CN110129879A - A kind of two-pack chamber single-crystal si cylinder growth furnace and monocrystalline silicon growing method - Google Patents
A kind of two-pack chamber single-crystal si cylinder growth furnace and monocrystalline silicon growing method Download PDFInfo
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- CN110129879A CN110129879A CN201910561717.6A CN201910561717A CN110129879A CN 110129879 A CN110129879 A CN 110129879A CN 201910561717 A CN201910561717 A CN 201910561717A CN 110129879 A CN110129879 A CN 110129879A
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- cylinder
- seed crystal
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Classifications
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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
-
- 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
- C30B15/12—Double crucible methods
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a kind of two-pack chamber single-crystal si cylinder growth furnace, including main chamber, main chamber is connected with vacuum pump, and crucible is equipped in main chamber, and the top of main chamber is symmetrical arranged there are two the concubine being connected to main chamber, and main chamber's inner surface is equipped with heating device；Lifting motor is equipped with by turntable at the top of concubine, lifting motor is connected with clamping device by lifting line, and gripper mechanism grips have seed crystal silicon cylinder, and concubine bottom is equipped with guide shell, cooling water-circulating pipe is provided in guide shell.The present invention can improve the deficiencies in the prior art, improve the yields of czochralski method production crystalline silicon cylinder target.
Description
Technical field
The present invention relates to technical field of semiconductors, especially a kind of two-pack chamber single-crystal si cylinder growth furnace and monocrystalline silicon growing side
Method.
Background technique
Crystalline silicon cylinder is generally used for the function of manufacture integrated circuit, electronic component, power battery as a kind of semiconductor target
Energy film, at present there are two types of the growing technologies of silicon tubular target: spray coating method and mechanical processing method.
Wherein spray coating method is currently widely used method, refers in patent CN107557737A and a kind of prepares tubular target
Method, in air atmosphere, using plasma spraying or cold spraying etc. comprising transition zone stainless steel backing pipe surface spray
Apply target layer.Because the purity of the target material in an atmosphere, obtained declines.A kind of silicon target knot involved in CN107620048A
It points out to form copper coating on silicon target welding surface in structure and its manufacturing method, the weldability of Lai Gaishan silicon target and other materials
It can so that silicon target can realize reliable combination with backboard, to meet the needs of silicon target component uses steadily in the long term.Market
For upper crystalline silicon cylinder target also by being machined to obtain to the rodlike substrate of solid polysilicon, silicon materials have cleavage surface, mechanical
Process can generate higher breakage, increase cost.In addition, the pyroprocess that machining generates is introduced to silicon target
It stains, reduces the purity of silicon target.
And lifting production crystalline silicon cylinder target is carried out using seed crystal silicon cylinder, since crystalline silicon cylinder is former for silicon during lifting
Expect that the disturbance of melt is larger, causes manufactured crystalline silicon cylinder target yields lower.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of optical isolation and its calibration method with calibration function,
The deficiencies in the prior art are able to solve, the yields of czochralski method production crystalline silicon cylinder target is improved.
In order to solve the above technical problems, the technical solution used in the present invention is as follows.
A kind of two-pack chamber single-crystal si cylinder growth furnace, including main chamber, main chamber are connected with vacuum pump, are equipped with crucible in main chamber,
The top of main chamber is symmetrical arranged there are two the concubine being connected to main chamber, and main chamber's inner surface is equipped with heating device；It is logical at the top of concubine
It crosses turntable and lifting motor is installed, lifting motor is connected with clamping device by lifting line, and gripper mechanism grips have seed crystal silicon cylinder,
Concubine bottom is equipped with guide shell, and cooling water-circulating pipe is provided in guide shell.
Preferably, the heating device include main chamber bottom surface rectangular array arrangement several primary heaters and
Several secondary heaters of main chamber's side wall annular arrangement.
