CN117364225B - Crystal growing method by co-rotating crystal and crucible - Google Patents
Crystal growing method by co-rotating crystal and crucible Download PDFInfo
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- CN117364225B CN117364225B CN202311672479.9A CN202311672479A CN117364225B CN 117364225 B CN117364225 B CN 117364225B CN 202311672479 A CN202311672479 A CN 202311672479A CN 117364225 B CN117364225 B CN 117364225B
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- 239000013078 crystal Substances 0.000 title claims abstract description 260
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000001301 oxygen Substances 0.000 claims abstract description 59
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 59
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 58
- 235000014347 soups Nutrition 0.000 claims abstract description 40
- 238000010899 nucleation Methods 0.000 claims abstract description 18
- 230000008569 process Effects 0.000 claims abstract description 12
- 239000000155 melt Substances 0.000 claims description 23
- 238000002844 melting Methods 0.000 claims description 17
- 230000008018 melting Effects 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 15
- 238000001514 detection method Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 7
- 230000007704 transition Effects 0.000 claims description 7
- 230000006641 stabilisation Effects 0.000 claims description 6
- 238000011105 stabilization Methods 0.000 claims description 6
- 230000006698 induction Effects 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 230000035939 shock Effects 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims 1
- 238000002109 crystal growth method Methods 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 4
- 238000001556 precipitation Methods 0.000 abstract description 2
- 238000004088 simulation Methods 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 11
- 238000009826 distribution Methods 0.000 description 10
- 230000001276 controlling effect Effects 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 238000009792 diffusion process Methods 0.000 description 6
- 230000000087 stabilizing effect Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 230000033228 biological regulation Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- -1 oxygen ions Chemical class 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000009827 uniform distribution 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
-
- 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
- C30B15/10—Crucibles or containers for supporting the melt
-
- 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
- C30B15/30—Mechanisms for rotating or moving either the melt or the crystal
-
- 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
Abstract
The invention discloses a crystal growth method by rotating crystals and a crucible in the same direction, belongs to the field of crystal growth, and relates to a crystal growth method capable of effectively controlling the oxygen content of a crystal bar. In the crystal growth process, crystal growth is carried out by adopting a mode that a crucible and a crystal rotate in the same direction, the crucible is started to rotate at a stable temperature before seeding, the rotation directions of the crucible and the crystal are the screwing directions of seed crystals arranged on a seed crystal shaft, the rotation speeds of the crystal and the crucible are set in stages according to the Reynolds coefficient ratio of the crystal to molten soup in the shouldering process, and a better solution is provided for PID setting in the shouldering stage. In the isodiametric step, the optimal crucible and crystal rotation speed is maintained according to the simulation result until ending. Through the adjustment of the rotation speeds of the crystal and the crucible and the cooperation of temperature PID adjustment, a mode that the crystal and the crucible rotate in the same direction is developed to perform crystal growth, so that the oxygen content of the crystal bar is effectively reduced, the resistivity of the crystal bar is optimized, and related oxygen precipitation defects are avoided.
Description
Technical Field
The invention belongs to the field of crystal growth, and particularly relates to a crystal growth method by which crystals and a crucible rotate in the same direction.
Background
The Czochralski method (CZ method) is the current mainstream crystal growth method, and as the microelectronics industry rapidly progresses, the demand for large diameter and high quality crystals increases.
Oxygen is the most common impurity in the crystal growth process, and the too high oxygen concentration can cause different degrees of crystal quality problems for different crystals. For lithium niobate crystals, the higher the concentration of oxygen ions in lithium niobate, the more unblocked the ion conducting channels, and thus the conductivity thereof is also greatly affected. Moreover, too high partial pressure of oxygen may also cause a change in the crystal structure of lithium niobate, which is detrimental to the crystal quality. For crystals such as monocrystalline silicon, the oxygen concentration also greatly affects the crystal quality, and high oxygen concentration can cause degradation of the solar cell and warpage of the silicon wafer, and in addition, oxide precipitates are formed during the growth process, dislocation is generated in the crystal, and thus metal impurities are accumulated. Therefore, in order to produce high quality, low cost crystals, it is necessary to control the crystal oxygen content by improving the crystal growth process.
In the existing crystal growth process, the rotation direction of the crystal and the crucible is opposite, and the oxygen transportation condition in the melt flow is greatly affected by the rotation of the crystal and the crucible. The crystal crucible rotates in the same direction to enable the molten soup to have higher critical thermal capillary Reynolds number, and the thermal capillary flow can be more stable than the reverse rotation of the crystal crucible. The taylor cell is inverted when the crystal is rotated equidirectionally faster than the crucible, and vice versa when the crystal is rotated slower than the crucible. During the growth process. The oxygen concentration along the solid-liquid interface is affected by competition between convection and diffusion mechanisms, with melt flow being more sensitive to crystal rotation speed in the case of rotation of the crystal at the same speed as the crucible. At small rotational speed differences between crucible and crystal, the effect of diffusion becomes stronger than the effect of convection on oxygen transport. In this case, if the unit cell flow under the crystal is positive, oxygen diffusion from the region under the free melt surface to the growth interface can be prevented, and the oxygen concentration at the solid-liquid interface will be reduced.
