JP2009249232A - Method and apparatus for growing silicon crystal by applying magnetic field - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide an apparatus and method for growing a silicon crystal by applying magnetic field, in which a rare earth-based permanent magnet is used as a magnetic field generation means in the growth of a silicon single crystal under a condition that a magnetic field is applied, and the apparatus cost (initial cost) and the operation cost (running cost) are thereby low and operations can be easily performed. <P>SOLUTION: In the apparatus for growing a silicon single crystal 9 by applying a magnetic field to a silicon melt 6, permanent magnets 3, 3' are provided as a magnetic field generation means for generating a magnetic field. The silicon melt 6 is accommodated in a crucible 5 and a magnetic field generated by the permanent magnets 3, 3' is applied to the crucible 5. As the permanent magnets 3, 3', rare earth-based permanent magnets are used. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention mainly relates to the field of semiconductor silicon (Si) crystal growth technology. In particular, the present invention relates to a technology for growing large (large diameter, long), high-quality Si single crystals by a rotating pull-up method (Czchoralski: CZ method) from a conductive Si melt melted in a quartz crucible. The present invention relates not only to Si but also to the technical field of compound semiconductor crystal growth such as GaAs and InP. The present invention relates to a technique for applying a magnetic field when growing a single crystal such as Si.

  In recent years, in growing Si single crystals for LSI substrates, a DC magnetic field is applied to the melt in the crucible in order to grow large-diameter dislocation crystals with a diameter of 300 mm or more, particularly with high yield while ensuring the uniformity of oxygen concentration distribution. Technology is essential.

  Also in the growth of Si single crystals for solar cell substrates, application of a magnetic field is becoming an indispensable technique for growing large-diameter dislocation-free single crystals having a diameter of about 200 mm or more, particularly at a low oxygen concentration.

  The history of applying a magnetic field during the growth of a semiconductor single crystal such as Si has a long history, dating back to the beginning of the 1980s. As shown schematically in FIG. 1, a horizontal magnetic field application (HM-CZ) method (FIG. 1 (a )), A vertical magnetic field (VM-CZ) method (FIG. 1B), a cusp magnetic field (CM-CZ) method (FIG. 1C), and the like have been proposed and studied.

  After that, the HM-CZ system characterized by non-axisymmetric magnetic field distribution with respect to the melt in the crucible targeted for the rotation axis and the CM-CZ system representing the axially symmetric magnetic field distribution are practical technologies, It has become an indispensable technique for growing shape and high-quality Si single crystals, and has been widely used.

  For example, Patent Document 1 discloses a silicon single crystal manufacturing method in which a magnetic field is applied by applying a current to a coil, and Patent Document 2 discloses a superconducting magnet device that applies a magnetic field using a superconducting magnet.

Japanese Patent Laid-Open No. 2002-249397 JP 2004-165538 A

  As mentioned in the “technical background” in the previous section, applying a magnetic field when growing a single crystal such as Si can improve the efficiency of the crystal growth process and greatly improve the quality of the grown crystal. It has been revealed by many studies conducted in the early 1980s.

  Nonetheless, the magnetic field application technology has been applied to practical use for some single-use crystal growth (for example, low oxygen concentration crystals for discrete semiconductor devices), and has been widely applied and put to practical use for Si single crystal growth. Did not come.

  The biggest decisive reason is that the device for generating a strong DC magnetic field for applying the magnetic field is very large, and as a result, the device price is very high (initial cost), and This is because the operation of the apparatus (running cost) has a large number of disadvantages such as a large amount of expenses required.

  As conventional DC magnetic field generation methods, the following two methods are broadly proposed and put into practical use.

  One method is to generate a DC magnetic field by passing a DC current through the coil, and achieve the required strength and distribution of the magnetic field, depending on the shape and dimensions of the coil, the location of the ferromagnetic core, and the magnitude of the flowing current. It is a method to do.

  The feature of this magnetic field generation method / technique is that there is an advantage that the magnetic field strength can be arbitrarily adjusted (including zero magnetic field strength except during crystal growth) by the flowing current. Requires a large current and a large electric power, and the running cost becomes enormous (the electric power equivalent to or higher than that required for crystal growth is consumed to generate a magnetic field), and the entire magnetic field generator is large and heavy. There are major drawbacks.

