JP5428741B2 - Manufacturing method of cylindrical sputtering target - Google Patents

Manufacturing method of cylindrical sputtering target Download PDF

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JP5428741B2
JP5428741B2 JP2009240414A JP2009240414A JP5428741B2 JP 5428741 B2 JP5428741 B2 JP 5428741B2 JP 2009240414 A JP2009240414 A JP 2009240414A JP 2009240414 A JP2009240414 A JP 2009240414A JP 5428741 B2 JP5428741 B2 JP 5428741B2
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cylindrical
material
adapter
target
bonding
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JP2011084795A (en
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優 佐藤
謙一 伊藤
哲夫 渋田見
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東ソー株式会社
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  The present invention relates to a method of manufacturing a cylindrical sputtering target used in a magnetron rotary cathode sputtering apparatus or the like.

  The magnetron rotary cathode sputtering apparatus has a magnetic field generator inside a cylindrical sputtering target, and performs sputtering while rotating the target while cooling from the inside of the target. In this apparatus, since the entire surface of the target material becomes an erosion surface and is evenly cut, the target usage efficiency (20-30%) is much higher than the target usage efficiency (20-30%) in the conventional flat plate type magnetron sputtering apparatus. 60% or more) is obtained. Further, the cooling efficiency is increased by rotating the target, and a higher power can be supplied per unit area than a conventional flat plate type magnetron sputtering apparatus, so that a high deposition rate can be obtained.

  However, since both ends of the cylindrical target are difficult to be sputtered, uniform erosion does not occur, and higher usage efficiency has been desired.

  Among such cylindrical sputtering targets, as an example of a method of manufacturing a ceramic target such as ITO (Indium Tin Oxide), a cylindrical target material made of a ceramic sintered body manufactured in advance and a cylindrical base material are solder materials, etc. There is a method of bonding using a bonding material. This method can use a ceramic sintered body having a higher density than a method of forming a ceramic material on a cylindrical base material by thermal spraying or the like, so that a film obtained by sputtering is of high quality, and the production yield is high. There are also advantages such as high.

  On the other hand, as a method of joining a cylindrical target material made of a ceramic sintered body and a cylindrical base material using a solder material, for example, one end of the cylindrical target material and the cylindrical base material is sealed. A method is known in which a cylindrical base material is inserted into a cylindrical target material containing a molten solder material with the sealed surface down (see, for example, Patent Document 1). In this method, when joining a plurality of cylindrical target materials, it has been proposed to seal and integrate the cylindrical target materials with heat-resistant tape.

  However, in this method, the heat-resistant tape used for sealing remains inside the cylindrical target material, and cracking and peeling may occur during use due to poor electrical conduction and thermal conduction at that portion.

  In addition, as a joining method in which cracking or peeling of the target does not occur during sputtering, a method in which a void layer is provided between the cylindrical base material and the cylindrical target material and joined with solder (for example, see Patent Document 2), A method has been disclosed in which a predetermined amount of gap is provided at a connection portion between cylindrical sputtering target materials when joining the cylindrical sputtering target (see, for example, Patent Document 3).

  However, in these methods, when the bonding material is injected into the space between the cylindrical target material and the cylindrical base material, the width of the space is as narrow as about 1 mm. It was not easy to obtain a uniform bonding layer because air was taken in during injection and voids or sinks occurred. Therefore, it has been attempted to apply ultrasonic vibration to the outer peripheral portion of the cylindrical target material when injecting the bonding material. However, it is difficult to completely suppress the intake of air by this method. It was difficult to suppress peeling and cracking. Further, since the bonding material is excessively adhered and solidified in the vicinity of the target end, smooth injection of the bonding material has been hindered.

JP-A-8-60351 JP 2008-184627 A JP 2008-184640 A

  An object of the present invention is to form a uniform joining layer without taking in air in a method of joining a cylindrical base material and a cylindrical target material using a joining material in a cylindrical sputtering target, and remarkably crack and peel off. It is providing the manufacturing method of the cylindrical sputtering target which can be reduced.

  As a result of intensive studies to solve the above problems, the present inventors have completed the present invention. That is, the present invention relates to a method of manufacturing a cylindrical sputtering target by bonding a cylindrical target material made of a ceramic sintered body and a cylindrical base material using a bonding material, and the cylindrical target material inner side surface and the cylindrical base material. When filling the bonding material into the space formed by the outer surface of the material, the bonding material is injected and filled through the adapter, and the manufacturing method of the cylindrical sputtering target is characterized. Hereinafter, the present invention will be described in detail.

In the present invention, the cylindrical target material is made of a ceramic sintered body, and various ceramic materials can be used. For example, at least one of In, Sn, Zn, Al, Ta, Nb, and Ti is used. Examples thereof include oxides having a main component. More specifically, for example, an ITO sintered body made of indium, tin and oxygen, an AZO sintered body made of zinc, aluminum and oxygen (Aluminum Zinc Oxide), an IZO sintered body made of indium, zinc and oxygen (Indium). Zinc Oxide), Ta 2 O 5 , Nb 2 O 5 , TiO 2 and the like. These sintered bodies may be further added with other elements in order to improve discharge characteristics and resistivity.

  Examples of the cylindrical base material that can be used in the present invention include Cu, Ti, Al, Mo, alloys containing at least one of these metals, SUS, and the like. What is necessary is just to have property, intensity | strength, etc.

  In the cylindrical sputtering target of the present invention, the lengths of the cylindrical base material and the cylindrical target material are not particularly limited, and the number of cylindrical target materials is not particularly limited.

