TWI568896B - Single crystal manufacturing method - Google Patents

Description

Single crystal manufacturing method

The present invention relates to a method of growing a single crystal such as ruthenium single crystal from a stock solution melt according to the Czochralski method. In detail, there is a method for producing a high-quality single crystal having few crystal defects. More specifically, there is a method of evaluating the moving average of the pulling speed required to obtain the desired quality of the single crystal and having a causal relationship with the quality of the single crystal, and correcting the target value of the pulling speed.

Generally, in the case of producing a single crystal, the pulling speed of the single crystal and the heater temperature are used as the operation amount, and the diameter of the single crystal is controlled. For example, a method for producing a single crystal is disclosed, which uses a Chaichen method to independently control an average pulling speed and a heater temperature to grow a single crystal (for example, refer to Patent Document 1) ). In the method for producing a single crystal, the growth length of the single crystal per unit time at intervals of 30 to 50 minutes in the growth of the single crystal is taken as the average pulling speed, and the average pulling speed is fixed at the steady state. At a constant speed, in the case of non-steady state, the deviation of the predicted crystal diameter and the target crystal diameter due to the crystal diameter during growth causes the pulling speed to vary only for a predetermined time, and, for the heater temperature, at steady state The temperature is maintained at a constant temperature, and in the case of the non-steady state, the diameter of the single crystal is controlled by the deviation of the predicted crystal diameter and the target crystal diameter of the crystal diameter during growth. here, The predetermined time for changing the pulling speed is a short period of time (the variation range is within ±0.02 mm/min) which is not affected by the average pulling speed at the steady state in the steady state, and the time is 30 seconds or less. Preferably. In the method for producing a single crystal composed in this manner, it is possible to efficiently extract a low-definition tantalum single crystal.

On the other hand, a method for producing a single crystal having a moving average of the pulling speed of a causal relationship between the quality of the single crystal and the single crystal is disclosed (for example, see Patent Document 2). In the method for producing a single crystal, the step of calculating the set value of the pulling speed of the single crystal is repeated in the process of extracting the single crystal according to the Chaichen method, and the lower limit value is determined based on the set value and the operation amount. The step of controlling the moving average of the pulling speed, whereby the diameter of the single crystal is controlled. Further, the upper and lower limits of the operation amount of the pulling speed are calculated such that the moving average value of the pulling speed is within the preset allowable range, and the diameter is controlled within the limiting condition, whereby the moving average of the pulling speed is also controlled. Within the allowable range of the preset. Further, before the start of the pulling of the single crystal, the target value of the pulling speed of the single crystal is set in advance for each pulling length, and the pulling speed of the single crystal is corrected to the measured value of the moving average of the pulling speed, and the target value is the same. .

In the method for producing a single crystal formed in this manner, in the process of pulling the single crystal, the steps of calculating the set value of the pulling speed of the single crystal and the upper and lower limits of the operating amount of the pulling speed are repeated, and The set value and the lower limit value above the operation amount are used to control the moving average of the pulling speed of the single crystal, and the diameter of the single crystal is controlled. That is, since the average value of the pulling speed of the single crystal is controlled at all times, the unevenness of the quality of the axial direction of the single crystal can be reduced. As a result, a high quality single crystal can be stably produced. Moreover, since the moving average value of the pulling speed is calculated within the allowable range, the axis of the single crystal can be further reduced. To the uneven quality, it is possible to manufacture high quality single crystals more stably. Further, before the start of the pulling of the single crystal, the target value of the pulling speed is set in advance, since the pulling speed of the single crystal is corrected to the measured value of the moving average of the pulling speed, and the target value is the same, so that single crystal can be obtained. The pulling speed is optimized, and the unevenness of the quality of the axial direction of the single crystal can be further reduced, and the high quality single crystal can be produced more stably.

