CN202744653U - Graphite crucible for preparing single crystal silicon by adopting Czochralski method - Google Patents

Graphite crucible for preparing single crystal silicon by adopting Czochralski method Download PDF

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Publication number
CN202744653U
CN202744653U CN 201220439456 CN201220439456U CN202744653U CN 202744653 U CN202744653 U CN 202744653U CN 201220439456 CN201220439456 CN 201220439456 CN 201220439456 U CN201220439456 U CN 201220439456U CN 202744653 U CN202744653 U CN 202744653U
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China
Prior art keywords
plumbago crucible
single crystal
graphite crucible
silicon single
crucible body
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CN 201220439456
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Chinese (zh)
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薛东
李德建
陈昌林
陈锐
陈剑春
付雁清
李福龙
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SHANGHAI JMS ELECTRONIC MATERIALS CO Ltd
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SHANGHAI JMS ELECTRONIC MATERIALS CO Ltd
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Abstract

The utility model discloses a graphite crucible for preparing a single crystal silicon by adopting the Czochralski method. The graphite crucible comprises a graphite crucible body consisting of a bottom and a side wall, wherein concave threaded gas guiding gutters are uniformly distributed on the outer surface of the side wall of the graphite crucible body, and an inclined included angle is formed between the threaded gas guiding gutters and the horizontal plane; the graphite crucible body comprises an inner bottom surface and an inner side surface which together define the internal capacity, as well as an outer bottom surface and an outer side surface which together define the heat transfer area; the shape of the inner bottom surface of the graphite crucible body adapts to that of the bottom of the graphite crucible body; the inner side surface is parallel to the central axis of the graphite crucible; the inner bottom surface is spherically arc-shaped, and the radius of the radian is R1; the inner bottom surface and the inner side surface are in spherically arc connection, and the radius of the radian is R2; and R1 is larger than or equal to R2. The graphite crucible further improves the airflow guiding in the crystal pulling process, so that the exhaust is smoother; and besides, the thermal conductivity of the crucible is enhanced and the thermal-field temperature control stability is optimized.

