CN104032370A - Device for producing silicon blocks - Google Patents
Device for producing silicon blocks Download PDFInfo
- Publication number
- CN104032370A CN104032370A CN201410068762.5A CN201410068762A CN104032370A CN 104032370 A CN104032370 A CN 104032370A CN 201410068762 A CN201410068762 A CN 201410068762A CN 104032370 A CN104032370 A CN 104032370A
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- China
- Prior art keywords
- container
- silicon
- crucible
- equipment
- suo shu
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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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/04—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method adding crystallising materials or reactants forming it in situ to the melt
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/04—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method adding crystallising materials or reactants forming it in situ to the melt
- C30B11/08—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method adding crystallising materials or reactants forming it in situ to the melt every component of the crystal composition being added during the crystallisation
- C30B11/10—Solid or liquid components, e.g. Verneuil 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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
Abstract
The present invention relates to a method for producing silicon blocks. The method includes the following steps: providing silicon melt (2) in a first container (3); providing silicon melt (2) in a second container (4); carrying out orientation solidification for the silicon melt (2) in the first container (3); and moving the liquid silicon from the second container (4) to the first container (3).
Description
Technical field
The present invention relates to a kind of equipment for the production of silico briquette.In addition, the invention still further relates to a kind of method for the production of silico briquette.Finally, the present invention relates to a kind of silico briquette.
Background technology
Known a kind of for equipment and the method for liquid-state silicon are provided by EP 2 251 459 A1.Arrange in this case, to filling (nachzuchargieren) liquid-state silicon after fusion crucible.
Summary of the invention
The object of the invention is to, improve the equipment for the production of silico briquette.
This object is achieved by feature claimed in claim 1.
Core of the present invention is, by least two container arrangement for holding semiconductor melt, in common chamber, wherein, at least one container in described container has outlet, and via described outlet, liquid-state silicon can flow out at least one other container.
Described second container is particularly useful for providing silicon melt, to load after an action of the bowels described the first container.Preferably, described second container is arranged on described the first container.This makes described liquid-state silicon flow out to described the first container and become easy from described second container.
The outlet of described second container especially can form with the form of spillway, preferably with stem bar form.Described outlet especially can be controlled, and especially can be closed.
Common chamber for holding said container is especially heat-insulating.It preferably can externally be isolated in airtight mode.By by described container arrangement in common chamber, improved the efficiency of described method.
Described container especially relative to each other position is fixedly arranged.Especially can abandon movable parts.This has simplified the structure of described equipment.In addition improved thus, the mechanical stability of described equipment.
According to an aspect of the present invention, the capacity V of described second container
2be less than the capacity V of described the first container
1, i.e. V
2< V
1.Especially be suitable for: V
2: V
1≤ 0.5, especially V
2: V
1≤ 0.1, especially V
2: V
1≤ 0.05, especially V
2: V
1≤ 0.01, especially V
2: V
1≤ 0.005.The capacity V of described second container
2especially be at least 0.5 liter (L).Described capacity V
1especially rise in the scope of 5000 liters in 100.Described capacity V
2especially rise in the scope of 20 liters in 0.5.
Described second container especially has following cross-sectional area A
2, it is less than the cross-sectional area A of described the first container
1, i.e. A
2< A
1.Especially be suitable for: A
2: A
1≤ 0.5, especially A
2: A
1≤ 0.25, especially A
2: A
1≤ 0.2.
Described second container especially can have following cross section, and described shown in cross section goes out the demarcation pattern of the cross section of described the first container.It preferably can arrange in the following way, that is, the symmetry characteristic of described the first container in the combination being made up of the first container and second container is guaranteed.Thus, can affect in the advantageous mode of tool the crystallization of the silicon melt in described the first container.
According to an aspect of the present invention, described equipment has heating unit, and described heating unit is applicable to not only in described the first container but also in described second container, make bulk silicon melting.
Described heating unit especially can comprise the top heater of described the first container.Described top heater is especially arranged on described the first container.It can be arranged on described second container or under.
Described top heater can have in 1kW(kilowatt) to power, the especially power in 10kW to 70kW scope, the especially power in 30kW to 55kW scope within the scope of 100kW.
Described top heater can be with respect to the upper limb of described the first container layout of apart turning up the soil.Spacing between the upper limb of described top heater and described the first container is especially in the scope in 1cm to 100cm, especially in the scope in 1cm to 20cm, especially in the scope in 5cm to 10cm.
Spacing between the upper limb of described top heater and described the first container is especially greater than the extension of described second container in the direction of the cross section perpendicular to it.But the spacing between described top heater and the upper limb of described the first container also can be less than the extension of described second container in the direction of the cross section perpendicular to it.
Described second container especially can be arranged in so-called " hot-zone (the Hot Zone) " of described the first container.In this case, described " hot-zone " refer in described chamber as lower area, described region can be heated in the temperature on the temperature of fusion in silicon by means of described heating unit, especially be heated to above in the temperature of 1450 DEG C, especially be heated to above in the temperature of 1500 DEG C.
In order to be arranged in described " hot-zone ", described second container can be arranged on graphite cake or by means of the support of being made up of graphite and remain in described chamber.Described support especially can be installed on a wall in described chamber, especially on sidewall or on roof.
According to an aspect of the present invention, described heating unit comprises multiple heating units.Described heating unit especially can be independent of each other and be controlled.Described heating unit forms especially in the following way,, at the silicon melt setting up period making in described the first container, can make the bulk silicon melting in described second container that is.Described heating unit especially can have the independent heating unit of the silicon melting for making described second container.They can be arranged on described second container and/or under and/or side, that is to say and be arranged in its neighboring area.