[Prior patent documents] [Patent Literature]

[Patent Document 1] Japanese Laid-Open Patent Publication No. 2005-082474 (paragraphs [0011], [0012], [0014]

[Patent Document 2] Japanese Laid-Open Patent Publication No. 2010-053015 (paragraphs [0007] to [0009], paragraphs [0011] to [0013])

However, in the method for producing a single crystal shown in the above-mentioned Patent Document 1, when the fluctuation range of the pulling speed is narrow and the operation time is also short, it is expected that the moving average of the pulling speed does not greatly affect. However, in the case where various diameters caused by a hot environment are unpredictable in the diameter of a single crystal, the range of the pulling speed may be as small as ±0.02 mm/min or less, and the predetermined time is as short as 30 seconds or less. It is difficult to suppress various disturbances to the diameter of a single crystal. Further, even in the case where the heater temperature is operated in order to suppress the disturbance to the diameter of the single crystal, since the time constant for the operation of the heater temperature to affect the diameter of the single crystal is large, it is difficult to control the diameter of the single crystal. Even with the above The method can control the diameter of the single crystal, and it cannot be said that since the operation amount of the pulling speed is small, the moving average value of the pulling speed does not greatly change, and the moving average value of the pulling speed is changed later. situation. Therefore, in the method for producing a single crystal shown in the above-mentioned Patent Document 1, it is difficult to accurately control the moving average value of the pulling speed to within ±1%, for example, by controlling the diameter of the single crystal. On the other hand, in the method for producing a single crystal shown in the above-mentioned Patent Document 2, by controlling the diameter of a single crystal, a high-quality single crystal is stably produced, but a large disturbance of the diameter of the single crystal occurs. In the case where the controllability of the average value is lowered, in order to improve the quality of the single crystal and to stably produce a single crystal, further improvement is desired.

An object of the present invention is to provide a method for producing a single crystal which is capable of producing a high quality crystal defect with a control property of improving the average value of the pulling speed of a causal relationship with the quality of a single crystal. Single crystal.

According to a first aspect of the present invention, in a method for producing a single crystal, a target value of a pulling speed of a single crystal is set in advance for each predetermined pulling length before starting the pulling of a single crystal according to the Chaucer method. In the pulling of a single crystal and the pulling speed of the predetermined pulling length, the moving value of the pulling speed is calculated from the actual value of the pulling speed from the pulling start time point to the current time point. When the moving average value of the pulling speed is different from the target value of the pulling speed, the average value of the moving speed of the pulling speed and the target value of the pulling speed become the same, and the moving average value is based on the target value of the pulling speed and the pulling speed. , calculate the correction value of the target value of the pulling speed at the current time point, and then based on the calculation A method for producing a single crystal of a single crystal of a correction value of a target value of a pulling speed, wherein a pulling length of a pulling length which is an actual value for calculating a moving average value of the pulling speed is set to When α is set to β in the future, the pull length (α + β) for calculating the correction value of the target value of the pulling speed is changed in accordance with the actual value of the diameter of the single crystal.

According to a second aspect of the present invention, in the invention of the first aspect, the single crystal pulling state is monitored, and when the target value and the actual value of the diameter of the single crystal are set to D ₀ and D ₁ respectively, |D ₁ - When D _{0 is} equal to or less than the threshold t ₁ , the pull length (α + β) of the correction value for calculating the target value of the pulling speed is set to be higher than the pulling average for evaluating the moving speed of the pulling speed. γ length is short, while | D ₁ -D ₀ | exceeds the threshold line pull length _{t. 1} and ₂ below threshold t, the correction value is calculated for the target value of the pulling speed (α + β) is maintained at a pulling length γ for evaluating the moving average of the pulling speed, and when |D ₁ -D ₀ | is exceeding the threshold t ₂ , the correction value for calculating the target value of the pulling speed is calculated The pulling length (α + β) is set to be longer than the pulling length γ for evaluating the moving average of the pulling speed.

According to a third aspect of the present invention, in the invention of the second aspect, after the actual pull value of the single crystal is evaluated, the threshold value t ₁ and the threshold value t _{2 are determined} .

According to a fourth aspect of the present invention, in the invention of the third aspect, when the actual pull value of the single crystal is evaluated and the unevenness σ of the diameter of the single crystal is calculated, the threshold t ₁ and the threshold t are set. _{2 is} determined to be t ₁ = 0.5 × σ, and t ₂ = 2 × σ.

According to a fifth aspect of the present invention, in the invention of the first to fourth aspects, the target value of the pulling speed is set to 0.3 to 1.2 mm/min.

According to a sixth aspect of the invention, the pulling length (α + β) of the single crystal is set to 30 to 70 mm.

According to a seventh aspect of the present invention, in the invention of the first to fourth aspects, the pulling length α of the single crystal pulling length (α + β) from the pulling start time point to the current time point and the remaining The pulling length β is set to 20 to 99% of the pulling length (α + β) and 80 to 1% of the pulling length (α + β), respectively.

