The present invention relates to a method and to a device for obtaining a multicrystalline semiconductor material, in particular silicon, by melting of the semiconductor material and subsequent directional solidification thereof.
The demand for semiconductor material, in particular silicon, with a high degree of purity, referred to as “solar purity”, is increasingly higher, in so far as said material is necessary for the production of high-efficiency photovoltaic cells.
To obtain such a material refinements are first made by means of traditional metallurgical method, and, finally, an ingot is formed, from which the wafers necessary for production of the photovoltaic cells can then be sectioned. Said ingot is formed with a method known as “directional solidification system” (DSS), i.e., by melting the semiconductor material in a crucible and then causing a directional solidification thereof to obtain at the end multicrystalline silicon.
To obtain the directional solidification it is necessary to bring about said solidification in the crucible by maintaining a vertical thermal gradient in the ingot being formed so as to obtain a rate of cooling such as to obtain advance of the solidification front of 1-2 cm/h. An advantage of said technology is that the impurities present in the starting material remain preferentially in the molten material and consequently rise upwards together with the solidification front. Once the ingot is solidified, it is consequently sufficient to eliminate the top part of the ingot itself to obtain refined multicrystalline silicon at the desired degree
To obtain said result it is necessary to be able to exert a very precise control of the thermal flows, in particular preventing any lateral leakage of heat from the crucible, i.e., thermal flows in a direction transverse to that of advance of the solidification front, which is vertical. In known DSS furnaces, whether they be provided with heating with electrical resistors or with induction heating, this is obtained by using heavy insulating layers, which increase the costs and the overall dimensions of the furnace and, consequently, the levels of energy consumption for managing it. Furthermore, the step of melting of the solid semiconductor material to be refined requires long times and high levels of energy consumption.
The aim of the present invention is to overcome the drawbacks of the known art by providing a device and a method for obtaining a multicrystalline semiconductor material, typically silicon, with a “solar” degree of purity that will be simple and inexpensive to implement, will enable a reliable and effective control of the thermal flows, and will enable reduction of the overall dimensions and the levels of energy consumption of the necessary equipment.
Here and in what follows by “solar” degree of purity is meant the degree of purity necessary for producing high-efficiency photovoltaic cells.
The invention hence regards a device for melting and subsequent directional solidification of a semiconductor material, typically to obtain multicrystalline silicon with solar degree of purity, according to claim 1, and to a method for obtaining a multicrystalline semiconductor material with solar degree of purity, typically silicon, by means of a step of melting of the semiconductor material and a subsequent step of directional solidification of the semiconductor material, according to claim 9.
In particular, the device according to the invention comprises: at least one bottom induction coil, which is vertically mobile so as to be able to vary in use its distance from the bottom wall of a cup-shaped graphite container housing the crucible, in which the semiconductor material to be refined is contained; and at least one lateral induction coil, comprising a plurality of turns set coaxial, set on top of one another in the vertical direction; and means for selectively short-circuiting the turns, all together or separately one or more at a time, or respectively connecting them with, or disconnecting them from, all together or separately one or more at a time, the a.c. electrical-supply means; in addition, at least the lateral induction coil includes means for varying the frequency of electrical supply of the turns, all together or separately one or more at a time, between at least two different values and such as to produce by induction selective heating of the graphite and/or of the semiconductor material contained in the crucible, once the latter has reached the conduction temperature.
The means for varying the frequency of electrical supply of the turns comprise a first battery of capacitors and a second battery of capacitors, coupled to the means for selectively short-circuiting the turns or respectively connecting them with, or disconnecting them from, the a.c. electrical-supply means. The means for selectively short-circuiting the turns or respectively connecting them with, or disconnecting them from, the a.c. electrical-supply means in turn comprise a bank of switches appropriately connected.
According to the method of the invention, the step of solidification is obtained by means of the steps of:
deactivating the at least one bottom induction coil, keeping, however, in circulation in the turns thereof a flow of a coolant;
approaching the bottom induction coil to the crucible, until it is brought substantially into contact with a bottom susceptor set under the crucible;
Furthermore, the melting step is performed by means of the steps of:
In this way, the melting step is obtained in a fast way and with reduced levels of energy consumption, in so far as at least part of the necessary heat is developed directly within the material to be melted, a fact that moreover limits any leakage by irradiation by the susceptors. Furthermore, in particular by acting appropriately on the frequencies, an induced effect of stirring on the molten material is obtained, which renders it perfectly homogeneous, bringing it into the ideal conditions to perform then the directional solidification.