In addition, described heating unit especially can be controlled in the following way, that is, the silicon melt in described the first container is directionally solidified.Especially can the silicon melt in described the first container be solidified according to so-called Vertical Gradient Freeze (VGF) (VGF) method.
Tool is advantageous especially, as the heating unit of the silicon melting for making described second container, uses electron rays or laser source.Available or additionally to this, one or more heating unit of resistance heater or induction type heating unit form can be set.
According to another aspect of the present invention, described equipment comprises the 3rd container for holding bulk silicon, and described the 3rd container is connected with described second container via e Foerderanlage.
Described the 3rd container especially can be arranged in the outside in described common chamber.Described e Foerderanlage can be pipe connecting.Described e Foerderanlage especially has control piece.What can serve as control piece is for example the removable cover that can open and close.
Preferably, described the 3rd container arrangement is on the common chamber for holding described the first container and described second container.Described the 3rd container is arranged especially in the following way, that is, can come to described the 3rd container heat supply by means of the waste heat in described common chamber.This can make block raw material in described the 3rd container with the advantageous mode of tool degassed (Entgasung).
According to another aspect of the present invention, described equipment comprises the element that delays for making to delay from the liquid-state silicon of described second container.The described element that delays can be to connect the form formation of dripping plate or guiding device.It also can have for by the chopping mechanism of each silica drop chopping from described second container.By by falling into the silica drop chopping of described the first container, can reduce the momentum that drop has in the time of the melt entering in described the first container.Thus, can reduce described drop and enter the placed-depth in the melt in described the first container.
Another object of the present invention is, improves a kind of method for the production of silico briquette.This object is achieved by feature claimed in claim 6.Advantage is learnt by the description to aforementioned device.
In the method according to the invention, especially arrange, liquid-state silicon is transferred to described the first container from described second container.During the melting process of silicon that this may be in described the first container, just occur.Also can realize, after the complete melting of silicon in described the first container, liquid-state silicon be transferred to described the first container from described second container.Especially also can realize, during the described silicon melt directional solidification making in described the first container, liquid-state silicon be transferred to described the first container from described second container.
The described transfer of transferring to described the first container from described second container is also referred to as rear filling.
Can find out according to the present invention, in described the first container, the amount of the silicon of crystallization can be amplified by rear filling.In addition, it can also be seen that, when silicon by rear filling time, can improve the quality of the silico briquette in the crystallization in described the first container with liquid form.
In addition, can find out, by rear filling liquid-state silicon, can affect the characteristic of the silico briquette of crystallization in described the first container.Especially can realize, affect the concentration of one or more hotchpotchs and therefore especially affect silico briquette in the described crystallization resistor-type exterior feature (Widerstandsprofil) on its height in the advantageous mode of tool by rear filling.Especially can realize, silico briquette has more uniform resistor-type exterior feature, especially has the resistance bandwidth (Widerstandsbandbreite) reducing.By means of the method according to this invention, especially can produce following silico briquette, its resistivity the whole height of described silico briquette at least 50% on, especially at least 60%, especially at least 70%, be less than 30% around the mean value fluctuation of described resistivity, be especially less than 20%, especially be less than 10%, be especially less than 5%.The mean value of described resistivity especially can be in 1.2 Ω cm(ohmcms) to the scope of 1.6 Ω cm, especially in the scope in 1.3 Ω cm to 1.5 Ω cm, especially in the scope in 1.3 Ω cm to 1.4 Ω cm.
By adding hotchpotch, also can realize other resistivity, especially another kind of resistor-type exterior feature.
According to another aspect of the present invention, can during one or more time period, realize continuously described rear filling.Especially can realize, carry out continuously rear filling in mode in batches.In this case, continuous rear filling is construed as the rear filling with constant rear filling speed.The in the situation that of filling after carrying out with multiple batches, each batch can be different.They especially can have different volumes.They also can have different concentration of dopant.
According to another aspect of the present invention, the liquid-state silicon of altogether transferring to described the first container from described second container has capacity V
n, wherein, be suitable for: V
n: V
1>=0.05, especially V
n: V
1>=0.01, especially V
n: V
1>=0.2, especially V
n: V
1>=0.3.Can be suitable for: V
n: V
1>=0.5, especially V
n: V
1>=0.7, especially V
n: V
1>=0.9.In the scope of the absolute magnitude of the silicon of rear filling in 0.1kg to 1000kg, especially in the scope in 1kg to 700kg, especially in the scope in 10kg to 500kg, especially within being greater than the scope of 50kg, especially within being greater than the scope of 100kg.
According to another aspect of the present invention, described rear filling speed is in 0.1kg/h(kg/hr) to the scope of 10kg/h, especially in the scope in 0.3kg/h to 3kg/h.Described rear filling speed can be controlled in the mode of the crystallization velocity that depends on the silicon melt in described the first container.
According to another aspect of the present invention, the silicon of described rear filling has one or more hotchpotchs of predetermined concentration.This especially can and/or add specific hotchpotch and realize by the raw material of corresponding doping given in advance in described the 3rd container.Silicon in described second container especially can not have hotchpotch.To this, alternatively, it can have one or more elements that are selected from element below of concentration given in advance: boron, aluminium, gallium, indium, phosphorus, arsenic and antimony.
Also can realize, the concentration changes with time of one or more this hotchpotchs, especially along with the process of described rear filling changes.Thus, especially can react on the variation of concentration of dopant in described silicon melt, the variation of described concentration of dopant is because separate effect (Segregationseffekten) can be observed during described silicon melt crystallization.By simple mode, can be with time dependent concentration of dopant by filling after realizing with mode in batches corresponding raw material given in advance in described the 3rd container.
