JP5067403B2 - Single crystal pulling device - Google Patents

Description

  The present invention relates to a single crystal pulling apparatus for growing a single crystal by the Czochralski method.

The Czochralski (CZ) method is used as a method for growing a single crystal rod such as silicon. The CZ method is, for example, a method in which a silicon polycrystalline raw material is melted in a quartz crucible, a single crystal seed crystal (seed) is immersed in a silicon melt, and the single crystal rod is pulled up while rotating.
In such a single crystal pulling apparatus, there are a method of using a shaft and a method of using a wire as a means for pulling a seed, but in recent years, a wire system that can reduce the pulling mechanism by increasing the pulling apparatus is the mainstream. .

An example of such a single crystal pulling apparatus using a wire is shown in FIG.
In the single crystal pulling apparatus 101 shown in FIG. 4, a crucible 107 capable of moving up and down containing a raw material melt 106 is housed in a main chamber 102 for growing a single crystal, and grown on the upper part of the main chamber 102. An upper chamber 103 for pulling up and taking out the single crystal is continuously provided. The upper chamber 103 is connected to the pull chamber 104 for storing the grown single crystal and the upper chamber, and is a sub chamber for retracting and storing the seed chuck 112 and the seed (seed crystal) 113 when the single crystal is taken out. 105.

When growing a single crystal using such a single crystal pulling apparatus 101, the seed 113 attached to the seed chuck 112 is immersed in the raw material melt 106, and then the seed 113 is moved in a desired direction by the pulling mechanism 108. The wire 111 is gently wound up while being rotated to grow a single crystal at the tip of the seed 113. At this time, in order to eliminate the dislocation that occurs when the seed 113 is deposited in the melt, the crystal at the initial stage of growth is once narrowed (necked), and the diameter is expanded to a desired diameter when the dislocation is removed, We will grow single crystals of the desired quality.
At this time, argon gas is supplied from the gas supply source 110 into the furnace through the upper chamber 103 and single crystal pulling is performed while discharging the gas in the furnace from the lower part of the main chamber 102 by the vacuum pump 109.

  In the single crystal pulling of the CZ method using such a single crystal pulling apparatus, the amount of silicon evaporation is such as a step of melting a silicon polycrystal raw material or a necking (drawing) step of immersing a seed to form a thin diameter portion. In many processes, silicon oxide adheres to the upper chamber and wires. Since the diameter of the quartz crucible is increased in the recent pulling apparatus, the evaporation amount of silicon oxide is also increased.

Further, the wire of the single crystal pulling apparatus is a non-rotating wire in which a tungsten wire or the like as shown in FIG. 5 is twisted. FIG. 5 shows three patterns of configuration examples of cross sections of wires used in a single crystal pulling apparatus. As shown in FIG. 5, the wire of the single crystal pulling device is a twist of a large number of strands. When a load is applied, the strands of the wires are returned and the wires are stretched. There is a possibility of dust generated by rubbing and adhering.
Further, since the wire is wound while being in contact with the pulley and the drum of the winding unit in the pulling mechanism, the abrasion powder (metal powder) of the pulley is generated by the friction between the metal pulley and the wire.

  Growing a silicon single crystal is called dislocation-free (DF). However, when slip dislocations enter and become dislocations when growing a single crystal, it must be remelted and grown again (DF). The cause of such slip dislocation is considered to be the fall of the oxide or metal powder adhering to the wire described above into the melt, and the oxide or metal powder floats in the molten silicon melt. Then, by being taken in during crystal growth, slip dislocation occurs due to the contaminant, and the crystal is dislocated.

As a conventional countermeasure against dislocation, the chamber, hot zone (in-furnace member), or wire is cleaned between operations. When dislocation is repeated during crystal growth, the dislocation crystal is taken out, the gate valve is closed, the upper chamber is cleaned, the wire is cleaned, and the production of the single crystal rod is resumed.
As a method for cleaning the wire, there are a method in which compressed air is blown to remove oxides and metal powders, and a method in which cotton is dipped in alcohol and wiped off. Cleaning by blowing air may contaminate the inside of the chamber or the pulling chamber, and the cleaning operation is difficult and burdensome because the chamber and the wire are at a high place. Further, since the cleaning operation cannot be performed unless the inside of the chamber is returned to the normal pressure, the operation takes half a day. If the cleaning in the lifting mechanism is included, one day is consumed.