  Another method is to generate a strong DC magnetic field using a superconducting magnet to achieve the required magnetic field strength and magnetic field distribution.

  The feature of this magnetic field generation method / technique is that it can generate a magnetic field with the required strength with a relatively small device, and the power required to generate the magnetic field is very small. On the other hand, in addition to the major disadvantage that the production price of superconducting magnets is very high, it is difficult to arbitrarily adjust the magnetic field strength in terms of device operation (including making the magnetic field strength zero except during crystal growth). Problems such as a number of complex and unstable factors remain above.

  As mentioned earlier, the reason why magnetic field application technology was already found to be a very effective technology for growing high-quality Si crystals in the early 1980s was not used for a long time. First, it can be said that the magnetic field application device as described above is very expensive (including both initial cost and running cost), and as a result, is reflected in the high cost of the Si wafer to be produced.

  However, even in the case of a magnetization application device having many drawbacks and problems as described above, magnetic field application must be applied as an essential technology in the field of growing large and high-quality Si single crystals having a diameter of 200 mm or more in recent years. In reality, there is a strong demand for the emergence of new technologies that can solve the above-mentioned drawbacks and problems.

  The present invention uses a rare earth-based permanent magnet as a magnetic field generating means in magnetic field application silicon single crystal growth, so that the apparatus price (initial cost) and operation cost (running cost) are low and the operation is easy. An object is to provide a crystal growth method and apparatus.

  The magnetic field application silicon crystal apparatus according to claim 1, which has been made to achieve the above object, is a magnetic field application silicon crystal growth apparatus for growing a silicon crystal by applying a magnetic field to a silicon melt. A permanent magnet is provided as the magnetic field generating means for generating the magnetic field.

  A magnetic field application silicon crystal device according to a second aspect is the one described in the first aspect, wherein the permanent magnet is a rare earth magnet.

  The magnetic field application silicon crystal device according to claim 3 is the one described in claim 1 or 2, and applies an axially symmetric magnetic field to an axisymmetric crucible containing the silicon melt. The permanent magnet is arranged in a part of the magnetic circuit.

  The magnetic field applying silicon crystal device according to claim 4 is the magnetic crystal applying device according to claim 3, wherein the magnetic circuit has a pair of permanent magnets on an inner wall of a ring-shaped yoke that horizontally surrounds the crucible. A plurality of sets in which the magnetic poles are arranged opposite to each other in the opposite direction to the upper part of the inner wall and the lower part of the inner wall are arranged at equal intervals along the inner wall.

  The magnetic field application silicon crystal device according to claim 5 is the one described in claim 1 or 2 for applying a non-axisymmetric magnetic field to an axisymmetric crucible containing the silicon melt. The permanent magnet is arranged in a part of the magnetic circuit.

  A magnetic field application silicon crystal device according to claim 6 is the one described in claim 5, wherein the magnetic circuit is configured by connecting a pair of opposing yokes with the crucible interposed therebetween by the permanent magnet. It is characterized by being.

  The magnetic field applying silicon crystal device according to claim 7 is the magnetic crystal applying device according to claim 5, wherein the magnetic circuit is configured by connecting a pair of opposing permanent magnets with the crucible interposed therebetween with a yoke. It is characterized by being.

  A magnetic field applying silicon crystal device according to an eighth aspect is the one described in the third to seventh aspects, wherein the permanent magnet is used as means for changing the strength and distribution of the magnetic field applied to the silicon melt. The structure (shape and size) of a part of the magnetic circuit including the structure is changed, and / or the relative position between the silicon melt and the magnetic circuit is changed.

  The magnetic field application silicon crystal device according to claim 9 is the one described in any one of claims 1 to 8, wherein the magnetic field application process is not required except for crystal growth (cooling process after crystal growth, crystal A magnetic field applying device that includes the permanent magnet and applies the magnetic field during a take-out process, a furnace cleaning process, a crystal growth preparation process (such as crucible and raw material filling, seed crystal attachment), and a raw material melting process) It is characterized in that it has a function / structure for separating or moving all or a part of this from the magnetic field applying silicon crystal growing apparatus and storing it in a standby place with necessary conditions.