Description

A kind of vertical pulling method prepares the employed plumbago crucible of silicon single crystal
Technical field
The utility model relates to a kind of plumbago crucible, and especially a kind of vertical pulling method prepares the employed plumbago crucible of silicon single crystal.
Background technology
Current preparation silicon single crystal is mainly by two kinds of technology, and is different according to crystal growth pattern, can be divided into study on floating zone silicon and pulling of silicon single crystal.Pulling of silicon single crystal is mainly used in microelectronic integrated circuit and solar cell aspect, is the main body of silicon single crystal.
Vertical pulling method is to use the condensation-crystallization driving principle of melt, at the solid-liquid interface place, descends by melt temperature, changes solid-state phase change with producing into by liquid rotating.For the silicon single crystal rod of growth quality qualified (single crystal silicon resistivity, oxygen level and oxygen concn distribution, carbon content, metals content impurity, defective etc.), when adopting Grown by CZ Method, must consider following problem.At first be according to technical requirements, secondly the single crystal growth apparatus that choice for use is suitable is preparation technology, the technology of a whole set of silicon single crystal of GPRS, comprising: the intrasystem thermal field design of (1) silicon single crystal, guarantee that the crystal growth has the thermograde of reasonably stability; (2) monocrystalline silicon growing 1 intrasystem argon gas system design; (3) silicon single crystal is seized the design of technological system on both sides by the arms; (4) for the design of the continuous charging system that enhances productivity; (5) silicon single crystal preparation technology's process control.
The transmission of heat is by three kinds of Main Patterns, that is radiation, convection current and thermal conduction.Because the growth of crystal is at high temperature to carry out, so these three kinds of patterns all are present in the system.In vertical pulling method, melt is to be heated by the radiant heat of graphite heater, and the thermal conduction of melt inside then is mainly against convection current, and the heat of crystal bar inside is transmitted mainly against conduction.In addition, being lost to peripheral heat from liquid level and crystal bar surface then is by radiation effect.Intrasystem temperature distribution has a great impact the crystal growth quality.Comprise precipitate generation of the density of defective and distribution, oxygen etc.
The growth interface of the silicon crystal in the CZ method is upwards expansion (along crystal growth direction) normally, so, its inner bottom surface of the quartz crucible that holds the silicon material commonly used is spherical or arcuation, quartz crucible places in the plumbago crucible, the inner bottom surface of plumbago crucible is the spherical or arcuation that adapts, and the crucible outer bottom is also made adapt spherical.During the preparation silicon seed, heater element by the crucible side provides thermal source, cause the temperature outside of melt higher than central shaft, the melt bottom is higher than liquid level temperature, because the density of silicon material increases with temperature and reduces, therefore the melt of bottom can up flow by buoyancy, and the preparation system is carried out heat exchange by the heating unit of plumbago crucible wall and both sides, and the plumbago crucible wall radiating effect of arcuation is not ideal.Because existing plumbago crucible is simple in structure, exist the shortcomings such as heat transfer efficiency is low, heating is slow, heat-up time is long, energy consumption is high; In addition, can produce gas in the preparation process of silicon, condensing into liquid after the gas chance is cold can flow to along the bottom surface of arc on the collet of plumbago crucible, causes at last plumbago crucible and collet adhesion.Reduce the work-ing life of crucible, be unfavorable for the production of silicon single crystal.
In view of this spy proposes the utility model.
The utility model content
The technical problems to be solved in the utility model is to overcome the deficiencies in the prior art, provide a kind of vertical pulling method to prepare the plumbago crucible of the threaded shape gas flow guiding of the employed sidewall outside surface of silicon single crystal groove, make it have more preferably heat transfer property, and optimize the temperature of thermal field control stiffness, improve the air-flow guiding in the crystal pulling process, so that exhaust is more smooth and easy.
For solving the problems of the technologies described above, the utility model adopts the basic conception of technical scheme to be: a kind of vertical pulling method prepares the employed plumbago crucible of silicon single crystal, comprise the plumbago crucible body that is formed by bottom and sidewall, described plumbago crucible body sidewall outside surface is evenly distributed with the shape of threads gas flow guiding groove of indent, has 20 °~70 ° slanted angle between shape of threads gas flow guiding groove and the horizontal plane.
Described shape of threads gas flow guiding groove is spaced apart 2~10mm, and shape of threads gas flow guiding well width is 2~10mm, and the degree of depth is less than 10mm.
Preferably, the slanted angle between described shape of threads gas flow guiding groove and the horizontal plane is 35 °~55 °.
According to the upgrowth situation of monocrystalline, need suitable intensification or cooling to allow the monocrystalline smooth growth in the process of preparation silicon single crystal, the heat conductivility that improves plumbago crucible is extremely important.After increasing the crucible surface screw thread, increased heat transfer area, improved heat conduction velocity, will more effectively reach steadily the control of temperature of thermal field like this.In the material process, can absorb faster well heater for the heat that reaches, material speed is accelerated; Cooling and stabilization process can be dispelled the heat faster, make temperature can drop to faster target temperature.
Described shape of threads gas flow guiding groove sense of rotation is left-handed or dextrorotation.The direction of rotation is left-handed or dextrorotation can set determine according to equipment and the crystal pulling technique of collocation, single crystal growing furnace intake and exhaust position for example, plumbago crucible sense of rotation etc.When plumbago crucible rotated, the monocrystalline furnace gas can accelerate under the promotion of shape of threads gas flow guiding groove downwards, so just so that the interior exhaust of stove is more smooth and easy, reduced the accumulation of oxide compound, made crystal forming rate higher.
Described plumbago crucible body comprises inner bottom surface, the medial surface that limits internal capacity and outer bottom, the outer side that limits heat transfer area, the shape of the inner bottom surface shape of plumbago crucible body and quartz crucible bottom adapts, wherein, outer side, medial surface all with the central axes of plumbago crucible, inner bottom surface is the ball arcuation, and radius of the radian is R1, is connected for spherical arc shape between inner bottom surface and the medial surface, radius of the radian is R2, and described R1 is more than or equal to R2.
