CN209989501U - Pipeline for nitrogen crystal pulling - Google Patents
Pipeline for nitrogen crystal pulling Download PDFInfo
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- CN209989501U CN209989501U CN201920143873.6U CN201920143873U CN209989501U CN 209989501 U CN209989501 U CN 209989501U CN 201920143873 U CN201920143873 U CN 201920143873U CN 209989501 U CN209989501 U CN 209989501U
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Abstract
The utility model provides a nitrogen gas pipeline for crystal pulling, including argon gas control pipeline and nitrogen gas control pipeline, the argon gas control pipeline is connected with the accessory room and the main room of single crystal growing furnace respectively, and the nitrogen gas control pipeline is connected with the accessory room and the main room of single crystal growing furnace respectively, and the argon gas control pipeline is equipped with the argon gas admission line, and the nitrogen gas control pipeline is equipped with the nitrogen gas admission line. The beneficial effects of the utility model are that nitrogen gas crystal pulling is with pipeline structure is simpler, and the installation of being convenient for, simultaneously, adopts the pipeline structure of this structure, separates argon gas and nitrogen gas, can control the input of nitrogen gas and argon gas respectively, and this pipeline still has the flowmeter, can control the input flow of nitrogen gas and argon gas often, and then the volume of argon gas and nitrogen gas accounts for in the control single crystal growing furnace and compares, guarantees the furnace pressure of single crystal growing furnace, guarantees the quality of drawing the single crystal.
Description
Technical Field
The utility model belongs to the technical field of vertical pulling single crystal equipment, especially, relate to a pipeline for nitrogen gas crystal pulling.
Background
The existing czochralski crystal growing furnace utilizes high-purity argon as protective gas to grow single crystal, the method for industrially preparing the high-purity argon is generally a cryogenic air separation method, and the proportion of the argon in the air is less than 0.93 percent; the gas source is short and the production cost is high. The industrial preparation method of high-purity nitrogen comprises a cryogenic air separation nitrogen preparation method, a pressure swing adsorption nitrogen preparation method and a membrane separation nitrogen preparation method, and the preparation methods are various; meanwhile, the proportion of nitrogen in the air is about 78.0 percent, the air source is rich, and the production cost is low. If the nitrogen gas can be used for replacing the argon gas as the protective gas to pull the single crystal, the limitation of a single gas source can be broken, the production cost of the single crystal can be reduced, and the price competitiveness of the single crystal can be improved.
Argon is a monoatomic molecule, is a typical inert gas, and does not have any reaction with silicon during the single crystal pulling process; the nitrogen is diatomic molecules, is not inert gas, is inactive in chemical property and can chemically react with certain substances at high temperature; the nitrogen does not react with the liquid silicon at the temperature of 1300 ℃ or above, but reacts with the solid silicon to generate infusible silicon nitride which floats on the surface of the molten silicon to influence the crystallization.
The existing nitrogen-doped czochralski crystal growing furnace realizes the equal-diameter whole process of single crystal growth, ending and stopping the furnace to use nitrogen, an added nitrogen pipeline can only supply gas to an auxiliary chamber of the single crystal growing furnace, the gas switching of a furnace body cannot be realized in the process of needing isolation, and the nitrogen is only argon in the process of isolation at present; if the main pipelines of argon and nitrogen are directly replaced under the condition that the structure of the current gas circuit is not changed, the whole crystal pulling process is switched to be the nitrogen atmosphere; however, nitrogen does not react with liquid silicon at 1300 ℃ or higher, but reacts with solid silicon to generate infusible silicon nitride which floats on the surface of the molten silicon to affect crystallization, and in the prior art, argon can not be used independently in the melting process, and nitrogen is used in other stages.
Disclosure of Invention
To the above problem, the to-be-solved problem of the utility model is to provide a pipeline is used in nitrogen gas crystal pulling, especially be fit for straight pull single crystal in-process and use, can realize that crystal pulling in-process argon gas and nitrogen gas switch at any time, and the flow size is controllable.
