CN115537914B - Monocrystalline silicon preparation device and method - Google Patents
Monocrystalline silicon preparation device and method Download PDFInfo
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- CN115537914B CN115537914B CN202211322995.4A CN202211322995A CN115537914B CN 115537914 B CN115537914 B CN 115537914B CN 202211322995 A CN202211322995 A CN 202211322995A CN 115537914 B CN115537914 B CN 115537914B
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- 229910021421 monocrystalline silicon Inorganic materials 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title abstract description 28
- 239000013078 crystal Substances 0.000 claims abstract description 230
- 238000010438 heat treatment Methods 0.000 claims abstract description 124
- 239000000155 melt Substances 0.000 claims abstract description 76
- 230000008859 change Effects 0.000 claims abstract description 70
- 238000004519 manufacturing process Methods 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims description 50
- 238000012937 correction Methods 0.000 claims description 42
- 230000009467 reduction Effects 0.000 claims description 28
- 230000007246 mechanism Effects 0.000 claims description 21
- 230000033228 biological regulation Effects 0.000 claims description 12
- 238000006073 displacement reaction Methods 0.000 claims description 11
- 230000003247 decreasing effect Effects 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 238000010899 nucleation Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 4
- 230000008569 process Effects 0.000 abstract description 15
- 238000004364 calculation method Methods 0.000 abstract description 5
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 238000004088 simulation Methods 0.000 abstract description 3
- 238000005303 weighing Methods 0.000 description 16
- 230000001276 controlling effect Effects 0.000 description 14
- 230000000694 effects Effects 0.000 description 9
- 230000002829 reductive effect Effects 0.000 description 6
- 230000001105 regulatory effect Effects 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000006870 function Effects 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 230000003111 delayed effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000004083 survival effect Effects 0.000 description 2
- 238000002231 Czochralski process Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000004308 accommodation Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 206010016165 failure to thrive Diseases 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000000452 restraining effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
- C30B15/22—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal
- C30B15/26—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal using television detectors; using photo or X-ray detectors
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The application provides a monocrystalline silicon preparation device, which comprises: a crucible for holding a melt to prepare a crystal; a heating unit for heating the crucible to provide a temperature required for preparing the crystal; the apparatus further comprises: an image sensing unit for tracking the diameter variation of the acquired crystal; and the control unit is used for adjusting the power of the heating unit according to the diameter change and the shouldering time of the crystal so as to enable the diameter of the crystal to reach the set diameter. The application also provides a preparation method of the monocrystalline silicon. The monocrystalline silicon preparation device and the monocrystalline silicon preparation method combine the crystal diameter change with the shouldering time, and the overall heating power in the shouldering process is adjusted by combining the simulation calculation, so that the monocrystalline silicon preparation device and the monocrystalline silicon preparation method have better applicability under different thermal fields. Meanwhile, in large-scale production, the same set of parameters can be used for correcting the difference between equipment, so that the stability of production is ensured.
Description
Technical Field
The application relates to the technical field of monocrystalline silicon, in particular to a monocrystalline silicon preparation device and method.
Background
With the increasing of the single crystal thermal field, the increase of the feeding amount brings about the improvement of the productivity, the increase of the feeding amount also causes the increase of the heat capacity, the influence of the increase of the thermal field size and the increase of the feeding amount on the thermal field temperature regulation is more obvious, and the influence is also reflected, no matter the manual regulation or the automatic regulation depending on the functions of the prior equipment has a certain deviation from the actual demand. This state continues consistently to the constant diameter process, thereby allowing for an abnormally increased production to reduce throughput. Therefore, the environment suitable for the crystal constant diameter needs to be adjusted before the crystal constant diameter is entered. The shouldering process requires correction of the thermal field temperature.
The Czochralski process is a necessary process from the seeding diameter to the desired crystal diameter (product diameter), with the crystal diameter increasing continuously, and the entire diameter increasing process being controlled so that the diameter increases smoothly and varies. Too slow a diameter increase proves that the thermal field temperature is high, and the lack of power for crystal growth (insufficient latent heat release) causes single crystal growth failure; the rapid increase in diameter proves that the temperature of the thermal field is low, and a plurality of crystallization nuclei are easy to form, so that the growth of the single crystal is failed. Therefore, the probability of shoulder placing failure is high due to the fact that fixed process parameters (length, pulling speed and temperature/power) are used for adjustment in the shoulder placing process, meanwhile, hidden danger is reserved for the equal diameter process, and finally the failure rate of shoulder placing and equal diameter is increased.
In the existing shouldering control method, the correction and adjustment of the shouldering state are usually performed by PID operation set on the basis of the shoulder length change, however, the actual state requirement of the shouldering link is continuously changed according to the state (diameter), and as the crystal growth belongs to dynamic change and the reaction time delay is more serious along with the increase of the thermal field. Therefore, the conventional PID operation is not suitable for correction adjustment of the shouldering state, and the ideal state is difficult to achieve by using the conventional PID adjustment mode.
Disclosure of Invention
The application aims to provide a technical scheme for solving the problem that the traditional PID control in the prior art is difficult to adapt to correction and adjustment of the shouldering state.
Based on the above problems, the present application provides a single crystal silicon manufacturing apparatus comprising:
a crucible for holding a melt to prepare a crystal;
a heating unit for heating the crucible to provide a temperature required for preparing the crystal;
characterized in that the device further comprises:
an image sensing unit for tracking and acquiring the diameter change of the crystal;
and the control unit is used for adjusting the power of the heating unit according to the diameter change and the shouldering time of the crystal so as to enable the diameter of the crystal to reach a set diameter.
