CN115044975A - Method for preparing czochralski silicon - Google Patents
Method for preparing czochralski silicon Download PDFInfo
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- CN115044975A CN115044975A CN202210867428.0A CN202210867428A CN115044975A CN 115044975 A CN115044975 A CN 115044975A CN 202210867428 A CN202210867428 A CN 202210867428A CN 115044975 A CN115044975 A CN 115044975A
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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
- C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
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Abstract
The present disclosure provides a method of preparing a pulled monocrystalline silicon, comprising: adding a granular silicon material into a raw material container to form a granular layer in the raw material container; placing a low melting point feedstock in the middle of the particle layer; the melting point of the low-melting-point raw material is lower than room temperature; czochralski silicon is produced by the Czochralski method using at least the raw material in the raw material container. The embodiment of the disclosure can ensure the accuracy of the content of the low-melting-point raw material in the czochralski silicon product, and further improve the accuracy of the resistivity of the czochralski silicon product.
Description
Technical Field
The disclosure relates to the technical field of monocrystalline silicon preparation, in particular to a method for preparing czochralski monocrystalline silicon.
Background
The Czochralski (CZ) method is an important method for producing a single-crystal silicon product.
The resistivity of the czochralski silicon is one of the important properties, and the resistivity is closely related to the doping concentration, and the resistivity of the czochralski silicon is influenced by slight change of the doping concentration.
In the czochralski silicon prepared by the prior art, for some doping elements (such as gallium) with melting points crossing the bottom, the accuracy of the dosage is difficult to ensure, thereby causing the inaccurate resistivity of the czochralski silicon product.
Disclosure of Invention
The present disclosure provides a method of czochralski silicon preparation.
In a first aspect, embodiments of the present disclosure provide a method of czochralski silicon preparation, comprising:
adding a granular silicon material into a raw material container to form a granular layer in the raw material container;
placing a low melting point feedstock in the middle of the particle layer; the melting point of the low-melting-point raw material is lower than room temperature;
czochralski silicon is produced by the Czochralski method using at least the raw material in the raw material container.
In some embodiments, the low melting feedstock comprises gallium.
In some embodiments, prior to said adding particulate silicon material to the feedstock vessel, further comprising:
and adding a massive silicon material into the raw material container.
In some embodiments, the silicon feedstock particles have a particle size between 1mm and 70 mm.
In some embodiments, the silicon feedstock particles have a particle size between 3 millimeters and 30 millimeters.
In some embodiments, the feedstock container comprises a czochralski crucible;
the production of czochralski silicon by the czochralski method using at least the raw material in the raw material container comprises: melting the raw materials in the Czochralski crucible to form a silicon melt, and preparing Czochralski single crystal silicon by the Czochralski method using the silicon melt.
In some embodiments, the particle layer in the czochralski crucible has a thickness of 1mm or more.
In some embodiments, the feedstock vessel comprises a feed cartridge;
the production of czochralski silicon by the czochralski method using at least the raw material in the raw material container comprises: after the raw materials in the czochralski crucible are melted to form silicon liquid, the raw materials in the feeding cylinder are added into the silicon liquid, and the czochralski silicon is prepared by the czochralski method by using the silicon liquid.
In some embodiments, the thickness of the layer of particles in the cartridge is above 20 mm.
In some embodiments, the particle layer in the loading drum is spaced from the upper edge of the loading drum by a distance of between 10 cm and 15 cm.
In the embodiment of the disclosure, the granular silicon material (crushed material) is added firstly to be spread and padded to form the granular layer, and the low-melting-point raw material (such as gallium) is placed on the granular layer, so that the low-melting-point raw material does not contact with the wall surface of the raw material container, and the low-melting-point raw material is not stained on the raw material container and lost, but is completely melted into the silicon liquid, namely completely enters the czochralski silicon product, and the accuracy of the doping concentration (resistivity) of the czochralski silicon product can be further ensured.
Drawings
The accompanying drawings are included to provide a further understanding of the disclosure and are incorporated in and constitute a part of this specification, illustrate embodiments of the disclosure and together with the detailed description serve to explain the disclosure and not limit the disclosure. The above and other features and advantages will become more apparent to those skilled in the art by describing in detail embodiments with reference to the attached drawings in which:
FIG. 1 is a flow chart of a method of Czochralski single crystal silicon preparation provided by embodiments of the present disclosure;
FIG. 2 is a cross-sectional view of a raw material container state in a method of Czochralski silicon production provided by an embodiment of the present disclosure;
FIG. 3 is a flow chart of another method of Czochralski single crystal silicon production provided by embodiments of the present disclosure;
FIG. 4 is a cross-sectional view of a feed material container in another Czochralski silicon production method provided by embodiments of the disclosure.
