sized oxygen precipitation nuclei can be formed at a higher density than the heat treatment sequence as shown in FIG.

A silicon single crystal ingot for slicing and obtaining a silicon wafer to be heat-treated in the present invention is grown by passing a temperature range from 1100 ° C. to 900 ° C. within 40 minutes in the cooling process during pulling by the Czochralski method. It is preferred that
In the case of a silicon single crystal ingot grown in this way, oxygen precipitation nuclei can be formed at a high density during the growth of the silicon single crystal ingot, so that the size of the oxygen precipitate after the heat treatment is further reduced. can do.

  The silicon wafer heat treatment method according to the present invention described above is performed in a non-oxidizing atmosphere such as an inert gas atmosphere or a reducing atmosphere. In the following examples, a case where 100% argon is used as an atmosphere is given as a representative example.

The silicon wafer according to the present invention is a silicon wafer manufactured by using the silicon wafer heat treatment method according to the present invention as described above, and the defect density in the surface layer portion from the wafer surface to a depth of 5 μm is 1 piece / cm. ² and a wafer bulk portion having a depth of 1 μm or more from the wafer surface lower than the oxygen concentration of 1 μm or more from the wafer surface and a depth of 5 μm or more from the wafer surface has a scattered light intensity of 5000 a. u. Less than oxygen precipitates having a density of 1 × 10 ⁹ pieces / cm ³ or more are formed.

  The scattered light intensity varies according to the size of the oxygen precipitate, and therefore serves as an index representing the size, and the scattered light intensity is 5000 a. u. If it is less than this, it can be defined that a small-sized oxygen precipitate that does not become a source of plastic deformation of the wafer is formed.

  As described above, when the silicon wafer according to the present invention uses the silicon wafer heat treatment method according to the present invention as described above, oxygen having a dislocation fixing action contained in the silicon wafer is diffused outward, Although the oxygen concentration within 1 μm depth from the wafer surface is lower than the oxygen concentration at 1 μm depth from the wafer surface, small-sized oxygen precipitates are formed at high density in the wafer bulk part at a depth of 5 μm depth from the wafer surface. Therefore, it has an effect that plastic deformation can be effectively suppressed in a heat treatment performed in a subsequent device formation process.

The oxygen concentration within a depth of 1 μm from the wafer surface is, for example, less than 1.0 × 10 ¹⁸ atoms / cm ³ , and the oxygen concentration at a depth of 1 μm or more from the wafer surface is, for example, 1.2 × 10 ¹⁸ atoms. / Cm ³ or more.

  In addition, the said oxygen concentration is the value evaluated by secondary ion mass spectrometry (SIMS; Secondary ion-microprobe Mass Spectrometry). The density of the oxygen precipitate having the scattered light intensity is evaluated by IR tomography after passing through a two-step heat treatment step (heat treatment at 780 ° C. for 3 hours and heat treatment at 1000 ° C. for 16 hours in the same heat treatment). It is the value. The measurement of the defect density in the surface layer portion from the wafer surface to a depth of 5 μm is a value evaluated at a wavelength of 680 nm with an LSTD scanner (Laser Scattering Topology Defect Scanner).

EXAMPLES Hereinafter, although this invention is demonstrated further more concretely based on an Example, this invention is not restrict | limited by the following Example.
[Example 1]
A 300 mm diameter silicon wafer (oxygen concentration 1.24 × 10 ¹⁸ atoms / cm ³ , nitrogen concentration 5 × 10 ¹⁴ atoms / cm ³ , boron concentration 2 × 10 ¹⁴ atoms / cm ³ , phosphorus and carbon are not doped) is loaded on the boat. Then, it was carried into a processing chamber of a vertical diffusion furnace maintained at 600 ° C. in a 100% argon atmosphere.

Thereafter, in the temperature raising process, as the first temperature raising process S1a shown in FIG. 1, the temperature rising rate from 600 ° C. to 800 ° C. is set to 1 ° C./min, and then, as the second temperature raising process S1b, 800 ° C. ° C. the heating rate up to reach a temperature T ₃ 1200 ° C. was controlled to 2 to 5 ° C. / min from the middle, 180 minutes at _{900 ℃ (T 4) (t1} ) and held.
Then, 60 minutes at 1200 ° C. is the highest temperature T ₃ (t2) and held, by controlling the heating rate from 1200 ° C. is the highest temperature T ₃ to 600 ° C. in 2 to 5 ° C. / min, 600 The heat-treated silicon wafer was taken out of the processing chamber of the vertical diffusion furnace at 0 ° C. to prepare an annealed wafer.