To solve the above problems, the invention patent publication No. CN106319620B discloses a method for pulling a Czochralski crystal, which can improve the quality of the ingot and increase the efficiency. However, in the case where the crystal is rotated in the opposite direction to the crucible, the maximum melt velocity is farther from the edge of the crystal, and stable convection is formed as the rotation rate of the crystal is changed. Compared with the reverse direction, the convection of the melt is obviously weakened in the same direction, the oxygen concentration distribution is also obviously weakened, and the transportation of oxygen in the melt is mainly influenced by diffusion, and the evaporated oxygen content on the surface of the free melt is much larger than the oxygen content absorbed on the surface of the free melt. The invention patent publication No. CN100374628C discloses a method and apparatus for growing a silicon single crystal, a silicon single crystal and a silicon semiconductor wafer, which describe a method for growing a crystal by rotating a single crystal and a crucible in the same direction, but the method does not take into consideration control of the oxygen content of the crystal, and as the rotation speed of the crystal increases, the concentration flux at the solid-liquid interface increases toward the surface of the free melt, wherein the oxygen content increases and the oxygen content distribution is more dispersed.
Disclosure of Invention
The invention aims at a crystal growing method for controlling the oxygen content of crystals by rotating the crystals and a crucible in the same direction.
The invention provides a crystal growing method by rotating crystals and a crucible in the same direction, which comprises the following steps:
a. the preparation step comprises the following steps: placing raw materials into a crucible of a crystal growth furnace, installing seed crystals, vacuumizing a furnace table for leak detection, melting and stabilizing the temperature, and simultaneously starting the seed crystals and the crucible to rotate in the same direction;
b. and (3) seeding: inserting a seed crystal into the melt, reducing the temperature to enable the melt to start to crystallize under the induction of the seed crystal, and increasing the rotating speed of the crucible to a certain value;
c. shoulder placing: starting shouldering, maintaining the rotation speed of the crucible unchanged, gradually increasing the rotation speed of the crystal until reaching a target rotation speed, ensuring that the rotation speed of the crystal is smaller than the rotation speed of the crucible, and maintaining a constant rotation speed difference, and setting the rotation speed of the crystal in a segmentation mode according to the shouldering length at the moment, wherein when the shoulder does not pass through an appearance inflection point in the earlier stage of shouldering, the e (t) value in the temperature PID is adjusted upwards, and when the shoulder passes through the appearance inflection point and enters the shoulder rotating process, the e (t) value in the temperature PID is adjusted downwards, so that thermal shock is reduced;
d. and (3) an isodiametric step: starting constant diameter growth, maintaining constant rotation speed difference, optimizing a crystal growth temperature curve, and adjusting the e (t) value in the temperature PID when the molten soup liquid level descends and passes through the vertical crucible wall, wherein the e (t) value in the temperature PID is adjusted downwards when the molten Shang Yemian passes through a transition zone of the arc profile at the bottom of the crucible;
e. ending: after the grown crystal is detached from the melt Shang Yemian, the ingot is cooled.
Preferably, in the preparing step, before melting, the crucible rotation speed is increased by adopting a step-type numerical value increasing method, namely 0-0.5 rpm is increased every 1-10 s, the final crucible rotation speed is not more than 5rpm, and melting is completed under the crucible rotation speed;
preferably, the preparing step is to put raw materials into a crucible of a crystal growth furnace, mount seed crystals on a seed crystal shaft, close a furnace chamber, vacuumize the furnace body, and charge inert gas, increase the power of the crystal growth furnace to the melting power, start the crucible to rotate and increase the rotation speed of the crucible to a target value, and make the rotation direction of the crucible and the screwing direction of the seed crystals on the seed crystal shaft be the same direction until melting is completed to form molten soup, and in order to avoid non-uniform melting of the bulk materials in the melting process, the mode of piling up the materials at the bottom of the crucible and piling up small materials in the upper layer area is adopted, and the materials are uniformly placed; the pressure of the furnace chamber after the vacuum pumping is neededLeak rate is requiredThe magnetic field is set to 123+/-0.3A, and the inert gas is one of Ar gas and He gas;
preferably, in the preparing step, the seed crystal is required to be reduced to a position close to the melting point Shang Yemian during temperature stabilization, the power of the crystal growth furnace is reduced to the temperature stabilization power, the temperature of molten soup is reduced to a target temperature, the target temperature is taken as a central value, the temperature tolerance is within +/-20 ℃, then a magnetic field of the crystal growth furnace is started, the seed crystal is started to rotate, the rotating speed of the crucible is further increased, and the rotating direction of the seed crystal and the rotating direction of the crucible are the screwing direction of a seed crystal shaft.
