CN114959880A - Quartz crucible, crucible assembly and crystal pulling furnace for producing single crystal silicon rods - Google Patents
Quartz crucible, crucible assembly and crystal pulling furnace for producing single crystal silicon rods Download PDFInfo
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- CN114959880A CN114959880A CN202210594928.1A CN202210594928A CN114959880A CN 114959880 A CN114959880 A CN 114959880A CN 202210594928 A CN202210594928 A CN 202210594928A CN 114959880 A CN114959880 A CN 114959880A
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- Prior art keywords
- crucible
- oxygen
- silicon
- quartz crucible
- single crystal
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- 239000010453 quartz Substances 0.000 title claims abstract description 60
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000013078 crystal Substances 0.000 title claims abstract description 58
- 229910021421 monocrystalline silicon Inorganic materials 0.000 title claims abstract description 26
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000001301 oxygen Substances 0.000 claims abstract description 43
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 43
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 37
- 239000010703 silicon Substances 0.000 claims abstract description 37
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000001257 hydrogen Substances 0.000 claims abstract description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 15
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 2
- 239000004917 carbon fiber Substances 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 230000002093 peripheral effect Effects 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 9
- 238000007654 immersion Methods 0.000 abstract description 4
- 230000006911 nucleation Effects 0.000 abstract description 3
- 238000010899 nucleation Methods 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 12
- 239000000155 melt Substances 0.000 description 10
- 230000008569 process Effects 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 229910002804 graphite Inorganic materials 0.000 description 8
- 239000010439 graphite Substances 0.000 description 8
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 5
- 230000007423 decrease Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 235000012431 wafers Nutrition 0.000 description 3
- 238000009826 distribution Methods 0.000 description 2
- 239000002019 doping agent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000000712 assembly Effects 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000005906 menstruation Effects 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
Images
Classifications
-
- 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
- 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
Abstract
The embodiment of the invention discloses a quartz crucible, which comprises: a bottom portion; a circumferential portion comprising an additional layer on a radially inner side; wherein the additional layer comprises an oxygen-rich layer and a silicon-based hydrogen-rich layer disposed on the oxygen-rich layer. The silicon-based hydrogen-rich layer of the quartz crucible is firstly decomposed and the decomposed hydrogen is immersed into the single crystal silicon rod under the action of convection, so that the separation of oxygen can be inhibited, further the nucleation of defects in the single crystal silicon rod is inhibited, the defects are further aggregated and grown up to control the defects to be smaller in size, and the problem that the local oxygen of the single crystal silicon rod is higher in the early stage of crystal pulling can be well solved, so that the overall yield of the crystal rod is improved; and along with the thinning of the silicon-based hydrogen-rich layer, the oxygen-rich layer is exposed in the silicon solution, a large amount of oxygen is separated out, the oxygen immersion in the silicon single crystal rod at the moment is improved, and further the content of the oxygen at the tail end of the silicon single crystal rod in the later period of crystal pulling is improved, so that the aim of uniformly distributing the whole oxygen content of the silicon single crystal rod is fulfilled.
Description
Technical Field
The invention relates to the field of semiconductor silicon wafer production, in particular to a quartz crucible for producing a monocrystalline silicon rod, a crucible assembly and a crystal pulling furnace.
Background
Silicon wafers for producing semiconductor electronic components such as integrated circuits are mainly produced by slicing a single crystal silicon rod drawn by the Czochralski (Czochralski) method. The czochralski method comprises melting polycrystalline silicon from a crucible assembly to obtain a silicon melt, immersing a single crystal seed crystal in the silicon melt, and continuously lifting the seed crystal away from the silicon melt surface, thereby growing a single crystal silicon rod at a phase interface during the movement. When the doping agent is added, the melting of the polycrystalline silicon is also accompanied by the dissolution of the doping agent, the melt in the quartz crucible is also continuously reduced along with the continuous growth of the single crystal silicon rod, and only a small amount of melt remains in the quartz crucible when the pulling of the single crystal silicon rod is completed.
With the continuous improvement of the quality of the silicon wafer, the crystal defect of the crystal bar in the crystal pulling process has higher control requirements. At present, two of the main factors influencing the crystal defects are crystal pulling process parameters and the structure and performance of the component providing the thermal field, the quality of the crystal ingot can be improved by optimizing the crystal pulling process parameters, and the quality of the structure and performance of the component providing the thermal field is a prerequisite for the quality of the crystal ingot. In addition, the performance of the components for improving the thermal field is also a crucial index for improving the quality of the crystal bar. Due to the increasing requirements for the crystal pulling environment of crystal pulling furnaces, the requirements for the performance and material of the components providing the thermal field are also increasing, and generally, the components are required to be resistant to high temperature, have good thermal stability and have high purity.