  As such wire cleaning, Patent Documents 1 and 2 disclose a mechanism for blowing air to the wire and a mechanism for vibrating the wire.

JP 2001-348295 A JP 2001-348293 A

  However, in the technique disclosed above, there is a problem that the adhered matter on the wire cannot be removed, and the inside of the chamber is contaminated by dust generated during wire cleaning.

  The present invention has been made in view of the above problems, and provides a single crystal pulling apparatus that can clean a wire used for pulling a single crystal with high cleanliness and efficiency without contaminating the inside of the chamber. The purpose is to provide.

  In order to achieve the above object, the present invention provides at least a single crystal pulling method for pulling a single crystal grown in a crucible stored in a main chamber into an upper chamber connected to the upper portion of the main chamber by a wire. An apparatus having at least a gas blowing nozzle for blowing an inert gas from the side to the wire to blow away deposits of the wire, and a through-hole through which the wire can be rotated up and down, A wire cleaning mechanism disposed in the upper chamber, comprising a gas suction pipe for sucking and discharging the inert gas blown from the gas blowing nozzle to the wire from the side opposite to the gas blowing nozzle There is provided a single crystal pulling apparatus characterized by comprising:

In this way, by blowing an inert gas onto the wire with a gas blowing nozzle, and sucking and discharging the blown inert gas with a gas suction tube, while efficiently removing deposits on the wire, The inside of the chamber can be prevented from being contaminated because the deposits can be sucked and exhausted together with the inert gas. Furthermore, by allowing the wire to pass through the through hole of the gas suction tube, the area of the wire where the inert gas is blown by the gas blowing nozzle is covered with the gas suction tube, so that the deposits can be sucked reliably. , Contamination in the chamber can be surely prevented. Also, the wire cleaning work time can be greatly shortened. In addition, since the adhering material does not fall, it can be cleaned with the melt in the crucible and even while the single crystal is being pulled up, the wire can be kept clean, and there is no single crystal to grow. Along with the improvement of the dislocation rate, since it is not necessary to stop the operation for cleaning, the productivity of the single crystal is greatly improved.
As described above, according to the single crystal pulling apparatus of the present invention, the wire cleaning can be performed efficiently without contaminating the inside of the chamber, and the productivity of the single crystal is improved.

In this case, the upper chamber includes a pull chamber and a sub chamber connected to the upper portion of the pull chamber and storing a seed chuck and a seed, and the wire cleaning mechanism is disposed in the sub chamber. It is preferable.
By arranging the cleaning mechanism in the sub chamber in this way, the entire wire can be efficiently cleaned above the upper chamber, and the wire can be cleaned in the vicinity of the wire pulling mechanism. Can be cleaned before the metal powder adhering to the wire scatters, and contamination in the chamber can be more reliably prevented.

At this time, it is preferable that the tip of the gas blowing nozzle is inserted into the gas suction pipe.
By inserting the tip of the gas blowing nozzle into the gas suction tube in this way, the inert gas from the gas blowing nozzle is concentrated in the area where the wire is cleaned, and the cleaning effect is enhanced. The adhered matter blown off can be sucked more reliably.

At this time, it is preferable that the flow rate of the inert gas discharged from the gas suction pipe is controlled to be larger than the flow rate of the inert gas blown from the gas blowing nozzle.
By controlling such a gas flow rate, gas and wire deposits from the gas blowing nozzle can be effectively sucked and discharged by the gas suction pipe, and contamination of the chamber and single crystal It is possible to reliably prevent dislocation.

It is preferable that the pressure in the gas suction pipe is controlled to be lower than the pressure in the upper chamber.
In this way, because the pressure inside the gas suction pipe is controlled to be lower than the pressure inside the upper chamber, the deposits blown off from the wire can be reliably sucked and discharged by the gas suction pipe. In addition, the blown inert gas does not leak into the chamber.

It is preferable to include a wire steadying device that suppresses shaking during pulling of the single crystal of the wire.
In this way, by providing the wire steadying device, it is possible to suppress the shake of the wire due to the inert gas blown from the gas blowing nozzle, and therefore the wire can be cleaned with the cleaning mechanism of the present invention even during the pulling of the single crystal. The single crystal can be pulled with good yield while removing the deposits on the wire.