In the method for producing a single crystal according to the first aspect of the present invention, the pulling length (α + β) for calculating the correction value of the target value of the pulling speed is changed according to the actual value of the diameter of the single crystal, thereby appropriately Controls the moving average of the pulling speed that is strongly correlated with the quality of the single crystal and has a causal relationship, and pulls a single crystal. That is, the control of the pulling speed and the diameter control of the single crystal are not independent of each other, but have an influence on each other, and the diameter of the single crystal is monitored while growing in a single crystal, and the pulling speed is calculated based on the actual value of the diameter of the single crystal. The pull length (α+β) of the correction value of the target value becomes shorter or longer, whereby the correction value of the target value of the pulling speed is calculated at all times in response to the actual value of the moving average value of the pulling speed, and then Single crystals are pulled according to the correction value. As a result, the control of the pulling speed and the diameter control of the single crystal can be performed with high precision. In this way, considering the actual value of the diameter of the single crystal, the moving average of the pulling speed which has a significant influence on the quality of the single crystal is evaluated, and the target value of the pulling speed is corrected, thereby reducing the unevenness of the quality of the single crystal. Moreover, the unevenness of the diameter of the single crystal is also suppressed, and a high-quality single crystal can be stably produced.

In the method for producing a single crystal according to the second aspect of the present invention, when |D ₁ -D ₀ | is less than or equal to the threshold t ₁ , that is, the control performance of the diameter of the single crystal is extremely good, The pulling length (α+β) of the correction value for calculating the target value of the pulling speed is set to be shorter than the pulling length γ for evaluating the moving average of the pulling speed, and the control performance of the moving average of the pulling speed is further improved. . Further, when |D ₁ -D ₀ | is greater than the threshold value t ₁ and less than the threshold value t ₂ , that is, the control performance of the diameter of the single crystal is relatively good, and the pulling speed is calculated. The pulling length (α + β) of the correction value of the target value is maintained at the pulling length γ for evaluating the moving average of the pulling speed, such as the control performance for setting the moving average of the pulling speed. Further, when |D ₁ -D ₀ | exceeds the threshold t ₂ , that is, the control performance of the diameter of the single crystal is slightly lowered, and the purpose of improving the controllability of the diameter of the single crystal is to be used. The pulling length (α+β) of the correction value for calculating the target value of the pulling speed is set to be longer than the pulling length γ for evaluating the moving average value of the pulling speed, so that the control performance of the moving average value of the pulling speed is changed. weak. As a result, the control of the diameter of the single crystal and the control of the moving average of the pulling speed are stably performed, and the controllability of the diameter of the single crystal can be improved in advance.

α‧‧‧The past pull length

Β‧‧‧ future pulling length

t ₁ ‧‧‧ threshold

t ₂ ‧‧‧ threshold

D ₀ ‧‧‧ target value of the diameter of a single crystal

D ₁ ‧‧‧ actual value of the diameter of a single crystal

Fig. 1 is a schematic view showing a method of calculating a correction value of a pulling speed target value according to the first embodiment of the present invention, and Fig. 1(a) is a view showing a control method of a case where the pulling speed is a target value. Fig. 1(b) is a view showing a control method in a case where the pulling speed is high.

Figure 2 is a flow chart for evaluating the moving average of the pulling speed.

Figure 3 is a graph showing the change in the future pull length β of the change in the pull length α in the past, showing the moving average of the pull speed according to the value of the parameter. Value control performance gives strength and weakness

Fig. 4 is a view showing a calculation result of a change in the correction value of the target value of the pulling speed of the change in the pulling length.

Fig. 5 is a view showing a change in the pulling speed of the change in the pulling length, and is a graph showing the controllability of the moving average of the pulling speed.

Fig. 6 is a view showing a change in the diameter of a single crystal which changes the length of the pulling, and is a graph showing the controllability of the diameter.

Next, an embodiment of the present invention will be described based on the drawings. In the present embodiment, the single crystal is extracted from the crucible melt stored in the crucible according to the Chaisky method. Before the start of the pulling of the single crystal, the target value of the pulling speed of the single crystal is set in advance every predetermined pulling length. Then, in the pulling process of the single crystal and the pulling speed of the predetermined pulling length, the moving average value of the pulling speed is calculated from the actual value of the pulling speed from the pulling start time point to the current time point of the predetermined pulling length. . Then, when the moving average value of the pulling speed is different from the target value of the pulling speed, the moving average value of the pulling speed and the target value of the pulling speed are matched, and the moving average is based on the moving speed target value and the pulling speed. The value is used to calculate the correction value of the target value of the pulling speed at the current time point. Further, the single crystal is pulled up based on the calculated correction value of the target value of the pulling speed.