Preferably, the main chamber bottom surface is provided with several lifting platforms, one first is equipped at the top of each lifting platform
Heater, the quantity of lifting platform are less than the quantity of primary heater quantity.
Preferably, being connected with a reflecting plate at the top of each secondary heater.
Preferably, the outer wall of the cooling water-circulating pipe is evenly arranged with several flanges, the medial surface setting of flange
There is flow deflector.
Preferably, the cooling water-circulating pipe axle center is provided with water conservancy diversion helix tube.
A kind of monocrystalline silicon growing method of above-mentioned two-pack chamber single-crystal si cylinder growth furnace, comprising the following steps:
A, it feeds
Silicon raw material is put into crucible；
B, it melts
Starting vacuum pump vacuumizes, and is maintained at main chamber pressure power less than 5Pa, opens heating device and is heated, and keeps silicon former
Material fusing；
C, steady temperature
Heating power is reduced after silicon raw material is fused into liquid, keep constant main chamber's temperature and is maintained；
D, seeding
Decline seed crystal silicon cylinder, seed crystal silicon cylinder and silicon raw material liquid level distance is made to be maintained at 3~5mm, seed crystal silicon cylinder is carried out pre-
Heat；Then seed crystal silicon cylinder is immersed in silicon raw material melt, then seed crystal silicon cylinder is lifted, pull rate 1.75mm/
min；
E, shouldering
Seed crystal silicon cylinder pull rate is controlled in 0.6mm/min, the conical shoulder knot of the monocrystalline silicon tubular grown is made
Structure；
F, turn shoulder
When silicon cylinder diameter increases the 80% of setting diameter, seed crystal silicon cylinder pull rate is controlled in 0.75mm/min, together
When rotate seed crystal silicon cylinder, the revolving speed of seed crystal silicon cylinder is 5rpm；
G, isodiametric growth
When silicon cylinder diameter increases setting diameter, seed crystal silicon cylinder pull rate is controlled in 0.5mm/min, seed crystal silicon cylinder
Revolving speed is 10rpm；The heated condition for adjusting heating device makes the thermal field of silicon raw material melt keep following state,
Axial temperature variation curve meets in crucible,
Wherein z > 0, k are the reality apart from the position silicon raw material liquid level 10cm
When coordinate value；
Radial temperature change meets the following conditions in crucible,
Form symmetrical round temperature gradient field centered on the axis of two seed crystal silicon cylinders, round temperature gradient field it is straight
Diameter is greater than 3 times of silicon cylinder setting diameter, and round temperature gradient field is y=0.1x by the change of gradient function at center to edge；
H, it finishes up
Seed crystal silicon cylinder pull rate is controlled in 1.5mm/min, blowing out is put off when length reaches setting value.
Preferably, when starting to adjust seed crystal silicon cylinder pull rate, pull rate adjustment process is divided into step G
Three phases, each stage are adjusted pull rate using identical percentage speed variation, kept between adjacent phases 40s~
The off time of 60s.
Preferably, in the adjusting stage of each pull rate, the revolving speed of seed crystal silicon cylinder is reduced to 1rpm in step G.
Brought beneficial effect is by adopting the above technical scheme: the present invention is passed through by the structure of improvement growth furnace
Guide shell with cooling device accurately controls the temperature of lifting crystallization process, while cooperating to the excellent of crucible temperature field
Change, realizes the synchronous pulling growth of the monocrystalline silicon of two-pack room, improve production efficiency.The structure of cooling water-circulating pipe can be mentioned effectively
The heat exchanger effectiveness and the uniformity of high cooling water.Thermal field design in crucible has fully considered hollow monocrystalline silicon cylinder to thermal field
It influences, using three dimensional temperature control method, reduces influence of the monocrystalline silicon cylinder to lifting crystallization process.In the isodiametric growth stage, lead to
It crosses and changes traditional pull rate control mode, reduce interference of the velocity variations to raw material liquid level.More it is essential that this hair
In bright change conventional method by way of stopping rotating and reducing liquid fluctuating, using the low speed rotation of seed crystal silicon cylinder, effectively drop
The low fluctuation of raw material liquid level.The present invention improves and crucible thermal field is regulated and controled by advanced optimizing the structure of heating device
Precision.The present invention of optimal control due to to(for) thermal field in crucible and liquid level does not need to carry out crucible during lifting
Promote operation, so that crucible, which is omitted, rises device, reduce equipment cost, avoid crucible rise process to the interference of raw material liquid level and
Bring difficulty is controlled to thermal field.
