CN112251805B - Nitrogen-doped P-type silicon master alloy and preparation method thereof, nitrogen-doped polycrystalline silicon ingot and preparation method thereof - Google Patents
Nitrogen-doped P-type silicon master alloy and preparation method thereof, nitrogen-doped polycrystalline silicon ingot and preparation method thereof Download PDFInfo
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- 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
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- C—CHEMISTRY; METALLURGY
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- 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
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Abstract
The invention provides a nitrogen-doped P-type silicon master alloy and a preparation method thereof, a nitrogen-doped polycrystalline silicon ingot and a preparation method thereof, wherein the preparation method of the nitrogen-doped P-type silicon master alloy comprises the following steps: feeding, namely feeding a silicon material and boron nitride into an ingot furnace; and (3) carrying out polycrystal ingot casting, and producing the nitrogen-doped P-type silicon master alloy ingot in an ingot furnace through the steps of vacuumizing, heating, melting, crystal growing, annealing and cooling in sequence. After the boron nitride and the silicon material are mixed, a polycrystalline ingot casting method is adopted, nitrogen elements are introduced into the mother alloy while the mother alloy with the required resistivity is obtained, and then the nitrogen elements are introduced into the mother alloy when the polycrystalline silicon ingot is produced, so that the mechanical strength of the polycrystalline silicon ingot can be increased, the fragment rate in slicing and other processes is effectively reduced, and the cost is greatly reduced. In addition, the method uses a polycrystalline ingot furnace to produce the nitrogen-doped P-type silicon master alloy, so that the yield of the master alloy can be increased, and the production cost can be reduced.
Description
Technical Field
The application relates to the technical field of polycrystalline silicon ingots, in particular to a nitrogen-doped P-type silicon master alloy and a preparation method thereof, and a nitrogen-doped polycrystalline silicon ingot and a preparation method thereof.
Background
With the development and wide use of diamond wire silicon wafer cutting technology, the thickness of the silicon wafer is continuously reduced. However, the reduction of the thickness of the silicon wafer increases the probability of fragments in the cutting process, the preparation of the solar cell, the cell assembly and other processes. Therefore, there is a need to increase the mechanical strength of silicon wafers to reduce the occurrence of chipping.
Researches find that the nitrogen element can effectively increase the mechanical strength of silicon, and the nitrogen element is doped into a crystal silicon ingot based on the nitrogen element, so that the aim of increasing the mechanical strength of the crystal ingot can be achieved. In the prior art, nitrogen is introduced in the silicon melting process, and reacts with the molten silicon to enter the silicon melt, and the cast polycrystalline silicon is formed after cooling. In the method, the nitrogen and the silicon melt can be fully reacted only by keeping the temperature for a long time under the high-temperature condition, and the nitrogen doping is not uniform.
In view of the above, it is desirable to provide a nitrogen-doped P-type silicon master alloy and a method for preparing the same, a nitrogen-doped polysilicon ingot and a method for preparing the same, so as to solve the above problems.
Disclosure of Invention
The invention aims to provide a nitrogen-doped P-type silicon master alloy and a preparation method thereof, a nitrogen-doped polycrystalline silicon ingot and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a nitrogen-doped P-type silicon master alloy comprises the following steps:
feeding, namely feeding a silicon material and boron nitride into an ingot furnace;
and (3) carrying out polycrystal ingot casting, and producing the nitrogen-doped P-type silicon master alloy ingot in an ingot furnace through the steps of vacuumizing, heating, melting, crystal growing, annealing and cooling in sequence.
As a further improvement of the invention, the sum of the amount of the boron element contained in the silicon material and the amount of the boron element in the boron nitride is consistent with the amount of the boron element in the preformed nitrogen-doped P-type silicon master alloy.
As a further improvement of the invention, the concentration of the boron element in the silicon material is lower than that in the preformed nitrogen-doped P-type silicon master alloy.
As a further improvement of the invention, the silicon material is a P-type silicon material, the resistivity is more than 1 omega cm, and the purity is more than 99.9999%.
As a further improvement of the invention, the method also comprises the following steps: before feeding, calculating the required dosage of boron nitride according to the concentration of boron element in a preformed nitrogen-doped P-type silicon master alloy ingot and the concentration of boron element contained in the silicon material.
