CN109778307B - Process control system suitable for monocrystalline silicon horizontal growth mechanism - Google Patents
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Abstract
The invention relates to the technical field of monocrystalline silicon material preparation, in particular to a process control system suitable for a monocrystalline silicon horizontal growth mechanism. It includes: a melting region temperature control module, a cooling region control module and a seed crystal pulling module. The melting area control module comprises 4 sections of settable temperature rising modules; the cooling area control module comprises 2 sections of settable temperature rising modules; the seed crystal pulling module comprises a controllable seed crystal rod advancing and retreating module. By utilizing the process control system and matching with the monocrystalline silicon production equipment by the horizontal pulling method, the continuous growth of ultrathin monocrystalline silicon wafers can be realized.
Description
Technical Field
The invention relates to the technical field of monocrystalline silicon material preparation, in particular to a process control system suitable for a monocrystalline silicon horizontal growth mechanism.
Background
Silicon has wide application as a nonmetal in the semiconductor field and the photovoltaic field. In the prior art, a single crystal silicon ingot is generally produced by a Czochralski method (CZ method) and a float zone method (HZ method). Monocrystalline silicon is widely used in the semiconductor field, and both monocrystalline silicon and polycrystalline silicon have applications in the photovoltaic industry.
In the conventional polycrystalline and monocrystalline silicon growth process, a vertical pulling method is usually adopted to grow monocrystalline and polycrystalline ingots, and ultrathin silicon wafers required in products are grown through a large amount of post-treatment (wire cutting, grinding and polishing and the like). Due to industry needs, researchers have subsequently begun developing equipment for the direct production of silicon wafers, the most widely used of which are: the die-casting method (EFG), the wire-drawn tape silicon method (SR), and the like. The method for growing the silicon wafer is to build a vertical temperature gradient to enable silicon crystals to grow from the bottom of a crucible, and to pull out the grown silicon by leading a silk thread or a seed crystal to enable the molten silicon to grow into the silicon wafer at a certain speed. Although this method enables a silicon wafer to be stably grown, the shape is not stable, partial post-processing is also required, and the production speed is not fast. Subsequently, the horizontal pulling theory that can rapidly (growth speed of 2 mm/s) produce ultra-thin silicon wafers is proposed. In recent years, the method is widely researched by scholars at home and abroad, the basic theory is relatively complete, and based on the theory, production equipment suitable for the horizontal growth method is designed and the process control of the equipment is automated.
Disclosure of Invention
The invention aims to provide a process control system and a process method suitable for a horizontal pulling method to produce monocrystalline silicon equipment, and aims to solve the problems of rapid heating, temperature field maintaining, automation of a pulling device and the like of horizontal production equipment.
In order to solve the problems, the invention provides a process control system suitable for a horizontal monocrystalline silicon growth mechanism, wherein the horizontal monocrystalline silicon growth mechanism comprises a heating furnace body and a lifting cabin communicated with an inner cavity of the heating furnace body, a graphite crucible is arranged at the bottom of the inner cavity of the heating furnace body, a heat insulation plate is arranged at the top end of the inner cavity of the heating furnace body to divide the inner cavity of the heating furnace body into a melting region, namely a hot region, and a cooling region, namely a cold region, a jet pipe is arranged on the front side or the rear side of the heating furnace body, and the jet pipe; the thermocouple is positioned above the heating furnace body and is vertically inserted into the inner cavity of the heating furnace body; the feeding pipe is arranged above the heating furnace body, is vertically inserted into the inner cavity of the heating furnace body and is positioned in the melting area; an air exhaust port is arranged at the bottom of the inner cavity of the heating furnace body, and an air exhaust pipe is vertically inserted below the furnace body and is connected with the air exhaust port; the one end of carrying the cabin and being close to heating furnace body is equipped with the closing plate, carries to carry and is equipped with the seed rod along the horizontal direction in the cabin, and the seed rod is connected with the servo motor who is located to carry outside the cabin, its characterized in that, process control system includes: a melting region temperature control module, a cooling region control module and a seed crystal pulling module; the melting area control module comprises 4 sections of settable temperature rising modules, heating target temperatures and heat preservation times of different stages are set in the settable temperature rising modules, and the heating target temperatures and the heat preservation times of the different stages are used for accurately controlling a temperature field of a melting area and ensuring the true and stable temperature reached by each stage; the cooling area control module comprises 2 sections of settable temperature rising modules, the settable temperature rising modules of the cooling area comprise target temperatures and holding time of the cooling area in different stages, the target temperature of the cooling area is used for ensuring that the temperature gradient at the outlet of the melting area is not too large in the melting stage so as not to cause the crystal to form an amorphous state, the target temperature of the cooling area can compensate the temperature of the cooling area in the crystal pulling process to ensure the smooth growth, the seed crystal pulling module comprises a controllable seed crystal rod advancing and retreating module, and whether the seed crystal is pulled or not can be judged according to the internal condition of the furnace body obtained by the observation port in the controllable seed crystal rod advancing and retreating module, the controllable forward and backward moving module comprises the movement speed settings of different forward and backward moving stages, and can be matched and adjusted according to specific process parameters to achieve the optimal pulling speed.