Detailed description of the invention
Fig. 1 is the growth furnace structure chart of a specific embodiment of the invention.
Fig. 2 is the structure chart of cooling water-circulating pipe in a specific embodiment of the invention.
Specific embodiment
Referring to Fig.1-2, a specific embodiment of the invention includes main chamber 1, and main chamber 1 is connected with vacuum pump 2, in main chamber 1
Crucible 3 is installed, the top of main chamber 1 is symmetrical arranged there are two the concubine 4 being connected to main chamber 1, and 1 inner surface of main chamber is equipped with heating
Device 5；Lifting motor 6 is equipped with by turntable 19 at the top of concubine 4, lifting motor 6 is connected with clamping device 8 by lifting line 7,
Clamping device 8 is clamped with seed crystal silicon cylinder 9, and 4 bottom of concubine is equipped with guide shell 10, cooling water-circulating pipe is provided in guide shell 10
11.Heating device 5 includes in several primary heaters 12 of 1 bottom surface rectangular array of main chamber arrangement and in 1 side wall of main chamber annular
Several secondary heaters 13 of arrangement.1 bottom surface of main chamber is provided with several lifting platforms 14, is equipped at the top of each lifting platform 14
One primary heater 12, the quantity of lifting platform 14 are less than the quantity of 12 quantity of primary heater.Each secondary heater 13
Top is connected with a reflecting plate 15.The outer wall of cooling water-circulating pipe 11 is evenly arranged with several flanges 16, flange 16 it is interior
Side is provided with flow deflector 17.Cooling 11 axle center of water-circulating pipe is provided with water conservancy diversion helix tube 18.
A kind of monocrystalline silicon growing method of above-mentioned two-pack chamber single-crystal si cylinder growth furnace, comprising the following steps:
A, it feeds
Silicon raw material is put into crucible 3；
B, it melts
Starting vacuum pump 2 vacuumizes, and is maintained at main chamber pressure power less than 5Pa, opens heating device 5 and is heated, makes silicon
Melting sources；
C, steady temperature
Heating power is reduced after silicon raw material is fused into liquid, keep constant main chamber's temperature and is maintained；
D, seeding
Decline seed crystal silicon cylinder 9, seed crystal silicon cylinder 9 and silicon raw material liquid level distance is made to be maintained at 3~5mm, seed crystal silicon cylinder 9 is carried out
Preheating；Then seed crystal silicon cylinder 9 is immersed in silicon raw material melt, then seed crystal silicon cylinder 9 is lifted, pull rate is
1.75mm/min；9 diameter of seed crystal silicon cylinder is 4 inches to 8 inches, and width is 1 millimeter to 20 millimeters；
E, shouldering
9 pull rate of seed crystal silicon cylinder is controlled in 0.6mm/min, the conical shoulder knot of the monocrystalline silicon tubular grown is made
Structure；
F, turn shoulder
When silicon cylinder diameter increases the 80% of setting diameter, 9 pull rate of seed crystal silicon cylinder is controlled in 0.75mm/min, together
When rotate seed crystal silicon cylinder 9, the revolving speed of seed crystal silicon cylinder 9 is 5rpm；
G, isodiametric growth
When silicon cylinder diameter increases setting diameter, 9 pull rate of seed crystal silicon cylinder is controlled in 0.5mm/min, seed crystal silicon cylinder 9
Revolving speed be 10rpm；The heated condition for adjusting heating device 5 makes the thermal field of silicon raw material melt keep following state,
Axial temperature variation curve meets in crucible 3,
Wherein z > 0, k are the reality apart from the position silicon raw material liquid level 10cm
When coordinate value；
Radial temperature change meets the following conditions in crucible 3,
Symmetrical round temperature gradient field is formed centered on the axis of two seed crystal silicon cylinders 9, round temperature gradient field
Diameter is greater than 3 times of silicon cylinder setting diameter, and round temperature gradient field is y=0.1x by the change of gradient function at center to edge；
H, it finishes up
9 pull rate of seed crystal silicon cylinder is controlled in 1.5mm/min, blowing out is put off when length reaches setting value.