Further, the single crystal silicon manufacturing apparatus further includes:
the temperature sensing unit is used for acquiring the actual temperature of the melt liquid level at a fixed distance from the edge of the crystal;
the temperature regulation and correction unit is used for generating a first power reduction according to the shouldering time, generating a second power reduction according to the diameter of the crystal, and generating a power regulation and correction amount according to the offset of the actual temperature of the melt liquid level at a fixed distance from the edge of the crystal and the preset liquid level temperature;
the control unit controls the power of the heating unit according to the first power reduction, the second power reduction and the power adjustment correction amount.
Further, the preset liquid level temperature is set according to the crystal diameter.
Further, the device also comprises a horizontal driving mechanism for driving the image sensing unit to move along the radial direction of the crystal in a plane basically parallel to the liquid level of the melt so that the edge of the crystal is positioned at the same position of the image shot by the image sensing unit;
the displacement amount of the image sensing unit is proportional to the variation amount of the crystal diameter.
Further, the temperature sensing unit moves along with the image sensing unit, and the displacement amount of the temperature sensing unit is proportional to the displacement amount of the image sensing unit.
Further, the device also comprises a lifting mechanism for lifting the crystal;
the control unit obtains the actual diameter change rate of the crystal according to the diameter change of the crystal, and generates a pull-up adjustment correction amount according to the offset of the actual diameter change rate of the crystal and the preset diameter change rate of the crystal;
and the control unit corrects the lifting speed of the lifting mechanism according to the lifting speed adjustment correction quantity.
Further, the control unit achieves the pull-rate adjustment correction amount using a fixed pull-rate variation amplitude and a fixed pull-rate variation frequency.
The application also provides a preparation method of the monocrystalline silicon, which comprises the following steps:
s1, melting materials, and heating to melt initial raw materials;
s2, seeding, wherein at least part of the seed crystal is immersed below the liquid level of the melt;
s3, necking, namely pulling the seed crystal at a speed in a set moving speed section to perform necking;
s4, shouldering, and controlling heating power and the lifting speed of the seed crystal so as to enable the diameter of the crystal to reach a set diameter;
s5, equal-diameter feeding, and equal-diameter growth of the crystal bar is carried out;
wherein, step S4 further includes:
s41, tracking and obtaining the change of the crystal diameter;
s42, adjusting the heating power according to the diameter change of the crystal and the shouldering time so as to enable the diameter of the crystal to reach a set diameter.
Further, the step S42 further includes:
s421, obtaining the actual temperature of the melt liquid level at a fixed distance from the edge of the crystal;
s422, generating a first power amplitude reduction according to the shouldering time, generating a second power amplitude reduction according to the diameter of the crystal, and generating a power adjustment correction amount according to the offset of the actual temperature of the melt liquid level at a fixed distance from the edge of the crystal and a preset liquid level temperature;
s423, controlling the heating power according to the first power decreasing amplitude, the second power decreasing amplitude and the power adjusting correction amount.
Further, the method further comprises:
acquiring the actual diameter change rate of the crystal according to the diameter change of the crystal, and generating a pull-up adjustment correction amount according to the offset of the actual diameter change rate of the crystal and the preset diameter change rate of the crystal;
and correcting the lifting speed of the lifting mechanism according to the lifting speed adjustment correction quantity.
According to the description, the monocrystalline silicon preparation device and the monocrystalline silicon preparation method provided by the application combine crystal diameter change and shouldering time, and the overall heating power in the shouldering process is adjusted by combining simulation calculation, so that the monocrystalline silicon preparation device and the monocrystalline silicon preparation method have better applicability under different thermal fields. Meanwhile, in large-scale production, the same set of parameters can be used for correcting the difference between equipment, so that the stability of production is ensured.
Drawings
FIG. 1 is a flow chart of a method for preparing monocrystalline silicon according to an embodiment of the present application;
FIG. 2 is a flowchart of step S4 in the method for producing single crystal silicon according to the embodiment of the present application;
FIG. 3 is a flowchart of step S42 in a method for producing a silicon single crystal according to an embodiment of the present application;
fig. 4 is a flowchart of step S43 in the method for preparing single crystal silicon according to the embodiment of the present application;
FIG. 5 is a flowchart of step S5 in the method for producing single crystal silicon according to the embodiment of the present application;
FIG. 6 is a flowchart of step S53 in the method for producing a silicon single crystal according to the embodiment of the present application;
FIG. 7 is a schematic view of an apparatus for producing single crystal silicon according to an embodiment of the present application;
FIG. 8 is a schematic diagram illustrating the working principle of an image sensing unit and a temperature sensing unit according to an embodiment of the present application;
FIG. 9 is a control block diagram of a single crystal silicon manufacturing apparatus according to an embodiment of the present application;
fig. 10 is a schematic view of an apparatus for producing single crystal silicon according to another embodiment of the present application.
Detailed Description
The present application will be described in detail below with reference to the specific embodiments shown in the drawings, but these embodiments are not limited to the present application, and structural, method, or functional modifications made by those skilled in the art based on these embodiments are included in the scope of the present application.
The preparation of monocrystalline silicon often requires the steps of material melting, seeding, necking, shouldering, isodiametric growth and the like. The shoulder placing step and the constant diameter growth step are important steps affecting the finished product of the monocrystalline silicon, and the monocrystalline silicon preparation device provided by the application can provide further control for the crystal growth in the shoulder placing step and the constant diameter growth step in order to improve the yield and the crystal quality. The method comprises the following steps:
as shown in fig. 1, the present application provides a method for preparing single crystal silicon, comprising the steps of:
s1, melting materials, and heating to melt initial raw materials;
s2, seeding, wherein at least part of the seed crystal is immersed below the liquid level of the melt;
s3, necking, namely pulling the seed crystal at a speed in a set moving speed section to perform necking;
s4, shouldering, and controlling heating power and the lifting speed of the seed crystal so as to enable the diameter of the crystal to reach a set diameter;
s5, equal-diameter feeding, and equal-diameter growth of the crystal bar is carried out;
as shown in fig. 2, step S4 further includes:
s41, tracking and obtaining the change of the crystal diameter;
s42, adjusting heating power according to the diameter change of the crystal and the shouldering time so as to enable the diameter of the crystal to reach a set diameter.