Preferably, in the seeding step, the diameter of the seeding crystals is controlled to be 4-5 mm, and after the rotation speed of the crucible is increased, the rotation speed of the final crucible is not more than 10rpm.
Preferably, in the shouldering step, the rotation speed of the crucible is not more than 10rpm, and in addition, the rotation speed of the crucible is designed in stages according to the length of the shouldering step, and the stage length is 10-30 mm. Setting the rotation speeds of the crucible and the crystal by the crystal diameter and the Reynolds numbers of the crystal and the molten soup, and ensuring that the Reynolds numbers of the crystal and the molten soup are smaller than a critical value;
in the shouldering step, the transition of the molten soup flow field can be determined according to the Reynolds numbers of the crystal and the molten soup, and when the rotation speed of the crystal is the same as the rotation speed of the crucible, the ratio of the Reynolds numbers of the crystal and the crucible is the critical ratio of the rotation Reynolds numbers of the crystal and the crucible. Wherein the method comprises the steps ofIs the reynolds number of the crystal; />To melt the Reynolds number of the soup, n s And n c The crystal rotation speed and the crucible rotation speed are respectively; r is (r) s And r c The radius of the crystal and the radius of the crucible are respectively; v is the kinematic viscosity of the molten soup. Under the condition of the same rotation direction, when the rotation speed of the crystal is the same as that of the crucible, the melt flows and changes, the oxygen concentration is lower, and the radial distribution is uniform. Rotating the crystal and the crucible in the same direction, along with the reduction of the ratio of the crystal pulling speed to the temperature gradient (namely V/G), the defect transition is flatter along the solid-liquid interface, when the ratio of the Reynolds number is smaller than the critical ratio, the melt flow field area is stable, and the generation of crystal defects is more favorably avoided;
preferably, the shoulder placing step is ensuredWhen->When the melt flow pattern is similar to that in reverse rotation, butThe flow speed of the melt is obviously reduced, and at the moment, oxygen atoms can diffuse upwards from the bottom of the crucible, but the oxygen content is obviously increased under the influence of temperature;
when shouldering, the e (t) value in the temperature PID can be properly adjusted up according to the growth condition of the crystal line, and the adjustment range is within 5. When the shoulder is turned in the later period of shoulder placement, if the actual temperature curve is higher than the set temperature curve by more than 3 ℃, the shoulder turning speed can be reduced, and the adjustment range is within 1 mm/min; if the deviation between the actual temperature and the set temperature exceeds +/-5 ℃, the PID of the shouldering later temperature can be closed; after shoulder placement is completed, the rotation speed difference of the two should be ensured to beWherein n is s And n c The crucible rotation speed and the crystal rotation speed are respectively.
And the e (t) value in the PID is regulated based on the difference value between the actual crystal growth temperature value and the set crystal growth temperature value, and the Ti value and the Td value are respectively an integral time constant and a differential time constant.
When shouldering, the taper of the shoulder shape of the crystal bar should be controlled to be 25-45 degrees.
Preferably, in the shoulder-stage and constant diameter steps, the difference in rotation speed between the crucible and the crystal is adjusted according to the detected data of the oxygen content after crystal growth, when the rotation speed of the crystal is closer to the rotation speed of the crucible, the distribution line of the oxygen content concentration is less distorted, and the melt flow speed is smaller, but when the rotation speed of the crystal is greater from the rotation speed of the crucible, the difficulty of crystal growth is also increased.
Preferably, the step of setting the rotation direction of the seed crystal to be identical to that of the crucible, and adjusting the rotation speed difference between the crucible and the crystal according to the oxygen content detection data after crystal growth to ensureAnd maintaining the rotation speed difference constant; the crucible is in a shape with vertical periphery and arc profile at the bottom, when the molten soup liquid level drops through the vertical crucible wall, the e (t) value in the temperature PID should be adjusted upwards, the adjustment range is within 0.5, but when the molten Shang Yemian passes through the arc profile at the bottom of the crucible, the molten steel transitsWhen the area is in the area, the value of e (t) is adjusted downwards, and the adjustment range is within 0.5.
The method has the beneficial effects that through adjustment of the rotation speeds of the crystal and the crucible and cooperation of temperature PID adjustment, a mode that the crystal and the crucible rotate in the same direction is developed to perform crystal growth, the oxygen content of the crystal bar is effectively reduced, the resistivity of the crystal bar is optimized, and related oxygen precipitation defects are avoided. Through the change of turning, the flow mode of molten soup, the molten soup speed and the temperature gradient at the solid-liquid interface are improved, the timely volatilization of oxygen through diffusion is ensured, and meanwhile, the uniform dispersion of the flow mode of molten soup is ensured, and the uniform distribution of radial oxygen concentration of the crystal bar is also ensured.
