CN112553683B - Material melting method for crystal growth - Google Patents
Material melting method for crystal growth Download PDFInfo
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- CN112553683B CN112553683B CN202011209784.0A CN202011209784A CN112553683B CN 112553683 B CN112553683 B CN 112553683B CN 202011209784 A CN202011209784 A CN 202011209784A CN 112553683 B CN112553683 B CN 112553683B
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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
- C30B15/14—Heating of the melt or the crystallised materials
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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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- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
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- Metallurgy (AREA)
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a material melting method for crystal growth, which comprises the following steps: in the first heating stage, the heater heats the raw materials with first power and lasts for first heating time; a second heating stage in which the heater continues to heat the feedstock at a second power for a second heating time, wherein the second power is lower than the first power; and a third heating stage, wherein the heater continuously heats the raw materials at a third power for a third heating time. According to the material melting method for crystal growth provided by the invention, the material melting process is divided into three stages, and the heating power of the second stage is lower than that of the first stage, so that the total material melting time is shortened, the temperature of the quartz crucible is prevented from exceeding the softening temperature, and the yield of crystal growth is improved.
Description
Technical Field
The invention relates to the technical field of crystal growth, in particular to a material melting method for crystal growth.
Background
With the rapid development of the Integrated Circuit (IC) industry, device manufacturers have placed more stringent requirements on IC-grade silicon single crystal materials, which are the substrate materials necessary for device fabrication. The Czochralski method is the most important method for growing single crystal from melt in the prior art, and is characterized by that the raw materials for forming crystal are placed in a quartz crucible, heated and melted, then the crystal is pulled up by inoculating seed crystal on the surface of melt, under the controlled condition, the seed crystal and melt are continuously rearranged in atom or molecule on the interface, and then the crystal is gradually solidified with the cooling down so as to grow out the crystal.
The existing material melting method is that the power of a heater respectively reaches preset power within a certain time, and after the power lasts for a certain time, the raw materials are completely melted and enter a temperature stabilizing procedure. In order to shorten the time of the material melting process and reduce the total power consumption, the preset power of the heater is usually increased as much as possible, but since the quartz crucible is easy to soften (the softening temperature is about 1600 ℃) and deform, and even has the possibility of local melting (the melting point temperature is 1713 ℃), the yield control of the subsequent long-time crystal growth and the risk of silicon liquid leakage are greatly influenced, and therefore, the proper total power of the heater is required in the material melting process. Therefore, the existing constant-power material melting method is difficult to realize that the quartz crucible is not consumed while the material melting time and the power consumption are reduced.
Therefore, there is a need to provide a new material melting method for crystal growth to solve the above problems.
Disclosure of Invention
In this summary, concepts in a simplified form are introduced that are further described in the detailed description. This summary of the invention is not intended to identify key features or essential features of the claimed subject matter, nor is it intended to be used as an aid in determining the scope of the claimed subject matter.
The invention provides a material melting method for crystal growth, which comprises the following steps:
in the first heating stage, the heater heats the raw materials with first power and lasts for first heating time;
a second heating phase in which the heater continues to heat the feedstock at a second power for a second heating time, wherein the second power is lower than the first power;
and a third heating stage, wherein the heater continuously heats the raw materials at a third power for a third heating time.
Further, the third power is higher than the second power, and the third power is lower than the first power.
Further, the material melting method for crystal growth further comprises the following steps: and when the raw materials are completely melted, entering a temperature stabilization stage, and in the temperature stabilization stage, adjusting the melting speed of the silicon melt by the heater with temperature stabilization power.
Further, the ratio of the first power to the temperature stabilizing power ranges from 1.4 to 2.0; the ratio of the second power to the temperature stabilizing power ranges from 1.1 to 1.4; the ratio of the third power to the temperature stabilizing power ranges from 1.2 to 1.5.
Further, the first heating time is 3-5 hours; the second heating time is more than 5 hours; the third heating time is 1-2 hours.
Further, the second heating stage includes a feed operation.
Further, the heater includes a bottom heater and/or a side heater.
According to the material melting method for crystal growth provided by the invention, the material melting process is divided into three stages, and the heating power of the second stage is lower than that of the first stage, so that the total material melting time is shortened, the temperature of the quartz crucible is prevented from exceeding the softening temperature, and the yield of crystal growth is improved.
Drawings
The following drawings of the invention are included to provide a further understanding of the invention. The drawings illustrate embodiments of the invention and, together with the description, serve to explain the principles of the invention.