The pulling speed target value is preferably set in the range of 0.3 to 1.2 mm/min. Further, the predetermined pulling length of the single crystal is preferably set to 30 to 70 mm, and more preferably set to 45 to 55 mm. Further, the pulling length of the predetermined pulling length of the single crystal from the pulling start time point to the current time point is preferably set to 20 to 99% of the predetermined pulling length, and is set to be predetermined. It is better in the range of 80 to 99% of the pulling length, and the remaining pulling length is preferably set to 80 to 1% of the predetermined pulling length, and is set to be in the range of 20 to 1% of the predetermined pulling length. Better. The predetermined pulling length of the single crystal of the crucible is limited to a range of 30 to 70 mm, which is because the stringing system is strictly dependent on the pulling device used, but according to the experimental result, the system having high correlation with the quality of the single crystal is obtained. The average value of the pulling speed of about 50 mm is preferably set to be about the same as about 50 mm. Further, the pulling length of the predetermined pulling length from the pulling start time point to the current time point and the remaining pulling length are respectively limited to a range of 20 to 99% of the predetermined pulling length and a predetermined pulling length. In the range of 80 to 1%, this is because the pulling length and the remaining pulling length are respectively less than 20% of the predetermined pulling length and 80% of the predetermined pulling length, and the pulling speed is The limit becomes too strong.

Fig. 1 is a schematic view showing a method of calculating a moving average value of the pulling speed. Specifically, Fig. 1(a) shows a rectangular shape in which the lengths in the lateral direction and the longitudinal direction are (α + β) and A, respectively. When the horizontal axis is the pulling length, the vertical axis is taken as the pulling speed, and the first Fig. (a) shows that the average value of the pulling speed is A in the section of the pulling length (α + β). Next, as shown in Fig. 1(b), it is considered that the lengths in the lateral direction and the longitudinal direction are rectangles of α and B, respectively, and the lengths in the lateral direction and the longitudinal direction are rectangles of β and C, respectively. Here, in the case where the total area of the two rectangles in the first figure (b) is equal to the area of one of the rectangles in the first figure (a), in the first figure (b), if the length B of the longitudinal direction is known, the longitudinal direction is The length C can be obtained by using the following mathematical formula (1) and mathematical formula (2). In Fig. 1(b), when the horizontal axis is the pulling length and the vertical axis is the pulling speed, the average pulling speed of the B system is the average value of the pulling speed of the C system. If using α, β, A, B Information, which can be used to calculate the moving average C of the pulling speed that should be the target of the future.

A × (α + β) = B × α + C × β ... (1)

C={A×(α+β)-B×α}/β......(2)

Here, the left side of the mathematical formula (1) represents the area of the portion to which the oblique hatching is applied in the first graph (a), and the right side of the mathematical formula (1) represents the portion of the first graph (b) to which the hatching is applied. The total area of the portion to which the horizontal line is applied. Further, the mathematical expression (1) indicates that the integral value in the interval (α + β) (mm) for calculating the correction value of the lifting speed target value is equal to the actual value for calculating the moving average value of the pulling speed. The integral value of α (mm) is the sum of the integral values of the future interval β (mm) for appropriately correcting the target value of the pulling speed.

Therefore, the mathematical formula (1) can be expressed as the following mathematical formula (3), and the mathematical expression (2) can be expressed as the following mathematical formula (4).

(lifting speed target value) × (α + β) = (actual value of moving average of pulling speed) × α + (correction value of lifting speed target value) × β (3)

(correction value of the pulling speed target value) = {(lifting speed target value) × (α + β) - (actual value of the pulling speed moving average value) × α} / β (4 )

It is known from Fig. 1(b) that when the actual value of the moving average value of the pulling speed is high, the lifting speed target value is corrected to be slightly lower.