During the latter step it is moreover possible, by using appropriate temperature sensors and intervening then, on the basis of the readings thereof, on the individual induction coils, to maintain an extremely good control of the thermal flows, in particular using the possibility of short-circuiting and/or supplying separately the turns of the lateral induction coil/coils and using the bottom induction coil, deactivated, as cooling element.
Further characteristics and advantages of the invention will appear clearly from the ensuing description of a non-limiting example of embodiment thereof, illustrated purely by way of example with reference to the figures of the annexed drawings, wherein:
With reference to
The device 1 comprises: at least one crucible 3 for the semiconductor material 2, preferably made of quartz or ceramic material, removably housed in a cup-shaped graphite container 4; and a fluid-tight casing 5, housing inside it the graphite container 4 and delimited by a bottom half-shell 6 and by a top half-shell 7, which are cup-shaped; the latter, which are preferably made of steel, are normally coupled on top of one another (
The device 1 further comprises means 10 for moving vertically the top half-shell 7 away from the bottom half-shell 6, in the case in point in such a way that the casing 5 will assume an “open” configuration, illustrated in
The device 1 further comprises, according to one aspect of the invention: at least one top induction coil (or a “block” of a number of separate induction coils) 12, comprising respective turns 13 that can be shaped, for example, according to a plane spiral, set facing, with at least interposition of a graphite plate 14, a mouth 15 of the graphite container 4; at least one lateral induction coil 16 (or a “block” of a number of separate induction coils), set, in use, when the half-shells 6, 7 are coupled together (
Finally, the device 1 comprises: a.c. electrical-supply means 20, which are known and are consequently represented schematically simply by blocks, for supplying the induction coils 12, 16 and 18 separately and independently of one another; and cooling means 21, which are also known and are consequently represented schematically by blocks, for supplying a coolant within the turns 13 of the induction coils 12, 16 and 18, which turns are hollow in so far as they are constituted by tubular elements.
According to the invention, the bottom induction coil 18 is vertically mobile so as to be able to vary in use its distance D (
In particular, the turns 13a, . . . 13e are formed each by a respective copper tube, which is bent to form a ring in one and the same plane and having an axis of symmetry A, terminating with two opposite ends 22 set adjacent and bent to form an angle so as to project radially on the outside of the ring formed by the turn. The turns 13a, . . . 13e, which have all the same dimensions, are then set packed on top of one another, in the direction of extension of the axis A, which is vertical, and are held together in a single functional unit, by respective vices 23. The ends 22 are provided with connectors 24 designed to make the hydraulic connection thereof to the cooling means 21 (defined by a known hydraulic circuit provided with pumps, not illustrated for simplicity.) and the electrical connection to the supply means 20.
In combination with the aforesaid characteristics, the at least one lateral induction coil 16 (
In particular, the means 25 described above in their functional aspect, can be implemented so as to comprise a bank of switches 25b, appropriately connected in a way obvious for the person skilled in the art, once the functions assigned thereto have been defined, which is consequently not described in detail. It is clear in fact that the switches 25b can perform both the functions of short-circuiting the turns 13, one or more at a time, represented schematically by the clip in
According to a last but by no means least important aspect of the invention, at least the lateral induction coil 16 (and possibly also the bottom induction coil 18) includes means 26 (illustrated as integrated in the block 25 in
In the case in point illustrated, the means 26 for varying the frequency of electrical supply of the turns 13a, . . . 13e comprise a first battery 27, and a second battery 28, illustrated schematically, of capacitors, coupled to the electrical-connection means 25 and in particular electrically connected to the bank of switches 25b.
The variation of the frequency of supply of the turns 13 produces a selective and localized variation of the magnetic field that comes to involve in use both the graphite elements 17, 19, and the semiconductor material 2 itself. A further or alternative localized variation of the magnetic field produced by the induction coil 16 considered as a whole can then be obtained by causing variation of the overall inductance thereof, for example, by disconnecting one or more turns 13 from the a.c. electrical-supply means 20.
In the preferred embodiment, the bottom half-shell 6 supports inside it the graphite container 4 by means of thermally insulating elements 29, as well as the bottom induction coil 18 and means 30, represented schematically with a block, for displacing vertically the latter away from and towards the bottom wall 19 of the graphite container 4. The means 30 can be constituted by any known motor that acts for vertical translation of a stem 31, which supports fixedly, at its top end, the plane induction coil 18 and carries inside it hydraulic and electrical lines for connection to the cooling means 21 and to the a.c. supply means 20 dedicated to the induction coil 18.