In the drawings:
FIG. 1 is a schematic view of an apparatus for crystal growth according to an exemplary embodiment of the present invention;
fig. 2 is a flowchart of a material melting method for crystal growth according to an exemplary embodiment of the present invention.
Reference numerals
1. Furnace body 2, crystal
3. Reflecting screen 4, raw materials
5. Crucible 6 and heater
7. Crucible lifting mechanism 8 and heat insulation structure
Detailed Description
In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present invention. It will be apparent, however, to one skilled in the art, that the present invention may be practiced without one or more of these specific details. In other instances, well-known features have not been described in order to avoid obscuring the invention.
In order to provide a thorough understanding of the present invention, a detailed description will be given in the following description to illustrate a material melting method for crystal growth of the present invention. It is apparent that the practice of the invention is not limited to the specific details known to those skilled in the art of crystal growth. The following detailed description of the preferred embodiments of the invention, however, the invention can be practiced otherwise than as specifically described.
It should be noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular is intended to include the plural unless the context clearly dictates otherwise. It will be further understood that the terms "comprises" and/or "comprising," when used in this specification, 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.
Exemplary embodiments according to the present invention will now be described in more detail with reference to the accompanying drawings. These exemplary embodiments may, however, be embodied in many different forms and should not be construed as limited to only the embodiments set forth herein. It is to be understood that these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of these exemplary embodiments to those skilled in the art. In the drawings, the thicknesses of layers and regions are exaggerated for clarity, and the same elements are denoted by the same reference numerals, and thus the description thereof will be omitted.
The crystal growth device shown in fig. 1 comprises a furnace body 1, wherein the furnace body 1 comprises a crucible 5, a heater 6 is arranged on the periphery of the crucible 5, a raw material 4 is arranged in the crucible 5, after the raw material 4 is in a melt state by heating and melting the material, a crystal 2 is formed above the raw material 4 in the melt state, and a reflecting screen 3 is arranged above the crucible 5 and surrounds the crystal 2. As an example, the crystal 2 is a single crystal silicon rod.
Illustratively, the furnace body 1 is a stainless steel cavity, and the furnace body 1 is vacuum or filled with protective gas. As an example, the shielding gas is argon, the purity of the shielding gas is more than 97%, the pressure is 5mbar-100mbar, and the flow rate is 70slpm-200 slpm.
Illustratively, the crucible 5 is made of a high temperature and corrosion resistant material, and the crucible 5 contains the raw material 4 in a melt state for crystal growth. In one embodiment, the crucible 5 comprises a quartz crucible and/or a graphite crucible. The crucible 5 contains a source material 4, such as polycrystalline silicon. The raw material 4 is heated in the crucible 5 to a silicon melt for growing the single crystal silicon rod, and specifically, a seed crystal is immersed in the silicon melt, rotated and slowly pulled by a seed crystal shaft, so that silicon atoms grow along the seed crystal to a single crystal silicon rod. The seed crystal is formed by cutting or drilling a silicon single crystal with a certain crystal orientation, the common crystal orientation is <100>, <111>, <110> and the like, and the seed crystal is generally a cylinder.
Illustratively, the periphery of the crucible 5 is provided with a heater 6, and the heater 6 may be a graphite heater and may be arranged on the side and/or the bottom of the crucible 5 for electrically heating the crucible 5. Further, the heater 6 includes one or more heaters disposed around the crucible 5 to make the thermal field distribution of the crucible 5 uniform.
Illustratively, a reflecting screen 3 is also arranged in the furnace body 1, is positioned above the crucible 5, and is positioned outside the crystal 2 and surrounds the crystal 2, so that the heat of the melt 4 is prevented from being transferred to the furnace body 1 in the form of heat radiation and the like to cause heat loss.
Further, the crystal growing apparatus further includes a crucible elevating mechanism 7 for supporting and rotating the crucible shaft to effect elevation of the crucible 5.
Further, the crystal growth device also comprises a heat insulation structure 8 which is arranged on the inner wall of the furnace body 1 to prevent heat loss and realize heat preservation of the furnace body 1. The insulation structure 8 is located above and outside the heater 6.