In order to solve the technical problem, the utility model discloses a technical scheme is: the utility model provides a pipeline is used in nitrogen gas crystal pulling, includes argon gas control pipeline and nitrogen gas control pipeline, and the argon gas control pipeline is connected with the accessory room and the main room of single crystal growing furnace respectively, and the nitrogen gas control pipeline is connected with the accessory room and the main room of single crystal growing furnace respectively, and the argon gas control pipeline is equipped with the argon gas admission line, and the nitrogen gas control pipeline is equipped with the nitrogen gas admission line.
Specifically, the argon control pipeline comprises an upper argon pipeline and a lower argon pipeline, and the upper argon pipeline is connected with the lower argon pipeline in parallel.
Further, go up the argon gas pipeline and include argon gas flowmeter and last argon gas valve, go up argon gas flowmeter input and argon gas admission line and be connected, go up argon gas flowmeter output and be connected with last argon gas valve one end, go up the other end and the accessory chamber of argon gas valve and be connected.
Further, the argon gas pipeline includes argon gas flowmeter, first argon gas valve and second argon gas valve down, and the input and the argon gas admission line of argon gas flowmeter are connected down, and the output of argon gas flowmeter is connected with the one end of first argon gas valve down, and the other end and the second of first argon gas valve are connected down the argon gas valve, and the other end and the inlet end of last argon gas valve of argon gas valve are connected down the second, and the inlet end of argon gas valve passes through the pipeline and is connected with the main room under the second.
Specifically, the nitrogen control pipeline comprises an upper nitrogen pipeline and a lower nitrogen pipeline, and the upper nitrogen pipeline is connected in parallel with the lower nitrogen pipeline.
Furthermore, go up the nitrogen gas pipeline and include nitrogen gas flowmeter and last nitrogen gas valve, go up the input and the nitrogen gas admission line connection of nitrogen gas flowmeter, go up the output and last nitrogen gas valve one end of nitrogen gas flowmeter and be connected, go up the other end and the auxiliary chamber connection of nitrogen gas valve.
Further, the lower nitrogen pipeline comprises a lower nitrogen flow meter, a first lower nitrogen valve and a second lower nitrogen valve, the input end of the lower nitrogen flow meter is connected with the nitrogen input pipeline, the output end of the lower nitrogen flow meter is connected with one end of the first lower nitrogen valve, the other end of the first lower nitrogen valve is connected with one end of the second lower nitrogen valve, the other end of the second lower nitrogen valve is connected with the air inlet end of the upper nitrogen valve, and the air inlet end of the second lower nitrogen valve is connected with the main chamber.
Furthermore, the upper argon flowmeter is a mass flowmeter, and the lower argon flowmeter is a float flowmeter.
Further, the upper nitrogen flow meter is a mass flow meter, and the lower nitrogen flow meter is a float flow meter.
Furthermore, the upper argon valve, the first lower argon valve, the second lower argon valve, the upper nitrogen valve, the first lower nitrogen valve and the second lower nitrogen valve are all electromagnetic valves.
The utility model has the advantages and positive effects that:
1. by adopting the technical scheme, the pipeline structure for pulling the nitrogen is simpler and convenient to install, meanwhile, the pipeline structure with the structure is adopted, the argon and the nitrogen are separated, the input of the nitrogen and the argon can be respectively controlled, the pipeline is also provided with a flowmeter, the input flow of the nitrogen and the argon can be controlled at any time, the volume ratio of the argon to the nitrogen in the single crystal furnace is further controlled, the furnace pressure of the single crystal furnace is ensured, and the quality of pulled single crystals is ensured;
2. the pipeline is adopted for pulling the single crystal, nitrogen is not introduced in the silicon melting process, and nitrogen is introduced in the other processes in the straight pulling single crystal process; the crystal formation and quality of the nitrogen-doped single crystal produced by the process method are not different from those of the conventional single crystal, the process method has actual production value, uses nitrogen to the maximum extent, and reduces the crystal pulling cost;
3. the argon and nitrogen can be switched randomly in the crystal pulling process, the nitrogen flow in the crystal pulling process is controllable, one gas can be switched to another gas when the other gas is abnormal, the abnormal condition is avoided, and the quality of the czochralski crystal is ensured.
Drawings
Fig. 1 is a schematic structural diagram of an embodiment of the present invention.