S43, adjusting the lifting speed of the lifting mechanism according to the change of the crystal diameter.
Wherein, step S42 and step S43 are not sequential, and the heating power and the pulling speed are adjusted in parallel in the shoulder link.
In the shouldering step, different from the traditional PID operation control method which is set on the basis of the variation of the shoulder length, the monocrystalline silicon preparation method provided by the application integrates the diameter variation and the shouldering time of the crystal, and adjusts the heating power so that the diameter of the crystal reaches the set diameter.
As an alternative implementation, the first power reduction associated with the shoulder time and the second power reduction associated with the crystal growth diameter may be designed based on experimental data statistics, and the first power reduction and the second power reduction may be combined, so that the heating power variation may be controlled.
According to the description, in the shouldering step, the preparation method of monocrystalline silicon provided by the embodiment of the application combines the crystal diameter change and the shouldering time, so that the overall heating power in the shouldering process is adjusted.
The method provided by the application is used for shouldering and cooling in a mode of combining the temperature change corresponding to the crystal diameter with the temperature change in the shouldering time process, so that the temperature deviation + -1.5 kw caused by initial power can be corrected, and the consistency of the shouldering state is ensured.
As shown in fig. 3, as an alternative implementation manner, in the method for preparing monocrystalline silicon provided in the embodiment of the present application, step S42 further includes:
s421, acquiring the actual temperature of the melt liquid level at a fixed distance from the edge of the crystal.
S422, generating a first power amplitude reduction according to the shoulder time, generating a second power amplitude reduction according to the diameter of the crystal, and generating a power adjustment correction amount according to the offset of the actual temperature of the melt liquid level at a fixed distance from the edge of the crystal and the preset liquid level temperature.
S423, controlling the heating power according to the first power decreasing amplitude, the second power decreasing amplitude and the power adjusting correction amount.
According to the above description, in the shoulder-setting step, the heating power is adjusted as a whole by combining the crystal growth diameter and the shoulder-setting time, and the heating power is corrected by comparing the actual temperature of the melt liquid level at a fixed distance from the edge of the crystal with the preset liquid level temperature.
For example, a first power reduction, which is changed (reduced) per hour, and a duration are set according to the shoulder time. Based on the crystal diameter, a second power reduction corresponding to the diameter is generated (for example, the power is reduced by 0.1kw at a crystal diameter of 100mm and the power is reduced by 0.5kw at a crystal diameter of 150 mm). The first power reduction and the second power reduction are combined to control the overall heating power. And further detecting the actual temperature of the melt liquid level at a fixed distance from the edge of the crystal, comparing the actual temperature with a preset liquid level temperature, and correcting the heating power.
The preset liquid level temperature is set according to the diameter of the crystal, and can be obtained through theoretical calculation according to the required diameter acceleration.
Different from the traditional PID mode operation, the preparation method of the monocrystalline silicon provided by the application adopts the combination of simulation calculation to carry out final correction output adjustment (temperature) based on scientific physical quantity (shoulder time and crystal diameter), and has good applicability under different thermal fields. Meanwhile, in large-scale production, the same set of parameters can be used for correcting the difference between equipment, so that the stability of production is ensured.
As an optional implementation manner, in the shoulder-setting step, the method provided by the embodiment of the application controls the pulling speed of the crystal in addition to the heating power. The pulling speed of the crystal can influence the shoulder diameter of the crystal, so that the pulling speed is correspondingly adjusted according to the size of the shoulder diameter or the speed increasing speed.
As shown in fig. 4, step S43 further includes:
s431, acquiring the actual diameter change rate of the crystal according to the diameter change of the crystal, and generating a pull-speed adjusting correction quantity according to the offset of the actual diameter change rate of the crystal and the preset diameter change rate of the crystal;
s432, correcting the lifting speed of the lifting mechanism according to the pulling speed adjustment correction quantity.
When the pulling speed is adjusted, attention is also paid to the change amplitude of the pulling speed, and the excessive change amplitude of the pulling speed can lead to the adjustment of parameters related to the diameter of the shoulder. For example: the temperature can be regulated in the opposite direction (the diameter increases fast and cools down slowly).
As an optional implementation manner, in the method for preparing monocrystalline silicon provided by the embodiment of the application, a fixed pull rate variation amplitude and a fixed pull rate variation frequency are adopted for adjusting the pull rate to achieve a pull rate adjustment correction amount.
Specifically, in the embodiment of the present application, the first pull-rate variation amplitude and the first pull-rate variation frequency may be set. When the pull rate adjustment correction amount is generated, the pull rate is adjusted stepwise according to the first pull rate variation amplitude and the first pull rate variation frequency, so as to finally achieve the pull rate adjustment correction amount. By means of the pull-up adjustment mode, parameters related to the shoulder diameter can be prevented from being adjusted due to the fact that the pull-up change amplitude is too large.
Compared with the traditional PID control pulling speed regulation, in the monocrystalline silicon preparation method provided by the embodiment of the application, the pulling speed does not forcedly regulate the shouldering form according to the overall trend (crystal diameter) and the stage trend change (crystal diameter change rate), the shouldering is carried out in a natural form of a thermal field, the pulling speed slowly approaches the requirement of the current crystal diameter state, the stability of shouldering is ensured, and the shouldering survival rate can be improved to a certain extent.
