CN113774474A - Preparation method for improving single crystal RRV - Google Patents
Preparation method for improving single crystal RRV Download PDFInfo
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- CN113774474A CN113774474A CN202111090014.3A CN202111090014A CN113774474A CN 113774474 A CN113774474 A CN 113774474A CN 202111090014 A CN202111090014 A CN 202111090014A CN 113774474 A CN113774474 A CN 113774474A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
- C30B15/04—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt adding doping materials, e.g. for n-p-junction
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
- C30B35/007—Apparatus for preparing, pre-treating the source material to be used for crystal growth
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- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a preparation method for improving single crystal RRV, which comprises the steps of selecting an industrial polycrystalline silicon raw material containing elements which are the same as or similar to those contained in a target master alloy, carrying out acid washing for 30 seconds, passing pure water, carrying out ultrasonic treatment, carrying out dust-free drying and packaging, matching according to the characteristics of the raw material and the target resistivity, calculating according to a doping formula, and carrying out mixed melting on the raw material, and then drawing by adopting a Czochralski method to obtain a uniform resistivity master alloy; according to the invention, the P-type master alloy with uniform resistivity is prepared by adopting boron-phosphorus co-doping, the target resistivity can be adjusted at any time according to the requirement, the resistivity uniformity is increased, and meanwhile, the stability of the output single crystal can be ensured by fixing the parameters.
Description
Technical Field
The invention relates to the technical field of equipment, in particular to a preparation method for improving single crystal RRV.
Background
The czochralski silicon is silicon single crystal which is pulled from silicon melt along the vertical direction and has certain size, crystal orientation, conductive type and resistivity range, raw materials are arranged in a crucible to be heated and melted, the end part of a thin single crystal (called seed crystal) cut into a specific crystal orientation is immersed in a melt to be slightly melted, then, the temperature is controlled, the seed crystal is slowly and vertically lifted, the pulled liquid is solidified into a single crystal, the required diameter of a single crystal rod can be obtained by adjusting the heating power, and the production process comprises six steps of feeding, melting, necking down growth, shouldering growth, equal-diameter growth and tail growth;
due to the growth characteristics of the czochralski silicon crystal, the comprehensive effects of impurity concentration boundary layer and impurity segregation and the like, the resistivity distribution on the slice is low at the center and high at the edge, namely the center doped impurity concentration is high and the edge doped impurity concentration is low, so the invention provides a preparation method for improving the single crystal RRV to solve the problems in the prior art.
Disclosure of Invention
In view of the above problems, the present invention is directed to a method for preparing an improved single crystal RRV, which is a method for preparing a P-type master alloy with uniform resistivity by co-doping boron and phosphorus, and can adjust the target resistivity at any time as required and increase the resistivity uniformity, and meanwhile, the parameters are fixed to ensure the stability of the produced single crystal.
In order to realize the purpose of the invention, the invention is realized by the following technical scheme: a preparation method for improving single crystal RRV comprises the following steps:
step one, raw material selection: selecting a raw material of industrial polycrystalline silicon containing the same or similar elements contained in the target master alloy, wherein the sum of the concentrations of metal elements in the selected raw material of industrial polycrystalline silicon is not higher than 1000 ppmw;
step two, raw material cleaning: cleaning an industrial polycrystalline silicon raw material with mixed acid for 30 seconds, then passing the industrial polycrystalline silicon raw material through pure water, sequentially performing ultrasonic treatment, drying and then performing dust-free packaging for later use;
step three, ingredient calculation: matching the washed silicon material according to the characteristics of the silicon material and the target resistivity, and calculating whether boron or phosphorus needs to be added according to a doping formula;
step four, preparing the uniform resistivity master alloy: the prepared raw materials are mixed and melted, and the mixture is drawn by a Czochralski method to obtain the master alloy with uniform resistivity.
The further improvement lies in that: the element which is the same as or similar to the element in the target master alloy in the step one is one of boron element and phosphorus element.
The further improvement lies in that: the mixed acid in the second step is one of a mixture of hydrofluoric acid, nitric acid and hydrochloric acid, when the mixed acid is the mixture of hydrofluoric acid and nitric acid, the mixed acid is mixed according to the mixing ratio of 1:5, is subjected to acid cleaning for 30 seconds, passes through pure water, is subjected to ultrasonic treatment for 120 seconds and is dried; when the mixed acid is a mixture of hydrofluoric acid and hydrochloric acid, mixing according to the mixing ratio of 2:3, carrying out acid cleaning for 30 seconds, passing through pure water, carrying out ultrasonic treatment for 140 seconds, and drying.
In a further improvement, the calculation formula when the dopant in the step three is boron is as follows:
where ρ is the resistivity in Ω · cm when the dopant is boron, and N is the dopant concentration in cm-3；
The calculation formula when the dopant is phosphorus is as follows:
where ρ is the resistivity in Ω · cm when the dopant is phosphorus, and N is the dopant concentration in cm-3。
The further improvement lies in that: and in the fourth step, crystal rotation and crucible rotation in the diameter process are adjusted before drawing, the crystal rotation is controlled to be 8-9 rotations, the crucible rotation is controlled to be 6-9 rotations, and other drawing parameters are fixed.