Drawings
FIG. 1 is a schematic diagram of the main components of a crystal growth furnace;
FIG. 2 is a flow pattern and oxygen concentration distribution comparison schematic of the crystal crucible rotation of comparative example 2 and example 3;
FIG. 3 is a diagram showing comparison of the rates of molten soup rotated by the crystal crucibles of comparative example 2 and example 3;
FIG. 4 is a schematic diagram showing comparison of the melt temperature fields of the crystal crucible rotations of comparative example 2 and example 3;
FIG. 5 is a process flow diagram of example 3 of the present invention;
wherein 11 is seed crystal, 12 is crucible, 13 is molten soup, 14 is crucible axis, 21 is flow pattern and oxygen concentration distribution diagram of counter-rotation of the crystal crucible, 22 is flow pattern and oxygen concentration distribution comparison diagram of counter-rotation of the crystal crucible, 31 is molten soup flow rate diagram of counter-rotation of the crystal crucible, 32 is molten soup flow rate diagram of counter-rotation of the crystal crucible, 41 is molten soup temperature field diagram of counter-rotation of the crystal crucible, and 42 is molten soup temperature field diagram of counter-rotation of the crystal crucible.
Detailed Description
Specific examples are set forth below to further illustrate the invention, and it should be understood that the examples are not intended to limit the scope of the invention.
Example 1: for lithium niobate crystal growth, the crystal and the crucible rotate in the same direction
a. The preparation step comprises the following steps: uniform in crucible14kg of raw material was placed, and the crucible was placed in a crystal growth furnace chamber and centered, after which a refractive plate was installed. 2 thermocouples are arranged at fixed positions, and the joint parts of the thermocouples are ensured not to be contacted. And installing a Pt cover plate and an upper heat insulation material, installing a seed crystal on a seed crystal shaft, and installing an upper cavity cover and a cooling cover without touching the Pt cover plate during installation. After the furnace chamber is closed, the furnace body is vacuumized to the furnace pressureLeak rate ofAnd after maintaining for 30min, argon is filled after the leak rate is confirmed to not exceed the leak rate standard. And adjusting the crucible shaft and the seed crystal shaft to preset crucible positions and crystal positions. Adjusting the temperature of a crystal growth furnace to 1290 ℃, starting material melting, wherein the rotating speed of a crucible is 0.5rpm of the conventional rotating speed, the rotating direction of the crucible is the same as the screwing direction of a seed crystal shaft, then increasing the rotating speed of the crucible by 0.5rpm every 10 seconds until the rotating speed is kept to be 4rpm, reducing the seed crystal shaft to a position near a reflector at a speed of 20mm/min, setting a cooling program at a cooling speed of 1 ℃/min, observing that the temperature of molten soup is stably maintained at 1250 ℃ from an observation window by using a radiation thermometer after 40 minutes, and if the temperature reaches the specified temperature, reducing the Td value in PID (proportion integration differentiation) until the material melting is completed, wherein the adjusting range is 0-0.5 s. And (3) lowering the crucible shaft to a position 3mm above the liquid level of the molten liquid, starting to stabilize the temperature, starting the rotation of the seed crystal during the temperature stabilization, wherein the rotating speed is 0.2rpm, and the screwing direction of the seed crystal shaft is the same as the screwing direction of the seed crystal shaft. And continuously lifting the rotating speed of the crucible, wherein the direction is kept the same as the rotating direction of the seed crystal. Stabilizing the temperature until the temperature of the molten soup is stabilized within +/-5 ℃;
b. and (3) seeding: inserting a seed crystal into the melt, reducing the temperature to enable the melt to start seeding under the induction of the seed crystal, controlling the seeding length to be 90mm, controlling the seeding crystal diameter to be 4.5+/-0.2 mm, and continuously lifting the rotating speed of the crucible to 10rpm and keeping unchanged;
c. shoulder placing: starting shouldering, setting the same as above, and setting the shouldering parameters as shown in the following table 1:
TABLE 1 setting of shoulder parameters
| Shoulder length (mm) | Expansion speed (mm/min) | Pulling speed (mm/min) | Seed crystal rotation speed (rpm) | Crucible rotation speed (rpm) |
| 0 | 0.1 | 0.55 | 0.5 | 10 |
| 30 | 0.5 | 0.55 | 1 | 10 |
| 60 | 1.2 | 0.55 | 3 | 10 |
| 90 | 2.4 | 0.6 | 5 | 10 |
| 100 | 2.5 | 0.6 | 5 | 10 |
| 110 | 2.5 | 0.6 | 5 | 10 |
The following description is given to parameter setting: if the expansion speed, the pulling speed, the seed crystal rotating speed and the crucible rotating speed corresponding to the shoulder length of 0mm are the node parameters. The shoulder length is 0-30 mm, and the increase of the related speed is regulated by the related PID;
d. and (3) an isodiametric step: starting the constant diameter, setting the rotation speed to be equal to the shoulder, and setting the rotation direction of the crucible and the rotation direction of the crystal to be equal to the screwing direction of the seed crystal, wherein the rotation speed of the crystal is 5rpm, the rotation speed of the crucible is 10rpm, and the diameter is set to be 210mm;
e. ending: after the ingot is cut from the melt Shang Yemian, the ingot is annealed.
