JP4805284B2 - Sputtering target and manufacturing method thereof - Google Patents

Description

  The present invention relates to a sputtering target for silicon and a method for manufacturing the same.

Conventionally, an equiaxed polycrystal has been used as a sputtering target for silicon, and a single target cut out from an ingot has been adopted.
Moreover, as a target of Fe, Co, and Ni-based alloys, Japanese Patent Laid-Open No. 63-238268 and Japanese Patent No. 2952853 have proposed a technique of processing a unidirectionally solidified ingot.

  However, the following problems remain in the conventional silicon sputtering target technology. That is, because the target is processed from equiaxed polycrystals, the final solidified component is dispersed inside, and therefore stress distortion is inherent, and there is a disadvantage that warpage occurs due to heating during sputtering. For this reason, the bonding location and the target itself were cracked due to bonding failure caused by warpage or warpage during heating and cooling of the bonded target. In particular, this phenomenon becomes remarkable with a large-area target. In addition, as a countermeasure, bonding may be performed using a soft metal that absorbs stress strain. In this case, even if bonding can be performed satisfactorily, the composition of the film formation characteristics during sputtering may vary. There was a fear. Further, the concentration of the dopant is concentrated in the final solidified portion due to segregation, causing variations in the electric resistance of the target, resulting in non-uniform sputtering and consequently cracking of the target.

  The present invention has been made in view of the above-described problems, and an object of the present invention is to provide a silicon sputtering target in which warpage due to stress strain is small and bonding failure, target cracking, and the like hardly occur, and a method for manufacturing the same.

The present invention employs the following configuration in order to solve the above problems. That is, the sputtering target of the present invention is columnar polycrystalline silicon grown in the preferential crystal growth direction, and the preferential crystal growth direction is the crystal plane orientation (001) plane, this (001) plane. And the (011) plane and the (111) plane, the amount of inevitable impurities contained is 10 ppm or less, the inevitable impurities are at least Al, and the in-plane distribution width of the specific resistance value is less than 10%. It is characterized by being.

  This sputtering target is columnar polycrystalline silicon, and the amount of inevitable impurities contained is 10 ppm or less. Therefore, stress cracking is reduced, and since the dopant concentration is uniform, there is little variation in electrical resistance.

  Further, in this sputtering target, since the columnar crystals are grown in the preferential crystal growth direction, etching by sputtering is uniform, so that the film has uniform film forming characteristics and is hardly cracked. The preferred crystal growth direction includes a crystal plane orientation (001) plane, a plane perpendicular to the (001) plane, a (011) plane, a (111) plane, and the like.

The sputtering target of the present invention is characterized in that the in-plane distribution width of the specific resistance value is less than 10%.
In this sputtering target, since the in-plane distribution width of the specific resistance value is less than 10%, there is little variation in electric resistance.

In addition, since the sputtering target of the present invention contains at least one of Fe, C, and N in addition to Al, there is little generation of residual stress and good film formation with little impurity contamination. Is possible .

  Further, the sputtering target of the present invention is characterized in that the material is square or circular. That is, in this sputtering target, since the material is square or circular (round), the residual stress produced by the product can be reduced and cracking is unlikely to occur.

  The method for producing a sputtering target of the present invention comprises a step of solidifying silicon melted in a crucible from the bottom upward to a solidification speed of 5 mm / min or less to produce a silicon ingot, and the silicon ingot in the solidification direction. And a step of producing a silicon target by slicing in a direction orthogonal to the manufacturing method, wherein the sputtering target according to any one of claims 1 to 5 is manufactured.

  That is, since the sputtering target manufacturing method is based on unidirectional solidification, the sputtering film forming property is good, and high film quality uniformity can be obtained.

  In the sputtering target manufacturing method of the present invention, a technique including a step of arranging a plurality of the silicon targets to form a large square target is employed. That is, in this sputtering target manufacturing method, a plurality of the above silicon targets are arranged to form a large square target, so that a large area target capable of high-quality film formation with little warpage can be obtained.