According to an aspect of the present invention, at the silicon melt setting up period making in described the first container, give described second container by bulk silicon from the 3rd container transport stagely or continuously.The conveying of described bulk silicon from described the 3rd container to described second container especially can realize in check mode.By carrying described bulk silicon to described second container, can affect described rear filling speed, filling speed after the maximum that especially impact can reach.Preferably, the silicon that flows to described second container has one or more hotchpotchs above-mentioned of concentration given in advance.It especially can not have hotchpotch yet.
Another object of the present invention is, improves a kind of silico briquette.This object is achieved by the feature described in claim 14.Advantage is by description above and learn.The notable feature of described silico briquette be especially can be given in advance hotchpotch type wide or be related and be the resistor-type exterior feature given in advance on the height of described with it.The resistance bandwidth that described silico briquette indicates above especially having on the height of described silico briquette.
Described silico briquette preferably has accurate single structure (Quasimono-Struktur).This is construed as, described silico briquette its volume at least 70% in, especially at least 80% of its volume, especially at least 90% of its volume, there is monoclinic crystal structure.In general, described silico briquette especially its volume at least 50% in there is monoclinic crystal structure.
Brief description of the drawings
Other features of the present invention and details are learnt by the description to multiple embodiment by reference to the accompanying drawings.
Fig. 1 illustrates according to the schematic diagram of the equipment for the production of silico briquette of the first embodiment;
Fig. 2 illustrates the schematic cross sectional views in the region of rear filling crucible (Nachchargiertiegels) according to the equipment of Fig. 1;
Fig. 3 illustrates the diagram according to Fig. 1 according to another kind of embodiment of the present invention;
Fig. 4 illustrates the diagram according to Fig. 1 according to another kind of embodiment of the present invention;
Fig. 5 illustrates the diagram according to Fig. 1 according to another kind of embodiment of the present invention;
Fig. 6 illustrates the diagram according to Fig. 1 according to another kind of embodiment of the present invention; And
Fig. 7 illustrates the detailed view of the described rear filling crucible in Fig. 1.
Embodiment
Below with reference to Fig. 1 and Fig. 2, the equipment 1 for the production of silico briquette is described.The general details of described equipment 1 that is also referred to as the crystallizer for making silicon melt 2 crystallizations is for example known by DE 10 2,005 013 410 B4 and DE 10 2,011 002 599 A1, they two be all incorporated to completely in the application as the application's integral part.
Described equipment 1 comprises the first container of fusion crucible or crystallization crucible 3 forms.Described crucible 3 is particularly useful for making silicon fusing and solidifies.It is particularly useful for holding described silicon melt 2.Details for the crucible 3 that is also referred to as ingot mould (Kokille) refers to DE 10 2,005 013 410 B4 and DE 10 2,011 002 599 A1.
In addition, described equipment 1 also comprises the second container of crucible 4 forms.Described the second crucible 4 is equally for holding silicon melt 5.It is particularly useful for making bulk silicon 6 meltings.Can, by means of e Foerderanlage 7, described bulk silicon 6 be flowed to described the second crucible 4 from the 3rd container 8.Described the 3rd container 8 refers in particular to the storage vessel for holding silicon raw material.Described e Foerderanlage 7 can be pipeline.Described e Foerderanlage 7 is especially made up of pottery or graphite.
Described the first crucible 3 and described the second crucible 4 are arranged in a common chamber 9.Described chamber 9 is also referred to as crystallization cavity.It is especially heat-insulating.It preferably forms airtightly.It especially can be connected with the scavenging arrangement 10 schematically showing.By means of described scavenging arrangement 10, can apply scavenging to described chamber 9, especially apply argon gas.In general,, by means of described scavenging arrangement 10, can control the air pressure in described chamber 9.Vacuum especially can be pumped in described chamber 9.Described chamber 9 especially can be configured to steel stove.It especially can be filled argon gas during described technique.
Special tool is advantageous, and described scavenging arrangement 10 can combine with described e Foerderanlage 7.Be different from the embodiment shown in accompanying drawing, especially can, via e Foerderanlage 7 identical as described bulk silicon 6, described scavenging be flowed to described chamber 9.
Described the 3rd container 8 is especially arranged in 9 outsides, described chamber.It is especially arranged on described chamber 9.Especially can be by coming from the waste heat in described chamber 9 to described the 3rd container heat supply.This can support the degassed of the interior described bulk silicon 6 of described container 8.In principle, described the 3rd container 8 also can be arranged in 9 inside, described chamber.
Described the second crucible 4 has outlet, and via described outlet, liquid-state silicon 11 can flow out to described the first crucible 3 from described the second crucible 4.Described outlet especially can be configured to spillway.It is especially configured to stem bar 12.
Described outlet also can be used as in the sidewall that gap is formed in described the second crucible 4.
In the region of described outlet, can be provided for filtering the filtering element of solid material.What be especially suitable for is the porcelain filter with vesicular structure for this reason.Details are especially consulted US 13/,561 456.
Described the first crucible 3 is especially arranged under described the second crucible 4.It is especially fixedly arranged with respect to described the first crucible 3 positions.
In addition, described equipment 1 comprises the heating unit with multiple heating units.Described heating unit especially can be controlled by means of the control device 13 schematically showing.They especially can be independent of each other and be controlled.Described heating unit preferably includes multiple side heat elements 14.Also can abandon described side heat element 14.In addition, they also comprise at least one top firing element 15.In addition, they can comprise bottom-heated element.Described heating unit is applicable to not only in described the first crucible 3 but also in described the second crucible 4, make bulk silicon melting.It can have the thermal power that is greater than 10 kilowatts (kW).
