EP3234232A1 - Double-walled graphite funnel - Google Patents
Double-walled graphite funnelInfo
- Publication number
- EP3234232A1 EP3234232A1 EP15822925.2A EP15822925A EP3234232A1 EP 3234232 A1 EP3234232 A1 EP 3234232A1 EP 15822925 A EP15822925 A EP 15822925A EP 3234232 A1 EP3234232 A1 EP 3234232A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- funnel
- graphite
- double
- walled
- walled graphite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 174
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 151
- 239000010439 graphite Substances 0.000 title claims abstract description 151
- 239000000463 material Substances 0.000 claims abstract description 41
- 238000007789 sealing Methods 0.000 claims description 17
- 239000000945 filler Substances 0.000 claims description 13
- 241000237942 Conidae Species 0.000 claims description 6
- 230000009467 reduction Effects 0.000 claims description 4
- 239000003575 carbonaceous material Substances 0.000 claims description 3
- 239000003779 heat-resistant material Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 description 15
- 239000011810 insulating material Substances 0.000 description 12
- 235000013339 cereals Nutrition 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 4
- 238000002231 Czochralski process Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000006978 adaptation Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000009950 felting Methods 0.000 description 2
- 230000009969 flowable effect Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000007770 graphite material Substances 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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
- C30B15/14—Heating of the melt or the crystallised materials
Definitions
- the present invention relates to a double-walled graphite funnel which is filled with a free-flowing filler material. Furthermore, the present invention relates to a kit for producing the double-walled graphite funnel.
- Graphite funnels also referred to as graphite pot or graphite cone, are used in high-temperature processes.
- One such high-temperature process involves the production of single crystals by the so-called Czochralski process.
- the material to be formed into a single crystal is melted at high temperatures in a crucible, and the single crystal forming a seed crystal is pulled out of the melt.
- This process is described, for example, in "Industrial Inorganic Chemistry", M. Bertau et al., Wiley-VCH Verlag GmbH & Co. KGaA, edition 4, 24 July 2013, pages 402-403.
- the graphite funnel is placed in the Czochralski plant so that it points with its lower, lower opening in the direction of the crucible.
- the monocrystal which is pulled out of the melt through the lower opening of the funnel toward the upper opening of the funnel, is encircled and thereby shielded by the funnel walls extending between the upper and lower openings of the funnel.
- the graphite funnels used in the Czochralski process have, depending on the type of installation in which they are used, essentially the shape of a truncated cone shell, which may be modified by circumferential enlargement or reduction in size, for example bearing surfaces or engagement surfaces as retaining elements for the corresponding Plant areas can be formed or intervened in such.
- the graphite funnels are, for example, double-walled and additionally insulated.
- the graphite funnel is constructed from an inner and an outer funnel, which are designed such that the smaller funnel is fitted into the outer funnel to form a cavity. The cavity is then filled with flat insulating material.
- graphite felts are used in the state of the art as sheet-like insulating material.
- soft felts and hard felts.
- the graphite felts have a low thermal conductivity, which makes them suitable as insulating material.
- these graphite felts are disadvantageous in terms of their manufacturing costs and the ease with which they fit into the cavity of the graphite funnel.
- the graphite hard felts have to be provided precisely fitting for the corresponding cavity, which requires individual production.
- the provision of graphite hard felt usually takes place as a component according to the required adaptation to the graphite funnel.
- This custom provision of custom-fit graphite hard felts is costly due to the material cost and the cost of customization.
- the life of the graphite felts is lower than that of the graphite hopper, which means that the insulating material must be replaced during the period of operation of the graphite hopper, so that the process must be repeated.
- Object of the present invention is therefore to overcome the disadvantages of the prior art and to provide a graphite funnel, which is inexpensive, can be produced without great technical effort and is adaptable to specific requirements in terms of thermal conductivity.
- thermal conductivity is used in the context of the present application, the thermal conductivity at room temperature is to be understood, unless stated otherwise. Room temperature is understood in the context of the present application, a temperature of 20 ° C.
- Expense can be provided for the appropriate application.