Further, the thermocouple is a double platinum rhodium thermocouple.
Furthermore, the exhaust tube is a slender quartz tube with the diameter of 3-5 mm.
Furthermore, a control panel is arranged on the left side of the heating furnace body, an HMI industrial touch screen is adopted by the control panel, and an ohm dragon PLC is adopted for writing a control program.
Furthermore, 2 silicon-molybdenum heating rods which are a group and 3 groups are distributed in the melting area in the inner cavity of the heating furnace body and are distributed on the left side, the right side and the rear side of the crucible; 2 groups of 2 silicon-molybdenum heating rods are distributed in the cooling area and distributed on the left side and the right side of the crucible; the resistance of the silicon-molybdenum heating rod can be increased along with the increase of the temperature; each group of silicon-molybdenum heating rods is a U-shaped structure formed by 2 silicon-molybdenum heating rods.
Further, a silicate heat-insulating sleeve is arranged outside the inner cavity of the heating furnace body.
The invention also comprises a flow process matched with the system, and the technical scheme is as follows:
(1) closing the heating furnace body and the sealing plate, and introducing nitrogen into the inner cavity of the heating furnace body at a uniform speed for 5-15 min to ensure that the inner cavity of the heating furnace body is in an inert atmosphere environment; after ventilation, the gas flow is reduced and ventilation is continued, the inner cavity of the heating furnace body is ensured to be in a positive pressure environment, the feeding pipe is opened for feeding, and the feeding pipe is closed after the completion.
(2) Setting sectional heating values of a melting area and a cooling area, wherein the first section of the melting area is heated at a target temperature of 300-350 ℃, the heat preservation time is 5-15 min, the second section is heated at a target temperature of 570-630 ℃, the heat preservation time is 15-30 min, the third section is heated at a target temperature of 1280-1330 ℃, the heat preservation time is 20-30 min, and the last section is heated at a target temperature of 1450-1620 ℃; continuously preserving heat; the target temperature of the first section of the cooling area is 600-650 ℃, the heat preservation time is 15-30 min, the target temperature of the second section of the cooling area is 1410-1450 ℃, and heat preservation is carried out continuously.
(3) Starting heating, wherein when the temperature is below 400 ℃, the heating power is preferably limited to 5-10%, when the temperature is more than 400 ℃ and less than or equal to 700 ℃, the heating power is preferably limited to 10-15%, the heating speed is preferably 3-4 ℃/min, when the temperature is more than 700 ℃ and less than or equal to 1280 ℃, the heating power is preferably limited to 15-30%, and the heating speed is preferably 1-4 ℃/min; when the temperature is higher than 1280 ℃ and lower than 1400 ℃, the heating power is increased to 100 percent in each time by a certain increment, the increment is preferably 2-5%/time, and the heating speed is preferably 3-4 ℃/min; when the temperature is 1400-1620 ℃, the heating speed is preferably 1-2 ℃/min; when the melting area and the cooling area reach the set temperature of the final stage, the heater power of the melting area is reduced to be below 80%, preferably 60% -70%, the heater power of the cooling area is reduced to be below 60%, preferably 40% -50%, the jet pipe is opened, high-temperature gas is introduced into the furnace body, the gas temperature is 600-800 ℃, the gas flow rate is 0.8-2.5 m/s, and meanwhile, the gas pump of the gas extraction opening is opened, so that the gas is extracted outwards at the same flow rate as the gas introduced into the jet pipe, and the gas pressure in the furnace body is not too high.