Next, a control method of the moving average value of the pulling speed will be described based on the flowchart of Fig. 2. First, the pull length (γ) used to evaluate the moving average of the pulling speed having a causal relationship with the crystal defect is determined. This pulling length (γ) can be uniquely determined from the construction of the pulling device. The reason for this is that the quality of the point defect concentration and the quality of the product (the single crystal to be pulled up) are determined according to the range in which the point defects which are taken in when the single crystal grows are diffused. The range of point defects is spread and the speed of the pulling The moving average has a strong correlation, so there is also a strong correlation between the quality of the product and the moving average of the pulling speed. However, it is related to the moving average of the pulling speed of a few mm of the pulling length, which is dependent on the pulling device used. In general, the evaluation of the Xu-cooled pulling device has a pulling average of the moving average of the pulling speed associated with the crystal defect, which is longer than that of the quenching type pulling device. Next, regarding the crystal defects, the target value of the pulling speed for producing the desired single crystal of the single crystal is determined. Here, the target value of the pulling speed of the single crystal for obtaining the desired quality is determined for each pulling length of the single crystal. Then, the pull length (α + β) and the control period for calculating the correction value of the pull target speed value are determined. Here, the control period is preferably set to be the same as the control period of the diameter control as long as it can be avoided to be set to be long. Further, the average value of the pulling speed is evaluated every control cycle, and after the correction value of the lifting speed target value is calculated according to the evaluation result, the lifting speed target value is corrected, and according to the correction value of the pulling speed target value, Lifting a single crystal. In this way, the moving average value of the pulling speed is evaluated every control cycle, and the target value of the pulling speed is corrected according to the evaluation, whereby the unevenness of the quality of the single crystal is reduced, and the high quality can be stably produced. Single crystal.

When setting the pull length (α + β) (mm) for calculating the correction value of the target value of the pulling speed, if α (mm) and β (mm) are set to (α + β) (mm) and ( When γ) (mm) is the same, the correction value of the target value of the pulling speed can be set so that the actual value of the moving average value of the pulling speed at the time of pulling (γ) (mm) coincides with the desired target value of the pulling speed. For example, if γ is set to 50 mm, and α (mm) and β (mm) are set to be the same as the actual value of the moving average value of the pulling speed when lifting 50 mm is required to match the desired target value of the pulling speed. The limit of α + β = γ = 50 (mm) is satisfied.

Moreover, in the pulling of the single crystal, if the diameter of the single crystal cannot be controlled, the pulling of the single crystal does not hold. Therefore, the controllability of the diameter of the single crystal is important, and it is desirable to control the diameter of the single crystal and the control of the moving average of the pulling speed. Therefore, in order to satisfy such a desire, the control performance of the moving average of the pulling speed is adjusted with high precision while monitoring the pulling state of the single crystal. That is, the pull length for calculating the correction value of the target value of the pulling speed is changed in accordance with the actual value of the diameter of the single crystal. Specifically, in the state of monitoring the pulling state of the single crystal, when the target value and the actual value of the diameter of the single crystal are set to D ₀ and D ₁ respectively, the |D ₁ -D ₀ | In the case of t ₁ or less, the pulling length controlled according to the moving average of the pulling speed is set to be shorter than the predetermined pulling length, and the |D ₁ -D ₀ | is exceeding the threshold t ₁ and the threshold t _In the case of ₂ or less, the pulling length controlled by the moving average of the pulling speed is maintained at the predetermined pulling length, and further, when |D ₁ -D ₀ | exceeds the threshold t ₂ , the pulling is performed according to the pulling The pull length controlled by the speed moving average is set to be longer than the predetermined pull length. Here, the threshold value t ₁ and the threshold value t ₂ can be arbitrarily set, but it is preferable to evaluate the actual pull value of the single crystal in the past, and it is preferable to calculate the unevenness σ of the diameter of the single crystal. It can be determined that t ₁ = 0.5 × σ and the threshold t ₂ = 2 × σ. That is, the unevenness σ is the unevenness (standard deviation) of the diameter of the single crystal of the conventional pull-up actual value, for example, when σ = 0.8 mm, t ₁ = 0.4 mm and t ₂ = 1.6 mm.

