CN114672874A - Novel seeding method for improving small-angle crystal boundary defects - Google Patents
Novel seeding method for improving small-angle crystal boundary defects Download PDFInfo
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- CN114672874A CN114672874A CN202210538760.2A CN202210538760A CN114672874A CN 114672874 A CN114672874 A CN 114672874A CN 202210538760 A CN202210538760 A CN 202210538760A CN 114672874 A CN114672874 A CN 114672874A
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- 239000013078 crystal Substances 0.000 title claims abstract description 92
- 238000000034 method Methods 0.000 title claims abstract description 84
- 238000010899 nucleation Methods 0.000 title claims abstract description 68
- 230000007547 defect Effects 0.000 title claims abstract description 51
- 230000008569 process Effects 0.000 claims abstract description 50
- 238000004781 supercooling Methods 0.000 claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 230000001105 regulatory effect Effects 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 4
- 241000219122 Cucurbita Species 0.000 claims description 3
- 235000009852 Cucurbita pepo Nutrition 0.000 claims description 3
- 230000006911 nucleation Effects 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 3
- 238000011946 reduction process Methods 0.000 claims 5
- 230000035755 proliferation Effects 0.000 abstract description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052710 silicon Inorganic materials 0.000 abstract description 3
- 239000010703 silicon Substances 0.000 abstract description 3
- 230000009471 action Effects 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 240000009087 Crescentia cujete Species 0.000 description 2
- 235000005983 Crescentia cujete Nutrition 0.000 description 2
- 235000009797 Lagenaria vulgaris Nutrition 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011112 process operation Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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- 230000000877 morphologic effect Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000000644 propagated effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/10—Crucibles or containers for supporting the melt
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
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Abstract
The invention relates to the technical field of small-angle grain boundaries, in particular to a novel seeding method for improving the defects of the small-angle grain boundaries. The novel crystal seeding method for improving the small-angle crystal boundary defects has the advantages that in the process of manufacturing the heavily boron-doped crystal orientation silicon single crystal by using a CZ (CZ) method, the small-angle crystal boundary defects become an industrial problem due to the influence of doping concentration and the limitation of a drawing process, the crystal seeding method is improved on the basis of reducing supercooling degree, the crystal pulling process is solidified, the small-angle crystal boundary defect obstacle is broken through, the internal defects of seed crystals are effectively eliminated by adopting a cucurbit crystal seeding mode, the ordered arrangement of atoms in the crystal manufacturing process is guaranteed, the pulling speed needs to be stable and slow in the whole manufacturing process, and the overturning dislocation proliferation of a solid-liquid interface can be influenced by frequent fluctuation, so that the small-angle crystal boundary is generated.
Description
Technical Field
The invention relates to the technical field of small-angle grain boundaries, in particular to a novel seeding method for improving the defects of the small-angle grain boundaries.
Background
In the production and manufacturing process of the heavily boron-doped drawn crystal-oriented monocrystalline silicon, the small-angle crystal boundary is a frequently-occurring crystal defect, the product quality is greatly influenced, and the production process needs to be avoided to the utmost extent. The influence of doping concentration on the small-angle grain boundary is researched through experiments, the drawing is carried out according to the prior art, the comprehensive data analysis is carried out, the macroscopic distribution and the morphological characteristics of the small-angle grain boundary are realized, the arrangement of atoms at the grain boundary is irregular, more defects exist, the atom diffusion speed is high, the small-angle grain boundary is easily generated when the doping concentration is close to the solid solubility, the small-angle grain boundary is regularly changed along with the change of the doping concentration, the small-angle grain boundary is gradually enlarged along with the increase of the doping concentration, the generation of the small-angle grain boundary under the high doping concentration is found to be inevitable by combining the crystal growth process and the crystal lattice compensation principle, the heavy boron doping is used for drawing the crystal orientation monocrystalline silicon at the present stage, the serious small-angle grain boundary defect is generated, and the influence on the product quality is intensified.
The method is characterized in that the reason for generating the small-angle crystal boundary is combed and deeply analyzed in the early crystal pulling process, the generation of the defect of the small-angle crystal boundary is reduced by reducing the supercooling degree in the production process, and five process methods of increasing the power of a heater, reducing the supercooling degree, increasing the caliber of a heat shield, reducing the supercooling degree, canceling the heat shield felt, reducing the supercooling degree, reducing the thermal field gradient and the heat preservation performance consistency, reducing the supercooling degree, reducing the crucible position, reducing the supercooling degree and the like are adopted, so that the growth of the heavy boron-doped crystal orientation single crystal without the small-angle crystal boundary cannot be successfully realized.