In step G, when starting to adjust seed crystal silicon 9 pull rate of cylinder, pull rate adjustment process is divided into three phases,
Each stage is adjusted pull rate using identical percentage speed variation, and the gap of 40s~60s is kept between adjacent phases
Time.
In step G, in the adjusting stage of each pull rate, the revolving speed of seed crystal silicon cylinder 9 is reduced to 1rpm.
When adjusting axial temperature in crucible 3, the reflection angle by changing reflecting plate 15 is realized to temperature axial in crucible 3
The fine tuning of degree.When adjusting radial temperature in crucible 3, the height by changing different lifting platforms 14 is realized to radial in crucible 3
The fine tuning of temperature.
Up to 99.9999%, yields can be promoted the purity for the monocrystalline silicon cylinder target that the present invention produces from less than 30%
To 80% or more.
In the description of the present invention, it is to be understood that, term " longitudinal direction ", " transverse direction ", "upper", "lower", "front", "rear",
The orientation or positional relationship of the instructions such as "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outside" is based on attached drawing institute
The orientation or positional relationship shown is merely for convenience of the description present invention, rather than the device or element of indication or suggestion meaning must
There must be specific orientation, be constructed and operated in a specific orientation, therefore be not considered as limiting the invention.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (9)
1. a kind of two-pack chamber single-crystal si cylinder growth furnace, including main chamber (1), main chamber (1) are connected with vacuum pump (2), peace in main chamber (1)
Equipped with crucible (3), it is characterised in that: the top of main chamber (1) is arranged symmetrically, and there are two the concubine (4) being connected to main chamber (1), main chambers
(1) inner surface is equipped with heating device (5)；Lifting motor (6) is installed by turntable (19) at the top of concubine (4), lifts motor
(6) it is connected with clamping device (8) by lifting line (7), clamping device (8) is clamped with seed crystal silicon cylinder (9), concubine (4) bottom peace
Equipped with guide shell (10), cooling water-circulating pipe (11) are provided in guide shell (10).
2. two-pack chamber single-crystal si cylinder growth furnace according to claim 1, it is characterised in that: the heating device (5) includes
In several primary heaters (12) of main chamber (1) bottom surface rectangular array arrangement and in the several of main chamber (1) side wall annular arrangement
A secondary heater (13).
3. two-pack chamber single-crystal si cylinder growth furnace according to claim 2, it is characterised in that: main chamber (1) the bottom surface setting
There are several lifting platforms (14), a primary heater (12), the number of lifting platform (14) are installed at the top of each lifting platform (14)
Amount is less than the quantity of primary heater (12) quantity.
4. two-pack chamber single-crystal si cylinder growth furnace according to claim 3, it is characterised in that: each secondary heater (13)
Top is connected with a reflecting plate (15).
5. two-pack chamber single-crystal si cylinder growth furnace according to claim 1, it is characterised in that: the cooling water-circulating pipe (11)
Outer wall be evenly arranged with several flanges (16), the medial surface of flange (16) is provided with flow deflector (17).
6. two-pack chamber single-crystal si cylinder growth furnace according to claim 5, it is characterised in that: the cooling water-circulating pipe (11)
Axle center is provided with water conservancy diversion helix tube (18).