(4) Continuously introducing high-temperature gas and exhausting, opening a sealing plate between the heating furnace body and the pulling cabin after the feedback temperatures of the melting area and the cooling area are stable, starting a seed crystal pulling module, guiding a seed crystal rod into the heating furnace body through the pulling cabin through a servo motor, wherein the feeding speed is 30-50 cm/min, and feeding at a slower speed after the seed crystal rod reaches the right boundary position of the heating furnace body, wherein the slower speed is 10-15 cm/min; and the seed rod reaches the boundary of the molten silicon in the graphite crucible in the heating furnace body, meanwhile, the seed crystal on the seed rod is contacted with the silicon melt in the graphite crucible, after 10-15 s, the seed crystal is pulled towards the right side, and the pulling speed is 1-3 mm/s.
(5) And (3) when the seed crystal rod is pulled out of the heating furnace body and enters the pulling cabin, closing the sealing plate, taking down the pulled monocrystalline silicon wafer, replacing the seed wafer, and repeating the steps (1) to (4) for continuous production.
The power of a silicon-molybdenum heating rod used for growing the silicon wafer by adopting a horizontal pulling method is adjusted by a 0-20 mA analog quantity signal output by a PLC (programmable logic controller) to output different conduction angles of a silicon controlled rectifier so as to adjust a used transformer for limiting; when the temperature is below 400 ℃, the heating power is limited to 5-10%, and the current reading on the control panel is observed, the heating power is properly increased and decreased, the increment and decrement of each heating power is preferably 1%, and the current is kept at 160A +/-5A. And when the temperature is higher than 400 ℃ and lower than or equal to 700 ℃, switching the heating module to a time heating mode, wherein the heating power is limited to 10-15%, and the heating speed is 3-4 ℃/min. When the temperature is higher than 700 ℃ and less than or equal to 1280 ℃, the heating power is limited to 15-30%, and the heating speed is 1-4 ℃/min. When the temperature is higher than 1280 ℃ and lower than 1400 ℃, the heating power is gradually increased to the full power according to the current reading of the control panel, and the increase of the heating power is limited to 2-5%/time. The heating rate should be limited to 3-4 deg.C/min. When the temperature is 1400-1620 ℃, the heating rate should be limited to 1-2 ℃/min.
Drawings
FIG. 1 is a schematic view of a horizontal silicon wafer pulling apparatus.
In FIG. 1, 1-inlet tube; 2, 3-thermocouple; 4-heating the furnace body; 5-insulating board; 6-jet pipe; 7-a graphite crucible; 8-receiving a crucible; 9-sealing plate; 10-a pulling cabin; 11-seed rods; 12-a servo motor; 13-silicate insulation cover; 14-air extraction opening.
Detailed Description
Reference will now be made in detail to embodiments of the invention, one or more examples of which are described below. Each example is provided by way of explanation, not limitation, of the invention.
When a monocrystalline silicon wafer with the thickness of 200-500 mu m and the width of 8-12 mm is grown, a heat-conducting graphite crucible is adopted. The protective atmosphere is argon, positive pressure and continuous ventilation of the inner cavity of the heating furnace body 4 are ensured, the high-temperature gas is argon at the temperature of 600-800 ℃, and the gas flow is 0.8-2.5 m/s. And plating a compact silicon nitride porous ceramic coating on the surface layer of the heat-conducting graphite crucible by adopting a plasma vapor deposition method. The thickness of the plating layer is 1.2-2.0 μm. The jet pipe 6 is a graphite pipe with a row of holes, the exhaust pipe at the exhaust opening 14 is a quartz pipe with the diameter of 3-5 mm, and the exhaust speed is consistent with the jet speed. The melting area is provided with 3 groups of silicon-molybdenum heating rods, and the cooling area is provided with 2 groups of silicon-molybdenum heating rods.
In the heating stage, 4 sections of heating intervals are arranged in a melting area, the target temperature of the first section is 350 ℃, and the heat preservation time is 5-15 min; the second stage heating target temperature is 600 ℃, and the heat preservation time is 15-30 min; the target temperature of the third section is 1300 ℃, and the heat preservation time is 20-30 min; the final stage target temperature is preferably 1480 ℃. The cooling area is provided with 2 sections of heating areas, the target temperature of the first section is 600-650 ℃, and the heat preservation time is 20 min; the target temperature of the second section is 1400-1420 ℃, and the heat is continuously preserved.