In the step S5, in the step of equal diameter growth of the ingot, in the method for preparing monocrystalline silicon provided by the embodiment of the application, the monocrystalline silicon rod can be pulled according to a constant pulling rate, and the diameter of the ingot can be adjusted by controlling the heating power.
As an alternative implementation mode, a weighing method can be adopted to obtain the increment of the crystal or the decrement of the melt, so that the temperature control in the crystal growth furnace is realized, and the crystal diameter is finally controlled.
The weighing method can be divided into an upper weighing method and a lower weighing method, wherein the lower weighing method is used for determining the growth condition of crystals by weighing the weight change amounts of the crucible body and the melt. The upper weighing rule is to weigh the weight change of the sum of the seed rod and the crystal rod to determine the growth condition of the crystal.
In the process of controlling the equal diameter growth of the crystal by a weighing method, the pulling speed of the crystal is kept constant, and the weight change of the crystal or the weight change of the melt in the crucible is weighed, so that the actual growth rate of the crystal can be calculated according to the weight change of the crystal or the weight change of the melt. The growth rate, i.e., the crystal growth rate, refers to the weight increased per unit time. On the premise of keeping the pulling speed of the crystal unchanged, the heating power is regulated to maintain the actual crystal growth rate, so that the isodiametric growth of the crystal can be realized. That is, during this process, it is desirable to maintain the crystal growth rate at a constant level.
However, the actual growth rate of the crystal fluctuates due to high temperature characteristics of the crystal during growth, delay in control, and complexity of the environment.
As shown in fig. 5, as an alternative implementation manner, step S5 includes:
s51, presetting a crystal growth rate according to the set crystal diameter and the pulling speed of the crystal bar;
s52, weighing the weight change of the crystal or the weight change of the melt in the crucible by using a weighing method, and calculating the actual growth rate of the crystal according to the weight change of the crystal or the weight change of the melt;
and S53, when the actual crystal growth rate is larger than the preset crystal growth rate, the crystal growth rate is too fast, the crystal diameter tends to be large, and at the moment, the heating power is controlled to be increased so as to inhibit the crystal growth. When the actual crystal growth rate is smaller than the preset crystal growth rate, the crystal growth rate is too slow, and the crystal diameter tends to be reduced, and at this time, the heating power is controlled to be reduced so as to promote the crystal growth.
However, during the heating power control process, the temperature to affect the solid-liquid growth interface needs to go through the following stages: the first stage is that a heater transmits heat to the outer wall of the crucible by means of heat radiation; the second stage mainly depends on heat conduction, and heat is transferred to the inner surface of the inner crucible through the outer wall of the crucible; and in the third stage, the coupling effect of heat radiation, heat conduction and heat convection exists in the melt, and the heat exchange is carried out on the surface of the melt and argon in the furnace body only by virtue of radiation heat dissipation. Therefore, there is a case where the effect is delayed by controlling the heating power of the main heater surrounding the crucible to affect the temperature of the solid-liquid growth interface. In addition, as the thermal field size increases, the problem of delayed action effect becomes more obvious, resulting in a gap between the actual output time of power and the temperature response time, and a problem of incapability of accurately controlling temperature.
In addition, the heating power of the main heater surrounding the crucible is frequently changed, so that the aging of the crucible is easily accelerated, and the service life of the crucible is consumed.
Based on the above problems, the embodiment of the application provides a method for preparing monocrystalline silicon. The method comprises the following steps:
the heating power is provided by at least two heating units, wherein,
the main heating unit is arranged in the crystal growth furnace body and is positioned outside the crucible;
the auxiliary heating unit is positioned between the crucible and the guide cylinder and is positioned above the liquid level of the melt and used for heating the melt;
the power of the main heating unit and/or the auxiliary heating unit is controlled to enable the crystal to grow in equal diameter, and the auxiliary heating unit is preferably selected to be controlled when the heating power is controlled.
As an alternative implementation, the main heating unit may comprise a first heater and a second heater. Wherein, the first heater is arranged in the crystal growing furnace body and is positioned below the crucible, and the second heater is arranged in the crystal growing furnace body and surrounds the side wall of the crucible.
The auxiliary heating unit comprises a third heater, wherein the third heater is positioned between the crucible and the guide cylinder and is positioned above the liquid level of the melt and used for heating the melt.
In another alternative implementation, the main heating unit may include only a second heater surrounding the crucible sidewall. In the embodiment of the present application, a scheme in which the main heating unit includes a first heater and a second heater is preferably adopted.
The main heating unit assumes most of the heating power during heating. The auxiliary heating unit distributes part of heating power in the heating process and mainly plays a role in temperature regulation.
The temperature of the melt liquid level can be changed more quickly by directly radiating heat to the melt liquid level, and the control delay is shortened, so that the constant diameter growth of crystals is controlled more favorably.
As shown in fig. 6, as an alternative implementation manner, according to the method provided by the present application, step S53 further includes:
s531, when the actual crystal growth rate is greater than the preset crystal growth rate, controlling the auxiliary heating unit to increase the power;
s532, when the actual crystal growth rate is smaller than the preset crystal growth rate, the auxiliary heating unit is controlled to reduce power.
And S533, when the heating power is adjusted to be out of the adjusting capacity range of the auxiliary heating unit, adjusting the power of the main heating unit.
According to the monocrystalline silicon preparation method provided by the embodiment of the application, the auxiliary heating unit which can directly radiate heat to the liquid surface of the melt is additionally designed, the auxiliary heating unit is preferentially regulated in the equal-diameter growth link of crystals, and the power regulation of the main heating unit surrounding the crucible is reduced as much as possible, so that the service life of the crucible can be effectively prolonged.