As a further improvement of the invention, the calculation method comprises the following steps:
calculating the concentration of boron element in the silicon material according to formula 1,
equation 1:
N0is the concentration of boron element in the silicon material, rho1Is the resistivity of the silicon material;
calculating the concentration of boron element in the silicon material and the boron nitride in the preformed N-doped P-type silicon master alloy crystal ingot according to the formula 2,
equation 2:
N1the concentration of boron elements in the silicon material and the boron nitride in a preformed nitrogen-doped P-type silicon master alloy crystal ingot, wherein M is the dosage of the silicon material, and M is the dosage of the boron nitride;
calculating the segregation concentrations of boron elements in the silicon material and the boron nitride at different heights in the silicon melt according to a formula 3,
equation 3:
N2the segregation concentrations of boron elements in the silicon material and the boron nitride at different heights in the silicon melt are shown, f is the segregation fraction, and k is the segregation coefficient of the boron elements in the silicon;
the resistivities of different heights in the preformed nitrogen-doped P-type silicon master alloy ingot were calculated according to equation 4,
equation 4:
ρ is the resistivity at different heights in the pre-formed nitrogen-doped P-type silicon master alloy ingot.
As a further improvement of the invention, the polycrystalline ingot casting step specifically comprises the following steps:
the vacuumizing specifically comprises: vacuumizing to 0.05mbar and below, and starting to operate the ingot furnace;
and/or, the heating specifically comprises: setting heating power, gradually increasing the heating power from 0 to 80%, operating for 8-10 h, continuously introducing argon gas in the process, and gradually increasing the pressure to 600 mbar; when the temperature of TC1 reaches 1500 ℃, entering a melting stage;
and/or, the melting specifically comprises: the process is operated for 8-10 h, the temperature of TC1 is kept between 1530 ℃ and 1550 ℃, and the pressure is kept at 600 mbar;
and/or, the crystal growth specifically comprises: in a crystal growth stage, opening a heat insulation cage to release heat, operating for 28-32 h, keeping the temperature of TC1 at 1400-1430 ℃ and keeping the pressure at 600 mbar;
and/or, the annealing specifically comprises: in the annealing stage, closing the heat insulation cage, reducing the temperature of TC1 to the annealing temperature, keeping the pressure at 600mbar, and operating the process for 2-3 h;
and/or, the cooling specifically comprises: and (3) entering a cooling stage, gradually opening the heat insulation cage to the maximum height, gradually increasing the argon gas inflow, increasing the pressure to 750mbar, and stopping the furnace and discharging ingots when the temperature of TC2 is reduced to 450 ℃.
In order to realize the purpose, the invention also provides a nitrogen-doped P-type silicon master alloy which is prepared by any one of the preparation methods of the nitrogen-doped P-type silicon master alloy.
In order to achieve the purpose, the invention also provides a preparation method of the nitrogen-doped polycrystalline silicon ingot, which comprises the preparation method of any one of the nitrogen-doped P-type silicon master alloy.
In order to realize the purpose, the invention also provides a nitrogen-doped polycrystalline silicon ingot prepared by the preparation method of the nitrogen-doped polycrystalline silicon ingot.
Compared with the prior art, the invention has the beneficial effects that: after the boron nitride and the silicon material are mixed, a polycrystalline ingot casting method is adopted, nitrogen elements are introduced into the mother alloy while the mother alloy with the required resistivity is obtained, and then the nitrogen elements are introduced into the mother alloy when the polycrystalline silicon ingot is produced, so that the mechanical strength of the polycrystalline silicon ingot can be increased, the fragment rate in slicing and other processes is effectively reduced, and the cost is greatly reduced. In addition, the method uses a polycrystalline ingot furnace to produce the nitrogen-doped P-type silicon master alloy, so that the yield of the master alloy can be increased, and the production cost can be reduced.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The present application will be described in detail below with reference to specific embodiments. These embodiments are not intended to limit the present application, and structural, methodological, or functional changes made by those skilled in the art according to these embodiments are included in the scope of the present application.
The inventor finds in research that boron nitride contains boron and nitrogen and can be used as a P-type dopant and can be introduced into a silicon ingot, so that the boron nitride can be added into a silicon material, a polycrystalline ingot furnace is used for producing a nitrogen-doped P-type silicon master alloy, and the nitrogen is further introduced into a common polycrystalline silicon ingot.
The invention discloses a method for producing nitrogen-doped P-type silicon master alloy by using a polycrystalline ingot furnace, which comprises the following steps:
feeding, namely feeding a silicon material and boron nitride into an ingot furnace;
and (3) carrying out polycrystal ingot casting, and producing the nitrogen-doped P-type silicon master alloy ingot in an ingot furnace through the steps of vacuumizing, heating, melting, crystal growing, annealing and cooling in sequence.