- the adaptation of the thermal conductivity of the graphite funnel with little technical effort and high flexibility to different technical requirements should be possible. So it should be possible without much technical effort adapt the thermal properties of the graphite funnel to the intended use.
- the intermediate space is "filled"
- the object of the present invention is achieved by providing a double-walled graphite funnel having an upper opening and a lower opening, wherein the openings have different clearances and are arranged parallel to each other, and wherein the double-walled graphite funnel from a internal funnel and an outer funnel is formed, inner funnel and outer funnel made of graphite, the inner funnel is designed in its dimensions and its shape such that it can be accommodated in the outer funnel, the inner funnel is received in the outer funnel so in that a space is formed between the inner funnel and the outer funnel, the space adjacent to the opening having a smaller clearance is defined by a contact surface formed between the inner funnel and the outer funnel, and the space adjacent to the opening communicates with the space gr is accessible ßeren clearance from the outside, wherein the space between the inner funnel and outer funnel is filled with a flowable filler material.
- a double-walled graphite funnel in which the outer funnel has the shape of a truncated cone shell. Also preferred is a double-walled graphite funnel in which the outer funnel has substantially the shape of a truncated cone shell which deviates at its outer periphery from the truncated cone shape by circumferential reductions and / or circumferential extensions.
- a double-walled graphite funnel in which the intermediate space formed between the inner funnel and the outer funnel is closed by means of a closure arrangement.
- the closure arrangement of the double-walled graphite funnel comprises at least one graphite closure element.
- closure arrangement comprises at least one sealing element which is selected from heat-resistant materials.
- the free-flowing filling material at room temperature has a typical thermal thermal conductivity of 0.02 W / mK to 75 W / mK, preferably 0.02
- a graphite funnel in which the free-flowing filler material is selected from elemental carbon-based materials, in particular graphite grains.
- kits for producing a graphite funnel according to the invention comprising an inner funnel, an outer graphite funnel and filling material.
- a set which further comprises a closure assembly comprising at least one graphite closure element and at least one sealing element.
- the double-walled graphite funnel according to the invention has significant advantages over prior art graphite funnels.
- the use of free-flowing filling material makes it possible to evenly fill the intermediate space formed without great technical effort.
- a suitable free-flowing insulating material can be selected.
- material mixtures of free-flowing materials in order to achieve the desired thermal conductivity of the graphite funnel according to the invention.
- Flowable materials are, for example, powders, granules, cereals and mixtures thereof.
- the graphite funnel according to the invention can be additionally individualized with its insulating properties.
- Materials suitable as filling material include, for example, elemental carbon-based materials such as graphite powders or graphite grains, but also process-compatible filler materials having a typical thermal thermal conductivity at room temperature in the range from 0.02 to 50 W / mK.
- the free-flowing filler material can be an insulating material.
- the typical thermal thermal conductivity of insulating materials at room temperature ranges from 0.02 W / mK to 10 W / mK. If these materials are exposed to operating temperatures of approx. 1500 ° C, this corresponds to values of 0.08 W / mK to 40 W / mK.
- a graphite hopper according to the invention which is provided for use in a common Czochralski plant, can be filled with a graphite semolina which has a thermal conductivity which corresponds to that of graphite felts. If, for example, a graphite semolina is used as free-flowing insulating material, then the double-walled graphite funnel can be subjected to graphite purification methods known in the prior art. In this case, such a high purity can be achieved that makes the graphite funnel according to the invention also usable in the field of semiconductor technology.
- the combination according to the invention of the double-walled graphite funnel formed by the inner and outer funnels, that is to say of a graphite shaped body, and the comparatively inexpensive filling material mean that a cost-effective price level can be achieved. Due to the flexibility of the reusable filling material, a broad application for differently shaped moldings is possible.
- the graphite funnel according to the invention can also have statements and areas of the intermediate space which are difficult to access, and nevertheless also have insulation in these areas. The introduction of laminar insulating material into these areas is, if at all feasible, at least associated with great expense.
- variable combination for example, reduce drawing costs and storage of semi-finished and finished parts.