The inert gas to be blown is preferably Ar gas.
Thus, since Ar gas is also a gas supplied into the chamber during the pulling of the single crystal, the contamination from the gas from the gas blowing nozzle even if it enters the chamber and mixes with the gas in the chamber. In addition, the purity in the chamber can be kept high.

It is preferable that the through hole has a larger upper hole than the lower side of the gas suction pipe.
With such a through-hole, metal powder and silicon oxide falling from the wire take-up part of the pulling mechanism can be sucked and discharged from the upper hole of the gas suction tube, so the cleanliness in the chamber is also high. Can be high.

Preferably, the gas suction pipe is connected to a gas replacement vacuum pump in the upper chamber, and the gas is sucked and discharged by the vacuum pump.
Thus, if the vacuum pump for gas replacement of the upper chamber is shared by the gas replacement of the upper chamber and the cleaning mechanism of the present invention, a new apparatus cost generated when the cleaning mechanism of the present invention is provided can be reduced.

  As described above, according to the single crystal pulling apparatus of the present invention, the wire cleaning can be efficiently performed without contaminating the inside of the chamber, and the productivity of the single crystal is improved.

It is the schematic which shows an example of the embodiment of the cleaning mechanism of the single crystal pulling apparatus of this invention. It is the schematic which shows an example of the embodiment of the single crystal pulling apparatus of this invention. It is the side view and front view which show the example of the blowing port of the gas blowing nozzle of the single crystal pulling apparatus of this invention. It is the schematic which shows an example of the conventional single crystal pulling apparatus. It is the cross-sectional schematic which shows the structural example of the cross section of the wire used for a general single crystal pulling apparatus.

Hereinafter, the present invention will be described in detail as an example of an embodiment with reference to the drawings, but the present invention is not limited thereto.
FIG. 1 is a schematic view showing an example of an embodiment of a cleaning mechanism of a single crystal pulling apparatus according to the present invention. FIG. 2 is a schematic view showing an example of an embodiment of the single crystal pulling apparatus of the present invention. FIG. 3 is a side view and a front view showing an example of a blowing port of a gas blowing nozzle of the single crystal pulling apparatus of the present invention.

  1 and 2, the single crystal pulling apparatus 23 of the present invention includes a crucible 20 in which a raw material melt 21 is housed and which can be moved up and down is housed in a main chamber 19 for growing a single crystal. An upper chamber 18 for accommodating and taking out the grown single crystal is connected to the upper portion of 19. Further, a pulling mechanism 22 for winding the wire 11 and pulling up the seed chuck 16 and the seed (seed crystal) 15 attached to the tip of the wire 11 is disposed on the upper portion of the upper chamber 18.

When a single crystal is grown using such a single crystal pulling apparatus 23, the seed 15 attached to the seed chuck 16 is immersed in the raw material melt 21, and then the seed 15 is moved in a desired direction by the pulling mechanism 22. The wire 11 is gently wound up while being rotated to grow a single crystal at the tip of the seed 15. At this time, in order to eliminate dislocations generated when the seed 15 is deposited on the melt 21, the crystal in the initial growth stage is once narrowed (necked), and the diameter is expanded to a desired diameter when the dislocations are removed. , Grow single crystals of the desired quality.
Further, in order to perform gas replacement in the furnace before pulling up the single crystal, for example, argon gas is supplied from the gas supply source 26 through the filter 31 into the furnace, and a vacuum pump connected to the lower portion of the main chamber 19. The gas in the furnace is replaced by 24, and similarly, argon gas is supplied and discharged during pulling of the single crystal. The supply gas flow rate at this time is controlled by the manual valve 33 or the pneumatic operation valve 30 while being measured by the flow meter 32. Further, the exhaust gas flow rate is controlled by the variable flow valve 29 and the pneumatic operation valve 30.

  And the single crystal pulling apparatus 23 of this invention blows in the inert gas to the wire 11 from the side, the gas blowing nozzle 12 which blows away the deposit | attachment of the wire 11, and the penetration which the wire 11 penetrates so that a vertical rotation is possible. The upper chamber 18 includes a gas suction pipe 10 that has a hole 14 and sucks and discharges the inert gas blown from the gas blowing nozzle 12 to the wire 11 from the opposite side of the gas blowing nozzle 12. The wire cleaning mechanism 1 is provided. At this time, it is preferable that the gas blowing nozzle 12 and the gas suction pipe 10 are made of a rust-resistant material such as stainless steel.