Comparative example 2: for single crystal silicon crystal growth, the crystal and crucible are counter rotated
a. The preparation step comprises the following steps: 400kg of raw material is placed in the crucible according to the crucible periphery #4 material and the middle #2 material, and the crucible is placed in a crystal growth furnace chamber and centered. And installing the seed crystal on the seed crystal shaft. After the furnace chamber is closed, the furnace body is vacuumized to the furnace pressureLeakage Rate->And after maintaining for 30min, argon is filled after the leak rate is confirmed to not exceed the leak rate standard. After adjusting the crucible shaft and the seed crystal shaft to preset crucible position and crystal position, adjusting the power of a main heater of the crystal growth furnaceTo 90kw, the sub-heater power is stepped up to 30kw. The rotation speed of the crucible is 0.5rpm of the conventional rotation speed, the rotation direction of the crucible is opposite to the screwing direction of the seed crystal shaft, then the rotation speed of the crucible is kept unchanged at 4rpm every 10 seconds of the crucible, and the melting is completed. And reducing the power of the main heater by 80kw to a position close to the melting point Shang Yemian, maintaining the temperature of the auxiliary heater by 30kw, starting to stabilize the temperature, starting a magnetic field of the crystal growth furnace at the same time of stabilizing the temperature, starting the rotation of the seed crystal, wherein the magnetic field strength is 123A, the rotating speed is 0.2rpm, and the direction is the same as the screwing direction of a seed crystal shaft. And continuously lifting the rotating speed of the crucible, and keeping the direction opposite to the rotating direction of the seed crystal. And (3) stabilizing the temperature until the temperature of the molten soup is stabilized within +/-20 ℃. The crucible rotation speed compensation value and the stepping length compensation value are set to 0, the e (t) value in the temperature PID is set to 0.05, the Ti value is set to 600s, and the Td value is set to 1s;
b. and (3) seeding: inserting a seed crystal into the melt, reducing the temperature to enable the melt to start seeding under the induction of the seed crystal, controlling the seeding length to be 130mm, controlling the seeding crystal diameter to be 4.5+/-0.2 mm, and continuously lifting the rotating speed of the crucible to 10rpm and keeping unchanged;
c. shoulder placing: starting shoulder setting, the rotation speed setting is the same as above, and the shoulder setting parameters are shown in the following table 2:
TABLE 2 setting of shoulder parameters
| Shoulder length (mm) | Expansion speed (mm/min) | Pulling speed (mm/min) | Seed crystal rotation speed (rpm) | Crucible rotation speed (rpm) |
| 0 | 0.1 | 0.6 | 0.2 | 10 |
| 30 | 0.55 | 0.6 | 0.2 | 10 |
| 60 | 1.2 | 0.6 | 0.2 | 10 |
| 90 | 2.44 | 0.65 | 0.2 | 10 |
| 100 | 2.97 | 0.65 | 0.2 | 10 |
| 110 | 3.5 | 0.7 | 0.2 | 10 |
| 120 | 3.8 | 0.7 | 0.2 | 10 |
| 130 | 3.8 | 0.75 | 0.2 | 10 |
| 140 | 3.8 | 0.8 | 0.2 | 10 |
The following description is given to parameter setting: if the expansion speed, the pulling speed, the seed crystal rotating speed and the crucible rotating speed corresponding to the shoulder length of 0mm are the node parameters, the shoulder length is 0-30 mm, and the relevant speed is increased through the relevant PID regulation;
d. and (3) an isodiametric step: and (3) starting the constant diameter, setting the rotation speed to be equal to the shoulder setting and setting the rotation direction of the crystal to be the screwing direction of the seed crystal, and setting the rotation direction of the crucible to be opposite to the screwing direction of the seed crystal, wherein the rotation speed of the crystal is 0.2rpm, the rotation speed of the crucible is-10 rpm, and the diameter is set to be 310mm. When the equal diameter length is 850mm, the transition area exists at the edge of the bottom of the crucible, the temperature is set to be adjusted downwards, the adjusting amplitude is 5 ℃, and in addition, the Td value in the PID is adjusted upwards, so that the amplitude is 0.2s;
e. ending: and the power of the main heater is reduced, and the pulling speed of the crystal is gradually increased according to the ending length. When the crystal is separated from the liquid level of the molten soup, the power of the main heater is reduced by 15kw every 10min after the crystal position and the crucible position return to zero point until the power of the main heater is 0kw, and the crystal bar is placed in the furnace chamber for 8h until the crystal bar is cooled to room temperature.