Detailed Description
In order to better understand the technical scheme of the present disclosure, the method and the device, the electronic equipment and the computer readable medium of the method for preparing the czochralski silicon provided by the present disclosure are described in detail in the following with the attached drawings.
The present disclosure will be described more fully hereinafter with reference to the accompanying drawings, but the illustrated embodiments may be embodied in different forms and should not be construed as limited to the embodiments set forth in the disclosure. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
The present disclosure may be described with reference to plan and/or cross-sectional views by way of idealized schematic illustrations of the present disclosure. Accordingly, the example illustrations can be modified in accordance with manufacturing techniques and/or tolerances.
Embodiments of the present disclosure and features of embodiments may be combined with each other without conflict.
The terminology used in the present disclosure is for the purpose of describing particular embodiments only and is not intended to be limiting of the disclosure. As used in this disclosure, the term "and/or" includes any and all combinations of one or more of the associated listed items. As used in this disclosure, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. The terms "comprises," "comprising," "made from … …," as used in this disclosure, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
Unless otherwise defined, all terms (including technical and scientific terms) used in this disclosure have the same meaning as commonly understood by one of ordinary skill in the art. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and the present disclosure, and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
The present disclosure is not limited to the embodiments shown in the drawings, but includes modifications of configurations formed based on a manufacturing process. Thus, the regions illustrated in the figures have schematic properties, and the shapes of the regions shown in the figures illustrate specific shapes of regions of elements, but are not intended to be limiting.
In a first aspect, embodiments of the present disclosure provide a method of czochralski silicon preparation.
The method of the embodiments of the present disclosure is used for producing single crystal silicon containing a doping element by the czochralski method (czochralski silicon).
Referring to fig. 1, a method of an embodiment of the present disclosure includes:
s101, adding a granular silicon material into a raw material container to form a granular layer in the raw material container.
Referring to fig. 2, in a raw material container of a czochralski silicon apparatus, a certain amount of granular silicon material (granular silicon material) is charged, thereby forming a "granular layer" of granular silicon material in the raw material container.
Wherein, the raw material container is a container for containing raw materials in the czochralski silicon equipment.
Wherein the granular silicon material is granular silicon material, or "crushed material" of silicon.
Wherein, the material of the granular silicon material can be pure silicon, also can be mother alloy (doped silicon), also can be silicon recycle material (such as leftover materials or waste materials like head and tail edges in the previously prepared Czochralski silicon); that is, any material having a granular shape and containing silicon as a main component may be referred to as a granular silicon material.
S102, placing the low-melting-point raw material in the middle of the particle layer.
Wherein the melting point of the low-melting-point raw material is lower than room temperature.
For a doping element that is required to be used in czochralski silicon, if its melting point is less than room temperature (e.g., 35 degrees celsius), it is referred to as a "low-melting point raw material".
Referring to fig. 2, it is necessary for the low-melting point raw material to be placed in the middle of the particle layer after the above particle layer is formed, thereby ensuring that the low-melting point raw material is in contact with only the particle layer (particulate silicon material) and not with the wall surfaces (including the bottom surface and the side surfaces) of the raw material container.
In some related art, since the low-melting-point raw material has a melting point lower than room temperature, it may be partially melted at room temperature before starting to heat and melt the raw material, and the melted low-melting-point raw material may be contaminated on the wall surface if contacting the wall surface of the raw material container, and the contaminated low-melting-point raw material may not be efficiently introduced into the silicon melt, that is, a part of the low-melting-point raw material may be lost without actually being introduced into the czochralski-silicon product, thereby causing inaccuracy in the doping concentration and inaccuracy in the resistivity of the czochralski-silicon product.
It should be understood that in the czochralski single crystal of the embodiment of the present disclosure, only the above low-melting point raw material may be contained as a doping element; in addition to the above low melting point raw material, other doping elements may be simultaneously contained, and specific usable doping elements include, but are not limited to, boron (B), phosphorus (P), aluminum (Al), zinc (Zn), selenium (Se), and the like.
Accordingly, other doping elements are also required to be added as raw materials, and the addition form thereof may be various. For example, other doping elements may be added with the silicon material (e.g., in the form of a master alloy), or may be added separately; the other doping elements may be added in the form of pure elements, in the form of master alloys, or in the form of other compounds, which are not described in detail herein.