- Another assembly of parts as with the use of graphite
- the graphite hopper according to the invention can be provided as a completely assembled unit. But it can also be done providing a set from which the user composes the graphite funnel.
- Inner and outer funnels are both made of graphite. Both funnels can be constructed of identical or, if necessary, of different graphite material. If the double-walled graphite funnel according to the invention is made available to a user, the user does not have to assemble various individual parts because of the completely assembled unit. For this purpose, a suitable filling material is selected and the user receives the graphite funnel according to the invention according to his needs, for example in a suitable size and shape and with suitable thermal properties such as the typical thermal conductivity. If the double-walled graphite funnel is intended for use in the Czochralski method, the intermediate space formed between the inner and outer funnels will be filled with a free-flowing insulating material.
- the graphite hopper of the present invention may be subjected, if necessary, to the cleaning methods for graphite materials known in the art.
- the graphite funnel according to the invention can also be provided in high purity.
- the provision of the graphite funnel with closure assembly simplifies its handling.
- the closure arrangement prevents filling material from falling out of the intermediate space during transport of the graphite funnel, for example.
- This also supports the provision of the graphite funnel for use at a location other than the manufacturing site.
- the closure arrangement prevents accidentally leaking filler material during use of the graphite funnel, which could happen, for example, when tilting the graphite funnel according to the invention.
- the closure arrangement is preferably selected so that the graphite funnel according to the invention can be used without further modification after closure with the closure arrangement.
- this closure arrangement can be formed by material removal from the inner or outer funnel.
- a graphite ring can be obtained by separating an annular structure from the upper edge of the inner or outer funnel. The graphite ring is thus obtained in this embodiment, for example, that it is cut off from the inner or outer funnel.
- This embodiment is particularly advantageous because the graphite ring thereby has the required dimensions to be accurately placed back on the hopper, because funnel and graphite ring previously formed a unit.
- FIG. 3 is a three-dimensional exploded view of an embodiment of the graphite funnel 1.
- Fig. 1 an embodiment of the double-walled graphite funnel 1 according to the invention is shown as a longitudinal section.
- the inner funnel 4 and the outer funnel 3 have different shapes.
- the inner and outer funnels have essentially the shape of a truncated cone shell, wherein the shell surface Chen the two funnels have different angles of inclination in the example shown. In the lower part of the inner and outer funnel they come into contact with each other.
- fixing means are formed in this embodiment, with which the outer funnel 3 and the inner funnel 4 are fastened to each other. Shown here are as fixing a circumferential ridge 5 and a groove 6, wherein ridge 5 engages the outer funnel 3 in a groove 6 on the inner funnel 4 (spring - groove - principle).
- the gap formed by the arrangement of inner funnel 4 and outer funnel 3 is indicated by 7. Interspace 7 is filled with a free-flowing material 8.
- the closure assembly comprises in this embodiment, in addition to a graphite closure element, here a graphite ring 9, and two sealing elements 10 and 1 first Seal member 10 is annular, seal member 1 1 is in this embodiment, a strip-shaped element which is arranged in a ring.
- the sealing elements are arranged between the inner funnel 4 and the outer funnel 3 and consist, for example, of graphite felt.
- the graphite closure element formed as a graphite ring 9 was originally part of the inner funnel 4.
- the closure arrangement 13 can be fixed by means on the double-walled graphite funnel 1 according to the invention, for example by at least one connecting means 2 such as a pin being introduced through the closure arrangement 13 into the upper edge of the outer funnel 3.
- This connecting means 2 is preferably a connecting means which can be removed without damaging the double-walled graphite hopper 1. Thereby, the closure assembly 13 of the filled graphite funnel 1 can be removed and the filler material exchanged or filled.
- the use of a closure assembly 13 is advantageous to ensure that during the handling of the graphite funnel according to the invention or during its transport no filling material emerges.
- closure assembly shown in this embodiment is merely exemplary and closure assembly without sealing members or with more than two sealing members may also be used.
- an outer funnel 3 which does not deviate from the truncated cone shape by circumferential reductions or circumferential extensions.