Compared with the existing method for producing the master alloy, the method for producing the master alloy has the advantages that after the boron nitride and the silicon material are mixed, a polycrystalline ingot casting method is adopted, nitrogen is introduced into the master alloy while the required resistivity master alloy is obtained, and further, when the polycrystalline silicon ingot is produced, the nitrogen is introduced into the master alloy, so that the mechanical strength of the polycrystalline silicon ingot can be increased, the fragment rate in slicing and other processes is effectively reduced, and the cost is greatly reduced. In addition, the method uses a polycrystalline ingot furnace to produce the nitrogen-doped P-type silicon master alloy, so that the yield of the master alloy can be increased, and the production cost can be reduced.
Furthermore, the sum of the amount of the boron element contained in the silicon material and the amount of the boron element in the boron nitride is consistent with the amount of the boron element in the preformed nitrogen-doped P-type silicon master alloy.
According to the segregation condition of the boron element in the silicon melt, the method calculates the required added boron nitride amount. Specifically, selecting the corresponding silicon material according to the concentration of the boron element in the nitrogen-doped P-type silicon master alloy, wherein the concentration of the boron element in the silicon material is lower than that of the boron element in the preformed nitrogen-doped P-type silicon master alloy; for example, the silicon material is a P-type silicon material, the resistivity is more than 1 omega cm, and the purity is more than 99.9999 percent.
According to the concentration of boron element in the preformed nitrogen-doped P-type silicon master alloy ingot and the concentration of boron element contained in the silicon material, the amount of boron nitride required to be added is accurately calculated, and the calculation process comprises the following steps:
calculating the concentration of boron element in the silicon material according to formula 1,
equation 1:
N0is the concentration of boron element in the silicon material, rho1Is the resistivity of the silicon material;
the formula 1 is described in GB/T13389-2014, the conversion rule of resistivity and dopant concentration of boron-doped, phosphorus-doped, arsenic-doped silicon single crystal.
Calculating the concentration of boron element in the silicon material and the boron nitride in the preformed N-doped P-type silicon master alloy crystal ingot according to the formula 2,
equation 2:
N1the concentration of boron elements in the silicon material and the boron nitride in a preformed nitrogen-doped P-type silicon master alloy crystal ingot, wherein M is the dosage of the silicon material, and M is the dosage of the boron nitride;
calculating the segregation concentrations of boron elements in the silicon material and the boron nitride at different heights in the silicon melt according to a formula 3,
equation 3:
N2the segregation concentrations of boron elements in the silicon material and the boron nitride at different heights in the silicon melt are shown, f is the segregation fraction, and k is the segregation coefficient of the boron elements in the silicon;
the resistivities of different heights in the preformed nitrogen-doped P-type silicon master alloy ingot were calculated according to equation 4,
equation 4:
rho is the resistivity of different heights in the preformed nitrogen-doped P-type silicon master alloy crystal ingot;
the formula 4 is described in GB/T13389-2014, the conversion rule between resistivity and dopant concentration of boron-doped, phosphorus-doped, arsenic-doped silicon single crystal.
Further, the polycrystalline ingot casting method specifically comprises the following steps:
the vacuumizing specifically comprises: vacuumizing to 0.05mbar and below, and starting to operate the ingot furnace;
and/or, the heating specifically comprises: setting heating power, gradually increasing the heating power from 0 to 80%, operating for 8-10 h, continuously introducing argon gas in the process, and gradually increasing the pressure to 600 mbar; when the temperature of TC1 reaches 1500 ℃, entering a melting stage;
and/or, the melting specifically comprises: the process is operated for 8-10 h, the temperature of TC1 is kept between 1530 ℃ and 1550 ℃, and the pressure is kept at 600 mbar;
and/or, the crystal growth specifically comprises: in a crystal growth stage, opening a heat insulation cage to release heat, operating for 28-32 h, keeping the temperature of TC1 at 1400-1430 ℃ and keeping the pressure at 600 mbar;
and/or, the annealing specifically comprises: in the annealing stage, closing the heat insulation cage, reducing the temperature of TC1 to the annealing temperature, keeping the pressure at 600mbar, and operating the process for 2-3 h;
and/or, the cooling specifically comprises: and (3) entering a cooling stage, gradually opening the heat insulation cage to the maximum height, gradually increasing the argon gas inflow, increasing the pressure to 750mbar, and stopping the furnace and discharging ingots when the temperature of TC2 is reduced to 450 ℃.