In addition, described heating unit also comprises the cooling element of heat groove 16 forms.Described heat groove 16 is arranged under described the first crucible 3, is especially arranged under the diapire 17 of described the first crucible 3.It especially has the active cooling device with control device 18.
Described heating unit and described heat groove 16 can be controlled especially in the following way, that is, can make the described silicon melt 2 in described the first crucible 3 directionally solidify.In this case, especially can control neatly the shape on the phase border (Phasengrenze) 24 between silicon 25 and the liquid-state silicon melt 2 having cured.In addition, in this case, the shape on described phase border 24 also depends on the side heat element 14 of described heating unit and the geometrical shape of all the other heating units and the manipulation to them.The shape on described phase border 24 especially also depends on the molten stream that can control by means of heating unit in described the first crucible 3.The shape on described phase border 24 especially can be controlled in the following way, that is, the shape on described phase border 24 flatly forms or forms to convex as illustrated in Fig. 1.The shape on described phase border 24 especially can be controlled in the following way, that is, the shape on described phase border 24 is axisymmetric with respect to central longitudinal axis 23.
In addition, described heating unit also comprises multiple especially four side heat elements 19, and it is for giving described the second crucible 4 heat supplies.Described side heat element 19 is especially arranged in all sides of described the second crucible 4.Their size is suitable for the sidewall 20 of described the second crucible 4.They especially can be controlled in the mode that is independent of described heating unit 14,15.Replace multiple side heat elements 19, also can be provided for to described the second crucible 4 heat supplies around side heat element.
For thering is the thermal power more than 10 kilowatts (kW) to the side heat element 19 of described the second crucible 4 heat supplies.The thermal power of described side heat element 19 especially can be controlled.Described thermal power especially can be controlled in the following way,, at silicon melt 2 setting up period that make in described the first crucible 3, can make bulk silicon 6 meltings in described the second crucible 4 that is.
Described the second crucible 4 can be fixed in described chamber 9 by means of stationary installation 21.Described stationary installation 21 is especially made up of graphite.
According in the embodiment of Fig. 1, described the second crucible 4 is arranged in the region between top firing element 15 and the first crucible 3.Therefore, described top firing element 15 is not only formed for the top heater of the first crucible 3 but also is formed for the top heater of the second crucible 4.Described top firing element 15 has breach 27.According in the embodiment of Fig. 1, described breach 27 is for making described e Foerderanlage guide to described the second crucible 4 from the 3rd container 8 break-through.By the second crucible 4 is arranged under top firing element 15 and can be guaranteed, the silicon in described the second crucible 4 equally directionally solidifies from bottom to up in the time that crystallisation process finishes.Can avoid thus, because the extension of remaining silicon in described the second crucible 4 damages described the second crucible 4.Described crucible 4 especially can repeatedly use.
As being schematically shown in Fig. 2, described top firing element 15 can form crankyly.In the embodiment shown in Fig. 1 and Fig. 2, described top firing element 15 is arranged on described the second crucible 4.Described top firing element 15 comprises multiple arms 22,22 that distribute as the crow flies
*.Described arm 22 has each identical width b.Described arm 22
*there is width b
*.Described width b
*be less than described width b.In the embodiment shown, be suitable for: b:b
*=2.In general, be suitable for: 0.5≤b:b
*≤ 5.In the embodiment shown in Fig. 2, the width b of described arm 22 is just in time corresponding to the width b of described crucible 4
t.But described crucible 4 also can have another width b that is different from arm 22
t.
By described arm 22
*less width b in region on described the second crucible 4
*can realize, compared with in other regions, in the region of described top firing element 15 on described the second crucible 4, unit surface discharges more power.Thus, can guarantee the melting of the bulk silicon 6 in described the second crucible 4.
In general, described top firing element 15 also can have heated zones bar-shaped and/or ring-type or annular.
As shown in exemplary in the accompanying drawings, the capacity V of described the second crucible 4
2be less than the capacity V of described the first crucible 3
1.Be suitable for: V
2: V
1< 1, especially V
2: V
1≤ 0.5, especially V
2: V
1≤ 0.1, especially V
2: V
1≤ 0.05, especially V
2: V
1≤ 0.01, especially V
2: V
1≤ 0.005.
In addition the cross-sectional area A of described the second crucible 4,
2be less than the cross-sectional area A of described the first crucible 3
1.Be suitable for: A
2< A
1, especially A
2: A
1≤ 0.5, especially A
2: A
1≤ 0.25, especially A
2: A
1≤ 0.2.
In a kind of preferred implementation, described the first crucible 3 has symmetry characteristic.It is especially mirror symmetry with respect to central longitudinal face.It is especially axisymmetric with respect to central longitudinal axis 23.It especially has quadruple symmetry.Advantageous in the accompanying drawings also in unshowned embodiment at a kind of tool, described the second crucible 4 forms in the following way and arranges, the combination, being made up of the first crucible 3 and the second crucible 4 is observed and is had identical symmetry characteristic as described the first crucible 3 from the outlet of described the second crucible 4.
To this alternatively, also can realize, the equipment being made up of crucible 3 and heating unit asymmetricly forms.This for example can be by correspondingly arranging that described side heat element 14 and/or its joint realize.In this case, can arrange, by suitably forming and/or arranging described the second crucible 4 at least in part, especially as far as possible fully, compensate this asymmetry, thereby adjust temperature field in described crucible 3, described temperature field is axisymmetric with respect to central longitudinal axis 23.