In the figure:
1. a second lower nitrogen gas valve 2, a first lower nitrogen gas valve 3 and a lower nitrogen gas valve flowmeter
4. An upper nitrogen valve flowmeter 5, a nitrogen inlet pipeline 6 and a main chamber
7. Argon gas inlet pipe 8, lower argon gas flowmeter 9, first lower argon gas valve
10. A second lower argon valve 11, an upper argon flow meter 12 and an upper argon valve
13. Auxiliary chamber 14, nitrogen feeding valve
Detailed Description
The present embodiment will be further described with reference to the accompanying drawings and specific embodiments.
Fig. 1 shows the structure of an embodiment of the utility model, the concrete tube coupling relation of this embodiment is specifically shown, this embodiment relates to a nitrogen gas draws and carries out nitrogen-doped single crystal drawing process with pipeline and adoption this nitrogen gas draws and uses the pipeline, be fit for using at the czochralski single crystal in-process, when the czochralski single crystal, join in marriage the dish with nitrogen gas and the dish is joined in marriage to argon gas and carry out the tube coupling, and be connected with the main room and the accessory chamber of single crystal growing furnace respectively, carry out the input of nitrogen gas and argon gas to the single crystal growing furnace, and the access time and the flow of control nitrogen gas and argon gas, the realization is pulled under the atmosphere of nitrogen gas and argon gas, realize furthest's use nitrogen gas, reduce the.
Specifically, foretell pipeline for nitrogen gas crystal pulling for control in each process of czochralski crystal in-process argon gas and the time and the flow of letting in of nitrogen gas, only let in argon gas in the silicon melting process, let in argon gas and nitrogen gas in other processes, realize that argon gas and nitrogen gas switch at any time in the crystal pulling process, and the flow size of nitrogen gas and argon gas is controllable, can realize furthest's nitrogen gas use, reduction in production cost. As shown in fig. 1, the pipeline for pulling the nitrogen gas comprises an argon gas control pipeline and a nitrogen gas control pipeline, wherein the argon gas control pipeline is respectively connected with an auxiliary chamber 13 and a main chamber 6 of a single crystal furnace, the nitrogen gas control pipeline is respectively connected with the auxiliary chamber 13 and the main chamber 6 of the single crystal furnace, the argon gas control pipeline is used for controlling argon gas entering the main chamber 6 and the auxiliary chamber 13 of the single crystal furnace and flow rate thereof, the nitrogen gas control pipeline is used for controlling nitrogen gas entering the main chamber 6 and the auxiliary chamber 13 of the single crystal furnace and flow rate thereof, the argon gas control pipeline is provided with an argon gas inlet pipeline 7, the argon gas inlet pipeline 7 is used for introducing the argon gas, the nitrogen gas control pipeline is provided with a nitrogen gas inlet pipeline 5, and the. When carrying out czochralski single crystal, argon gas and nitrogen gas are respectively led in from argon gas inlet pipe 7 and nitrogen gas inlet pipe 5, in the process of melting the silicon material, the nitrogen gas control pipeline is closed, the argon gas control pipeline is opened, argon gas is led in to the single crystal furnace, after the process of melting the silicon material, the seeding process begins, the nitrogen gas control pipeline is opened, nitrogen gas is led in to the single crystal furnace, argon gas and nitrogen gas are provided in the single crystal furnace, seeding, necking down, shouldering, shoulder rotating, diameter equalizing and ending processes are carried out under the atmosphere of the mixed gas of argon gas and nitrogen gas, and the czochralski single crystal is carried out.
The argon control pipeline is respectively connected with the main chamber 6 and the auxiliary chamber 13 of the single crystal furnace and used for providing argon for the main chamber 6 and the auxiliary chamber 13 of the single crystal furnace, the argon control pipeline comprises an upper argon pipeline and a lower argon pipeline, the upper argon pipeline is connected with the lower argon pipeline in parallel, the upper argon pipeline is used for providing argon for the auxiliary chamber 13 of the single crystal furnace, the lower argon pipeline is used for providing argon for the main chamber 6 of the single crystal furnace, so that the atmosphere concentration of the argon in the single crystal furnace is ensured, the normal pulling of the czochralski single crystal is ensured, and the quality of the single crystal is ensured.