In the crystal growth process, the process of melting a polycrystalline silicon raw material into a silicon melt for growing a single crystal silicon rod is called a melting process, and is an important component of the crystal growth process. Aiming at the defects of the existing material melting method, the invention provides a material melting method for crystal growth, which comprises the following steps as shown in figure 2:
s201: in the first heating stage, the heater heats the raw materials with first power and lasts for first heating time;
s202: a second heating phase in which the heater continues to heat the feedstock at a second power for a second heating time, wherein the second power is lower than the first power;
s203: and a third heating stage, wherein the heater continuously heats the raw materials at a third power for a third heating time.
Before the material melting, the method also comprises the step of placing the raw material 4 into the crucible 5.
Illustratively, the feedstock 4 includes, but is not limited to, polycrystalline silicon. Further, the polycrystalline silicon comprises lump materials with a large volume and crushed materials with a small volume, and because the lump polycrystalline silicon raw materials are loaded into the crucible 5 with gaps between the raw materials, the lump materials and the crushed materials are proportioned to improve the filling rate of the raw materials in the crucible 5.
Illustratively, the crucible 5 includes a quartz crucible at an inner side and a graphite crucible at an outer side, wherein the graphite crucible serves to support and protect the quartz crucible.
In one embodiment, about 180kg of lump high-purity polycrystalline silicon and about 40kg of crushed material are carefully charged into a 32-inch high-purity quartz crucible having a packing rate of 50% to 70% in a highly dust-free clean environment, and are put into the furnace body 1 together, and then the furnace body 1 is evacuated to replace the internal air, and the material-melting process is started with the protective gas filled therein.
Illustratively, the heater 6 includes a side heater (S/H) disposed at a side of the crucible 5, and a bottom heater (B/H) disposed at a bottom of the crucible 5. Further, the total power of the heater is represented by Pt, the heating power of the side heater is represented by Ps, and the heating power of the bottom heater is represented by Pb, where Pt is Ps + Pb.
In the traditional material melting process, the power of the heater is kept unchanged. In one embodiment, Ps is 120kW, Pb is 40kW, the material melting time is 10h, the temperature stabilizing stage is started after the material melting is completed, and the temperature stabilizing power Pw is 100 kW. In the crystal growth process, the crucible is easy to deform, the crucible bottom is softened and bulges, or the crucible is overheated, and the inner hole of the inner wall is broken, so that the service life of the crucible is shortened, and the cost is increased; and the crystal edge breaking and crystal growth failure can be caused, and the crystal growth yield is low.
As shown in fig. 2, step S201 is first executed: in the first heating stage, the heater heats the raw material with first power for a first heating time.
Illustratively, the ratio of the first power to the ramp power for the subsequent ramp phase ranges from 1.4 to 2.0, i.e., Pt1Pw is 1.4-2.0: 1; the first heating time is 3-5 hours.
In one embodiment, the first power Pt1About 180kW, specifically, Ps1About 120kW and Pb1About 60kW, the first heating time is about 3 h.
The first heating stage further comprises two stages: a rapid heating-up stage and a material melting starting stage. At the initial stage of material melting, the temperature of the thermal field, the crucible and the silicon material in the furnace is low, and the contained heat capacity is low, so that the temperature and the heat capacity of the thermal field in the furnace can be rapidly increased by adopting set higher power for heating, and the purpose of shortening the total material melting time is achieved. The heating power of the side heater and the bottom heater is repeatedly turned on, so that the temperature and the heat in the furnace body 1 are quickly raised; after the heater heats the raw material at the first power for a certain time, the polycrystalline silicon in the inner and outer portions of the quartz crucible starts to melt, because the increased heat in the furnace body is almost consumed in the latent heat of dissolution of the polycrystalline silicon, the temperature of the liquefied polycrystalline silicon tends to be stable, and the speed of liquefaction (the melting quality of polycrystalline silicon per hour) and the increased heat Q in the furnace body are in a linear relationship.
Next, step S202 is performed: and a second heating stage, wherein the heater continuously heats the raw material at a second power for a second heating time.
Illustratively, the second power is lower than the first power.
Illustratively, the second heating time is greater than the first heating time.
Illustratively, the ratio of the second power to the steady-temperature power of the subsequent steady-temperature phase ranges from 1.1 to 1.4, i.e., Pt2Pw is 1.1-1.4: 1; the second heating time is 5 hours or more.
In one embodiment, the second power Pt2About 130kW, specifically, Ps2About 100kW and Pb2About 30kW and a second heating time of about 9 h.