As shown in exemplary in Fig. 1, be furnished with one or more crystal seed plate (Keimplatten) 26 in the bottom of described the first crucible 3.Described crystal seed plate 26 especially has definite axial crystalline orientation.It also can especially have definite transverse crystal orientation.Described crystal seed plate 26 is especially made up of silicon single crystal.Described crystal seed plate 26 especially has axial <110> or <100> orientation.Also can realize, use the crystal seed plate 26 with polycrystal structure.Alternatively, also can abandon described crystal seed plate 26.
In addition, can be provided for hiding the cover plate 28 of described the first crucible 3.Described cover plate 28 is especially arranged on the crucible edge above of described the first crucible 3.It can be placed on described the first crucible 3.Described cover plate 28 is especially made up of graphite.It has break-through mouth 29, liquid-state silicon can be transferred to described the first crucible 3 from described the second crucible 4 through described break-through mouth 29.Described cover plate 28 can produce actively impact to the temperature field in described the first crucible 3.It especially can make to produce more uniform temperature field in described the first crucible 3.Described break-through mouth 29 is preferably relatively little.Described break-through mouth 29 has following area, and described area is especially less than the cross-sectional area A of described the first crucible 3
110%, be especially less than described cross-sectional area A
15%, be especially less than described cross-sectional area A
11%, be especially less than described cross-sectional area A
10.1%.Multiple break-through mouths 29 also can be set in described cover plate 28.They especially can arrange in the following way, that is, the symmetry characteristic of described the first crucible 3 remains unchanged.They especially can especially symmetrically be arranged symmetrically with respect to central longitudinal axis 23.
Described cover plate 28, especially described break-through mouth 29, forms especially in the following way and arranges, that is and, the temperature field in described the first crucible 3 is symmetrical with respect to described central longitudinal axis 23.Described temperature field especially has at least quadruple symmetry.
Method for the production of silico briquette is described below.First, provide described equipment 1.Then, crystal seed plate 26 is arranged on the bottom 17 of crucible 3.In addition, fill bulk silicon to described crucible 3.And then, make described bulk silicon melting in order to provide silicon melt 2 in described the first crucible 3.Especially make in the following way the raw materials melt in described the first crucible, that is, only partly, that is to say not completely, make described crystal seed plate 26 meltings.
To this alternatively, can realize, in outside fusion crucible, make described bulk silicon melting, and described bulk silicon is inserted in described the first crucible 3 with liquid form.
And then, make silicon melt 2 directional solidifications in described the first crucible 3.This can be by suitably controlling described heating unit and described heat groove 16 is realized, and details refer to DE 10 2,005 013 410 B4 and DE 10 2,011 002 599 A1.
In addition, in described the second crucible 4, provide silicon melt 2.For this reason, fill the bulk silicon 6 from described the 3rd container 8 to described the second crucible 4.In described the second crucible 4, make described bulk silicon 6 meltings by means of side heat element 19 or heating unit.As hotchpotch, can add the phosphorus (Phosphor) of the form of high doped (hochdotiertem) silicon." high doped silicon " is construed as concentration is every cubic centimetre of (cm
3) 10
15to 10
21the silicon of individual atoms of dopant.Described hotchpotch also can mix with described bulk silicon 6 with the form of P contained compound.
Described liquid-state silicon is transferred to described the first crucible 3 from described the second crucible 4.During this can occur in the silicon melting making in described the first crucible 3.This also can only just occur after the silicon melting making in described the first crucible 3.During this especially also can occur in silicon melt 2 directional solidifications that make in described the first crucible 3.
The described transfer of liquid-state silicon from the second crucible 4 to first crucibles 3 is also referred to as the rear filling (Nachchargieren) of described the first crucible 3.Described rear filling realizes especially continuously, that is to say with rear filling speed given in advance and realizes.It especially realizes continuously during that is to say one or more timed interval during one or more time period.The time period of described continuous rear filling especially in 1 minute (min) to the scope of 30 hours (h).The described time period is especially 10min at least, especially at least 30min, especially at least 1h.
In general, setting at silicon melt 2 setting up period that make in described the first crucible 3, flows to described the second crucible 4 by bulk silicon 6 from described the 3rd container 8 at least stagely.
Described rear filling speed is in 0.1kg/h(kg/hr) to the scope of 10kg/h, especially in the scope in 0.3kg/h to 3kg/h.Low rear filling speed is that tool is advantageous, to guarantee that the crystallization of described silicon melt 2 in described the first crucible 3 can not be subject to the negative impact of described rear filling.Especially can guarantee, the described liquid-state silicon melt 2 in the volume Shu Buhui of the silicon of rear filling and described the first crucible 3 blendes together one, and especially can not arrive described phase border 24.Can arrange for this reason, suitably reduce described rear filling speed at the end of crystallisation process.
During whole crystallisation process, described rear filling can realize during one or more time period.Loading capacity V later altogether from described the second crucible 4 to described the first crucible 3
n, described capacity V
nin the capacity V of described the first crucible 3
15% to 100% scope in.Especially be suitable for: V
n: V
1>=0.05, especially V
n: V
1>=0.01, especially V
n: V
1>=0.2, especially V
n: V
1>=0.3.Can be suitable for: V
n: V
1>=0.5, especially V
n: V
1>=0.7, especially V
n: V
1>=0.9.
On absolute number, the amount of the silicon of described rear filling is especially in the scope in 0.1kg to 1000kg, especially in the scope in 0.3kg to 3kg.
The silicon of described rear filling has one or more hotchpotchs of predetermined concentration.It especially can not have hotchpotch.Nominally the silicon of described rear filling can be especially there is no hotchpotch.It especially has and is less than every cubic centimetre 210
13the concentration of dopant of individual atom.