It should be understood that the disclosed embodiments define only the need to place the low melting point feedstock after the particle layer is laid down, but are not limiting as to whether additional feeding steps are present.
For example, other raw materials, such as bulk silicon, may also be added prior to the laying of the particulate layer; after the low melting point material is placed, other materials can be added continuously, for example, the low melting point material can be covered by the granular silicon material. For example, the above other doping elements may be added in a separate step, and the addition may be performed before or after the addition of the low melting point raw material, or simultaneously with the addition of the low melting point raw material.
It is to be understood that the specific addition amount of the low melting point raw material may be determined depending on the quality of the CZ single crystal silicon to be produced and the doping concentration (content) of the low melting point raw material therein.
For example, in czochralski silicon, the doping concentration of gallium as a low-melting-point feedstock can generally be 6 × 10 14 ～3*10 16 atoms/com 3 。
S103, preparing the czochralski silicon by a czochralski method by using at least raw materials in the raw material container.
After the raw materials are charged into the raw material container, the raw materials in the raw material container (although other sources of raw materials may be included) can be utilized to produce czochralski silicon by the czochralski method.
For example, the feedstock in a Czochralski crucible can be melted into silicon liquid, the silicon liquid can then be contacted with a seed crystal, and the seed crystal can then be pulled upwardly to gradually form the Czochralski single crystal silicon product.
Wherein, the whole Czochralski silicon product can be a bar, the height of the bar can be 500-9000 mm, and the diameter of the bar can be 50-350 mm.
It should be understood that, for the czochralski silicon product, the silicon wafer can be further cut into silicon wafers after the head and tail edges are removed, and the silicon wafers are used for the subsequent preparation of solar cells, semiconductor devices and the like, and are not described in detail herein.
In the embodiment of the disclosure, the granular silicon material (crushed material) is added firstly to be spread and padded to form the granular layer, and the low-melting-point raw material (such as gallium) is placed on the granular layer, so that the low-melting-point raw material does not contact with the wall surface of the raw material container, and the low-melting-point raw material is not stained on the raw material container and lost, but is completely melted into the silicon liquid, namely completely enters the czochralski silicon product, and further the accuracy of the doping concentration (resistivity) of the czochralski silicon product can be ensured.
In some embodiments, the low melting feedstock comprises gallium.
As one mode of the embodiment of the present disclosure, the low melting point material may be gallium (Ga), which has a melting point of 29.8 degrees celsius and is a doping element (P-type doping element) commonly used in single crystal silicon, and thus may be used as an example of the low melting point material.
It should be understood that the particular form of the low melting feedstock is not limited to gallium.
For example, the low melting point material may also be some other element, or may be an alloy or combination of different elements; as long as the raw material is a raw material for pulling the silicon single crystal and the melting point of the whole is lower than room temperature, the raw material can be added as a low melting point raw material in the manner of the embodiment of the present disclosure.
In some embodiments, referring to fig. 3, prior to adding the particulate silicon material to the feedstock vessel (S101), further comprising:
and S100, adding a massive silicon material into the raw material container.
As a mode of the embodiment of the present disclosure, referring to fig. 3, before the particulate silicon material is added to form the particulate layer, a large block of raw material (bulk silicon material) may be added to the raw material container; thus, referring to FIG. 4, a granular layer is formed above these bulk materials, and the low melting point material (shown in bold lines) is again located above the granular layer.
However, the reason why the low-melting-point raw material is not directly provided on the bulk silicon material is that the gap between the bulk silicon material and the low-melting-point raw material is relatively large because of the large size of the bulk silicon material, and if the low-melting-point raw material is directly placed thereon, the low-melting-point raw material is likely to fall from the gap and still contact the wall surface of the raw material container.
Wherein, the grain diameter of the block silicon material can be between 80mm and 400mm, and can be different according to different raw material containers. For example, the bulk silicon material used in the Czochralski crucible can be relatively large, e.g., about 300mm in diameter, and the bulk silicon material used in the feed cylinder can be relatively small, e.g., about 90mm in diameter.
Like the above granular silicon material, the material of the bulk silicon material may be pure silicon, or a master alloy, or a recycled material of silicon.
In some embodiments, the silicon feedstock particles have a particle size between 1 millimeter and 70 millimeters.
In some embodiments, the silicon feedstock particles have a particle size between 3 millimeters and 30 millimeters.