- circumferential deviations may be required depending on the type of installation for which the double-walled graphite funnel 1 according to the invention is provided.
- FIG. 2 shows a detailed view of the closure arrangement 13 with two sealing elements, namely graphite felt upper ring 10 and graphite felt insert 11, which are arranged between the inner funnel 3 and the outer funnel 4.
- the conclusion forms graphite closure element, here a graphite ring 9.
- Fig. 3 shows a three-dimensional exploded view of an embodiment of the double-walled graphite funnel 1 according to the invention. Shown is how the inner hopper 4 is received in the outer hopper 3 and the sealing elements 10 and 1 1 between the outer hopper 3 and inner hopper 4 are arranged. Above the funnels 3 and 4, graphite ring 9 is shown.
- the production takes place by shaping methods known in the art, namely turning and milling. Since the double-walled graphite funnel according to the invention is provided for differently dimensioned and differently constructed systems, ie, for example, different Czochralski systems, variants in different sizes and diverse designs are made available. The example described below only explains one possible embodiment of the double-walled graphite funnel according to the invention and should not be understood as limiting the invention to this exemplary embodiment.
- An outer hopper 3 and an inner hopper 4 were made of graphite semi-finished product.
- the inner funnel 4 has an upper diameter of 480mm and a lower diameter of 220mm.
- the height of the inner funnel 4 is 309mm in this embodiment.
- the outer funnel 3 has an upper diameter of 500mm and a lower diameter of 328mm.
- the height of the outer funnel 3 is 309mm.
- Inner funnel 4 and outer funnel 3 have the shape of a truncated cone shell, differing in the angle formed between the respective generatrix and truncated cone axis.
- the filling material 8 used is a graphite semolina which can be obtained from SGL Carbon GmbH and has the following properties:
- the thermal conductivity is determined appropriately with the so-called Hot Disk ⁇ method.
- This is a disc-shaped sensor element, the eponymous Hot Disk ⁇ , which consists of a conductor spiral and the is electrically insulated, introduced into the bed - here the Graphitgrello-.
- the sensor is heated electrically and the temperature increase is recorded over time.
- the sensor is also a heating element and resistance thermometer.
- the heat conductivity can be calculated from the recorded measurement data.
- this material is exemplary only, other filler materials may be used, such as other graphite grains.
- the filling of the gap 7 with the graphite semolina occurs by pouring without inert gas.
- compacting of the powder or granulate will be carried out primarily by means of a vibrating device.
- a closure assembly 13 is used in this embodiment, which comprises an annular sealing element 10, an annularly arranged strip-shaped sealing element 1 1 and a graphite closure element, in this case graphite ring 9 comprises.
- the annularly arranged, strip-shaped sealing element 1 1 was formed edgewise to the ring.
- the sealing elements used in this example consist of graphite soft felt with a thickness of 5 mm from GFA5 from SGL CARBON GmbH.
- the graphite ring 9 is placed on the double-walled graphite funnel 1 according to the invention and thus the intermediate space is closed.
- the graphite ring 9 is made in this embodiment of identical material as the outer hopper 3 and inner hopper 4.
- the graphite ring 9 is dimensioned so that it clears the gap 7 between the inner and outer hopper in the region of the opening 12 with the larger Can cover wide.
- the graphite ring 9 is preferably designed such that it rests on the graphite funnel 1 according to the invention, if necessary fixed thereto.
- a fixation can be achieved by means of a connecting element 2. can follow, but can also be done by engaging a groove formed in the graphite ring 9 in the funnel edge, according to the principle of tongue and groove.
- the closure assembly 13 is fixed in the present embodiment with a connecting means 2 on the graphite funnel 1 according to the invention.
- a connecting means 2 on the graphite funnel 1 according to the invention.
- an opening is introduced into the graphite ring 9, through which a pin 2 is introduced into the edge of the outer funnel.
- a graphite ring 9 is used, in which already one passage opening or more passage openings are introduced for at least one connecting means.
- the inventive graphite funnel 1 described in this example is suitable for use in Czochralski processes.