The crucible assembly, one of the most important components in the thermal field, is generally divided into an inner portion and an outer portion, wherein the inner portion is a quartz crucible for containing silicon solution, oxygen in the ingot is decomposed from the quartz crucible, and the outer portion is a graphite crucible for supporting the quartz crucible and transferring heat. However, a problem common to the use of existing crucible assemblies is that: the quartz crucible causes the uneven distribution of oxygen in the drawn ingot, and the graphite crucible has a short service life.
Disclosure of Invention
In order to solve the above-described technical problems, embodiments of the present invention are intended to provide a quartz crucible, a crucible assembly, and a crystal pulling furnace capable of promoting the oxygen concentration distribution in a single crystal silicon rod and having a long life.
The technical scheme of the invention is realized as follows:
in a first aspect, an embodiment of the present invention provides a quartz crucible, including: a bottom portion; a circumferential portion comprising an additional layer on a radially inner side; wherein the additional layer comprises an oxygen-rich layer and a silicon-based hydrogen-rich layer disposed on the oxygen-rich layer.
In a second aspect, embodiments of the present invention provide a crucible assembly, comprising: the quartz crucible according to the first aspect; an outer crucible; wherein the quartz crucible is nested in the outer crucible for supporting and transferring heat to the quartz crucible.
In a third aspect, embodiments of the present invention provide a crystal pulling furnace comprising a crucible assembly according to the second aspect.
The embodiment of the invention provides a quartz crucible, a crucible assembly and a crystal pulling furnace for producing a monocrystalline silicon rod, wherein an additional layer is formed on the radial inner side of the quartz crucible, and comprises an oxygen-rich layer and a silicon-based hydrogen-rich layer arranged on the oxygen-rich layer; and along with the thinning of the silicon-based hydrogen-rich layer, the oxygen-rich layer is exposed in the silicon solution, a large amount of oxygen is separated out, the oxygen immersion in the silicon single crystal rod at the moment is improved, and further the content of the oxygen at the tail end of the silicon single crystal rod in the later period of crystal pulling is improved, so that the aim of uniformly distributing the whole oxygen content of the silicon single crystal rod is fulfilled.
Drawings
FIG. 1 is a schematic view of one implementation of a conventional crystal pulling furnace;
FIG. 2 is another schematic view of the conventional crystal pulling furnace of FIG. 1;
FIG. 3 is a schematic view of a quartz crucible according to an embodiment of the present invention;
FIG. 4 is a schematic view of a quartz crucible according to another embodiment of the present invention;
FIG. 5 is a schematic view of a crucible assembly according to an embodiment of the present invention;
FIG. 6 is a schematic view of a crucible assembly according to another embodiment of the present invention;
FIG. 7 is a schematic view of a crucible assembly according to yet another embodiment of the present invention;
FIG. 8 is a schematic view of a crystal pulling furnace according to an embodiment of the present invention.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.
Referring to fig. 1 and 2, one implementation of a conventional crystal pulling furnace is shown. As shown in fig. 1, the crystal pulling furnace 1 includes: a furnace chamber enclosed by the housing 2, a crucible assembly 10 disposed in the furnace chamber, a graphite heater 20, a crucible rotating mechanism 30, and a crucible carrying device 40. The crucible assembly 10 is carried by a crucible carrying device 40, and a crucible rotating mechanism 30 is located below the crucible carrying device 40 for driving the crucible assembly 10 to rotate about its axis in the direction R.
When the crystal pulling furnace 1 is used to pull a single crystal silicon rod, first, a high purity polycrystalline silicon raw material is put into the crucible assembly 10, and the crucible assembly 10 is continuously heated by the graphite heater 20 while the crucible rotating mechanism 40 drives the crucible assembly 10 to rotate in the direction R to melt the polycrystalline silicon raw material contained in the crucible assembly 10 into a molten state, i.e., into a melt S2, wherein the heating temperature is maintained at about one thousand or more degrees celsius, and the gas in the furnace is typically an inert gas to melt the polycrystalline silicon without causing unwanted chemical reactions. When the liquid surface temperature of the melt S2 is controlled at the critical point of crystallization by controlling the thermal field provided by the graphite heater 20, the melt S2 rises with the pulling of the single crystal seed crystal S1 by pulling the single crystal seed crystal S1 located above the liquid surface upward in the direction T from the liquid surface to grow a single crystal silicon rod S3 in the crystal orientation of the single crystal seed crystal S1.
As the crystal pulling process progresses, the melt S2 gradually decreases. As shown in FIG. 2, when the single crystal silicon rod S3 is completely separated from the melt S2 at the end of the pulling process, only a small amount of the melt S2 remains in the crucible assembly 10. As the melt S2 gradually decreases during the crystal pulling process, the contact area of the melt S2 with the crucible assembly 10 also gradually decreases, which results in non-uniform oxygen content in the single crystal silicon rod S3, which may be low head to tail. In addition, the conventional crucible assembly generally comprises a graphite crucible and a quartz crucible nested in the graphite crucible, wherein the graphite crucible plays a role in supporting the quartz crucible and transferring heat, however, the service life of the graphite material is short, and more than 30 furnaces are required to be replaced.