  The magnetic field application silicon crystal growth method according to claim 10 is characterized in that a silicon melt is accommodated in a crucible and a silicon crystal is grown by applying a magnetic field generated by a permanent magnet to the crucible. To do.

  A magnetic field application silicon crystal growth method according to an eleventh aspect is the one described in the tenth aspect, wherein a rare earth magnet is applied to the permanent magnet and a magnetic field generated by the rare earth magnet is applied to the crucible. It is characterized by.

  The magnetic field application silicon crystal growth method according to claim 12 is the one described in claim 10 or 11, wherein the permanent magnet is disposed in a part of a magnetic circuit, and the silicon melt is placed in the axisymmetric crucible. The silicon crystal is grown by applying an axially symmetric magnetic field to the crucible with the magnetic circuit.

  The magnetic-field-applied silicon crystal growth method according to claim 13 is the one described in claim 10 or 11, wherein the permanent magnet is arranged in a part of a magnetic circuit, and silicon melt is applied to the axisymmetric crucible. The silicon crystal is grown by applying a non-axisymmetric magnetic field to the crucible with the magnetic circuit.

  The magnetic field application silicon crystal growth method according to claim 14 is the method according to claim 12 or 13, wherein the structure (shape and size) of a part of the magnetic circuit including the permanent magnet is changed, or The relative position between the silicon melt and the magnetic circuit is changed to change the strength and distribution of the magnetic field applied to the silicon melt.

  The magnetic field application silicon crystal growth method according to claim 15 is the method described in any one of claims 10 to 14, wherein a step that does not require magnetic field application other than during crystal growth (cooling step after crystal growth, During the crystal extraction process, the furnace cleaning process, the crystal growth preparation process (crucible and raw material filling, seed crystal mounting, etc.), raw material melting process, etc.) The part is separated and moved from the magnetic field applying silicon crystal growing apparatus, and stored in a standby place having necessary conditions.

  As described above in detail in the technical background related to the present invention, the problems to be solved by the invention in the disclosure of the invention and the means for solving the problems, the Si single crystal growth and solar cell for LSI substrates having a diameter of 300 mm or more In the field of magnetic field application technology that is becoming an essential technology in the growth of Si single crystals for substrates, there are the following specific effects.

  (1) By using a permanent magnet as a means for generating a strong magnetic field, the price (initial cost) of the magnetic field application device can be greatly reduced to 1/2 to 1/5.

  (2) Similarly, by using a permanent magnet, its operating cost (running cost) can be drastically reduced (basically no operating cost is required).

  (3) Similarly, by using a permanent magnet, the configuration and structure of the apparatus are simplified, and the operation of the apparatus is simplified and facilitated.

  (4) By devising the configuration and structure of the magnetic circuit to be applied, it is possible to control the required magnetic field distribution (the direction of the magnitude of the magnetic field) with a simple operation.

  (5) By devising the configuration and structure of the magnetic circuit to be applied, in a process that does not require the application of a magnetic field, all or part of the magnetic field application device to which a permanent magnet is applied is separated and moved from the crystal growth device; It is also possible to store in a standby place with necessary conditions.

  As described above, the present invention applies a permanent magnet in place of an electromagnet or a superconducting magnet that generates a magnetic field by flowing a large current through a conventional coil in order to solve the disadvantages and problems of the conventional magnetic field application crystal growing apparatus. This is the main point.

  As a permanent magnet material to be applied in particular, it is an important viewpoint of the present invention that the shortcomings and problems of the prior art can be easily solved by applying rare-earth ferromagnets whose technological progress has been remarkable in recent years. .

  The rare earth magnet is a magnet made of a rare earth element (Group 3 element or lanthanoid excluding actinium), and examples thereof include a samarium cobalt magnet, a neodymium magnet, and a praseodymium magnet.

  FIG. 2 is a schematic view showing an embodiment of a Si crystal growing apparatus for explaining an example of the problem solving means of the present invention. FIG. 2A is an elevational (sectional) view when a non-axisymmetric magnetic field according to the present invention is applied, and FIG. 2B is a plan (sectional) view.

  In FIG. 2, 1 is a permanent magnet according to the present invention, 2 and 2 'are yokes forming a magnetic circuit, and 3 and 3' are a magnetic pole (N pole) and a magnetic pole (S pole), respectively.