The aforesaid is gone up the argon gas pipeline and is included argon gas flowmeter 11 and last argon gas valve 12, and it is connected with argon gas admission line 7 through gas transmission pipeline to go up argon gas flowmeter 11 input, goes up 11 output of argon gas flowmeter and last 12 one ends of argon gas valve and passes through gas transmission pipeline connection, and the other end of going up argon gas valve 12 passes through gas transmission pipeline connection with accessory chamber 13 for the argon gas gets into gas transmission pipeline by argon gas admission line 7, and the process is gone up in argon gas flowmeter 11 and last argon gas valve 12 get into single crystal growing furnace accessory chamber 13. The upper argon gas flow meter 11 is a mass flow meter and measures the mass flow of argon gas passing through the upper argon gas line, so that an operator can clearly know the total amount of argon gas entering the auxiliary chamber 13 of the single crystal furnace through the upper argon gas line. The upper argon gas valve 12 is a solenoid valve, and the solenoid valve is electrically connected with the controller, and the opening and closing of the solenoid valve are controlled by the controller. The mass flow meter is electrically connected with the controller, and displays the measured mass flow of the argon gas on the controller at any time, so that an operator can conveniently master the flow of the argon gas entering the auxiliary chamber 13 of the single crystal furnace at any time.
The lower argon gas pipeline comprises a lower argon gas flowmeter 8, a first lower argon gas valve 9 and a second lower argon gas valve 10, wherein the input end of the lower argon gas flowmeter 8 is connected with an argon gas inlet pipeline 7 through a gas transmission pipeline, the output end of the lower argon gas flowmeter 8 is connected with one end of the first lower argon gas valve 9 through a gas transmission pipeline, the other end of the first lower argon gas valve 9 is connected with one end of the second lower argon gas valve 10 through a gas transmission pipeline, the other end of the second lower argon gas valve 10 is connected with the gas inlet end of an upper argon gas valve 12 through a gas transmission pipeline, the gas inlet end of the second lower argon gas valve 10 is connected with the main chamber 6 through a gas transmission pipeline, meanwhile, the gas outlet end of the first lower argon gas valve 9 is connected with the main chamber 6 of the single crystal furnace through a gas transmission pipeline, so that argon gas enters the main chamber 6 of the single crystal furnace through the lower argon gas pipeline, the argon gas enters the main chamber 6 of the single crystal, meanwhile, argon gas passing through the upper argon gas flow meter 11 enters the main chamber 6 of the single crystal furnace through the second lower argon gas valve 10. That is, the argon gas pipeline divides the argon gas entering the pipeline into two ways, and the two ways enter the main chamber 6 and the sub-chamber 13 of the single crystal furnace respectively, so as to provide argon gas for the main chamber 6 and the sub-chamber 13 of the single crystal furnace, the argon gas entering the sub-chamber 13 of the single crystal furnace also passes through the second argon gas valve 10, the second argon gas valve 10 is a one-way solenoid valve, so that the argon gas enters the main chamber 6 of the single crystal furnace through the first argon gas valve 10, and provides argon gas for the main chamber 6 of the single crystal furnace, the upper argon gas pipeline and the lower argon gas pipeline of the argon gas control pipeline respectively provide argon gas for the main chamber 6 and the sub-chamber 13 of the single crystal furnace, the argon gas entering the main chamber 6 is two ways of argon gas, and.
The lower argon gas flowmeter 8 is a float flowmeter and is used for measuring the volume flow of argon gas entering a lower argon gas pipeline, so that an operator can know the flow of the argon gas entering the main chamber 6 of the single crystal furnace at any time. Foretell argon gas valve 9 under is the solenoid valve, is the water-cooling solenoid valve, argon gas valve 10 is the solenoid valve under the second, and argon gas valve 10 is connected with the controller electricity under first argon gas valve 9 and the second respectively, the opening and closing of argon gas valve 10 under the controller control first argon gas valve 9 and the second, and then the argon gas in control main room 6 and the accessory chamber 13 that get into the single crystal growing furnace, and simultaneously, the float flowmeter is connected with the controller electricity, the operating personnel of being convenient for master the volume flow who gets into the interior argon gas of single crystal growing furnace main room 6 often, the drawing of the czochralski crystal of being convenient for.