7. a kind of monocrystalline silicon growing method of two-pack chamber single-crystal si cylinder growth furnace as claimed in any one of claims 1 to 6, special
Sign be the following steps are included:
A, it feeds
Silicon raw material is put into crucible (3)；
B, it melts
Starting vacuum pump (2) vacuumizes, and is maintained at main chamber pressure power less than 5Pa, opens heating device (5) and is heated, makes silicon
Melting sources；
C, steady temperature
Heating power is reduced after silicon raw material is fused into liquid, keep constant main chamber's temperature and is maintained；
D, seeding
Decline seed crystal silicon cylinder (9), make seed crystal silicon cylinder (9) and silicon raw material liquid level distance is maintained at 3~5mm, to seed crystal silicon cylinder (9) into
Row preheating；Then seed crystal silicon cylinder (9) is immersed in silicon raw material melt, then seed crystal silicon cylinder (9) is lifted, pull rate is
1.75mm/min；
E, shouldering
Seed crystal silicon cylinder (9) pull rate is controlled in 0.6mm/min, the conical shoulder knot of the monocrystalline silicon tubular grown is made
Structure；
F, turn shoulder
When silicon cylinder diameter increases the 80% of setting diameter, seed crystal silicon cylinder (9) pull rate is controlled in 0.75mm/min, simultaneously
It rotates seed crystal silicon cylinder (9), the revolving speed of seed crystal silicon cylinder (9) is 5rpm；
G, isodiametric growth
When silicon cylinder diameter increases setting diameter, seed crystal silicon cylinder (9) pull rate is controlled in 0.5mm/min, seed crystal silicon cylinder (9)
Revolving speed be 10rpm；The heated condition for adjusting heating device (5) makes the thermal field of silicon raw material melt keep following state,
Axial temperature variation curve meets in crucible (3),
Wherein z > 0, k are the real-time seat apart from the position silicon raw material liquid level 10cm
Scale value；
Radial temperature change meets the following conditions in crucible (3),
Form symmetrical round temperature gradient field centered on the axis of two seed crystal silicon cylinders (9), round temperature gradient field it is straight
Diameter is greater than 3 times of silicon cylinder setting diameter, and round temperature gradient field is y=0.1x by the change of gradient function at center to edge；
H, it finishes up
Seed crystal silicon cylinder (9) pull rate is controlled in 1.5mm/min, blowing out is put off when length reaches setting value.
8. the monocrystalline silicon growing method of two-pack chamber single-crystal si cylinder growth furnace according to claim 7, it is characterised in that: step
In G, when starting to adjust seed crystal silicon cylinder (9) pull rate, pull rate adjustment process is divided into three phases, each stage adopts
Pull rate is adjusted with identical percentage speed variation, the off time of 40s~60s is kept between adjacent phases.
9. the monocrystalline silicon growing method of two-pack chamber single-crystal si cylinder growth furnace according to claim 8, it is characterised in that: step
In G, in the adjusting stage of each pull rate, the revolving speed of seed crystal silicon cylinder (9) is reduced to 1rpm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910561717.6A CN110129879A (en) | 2019-06-26 | 2019-06-26 | A kind of two-pack chamber single-crystal si cylinder growth furnace and monocrystalline silicon growing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910561717.6A CN110129879A (en) | 2019-06-26 | 2019-06-26 | A kind of two-pack chamber single-crystal si cylinder growth furnace and monocrystalline silicon growing method |
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| Publication Number | Publication Date |
|---|---|
| CN110129879A true CN110129879A (en) | 2019-08-16 |
Family
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| CN201910561717.6A Pending CN110129879A (en) | 2019-06-26 | 2019-06-26 | A kind of two-pack chamber single-crystal si cylinder growth furnace and monocrystalline silicon growing method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111826709A (en) * | 2020-08-21 | 2020-10-27 | 井兵涛 | Czochralski method monocrystalline silicon growth furnace |
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Application publication date: 20190816 |