The further improvement lies in that: and in the fourth step, the pressure in the furnace is controlled at 750kPa during the drawing, and the temperature in the furnace is controlled at 600-900 ℃ by a heater.
The further improvement lies in that: and step four, after the drawing is finished, introducing argon into the furnace to cool the master alloy with uniform resistivity, wherein the flow rate of the argon is 55-70slm, and replacing gas in the furnace when the argon is introduced to ensure that the pressure in the furnace is kept floating within 750 +/-10 kPa.
The invention has the beneficial effects that: according to the invention, the P-type master alloy with uniform resistivity is prepared by adopting boron-phosphorus co-doping, the target resistivity can be adjusted at any time according to the requirement, the resistivity uniformity is increased, and meanwhile, the stability of the output single crystal can be ensured by fixing the parameters.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a flow chart of the preparation method of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1
According to fig. 1, the present embodiment provides a method for preparing an improved single crystal RRV, comprising the following steps:
step one, raw material selection: selecting a raw material of industrial polycrystalline silicon containing the same or similar elements as those contained in the target master alloy, wherein the total concentration of metal elements in the selected raw material of industrial polycrystalline silicon is not higher than 1000ppmw, and the element same as or similar to those in the target master alloy is boron element;
step two, raw material cleaning: cleaning an industrial polycrystalline silicon raw material for 30 seconds by using mixed acid, passing the industrial polycrystalline silicon raw material through pure water, sequentially performing ultrasonic treatment, drying, and then performing dust-free packaging for later use, wherein the mixed acid is a mixture of hydrofluoric acid and nitric acid and is mixed according to the mixing ratio of 1:5, and performing ultrasonic treatment for 120 seconds and drying;
step three, ingredient calculation: matching the washed silicon material according to the characteristics of the silicon material and the target resistivity, and calculating whether boron needs to be added according to a doping formula;
the formula for the dopant boron is:
where ρ is the resistivity in Ω · cm when the dopant is boron, and N is the dopant concentration in cm-3；
Step four, preparing the uniform resistivity master alloy: mixing the prepared raw materials, melting, drawing by adopting a Czochralski method to obtain a uniform resistivity master alloy, controlling the pressure in a furnace to be 750kPa during drawing, controlling the temperature in the furnace to be 600-900 ℃ by a heater, adjusting crystal rotation and crucible rotation in the process of equal diameter before drawing, controlling the crystal rotation to be 9 rotations, controlling the crucible rotation to be 6 rotations, fixing the rest drawing parameters, introducing argon into the furnace after drawing is finished to cool the uniform resistivity master alloy, wherein the flow of the argon is 55-70slm, replacing the gas in the furnace when the argon is introduced, and ensuring that the pressure in the furnace is kept floating within 750 +/-10 kPa.
Example 2
According to fig. 1, the present embodiment provides a method for preparing an improved single crystal RRV, comprising the following steps:
step one, raw material selection: selecting a raw material of industrial polycrystalline silicon containing the same or similar elements as those contained in the target master alloy, wherein the total concentration of metal elements in the selected raw material of industrial polycrystalline silicon is not higher than 1000ppmw, and the element which is the same as or similar to those in the target master alloy is phosphorus;
step two, raw material cleaning: cleaning an industrial polycrystalline silicon raw material for 30 seconds by using mixed acid, passing the industrial polycrystalline silicon raw material through pure water, sequentially performing ultrasonic treatment, drying, and then performing dust-free packaging for later use, wherein the mixed acid is a mixture of hydrofluoric acid and hydrochloric acid and is mixed according to the mixing ratio of 2:3, and performing ultrasonic treatment for 140 seconds and drying;
step three, ingredient calculation: matching the washed silicon material according to the characteristics of the silicon material and the target resistivity, and calculating whether phosphorus needs to be added according to a doping formula;
the formula for the dopant to be phosphorus is:
where ρ is the resistivity in Ω · cm when the dopant is boron, and N is the dopant concentration in cm-3；
Step four, preparing the uniform resistivity master alloy: mixing the prepared raw materials, melting, drawing by adopting a Czochralski method to obtain a uniform resistivity master alloy, controlling the pressure in a furnace to be 750kPa during drawing, controlling the temperature in the furnace to be 600-900 ℃ by a heater, adjusting crystal rotation and crucible rotation in the process of equal diameter before drawing, controlling the crystal rotation to be 9 rotations, controlling the crucible rotation to be 6 rotations, fixing the rest drawing parameters, introducing argon into the furnace after drawing is finished to cool the uniform resistivity master alloy, wherein the flow of the argon is 55-70slm, replacing the gas in the furnace when the argon is introduced, and ensuring that the pressure in the furnace is kept floating within 750 +/-10 kPa.