  The present invention has the following effects. That is, according to the sputtering target of the present invention, since it is columnar polycrystalline silicon and the amount of unavoidable impurities contained is 10 ppm or less, stress cracking is reduced and dopant segregation is extremely small. High quality characteristics with little variation in electrical resistance. Further, since the specific resistance value distribution is uniform, there is little variation in electrical resistance.

  Hereinafter, an embodiment of a sputtering target and a manufacturing method thereof according to the present invention will be described with reference to FIGS. 1 and 2.

  As shown in FIG. 1, a method for manufacturing a sputtering target according to the present embodiment is first performed from a silicon melt L in a crucible 1 to which a dopant such as B (boron) is added using a silicon ingot manufacturing apparatus. A directionally solidified polycrystalline silicon ingot C is obtained. In this silicon ingot manufacturing apparatus, a hollow chill plate 3 is placed on an underfloor heater 2, and a silica crucible 1 having a square (square) horizontal cross section is placed on the hollow chill plate 3. A ceiling heater 4 is provided above the crucible 1, and a heat insulating material 5 is provided around the crucible 1. Reference numeral 6 denotes an Ar gas supply pipe.

In order to produce the silicon ingot C by this manufacturing apparatus, the silicon raw material is melted in the crucible 1 to form the silicon melt L, and then the energization of the underfloor heater 2 is stopped and the hollow chill plate 3 is connected to the supply pipe 6. Ar gas is supplied to cool the bottom of the crucible 1. Further, by gradually decreasing the energization of the ceiling heater 4, the silicon melt L is cooled from the bottom and solidifies in one direction from the bottom to the top, as shown in FIGS. 2 (a) and 2 (b). Finally, a silicon ingot C having a unidirectionally solidified polycrystalline structure C0 having an angular cross section is grown. That is, a polycrystalline silicon ingot C composed of columnar crystals directed from the bottom upward is obtained.
In addition, it is desirable to control the solidification speed of unidirectional solidification to 5 mm / min or less. This is because if the solidification speed is faster than the above speed, stress strain and impurities remain easily, and the warpage due to this is not controllable.

The silicon ingot C grown in this way is cut (sliced) in a direction perpendicular to the solidification direction (vertical direction of the ingot) except for the final solidified portion, as shown in FIG. A plurality of rectangular plate-like silicon targets T1 are produced.
The silicon target T1 is columnar polycrystalline silicon, and unavoidable impurities are concentrated in the final solidified portion by unidirectional solidification, so that the amount of unavoidable impurities contained is 10 ppm or less. The inevitable impurities are Al, Fe, C, and N. The columnar crystals of the silicon target T1 are arranged and grown so as to be in the vicinity of the plane orientation (001) plane, which is the preferential crystal growth direction of the crystals. The preferred crystal growth direction includes a plane perpendicular to the (001) plane, a (011) plane, a (111) plane, and the like.

  Further, as shown in FIG. 2 (c), these silicon targets T1 are aligned and bonded or diffusion bonded using Au (gold), Ag (silver) or the like on a support base (not shown). A large square target T2 is manufactured. Note that it is preferable to use diffusion bonding or welding capable of forming a high-purity silicon film as the bonding means.

  As the conditions for the above bonding and bonding, in order to prevent warping and bonding failure, Au-based brazing material (for example, Au-Sn, Au-Ag) is used in Au bonding while heating the targets below the melting temperature of the brazing material. -Sn-based) is melted at about 400 ° C., applied to the lower part of the target bonding surface, and bonded. In the Ag solder bond, for example, Sn—Ag solder is preferably melted and bonded at approximately 240 ° C. to 280 ° C. while heating the targets in the same manner as described above. In the case of diffusion bonding, the targets are preliminarily heated to a temperature close to the melting point and a temperature at which columnar crystals do not break down to about 115 ° C., and are pressed by HIP under a vacuum of 250 kg. As a condition of the pressure press, cooling is gradually performed after the pressure press. In addition, it is good to perform a press press by about 5 hours-1 hour with a hydrostatic pressure press. In the case of welding, it is preferable to perform welding by arc or electric welding with the same member as the target. In bonding, vapor deposition and plating may be performed on the bonding surface in advance with solder. Further, if possible, it is preferable to adjust the amount of brazing material, joining conditions, etc. so that the brazing material does not ooze out on the joining surfaces of the targets. If it does as mentioned above, since it is a unidirectional solidification target, there is no initial curvature, and since it joins by the bonding method with few curvature, a curvature and a crack do not occur at all.