[Example 2]
Silicon wafers similar to those in Example 1 were loaded on a boat and carried into a processing chamber of a vertical diffusion furnace maintained at 600 ° C. in a 100% argon atmosphere.
Thereafter, in the temperature raising process, as the first temperature raising process S1a shown in FIG. 2, the temperature rising rate from 600 ° C. to 900 ° C. (T ₄ ) is 1 ° C./min, and the temperature is 900 ° C. for 180 minutes (t1). Thereafter, as the second temperature raising step S1b, the temperature raising rate from 900 ° C. to 1200 ° C., which is the maximum temperature T ₃ , was controlled to 2 to 5 ° C./min.
Then, 60 minutes at 1200 ° C. is the highest temperature T ₃ (t2) and held, by controlling the heating rate from 1200 ° C. is the highest temperature T ₃ to 600 ° C. in 2 to 5 ° C. / min, 600 The heat-treated silicon wafer was taken out of the processing chamber of the vertical diffusion furnace at 0 ° C. to prepare an annealed wafer.

[Comparative Example 1]
An annealing wafer was produced in the same manner as in Example 1 except that the temperature rising rate from 600 ° C. to 1200 ° C. was controlled at 2 to 5 ° C./min without holding at 900 ° C. .

[Comparative Example 2]
The temperature increase rate from 600 ° C. to 1200 ° C. is controlled to 0.5 ° C./min, and held at 900 ° C. for 300 minutes (t1). A wafer was produced.

  The annealed wafers obtained in the above examples and comparative examples were subjected to a two-step heat treatment step (heat treatment at 780 ° C. for 3 hours and heat treatment at 1000 ° C. for 16 hours within the same heat treatment), and then the depth from the wafer surface. The density and size (scattered light intensity) of oxygen precipitates in a wafer bulk portion of 5 μm or more were measured by IR tomography (MO-411 manufactured by Raytex Co., Ltd.). Further, the slip length in the heat treatment was measured by X-ray topography (XRT300 manufactured by Rigaku Corporation).

Furthermore, the annealed wafers obtained in the above examples and comparative examples were rapidly heated at a maximum temperature of 1350 ° C. and a holding time of 15 seconds using a single wafer rapid heating / cooling heat treatment apparatus (hereinafter referred to as RTP apparatus). After the heating / rapid cooling heat treatment, the slip length of the annealed wafer was measured by the same method as in Example 1. This rapid heating / cooling heat treatment (hereinafter referred to as RTP) was assumed to be a heat treatment performed in the device formation process.
These measurement results are summarized in Table 1.

As shown in Table 1, in Comparative Example 1, the density of oxygen precipitates in the wafer bulk portion of the silicon wafer after the heat treatment was as low as less than 1 × 10 ⁹ pieces / cm ³ . The scattered light intensity a. u. Is 5000a. u. As described above, it was recognized that oxygen precipitates having a large size were formed. Further, plastic deformation called slip occurred at the boat support position of the annealed wafer, and the slip length became larger after RTP.

On the other hand, in Comparative Example 2, although the oxygen precipitate density in the wafer bulk portion is 1 × 10 ⁹ pieces / cm ³ or more, the scattered light intensity indicating the size of the oxygen precipitate is 5000 a. u. It was more than that. Further, no slip was observed on the annealed wafer after the heat treatment, but after RTP, a slip due to the large size of the oxygen precipitate was observed.

In contrast, in Examples 1 and 2, the scattered light intensity is 5000 a. u. It was confirmed that small-sized oxygen precipitates of less than 1 were formed at a high density of 1 × 10 ⁹ pieces / cm ³ or more. Also, no slip was observed after the heat treatment and after the subsequent RTP.

  Moreover, the defect density in the surface layer part from the wafer surface to the depth of 5 μm in the annealed wafers obtained in the above examples and comparative examples was evaluated with a LSTD scanner (wavelength 680 nm), and the depth direction from the wafer surface was measured. The oxygen concentration was evaluated by SIMS.

As a result, in any annealed wafer, the defect density in the surface layer portion from the wafer surface to a depth of 5 μm is less than 1 piece / cm ² , and the oxygen concentration within a depth of 1 μm from the wafer surface is 1.0 × 10 ^18. atoms / cm less than ^3, the oxygen concentration of more depth 1μm from the wafer surface was 1.2 × 10 ¹⁸ atoms / cm ³ or more.

[Examples 3 to 8, Comparative Example 3]
Annealed wafers were produced in the same manner as in Example 1 except that the rate of temperature increase from 600 ° C. to 800 ° C. was changed from 0.7 ° C./min to a maximum of 5.0 ° C./min.
For each of the obtained annealed wafers, the density and size of oxygen precipitates (scattered light intensity) and the slip length in the heat treatment were measured in the same manner as in Example 1.

Further, the obtained annealed wafer was subjected to RTP with an RTP apparatus in the same manner as in Example 1, and then the slip length was further evaluated.
These temperature rising rate conditions and measurement results are summarized in Table 2.