The nitrogen control pipeline comprises an upper nitrogen pipeline and a lower nitrogen pipeline, and the upper nitrogen pipeline and the lower nitrogen pipeline are connected in parallel and used for conveying nitrogen to the main chamber 6 and the auxiliary chamber 13 of the single crystal furnace. The upper nitrogen pipeline comprises an upper nitrogen flow meter 4 and an upper nitrogen valve 14, the input end of the upper nitrogen flow meter 4 is connected with the nitrogen inlet pipeline 5 through a gas transmission pipeline, the output end of the upper nitrogen flow meter 4 is connected with one end of the upper nitrogen valve 14 through the gas transmission pipeline, and the other end of the upper nitrogen valve 14 is connected with the auxiliary chamber 13 through the gas transmission pipeline. The nitrogen enters the auxiliary chamber 13 of the single crystal furnace through the nitrogen inlet pipeline 5 through the upper nitrogen flow meter 4 and the upper nitrogen valve 14 to provide the nitrogen for the auxiliary chamber 13 of the single crystal furnace, the upper nitrogen flow meter 4 is a mass flow meter and measures the mass flow of the nitrogen passing through the upper nitrogen pipeline, so that an operator can clearly know the total amount of the nitrogen entering the auxiliary chamber 13 of the single crystal furnace through the upper nitrogen pipeline. The nitrogen adding valve 14 is an electromagnetic valve, and the electromagnetic valve is electrically connected with the controller, and the opening and closing of the electromagnetic valve are controlled by the controller. The mass flow meter is electrically connected with the controller, and displays the measured mass flow of the nitrogen on the controller at any time, so that an operator can conveniently master the flow of the nitrogen entering the auxiliary chamber 13 of the single crystal furnace at any time.
The lower nitrogen pipeline comprises a lower nitrogen flow meter 3, a first lower nitrogen valve 2 and a second lower nitrogen valve 1, the input end of the lower nitrogen flow meter 3 is connected with a nitrogen inlet pipeline 5 through a gas transmission pipeline, the output end of the lower nitrogen flow meter 3 is connected with one end of the first lower nitrogen valve 2 through a gas transmission pipeline, the other end of the first lower nitrogen valve 2 is connected with one end of the second lower nitrogen valve 1 through a gas transmission pipeline, the other end of the second lower nitrogen valve 1 is connected with the gas inlet end of the upper nitrogen valve 14 through a gas transmission pipeline, meanwhile, the gas inlet end of the second nitrogen down valve 1 is connected with the main chamber 6 through a gas transmission pipeline, that is, the gas outlet end of the first nitrogen down valve 2 is connected with the main chamber 6 of the single crystal furnace through a gas transmission pipeline, so that nitrogen enters the main chamber 6 of the single crystal furnace through the lower nitrogen pipeline, and the nitrogen enters the main chamber 6 of the single crystal furnace through the nitrogen inlet pipeline 5 through the lower nitrogen flow meter 3 and the first lower nitrogen valve 2. That is, the nitrogen control pipeline divides the nitrogen entering the pipeline into two paths, the two paths enter the main chamber 6 and the sub-chamber 13 of the single crystal furnace respectively, the nitrogen is provided for the main chamber 6 and the sub-chamber 13 of the single crystal furnace, the nitrogen entering the upper nitrogen pipeline in the sub-chamber 13 of the single crystal furnace also passes through the second lower nitrogen valve 1, the second lower nitrogen valve 1 is a one-way solenoid valve, so that the nitrogen enters the main chamber 6 of the single crystal furnace and provides the nitrogen for the main chamber 6 of the single crystal furnace, but the nitrogen in the lower nitrogen pipeline cannot enter the sub-chamber 13 of the single crystal furnace, the upper nitrogen pipeline of the nitrogen control pipeline provides the nitrogen for the sub-chamber 13 and the main chamber 6 of the single crystal furnace, and the lower nitrogen pipeline provides the nitrogen for the main chamber 6 of the single.