In addition, relatively severe temperature fluctuations often occur when there is too little residue in the crucible, for example, when the melt level enters below the crucible R angle. The reason for the temperature fluctuation is mainly as follows: when the crystal is prepared, the magnetic field is used for inhibiting the thermal convection of the melt, so that the stability of the temperature is ensured, and when the liquid level of the melt enters below the R angle of the crucible, the residual amount in the crucible is small, and the inhibiting effect of the magnetic field is easily affected due to the change of the shape of the crucible, so that the thermal convection of the melt is moved, and the temperature change is caused.
Convection mainly occurs inside the melt, and if it is desired to adjust the power of the main heating unit to further affect the melt level temperature, the power adjustment of the main heating unit surrounding the crucible is not ideal for controlling the melt level temperature due to the influence of convection. Moreover, due to the hysteresis of the heater acting on adjusting the temperature of the solid-liquid interface of the melt, severe fluctuation of the diameter and the pulling speed often occurs, and the quality of the semiconductor single crystal silicon rod is greatly influenced.
In this regard, the method for preparing monocrystalline silicon provided by the embodiment of the application comprises the following steps:
and when the residual amount in the crucible is lower than a preset allowance threshold (for example, when the melt liquid level enters the crucible under the R angle), the ratio of the heating power of the auxiliary heating unit in the overall heating power is increased, wherein the overall heating power is the sum of the heating powers of the main heating unit and the auxiliary heating unit. That is, the overall heating power is the sum of the heating powers of the first heater, the second heater, and the third heater. The auxiliary heating unit keeps a larger power, and the influence of the power regulation effect of the auxiliary heating unit on the melt liquid level temperature is enhanced so as to maintain the melt surface temperature stable.
For example, the power of the secondary heating unit may be in the range of 10-20kw. As an alternative implementation, the power adjustable range of the auxiliary heating unit is designed to be related to the area of the melt liquid surface, and the larger the melt liquid surface area is, the corresponding maximum power of the auxiliary heating unit is required to be increased.
The method provided by the application directly radiates heat to the liquid level of the melt through the auxiliary heating unit, so that the temperature of a solid-liquid interface is changed rapidly, the method has more direct effect on the temperature of the melt, is free from the limitation of the size of a thermal field, and has no adjustable hysteresis and inertia of thermal field reaction, thereby keeping the actual growth rate of crystals stable and realizing the equal-diameter growth of the crystals at a constant pulling rate.
When the residual quantity is small, the method provided by the application does not need to transfer heat conducted from the crucible to the liquid level through convection, when the magnetic field acts and causes the temperature fluctuation of the melt due to the small residual quantity, the power of the auxiliary heating unit directly radiating the surface of the melt is regulated according to the temperature of the liquid level so as to maintain the temperature of the liquid level or raise the temperature, thereby having the effect of restraining and compensating more rapidly, reducing the fluctuation interval of the diameter and the pulling speed and avoiding the large expansion and contraction of the crystal diameter.
As shown in fig. 7, according to the method for preparing single crystal silicon provided by the embodiment of the present application, the present application also provides a single crystal silicon preparation apparatus 100, which includes a crystal growth furnace body 11, a crucible 12, a lifting mechanism (not shown in the figure), a guide cylinder 13, a heating unit 14, and a control unit (not shown in the figure).
Wherein an accommodating space is defined in the crystal growing furnace body 11.
A crucible 12 is provided in the accommodation space for melting the polycrystalline silicon raw material and holding the silicon melt.
A lifting mechanism is provided above the crucible 12 for vertically lifting and lowering the seed crystal and extending the seed crystal into the melt to directly elongate the crystal to obtain crystal 101.
A guide cylinder 13 is provided above the crucible 12 and surrounds a portion of the crystal 101.
A heating unit 14 for heating the crucible 12 to provide a temperature required for preparing the crystal 101.
And the control unit is used for controlling the heating power and the pulling speed so as to directly lengthen the crystal to obtain the crystal bar.
As an alternative implementation manner, in the shouldering step, unlike the conventional PID operation control method set based on the variation of the shoulder length, the single crystal silicon preparation apparatus 100 provided by the present application synthesizes the variation of the diameter of the crystal 101 and the shouldering time, and adjusts the heating power so that the diameter of the crystal 101 reaches the set diameter.
With reference to fig. 8 and fig. 9, as an alternative implementation manner, an apparatus provided by an embodiment of the present application further includes: an image sensing unit 16 for tracking the diameter variation of the acquisition crystal 101. So that the control unit 15 can adjust the power of the heating unit 14 according to the diameter variation of the crystal 101 and the shoulder time so that the diameter of the crystal 101 reaches the set diameter.
As an alternative implementation, the apparatus provided in the embodiment of the present application further includes a temperature adjustment correction unit 18. The temperature adjustment correction unit 18 may design a first power reduction amplitude related to the shoulder time and a second power reduction amplitude related to the growth diameter of the crystal 101 based on experimental data statistics, and combine the first power reduction amplitude and the second power reduction amplitude, so that the control unit 15 may control the power variation of the heating unit 14.
As an alternative implementation manner, the single crystal silicon manufacturing apparatus 100 provided in the embodiment of the present application further includes a temperature sensing unit 17, where the temperature sensing unit 17 is configured to obtain the actual temperature of the melt level 102 at a fixed distance from the edge of the crystal 101. The temperature adjustment correction unit 18 may generate the power adjustment correction amount according to an offset amount of the actual temperature of the melt level 102 from the preset level temperature by a fixed distance from the edge of the crystal 101. Wherein the preset liquid level temperature is set according to the actual diameter of the crystal 101.