In order to solve the above problem, in a first aspect, an embodiment of the present invention provides a quartz crucible. Specifically, referring to fig. 3, an embodiment of the present invention provides a quartz crucible 100 for pulling a crystal ingot, the quartz crucible 100 including: a bottom portion 101; a circumferential portion 102, said circumferential portion 102 comprising an additional layer 103 on the radially inner side; wherein the additional layer 103 comprises an oxygen-rich layer 103A and a silicon-based hydrogen-rich layer 103B disposed on the oxygen-rich layer 103A.
The embodiment of the invention provides a quartz crucible; an additional layer 103 is formed on the radial inner side of the quartz crucible, the additional layer 103 comprises an oxygen-rich layer 103A and a silicon-based hydrogen-rich layer 103B arranged on the oxygen-rich layer 103A, and in the process of producing the single crystal silicon rod by using the quartz crucible, the crucible assembly or the crystal pulling furnace provided by the embodiment of the invention, the silicon-based hydrogen-rich layer of the quartz crucible is firstly decomposed, and the decomposed hydrogen is immersed into the single crystal silicon rod under the action of convection, so that the separation of oxygen can be inhibited, meanwhile, the hydrogen can effectively inhibit the nucleation of defects in the single crystal silicon rod and further aggregate and grow to control the defects to be smaller in size, and the problem that the local oxygen of the single crystal silicon rod is higher in the early stage of crystal pulling can be well solved, so that the overall yield of the crystal rod is improved; and along with the thinning of the silicon-based hydrogen-rich layer, the oxygen-rich layer is exposed in the silicon solution, a large amount of oxygen is separated out, the oxygen immersion in the silicon single crystal rod at the moment is improved, and further the content of the oxygen at the tail end of the silicon single crystal rod in the later period of crystal pulling is improved, so that the aim of uniformly distributing the whole oxygen content of the silicon single crystal rod is fulfilled.
For the provision of an additional layer, preferably, referring to fig. 4, said circumferential portion 102 comprises a straight wall portion 102A and a circular arc wall portion 102B located between said straight wall portion 102A and said bottom portion 101, wherein said additional layer 103 is provided on said circular arc wall portion 102B.
In the pulling process of the single crystal silicon rod, the oxygen in the single crystal silicon rod exhibits a condition of a high head and a low tail in a length direction due to segregation of the oxygen, however, by using the quartz crucible provided according to the embodiment of the present invention, since the additional layer is formed on the circular arc wall portion 102B, at the beginning of the constant diameter of the crystal pulling process, the silicon-based hydrogen-rich layer at the circular arc wall portion 102B will be decomposed first, to restrain further aggregation and growth of defects in the single crystal silicon rod after nucleation by suppressing oxygen precipitation at the arc wall portion 102B, thereby solving the problems that the defects are further grown up due to the fluctuation of the pulling speed at the initial stage of constant diameter and the head oxygen of the pulled monocrystalline silicon rod is higher, in the latter period of the menstruation period, along with the exposure of the oxygen-rich layer, a large amount of oxygen is separated out, so that the oxygen immersion in the silicon single crystal rod at the moment is improved, and further, the oxygen content at the tail end of the silicon single crystal rod is improved.
According to an embodiment of the present invention, the thickness of each portion of the quartz crucible 100 may be different, and preferably, the thickness of the circumferential portion 102 is greater than the thickness of the bottom portion 101.
Further, it is preferable that the thickness of the circular arc wall portion 102B is larger than that of the straight wall portion 102A.
According to a preferred embodiment of the present invention, the thickness ratio of the straight wall portion 102A, the circular arc wall portion 102B and the bottom portion 101 is: 6: 8: 5. In the process of pulling the single crystal silicon rod, the silicon solution can wash the radial inner side of the quartz crucible, wherein the silicon solution has the strongest washing effect on the arc wall part and the smallest washing effect on the bottom part, so that the wall thickness of the arc wall part is set to be the thickest, and the wall thickness of the bottom part is set to be the thinnest, and the service life of the quartz crucible can be optimized on the premise of ensuring reasonable cost.
In a second aspect, referring to fig. 5, an embodiment of the present invention provides a crucible assembly GS, including: the quartz crucible 100 according to the first aspect; an outer crucible 200; wherein the quartz crucible 100 is nested in the outer crucible 200, and the outer crucible 200 is used for supporting the quartz crucible 100 and transferring heat to the quartz crucible 100.