Further, the second heating stage may further include a charging operation, which may be repeated several times, by adding more polycrystalline silicon raw material to the quartz crucible to increase the filling rate of the crucible and melting more raw material in the crucible.
The second heating stage is a material melting main stage, and the polycrystalline silicon raw material is gradually melted by stably supplementing heat. Since the temperature rise rate of the quartz crucible is related to the melting rate of polycrystalline silicon (melting quality of polycrystalline silicon per hour) or the total power Pt of the heater, when the total power of the heater is too high, the melting rate of polycrystalline silicon is increased and the temperature of the quartz crucible also rises relatively fast. The invention prevents the temperature of the quartz crucible from exceeding the softening temperature of the quartz by reducing the heating power of the second heating stage, thereby avoiding the damage to the quartz crucible and providing the yield of the subsequent crystal growth.
Next, step S203 is executed: and a third heating stage, wherein the heater continuously heats the raw materials at a third power for a third heating time.
Illustratively, the third power is higher than the second power, and the third power is lower than the first power.
Illustratively, the third heating time is less than the first heating time.
Illustratively, the ratio of the third power to the steady-temperature power of the subsequent steady-temperature phase ranges from 1.2 to 1.5, i.e., Pt3Pw is 1.2-1.5: 1; the third heating time is 1-2 hours.
In one embodiment, thirdPower Pt3About 155kW, specifically, Ps3About 110kW and Pb3About 45kW and a third heating time of about 1-2 h.
The third heating stage is a residual material treatment stage, after melting is finished and before temperature stabilization is started, power is properly increased within a certain time, the silicon material can be fully melted, the quartz crucible and the silicon melt are fully fused, the silicon melt is prevented from containing unmelted residual silicon material, and the crystal pulling yield is improved.
And then, after the raw materials are completely melted, entering a temperature stabilizing stage, wherein the heater adjusts the melting speed of the silicon melt with temperature stabilizing power so as to reach the condition suitable for crystal growth.
In one embodiment, the soaking power Pw is about 100 kW.
According to the material melting method for crystal growth provided by the invention, the material melting process is divided into three stages, and the heating power of the second stage is lower than that of the first stage, so that the total material melting time is shortened, the damage of the quartz crucible caused by the fact that the temperature of the quartz crucible exceeds the softening temperature of quartz is avoided, and the yield of crystal growth is improved.
The present invention has been illustrated by the above embodiments, but it should be understood that the above embodiments are for illustrative and descriptive purposes only and are not intended to limit the invention to the scope of the described embodiments. Furthermore, it will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that many variations and modifications may be made in accordance with the teachings of the present invention, which variations and modifications are within the scope of the present invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (4)
1. A material melting method for crystal growth is characterized by comprising a first heating stage, a second heating stage and a third heating stage which are sequentially carried out, wherein:
in the first heating stage, the heater heats the raw materials with first power and lasts for first heating time;
a second heating phase in which the heater continues to heat the feedstock at a second power for a second heating time, wherein the second power is lower than the first power;
a third heating stage in which the heater continues to heat the feedstock at a third power for a third heating time, the third power being higher than the second power and the third power being lower than the first power;
further comprising: when the raw materials are completely melted, entering a temperature stabilization stage, and in the temperature stabilization stage, adjusting the melting speed of the silicon melt by the heater with temperature stabilization power;
the ratio of the first power to the temperature stabilizing power ranges from 1.4 to 2.0; the ratio of the second power to the temperature stabilizing power ranges from 1.1 to 1.4; the ratio of the third power to the temperature stabilizing power ranges from 1.2 to 1.5.
2. A material melting method for crystal growth as claimed in claim 1, wherein the first heating time is 3 to 5 hours; the second heating time is more than 5 hours; the third heating time is 1-2 hours.
3. The method of claim 2, wherein the second heating stage comprises a feeding operation.
4. A melting method for crystal growth as claimed in claim 1, characterized in that the heater comprises a bottom heater and/or a side heater.
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| CN109023509A (en) * | 2018-08-31 | 2018-12-18 | 包头美科硅能源有限公司 | A method of preparing solar level n type single crystal silicon |
| CN109972200A (en) * | 2019-04-18 | 2019-07-05 | 邢台晶龙电子材料有限公司 | Continuous pulling silicon single crystal growing method |
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2020
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| CN1147032A (en) * | 1995-07-25 | 1997-04-09 | Memc电子材料有限公司 | Method for preparing molten silicon melt from polycrystalline silicon charge |
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