It also can have one or more hotchpotchs that are selected from list below: boron, aluminium, gallium, indium, phosphorus, arsenic and antimony.Preferably, described bulk silicon 6 or the silicon melt 2 for described the first crucible 3 of rear filling that is arranged in the second crucible 4 only comprise unique hotchpotch.
There is the silicon of one or more hotchpotchs of predetermined concentration by rear filling, can affect the concentration of dopant in the silicon ingot of crystallization.It especially can be controlled in the following way,, compensates the variation of the concentration of dopant in the interior described silicon melt of described the first crucible 3, when the variation of described concentration of dopant may appear at described silicon melt 2 crystallization due to separate effect that is.What especially can realize is, by targetedly afterwards filling have definite concentration one or more hotchpotchs silicon or there is no the silicon of hotchpotch by rear filling, make the silico briquette of crystallization in described the first crucible 3 there is uniform concentration of dopant and therefore there is uniform resistor-type exterior feature.
In addition, can arrange, by means of electromagnetic field, especially by means of the electromagnetic field that can produce and control by side heat element 14, the silicon melt 2 in described the first crucible 3 be mixed thoroughly.
The silico briquette of producing according to the method according to this invention especially has following resistor-type exterior feature, on crystallization direction, is substantially constant at the above resistor-type exterior feature of whole extension of silico briquette.Be less than 30% of average resistivity, especially be less than 20% of average resistivity, especially be less than in 10% situation of average resistivity, described resistance width especially the height in described silico briquette at least 50% on, especially at least 60% of the height in described silico briquette, especially at least 70% of the height in described silico briquette, especially at least 80% of the height in described silico briquette.In this case, described resistance width is construed as described resistivity in the maximum differential on observed volume between two regions.In other words, described resistance width has indicated measured maximum resistance and the measured minimum resistance difference on observed volume.The average resistivity of described silico briquette in this homogeneous area is especially in 1.2 Ω cm(ohmcms) to the scope of 1.6 Ω cm, especially in the scope in 1.3 Ω cm to 1.5 Ω cm, especially in the scope in 1.3 Ω cm to 1.4 Ω cm.
Described silico briquette can be especially N-shaped silico briquette.Described silico briquette is especially doped with phosphorus, and is therefore N-shaped conduction (n-leitend) from conduction type.For Doping Phosphorus, alternatively or additionally, described silico briquette also can have with the doping material of one or more aforementioned hotchpotchs or coordinate doping material.
Tool is advantageous especially, and the concentration of one or more hotchpotchs of the silicon of described rear filling changes in the process of crystallization processes.In other words, the silicon of described rear filling can have time-varying concentration of dopant.
In stage rear filling, that is to say in the situation of loading after batch-type, this can realize in the following way in simple mode, that is, in batches the raw material with different concentration of dopant is transferred to described the second crucible 4 from described the 3rd container 8.
Other details and the characteristic of described equipment 1 are described below.By means of described the second crucible 4 and especially by means of attaching troops to a unit in its heating unit, especially side heat element 19, can will be loaded into after liquid-state silicon in the first crucible 3 in simple mode.Especially can load afterwards continuously described liquid-state silicon.After can coming with controlled flexibly rear filling speed, load described liquid-state silicon.By rear filling liquid-state silicon, prevent because relatively cold raw material makes described silicon melt 2 local coolings in described the first crucible 3.Thus, improved the crystalline structure of described silico briquette.
Due to await melting in described the second crucible 4 raw material 5 load afterwards flexibly possibility and especially due to its simple controllability of characteristic, can be flexibly and exactly the silico briquette in crystallization control concentration of dopant and therefore control its distribution of resistance.Can produce thus the silico briquette on its most of height with very narrow distribution of resistance.
Can the described liquid-state silicon of rear filling on different time points and/or in different crystallization processes.
In order to carry out described rear filling, make bulk silicon 6 meltings of relatively little amount respectively in described the second crucible 4.This has improved the controllability of described method.
In the exemplary form of implementation of described method, make the silicon melting of 400kg in described the first crucible 3, and be on 30h, to make its crystallization in the time length.In this case, start to count 10h to starting to count from crystallization in the timed interval between 25h from crystallization, be namely on 15h in the time length, the silicon of rear filling 200kg.Therefore, average rear filling speed is 13.3kg/h.
The partial enlarged drawing of the advantageous embodiment of a kind of tool of described the second crucible 4 shown in Figure 7.As shown in exemplary in Fig. 7, described crucible 4 comprises two chambeies 31,32 connected to one another.Described chamber 31,32 is spaced by dividing plate 33.In this case, between described dividing plate 33 and the bottom 34 of described crucible 4, leave break-through mouth 35.Described break-through mouth 35 forms the mobile connection between described chamber 31,32.
Described dividing plate 33 arranges in the following way and forms, that is, and and the defining under rib of bottom of defining rib 36 and be especially arranged in the especially described stem bar 12 of described outlet of its bottom.Therefore, described dividing plate 33 especially serves as the confinement element of the immobilization material on the silicon melt 2 for swimming in described crucible 4, in particular for swimming in the confinement element of the bulk silicon 6 on described silicon melt 2.
The outlet of described the second crucible 4 is arranged on its bottom 34.Can guarantee thus while filling, always have minimum silicon melt 2 to stay in described the second crucible 4 after carrying out.Can guarantee thus, described bulk silicon 6 can not fall into empty crucible 4 from described the 3rd container 8, but directly falls into liquid-state silicon.Can improve thus the heating to described bulk silicon 6.
Described the second crucible 4 can be by silicon nitride (Si
3n
4), silicon-dioxide (SiO
2) or formed by the plastics of carbon fiber reinforcement.