In the crystal pulling stage, the sealing plate 9 between the heating furnace body 4 and the pulling cabin 10 should be opened first, and after the temperature is stabilized, the jet cooling module and the exhaust module are started. The module can freely control the jet flow rate, which is 1m/s in the example and the jet gas temperature is 800 ℃. After the jet flow program is started, the heating power of the melting zone heater is limited to be less than 80%, preferably 60% -70%, and the heating power of the cooling zone heater is limited to be less than 60%, preferably 40% -50%, so that the silicon-molybdenum heating rod is not damaged under a large temperature gradient. When the temperature is stable, starting a pulling program, leading a seed rod to quickly approach the heating furnace body 4, then slowly entering the inner cavity of the heating furnace body 4 to be contacted with molten silicon, keeping for 10-15 s, confirming the generation of crystals through a CCD (charge coupled device) of an observation port, and then starting to pull to the right, wherein the pulling speed is preferably 1.2-1.9 mm/s in the example. After the silicon wafer is pulled to reach the limited position, the produced silicon wafer is cut off, the heating furnace body 4 and the sealing plate 9 are closed, the seed wafer is replaced, and the actions are repeated, so that the continuous growth of the ultrathin monocrystalline silicon wafer can be realized.
Claims (10)
1. A process control system suitable for a horizontal monocrystalline silicon growth mechanism comprises a heating furnace body and a lifting cabin communicated with an inner cavity of the heating furnace body, wherein a graphite crucible is arranged at the bottom of the inner cavity of the heating furnace body, a heat insulation plate is arranged at the top end of the inner cavity of the heating furnace body to divide the inner cavity of the heating furnace body into a melting region, namely a hot region, and a cooling region, namely a cold region, a jet pipe is arranged on the front side or the rear side of the heating furnace body, and the jet pipe extends into the inner cavity of the heating furnace; the thermocouple is positioned above the heating furnace body and is vertically inserted into the inner cavity of the heating furnace body; the feeding pipe is arranged above the heating furnace body, is vertically inserted into the inner cavity of the heating furnace body and is positioned in the melting area; an air exhaust port is arranged at the bottom of the inner cavity of the heating furnace body, and an air exhaust pipe is vertically inserted below the furnace body and is connected with the air exhaust port; the one end of carrying the cabin and being close to heating furnace body is equipped with the closing plate, carries to carry and is equipped with the seed rod along the horizontal direction in the cabin, and the seed rod is connected with the servo motor who is located to carry outside the cabin, its characterized in that, process control system includes: a melting region temperature control module, a cooling region control module and a seed crystal pulling module; the melting area control module comprises 4 sections of settable temperature rising modules, heating target temperatures and heat preservation times of different stages are set in the settable temperature rising modules, and the heating target temperatures and the heat preservation times of the different stages are used for accurately controlling a temperature field of a melting area and ensuring the true and stable temperature reached by each stage; the cooling area control module comprises 2 sections of settable temperature rising modules, the settable temperature rising modules of the cooling area comprise target temperatures and holding time of the cooling area in different stages, the target temperature of the cooling area is used for ensuring that the temperature gradient at the outlet of the melting area is not too large in the melting stage so as not to cause the crystal to form an amorphous state, the target temperature of the cooling area can compensate the temperature of the cooling area in the crystal pulling process to ensure the smooth growth, the seed crystal pulling module comprises a controllable seed crystal rod advancing and retreating module, and whether the seed crystal is pulled or not can be judged according to the internal condition of the furnace body obtained by the observation port in the controllable seed crystal rod advancing and retreating module, the controllable forward and backward moving module comprises the movement speed settings of different forward and backward moving stages, and can be matched and adjusted according to specific process parameters to achieve the optimal pulling speed.
2. The process control system for a single crystal silicon horizontal growth mechanism as claimed in claim 1, wherein said thermocouple is a double platinum rhodium thermocouple.
3. The process control system for a horizontal growth mechanism of monocrystalline silicon according to claim 1, wherein the pumping tube is an elongated quartz tube having a diameter of 3-5 mm.
4. The process control system suitable for the horizontal growth mechanism of monocrystalline silicon according to claim 1, wherein a control panel is arranged on the left side of the heating furnace body, the control panel adopts an HMI industrial touch screen, and a control program is compiled by adopting an ohm dragon PLC.
5. The process control system for a horizontal growth mechanism of single crystal silicon according to claim 1, wherein 2 groups of 3 groups of silicon molybdenum heating rods are distributed in the melting region in the inner cavity of the heating furnace body and distributed on the left and right sides and the rear side of the crucible; 2 groups of 2 silicon-molybdenum heating rods are distributed in the cooling area and distributed on the left side and the right side of the crucible; the resistance of the silicon-molybdenum heating rod can be increased along with the increase of the temperature; each group of silicon-molybdenum heating rods is a U-shaped structure formed by 2 silicon-molybdenum heating rods.