Described plumbago crucible body sidewall is comprised of at least two identical side member; Plumbago crucible body bottom is an individual configurations independently, perhaps is comprised of the bottom part identical with side member quantity, and each bottom part is corresponding to be integrated with each side member.
In order to make things convenient for picking and placeing and clearing up of plumbago crucible, plumbago crucible is generally made by at least three identical many lobes crucibles that are made of bottom and side member.Plumbago crucible body sidewall described in the utility model comprises three or four identical side member.
Change in addition plumbago crucible base side wall thickness and bottom thickness all there is impact in the thermal conduction effect of plumbago crucible, because plumbago crucible body bottom is the ball arcuation, sidewall is also with the bottom that arc is spherical to be connected, therefore the thickness of sidewall and bottom is a numerical range, through experiment, when finding that ratio range when plumbago crucible base side wall thickness and bottom thickness is 1:3~3:1, the heat conductivility of plumbago crucible is more satisfactory, when ratio range is 1:2~2:1, best results.
After adopting technique scheme, the utility model compared with prior art has following beneficial effect.
The utility model is provided with shape of threads gas flow guiding groove at plumbago crucible sidewall outside surface, can be so that the thermal field exhaust be the eddy current shape, and exhaust is more smooth and easy, reduces the accumulation of oxide compound, makes crystal forming rate higher; Experiment shows, in the situation that this structure auxiliary improvement air-flow, keeps pressing in the equal crystal pulling furnace, and the gas output is many 6%~10%, and crystal forming rate has 2%~3% raising.
In addition, shape of threads gas flow guiding groove has increased the heat transfer area of plumbago crucible outside surface relatively, has improved heat conduction velocity, will more effectively reach steadily the control of temperature of thermal field like this; Experimental data shows, in the situation that strict controlled working technology, increase shows that screw thread is on the not obviously impact of crucible life-span itself; The material time shorten 4%~6%; Because temperature control is more accurate, crystal forming rate has 1%~2% raising relatively.
Below in conjunction with accompanying drawing embodiment of the present utility model is described in further detail.
Description of drawings
Fig. 1 is the utility model graphite crucible structure schematic diagram;
Fig. 2 be among Fig. 1 plumbago crucible A to schematic diagram;
Fig. 3 is the local enlarged diagram in B place among Fig. 2;
Fig. 4 is the utility model plumbago crucible body bottom schematic view.
Embodiment
As shown in Figures 1 to 4, plumbago crucible described in the utility model, comprise the plumbago crucible body 1 that is formed by bottom 11 and sidewall 12, described plumbago crucible body sidewall 12 outside surfaces are evenly distributed with the shape of threads gas flow guiding groove 2 of indent, has slanted angle α between shape of threads gas flow guiding groove 2 and the horizontal plane, α is 20 °~70 °, is preferably 35 °~55 °; Shape of threads gas flow guiding groove 2 interval L1 are 2~10mm, and shape of threads gas flow guiding well width L2 is 2~10mm, and degree of depth L3 consults Fig. 3 less than 10mm(), the ratio range of plumbago crucible body sidewall 12 thickness and bottom 11 thickness is 1:3~3:1.
Described shape of threads gas flow guiding groove 2 sense of rotation are left-handed or dextrorotation.The direction of rotation is left-handed or dextrorotation can set determine according to equipment and the crystal pulling technique of collocation, single crystal growing furnace intake and exhaust position for example, plumbago crucible sense of rotation etc.When plumbago crucible rotated, the monocrystalline furnace gas can accelerate under the promotion of shape of threads gas flow guiding groove downwards, so just so that the interior exhaust of stove is more smooth and easy, reduced the accumulation of oxide compound, made crystal forming rate higher.As shown in Figure 1, the sense of rotation of shape of threads gas flow guiding groove 2 is left-handed.
Described plumbago crucible body 1 comprises inner bottom surface D11, the medial surface D12 that limits internal capacity and outer bottom C11, the outer side C12 that limits heat transfer area, and outer bottom C11 is mutually vertical with outer side C12; The medial surface D12 of plumbago crucible body and vertical central axes, inner bottom surface D11 is the ball arcuation, and radius of the radian is R1, and for spherical arc shape is connected, radius of the radian is R2 between inner bottom surface D11 and the medial surface D12, and R1 is greater than R2.
Described plumbago crucible body sidewall 12 is comprised of at least two identical side member 13; Plumbago crucible body bottom 11 is an individual configurations independently, perhaps is comprised of the bottom part identical with side member quantity, and each bottom part is corresponding to be integrated with each side member.
Embodiment one
This slanted angle α that implements between described shape of threads gas flow guiding groove 2 and the horizontal plane is 35 °~55 °, and shape of threads gas flow guiding groove 2 interval L1 are 3~6mm, and shape of threads gas flow guiding well width L2 is 4~8mm, and degree of depth L3 is 2~5mm.
The ratio range of described plumbago crucible body bottom 11 thickness and sidewall 12 thickness is 1:2~2:1.
Embodiment two
This slanted angle α that implements between described shape of threads gas flow guiding groove 2 and the horizontal plane is 40 °~50 °, and shape of threads gas flow guiding groove 2 interval L1 are 4~6mm, and shape of threads gas flow guiding well width L2 is 5~8mm, and degree of depth L3 is 3~6mm.
The ratio range of described plumbago crucible body bottom 11 thickness and sidewall 12 thickness is 1:2~1:1.
Embodiment three
The described plumbago crucible body of the present embodiment is two lobe crucibles, comprises two identical graphite crucible assembles, and every graphite crucible assemble is integrally formed structure by bottom part and side member.
Embodiment four
The described plumbago crucible body of the present embodiment is three lobe crucibles, comprises three identical graphite crucible assembles, and every graphite crucible assemble is integrally formed structure by bottom part and side member.
Embodiment five
The difference of the present embodiment and embodiment four is: described plumbago crucible body bottom is one independently whole (consulting Fig. 1 and Fig. 2).
Embodiment six
The described plumbago crucible body of the present embodiment is the pintongs crucible, comprises independently plumbago crucible body bottom of the plumbago crucible body sidewall and that is made of four same side wall components.
Embodiment seven
The described shape of threads gas flow guiding of the present embodiment groove sense of rotation is dextrorotation, and other conditions are with above-mentioned embodiment.
Embodiment in above-described embodiment can further make up or replace; and embodiment is described preferred embodiment of the present utility model; be not that design of the present utility model and scope are limited; under the prerequisite that does not break away from the utility model design philosophy; the various changes and modifications that the professional and technical personnel makes the technical solution of the utility model in this area all belong to protection domain of the present utility model.