Can be by described bulk silicon 6 be added to described the second crucible 4 and is controlled from described the 3rd container 8 by the mass flow of the liquid-state silicon of rear filling.This can be controlled in 9 outsides, described chamber.
Attach troops to a unit and can regulate by setting device in the thermal power of the heating unit of described the second crucible 4.For this reason, unshowned thermopair in the accompanying drawings can be set in the region of described top heater.Described power especially can regulate in the following way,, reaches design temperature given in advance in the region of described the second crucible 4 that is.As long as do not have to load liquid-state silicon behind stage ground during the crystallization processes of silicon melt 2 in described the first crucible 3, so just can reduce the thermal power of attaching troops to a unit in the heating unit of described the second crucible 4.
The another kind of embodiment of described equipment 1 is described below with reference to Fig. 3.Identical parts are as retain identical Reference numeral according in the embodiment of Fig. 1, hereby referring to description of them.According in the embodiment of Fig. 3, described the second crucible 4 is arranged on described top firing element 15.This heat on the one hand can improving from described top firing element 15 to described the second crucible 4 injects.In addition can improve, the homogeneity in the temperature field in described the first crucible 3 by this layout.By described top firing element 15 being arranged between the first crucible 3 and the second crucible 4, especially can guarantee, described the second crucible 4 can not have a negative impact to the temperature field in the first crucible 3, can not exert an influence to the temperature field in the first crucible 3 especially completely.In the present embodiment, all arms 22 of described top firing element 15 can have identical width b.
The another kind of embodiment of described equipment 1 is described below with reference to Fig. 4.Identical parts are as retain identical Reference numeral according in the embodiment of Fig. 3, hereby referring to description of them.
With respect to according to the embodiment of Fig. 3 additionally, according in the embodiment of Fig. 4, additional top firing element 37 is arranged on described the second crucible 4.The heat that can further improve in described the second crucible 4 thus, injects.Especially can realize, the heat of controlling more targetedly in described the second crucible 4 by means of described top firing element 37 injects.Described top firing element 37 can be resistance heating element.Described top firing element 37 also can be configured to electron rays or laser source, or comprises this element.In this case, described the second crucible 4 can be especially little construct.It only especially can have and 0.5 rises to the capacity of 2 liters.Electron rays or laser source can be realized especially accurately and flexibly controlling of extra high energy injection and the melting to the bulk silicon 6 in described the second crucible 4.
The another kind of embodiment of described equipment 1 is described below with reference to Fig. 5.Identical parts are as retain identical Reference numeral according in the embodiment of Fig. 1, hereby referring to description of them.
According in the embodiment of Fig. 5, additional bottom-heated element 38 is arranged under described the second crucible 4.Thus, described bottom-heated element 38 is especially arranged in the region between described the first crucible and described the second crucible.The heat that can improve on the one hand in described the second crucible 4 thus, injects.In addition, by means of the described bottom-heated element 38 that simultaneously can be formed for the top firing element of described the first crucible 3, can be at least in part, especially complete, compensate the impact being caused by described the second crucible 4 in the temperature field in described the first crucible 3.
As Fig. 5 exemplary as shown in, can abandon the cover plate 28 on described the first crucible 3.This is also feasible in other embodiments.Equally, also can be according to cover plate 28 is set in the embodiment of Fig. 5.
In addition, in Fig. 5, schematically shown by way of example and be configured to the layout that delays element that connects a plate 39.A described plate 39 that connects can be arranged on described the second crucible 4.It also can be arranged on described chamber 9.Described in arranging, connect a plate 39, be especially provided with the holding device of being made by graphite.A described plate 39 that connects also can be arranged in the mode of height-adjustable.Drip plate 39 by means of described connecing, can make to be delayed before entering into the silicon melt 2 of described the first crucible 3 from the liquid-state silicon of described the second crucible 4.
The another kind of embodiment of described equipment 1 is described below with reference to Fig. 6.Identical parts are as retain identical Reference numeral according in the embodiment of Fig. 1, hereby referring to description of them.As shown in exemplary in Fig. 6, can abandon the side heat element 19 in the region of described the second crucible 4.Show simple especially solution in design according to the embodiment of Fig. 6.This solution especially can realize by adding to described the second crucible 4 and described storage vessel 8 to load onto to the e Foerderanlage 7 of the crystallizer existing.
In principle, described equipment 1 also can comprise two or more second crucibles 4 and/or two or more the first crucibles 3.These all crucibles can be arranged in identical chamber 9.
Claims (14)
1. the equipment for the production of silico briquette (1), it comprises:
A, at least one first container (3) for holding semiconductor melt;
B, at least one second container for holding semiconductor melt (4);
C, wherein, described at least one second container (4) has outlet (12), and via described outlet (12), liquid-state silicon can flow out to described at least one first container (3) from described at least one second container (4); And
D, wherein, described container (3,4) is arranged in common chamber (9).
2. equipment according to claim 1 (1), is characterized in that, the capacity (V of described second container (4)
2) be less than the capacity (V of described the first container (3)
1), i.e. V
2< V
1.
3. according to the equipment one of claim 1 to 2 Suo Shu (1), it is characterized in that, described equipment (1) comprises heating unit (15), and described heating unit (15) is applicable to not only in described the first container (3) but also in described second container (4), make silicon (6) melting.
4. equipment according to claim 3 (1), it is characterized in that, described heating unit (15) forms in the following way,, at silicon melt (2) setting up period making in described the first container (3), can make bulk silicon (6) melting in described second container (4).
5. according to the equipment one of aforementioned claim Suo Shu (1), it is characterized in that the 3rd container (8) for holding bulk silicon (6), described the 3rd container (8) is connected with described second container (4) via e Foerderanlage (7).
