CN115522256A - Method for processing crystal growth graphite crucible for integrated circuit - Google Patents
Method for processing crystal growth graphite crucible for integrated circuit Download PDFInfo
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- CN115522256A CN115522256A CN202110708403.1A CN202110708403A CN115522256A CN 115522256 A CN115522256 A CN 115522256A CN 202110708403 A CN202110708403 A CN 202110708403A CN 115522256 A CN115522256 A CN 115522256A
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- groove
- graphite crucible
- crucible
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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
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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)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
Abstract
The invention introduces a processing method of a crystal growth graphite crucible for an integrated circuit, and mainly aims to solve the problem that the normal growth of a crystal is influenced by gas bubbling generated by the reaction of the inner surface of the graphite crucible and the outer surface of a quartz crucible. The inner surface of the graphite crucible is processed, the groove with the shape is stored in the graphite crucible, and the groove extends to the upper edge of the graphite crucible. Through the design, the graphite crucible can discharge generated gas under the condition of not influencing the original strength and heat transfer uniformity of the graphite crucible under the crystal growth environment, and the influence of bubbling on the crystal growth is eliminated.
Description
Technical Field
The invention relates to monocrystalline silicon growth equipment for integrated circuits, in particular to a graphite crucible for growing monocrystalline silicon.
Background
In the growth of electronic grade silicon single crystal by the CZ method, generally, a silicon single crystal ingot is pulled using a quartz crucible, and in the growth of silicon single crystal, a reaction between the quartz crucible and a silicon material is generally a point of concern, but in addition to this, a quartz crucible is usedAnother reaction of the crucible needs to be concerned; the crucible used for the crystal growth by the CZ method is generally divided into two parts, namely a graphite crucible at the outer layer and a quartz crucible at the inner layer, wherein the graphite crucible mainly comprises graphite (the content accounts for 45-55 percent), silicon carbide, silica, refractory clay, asphalt tar and the like, and the graphite crucible mainly plays a role in uniformly transferring heat and keeping the shape of the quartz crucible; in practical production, siO in quartz crucible is grown in monocrystalline silicon growing environment 2 The reaction can be carried out with the main component graphite (C) in the graphite crucible, CO gas can be generated in a reaction generation product, because the inner wall of the graphite crucible is tightly attached to the inner wall of the quartz crucible, the generation of the CO gas can generate local bubbling in an attaching mode, because the physical property of the quartz crucible is soft under the high-temperature condition of crystal growth, the formation of the bubbling can influence the heat transfer to influence the heating of the quartz crucible, and the deformation generated by the bubbling can also cause the change of a flow field of a melt in polysilicon in the crucible, thereby influencing the uniformity of the crystal growth, and even damaging the quartz crucible in serious cases.
In the prior art, the problem is generally solved by adopting a mode of punching holes on the surface of a graphite crucible, but the method has certain defects that firstly, the strength of the graphite crucible is reduced due to a large number of holes, and the effect is reduced due to the fact that all bubbles influencing the growth of crystals are discharged due to a small number of holes; and secondly, the opening of the hole can cause uneven heating of the quartz crucible at the hole, thereby influencing the normal growth of the crystal.
Since there are technical problems affecting the yield of products in the prior art, there is a need for improvement of the prior art.
Disclosure of Invention
Therefore, the invention aims to design a graphite crucible to solve the problem that the normal growth of crystals is influenced by bubbling of gas generated by reaction between the inner surface of the graphite crucible and the outer surface of a quartz crucible.
A solution for solving the technical problem;
the invention carries out new design on the graphite crucible for the crystal growth of the integrated circuit, and can solve the problem of CO bubbling at the contact position of the crucible by designing a plurality of grooves on the inner surface of the graphite crucible and designing the groove type and the slotting mode of the grooves
The opening shape of the groove in the invention conforms to the equation
Wherein
C = σ; the value mode of the sigma is as follows: when 200mm crystal growth is carried out, 2 is more than or equal to sigma and less than or equal to 3, when 300mm crystal growth is carried out, 3 is more than sigma and less than or equal to 4, R value satisfies 15 is more than or equal to R and less than or equal to 24.