- the graphite funnel according to the invention still has the original insulation properties even after a long period of use. This suggests that replacement of the filler is unlikely to be required over the lifetime. However, this depends on the process conditions of the plant in which the graphite hopper is used. In any case, the duration of the usability of the graphite funnel according to the invention will exceed the period of time after which insulating material in the funnels of the prior art
- the present invention provides a double-walled graphite hopper which has significant advantages over the prior art.
- the graphite funnel according to the invention is filled with a filling material, whereby the thermal properties of the graphite funnel are influenced.
- the disclosed double-walled graphite hopper in one embodiment is filled with a graphite semolina and, due to the insulating properties in Czochralski systems, is suitable for shielding the monocrystal drawn therein. It is advantageous, inter alia, that the Filling individually and inexpensively, with genngem technical effort can be done.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Gasket Seals (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102014226297.6A DE102014226297A1 (en) | 2014-12-17 | 2014-12-17 | Double-walled graphite funnel |
| PCT/EP2015/080097 WO2016097057A1 (en) | 2014-12-17 | 2015-12-16 | Double-walled graphite funnel |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP3234232A1 true EP3234232A1 (en) | 2017-10-25 |
Family
ID=55080087
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP15822925.2A Withdrawn EP3234232A1 (en) | 2014-12-17 | 2015-12-16 | Double-walled graphite funnel |
Country Status (5)
| Country | Link |
|---|---|
| EP (1) | EP3234232A1 (en) |
| CN (1) | CN107109685A (en) |
| DE (1) | DE102014226297A1 (en) |
| SG (1) | SG11201704876UA (en) |
| WO (1) | WO2016097057A1 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6304424B1 (en) | 2017-04-05 | 2018-04-04 | 株式会社Sumco | Heat shielding member, single crystal pulling apparatus, and method for manufacturing single crystal silicon ingot |
| CN110438559B (en) * | 2019-08-28 | 2024-04-16 | 包头美科硅能源有限公司 | Diameter-variable guide cylinder for single crystal furnace |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09183686A (en) * | 1995-12-27 | 1997-07-15 | Shin Etsu Handotai Co Ltd | Method and apparatus for pulling up single crystal |
| US6197111B1 (en) * | 1999-02-26 | 2001-03-06 | Memc Electronic Materials, Inc. | Heat shield assembly for crystal puller |
| JP2004107132A (en) * | 2002-09-18 | 2004-04-08 | Sumitomo Mitsubishi Silicon Corp | Heat shielding member for silicon single crystal pulling apparatus |
| US6797062B2 (en) * | 2002-09-20 | 2004-09-28 | Memc Electronic Materials, Inc. | Heat shield assembly for a crystal puller |
| JP4161804B2 (en) * | 2003-05-30 | 2008-10-08 | 株式会社Sumco | Heat shielding member of silicon single crystal pulling device |
| US8152921B2 (en) * | 2006-09-01 | 2012-04-10 | Okmetic Oyj | Crystal manufacturing |
| CN102352530B (en) * | 2011-11-09 | 2014-04-16 | 内蒙古中环光伏材料有限公司 | Heat shield device for CZ-Si single crystal furnace |
| KR101494521B1 (en) * | 2013-04-30 | 2015-02-17 | 웅진에너지 주식회사 | Heat shield structure |
-
2014
- 2014-12-17 DE DE102014226297.6A patent/DE102014226297A1/en not_active Withdrawn
-
2015
- 2015-12-16 CN CN201580068934.1A patent/CN107109685A/en active Pending
- 2015-12-16 WO PCT/EP2015/080097 patent/WO2016097057A1/en not_active Ceased
- 2015-12-16 EP EP15822925.2A patent/EP3234232A1/en not_active Withdrawn
- 2015-12-16 SG SG11201704876UA patent/SG11201704876UA/en unknown
Non-Patent Citations (2)
| Title |
|---|
| None * |
| See also references of WO2016097057A1 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107109685A (en) | 2017-08-29 |
| SG11201704876UA (en) | 2017-07-28 |
| DE102014226297A1 (en) | 2016-06-23 |
| WO2016097057A1 (en) | 2016-06-23 |
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