  Similarly, in FIG. 2, reference numeral 4 denotes a chamber of the main part of the Si crystal growth apparatus arranged so as to be sandwiched between the magnetic pole (N pole) 3 and the magnetic pole (S pole) 3 ′.

  Further, inside the chamber 4, a Si melt 6 melted in a quartz crucible 5 usually required for Si crystal growth, a heating element 7 and a heat insulating material 8 for heating the quartz crucible 5 and the Si melt 6. And the like are not different from the configuration of a normal pulling (Czchoralski: CZ) Si single crystal growth apparatus.

  FIG. 2 shows a state where the Si single crystal 9 that is actually growing is pulled upward by the crystal pulling wire-10.

  In FIG. 2, in the conventional electromagnet system, as a means for generating a magnetic field, a large current coil (winding) is arranged in a part of the magnetic circuit. Thus, the permanent magnet 1 made of a rare earth magnet material or the like is disposed in a part of the magnetic circuit. Specifically, the magnetic circuit is configured by connecting a pair of opposing yokes with a crucible interposed therebetween by a permanent magnet 1 of a rare earth magnet. Thus, by using a rare earth magnet, a magnetic field of about 0.04 to 0.4 T (Tesla) can be generated between the magnetic poles 3 and 3 '.

  In FIG. 2 of one embodiment of the present invention, in addition to the shape and dimensions of the permanent magnet 1, the shapes and dimensions of the yokes 2, 2 'and the magnetic poles 3, 3' are variously adjusted at the time of designing the magnetic circuit. Thus, it is possible to apply a predetermined magnetic field strength (magnitude and direction) to the Si melt 6 in the quartz crucible 5.

  FIG. 3 is a plan (cross-sectional) view showing a schematic diagram of an Si crystal growing apparatus in the case of applying a non-axisymmetric magnetic field for explaining another example of the problem solving means of the present invention.

  In FIG. 3, the permanent magnets 1 and 1 'according to the present invention are characterized in that they are arranged in the magnetic pole part of the magnetic circuit. The permanent magnet 1 constitutes the N pole and the permanent magnet 1' constitutes the S pole. . That is, the magnetic circuit is configured by connecting a pair of opposing permanent magnets 1 and 1 ′ with a crucible interposed therebetween by a yoke.

  Also, the difference between FIG. 3A and FIG. 3B is that sliding portions 11, 11 ′ are provided in part of the yoke 2, 2 ′ of the magnetic circuit, and the sliding portions 11, 11 ′ are slid. The magnetic field strength between the magnetic poles 1 and 1 ′ can be adjusted by changing the distance (interval) of the magnetic poles 1 and 1 ′ from L to L ′ by moving.

  Further, the function of changing the magnetic pole interval by the sliding portions 11 and 11 ′ is an important function that also serves to facilitate separation and movement of the whole or a part of the magnet device from the crystal growth device portion. .

  FIG. 4 is an elevational (sectional) view of a schematic diagram for explaining means for adjusting the magnetic field distribution of the Si melt 6 part in the quartz crucible 5 of the non-axisymmetric magnetic field according to the present invention.

  In FIG. 4, by adjusting the relative position between the magnetic poles 1, 1 ′ and the crystal growing device 4 up and down, the center position of the magnetic field is in the vicinity of the surface of the melt in the case of FIG. In the case of FIG. 4B, the magnetic field distribution of the Si melt 6 in the quartz crucible 5 can be easily changed so that the center position of the magnetic field is at the bottom of the quartz crucible 5.

  Adjusting the relative position between the magnetic poles 1 and 1 'and the crystal growing device 4 up and down is not easy to move a current circuit with a large amount of cooling water in the conventional electromagnet system. It is also a great feature of the present invention that it is possible easily with the permanent magnets related to the above.

  FIG. 5 is an elevation (cross-sectional) view (FIG. 5 (a)) and a plan view showing the configuration of a magnetic circuit for applying an axially symmetric magnetic field to an axisymmetric crucible 5 containing a silicon melt. (Cross section) FIG. (FIG.5 (b)).

  In FIG. 5, permanent magnets 12 and 12 'are fixed via a yoke 13 constituting a magnetic circuit to form an independent permanent magnet 14, and a magnetic field distribution 15 is given to the crucible 5 portion.