The control unit 15 may control the power of the heating unit 14 according to the first power reduction, the second power reduction, and the power adjustment correction amount.
As an alternative implementation, the device provided by the embodiment of the present application further includes a horizontal driving mechanism 19. The horizontal driving mechanism 19 is used to drive the image sensing unit 16 to move in the radial direction of the crystal 101 in a plane substantially parallel to the melt level 102 so that the edge of the crystal 101 is located at the same position of the image captured by the image sensing unit 16.
In particular, in an ideal case, the image sensing unit 16 moves in a plane parallel to the melt level 102, and the direction of movement of the image sensing unit 16 is along the radial direction of the crystal 101. When the image sensing unit 16 tracks the diameter of the crystal 101 at a fixed angle, the image sensing unit 16 is also displaced accordingly as the crystal 101 grows in order to keep the edge of the crystal 101 at the same position as the captured image, and in this case, the displacement amount of the image sensing unit 16 is proportional to the change amount of the diameter of the crystal 101 (for example, the displacement amount of the image sensing unit 16 is equal to the change amount of the diameter of the crystal 101), so that the change of the diameter of the crystal 101 can be obtained easily by measuring the displacement amount of the image sensing unit 16.
As an alternative implementation, the image sensing unit 16 may be a camera or a CCD.
As an alternative implementation, the displacement amount of the temperature sensing unit 17 is proportional to the displacement amount of the image sensing unit 16. For example, the temperature sensor 17 and the image sensor 16 may be connected to each other, and the relative position between the temperature sensor 17 and the image sensor 16 may be kept fixed, and at this time, the temperature sensor 17 moves along with the image sensor 16. The detection angle of the temperature sensor unit 17 is adjusted such that it forms a fixed angle with the melt level 102 during movement. In this way, the actual temperature of the melt level 102 at a fixed distance from the edge of the crystal 101 can be obtained relatively simply.
As an alternative implementation, the temperature sensing unit 17 may be an infrared temperature sensor.
As shown in fig. 8, in an alternative implementation, in the apparatus provided in the embodiment of the present application, the horizontal driving mechanism 19 includes a bracket 191, a screw 192, a guide rail 193, and a slider 194.
Wherein the bracket 191 provides a location for mounting the guide rail 193 and the screw 192. A guide rail 193 is mounted on the support 191 substantially parallel to the melt level 102 for providing a guide for the movement of the slider 194 that guides radially of the crystal 101. The screw 192 is mounted on the bracket 191 in parallel with the guide rail 193. The stepper motor 195 drives the slider 194 to move through the screw 192. The image sensing unit 16 and the temperature sensing unit 17 may be provided on the slider 194 such that the movement of the image sensing unit 16 and the temperature sensing unit 17 may be controlled by the stepping motor 195.
In the shoulder stage, in addition to the heating power control, the pulling rate of the crystal 101 needs to be controlled.
As an alternative implementation manner, the control unit 15 obtains the actual diameter change rate of the crystal 101 according to the diameter change of the crystal 101, and generates a pull-speed adjustment correction amount according to the offset between the actual diameter change rate of the crystal 101 and the preset diameter change rate of the crystal 101;
the control unit 15 corrects the lifting speed of the lifting mechanism based on the pulling speed adjustment correction amount.
As an alternative implementation, in the shoulder-setting step, the control unit 15 uses a fixed pull-rate variation amplitude and a fixed pull-rate variation frequency to achieve the pull-rate adjustment correction.
For example, in the embodiment of the present application, the control unit 15 is provided with a first pull-speed variation amplitude and a first pull-speed variation frequency. When the control unit 15 generates the pull-speed adjustment correction amount, the control unit 15 controls the lifting mechanism to stepwise adjust the pull-speed stepwise according to the first pull-speed variation amplitude and the first pull-speed variation frequency, so as to finally achieve the pull-speed adjustment correction amount.
According to the monocrystalline silicon preparation method and device provided by the application, the crystal 101 pulling speed is adjusted by utilizing the diameter change of the crystal 101, the diameter of the crystal 101 and the shouldering time are combined to regulate and control the heating power, so that the shouldering link is controlled, and the shouldering survival rate is improved.
As shown in fig. 10, in an alternative implementation manner, in the single crystal silicon manufacturing apparatus 100 provided in the embodiment of the present application, the heating unit 14 includes a main heating unit 141 and a sub heating unit 142. Wherein the main heating unit 141 includes a first heater 1411 and a second heater 1412, and the sub-heating unit 142 includes a third heater 142.
As an alternative implementation, the first heater 1411 is provided within the crystal growing furnace body 11 and below the crucible 12. The second heater 1412 is provided in the crystal growing furnace body 11 and surrounds the side wall of the crucible 12. A third heater 142 is located between crucible 12 and guide cylinder 13 above melt level 102 for heating the melt.
Among them, the first heater 1411 and the second heater 1412 may serve as main heaters, and bear most of heating power. The third heater 142 may radiate heat directly to the melt level 102, splitting part of the heating power.
As an alternative implementation, the control unit 15 is configured to control the power of one or more of the first heater 1411, the second heater 1412, and the third heater 142 to grow the crystal 101 in an equal diameter. Wherein the control unit 15 preferentially selects to control the third heater 142 when controlling the power of the heating unit 14.
Specifically, the control unit 15 mainly adjusts the power of the third heater 142 to rapidly influence the temperature gradient of the crystal 101 and the solid-liquid growth interface, so as to enhance the control effect of the power variation on the diameter.