6. for the production of a method for silico briquette, it comprises the steps:
A, provide a kind of according to the equipment one of aforementioned claim Suo Shu (1);
B, in described the first container (3), provide silicon melt (2);
C, in described second container (4), provide silicon melt (2);
D, make described silicon melt (2) directional solidification in described the first container (3); And
E, liquid-state silicon is transferred to described the first container (3) from described second container (4).
7. method according to claim 6, is characterized in that, during described silicon melt (2) directional solidification making in described the first container (3), liquid-state silicon is transferred to described the first container (3) from described second container (4).
8. according to the method one of claim 6 to 7 Suo Shu, it is characterized in that, during one or more time period, continuously liquid-state silicon is transferred to described the first container (3) from described second container (4).
9. according to the method one of claim 6 to 8 Suo Shu, it is characterized in that, described the first container (3) has capacity (V
1), the liquid-state silicon of altogether transferring to described the first container (3) from described second container (4) has capacity (V
n), wherein, be suitable for: 0.05V
1≤ V
n.
10. according to the method one of claim 6 to 9 Suo Shu, it is characterized in that, the described transfer from described second container (4) to described the first container (3) realizes with the speed in 0.1kg/h to 10kg/h scope.
11. according to the method one of claim 6 to 10 Suo Shu, it is characterized in that, the silicon in described second container (4) has one or more hotchpotchs of predetermined concentration.
12. according to the method one of claim 6 to 11 Suo Shu, it is characterized in that, at silicon melt (2) setting up period making in described the first container (3), bulk silicon (6) is flowed to described second container (4) from the 3rd container (8) at least stagely.
13. methods according to claim 12, is characterized in that, the silicon (6) that flows to described second container has one or more hotchpotchs of predetermined concentration.
14. 1 kinds of silico briquettes, it is according to producing according to the method one of claim 6 to 13 Suo Shu.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102013203740.6A DE102013203740B4 (en) | 2013-03-05 | 2013-03-05 | Device and method for producing silicon blocks |
| DE102013203740.6 | 2013-03-05 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104032370A true CN104032370A (en) | 2014-09-10 |
Family
ID=51385482
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410068762.5A Pending CN104032370A (en) | 2013-03-05 | 2014-02-27 | Device for producing silicon blocks |
Country Status (3)
| Country | Link |
|---|---|
| CN (1) | CN104032370A (en) |
| DE (1) | DE102013203740B4 (en) |
| TW (1) | TWI547601B (en) |
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|---|---|---|---|---|
| CN101006205A (en) * | 2004-06-18 | 2007-07-25 | Memc电子材料有限公司 | Melter assembly and method for charging a crystal forming apparatus with molten source material |
| CN102126725A (en) * | 2011-01-29 | 2011-07-20 | 大连隆田科技有限公司 | Method and equipment for purifying polycrystalline silicon by melting in electron beam shallow pool |
| CN102272361A (en) * | 2008-11-10 | 2011-12-07 | Axt公司 | Systems, methods and substrates of monocrystalline germanium crystal growth |
| JP2012001435A (en) * | 2011-10-05 | 2012-01-05 | Solaicx Inc | System for continuous growth of single crystal silicon |
| US20120279437A1 (en) * | 2011-05-06 | 2012-11-08 | GT Advanced CZ, LLC | Growth of a uniformly doped silicon ingot by doping only the initial charge |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4018967A1 (en) * | 1990-06-13 | 1991-12-19 | Wacker Chemitronic | Polycrystalline silicon blocks with column crystallised structure |
| US20020062784A1 (en) | 1999-09-09 | 2002-05-30 | Pandelisev Kiril A. | Material purification |
| DE102005013410B4 (en) | 2005-03-23 | 2008-01-31 | Deutsche Solar Ag | Apparatus and method for crystallizing non-ferrous metals |
| DE102009021003A1 (en) | 2009-05-12 | 2010-11-18 | Centrotherm Sitec Gmbh | Process and apparatus for providing liquid silicon |
| DE102011002599B4 (en) | 2011-01-12 | 2016-06-23 | Solarworld Innovations Gmbh | Process for producing a silicon ingot and silicon ingot |
-
2013
- 2013-03-05 DE DE102013203740.6A patent/DE102013203740B4/en not_active Expired - Fee Related
-
2014
- 2014-02-10 TW TW103104251A patent/TWI547601B/en not_active IP Right Cessation
- 2014-02-27 CN CN201410068762.5A patent/CN104032370A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101006205A (en) * | 2004-06-18 | 2007-07-25 | Memc电子材料有限公司 | Melter assembly and method for charging a crystal forming apparatus with molten source material |
| CN102272361A (en) * | 2008-11-10 | 2011-12-07 | Axt公司 | Systems, methods and substrates of monocrystalline germanium crystal growth |
| CN102126725A (en) * | 2011-01-29 | 2011-07-20 | 大连隆田科技有限公司 | Method and equipment for purifying polycrystalline silicon by melting in electron beam shallow pool |
| US20120279437A1 (en) * | 2011-05-06 | 2012-11-08 | GT Advanced CZ, LLC | Growth of a uniformly doped silicon ingot by doping only the initial charge |
| JP2012001435A (en) * | 2011-10-05 | 2012-01-05 | Solaicx Inc | System for continuous growth of single crystal silicon |
Also Published As
| Publication number | Publication date |
|---|---|
| TWI547601B (en) | 2016-09-01 |
| DE102013203740A1 (en) | 2014-09-11 |
| TW201441434A (en) | 2014-11-01 |
| DE102013203740B4 (en) | 2020-06-18 |
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Application publication date: 20140910 |