Experiments show that the low crucible position has certain advantages for growing the heavily doped boron single crystal without the small-angle crystal boundary by combining the crystal growth condition in the production process and data contrast analysis, but the defect of the small-angle crystal boundary cannot be completely avoided.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a novel seeding method for improving the defect of the small-angle crystal boundary, which has the advantages of improving the defect of the small-angle crystal boundary, ensuring the orderly arrangement of atoms in the crystal manufacturing process and the like, and solves the problems.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: the utility model provides a novel seeding method for improving small angle grain boundary defect, has cubic undergauge process including whole seeding process, is discontinuous undergauge process, the calabash form node is put in the regulation and control of undergauge process pull speed for the first time, reaches undergauge target diameter through the undergauge process for the second time, and the calabash crystal node of second time is realized in the regulation and control of pull speed, through third undergauge to target diameter, then carries out next process operation, gets rid of the dislocation through artificial many times in this process, makes grain boundary department atom ordered arrangement, reduces the defect in the very big degree and produces
Preferably, the process from the seeding start to the seeding target diameter is a discontinuous diameter reducing process, and at least comprises a first diameter reducing process, an equal fine grain process and a second diameter reducing process in sequence, wherein the seeding temperature is regulated and controlled in the equal fine grain process, the length of the first diameter reducing process is 60-80mm, the diameter of the necking is 4-7mm, the length of the second diameter reducing process is 15-30mm, the diameter of the necking is 4-7mm, the first section and the second section between the first section and the second section are respectively phi 9-15mm and the second section is phi 10-16mm, the diameter of the equal fine grain process is 4-7mm, and the length is more than 60 mm.
Preferably, in the seeding temperature regulation period, if the seeding speed deviation is positive, the seeding temperature is finely adjusted in a positive direction, and if the seeding speed deviation is negative, the seeding temperature is finely adjusted in a negative direction.
Preferably, the original crystal seeding mode is changed on the basis of reducing the supercooling degree, the crystal seeding is started to enable the shape of the crystal seeding to be in a gourd shape, the crystal seeding shape is regulated and controlled by the crystal seeding speed deviation, and the crystal seeding speed deviation is regulated and controlled in the crystal seeding period.
Preferably, on the premise of ensuring the thermal field heat preservation consistency, the crucible is pulled at a low position, the shouldering shape is a tower shoulder, the shouldering time is increased, the supercooling degree of a solid-liquid interface is reduced, atoms are difficult to diffuse in a relatively low-temperature state along with the reduction of the supercooling degree, the defect nucleation rate is reduced, and the defect proportion of small-angle crystal boundary is reduced.
Preferably, the seeding mode adopts cucurbit crystal, so that internal defects of seed crystals can be effectively eliminated, ordered arrangement of atoms in the crystal preparation process is guaranteed, the pulling speed needs to be stable and slow in the whole preparation process, and the overturning dislocation proliferation of a solid-liquid interface can be influenced by frequent fluctuation, so that a small-angle crystal boundary is generated.
(III) advantageous effects
Compared with the prior art, the invention provides a novel seeding method for improving the defect of a small-angle grain boundary, which has the following beneficial effects:
the novel crystal seeding method for improving the small-angle crystal boundary defects has the advantages that in the process of manufacturing the heavily boron-doped crystal orientation silicon single crystal by using a CZ (CZ) method, the small-angle crystal boundary defects become an industrial problem due to the influence of doping concentration and the limitation of a drawing process, the crystal seeding method is improved on the basis of reducing supercooling degree, the crystal pulling process is solidified, the small-angle crystal boundary defect obstacle is broken through, the crystal pulling process is led by the industry when the defects are solved, the internal defects of seed crystals are effectively eliminated by adopting a crystal seeding mode, the ordered arrangement of atoms in the crystal manufacturing process is guaranteed, the pulling speed needs to be stable and slow in the whole manufacturing process, and the overturning dislocation proliferation of a solid-liquid interface can be influenced by frequent fluctuation, so that the small-angle crystal boundary is generated.
Drawings
FIG. 1 is a schematic structural diagram of a novel seeding method for improving small-angle grain boundary defects according to 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.
Referring to fig. 1, a novel seeding method for improving small-angle grain boundary defects comprises a three-time diameter reducing process in the whole seeding process, wherein the three-time diameter reducing process is a discontinuous diameter reducing process, calabash-shaped nodules are released by the first diameter reducing process through pulling speed regulation, the diameter reducing target diameter is reached through the second diameter reducing process, the second calabash-shaped nodules are realized through pulling speed regulation, the third diameter reducing is carried out to the target diameter, then the next process operation is carried out, and dislocation is eliminated manually for multiple times in the process, so that atoms at the grain boundary are arranged in order, and the defects are reduced to the maximum extent;
the adopted technical scheme is that an original crystal introduction mode is changed on the basis of reducing supercooling degree, crystal introduction is started to enable the shape of the crystal introduction to be in a gourd shape, dislocation is manually eliminated for multiple times, atoms at a crystal boundary are orderly arranged, the generation of defects is greatly reduced, dislocation defects are not thoroughly eliminated in the original crystal introduction process, and dislocation defects are propagated and evolved into small-angle crystal boundaries by turning over a shoulder-placed and shoulder-rotated solid-liquid interface;
according to the technical scheme for reducing the supercooling degree, the supercooling degree is reduced through earlier demonstration, on the premise that the heat field heat preservation consistency is guaranteed, the crystal is pulled at the low crucible position, the shouldering shape is a tower shoulder, the shouldering time is prolonged, the supercooling degree of a solid-liquid interface is reduced, atoms are difficult to diffuse in a relatively low-temperature state along with the reduction of the supercooling degree, the defect nucleation rate is reduced, and the defect proportion of small-angle crystal boundaries is reduced.