For example, the power of the third heater 142 is preferentially controlled at a constant pull rate to control the actual growth rate of the crystal 101, and when the actual growth rate of the crystal 101 is greater than the preset crystal 101 growth rate, the control unit 15 controls the third heater 142 to increase the power, and when the actual growth rate of the crystal 101 is less than the preset crystal 101 growth rate, the control unit 15 controls the third heater 142 to decrease the power.
Wherein the preset crystal 101 growth rate is designed according to the pull rate and the diameter of the desired crystal 101 growth.
As an alternative implementation, when the heating power adjustment is outside the adjustment capability range of the third heater 142, the power of the first heater 1411 and/or the second heater 1412 is adjusted.
For example, the first heater 1411, the second heater 1412, and the third heater 142 collectively provide an overall heating power, wherein the third heater 142 provides a first heating power, and the maximum heating power that the third unit can provide is a second heating power. When the control unit 15 adjusts the overall heating power, the third heater 142 is preferentially adjusted.
In the case of increasing the heating power, if the adjustment amount of the heating power is larger than the difference between the second heating power and the first heating power, the heating power is adjusted to be out of the adjustment capability range of the third heater 142, and the power of the first heater 1411 and/or the second heater 1412 needs to be adjusted in cooperation.
In the case of reducing the heating power, if the adjustment amount of the heating power is larger than the first heating power, the heating power is adjusted beyond the adjustment capability range of the third heater 142, and the power of the first heater 1411 and/or the second heater 1412 needs to be adjusted in cooperation.
As an alternative implementation manner, the third heater 142 provided in the embodiment of the present application may perform a temperature adjustment function in the equal diameter growth link of the crystal 101, and may also perform a temperature adjustment function in the shoulder-placing link.
According to the above description, the single crystal silicon manufacturing apparatus 100 provided by the embodiment of the present application preferentially controls the power of the third heater that directly radiates heat to the melt level 102 to enhance the control effect of the power variation on the diameter. And, this approach greatly reduces the frequency of power adjustments to the first and second heaters 1411, 1412 during the production process, and serves to protect the crucible 12 to some extent, delaying the life of the crucible 12.
As an alternative implementation manner, the monocrystalline silicon preparation apparatus 100 further includes a thermal energy reflection housing (not shown in the drawing), and the thermal energy reflection housing is located above the third heater 142, and is used for controlling the heat output direction of the third heater 142, so that the heat output direction of the third heater 142 is substantially directed to the melt level 102. In this way, the effect of the power regulation of the third heater 142 on the temperature of the melt level 102 may be enhanced.
As an alternative implementation, the third heater 142 may be connected to the first heater 1411 and/or the second heater 1412, powered by the same power source.
As another alternative implementation, third heater 142 may be coupled to barrel 13 such that third heater 142 may be raised and lowered along with barrel 13, thereby controlling the distance between third heater 142 and melt level 102.
As an alternative implementation, the third heater may be lowered as the melt level 102 is lowered to maintain the distance between the third heater 142 and the melt level 102 within a preset range.
As an alternative implementation manner, the single crystal silicon preparation device 100 provided by the application can draw a crystal rod at a constant pulling rate in the equal diameter growth link of the crystal 101, and the growth rate of the crystal rod is controlled by adjusting the heating power.
As an alternative implementation manner, the single crystal silicon manufacturing apparatus 100 provided by the present application further includes a weighing mechanism (not shown in the figure).
In one embodiment, a weighing mechanism is provided for weighing the crucible 12 and the amount of change in weight of the melt. In another embodiment, the weighing mechanism is configured to weigh the amount of weight change of the sum of seed rods and crystal 101 rods. Both weighing methods can determine the amount of growth of the crystal 101 per unit time (i.e., the growth rate of the crystal 101) based on the amount of weight change measured. At a constant pulling rate, the constant diameter growth of the crystal 101 can be realized by adjusting the heating power to keep the growth rate of the crystal 101 stable at a preset value.
As an alternative implementation, the weight change of the melt or the weight change of the crystal 101 is weighed by the weighing mechanism, so that the amount of the residual material in the crucible 12 can be further determined, and when the amount of the residual material in the crucible 12 is small (for example, when the melt level 102 enters below the R angle 103 of the crucible 12), the third heater 142 maintains a large power, so that the influence of the power adjustment effect of the third heater 142 on the temperature of the melt level 102 is enhanced, so as to maintain the temperature stability of the melt surface.
As an alternative implementation manner, in the step of equal diameter growth of the crystal 101, the growth condition of the crystal 101 can be further confirmed by the image sensing unit 16 provided by the present application. At the same time, the temperature of melt level 102 may also be detected by image sensing unit 16.
In summary, in the shoulder-setting step, the single crystal silicon preparation apparatus 100 and the method provided by the application combine with analog calculation according to the diameter change of the crystal 101 and the shoulder-setting time, so that the overall heating power in the shoulder-setting process is adjusted, and the single crystal silicon preparation apparatus has better applicability under different thermal fields. In addition, in the constant diameter growth link, the third heater 142 which directly radiates heat to the melt liquid level 102 is added, and the temperature of the melt liquid level 102 is rapidly influenced by adjusting the power of the third heater 142, so that the temperature of the melt liquid level 102 can be stabilized after the melt liquid level 102 enters the R angle 103 or below, and the diameter of the crystal 101 is prevented from expanding and shrinking greatly.
The above disclosure is illustrative of the preferred embodiments of the present application, but it should not be construed as limiting the scope of the application as will be understood by those skilled in the art: changes, modifications, substitutions, combinations, and simplifications may be made without departing from the spirit and scope of the application and the appended claims, and equivalents may be substituted and still fall within the scope of the application.