6. The process control system suitable for the horizontal growth mechanism of monocrystalline silicon, as claimed in claim 5, wherein the power of the silicon molybdenum heating rod is limited by adjusting different conduction angles of the output of the silicon controlled rectifier through a 0-20 mA analog quantity signal output by the PLC, so as to adjust the transformer used for limitation.
7. The process control system for a horizontal growth mechanism of single crystal silicon according to claim 1, wherein a silicate insulating sleeve is provided outside the inner cavity of the heating furnace body.
8. A method for continuously growing ultra-thin single crystal silicon wafers using the process control system of claim 1, comprising the steps of:
(1) closing the heating furnace body and the sealing plate, and introducing nitrogen into the heating furnace body at a uniform speed for 5-15 min to ensure that the heating furnace body is in an inert atmosphere environment; after ventilation, reducing the gas flow and continuously ventilating to ensure that the heating furnace body is in a positive pressure environment, opening the feeding pipe, feeding, and closing the feeding pipe after the feeding is finished;
(2) setting sectional heating values of a melting area and a cooling area, wherein the first section of the melting area is heated at a target temperature of 300-350 ℃, the heat preservation time is 5-15 min, the second section is heated at a target temperature of 570-630 ℃, the heat preservation time is 15-30 min, the third section is heated at a target temperature of 1280-1330 ℃, the heat preservation time is 20-30 min, and the last section is heated at a target temperature of 1450-1620 ℃; continuously preserving heat; the first section of the cooling area is heated at the target temperature of 600-650 ℃, the heat preservation time is 15-30 min, the second section of the cooling area is heated at the target temperature of 1410-1450 ℃, and heat preservation is carried out continuously;
(3) starting heating, wherein when the temperature is below 400 ℃, the heating power is limited to 5-10%, when the temperature is more than 400 ℃ and less than or equal to 700 ℃, the heating power is limited to 10-15%, the heating speed is 3-4 ℃/min, when the temperature is more than 700 ℃ and less than or equal to 1280 ℃, the heating power is limited to 15-30%, and the heating speed is 1-4 ℃/min; when the temperature is higher than 1280 ℃ and lower than 1400 ℃, the heating power is increased to 100 percent in a certain increment every time, the increment is 2-5%/time, and the heating speed is 3-4 ℃/min; when the temperature is 1400-1620 ℃, the heating speed is 1-2 ℃/min; when the melting area and the cooling area reach the set temperature of the final stage, the power of a heater of the melting area is reduced to be below 80% and 60% -70%, the power of a heater of the cooling area is reduced to be below 60% and 40% -50%, a jet pipe is opened, high-temperature gas starts to be introduced into the furnace body, the gas temperature is 600-800 ℃, and the gas flow rate is 0.8-2.5 m/s; simultaneously, an air pump of the air pumping port is opened, and air is pumped outwards at the same flow rate as that of the air pumped into the jet pipe so as to ensure that the air pressure in the furnace body is not too high;
(4) continuously introducing high-temperature gas and exhausting, opening a sealing plate between the heating furnace body and the pulling cabin after the feedback temperatures of the melting area and the cooling area are stable, starting a seed crystal pulling module, guiding a seed crystal rod into the heating furnace body through the pulling cabin through a servo motor, wherein the feeding speed is 30-50 cm/min, and feeding at a slower speed after the seed crystal rod reaches the right boundary position of the heating furnace body, wherein the slower speed is 10-15 cm/min; the seed rod reaches the boundary of molten silicon in a graphite crucible in the heating furnace body, meanwhile, the seed crystal on the seed rod is contacted with the silicon melt in the graphite crucible, after 10-15 s, the seed crystal is pulled to the right side, and the pulling speed is 1-3 mm/s;
(5) and (3) when the seed crystal rod is pulled out of the heating furnace body and enters the pulling cabin, closing the sealing plate, taking down the pulled monocrystalline silicon wafer, replacing the seed wafer, and repeating the steps (1) to (4) for continuous production.
9. The method of claim 8, wherein the heating power is limited to 5% -10% at a temperature below 400 ℃, and the current is maintained at 160A ± 5A by observing the current reading on the control panel and appropriately increasing or decreasing the heating power, preferably by 1% for each heating power increase or decrease.
10. The method as set forth in claim 8, wherein the heating module is switched to the time heating mode when the temperature is greater than 400 ℃ and equal to or less than 700 ℃.
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| CN102260903B (en) * | 2011-07-11 | 2013-07-24 | 浙江碧晶科技有限公司 | Method for growing thin silicon crystals |
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