The sample wafer of the crystal bar is selected for oxygen content detection, and the positions of the center and the edge of the wafer, which are 10mm away, are respectively selected for detection, wherein the oxygen content detection data are shown in the following table 3:
TABLE 3 results of the oxygen content measurements on the ingots of comparative example 2
| Sample wafer number | Oxygen content (center) | Oxygen content-1 (edge 10 mm) | Oxygen content-2 (edge 10 mm) | Oxygen content-3 (edge 10 mm) | Oxygen content-4 (edge 10 mm) |
| C | 12.211 | 12.179 | 12.005 | 11.504 | 12.199 |
| F | 11.47 | 11.286 | 11.092 | 11.394 | 11.529 |
| J | 11.104 | 11.01 | 10.554 | 10.949 | 11.115 |
| N | 10.559 | 10.584 | 10.58 | 10.38 | 10.499 |
| Q | 10.564 | 10.259 | 10.395 | 10.145 | 10.628 |
| U | 10.186 | 10.039 | 10.002 | 10.217 | 10.24 |
Example 3: for single crystal silicon crystal growth, the crystal and crucible are rotated in the same direction (process flow diagram see FIG. 5)
a. The preparation step comprises the following steps: 400kg of raw material was placed in the crucible according to crucible periphery #4 and middle #2, and the crucible was placed in a growth chamber and centered (growth chamber see FIG. 1). And installing the seed crystal on the seed crystal shaft. After the furnace chamber is closed, the furnace body is vacuumized to the furnace pressureLeakage Rate->And after maintaining for 30min, argon is filled after the leak rate is confirmed to not exceed the leak rate standard. And after adjusting the crucible shaft and the seed crystal shaft to preset crucible positions and crystal positions, adjusting the power of a main heater of the crystal growth furnace to be gradually increased to 90kw, and the power of a secondary heater to be gradually increased to 30kw. The rotation speed of the crucible is 0.5rpm of the conventional rotation speed, the rotation direction of the crucible is the same as the screwing direction of the seed crystal shaft, then the rotation speed of the crucible is kept unchanged at 4rpm every 10 seconds of the crucible, and the melting is completed. And reducing the power of the main heater by 80kw to a position close to the melting point Shang Yemian, maintaining the temperature of the auxiliary heater by 30kw, starting to stabilize the temperature, starting a magnetic field of the crystal growth furnace at the same time of stabilizing the temperature, starting the rotation of the seed crystal, wherein the magnetic field strength is 123A, the rotating speed is 0.2rpm, and the direction is the same as the screwing direction of a seed crystal shaft. And continuously lifting the rotating speed of the crucible, wherein the rotating direction is the same as the rotating direction of the seed crystal. And (3) stabilizing the temperature until the temperature of the molten soup is stabilized within +/-20 ℃. The crucible rotation speed compensation value and the stepping length compensation value are set to 0, the e (t) value in the temperature PID is set to 0.05, the Ti value is set to 600, and the Td value is set to 1;
b. and (3) seeding: inserting a seed crystal into the melt, reducing the temperature to enable the melt to start seeding under the induction of the seed crystal, controlling the seeding length to be 130mm, controlling the seeding crystal diameter to be 4.5+/-0.2 mm, and continuously lifting the rotating speed of the crucible to 10rpm and keeping unchanged;
c. shoulder placing: starting shoulder setting, the rotation speed setting is the same as above, and the shoulder setting parameters are shown in the following table 4:
TABLE 4 setting of shoulder parameters
| Shoulder length (mm) | Expansion speed (mm/min) | Pulling speed (mm/min) | Seed crystal rotation speed (rpm) | Crucible rotation speed (rpm) |
| 0 | 0.1 | 0.6 | 0.5 | 10 |
| 30 | 0.55 | 0.6 | 1 | 10 |
| 60 | 1.2 | 0.6 | 3 | 10 |
| 90 | 2.44 | 0.65 | 5 | 10 |
| 100 | 2.97 | 0.65 | 5 | 10 |
| 110 | 3.5 | 0.7 | 5 | 10 |
| 120 | 3.8 | 0.7 | 5 | 10 |
| 130 | 3.8 | 0.75 | 5 | 10 |
| 140 | 3.8 | 0.8 | 5 | 10 |
The following description is given to parameter setting: if the expansion speed, the pulling speed, the seed crystal rotating speed and the crucible rotating speed corresponding to the shoulder length of 0mm are the node parameters, the shoulder length is 0-30 mm, and the relevant speed is increased through the relevant PID regulation;
d. and (3) an isodiametric step: and (3) starting the constant diameter, setting the rotation speed at the same shoulder, and setting the rotation direction of the crucible and the rotation direction of the crystal at the same seed crystal screwing direction, wherein the rotation speed of the crystal is 5rpm, the rotation speed of the crucible is 10rpm, and the diameter is set to 310mm. When the constant diameter length is 850mm, the transition area exists at the edge of the bottom of the crucible, the temperature is set to be adjusted downwards, the adjusting amplitude is 5 ℃, and in addition, the Td value in the PID is adjusted upwards, so that the amplitude is 0.2;
e. ending: and the power of the main heater is reduced, and the pulling speed of the crystal is gradually increased according to the ending length. When the crystal is separated from the liquid level of the molten soup, the power of the main heater is reduced by 15kw every 10min after the crystal position and the crucible position return to zero point until the power of the main heater is 0kw, and the crystal bar is placed in the furnace chamber for 8h until the crystal bar is cooled to room temperature.