In the process, the pressure, the temperature, the time and the like are allowed to float up and down within the error range, and the influence on the product is avoided. As can be understood by those skilled in the art, the space in the ingot furnace is large and the temperature is not completely uniform, the TC1 temperature is the temperature measured by the detection-temperature control thermocouple, and when the temperature measured by the detection-temperature control thermocouple reaches the required value, the control enters the next procedure; the TC2 temperature is the temperature measured by another probe thermocouple, and is used for detecting whether the temperature index meets the requirements of blowing out and discharging ingots.
The method for producing a nitrogen-doped P-type silicon master alloy using a polycrystalline ingot furnace according to the present invention will be described below with a specific example, and the nitrogen-doped P-type silicon master alloy will be referred to as a target master alloy for the sake of simplicity of description.
870kg of P-type silicon material with the resistivity of 1.4 omega cm and the purity of 99.9999 percent is selected to produce the target master alloy, the resistivity of the target master alloy ingot at a position 10mm away from the bottom is required to be 0.0024 omega cm, and the required amount of boron nitride can be calculated to be 161.53g according to the formula 1, 2, 3 and 4. The specific calculation method is as follows:
from equation 1, N can be calculated0＝1.01365×1016atom/cm3，
From equation 4, N can be calculated2＝4.60958×1019atom/cm3；
From equation 3, N can be calculated1＝5.658×1019atom/cm3；
According to equation 2, m is 161.53 g.
161.53g of boron nitride and 870kg of silicon material are weighed and fed into a furnace, and a polycrystalline ingot casting method is used, and comprises the following specific steps:
a) vacuumizing: vacuumizing to below 0.05mbar, and starting to operate the ingot furnace;
b) heating: setting heating power, gradually increasing the heating power from 0 to 80%, operating for 8-10 h, continuously introducing argon gas in the process, gradually increasing the pressure to 600mbar, and entering a melting stage when the temperature of TC1 reaches 1500 ℃;
c) melting: the process is operated for 8 to 10 hours, the temperature of TC1 is kept at 1530 to 1550 ℃, and the pressure is kept at 600 mbar;
d) crystal growth: in the crystal growth stage, the heat insulation cage is opened to release heat, the process is operated for 28 to 32 hours, the temperature of TC1 is kept at 1400 to 1430 ℃, and the pressure is kept at 600 mbar;
e) annealing: in the annealing stage, closing the heat insulation cage, reducing the temperature of TC1 to the annealing temperature, keeping the pressure at 600mbar, and operating the process for 2-3 h;
f) (ii) a And (3) cooling: and (3) entering a cooling stage, gradually opening the heat insulation cage to the maximum height, gradually increasing the argon gas inflow, increasing the pressure to 750mbar, and stopping the furnace and discharging ingots when the temperature of TC2 is reduced to 450 ℃.
The nitrogen-doped P-type silicon master alloy obtained by any one of the methods can replace the traditional master alloy to prepare a polycrystalline silicon ingot.
Specifically, after the target master alloy ingot is taken out of the furnace, the target master alloy ingot is cut into silicon blocks with the thickness of 20mm, and the silicon blocks are graded according to the required resistivity and put into corresponding polycrystalline silicon materials to produce the nitrogen-doped polycrystalline silicon ingot.
The process for preparing the nitrogen-doped polycrystalline silicon ingot by using the nitrogen-doped P-type silicon master alloy of the invention is that the traditional master alloy is replaced by the nitrogen-doped P-type silicon master alloy, and other processes adopt the prior art, so that the process is not repeated. The nitrogen-doped polycrystalline silicon ingot obtained by the method has high mechanical strength, and can effectively reduce the fragment rate in the processes of slicing and the like.
In conclusion, after the boron nitride and the silicon material are mixed, a polycrystalline ingot casting method is adopted, nitrogen elements are introduced into the mother alloy while the mother alloy with the required resistivity is obtained, and further, when the polycrystalline silicon ingot is produced, the nitrogen elements are introduced into the mother alloy, so that the mechanical strength of the polycrystalline silicon ingot can be increased, the fragment rate in slicing and other processes is effectively reduced, and the cost is greatly reduced. In addition, the method uses a polycrystalline ingot furnace to produce the nitrogen-doped P-type silicon master alloy, so that the yield of the master alloy can be increased, and the production cost can be reduced.
It should be understood that although the present description refers to embodiments, not every embodiment contains only a single technical solution, and such description is for clarity only, and those skilled in the art should make the description as a whole, and the technical solutions in the embodiments can also be combined appropriately to form other embodiments understood by those skilled in the art.
The above list of details is only for the concrete description of the feasible embodiments of the present application, they are not intended to limit the scope of the present application, and all equivalent embodiments or modifications that do not depart from the technical spirit of the present application are intended to be included within the scope of the present application.