Instead, the top induction coil 12, together with the graphite plate 14, the lateral induction coil 16 and other insulating elements 29, are fixed with respect to the top half-shell 7 so as to surround the graphite container 4 with the half-shells 6, 7 coupled to one another (
In particular, it should be noted that the insulating elements 29 define, with the half-shells 6, 7 coupled, a compartment set within which is the at least one bottom induction coil 18, which thus directly faces the susceptor 19 associated thereto, whilst the insulating elements 29 surround the susceptors 14, 17, 19 so that the induction coils 12 and 16 are, instead, preferably arranged on the outside of said compartment and, hence, with the insulating elements 29 set between them and the susceptors 14, 17 associated thereto.
In a known way, the device 1 described comprises also known means 32, indicated by a block (
According to a final aspect of the invention, the cooling means 21 are made so that the coolant used by them that circulates in the hollow turns 13 of at least one of the induction coils 12, 16, 18, for example, those of the induction coil 18, can be a diathermic oil, instead of water. In this way, in the case of any leakage of coolant within the casing 5, during the process of melting or of directional solidification, or in the event of failure of the crucible 3 with Consequent spilling of the molten silicon 2 in the bottom half-shell 6, there is no risk of explosions consequent upon the possible chemical reactions of silicon with water.
On the basis of what has been described, it is clear that, by means of the device 1 it is possible to implement effectively a method for obtaining a multicrystalline semiconductor material with solar degree of purity, typically silicon, by means of a step of melting of the semiconductor material 2 and a subsequent step of directional solidification of the semiconductor material 2 itself obtained by using at least three induction coils, in the case in point the induction coils 12, 16 and 18, which can be supplied separately and independently of one another in alternating current and are arranged respectively at the top, at the bottom, and alongside a crucible 3 containing the semiconductor material 2, with interposition of graphite susceptors 14, 17, and 19. In particular, according to the method of the invention, the step of solidification is obtained by means of the steps of:
deactivating the bottom induction coil 18, keeping, however, in circulation in the turns 13 thereof a flow of a coolant;
approaching the bottom induction coil 18 to the crucible 3, until it is brought substantially into contact with the bottom susceptor 19 set under the crucible 3;
activating and deactivating selectively and independently of one another one or more turns 13a . . . 13e of the lateral induction coil 16, having obtained said turns as turns set coaxial to one another in the vertical direction and so as to cover in use at least the entire height occupied in the crucible 3 by the molten semiconductor material 2, in such a way as to achieve by induction a localized production of heat in the susceptor 17 set alongside the crucible 3 such as to compensate for the lateral thermal leakages of the crucible 3 itself; and
selectively short-circuiting at least one turn 13a . . . 13e at a time of the lateral induction coil 16, selecting the turn or turns to be short-circuited from among the ones set progressively higher up (i.e., 13e . . . 13a), so as to form with it/them a shield of electromagnetic field that follows substantially the solidification front of the semiconductor material 2.
Once again according to an aspect by no means less important of the invention, the melting step is obtained by means of the steps of:
activating the induction coils 12, 16 and 18 supplying them at a first pre-set frequency such as to produce by electromagnetic induction heating of the susceptors 14, 17, 19; and
as soon as the semiconductor material 2 is heated by the susceptors 14, 17, 19 to a temperature such as to become conductive (for example approximately 900° C. for silicon), reducing the frequency of supply of at least some turns 13 of the lateral induction coil 16 and, possibly, of the bottom induction coil 18, down to a second pre-set frequency in which at least part of the electromagnetic induction comes to involve directly the semiconductor material 2.
The first pre-set frequency is chosen in the kilohertz range, typically around approximately 2 kHz, whereas the second pre-set frequency is chosen in a range from a few hertz to hundreds of hertz, typically approximately 500 Hz. With the silicon at the conduction temperature, it has been seen that the frequency of 500 Hz ensures a direct supply of power in the silicon of approximately 300 of the power supplied by the supply means 20, whereas at 50 Hz all the power supplied by the supply means 20 enters the silicon.
Finally, according to the method of the invention, at least before implementing the step of directional solidification, the semiconductor material 2 in the molten state and/or in the state of incipient melting is stirred to'cause homogenization thereof by causing localized variation in the semiconductor material 2 of the frequency and/or intensity of the magnetic field so as to produce in the material 2 itself convective motions. Said localized variation of the magnetic field is obtained by supplying at least some of the turns 13a . . . 13e of the lateral induction coil 16 at an appropriate frequency, of some orders of magnitude lower than that used for heating the susceptors 14, 17, 19 and/or by not supplying at least one of the turns 13a . . . 13e of the lateral induction coil 16 so as to vary the inductance thereof.
Number | Date | Country | Kind |
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TO2009A000793 | Oct 2009 | IT | national |
Filing Document | Filing Date | Country | Kind | 371c Date |
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PCT/IB2010/002685 | 10/10/2010 | WO | 00 | 8/2/2012 |