The sample wafer of the crystal bar is selected for oxygen content detection, and the positions of 10mm at the center and the edge of the wafer are respectively selected for detection, wherein the oxygen content detection data are shown in the following table 5:
TABLE 5 results of the oxygen content measurements on the boules in example 3
| Sample wafer number | Oxygen content (center) | Oxygen content-1 (edge 10 mm) | Oxygen content-2 (edge 10 mm) | Oxygen content-3 (edge 10 mm) | Oxygen content-4 (edge 10 mm) |
| C | 6.364 | 6.287 | 6.046 | 6.332 | 6.202 |
| F | 5.418 | 5.264 | 5.31 | 5.522 | 5.43 |
| J | 5.134 | 4.856 | 5.238 | 5.242 | 5.101 |
| N | 4.91 | 4.719 | 4.668 | 4.75 | 4.925 |
| Q | 4.857 | 4.574 | 4.063 | 4.714 | 4.736 |
| U | 3.885 | 4.288 | 4.219 | 4.27 | 4.452 |
From the above, the oxygen content can be effectively reduced by using the crystal rotation and the crucible rotation in the same direction under the same operation conditions. From the aspects of the flow mode of the molten soup, the oxygen concentration distribution (see figure 2) and the flow rate of the molten soup (see figure 3), the flow of the molten soup at the solid-liquid interface is obviously dispersed and uniform, in addition, the flow speed at the interface is obviously reduced, the flow speed of the molten soup is quite uniform under the same-direction rotation, the internal flow of the molten soup is not violent, the timely volatilization of the oxygen in the molten soup through diffusion is ensured, and the oxygen content in the crystal is effectively reducedAmount of the components. From the view of the molten soup temperature field (see fig. 4), the molten soup temperature distribution is obviously more uniform in the same-direction rotation than in the opposite-direction rotation, the relative consistency of the temperature gradient is ensured, the solid-liquid interface is wholly concave to the crystal, and the solid-liquid interface is more suitable for crystal growth. In addition, when ensuringWhen the method is used, the maximum temperature of the crucible is moderate, the change of a flow field of the melt Shang Rechang caused by deformation and collapse of the crucible is effectively avoided, and the crystal quality is ensured. For the growth of lithium niobate crystals, the co-rotating reduces the oxygen content of the crystals, improves the quality of crystal bars, ensures the stability of the resistivity of the crystals and the uniformity of radial distribution. For single crystal silicon, the co-rotation not only reduces the overall oxygen concentration, but also improves the radial oxygen concentration profile so that it is more uniform.
Although embodiments of the present invention have been shown and described, it would be appreciated by those skilled in the art that changes, modifications and alternatives may be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the claims and their equivalents.