  As described above, the inert gas is blown to the wire 11 by the gas blowing nozzle 12, and the blown inert gas is sucked and discharged by the gas suction pipe 10, so that the deposits on the wire 11 can be efficiently removed. While removing, the deposit can be sucked and exhausted together with the inert gas, so that the inside of the chamber can be prevented from being contaminated. Furthermore, since the wire 11 is inserted through the through hole 14 of the gas suction tube 10, the region of the wire 11 where the inert gas is blown by the gas blowing nozzle 12 is covered with the gas suction tube 10, so that Adherents can be sucked into the chamber, and contamination in the chamber can be reliably prevented. Also, the wire cleaning work time can be greatly shortened. Further, since the deposits do not fall, cleaning can be performed with the melt 21 in the crucible 20 and even during pulling of the single crystal, and the wire 11 can be kept clean and can be grown. Along with the improvement of the dislocation-free rate of the crystal, it is not necessary to stop the operation for cleaning, so that the productivity of the single crystal is greatly improved.

Such an inert gas blown by the cleaning mechanism 1 of the present invention is not particularly limited, but Ar gas is preferable.
Thus, since Ar gas is also a gas supplied into the chamber during the pulling of the single crystal, even if the gas from the gas blowing nozzle 12 enters the chamber and mixes with the gas in the chamber, There is no contamination and the purity in the chamber can be kept high. Therefore, the single crystal growth is not adversely affected.

As shown in FIGS. 1 and 2, the upper chamber 18 includes a pull chamber 17 that stores the grown single crystal, and a sub chamber 13 that is connected to the upper chamber 18 and stores the seed chuck 16 and the seed 15. In this case, it is preferable that the wire cleaning mechanism 1 of the present invention is disposed in the sub chamber 13.
By arranging the cleaning mechanism 1 in the sub chamber 13 in this way, the entire wire 11 can be efficiently cleaned above the upper chamber 18, and the wire cleaning can be performed near the pulling mechanism 22 of the wire 11. Before the metal powder adhering to the wire 11 is scattered from the wire take-up portion 22 or the like, it can be cleaned, and contamination in the chamber can be more reliably prevented. When the upper chamber 18 does not include the sub chamber 13, the entire wire 11 can be efficiently cleaned by disposing the cleaning mechanism 1 of the present invention above the upper chamber 18. preferable.

At this time, it is preferable that the gas suction pipe 10 is connected to the gas replacement vacuum pump 25 in the upper chamber 18 and sucks and discharges the gas by the vacuum pump 25.
In this way, if the vacuum pump 25 for gas replacement of the upper chamber 18 is shared by the gas replacement of the upper chamber 18 and the cleaning mechanism 1 of the present invention, a new device that is generated when the cleaning mechanism 1 of the present invention is provided. The installation cost can be reduced. Of course, the vacuum pump at this time may not be used as described above but may be provided separately, and as a type, for example, it is preferable to use a dry vacuum pump effective for sucking oxide.

Moreover, it is preferable that the single crystal pulling device 23 of the present invention includes a wire steadying device 28 that suppresses the shake during pulling of the single crystal of the wire 11.
As described above, since the wire steadying device 28 is provided, it is possible to suppress the shake of the wire 11 due to the inert gas blown from the gas blowing nozzle 12. The single crystal can be pulled up with good yield while removing the deposits on the wire 11.
The wire steadying device 28 is not particularly limited, and a well-known device can be used, and a device or the like that takes into account the deflection period depending on the wire length can be used.

The shapes of the gas blowing nozzle 12 and the gas suction pipe 10 are not particularly limited. For example, as shown in FIG. 1, the tip of the gas blowing nozzle 12 is inserted into the gas suction pipe 10. preferable.
By inserting the tip of the gas blowing nozzle 12 into the gas suction tube 10 in this way, the inert gas from the gas blowing nozzle 12 is concentrated in the area where the wire 11 is cleaned, and the cleaning effect is enhanced. Furthermore, the deposits blown off from the wire 11 can be sucked more reliably.
Further, in this case, as shown in FIG. 1, by narrowing the tip of the gas suction tube 10, the gap with the gas blowing nozzle 12 can be reduced, and the gas can be sucked and discharged more efficiently. it can. Further, the cleaning effect can be enhanced by bringing the tip of the gas blowing nozzle 12 closer to the wire 11. Further, when the gas blowing nozzle 12 is not inserted into the gas suction tube 10, the tip of the gas suction tube 10 is widened so that the gas can effectively strike the wire 11, and the blown-off deposits are captured. It can also be made easier.