The maximum depth of the groove during processing is H, which is slightly less than H
And H ranges from 2.7mm to 4.4mm.
When the quartz crucible deforms and expands under the condition of crystal growth, the expansion surface of the quartz crucible keeps circular, the surface of the quartz crucible is blocked by the opening of the common circular groove, so that gas cannot be discharged, and the groove in the invention is designed in a shape that a gap is still left between the expanded quartz crucible and the graphite crucible at the groove, so that the gas can be normally discharged.
After the shape of the groove is determined, the invention designs the grooving linearity of the groove, and the inner surface of the crucible is divided into a vertical surface M 1 (hereinafter referred to as M) 1 Faces) and curved surfaces M 2 (hereinafter referred to as M) 2 Flour). M is a group of 1 Flour and M 2 The grooves on the surface are divided into two parts, namely longitudinal grooves Y (hereinafter referred to as grooves Y) and transverse grooves X (hereinafter referred to as grooves X).
Said M 1 The grooving mode of the grooves at the surfaces is as follows: at M 1 N equidistant reference lines L are selected at the surface, the L is taken as the upper edge of the graphite crucible with the x axis and is taken as the Y axis to perform the slotting of the groove Y, and the slotting line type meets the equation:
y=u·sin（vx） （2）
wherein u is 7.5-9.5, v is 0.7-1.4; the number of grooves n during grooving is 24-36.
At M 1 After the groove Y of the surface is processed, M is carried out 1 The processing mode of the surface groove X is as follows: delay M 1 And processing the grooves X on a horizontal plane parallel to the upper edge of the crucible, wherein the distance between every two grooves X is equal to be calculated as D, and the value range of D is 50-70mm.
Said M 2 The groove grooving mode at the face is as follows: from M 1 And starting from the intersection point of the groove Y of the surface and the interface A to the lowest point of the curved surface, and slotting along the straight line of the curved surface. M 2 The surface is also provided with grooves X, M 2 The first groove X on the surface 21 And M 1 Last groove X on the face 1n Is also equal to D, and M 2 The vertical distance between the grooves X at the faces is also D.
And after the grooving is finished, the graphite crucible is processed, and the graphite crucible can be used for producing crystal bars in a normal crystal growth process.
Drawings
FIG. 1 is a schematic view of the inner surface of a graphite crucible, wherein M 1 Is a vertical plane, M 2 Is a curved surface, and S is an interface of a vertical surface and the curved surface.
FIG. 2 is a schematic view of a groove type, wherein A is a surface of a quartz crucible which can be reached after thermal expansion, and B is an original inner surface of a graphite crucible.
Fig. 3 is a schematic diagram of a groove line of a partial groove on the inner surface of a graphite crucible, wherein X is a transverse groove, Y is a longitudinal groove, and L is a reference line of 1 groove Y, and the number and length of the grooves in the diagram are not equal to the number of grooves in actual processing, and are only used for showing the rule.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1
The growth of a 200mm crystal bar is needed in the production, the required quartz crucible is processed, and the slotting shape is designed as follows:
wherein
，c=3，R=15。
The processing depth H =2.7mm. After the groove shape is determined, a groove line is designed, wherein the linear equation of the groove Y is Y =7.5sin (0.7X), the number of grooves n =30, and the distance D =50mm between the grooves X. The inner wall of the graphite crucible was processed in this manner, and the growth of a 200mm silicon single crystal rod was carried out according to the flow of crystal growth.
After the pulling of a plurality of crystal bars is finished, the outer surface of the quartz crucible and the whole graphite crucible are observed when the crucible is replaced, the quartz crucible is not damaged or abnormally seriously deformed, and the graphite crucible is not cracked. And then detecting the change condition of the radial resistivity of the 4 crystal bars, wherein the data are as follows: a1=2.51%, A2=1.81%, A3=1.83%, A4=1.71%, A5=3.12%, B1=2.72%, B2=2.23%, B3=2.17%, B4=2.31%, B5=2.92%, C1=2.41%, C2=1.97%, C3=1.99%, C4=1.99%, C5=3.51%, D1=2.55%, D2=1.79%, D3=2.02%, D4=2.01%, D5=2.71%.