If the particle size of the silicon material particles is too small, the silicon material particles are closer to powder and are easy to lose, can not effectively bear low-melting-point raw materials, and can easily fall into gaps of the massive silicon material; on the other hand, if the particle diameter of the silicon material particles is too large, the particles are close to the above bulk silicon material, and the gaps between the particles are too large, which easily causes the low melting point raw material to fall off.
Therefore, as an aspect of the embodiment of the present disclosure, silicon material having a particle diameter of 1 to 70mm may be used as the silicon material particles, and the particle diameter of the silicon material particles may further be 3 to 30mm, for example, 3mm, 5mm, 10mm, 20mm, 30 mm.
In some embodiments, the feedstock container comprises a czochralski crucible; the production of Czochralski silicon by the Czochralski method using at least raw materials in a raw material container (S103) includes:
and S1031, melting the raw materials in the Czochralski crucible to form silicon liquid, and preparing the Czochralski silicon by the Czochralski method by using the silicon liquid.
As a way of an embodiment of the present disclosure, the above raw material container may be a Czochralski crucible, that is, at least a part of the low melting point raw material may be added to the Czochralski crucible.
The czochralski crucible can be made of quartz, graphite and other materials, and is a container for holding and drawing main raw materials, namely, silicon liquid is generated after the raw materials in the czochralski crucible are melted, and czochralski silicon can be obtained by drawing from the silicon liquid.
For example, referring to fig. 2, in the czochralski crucible, the particle layer may be formed by directly laying silicon material particles on the bottom of the czochralski crucible.
In some embodiments, the particle layer in the czochralski crucible has a thickness of greater than 1 millimeter.
As a mode of the embodiment of the present disclosure, in the czochralski crucible, the above particle layer should have a thickness of at least 1mm, for example, 5mm, 10mm, 30mm, including the case where all the silicon material is a granular silicon material.
In some embodiments, the feedstock container comprises a feed cartridge; the production of Czochralski silicon by the Czochralski method using at least raw materials in a raw material container (S103) includes:
s1032, after the raw materials in the Czochralski crucible are melted to form silicon liquid, the raw materials in the feeding cylinder are added into the silicon liquid, and the Czochralski silicon is prepared from the silicon liquid by a Czochralski method.
As another way of the embodiments of the present disclosure, the above raw material container may be a charging barrel (charger) for secondary charging, that is, at least part of the low melting point raw material may be charged into the charging barrel.
The charging barrel is used for secondary charging, namely, part of raw materials can be loaded in the czochralski crucible, and the other part of raw materials can be loaded in the charging barrel; when the raw materials in the czochralski crucible are melted into silicon liquid, the liquid level of the silicon liquid is reduced compared with the original surface of the solid raw materials due to the disappearance of gaps among the solid raw materials, so that a vacant space appears in the czochralski crucible; therefore, the raw material in the charging barrel can be added (for example, the bottom of the charging barrel is opened and added) into the silicon liquid of the Czochralski crucible to be melted together, and then the whole silicon liquid is used for pulling the Czochralski silicon.
For example, referring to fig. 4, in the charging barrel, the above bulk silicon material may be charged first, and then the particle layer is formed and the low melting point raw material is placed.
In some embodiments, the thickness of the layer of particles in the cartridge is above 20 millimeters.
As a way of the disclosed embodiment, in the charging cylinder, the thickness of the above particle layer should be at least 20mm, for example 30mm, 50mm, 100mm, including the case where all the silicon material is a granular silicon material.
In some embodiments, the particle layer in the loading cylinder is spaced from the upper edge of the loading cylinder by a distance of between 10 cm and 15 cm.
Referring to fig. 4, as a mode of the embodiment of the present disclosure, in the charging barrel, a distance between an upper surface of the above-formed particle layer (i.e., a position where the low melting point raw material is placed) and an upper edge of the charging barrel may be 10 to 15 cm. Typically, the height of the cartridge is relatively large (e.g. may be around 200 cm), i.e. the above particulate layer and low melting point feedstock may be located relatively close to the upper end of the cartridge.
It is to be understood that the low melting point raw material may be added entirely to the Czochralski crucible (including no secondary addition, or a secondary addition but excluding the low melting point raw material), entirely to the addition cartridge, or partly to the Czochralski crucible and partly to the addition cartridge, without limitation.