Further, the blowing port of the gas blowing nozzle 12 is not particularly limited. For example, the tip as shown in FIG. 3 is crushed to form a slit-shaped blowing port (FIG. 3A), or a plurality of small holes are formed. By using the provided blowing port (FIG. 3B), the gas flow rate can be increased at the blowing port, and the wire can be cleaned more effectively.
Such a gas blowing nozzle 12 is connected to a gas supply source 27 and measured with a flow meter 32 while being controlled with a manual valve 33 and a pneumatic operation valve 30 and cleaned with a filter 31. Gas can be sprayed onto the wire 11.

Further, as shown in FIG. 1, it is preferable that the through hole 14 of the gas suction tube 10 has a larger hole on the upper side than the lower side of the gas suction tube 10.
If the through hole has such a shape, the metal powder and silicon oxide falling from the wire take-up portion of the pulling mechanism 22 can be sucked and discharged from the upper hole of the gas suction pipe 10, so that the cleaning in the chamber It can be higher.

In this case, it is preferable that the flow rate of the inert gas discharged from the gas suction pipe 10 is controlled to be larger than the flow rate of the inert gas blown from the gas blowing nozzle 12.
By controlling the gas flow rate to such a level, the gas from the gas blowing nozzle 12 and the deposits on the wire 11 can be effectively sucked and discharged by the gas suction pipe 10, and the contamination of the chamber Single crystal dislocations can be reliably prevented.

Moreover, it is preferable that the pressure in the gas suction pipe 10 is controlled to be lower than the pressure in the upper chamber 18.
In this way, by controlling the pressure in the gas suction tube 10 to be lower than the pressure in the upper chamber 18, the deposits blown off from the wire 11 can be reliably sucked and discharged by the gas suction tube 10. Therefore, contamination in the chamber can be prevented, and the blown inert gas does not leak into the chamber.
At this time, as a pressure control method, as shown in FIG. 2, a variable flow rate is detected while detecting a pressure difference between the gas suction pipe 10 and the sub chamber 13 using a diaphragm vacuum gauge (differential pressure gauge) 34. It is controlled by a valve (conductance valve) 29 or the like.

  As described above, the wire cleaning in the single crystal pulling apparatus 23 of the present invention is performed, for example, immediately after the polycrystalline silicon is completely melted and seeded to grow the silicon single crystal (immediately before the single crystal pulling), or the grown silicon. This can be performed immediately before the single crystal rod is taken out of the chamber. The case where the wire cleaning in the single crystal pulling apparatus 23 of the present invention as shown in FIGS. 1 and 2 is performed immediately before pulling the single crystal will be described below.

  Immediately before pulling up the single crystal, the crucible 20 contains a melt 21 in which a silicon polycrystalline material is melted. Further, for example, argon gas is introduced into the upper chamber 18 from the gas supply source 26 and is exhausted from the lower portion of the main chamber 19 by the vacuum pump 24, and the furnace pressure is controlled by the variable flow valve 29 of the exhaust pipe. Further, the wire 11 is almost wound up, and the seed chuck 16 and the seed 15 are stored in the sub chamber 13 and are in a state as shown in FIG.

Here, the vacuum pump 25 to which the gas suction tube 10 is connected is operated to open the pneumatic operation valve 30 on the gas blowing nozzle 12 side and open the pneumatic operation valve 30 on the gas suction tube 10 side.
The gas flow rate (purge gas flow rate) from the spray nozzle 12 can be set in the range of 2 to 100 l / min. Further, by setting the exhaust amount of the vacuum pump 25 (the exhaust gas flow rate of the gas suction pipe 10) to be larger than the purge gas flow rate, the gas from the blowing nozzle 12 can be prevented from leaking into the chamber. Further, the pressure in the gas suction tube 10 can be controlled by a variable flow valve 29 provided in the vacuum pump 25 on the gas suction tube 10 side so that the pressure in the chamber is lower than the pressure in the chamber. Is preferably controlled to about −10 to −100 hPa.