When |D ₁ -D ₀ | is less than or equal to the threshold t ₁ , it can be judged that the controllability of the diameter of the single crystal is extremely good. In this case, if the average value is moved according to the pulling speed as described above, The controlled pulling length is set to be shorter than the predetermined pulling length, that is, α and β are set to calculate the relationship between the pulling length (α+β) of the correction value of the lifting speed target value and (α+β)<γ. , the control performance of the moving average of the pulling speed can be improved. Further, when |D ₁ -D ₀ | exceeds the threshold value t ₁ and is less than the threshold value t ₂ , it can be judged that the controllability of the diameter of the single crystal is relatively good. In this case, as shown above. The pulling length controlled according to the moving average of the pulling speed is maintained at a predetermined pulling length, that is, α and β are set such that the pulling length (α+β) of the correction value for calculating the target value of the pulling speed is satisfied (α) With the relationship of +β)=γ, the moving average of the pulling speed can be controlled as set. Further, when |D ₁ -D ₀ | exceeds the threshold value t ₂ , it can be judged that the controllability of the diameter of the single crystal is slightly lowered. In this case, as shown above, the average value is moved according to the pulling speed. The controlled pulling length is set to be longer than the predetermined pulling length, that is, α and β are set to calculate the relationship between the pulling length (α+β) of the correction value of the lifting speed target value and (α+β)>γ. , the control performance of the moving average of the pulling speed can be intentionally suppressed. This is a method for improving the controllability of the diameter of the single crystal. For example, the control performance of the lifting average of the pulling speed of 50 mm can be adjusted according to the third figure. Here, the control performance of moving the average value of the pulling speed is weakened in order to improve the control performance of the diameter control. That is, in the case of maintaining the control performance of the moving average of the pulling speed, the control of setting the α and β of the relational expression satisfying (α + β) = 50 (mm) is performed, and the control of moving the average value of the pulling speed is performed. In the case where the performance becomes strong, the control of setting (α + β) to less than 50 (mm) is performed, but in the case of improving the control performance of the diameter control, setting (α + β) to be larger than 50 (mm) is performed. The control is due to the need to make the control performance of the moving average of the pulling speed weak. These relations are shown in Fig. 3, and "□" in Fig. 3 shows an example in which the control performance of the moving average value of the pulling speed is increased, and "△" in Fig. 3 indicates the moving average value of the pulling speed. An example of the case where the control performance is weak. As a result, the control of the diameter of the single crystal and the control of the moving average of the pulling speed can be more stably performed.

On the other hand, the calculation of the correction value of the lifting speed target value may be performed every control cycle, or may be performed every multiple times of the control cycle. The pulling speed target value is updated in each cycle of calculating the correction value of the lifting speed target value, and then the diameter of the single crystal is controlled according to the pulling speed target value, whereby the moving average of the pulling speed can be evaluated . Specifically, when the control period is set to 10 seconds, the first step and the second step are repeated every 10 seconds, and the first step is based on the set past pull length α and the future pull. a step of calculating a correction value V ₁ of the target value of the pulling speed according to the mathematical formula (4), wherein the second step is a step of pulling the single crystal by using the corrected pulling speed V ₁ as a target value. . Further, since the single crystal is pulled by about 0.05 to 0.2 mm in 10 seconds, the pulling speed V ₁ is updated every about 0.05 to 0.2 mm. More specifically, a time point of about 0.05 to 0.2 mm is pulled as an origin, from which the lifting speed target value is corrected (updated) based on the past pulling length α and the future pulling length β. . Further, after 10 seconds, a time point of about (0.05 to 0.2) × 2 mm is extracted as an origin, from which the correction (update) is based on the past pull length α and the future pull length β. Lifting speed target value. Repeat this operation. Further, in the case where the moving average value of the pulling speed coincides with the target value of the pulling speed set before the pulling, since the pulling speed is operated as the operation amount of the diameter control, it is difficult to completely match, and the inclusion is located The allowed range is considered to be consistent. The allowable range is, for example, managed based on the management lower limit value and the management upper limit value.

Moreover, in order to make the feedback of the control of the moving average of the pulling speed faster, when the lifting speed target value is corrected, the moving average of the pulling speed is calculated. The smaller the pull length α of the actual value of the value is, the more advantageous it is, but the operating range of the pulling speed in the future is limited, and the controllability of the diameter is weakened. Here, the moving average of the pulling speed is an average value of the pulling speed at the time of pulling 50 mm, for example. Further, in the case where the unevenness of the moving average value of the pulling speed is large, the pulling length α is also set to be preferably increased. Here, the pulling length α is set to, for example, 40 mm. Further, when the unevenness of the pulling speed is small, the actual value of the moving average value of the pulling speed is high in relation to the moving average value of the pulling speed which is high in relation to the quality of the single crystal, and the pulling length α is shortened. It is set that the control performance of the moving average of the pulling speed is improved. Here, the pulling length α is set to, for example, 30 mm. That is, the pulling length α may be set so that the average value can be moved at a high-predicted pulling speed.