It should be understood that the low melting point source material may also be added to the source material container in the above manner if there are other forms of source material containers for holding the source material, i.e., the specific form of the source material container in the embodiments of the present disclosure is not limited to a czochralski crucible and a charging barrel.
In the disclosed embodiment, in order to better control the doping concentration (resistivity) of the low-melting point element in the czochralski silicon product, the melting of the low-melting point raw material is prevented as much as possible in other steps.
For example, the storage site for low melting point feedstock (e.g., gallium) should not be at a temperature greater than 20 degrees celsius to ensure that gallium is completely solid during storage for easy weighing.
After leaving the storage site, gallium is added to the raw material container (czochralski crucible or charging barrel) within 15 minutes to avoid loss of gallium due to melting before it is added; at the same time, before the gallium is added to the raw material container, it should be checked whether it has melted, ensuring that there is no loss of the amount of material added to the raw material container.
The present disclosure has disclosed example embodiments and, although specific terms are employed, they are used and should be interpreted in a generic and descriptive sense only and not for purposes of limitation. In some instances, features, characteristics and/or materials described in connection with a particular embodiment may be used alone or in combination with features, characteristics and/or elements described in connection with other embodiments, unless expressly stated otherwise, as would be apparent to one skilled in the art. It will, therefore, be understood by those skilled in the art that various changes in form and details may be made therein without departing from the scope of the disclosure as set forth in the appended claims.
Claims (10)
1. A method of Czochralski silicon production, comprising:
adding a granular silicon material into a raw material container to form a granular layer in the raw material container;
placing a low melting point feedstock in the middle of the particle layer; the melting point of the low-melting-point raw material is lower than room temperature;
czochralski silicon is produced by the Czochralski method using at least the raw material in the raw material container.
2. The method of claim 1, wherein,
the low melting feedstock comprises gallium.
3. The method of claim 1, wherein prior to said adding particulate silicon material to the feedstock vessel, further comprising:
and adding a massive silicon material into the raw material container.
4. The method of claim 1, wherein,
the particle size of the silicon material particles is between 1mm and 70 mm.
5. The method of claim 1, wherein,
the particle size of the silicon material particles is between 3mm and 30 mm.
6. The method of claim 1, wherein,
the raw material container comprises a straight pull crucible;
the production of czochralski silicon by the czochralski method using at least the raw material in the raw material container comprises: melting the raw materials in the Czochralski crucible to form a silicon liquid, and preparing the Czochralski silicon by the Czochralski method by using the silicon liquid.
7. The method of claim 6, wherein,
the thickness of the particle layer in the czochralski crucible is more than 1 mm.
8. The method of claim 1, wherein,
the raw material container comprises a feeding cylinder;
the production of czochralski silicon by the czochralski method using at least the raw material in the raw material container comprises: after the raw materials in the czochralski crucible are melted to form silicon liquid, the raw materials in the feeding cylinder are added into the silicon liquid, and the czochralski silicon is prepared by the czochralski method by using the silicon liquid.
9. The method of claim 8, wherein,
the thickness of the particle layer in the charging barrel is more than 20 mm.
10. The method of claim 8, wherein,
the distance between the particle layer in the feed cylinder and the upper edge of the feed cylinder is between 10 and 15 centimeters.
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| CN103249875A (en) * | 2010-09-03 | 2013-08-14 | Gt高级锆石有限责任公司 | Silicon single crystal doped with gallium, indium, or aluminum |
| CN102409395A (en) * | 2011-11-15 | 2012-04-11 | 浙江长兴众成电子有限公司 | Gallium element doping device and method for Czochralski silicon |
| CN104846437A (en) * | 2015-06-02 | 2015-08-19 | 江苏协鑫硅材料科技发展有限公司 | Gallium-doped crystalline silicon with uniformly distributed resistivity and preparation method thereof |
| CN105821474A (en) * | 2016-04-13 | 2016-08-03 | 江西赛维Ldk太阳能高科技有限公司 | Preparation method of crystalline silicon and crystalline silicon |
| CN112160020A (en) * | 2020-09-29 | 2021-01-01 | 晶科能源有限公司 | Dopant feeder, preparation system and method for doped semiconductor material |
| CN113122919A (en) * | 2021-04-16 | 2021-07-16 | 上海新昇半导体科技有限公司 | Secondary feeding method and device, and monocrystalline silicon growth method and device |
| CN114059152A (en) * | 2021-11-19 | 2022-02-18 | 包头美科硅能源有限公司 | Gallium element doping method for producing silicon single crystal rod by Czochralski method |
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