The lower nitrogen gas flowmeter 3 is a float flowmeter and is used for measuring the volume flow of nitrogen gas passing through the lower nitrogen gas pipeline, so that an operator can know the flow of nitrogen gas entering the main chamber 6 of the single crystal furnace at any time. Foretell first nitrogen gas valve 2 is the solenoid valve, is the water-cooling solenoid valve, nitrogen gas valve 1 is the solenoid valve under the second, and nitrogen gas valve 2 and second are nitrogen gas valve 1 down and are connected with the controller electricity respectively, the opening and closing of nitrogen gas valve 1 under the controller control first nitrogen gas valve 2 and the second, and then the nitrogen gas in control main room 6 and the locellus 13 that get into the single crystal growing furnace, and simultaneously, the float flowmeter is connected with the controller electricity, the operating personnel of being convenient for master the volume flow who gets into single crystal growing furnace main room 6 interior nitrogen gas often, the drawing of the czochralski crystal of being convenient for.
In the nitrogen pulling pipeline, an upper argon valve 12, a first lower argon valve 9, a second lower argon valve 10, an upper nitrogen valve 14, a first lower nitrogen valve 2, a second lower nitrogen valve 1, an upper argon flow meter 11, a lower argon flow meter 8, an upper nitrogen flow meter 4 and a lower nitrogen flow meter 3 are respectively electrically connected with a controller, and the controller controls the upper argon valve 12, the first lower argon valve 9, the second lower argon valve 10, the upper nitrogen valve 14, the first lower nitrogen valve 2 and the second lower nitrogen valve 1 to be opened and closed according to the size of data measured by the upper argon flow meter 8, the lower argon flow meter 11, the upper nitrogen flow meter 4 and the lower nitrogen flow meter 3.
The first lower argon gas valve 9 is kept in a normally open state during the use process, so that the argon gas enters the main chamber of the single crystal furnace from time to time.
In the czochralski single crystal process, when dismantling the stove, after the stove loading, melt the siliconization material process, open the argon gas control pipeline, close the nitrogen gas control pipeline, to single crystal furnace main room 6 and accessory room 13 fill argon gas, the argon gas is by the argon gas admission line through last argon gas flowmeter 11 and last argon gas valve 12 get into in the single crystal furnace accessory room 13, simultaneously the argon gas is by argon gas admission line 7 through argon gas flowmeter 8 and first argon gas valve 9 get into single crystal furnace main room 6 under down, simultaneously through last argon gas flowmeter 11 and second under the argon gas valve 10 get into in the single crystal furnace main room 6, make in the siliconization material process, the protective gas in the single crystal furnace is the argon gas. And after the silicon melting material is finished, opening the nitrogen control pipeline, keeping the opening of the argon control pipeline, and filling nitrogen and argon into the single crystal furnace to ensure that the protective gas in the single crystal furnace is the mixed gas of the argon and the nitrogen. Nitrogen gas gets into single crystal growing furnace auxiliary chamber 13 through last nitrogen gas flowmeter 4 and last nitrogen gas valve 14 through nitrogen gas inlet pipe 5 in, nitrogen gas gets into single crystal growing furnace main chamber 6 through nitrogen gas flowmeter 3, first nitrogen gas valve 2 down by nitrogen gas inlet pipe 5 simultaneously, and nitrogen gas gets into single crystal growing furnace main chamber 6 through nitrogen gas flowmeter 4 and second nitrogen gas valve 1 down for when carrying out seeding, the necking down, shoulder, the shoulder that turns round, constant diameter and ending, be the mixed atmosphere of argon gas and nitrogen gas in the single crystal growing furnace.
The nitrogen gas does not react with the liquid silicon at the temperature of more than 1300 ℃, but reacts with the solid silicon to generate infusible silicon nitride which floats on the surface of the molten silicon to influence the crystallization, and the nitrogen gas and the argon gas are used as protective gases in the process of pulling the single crystal, thereby reducing the content of air in a single crystal furnace and the influence on the pulled single crystal. Therefore, in the czochralski single crystal process, when melting the siliconization material process, open the argon gas control pipeline, close the nitrogen gas control pipeline, make at the siliconization material in-process of melting, be the argon gas atmosphere in main room and the accessory room of single crystal growing furnace, after melting the siliconization material process, carry out the seeding process, at this moment, open the nitrogen gas control pipeline, to filling into nitrogen gas in main room and the accessory room of single crystal growing furnace, make the main room and the accessory room of single crystal growing furnace in be the mist of nitrogen gas and argon gas, follow-up process with this czochralski single crystal carries out. Therefore, two kinds of protective gas are ensured to be provided in the Czochralski single crystal process, when one kind of protective gas pipeline is abnormal, the other kind of protective gas can be used for protecting the Czochralski single crystal process, and the abnormal condition is avoided.