  The plan (cross-sectional) view of FIG. 5B shows a case where four independent permanent magnets 14 are arranged at intervals of 90 °, and four times having the same rotational axis with respect to the axially symmetric crucible 5. A magnetic field distribution 15 with rotational axis symmetry can be provided.

  FIG. 6 is an elevational view (cross section) showing an example of a more practical configuration of a magnetic circuit configuration for applying an axially symmetric magnetic field to the axially symmetric crucible 5 containing the silicon melt of FIG. FIG. 6 (FIG. 6A) and a plan (cross-sectional) view (FIG. 6B).

  FIG. 6 corresponds to the case where 16 independent permanent magnets 14 described in FIG. 5 are arranged at intervals of 22.5 °, and the two permanent magnets 12 and 12 ′ are formed by a ring-shaped common yoke 16 to form a magnetic circuit. The magnetic field application apparatus according to the present invention is formed as a whole. In other words, the magnetic circuit has a ring-shaped yoke 16 that horizontally surrounds the crucible 5 and a pair of permanent magnets 12 and 12 ′ facing the upper and lower portions of the inner wall in the opposite direction, S and N poles. A plurality of sets are arranged at equal intervals along the inner wall.

  FIG. 7 shows a process of applying a magnetic field having an axial symmetry explained with reference to FIG. 6 without applying a magnetic field (cooling process after crystal growth, crystal extracting process, in-furnace During the cleaning process, crystal growth preparation process (crucible and raw material filling, seed crystal mounting, etc.), raw material melting process, etc.) all or part of the magnetic field application device to which a permanent magnet is applied is removed from the crystal growth device. It is explanatory drawing which shows the specific method in the case of isolate | separating and moving, and storing in the standby place provided with the required conditions.

  7A, the common yoke 16 is designed and manufactured in advance so that it can be separated into two semicircular magnet devices 12 ′ and 12 ″. As a result, as shown in FIG. 12 'and 12 "can be separated from chamber-4.

  Further, the magnet devices 12 ′ and 12 ″ are separated from the crystal growth device, and moved to and stored in a storage place 17 having conditions necessary for safely storing the magnet device such as a magnetic shield function. Is also possible.

  The permanent magnet used in the present invention is not limited to a rare earth magnet, and any permanent magnet that generates a magnetic field of the same level or higher can be used.

FIG. 1 is a schematic diagram of three types of magnetic field application methods in conventionally known magnetic field application silicon crystal growth. FIG. 2 is a schematic view showing an embodiment of a non-axisymmetric magnetic field application silicon crystal growing apparatus for explaining an example of the problem solving means of the present invention. FIG. 3 is a schematic view of a silicon crystal growing apparatus in the case of applying a non-axisymmetric magnetic field for explaining another example of the problem solving means of the present invention. FIG. 4 is an elevational (sectional) view of a schematic diagram for explaining means for adjusting the magnetic field distribution of a non-axisymmetric magnetic field according to the present invention. FIG. 5 is a schematic diagram showing a configuration of a magnetic circuit for applying an axially symmetric magnetic field. FIG. 6 is a schematic diagram showing an example in which the magnetic circuit configuration for applying the axially symmetric magnetic field in FIG. 5 is made more practical. FIG. 7 shows a configuration of a magnetic field applying apparatus characterized by applying the axially symmetric magnetic field described with reference to FIG. 6. All or part of the magnetic field applying apparatus to which a permanent magnet is applied is separated from the crystal growing apparatus. It is explanatory drawing which shows the specific method in the case of moving and accommodating in the standby place provided with the required conditions.

Explanation of symbols

  1, 1 'is a permanent magnet, 2, 2' is a yoke, 3 is a magnetic pole (3 is an N pole, 3 'is an S pole), 4 is a chamber of a crystal growth apparatus, 5 is a crucible, 6 is a silicon melt, 7 is a heating element, 8 is a heat insulating material, 9 is a grown silicon crystal, 10 is a crystal pulling wire, 11 is a sliding part, 12 and 12 'are permanent magnets, 12' and 12 "are magnet devices, and 13 is a joint Iron, 14 is an independent magnet device, 15 is an example of magnetic field distribution, 16 is a common yoke, and 17 is a storage location of the magnet device.