The seeding mode adopts the cucurbit crystal, so that the defects in the seed crystal are effectively eliminated, the ordered arrangement of atoms in the crystal manufacturing process is ensured, the pulling speed needs to be stable and slow in the whole manufacturing process, and the overturning dislocation proliferation of a solid-liquid interface is also influenced by frequent fluctuation, so that a small-angle crystal boundary is generated.
The electrical components in the document are electrically connected with an external master controller and 220V mains supply, and the master controller can be a computer or other conventional known devices for playing a role in control.
In summary, the novel seeding method for improving the small-angle crystal boundary defects has the advantages that the small-angle crystal boundary defects become an industrial problem due to the influence of doping concentration and drawing process limitation in the process of using CZ (Czochralski) to draw heavily boron-doped crystal orientation silicon single crystals, the seeding method is improved on the basis of reducing supercooling degrees, the crystal pulling process is solidified, the small-angle crystal boundary defect obstacle is broken through, the crystal pulling process is advanced in industry when solving the defects, the internal defects of seed crystals are effectively eliminated by adopting cucurbit crystals in the seeding mode, the ordered arrangement of atoms in the crystal manufacturing process is guaranteed, the pulling speed is required to be stable and slow in the whole manufacturing process, and the overturning dislocation proliferation of a solid-liquid interface can be influenced by frequent fluctuation to further generate the small-angle crystal boundary.
It should be noted that, in this document, relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. The utility model provides a improve novel seeding method of small angle grain boundary defect, has cubic undergauge process including whole seeding process, is discontinuous undergauge process, its characterized in that: the calabash-shaped nodules are placed in the first diameter reducing process through pulling speed regulation, the diameter reducing target diameter is achieved through the second diameter reducing process, the calabash-shaped nodules are achieved through pulling speed regulation, the second calabash-shaped nodules are reduced to the target diameter through the third diameter reducing, then the next procedure operation is carried out, dislocation is eliminated through manual multiple times in the process, atoms at the crystal boundary are orderly arranged, and defects are reduced to the maximum degree.
2. The novel seeding method for improving the defects of the small-angle grain boundaries as claimed in claim 1, wherein the seeding method comprises the following steps: the process from the start of seeding to the achievement of the seeding target diameter is a discontinuous diameter reduction process and at least comprises a first diameter reduction process, a fine crystal waiting process and a second diameter reduction process in sequence, wherein the seeding temperature is regulated and controlled in the fine crystal waiting process, the length of the first diameter reduction process is 60-80mm, the diameter of a necking neck is 4-7mm, the length of the second diameter reduction process is 15-30mm, the diameter of the necking is 4-7mm, the first section and the second section between the first section and the second section are respectively phi 9-15mm and the second section is phi 10-16mm, the diameter of the fine crystal waiting process is phi 4-7mm, and the length is more than 60 mm.
3. The novel seeding method for improving the defects of the small-angle grain boundaries as claimed in claim 1, wherein the seeding method comprises the following steps: and in the seeding temperature regulation period, if the seeding speed deviation is positive, the seeding temperature is finely regulated in a positive direction, and if the seeding speed deviation is negative, the seeding temperature is finely regulated in a negative direction.
4. The novel seeding method for improving the defects of the small-angle grain boundaries as claimed in claim 1, wherein the seeding method comprises the following steps: the original crystal seeding mode is changed on the basis of reducing the supercooling degree, the seeding is started to enable the shape of the crystal to be in a gourd shape, the seeding shape is regulated and controlled by the seeding speed deviation, and the seeding speed deviation is the regulation and control of the seeding speed in the seeding period.
5. The novel seeding method for improving the defects of the small-angle grain boundaries as claimed in claim 1, wherein the seeding method comprises the following steps: on the premise of ensuring the heat preservation consistency of the thermal field, the crucible is pulled at a low position, the shouldering shape is a tower shoulder, the shouldering time is increased, the supercooling degree of a solid-liquid interface is reduced, atoms are difficult to diffuse in a relatively low-temperature state along with the reduction of the supercooling degree, the defect nucleation rate is reduced, and the defect proportion of small-angle crystal boundary is reduced.
6. The novel seeding method for improving the defects of the small-angle grain boundaries as claimed in claim 1, wherein the seeding method comprises the following steps: the seeding mode adopts cucurbit crystal, so that internal defects of seed crystals can be effectively eliminated, the ordered arrangement of atoms in the crystal manufacturing process is guaranteed, the pulling speed needs to be stable and slow in the whole manufacturing process, and the overturning dislocation multiplication of a solid-liquid interface is also influenced by frequent fluctuation, so that small-angle crystal boundaries are generated.
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