Claims (7)
1. The crystal growing method by the same rotation of the crystal and the crucible is characterized by comprising the following steps:
a. the preparation step comprises the following steps: placing raw materials into a crucible of a crystal growth furnace, installing seed crystals, carrying out vacuum pumping leak detection on a furnace table, carrying out material melting and temperature stabilization, and simultaneously starting the seed crystals and the crucible to rotate in the same direction, wherein before material melting, the rotation speed of the crucible is increased by adopting a step-type numerical value increasing method, namely 0-0.5 rpm is increased every 1-10 s, 0rpm is not taken, the rotation speed of the crucible is finally increased to be not more than 5rpm, and material melting is completed under the rotation speed of the crucible;
b. and (3) seeding: inserting a seed crystal into the melt, reducing the temperature to enable the melt to start to crystallize under the induction of the seed crystal, and increasing the rotating speed of the crucible to a certain value;
c. shoulder placing: starting to put the shoulder, maintaining the rotation speed of the crucible unchanged, gradually increasing the rotation speed of the crystal until reaching the target rotation speed, and ensuring the crystalThe rotating speed is smaller than the rotating speed of the crucible, constant rotating speed difference is maintained, and the rotating speed of the crystal is set in a segmented mode according to the length of the shoulder; when the shoulder shape passes through the outline inflection point, the e (t) value in the temperature PID is adjusted up within 5 according to the growth condition of the crystal line, when the shoulder shape passes through the outline inflection point and enters the shoulder turning process, the e (t) value in the temperature PID is adjusted down to reduce thermal shock, if the actual temperature curve is higher than the set temperature curve by more than 3 ℃, the shoulder turning speed is reduced, the adjustment range is within 1mm/min, and if the deviation between the actual temperature and the set temperature exceeds +/-5 ℃, the shoulder turning later temperature PID is closed; after shoulder placement is completed, the rotation speed difference of the two should be ensured to beWherein n is s And n c The crucible rotation speed and the crystal rotation speed are respectively;
d. and (3) an isodiametric step: starting constant diameter growth, maintaining constant rotation speed difference, optimizing a crystal growth temperature curve, wherein the crucible is in a shape with vertical periphery and circular arc profile at the bottom, and when the molten soup liquid level descends to pass through the vertical crucible wall, the e (t) value in the temperature PID should be adjusted upwards, but when the molten Shang Yemian passes through the circular arc profile transition zone at the bottom of the crucible, the e (t) value in the temperature PID should be adjusted downwards;
e. ending: after the grown crystal is detached from the melt Shang Yemian, the ingot is cooled.
2. The method for growing crystals by rotating the crystals and the crucible in the same direction as one of claim 1, wherein the preparing step comprises the steps of placing raw materials in a crucible of a crystal growing furnace, mounting seed crystals on a seed crystal shaft, closing a furnace chamber, vacuumizing the furnace body, filling inert gas, increasing the power of the crystal growing furnace to the power of the material to be melted, starting the crucible to rotate and increasing the rotation speed of the crucible to a target value, rotating the crucible in the same direction as the screwing direction of the seed crystals on the seed crystal shaft until the material to be melted is completely melted, uniformly placing the crucible in such a way that the bottom of the crucible stacks the large materials and the upper region stacks the small materials, and pressing the furnace chamber after vacuumizingForce requirementsLeakage rate is->The magnetic field was set to 123.+ -. 0.3A, and the inert gas was one of Ar and He gas.
3. The method for growing crystals by rotating crystals and a crucible in the same direction as the method of claim 1, wherein in the step of preparing materials, during the temperature stabilization, seed crystals need to be lowered to a position close to a melting point Shang Yemian, the power of a crystal growing furnace is lowered to a temperature stabilization power, so that the temperature of molten soup is lowered to a target temperature, the target temperature is taken as a central value, the temperature tolerance is within +/-20 ℃, then a magnetic field of the crystal growing furnace is started, the seed crystals are started to rotate, the rotation speed of the crucible is further improved, and the rotation directions of the seed crystals and the crucible are the screwing directions of a seed crystal shaft.
4. The method for growing crystals by co-rotating a crystal and a crucible according to claim 1, wherein the diameter of the crystal to be grown is controlled to be 4-5 mm in the seeding step, and the final crucible rotation speed is not more than 10rpm after the crucible rotation speed is raised.
5. The method for growing crystals by co-rotating crystals and a crucible according to claim 1, wherein the shouldering step is characterized in that the rotation speed of the crucible is not more than 10rpm, the rotation speed of the crucible is designed in stages according to the length of the crucible to be shouldered, the sectional length of the crucible is 10-30 mm, the rotation speeds of the crucible and the crystals are set through the crystal diameter and the reynolds coefficients of the crystals and molten soup, and the reynolds coefficients of the crystals and molten soup are required to be ensured to be smaller than a critical value.
6. The method for growing crystals by co-rotating crystals and a crucible according to claim 1, wherein the shoulder-step is performed with the shoulder-shaped taper of the ingot controlled to be 25-45 °.
7. According to the weightsThe method for growing crystals by co-rotating a crystal and a crucible as set forth in claim 1, wherein the step of constant diameter sets the rotation direction of the seed crystal to be consistent with that of the crucible, and adjusts the rotation speed difference between the crucible and the crystal according to the oxygen content detection data after growing the crystal to ensureAnd maintaining the rotation speed difference constant; the crucible is in a shape with vertical periphery and arc profile at the bottom, the e (t) value in the temperature PID should be adjusted upwards in the adjustment range within 0.5 in the process that the molten soup liquid level descends through the vertical crucible wall, but the e (t) value should be adjusted downwards in the adjustment range within 0.5 when the molten steel Shang Yemian passes through the arc profile transition zone at the bottom of the crucible.
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