The nitrogen-doped single crystal pulling process comprises the steps of disassembling a furnace, charging the furnace, melting silicon, seeding, necking, shouldering, turning shoulder, equalizing diameter and ending in sequence, so that the straight pulling of the single crystal is carried out, in the process of melting silicon, an argon control pipeline is opened, argon is introduced, the nitrogen control pipeline is closed, nitrogen is not introduced, only argon is introduced in the process of melting silicon, the argon serves as protective gas, the doping of impurities in the process of pulling the single crystal is reduced, and meanwhile, the argon does not react with the molten silicon and solid silicon, so that the normal operation of the process of melting silicon is ensured; after the material that melts the siliconization, the seeding is carried out in proper order, the necking down, put the shoulder, the shoulder rotates, constant diameter and ending, carry out the czochralski single crystal, at the seeding, the necking down, put the shoulder, the shoulder rotates, constant diameter and ending in-process, open nitrogen control pipeline, let in nitrogen gas to the main room and the accessory room of single crystal growing furnace, keep the state that argon gas control pipeline opened simultaneously, make nitrogen gas control pipeline and argon gas control pipeline all open, let in nitrogen gas and argon gas simultaneously in the main room and the accessory room of single crystal growing furnace, make argon gas and nitrogen gas all regard as protective gas, guarantee the normal clear of czochralski single crystal, and adopt nitrogen gas as protective gas, can carry out nitrogen doping to the single crystal at the czochralski single crystal in-process, guarantee the resistivity of single crystal, guarantee.
In the Czochralski single crystal pulling process, the first lower argon valve 9 is kept in a normally open state, the flow of argon is 25-30slpm, after the silicon melting material is finished, the nitrogen control pipeline is opened when seeding, necking, shouldering, shoulder rotating, diameter equalizing and ending are carried out, the flow of nitrogen is 20-35slpm, the real-time volume proportion of nitrogen is 38% -44%, preferably, the real-time volume proportion of nitrogen is 41.0%, and when nitrogen and argon are introduced simultaneously, the furnace pressure of the single crystal furnace is ensured, the furnace pressure of the single crystal furnace is 9-15torr, and the fluctuation of the furnace pressure to the temperature in the single crystal furnace is avoided. The nitrogen is diatomic molecules, and can absorb part of heat in the furnace when being decomposed, so that the parameter set temperature reduction amount in the furnace is properly reduced when the nitrogen is introduced until the temperature stabilization is finished and the temperature in the furnace is stabilized.
The utility model has the advantages and positive effects that: by adopting the technical scheme, the pipeline structure for pulling the nitrogen is simpler and convenient to install, meanwhile, the pipeline structure with the structure is adopted, the argon and the nitrogen are separated, the input of the nitrogen and the argon can be respectively controlled, the pipeline is also provided with a flowmeter, the input flow of the nitrogen and the argon can be controlled at any time, the volume ratio of the argon to the nitrogen in the single crystal furnace is further controlled, the furnace pressure of the single crystal furnace is ensured, and the quality of pulled single crystals is ensured; the pipeline is adopted for pulling the single crystal, nitrogen is not introduced in the silicon melting process, and nitrogen is introduced in the other processes in the straight pulling single crystal process; the crystal formation and quality of the nitrogen-doped single crystal produced by the process method are not different from those of the conventional single crystal, the process method has actual production value, uses nitrogen to the maximum extent, and reduces the crystal pulling cost; the argon and nitrogen can be switched randomly in the crystal pulling process, the nitrogen flow in the crystal pulling process is controllable, one gas can be switched to another gas when the other gas is abnormal, the abnormal condition is avoided, and the quality of the czochralski crystal is ensured.