Next, the wire 11 is lowered while rotating to the vicinity of the melt surface of the melt 21 while operating the pulling mechanism 22, so that the oxide and metal powder adhering to the surface of the wire 11 are blown off and sucked to be cleaned. it can. Moreover, the cleaning effect is further improved by further raising and lowering the wire 11 to perform cleaning a plurality of times.
The speed at which the wire 11 moves up and down as described above can be adjusted, for example, in the range of 1 to 1000 mm / min and the rotation speed in the range of 1 to 30 rpm.

As described above, the wire cleaning can be completed in several tens of minutes. Finally, the vacuum pump 25 is stopped by closing the gas blowing nozzle 12 and the pneumatic operation valve 30 of the gas suction pipe 10.
Further, when performing such wire cleaning before taking out the crystal, by performing the wire cleaning operation when the grown silicon single crystal rod is pulled up to the pull chamber 17, oxide contamination to the pulling mechanism 22 is also reduced. it can.

  With the single crystal pulling apparatus of the present invention as described above, the DF conversion (dislocation-free) rate (the number of DF pulling times / total number of pulling crystals) is improved by about 20 to 30% compared to the conventional apparatus. Is done.

  The present invention is not limited to the above embodiment. The above-described embodiment is an exemplification, and the present invention has substantially the same configuration as the technical idea described in the claims of the present invention, and any device that exhibits the same function and effect is the present invention. It is included in the technical scope of the invention.

1 ... Wire cleaning mechanism,
10 ... Gas suction tube, 11 ... Wire, 12 ... Gas blowing nozzle,
13 ... sub chamber, 14 ... through hole, 15 ... seed,
16 ... Seed chuck, 17 ... Pull chamber, 18 ... Upper chamber,
19 ... main chamber, 20 ... crucible, 21 ... melt 22 ... pulling mechanism, 23 ... single crystal pulling device,
24, 25 ... vacuum pump, 26, 27 ... gas supply source,
28 ... Wire steady rest device, 29 ... Variable flow valve, 30 ... Pneumatic operation valve,
31 ... filter, 32 ... flow meter, 33 ... manual valve, 34 ... diaphragm gauge.

Claims (9)

At least a single crystal pulling apparatus that pulls a single crystal grown from a melt in a crucible housed in a main chamber into an upper chamber connected to the upper portion of the main chamber with a wire,
At least a gas blowing nozzle for blowing an inert gas from the side to the wire to blow away the deposits on the wire, and a through-hole through which the wire can be rotated up and down, from the gas blowing nozzle It comprises a gas suction pipe that sucks and discharges the inert gas blown to the wire from the side opposite to the gas blowing nozzle, and includes a wire cleaning mechanism disposed in the upper chamber. There is a single crystal pulling apparatus.   The upper chamber includes a pull chamber and a sub chamber connected to the upper portion of the pull chamber and storing a seed chuck and a seed, and the wire cleaning mechanism is disposed in the sub chamber. The single crystal pulling apparatus according to claim 1.   The single crystal pulling apparatus according to claim 1 or 2, wherein a tip of the gas blowing nozzle is inserted into the gas suction pipe.   The flow rate of the inert gas discharged from the gas suction pipe is controlled to be larger than the flow rate of the inert gas blown from the gas blowing nozzle. 4. The single crystal pulling apparatus according to claim 3.   The single crystal pulling apparatus according to any one of claims 1 to 4, wherein a pressure in the gas suction pipe is controlled to be lower than a pressure in the upper chamber. .   The single crystal pulling apparatus according to any one of claims 1 to 5, further comprising a wire steadying device that suppresses a swing of the wire during the pulling of the single crystal.   The single crystal pulling apparatus according to claim 1, wherein the inert gas blown is Ar gas.   The single crystal pulling apparatus according to any one of claims 1 to 7, wherein the through hole has a larger upper hole than the lower side of the gas suction pipe.   9. The gas suction pipe is connected to a vacuum pump for gas replacement in the upper chamber, and sucks and discharges gas by the vacuum pump. The single crystal pulling apparatus according to any one of the above.

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