According to the data, the change of the integral radial resistivity of the crystal bar is in a reasonable range, and the crystal growth process is normally carried out.
Example 2
The growth of a 200mm crystal bar is needed in the production, the required quartz crucible is processed, and the slotting shape is designed as follows:
in which
，c=2，R=24。
The processing depth H =4.4mm. After the groove type is determined, designing a groove line of the groove, wherein the linear equation of the groove Y is Y =9.5sinx, the grooving number n =24, and the distance D =60mm between the grooves X. The inner wall of the graphite crucible was processed in this manner, and the growth of a 200mm silicon single crystal rod was carried out according to the flow of crystal growth.
After the pulling of a plurality of crystal bars is finished, the outer surface of the quartz crucible and the whole graphite crucible are observed when the crucible is replaced, the damage and the abnormal serious deformation trace of the quartz crucible are not found, and the graphite crucible does not have cracks. And then detecting the change condition of the radial resistivity of the 4 crystal bars, wherein the data is as follows: a1=2.24%, A2=1.94%, A3=1.73%, A4=1.75%, A5=1.96%, B1=1.71%, B2=1.49%, B3=1.40%, B4=1.63%, B5=1.68%, C1=3.04%, C2=2.59%, C3=2.66%, C4=2.74%, C5=3.22%, D1=1.53%, D2=1.38%, D3=1.27%, D4=1.27%, D5=1.76%.
According to the data, the change of the integral radial resistivity of the crystal bar is within a reasonable range, and the crystal growth process is normally carried out.
Example 3
The growth of a 300mm crystal bar is needed in the production, the required quartz crucible is processed, and the slotting shape is designed as follows:
wherein
，c=4，R=20。
The processing depth H =3.5mm. After the groove type is determined, designing a groove line of the groove, wherein the linear equation of the groove Y is Y =8sin (1.4X), the number of grooves n =24, and the distance D =70mm between the grooves X. The inner wall of the graphite crucible was processed in this manner, and the growth of a 300mm silicon single crystal rod was carried out according to the flow of crystal growth.
After the pulling of a plurality of crystal bars is finished, the outer surface of the quartz crucible and the whole graphite crucible are observed when the crucible is replaced, the quartz crucible is not damaged or abnormally seriously deformed, and the graphite crucible is not cracked. And then detecting the change condition of the radial resistivity of the 4 crystal bars, wherein the data are as follows: a1=2.30%, A2=1.71%, A3=1.85%, A4=1.80%, A5=2.19%, B1=2.54%, B2=2.16%, B3=2.11%, B4=1.94%, B5=2.83%, C1=1.57%, C2=1.12%, C3=1.32%, C4=1.36%, C5=1.78%, D1=3.27%, D2=2.64%, D3=2.70%, D4=2.71%, D5=2.90%.
According to the data, the change of the integral radial resistivity of the crystal bar is within a reasonable range, and the crystal growth process is normally carried out.
Example 4
The growth of a 300mm crystal bar is needed in the production, the required quartz crucible is processed, and the slotting shape is designed as follows:
wherein
，c=3，R=15。
The processing depth H =2.7mm. After the groove shape is determined, a groove line is designed, wherein the linear equation of the groove Y is Y =7.5sin (0.7X), the number of grooves n =36, and the distance D =50mm between the grooves X. The inner wall of the graphite crucible was processed in this manner, and the growth of a 300mm silicon single crystal rod was carried out according to the flow of crystal growth.
After the pulling of a plurality of crystal bars is finished, the outer surface of the quartz crucible and the whole graphite crucible are observed when the crucible is replaced, the damage and the abnormal serious deformation trace of the quartz crucible are not found, and the graphite crucible does not have cracks. And then detecting the change condition of the radial resistivity of the 4 crystal bars, wherein the data are as follows: a1=3.07%, A2=2.42%, A3=2.61%, A4=2.65%, A5=2.94%, B1=1.97%, B2=1.32%, B3=1.21%, B4=1.20%, B5=1.34%, C1=2.47%, C2=2.09%, C3=2.13%, C4=2.10%, C5=2.29%, D1=2.25%, D2=1.70%, D3=1.78%, D4=1.56%, D5=1.85%.