Claims (9)

1. a vertical pulling method prepares the employed plumbago crucible of silicon single crystal, comprise the plumbago crucible body that is formed by bottom and sidewall, it is characterized in that: described plumbago crucible body sidewall outside surface is evenly distributed with the shape of threads gas flow guiding groove of indent, has 20 °~70 ° slanted angle between shape of threads gas flow guiding groove and the horizontal plane.
2. a kind of vertical pulling method according to claim 1 prepares the employed plumbago crucible of silicon single crystal, it is characterized in that: described shape of threads gas flow guiding groove is spaced apart 2~10mm, and shape of threads gas flow guiding well width is 2~10mm, and the degree of depth is less than 10mm.
3. a kind of vertical pulling method according to claim 1 and 2 prepares the employed plumbago crucible of silicon single crystal, it is characterized in that: the slanted angle between described shape of threads gas flow guiding groove and the horizontal plane is 35 °~55 °.
4. a kind of vertical pulling method according to claim 1 prepares the employed plumbago crucible of silicon single crystal, it is characterized in that: described shape of threads gas flow guiding groove sense of rotation is left-handed or dextrorotation.
5. a kind of vertical pulling method according to claim 1 prepares the employed plumbago crucible of silicon single crystal, it is characterized in that: described plumbago crucible body comprises inner bottom surface, the medial surface that limits internal capacity and outer bottom, the outer side that limits heat transfer area, wherein, the central axes of medial surface and plumbago crucible, inner bottom surface is the ball arcuation, and radius of the radian is R1, is connected for spherical arc shape between inner bottom surface and the medial surface, radius of the radian is R2, and described R1 is more than or equal to R2.
6. a kind of vertical pulling method according to claim 1 prepares the employed plumbago crucible of silicon single crystal, it is characterized in that: described plumbago crucible body sidewall is comprised of at least two identical side member; Plumbago crucible body bottom is an individual configurations independently, perhaps is comprised of the bottom part identical with side member quantity, and each bottom part is corresponding to be integrated with each side member.
7. a kind of vertical pulling method according to claim 6 prepares the employed plumbago crucible of silicon single crystal, it is characterized in that: described plumbago crucible body sidewall comprises three or four identical side member.
8. a kind of vertical pulling method according to claim 1 prepares the employed plumbago crucible of silicon single crystal, it is characterized in that: the ratio range of described plumbago crucible body bottom thickness and sidewall thickness is 1:3~3:1.
9. a kind of vertical pulling method according to claim 8 prepares the employed plumbago crucible of silicon single crystal, it is characterized in that: the ratio range of described plumbago crucible body bottom thickness and sidewall thickness is 1:2~2:1.
CN 201220439456 2012-08-30 2012-08-30 Graphite crucible for preparing single crystal silicon by adopting Czochralski method Expired - Fee Related CN202744653U (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103668438A (en) * 2012-08-30 2014-03-26 上海杰姆斯电子材料有限公司 Graphite crucible used for preparing monocrystalline silicon by czochralski method
WO2016000617A1 (en) * 2014-07-02 2016-01-07 攀时(上海)高性能材料有限公司 Crucible for crystal cultivation
CN108396373A (en) * 2018-04-20 2018-08-14 周俭 A kind of monocrystalline silica crucible
CN108396372A (en) * 2018-04-20 2018-08-14 周俭 A kind of monocrystalline silica crucible
CN108624951A (en) * 2018-04-20 2018-10-09 周俭 A kind of monocrystalline silica crucible

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103668438A (en) * 2012-08-30 2014-03-26 上海杰姆斯电子材料有限公司 Graphite crucible used for preparing monocrystalline silicon by czochralski method
WO2016000617A1 (en) * 2014-07-02 2016-01-07 攀时(上海)高性能材料有限公司 Crucible for crystal cultivation
CN108396373A (en) * 2018-04-20 2018-08-14 周俭 A kind of monocrystalline silica crucible
CN108396372A (en) * 2018-04-20 2018-08-14 周俭 A kind of monocrystalline silica crucible
CN108624951A (en) * 2018-04-20 2018-10-09 周俭 A kind of monocrystalline silica crucible

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Granted publication date: 20130220

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