Claims (15)

  A magnetic field applying silicon crystal growing apparatus for growing a silicon crystal by applying a magnetic field to a silicon melt, comprising a permanent magnet as a magnetic field generating means for generating the magnetic field.   The magnetic field application silicon crystal growing apparatus according to claim 1, wherein the permanent magnet is a rare earth magnet.   3. The permanent magnet is disposed in a part of a magnetic circuit for applying an axially symmetric magnetic field to an axially symmetric crucible containing the silicon melt. The magnetic field application silicon crystal device described.   The magnetic circuit is a set in which a pair of permanent magnets are arranged on the inner wall of a ring-shaped yoke that horizontally surrounds the crucible with the magnetic poles facing the upper part of the inner wall and the lower part of the inner wall in opposite directions. The magnetic field applying silicon crystal device according to claim 3, wherein a plurality of sets are arranged at equal intervals along the inner wall.   3. The permanent magnet is disposed in a part of a magnetic circuit for applying a non-axisymmetric magnetic field to an axisymmetric crucible for storing the silicon melt. The magnetic field application silicon crystal growth apparatus described in 1.   6. The magnetic field application silicon crystal growing apparatus according to claim 5, wherein the magnetic circuit is configured by connecting a pair of opposing yokes with the crucible interposed therebetween by the permanent magnet.   6. The magnetic field application silicon crystal growing apparatus according to claim 5, wherein the magnetic circuit is configured by connecting a pair of opposing permanent magnets with the crucible interposed therebetween by yokes.   As means for changing the strength and distribution of the magnetic field applied to the silicon melt, changing the structure (shape and size) of a part of the magnetic circuit including the permanent magnet, and / or the silicon melt and the silicon melt 8. The magnetic field application silicon crystal growing apparatus according to claim 3, wherein a relative position of the magnetic circuit is changed.   Processes that do not require the application of a magnetic field except during crystal growth (cooling process after crystal growth, crystal extraction process, furnace cleaning process, crystal growth preparation process (crucible and raw material filling, seed crystal mounting, etc.), raw material During the melting step, etc., all or part of the magnetic field applying device that includes the permanent magnet and applies the magnetic field is separated from the magnetic field applying silicon crystal growing device and moved to a standby place with necessary conditions. 9. The magnetic field application silicon crystal growing device according to claim 1, further comprising a function / structure for housing.   A magnetic field application silicon crystal growth method characterized by containing a silicon melt in a crucible and growing a silicon crystal by applying a magnetic field generated by a permanent magnet to the crucible.   The magnetic field application silicon crystal growth method according to claim 10, wherein a rare earth magnet is applied to the permanent magnet, and a magnetic field generated by the rare earth magnet is applied to the crucible.   The permanent magnet is disposed in a part of the magnetic circuit, the silicon melt is accommodated in the axisymmetric crucible, and the silicon crystal is grown by applying an axially symmetric magnetic field to the crucible in the magnetic circuit. The magnetic field application silicon crystal growth method according to claim 10 or 11, wherein:   The permanent magnet is disposed in a part of the magnetic circuit, the silicon melt is accommodated in the axisymmetric crucible, and a non-axisymmetric magnetic field is applied to the crucible by the magnetic circuit to form the silicon crystal. The method of growing a magnetic field-applied silicon crystal according to claim 10 or 11, wherein the method is grown.   A magnetic field applied to the silicon melt by changing the structure (shape and size) of a part of the magnetic circuit including the permanent magnet or / and changing the relative position of the silicon melt and the magnetic circuit. 14. The method for growing a magnetic field-applied silicon crystal according to claim 12, wherein the intensity and distribution of the magnetic field are changed.   Processes that do not require application of a magnetic field except during crystal growth (cooling process after crystal growth, crystal removal process, furnace cleaning process, crystal growth preparation process (crucible and raw material filling, seed crystal mounting, etc.), raw material During the melting step, etc., all or a part of the magnetic field applying device to which the permanent magnet is applied is separated from the magnetic field applying silicon crystal growing device and moved and stored in a standby place having necessary conditions. The magnetic field application silicon crystal growth method according to any one of claims 10 to 14.

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