  The silicon target T1 is, for example, a quadrangular shape with a side of 60 cm or more and a thickness of about 300 mm, and the large rectangular target T2 is, for example, a size of 100 cm × 130 cm. The silicon target T1 has a warp caused by stress strain at a temperature of 1200 ° C. within 0.01 to 4 mm, and the warp of the silicon target T1 cooled to room temperature is 0.001 to 0.5 mm or less. Furthermore, the large rectangular target T2 has a surface unevenness of 0.01 to 1 mm or less due to warpage, and the warpage does not exceed 0.01 to 2 mm even near a heated temperature of 1200 ° C., and warpage and cracks based on the warpage are generated. There wasn't.

  As described above, the silicon target T1 of the present embodiment is columnar polycrystalline silicon, and the amount of inevitable impurities contained is 10 ppm or less. Therefore, stress cracking is reduced and dopant segregation is extremely small. It has high quality characteristics with little variation in electrical resistance. That is, the specific resistance value distribution is uniform.

  In addition, since the silicon ingot C obtained by unidirectional solidification from the square crucible 1 is sliced to produce the square plate-like silicon target T1, the stress strain inherent in the case of slicing from a normal equiaxed crystal ingot is increased. Can be reduced. In particular, since the square crucible 1 is used, an ingot with a square cross section is obtained, and the stress distortion is less than when processing an ingot with a normal round crucible into a square, and warping during heating and cooling (sputtering and bonding, etc.) Is unlikely to occur. As a result, it is possible to obtain a large polycrystalline silicon rectangular target T2 in which bonding failure, crack after bonding, bonding failure, or the like hardly occurs.

The technical scope of the present invention is not limited to the above embodiment, and various modifications can be made without departing from the spirit of the present invention.
In the above embodiment, the rectangular plate-like silicon target T1 is used, but other external shapes, particularly a circular plate shape, may be used. In addition, it manufactures with a square ingot with respect to a square target, and it manufactures with a round ingot with respect to a round target.
Moreover, although the P-type ingot using B was used as the dopant, it may be an N-type ingot added with other elements or P (phosphorus).

1 is a schematic cross-sectional view showing a silicon ingot manufacturing apparatus in an embodiment of a sputtering target and a manufacturing method thereof according to the present invention. In one Embodiment of the sputtering target which concerns on this invention, and its manufacturing method, it is explanatory drawing which showed the manufacturing method to process order.

Explanation of symbols

1 crucible
C Silicon ingot
L Silicon melt
T1 silicon target
T2 Large square target

Claims (5)

Columnar polycrystalline silicon grown in the preferred crystal growth direction,
The preferential crystal growth direction is a crystal plane orientation (001) plane, a plane perpendicular to the (001) plane, and (011) plane and (111) plane,
The amount of inevitable impurities contained is 10 ppm or less, and this inevitable impurity is at least Al,
A sputtering target characterized in that the in-plane distribution width of the specific resistance value is less than 10%. The sputtering target according to claim 1,
The sputtering target, wherein the inevitable impurities include at least one of Fe, C, and N in addition to Al. In the sputtering target according to claim 1 or 2,
A sputtering target characterized in that the material is rectangular or circular.   A silicon ingot is produced by solidifying unidirectionally the silicon melted in the crucible from the bottom upward at a solidification speed of 5 mm / min or less; and slicing the silicon ingot in a direction perpendicular to the solidification direction A method for producing a sputtering target, comprising: producing a sputtering target according to any one of claims 1 to 3. In the manufacturing method of the sputtering target according to claim 4,
A method for producing a sputtering target, comprising a step of arranging a plurality of the silicon targets to form a large square target.

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