On the other hand, the pull length β is a value that is automatically determined based on α and (α + β). Further, the pulling length β can be adjusted for a long time or adjusted in a short time, and the controllability of the moving average value of the pulling speed is low, and since it is fiercely corrected, there is a possibility of disturbance, so the flower length is long. It is preferable to adjust the time. In this case, the pulling length β is set to be increased. Here, the pulling length β is set to, for example, 40 mm. Further, in the case where the controllability of the moving average value of the pulling speed is high, the adjustment may be performed in a short time. In this case, the pulling length β is set to be short. Here, the pulling length β is set to, for example, 10 mm. Further, the control cycle may be set, for example, every 10 seconds, every 10 seconds. Furthermore, the setting of (α + β) can be implemented manually or automatically. Further, the setting of α and β may be set in advance by the pulling length, or may be changed manually or automatically at the time of pulling.

Further, in this embodiment, as a single crystal, a single knot is listed. Crystal, but not limited to this.

[Examples]

Next, an embodiment of the present invention will be described in detail together with a comparative example.

<First Embodiment>

According to the Chaisky method, the ruthenium single crystal used for the 300 mm-diameter wafer for semiconductors is pulled from the ruthenium stored in the ruthenium. Further, it is controlled as shown below in the range of the pulling length of 800 to 1400 mm. First, the pulling speed target value is set to the desired quality of the single crystal by the pulling length. Next, the pulling length (α + β) for calculating the correction value of the pulling speed target value which is high in relation to the quality of the single crystal is set to 50 mm. Then, in order to actively control the moving average of the pulling speed, it is basically set to α = 10 mm, β = 40 mm, and the control period is 10 seconds. The actual value of the moving average value of the pulling speed when pulling 10 mm is calculated every control cycle, and the correction value of the lifting speed target value is calculated according to the following mathematical formula (4), and then according to the lifting speed target value The revised value continues to be implemented.

(correction value of the pulling speed target value) = {(lifting speed target value) × (α + β) - (actual value of the pulling speed moving average value) × α} / β (4 )

However, in the range of the pulling length of 900 to 1100 mm, since the control of the diameter of the single crystal of the crucible is good, in order to make the control of the moving average of the pulling speed strong, the correction value for the target value of the pulling speed is calculated. The pulling length (α + β) is set to 45 mm, α is set to 10 mm, and β is set to 35 mm. Moreover, in the range of the pulling length of 1100 to 1200 mm, since the control of the diameter of the single crystal is slightly lower than the range of the pulling length of 900 to 1100 mm, the control of the diameter of the single crystal is emphasized, in order to increase the pulling speed. The control of the moving average becomes weak, The pull length (α + β) for calculating the correction value of the pull speed target value is set to 55 mm, α is set to 10 mm, and β is set to 45 mm.

<1st test and evaluation>

Fig. 4 is a view showing changes in the correction value of the pulling speed target value at the pulling length of 800 to 1400 mm in the first embodiment. When the lifting speed target value in Fig. 4 is not corrected, "0%" is set. Further, Fig. 5 shows a change in the correction value of the moving average value of the pulling speed at the pulling length of 800 to 1400 mm in the first embodiment. The target value of the pulling speed in Fig. 5 is set to "1" in arbitrary units. Further, Fig. 6 shows the controllability of the diameter of the single crystal in the control of the moving average of the pulling speed in the first embodiment. In Fig. 6, the target value of the diameter of the single crystal is set to "100%".

It is known from Fig. 4 that the correction value of the lifting speed target value can be controlled within a range from +0.6% to -0.8% for the lifting speed target value. Further, as is understood from Fig. 5, the actual value of the moving average value of the pulling speed can be controlled within ±1.0% of the target value of the pulling speed. Further, as is understood from Fig. 5, the actual value of the moving average of the pulling speed is substantially controlled within ±0.5% of the target value of the pulling speed at a pulling length of 900 to 1100 mm. Further, as is understood from Fig. 6, the diameter of the single crystal is 100% of the target value, and can be controlled within the range of 99.90% to 100.10%, that is, within the range of ±0.10%. From these results, it was found that the moving average of the pulling speed and the diameter of the single crystal can be well controlled.

<Second embodiment>

The pulling length for calculating the correction value of the target value of the pulling speed is a value determined from the correlation between the moving average value of the pulling speed and the quality of the single crystal, and this value is regarded as 50 mm, and the pulling sheet is obtained. Lifting speed of crystallization The correction value of the target value. Specifically, the pulling speed target value, the actual value of the moving average of the pulling speed, the past pulling length α (the pulling length for calculating the actual value of the moving average of the pulling speed), and the future pulling The length β is substituted into the following mathematical expression (4), and the correction value of the target value of the pulling speed is calculated.