Claims (8)
1. An apparatus for producing single crystal silicon, the apparatus comprising:
a crucible for holding a melt to prepare a crystal;
a heating unit for heating the crucible to provide a temperature required for preparing the crystal;
characterized in that the device further comprises:
an image sensing unit for tracking and acquiring the diameter change of the crystal;
the control unit is used for adjusting the power of the heating unit according to the diameter change and the shouldering time of the crystal so as to enable the diameter of the crystal to reach a set diameter;
the single crystal silicon manufacturing apparatus further includes:
the temperature sensing unit is used for acquiring the actual temperature of the melt liquid level at a fixed distance from the edge of the crystal;
the temperature regulation and correction unit is used for generating a first power reduction according to the shouldering time, generating a second power reduction according to the diameter of the crystal, and generating a power regulation and correction amount according to the offset of the actual temperature of the melt liquid level at a fixed distance from the edge of the crystal and the preset liquid level temperature;
the control unit controls the power of the heating unit according to the first power reduction, the second power reduction and the power adjustment correction amount.
2. The apparatus according to claim 1, wherein the preset liquid surface temperature is set according to a crystal diameter.
3. The apparatus according to claim 1, further comprising a horizontal driving mechanism for driving the image sensing unit to move in a radial direction of the crystal in a plane substantially parallel to a melt level so that edges of the crystal are located at the same position of an image taken by the image sensing unit;
the displacement amount of the image sensing unit is proportional to the variation amount of the crystal diameter.
4. A single crystal silicon manufacturing apparatus according to claim 3, wherein the temperature sensing unit moves following the image sensing unit, and the displacement amount of the temperature sensing unit is proportional to the displacement amount of the image sensing unit.
5. The apparatus for producing single crystal silicon according to claim 1, further comprising a lifting mechanism for pulling up the crystal;
the control unit obtains the actual diameter change rate of the crystal according to the diameter change of the crystal, and generates a pull-up adjustment correction amount according to the offset of the actual diameter change rate of the crystal and the preset diameter change rate of the crystal;
and the control unit corrects the lifting speed of the lifting mechanism according to the lifting speed adjustment correction quantity.
6. The apparatus for producing a single crystal silicon according to claim 5, wherein,
the control unit achieves the pull-rate adjustment correction amount using a fixed pull-rate variation amplitude and a fixed pull-rate variation frequency.
7. A method for producing single crystal silicon, the method comprising:
s1, melting materials, and heating to melt initial raw materials;
s2, seeding, wherein at least part of the seed crystal is immersed below the liquid level of the melt;
s3, necking, namely pulling the seed crystal at a speed in a set moving speed section to perform necking;
s4, shouldering, and controlling heating power and the lifting speed of the seed crystal so as to enable the diameter of the crystal to reach a set diameter;
s5, equal-diameter feeding, and equal-diameter growth of the crystal bar is carried out;
wherein, step S4 further includes:
s41, tracking and obtaining the change of the crystal diameter;
s42, adjusting the heating power according to the diameter change of the crystal and the shouldering time so as to enable the diameter of the crystal to reach a set diameter;
the step S42 further includes:
s421, obtaining the actual temperature of the melt liquid level at a fixed distance from the edge of the crystal;
s422, generating a first power amplitude reduction according to the shouldering time, generating a second power amplitude reduction according to the diameter of the crystal, and generating a power adjustment correction amount according to the offset of the actual temperature of the melt liquid level at a fixed distance from the edge of the crystal and a preset liquid level temperature;
s423, controlling the heating power according to the first power decreasing amplitude, the second power decreasing amplitude and the power adjusting correction amount.
8. The method for producing a single crystal silicon according to claim 7, characterized in that the method further comprises:
acquiring the actual diameter change rate of the crystal according to the diameter change of the crystal, and generating a pull-up adjustment correction amount according to the offset of the actual diameter change rate of the crystal and the preset diameter change rate of the crystal;
and correcting the lifting speed of the lifting mechanism according to the lifting speed adjustment correction quantity.
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| WO2008128378A1 (en) * | 2007-04-19 | 2008-10-30 | Tianjin Huanou Semiconductor Material And Technology Co., Ltd. | Vertical pulling and zone melting method for producing monocrystalline silicon |
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| CN113818075A (en) * | 2021-09-24 | 2021-12-21 | 西安奕斯伟材料科技有限公司 | Method, device and equipment for accurately adjusting ADC camera and computer storage medium |
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| WO2008128378A1 (en) * | 2007-04-19 | 2008-10-30 | Tianjin Huanou Semiconductor Material And Technology Co., Ltd. | Vertical pulling and zone melting method for producing monocrystalline silicon |
| KR20150036923A (en) * | 2013-09-30 | 2015-04-08 | 주식회사 엘지실트론 | Ingot growing controller and ingot growing control method for it |
| CN109183141A (en) * | 2018-10-29 | 2019-01-11 | 上海新昇半导体科技有限公司 | A kind of crystal growth control method, device, system and computer storage medium |
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Effective date of registration: 20231205 Address after: 312300 No. 218 Tongjiang West Road, Shangyu District, Shaoxing, Zhejiang. Patentee after: ZHEJIANG JINGSHENG M&E Co.,Ltd. Patentee after: ZHEJIANG QIUSHI SEMICONDUCTOR EQUIPMENT Co.,Ltd. Patentee after: Ningxia Jingchuang Intelligent Equipment Co.,Ltd. Address before: 311100 Room 102, building 1, No. 500, Shunda Road, Linping street, Linping District, Hangzhou City, Zhejiang Province Patentee before: ZHEJIANG QIUSHI SEMICONDUCTOR EQUIPMENT Co.,Ltd. |