Example 3
According to fig. 1, the present embodiment provides a method for preparing an improved single crystal RRV, comprising the following steps:
step one, raw material selection: selecting a raw material of industrial polycrystalline silicon containing the same or similar elements as those contained in the target master alloy, wherein the total concentration of metal elements in the selected raw material of industrial polycrystalline silicon is not higher than 1000ppmw, and the element same as or similar to those in the target master alloy is boron element;
step two, raw material cleaning: cleaning an industrial polycrystalline silicon raw material for 30 seconds by using mixed acid, passing the industrial polycrystalline silicon raw material through pure water, sequentially performing ultrasonic treatment, drying, and then performing dust-free packaging for later use, wherein the mixed acid is a mixture of hydrofluoric acid and hydrochloric acid and is mixed according to the mixing ratio of 2:3, and performing ultrasonic treatment for 140 seconds and drying;
step three, ingredient calculation: matching the washed silicon material according to the characteristics of the silicon material and the target resistivity, and calculating whether boron needs to be added according to a doping formula;
the formula for the dopant boron is:
where ρ is the resistivity in Ω · cm when the dopant is boron, and N is the dopant concentration in cm-3；
Step four, preparing the uniform resistivity master alloy: mixing the prepared raw materials, melting, drawing by a Czochralski method to obtain a uniform resistivity master alloy, controlling the pressure in a furnace to be 750kPa during drawing, controlling the temperature in the furnace to be 600-900 ℃ by a heater, adjusting crystal rotation and crucible rotation in the process of equal diameter from 150mm before drawing, controlling the crystal rotation to be 8 rotations, controlling the crucible rotation to be 9 rotations, fixing the other drawing parameters, introducing argon into the furnace after drawing to cool the uniform resistivity master alloy, wherein the flow of the argon is 55-70slm, replacing gas in the furnace when introducing the argon, and ensuring that the pressure in the furnace floats within 750 +/-10 kPa.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. A preparation method for improving single crystal RRV is characterized by comprising the following steps:
step one, raw material selection: selecting a raw material of industrial polycrystalline silicon containing the same or similar elements contained in the target master alloy, wherein the sum of the concentrations of metal elements in the selected raw material of industrial polycrystalline silicon is not higher than 1000 ppmw;
step two, raw material cleaning: cleaning an industrial polycrystalline silicon raw material with mixed acid for 30 seconds, then passing the industrial polycrystalline silicon raw material through pure water, sequentially performing ultrasonic treatment, drying and then performing dust-free packaging for later use;
step three, ingredient calculation: matching the washed silicon material according to the characteristics of the silicon material and the target resistivity, and calculating whether boron or phosphorus needs to be added according to a doping formula;
step four, preparing the uniform resistivity master alloy: the prepared raw materials are mixed and melted, and the mixture is drawn by a Czochralski method to obtain the master alloy with uniform resistivity.
2. The method of claim 1, wherein the step of preparing the single crystal RRV further comprises: the element which is the same as or similar to the element in the target master alloy in the step one is one of boron element and phosphorus element.
3. The method of claim 1, wherein the step of preparing the single crystal RRV further comprises: the mixed acid in the second step is one of a mixture of hydrofluoric acid, nitric acid and hydrochloric acid, when the mixed acid is the mixture of hydrofluoric acid and nitric acid, the mixed acid is mixed according to the mixing ratio of 1:5, is subjected to acid cleaning for 30 seconds, passes through pure water, is subjected to ultrasonic treatment for 120 seconds and is dried; when the mixed acid is a mixture of hydrofluoric acid and hydrochloric acid, mixing according to the mixing ratio of 2:3, carrying out acid cleaning for 30 seconds, passing through pure water, carrying out ultrasonic treatment for 140 seconds, and drying.
4. The method of claim 1, wherein the formula for the dopant boron in step three is:
where ρ is the resistivity in Ω · cm when the dopant is boron, and N is the dopant concentration in cm-3；
The calculation formula when the dopant is phosphorus is as follows:
where ρ is the resistivity in Ω · cm when the dopant is phosphorus, and N is the dopant concentration in cm-3。
5. The method of claim 1, wherein the step of preparing the single crystal RRV further comprises: and in the fourth step, crystal rotation and crucible rotation in the diameter process are adjusted before drawing, the crystal rotation is controlled to be 8-9 rotations, the crucible rotation is controlled to be 6-9 rotations, and other drawing parameters are fixed.
6. The method of claim 1, wherein the step of preparing the single crystal RRV further comprises: and in the fourth step, the pressure in the furnace is controlled at 750kPa during the drawing, and the temperature in the furnace is controlled at 600-900 ℃ by a heater.
7. The method of claim 1, wherein the step of preparing the single crystal RRV further comprises: and step four, after the drawing is finished, introducing argon into the furnace to cool the master alloy with uniform resistivity, wherein the flow rate of the argon is 55-70slm, and replacing gas in the furnace when the argon is introduced to ensure that the pressure in the furnace is kept floating within 750 +/-10 kPa.
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| CN114808112A (en) * | 2022-03-31 | 2022-07-29 | 上海新昇半导体科技有限公司 | Single crystal growth method and wafer |
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| CN114808112B (en) * | 2022-03-31 | 2024-09-20 | 上海新昇半导体科技有限公司 | Single crystal growth method and wafer |
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