For better support of the quartz crucible 100, preferably, with reference to fig. 6, the outer crucible 200 comprises a first flange 201 extending radially outwardly in a horizontal direction at the mouth of the outer crucible 200, and the quartz crucible 100 comprises a second flange 104 extending radially outwardly in a horizontal direction at the mouth of the quartz crucible, the first flange 201 and the second flange 104 being arranged such that the second flange 104 rests on the first flange 201 when the quartz crucible 100 is nested in the outer crucible 200.
Referring to FIG. 6, the outer crucible 200 has a substantially cylindrical shape, and in use, the outer crucible 200 is used for receiving heat from the heater and uniformly transmitting the heat to the quartz crucible 100 nested inside the outer crucible 200, and the quartz crucible 100 uniformly transmits the heat to the silicon solution contained therein, and since the quartz crucible is softened and collapsed during heating, the outer crucible is required to be well supported, and according to an embodiment of the present invention, by providing both the outer crucible 200 and the quartz crucible 100 with horizontal flanges at the mouth, and providing the flanges of both the outer crucible 200 and the quartz crucible 100 such that the flange of the quartz crucible 100 overlaps the flange of the outer crucible 200 when the quartz crucible 100 is nested in the outer crucible 200, better support of the quartz crucible 100 by the outer crucible 200 is achieved, and softening and collapsing of the quartz crucible 100 is prevented.
In order to provide the outer crucible with a better service life, it is preferable that the outer crucible 200 is made of a carbon fiber composite material.
According to the preferred embodiment of the present invention, referring to fig. 7, the outer crucible 200 is formed in a cylindrical shape having a flat bottom surface, whereby the outer crucible 200 can be heated more uniformly and can also transfer heat to the solution uniformly, and moreover, it is more stable during rotation, and the shaking of the melt of the silicon solution is effectively suppressed.
In a third aspect, referring to fig. 8, embodiments of the present invention provide a crystal pulling furnace LF including a crucible assembly GS in accordance with the second aspect described above.
It should be noted that: the technical schemes described in the embodiments of the present invention can be combined arbitrarily without conflict.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (9)
1. A quartz crucible for producing a single crystal silicon rod, characterized by comprising:
a bottom portion;
a circumferential portion comprising an additional layer on a radially inner side;
wherein the additional layer comprises an oxygen-rich layer and a silicon-based hydrogen-rich layer disposed on the oxygen-rich layer.
2. The quartz crucible of claim 1, wherein the circumferential portion comprises a straight wall portion and a radiused wall portion between the straight wall portion and the bottom portion, wherein the additional layer is disposed on the radiused wall portion.
3. The quartz crucible of claim 2, wherein the thickness of the peripheral portion is greater than the thickness of the bottom portion.
4. The quartz crucible of claim 3, wherein the thickness of the circular arc wall portion is greater than the thickness of the straight wall portion.
5. A crucible assembly, comprising:
the quartz crucible according to any one of claims 1 to 4;
an outer crucible;
wherein the quartz crucible is nested in the outer crucible for supporting and transferring heat to the quartz crucible.
6. The crucible assembly of claim 5, wherein the outer crucible comprises a first flange extending radially outwardly in a horizontal direction at a mouth of the outer crucible, and the quartz crucible comprises a second flange extending radially outwardly in a horizontal direction at a mouth of the quartz crucible, the first and second flanges being arranged such that when the quartz crucible is nested in the outer crucible, the second flange rests on the first flange.
7. The crucible assembly of claim 5 or 6, wherein the outer crucible is made of a carbon fiber composite material.
8. The crucible assembly of claim 5 or 6, wherein the outer crucible is formed in a cylindrical shape having a bottom surface that is planar.
9. A crystal pulling furnace, comprising the crucible assembly of any one of claims 5 to 8.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210594928.1A CN114959880B (en) | 2022-05-27 | 2022-05-27 | Quartz crucible, crucible assembly and crystal pulling furnace for producing monocrystalline silicon rod |
| TW111137961A TWI815688B (en) | 2022-05-27 | 2022-10-06 | A quartz crucible, crucible component and crystal pulling furnace for producing single crystal silicon rods |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210594928.1A CN114959880B (en) | 2022-05-27 | 2022-05-27 | Quartz crucible, crucible assembly and crystal pulling furnace for producing monocrystalline silicon rod |
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| CN114959880A true CN114959880A (en) | 2022-08-30 |
| CN114959880B CN114959880B (en) | 2024-02-13 |
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| TW (1) | TWI815688B (en) |
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2022
- 2022-05-27 CN CN202210594928.1A patent/CN114959880B/en active Active
- 2022-10-06 TW TW111137961A patent/TWI815688B/en active
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Also Published As
| Publication number | Publication date |
|---|---|
| CN114959880B (en) | 2024-02-13 |
| TWI815688B (en) | 2023-09-11 |
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