While one embodiment of the present invention has been described in detail, the description is only a preferred embodiment of the present invention, and should not be considered as limiting the scope of the present invention. All the equivalent changes and improvements made according to the application scope of the present invention should still fall within the patent coverage of the present invention.
Claims (10)
1. A pipeline for pulling nitrogen is characterized in that: the argon control pipeline is respectively connected with an auxiliary chamber and a main chamber of the single crystal furnace, the nitrogen control pipeline is respectively connected with the auxiliary chamber and the main chamber of the single crystal furnace, the argon control pipeline is provided with an argon inlet pipeline, and the nitrogen control pipeline is provided with a nitrogen inlet pipeline.
2. A nitrogen crystal puller as set forth in claim 1 wherein: the argon gas control pipeline comprises an upper argon gas pipeline and a lower argon gas pipeline, and the upper argon gas pipeline is connected with the lower argon gas pipeline in parallel.
3. A nitrogen crystal puller as set forth in claim 2 wherein: go up the argon gas pipeline and include argon gas flowmeter and last argon gas valve, go up argon gas flowmeter input with the argon gas admission line is connected, go up argon gas flowmeter output with it connects to go up argon gas valve one end, go up the other end of argon gas valve with the accessory chamber is connected.
4. A nitrogen crystal puller as set forth in claim 3 wherein: argon gas pipeline includes argon gas flowmeter, first argon gas valve and second argon gas valve down, argon gas flowmeter's input down with the argon gas admission line is connected, argon gas flowmeter's output down with the one end of first argon gas valve is connected, the other end of first argon gas valve with the argon gas valve is connected under the second, the other end of second argon gas valve with the inlet end of going up the argon gas valve is connected, the inlet end of second argon gas valve pass through the pipeline with the main room is connected down.
5. A nitrogen crystal puller as set forth in any one of claims 1 to 4 wherein: the nitrogen control pipeline comprises an upper nitrogen pipeline and a lower nitrogen pipeline, and the upper nitrogen pipeline is connected with the lower nitrogen pipeline in parallel.
6. A nitrogen crystal puller as set forth in claim 5 wherein: go up the nitrogen gas pipeline and include nitrogen gas flowmeter and last nitrogen gas valve, go up the input of nitrogen gas flowmeter with nitrogen gas admission line connects, go up nitrogen gas flowmeter's output with last nitrogen gas valve one end is connected, go up the other end of nitrogen gas valve with the accessory chamber is connected.
7. A nitrogen crystal puller as set forth in claim 6 wherein: the lower nitrogen pipeline comprises a lower nitrogen flow meter, a first lower nitrogen valve and a second lower nitrogen valve, the input end of the lower nitrogen flow meter is connected with the nitrogen inlet pipeline, the output end of the lower nitrogen flow meter is connected with one end of the first lower nitrogen valve, the other end of the first lower nitrogen valve is connected with one end of the second lower nitrogen valve, the other end of the second lower nitrogen valve is connected with the inlet end of the upper nitrogen valve, and the inlet end of the second lower nitrogen valve is connected with the main chamber.
8. A nitrogen crystal puller as set forth in claim 4 wherein: the upper argon flowmeter is a mass flowmeter, and the lower argon flowmeter is a float flowmeter.
9. A nitrogen crystal puller as set forth in claim 7 wherein: the upper nitrogen flowmeter is a mass flowmeter, and the lower nitrogen flowmeter is a float flowmeter.
10. A nitrogen crystal puller as set forth in claim 9 wherein: the upper argon gas valve, the first lower argon gas valve, the second lower argon gas valve, the upper nitrogen valve, the first lower nitrogen valve and the second lower nitrogen valve are all electromagnetic valves.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109695056A (en) * | 2019-01-28 | 2019-04-30 | 内蒙古中环光伏材料有限公司 | A kind of nitrogen crystal pulling pipeline and nitrating crystal-pulling technique |
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2019
- 2019-01-28 CN CN201920143873.6U patent/CN209989501U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109695056A (en) * | 2019-01-28 | 2019-04-30 | 内蒙古中环光伏材料有限公司 | A kind of nitrogen crystal pulling pipeline and nitrating crystal-pulling technique |
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