According to the data, the change of the integral radial resistivity of the crystal bar is within a reasonable range, and the crystal growth process is normally carried out.
Claims (5)
1. A graphite crucible for crystal growth of integrated circuits is characterized in that a groove is formed in the inner surface of the graphite crucible, and the shape of the groove satisfies the equation:
wherein
C = σ, and the value mode of σ is as follows: sigma is more than or equal to 2 and less than or equal to 3 when crystal growth is carried out for 200mm, sigma is more than 3 and less than or equal to 4 when crystal growth is carried out for 300mm, R value satisfies that R is more than or equal to 15 and less than or equal to 24, the maximum depth of groove processing is H, and the value is slightly less than
And H ranges from 2.7mm to 4.4mm.
2. The graphite crucible as claimed in claim 1, wherein the graphite crucible inner surface is divided into vertical planes (M) 1 ) And curved surface (M) 2 ) Vertical plane (M) 1 ) And curved surface (M) 2 ) Both are provided with a longitudinal groove (Y) and a horizontal groove (X).
3. Quartz crucible according to claim 2, characterized in that the vertical surface (M) is 1 ) The grooving mode of the longitudinal groove (Y) is as follows: vertical plane (M) 1 ) N equidistant reference lines (L) are selected, the reference lines (L) are used as an x axis, the upper edge of the graphite crucible is used as a Y axis, and the grooving of the longitudinal groove (Y) is carried out, wherein the grooving line type meets the equation:
y=u·sin（vx） （2）
wherein u is 7.5-9.5, v is 0.7-1.4; the number of grooves n during grooving is 24-36.
4. Quartz crucible according to claim 2, characterized in that the vertical surface (M) 1 ) The slotting mode of the upper horizontal slot (X) is as follows: extended vertical plane (M) 1 ) Processing the horizontal grooves (X) on a horizontal plane parallel to the upper edge of the crucible, wherein the equal distance between every two horizontal grooves (X) is calculated as D, and the value range of D is 50-70mm.
5. Quartz crucible according to claim 2, characterized in that the curved surface (M) is 2 ) The grooving mode of the upper groove is as follows: from the vertical plane (M) 1 ) OfStarting from the intersection point of the groove (Y) and the interface (A) to the lowest point of the curved surface, starting to form a groove along the curved surface, and forming a curved surface (M) 2 ) A horizontal groove (X) and a curved surface (M) are arranged on the upper part 2 ) Go up the first groove (X) 21 ) And M 1 Last groove on the face (X) 1n ) Distance between them is equal to D, and curved surface (M) 2 ) The distance between the upper horizontal grooves (X) in the vertical direction is equal to D.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008201619A (en) * | 2007-02-20 | 2008-09-04 | Shin Etsu Handotai Co Ltd | Graphite crucible and apparatus for manufacturing silicon single crystal with it |
| US20110048315A1 (en) * | 2009-09-02 | 2011-03-03 | Heraeus Shin-Etsu America, Inc. | Method and apparatus for venting gas between a crucible and a susceptor |
| CN102094235A (en) * | 2009-12-11 | 2011-06-15 | 硅电子股份公司 | Graphite crucible and silicon single crystal manufacturing apparatus |
| CN209292207U (en) * | 2018-10-17 | 2019-08-23 | 宁晋晶兴电子材料有限公司 | A kind of silica crucible graphite jig |
-
2021
- 2021-06-25 CN CN202110708403.1A patent/CN115522256A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008201619A (en) * | 2007-02-20 | 2008-09-04 | Shin Etsu Handotai Co Ltd | Graphite crucible and apparatus for manufacturing silicon single crystal with it |
| US20110048315A1 (en) * | 2009-09-02 | 2011-03-03 | Heraeus Shin-Etsu America, Inc. | Method and apparatus for venting gas between a crucible and a susceptor |
| CN102094235A (en) * | 2009-12-11 | 2011-06-15 | 硅电子股份公司 | Graphite crucible and silicon single crystal manufacturing apparatus |
| CN209292207U (en) * | 2018-10-17 | 2019-08-23 | 宁晋晶兴电子材料有限公司 | A kind of silica crucible graphite jig |
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