(correction value of the pulling speed target value) = {(lifting speed target value) × (α + β) - (actual value of the pulling speed moving average value) × α} / β (4 )

<2nd Test and Evaluation>

The result is shown in the first table. In the first table, together with the correction value of the lifting speed target value, the actual value of the pulling speed target value, the pulling speed moving average value, the past pulling length α, and the future pulling length β are described.

It is known from the first table that the shorter the pulling length β in the future, the shorter the pulling length is required to enter the predetermined range of the pulling speed target value, so the target value of the pulling speed set before the pulling is required. Apply a big correction. If the deviation is too large, there is a possibility that the controllability of the diameter of the single crystal is lowered. Sexuality, so in order to control the diameter of the single crystal on one side, it is important to control the moving average of the pulling speed so that the future pulling length β is not too short.

(α+β)‧‧‧Length length

A‧‧‧length length

‧‧‧‧Length length

B‧‧‧Longitudinal length

‧‧‧‧Length length

C‧‧‧Longitudinal length

Claims (7)

A method for producing a single crystal, wherein a target value of a pulling speed of the single crystal is set in advance according to a predetermined pulling length before starting the pulling of the single crystal according to the Chaisky method, and the pulling of the single crystal is performed And in the middle of the pulling of the predetermined pulling length, the moving value of the pulling speed is calculated from the actual value of the pulling speed of the predetermined pulling length from the pulling start time point to the current time point, and the moving average value is increased at the pulling speed. When the value is different from the target value of the pulling speed, the moving average value of the pulling speed is matched with the target value of the pulling speed, and the moving average is based on the target value of the pulling speed and the pulling speed. The value is calculated as a correction value of the target value of the pulling speed at the current time point, and the single crystal is extracted based on the corrected value of the calculated target value of the pulling speed, which is characterized in that it is used to calculate the When the pull length of the pull length of the actual value of the pull speed moving average is set to α and the future pull length is set to β, the change is calculated based on the actual value of the diameter of the single crystal. Pull speed The pull length (α + β) of the correction value of the target value is set such that ( Δ + β ) is set to be longer as the actual value of the single crystal diameter deviates from the target value. A method for producing a single crystal according to the first aspect of the patent application, wherein the pulling state of the single crystal is monitored, and when the target value and the actual value of the diameter of the single crystal are respectively set to D ₀ and D ₁ , at |D ₁ -D ₀ | is the case where the threshold value t ₁ or less is set, and the pull length (α + β) of the correction value for calculating the target value of the pulling speed is set to be larger than the moving average for evaluating the pulling speed The pulling length γ of the value is short, and when |D ₁ -D ₀ | is greater than the threshold value t ₁ and less than the threshold value t ₂ , the correction value for calculating the target value of the pulling speed is used. The pull length (α + β) is maintained at a pull length γ for evaluating the moving average of the pull speed, and when |D ₁ -D ₀ | exceeds the threshold t ₂ , it is used to calculate the pull The pull length (α + β) of the correction value of the target value of the speed is set to be longer than the pull length γ for evaluating the moving average of the pulling speed. The manufacturing method of the single crystal of the second aspect of the patent application, wherein the threshold value t ₁ and the threshold value t _{2 are} determined after the actual value of the pulling of the single crystal in the past is evaluated. The manufacturing method of the single crystal of the third aspect of the patent application, wherein the threshold value t ₁ and the threshold value are obtained when the actual value of the pulling of the single crystal in the past is evaluated and the unevenness σ of the diameter of the single crystal is calculated. t _{2 is} determined to be t ₁ = 0.5 × σ, and t ₂ = 2 × σ. The method for producing a single crystal according to any one of claims 1 to 4, wherein the target value of the pulling speed is set to 0.3 to 1.2 mm/min. The method for producing a single crystal according to any one of claims 1 to 4, wherein the pulling length (α + β) of the single crystal is set to 30 to 70 mm. The method for producing a single crystal according to any one of claims 1 to 4, wherein the pulling length (α + β) of the single crystal is from the pulling start time point to the current time point pulling length α And the remaining pulling length β is set to be 20 to 99% of the pulling length (α + β) and 80 to 1% of the pulling length (α + β), respectively.