  Further, based on the results of Table 2, FIG. 3 shows the relationship between the temperature rise rate and the oxygen precipitate density in the wafer bulk portion of the silicon wafer after the heat treatment, and FIG. 4 shows the temperature rise rate and the heat treatment after the heat treatment. The relationship with the size of the oxygen precipitate in the wafer bulk part of a silicon wafer is shown as a plot diagram.

From the results shown in Table 2, FIG. 3 and FIG. 4, when the temperature rising rate is 3.1 ° C./min or less, the scattered light intensity is 5000 a. u. It was confirmed that small-sized oxygen precipitates of less than 1 were formed at a high density of 1 × 10 ⁹ pieces / cm ³ or more. Also, no slip was observed after the heat treatment and after the subsequent RTP.

On the other hand, in Comparative Example 3, although the oxygen precipitate density in the wafer bulk portion is 1 × 10 ⁹ pieces / cm ³ or more, the scattered light intensity indicating the size of the oxygen precipitate is 5000 a. u. It was more than that. In addition, a slip occurred at the boat support position of the annealed wafer, and the slip length further increased after RTP.

When the rate of temperature increase is 2.0 ° C./lower, the scattering intensity indicating the size of the oxygen precipitate is 3300 a. u. The following and lower oxygen precipitates were obtained at a high density of 2.5 × 10 ⁹ pieces / cm ³ or more.
Further, when the heating rate is 0.7 ° C./lower, the scattering intensity is 1995 a. u. The following and lower oxygen precipitates were obtained at a higher density of 1.5 × 10 ¹⁰ pieces / cm ³ or more.

  In addition, the defect density in the surface layer portion from the wafer surface to a depth of 5 μm in the annealed wafers obtained in Examples 3 to 8 and Comparative Example 3 was evaluated with an LSTD scanner (wavelength 680 nm), and deep from the wafer surface. The oxygen concentration in the vertical direction was evaluated by SIMS.

As a result, in any annealed wafer, the defect density in the surface layer portion from the wafer surface to a depth of 5 μm is less than 1 piece / cm ² , and the oxygen concentration within a depth of 1 μm from the wafer surface is 1.0 × 10 ^18. less atoms / cm ^3, an oxygen concentration of more depth 1μm from the wafer surface was 1.2 × 10 ¹⁸ atoms / cm ³ or more.

Claims (7)

A method of heat treating a silicon wafer obtained by slicing a silicon single crystal ingot grown by the Czochralski method,
After loading the silicon wafer into the processing chamber which is held at a first temperature T ₁ of the 600 ° C. or less, the first second from the temperature T ₁ of the 700 ° C. or higher 800 ° C. below the temperature T ₂ (T ₁ < A first temperature rising process in which the temperature is increased at a rate of temperature increase of 3.1 ° C./min or less until T ₂ );
The temperature is raised from the second temperature T ₂ to the highest temperature T ₃ (T ₂ <T ₃ ), and between 800 ° C. and 1100 ° C. between the second temperature T ₂ and the highest temperature T _3. A second temperature raising step including a step of maintaining at a constant temperature T ₄ in the temperature range of 30 minutes to 240 minutes,
A maximum temperature holding process in which the maximum temperature T ₃ is maintained for a predetermined time;
A temperature lowering process in which the temperature is lowered from the maximum temperature T ₃ to a temperature at which the silicon wafer is carried out of the processing chamber;
A silicon wafer heat treatment method characterized by comprising: Heat treatment method for a silicon wafer according to claim 1 wherein said predetermined temperature T ₄ is characterized in that at 850 ° C. or higher 950 ° C. or less. 3. The temperature rising rate when the temperature is raised from the second temperature T ₂ to the maximum temperature T ₃ (T ₂ <T ₃ ) is 1 ° C./min or more. Heat treatment method for silicon wafers.   The method for heat-treating a silicon wafer according to any one of claims 1 to 3, wherein a cooling rate in the cooling process is 1 ° C / min or more.   2. The silicon single crystal ingot is grown by passing through a temperature range from 1100 ° C. to 900 ° C. within 40 minutes in a cooling process during pulling by the Czochralski method. The heat processing method of the silicon wafer in any one of -4. The maximum temperature T ₃ is 1150 ° C. or higher and 1300 ° C. or lower, and the holding time in the maximum temperature holding process is 1 minute or longer and 180 minutes or shorter. Heat treatment method for silicon wafers. The defect density in the surface layer from the wafer surface to a depth of 5 μm is less than 1 piece / cm ² , the oxygen concentration within 1 μm depth from the wafer surface is lower than the oxygen concentration at a depth of 1 μm or more from the wafer surface, and the wafer The wafer bulk portion having a depth of 5 μm or more from the surface has a scattered light intensity of 5000 a. u. A silicon wafer, wherein oxygen precipitates of less than 1 × 10 ⁹ pieces / cm ³ are formed.

Images