Claims (8)
1. A preparation method of a nitrogen-doped P-type silicon master alloy is characterized by comprising the following steps:
feeding, namely feeding a silicon material and boron nitride into an ingot furnace;
polycrystalline ingot casting, wherein a nitrogen-doped P-type silicon master alloy ingot is produced in an ingot furnace through the steps of vacuumizing, heating, melting, crystal growing, annealing and cooling in sequence;
before feeding, calculating the amount of boron nitride required to be added according to the concentration of boron element in a preformed nitrogen-doped P-type silicon master alloy ingot and the concentration of boron element contained in the silicon material, wherein the calculation method comprises the following steps:
calculating the concentration of boron element in the silicon material according to formula 1,
equation 1:
N0is the concentration of boron element in the silicon material, rho1Is the resistivity of the silicon material;
calculating the concentration of boron element in the silicon material and the boron nitride in the preformed N-doped P-type silicon master alloy crystal ingot according to the formula 2,
equation 2:
N1the concentration of boron elements in the silicon material and the boron nitride in a preformed nitrogen-doped P-type silicon master alloy crystal ingot, wherein M is the dosage of the silicon material, and M is the dosage of the boron nitride;
calculating the segregation concentrations of boron elements in the silicon material and the boron nitride at different heights in the silicon melt according to a formula 3,
equation 3:
N2the segregation concentration of boron element in the silicon material and the boron nitride at different heights in the silicon melt is shown in the specification, f is the segregation fraction, and k is boronSegregation coefficient of element in silicon;
the resistivities of different heights in the preformed nitrogen-doped P-type silicon master alloy ingot were calculated according to equation 4,
equation 4:
ρ is the resistivity at different heights in the pre-formed nitrogen-doped P-type silicon master alloy ingot.
2. The method for preparing the nitrogen-doped P-type silicon master alloy according to claim 1, wherein the method comprises the following steps: the sum of the amount of boron element contained in the silicon material and the amount of boron element in the boron nitride is consistent with the amount of boron element in the preformed nitrogen-doped P-type silicon master alloy.
3. The method for preparing the nitrogen-doped P-type silicon master alloy according to claim 2, wherein the method comprises the following steps: the concentration of the boron element in the silicon material is lower than that of the boron element in the preformed nitrogen-doped P-type silicon master alloy.
4. The method for preparing the nitrogen-doped P-type silicon master alloy according to claim 3, wherein the method comprises the following steps: the silicon material is a P-type silicon material, the resistivity is more than 1 omega cm, and the purity is more than 99.9999%.
5. The method for preparing the nitrogen-doped P-type silicon master alloy according to claim 1, wherein the method comprises the following steps: the polycrystalline ingot casting step specifically comprises:
the vacuumizing specifically comprises: vacuumizing to 0.05mbar and below, and starting to operate the ingot furnace;
and/or, the heating specifically comprises: setting heating power, gradually increasing the heating power from 0 to 80%, operating for 8-10 h, continuously introducing argon gas in the process, and gradually increasing the pressure to 600 mbar; when the temperature of TC1 reaches 1500 ℃, entering a melting stage;
and/or, the melting specifically comprises: the process is operated for 8-10 h, the temperature of TC1 is kept between 1530 ℃ and 1550 ℃, and the pressure is kept at 600 mbar;
and/or, the crystal growth specifically comprises: in a crystal growth stage, opening a heat insulation cage to release heat, operating for 28-32 h, keeping the temperature of TC1 at 1400-1430 ℃ and keeping the pressure at 600 mbar;
and/or, the annealing specifically comprises: in the annealing stage, closing the heat insulation cage, reducing the temperature of TC1 to the annealing temperature, keeping the pressure at 600mbar, and operating the process for 2-3 h;
and/or, the cooling specifically comprises: and (3) entering a cooling stage, gradually opening the heat insulation cage to the maximum height, gradually increasing the argon gas inflow, increasing the pressure to 750mbar, and stopping the furnace and discharging ingots when the temperature of TC2 is reduced to 450 ℃.
6. A nitrogen-doped P-type silicon master alloy is characterized in that: prepared by any one of claims 1 to 5.
7. A preparation method of a nitrogen-doped polycrystalline silicon ingot, which is characterized by comprising the preparation method of the nitrogen-doped P-type silicon master alloy as claimed in any one of claims 1 to 5.
8. A nitrogen-doped polycrystalline silicon ingot is characterized in that: prepared by the method of claim 7.
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