  As the bonding material, a material generally used as a solder material, a thermosetting conductive resin, or the like can be used. Preferably, it is a low melting point solder material, specifically, In, In alloy, Sn, Sn alloy or the like.

  The shape of the adapter used in the present invention is not particularly limited as long as it is a shape capable of injecting a bonding material through the adapter. For example, the shape seen from above is circular, semi-circular, fan-shaped or the like. In addition, the bonding material is injected into the above-described space through the adapter, but the shape of the portion corresponding to the outlet from the adapter (hereinafter referred to as the adapter outlet portion) is not particularly limited. In particular, when the adapter is used at the upper end of the cylindrical target material, the shape of the adapter outlet portion is a circle or a part of a circle having the same radius of curvature as the inner diameter of the cylindrical target material. If the adapter is installed so that the inner circumference of the cylindrical target material coincides with that of the cylindrical target material, the bonding material can be injected efficiently.

  At this time, if the radius of curvature of the adapter outlet portion is smaller than the radius of curvature of the inner diameter of the cylindrical target material, the adapter outlet portion is close to the outer surface of the cylindrical base material, so that the injection amount is insufficient and filling takes time. become. On the other hand, when the radius of curvature of the adapter outlet portion is larger than the radius of curvature of the inner diameter of the cylindrical target material, the molten solder adheres to the upper end portion of the cylindrical target material, making it impossible to smoothly fill and fill the space.

The height of the adapter is not particularly limited, but when the adapter is installed at the upper end portion of the cylindrical target material, it is desirable that the height be equal to or lower than the end portion of the cylindrical base material.
On the other hand, if the width (thickness) of the adapter is smaller than the thickness of the cylindrical target material, a sufficient taper cannot be obtained. Therefore, the adapter is preferably at least as thick as the cylindrical target material. Since it may be installed at the upper end of the material, the maximum width of the adapter is preferably 1.5 to 2 times the thickness of the cylindrical target material in consideration of its stability.

  Further, when the adapter has a tapered shape or a groove is formed on the surface in contact with the bonding material, the bonding material can be injected more smoothly. At this time, the taper angle is not particularly limited. The groove will also play the role of a runway. In the case of an adapter having a groove, the depth of the groove may be such that the bonding material does not adhere to the adapter end, and is preferably 0.1 mm to 1 mm. Furthermore, since the width of the space between the outer surface of the cylindrical substrate and the inner surface of the cylindrical target material is usually about 1 mm, it is preferable that the bottom of the groove coincides with the inner periphery of the cylindrical target material. This is because if the bottom of the groove is outside the inner periphery of the cylindrical target material, the bonding material comes into contact with the upper end of the cylindrical target material, which may cause solidification in the vicinity thereof.

  The adapter may be made of any material as long as it is not changed by the melting temperature of the bonding material. Examples thereof include Cu, Ti, Al, Mo, alloys containing at least one of these metals, and SUS. Moreover, what has appropriate thermal conductivity, intensity | strength, etc. is preferable.

  Next, the manufacturing method of the cylindrical sputtering target of this invention is shown more specifically. An example of the use of the adapter and an example of the shape of the adapter are shown in FIGS. 1 and 2 show an example of assembling a cylindrical sputtering target when joining a cylindrical target material and a cylindrical base material in the present invention. As shown in FIG. 2, the cylindrical target material 20 is fixed to a predetermined position of the cylindrical base material 10 using a sealing jig 40 to form a space 70 filled with a bonding material. The space between the cylindrical target material 20 and the sealing jig 40 and the space between the cylindrical base material 10 and the sealing jig 40 are sealed with a sealing material 50. When the bonding material is a low melting point solder, a thermosetting conductive resin, or the like, heat treatment is performed. Therefore, it is necessary to use a heat-resistant packing or an O-ring for the sealing material 50, in which case Teflon (registered trademark) or Materials such as silicon can be used.

  In the case where the bonding material is a low melting point solder, in order to fill the space 70 between the cylindrical base material 10 and the cylindrical target material 20 with the molten solder, it has a tapered shape as shown in FIGS. A semicircular adapter 30 may be installed at the upper end of the cylindrical target material, and molten solder may be injected and filled through the adapter.

  In FIG. 1 and FIG. 2, the inside of the adapter has a tapered shape, but in the adapter of FIG. 3, a groove serving as a runner is formed linearly from the outer periphery toward the center portion on the surface that contacts the solder material. FIG. 4 is a top view of a circular adapter having a tapered shape and a groove. Further, FIG. 5 is a top view of an adapter having a spiral groove and a tapered shape as another groove shape.

  FIG. 6 shows a cross-sectional view of an adapter in which a tapered shape and a columnar shape are combined so that molten solder is injected along the inner wall of the cylindrical target as another adapter shape. In FIG. 6, grooves are formed on the tapered surface and the inner wall surface of the cylinder. However, the shape and number of grooves are not limited as long as the smooth flow of the bonding material is not hindered.

  As another example of the adapter shape, a fan-shaped adapter can be shown as shown in FIG. This adapter is provided with walls so that the joining material does not overflow from both sides. As shown in FIG. 8, the joining material is inserted into the space between the cylindrical target material 20 and the cylindrical base material 10 from the tapered surface. Since there is a portion where the adapter is not installed but the space of the portion becomes the air vent opening 80, the air escape from the space is good and a uniform bonding layer without air bubbles is formed. The

  9 and 10 show a shape in which a groove is formed in a fan-shaped adapter. 11 and 12 show examples of its use. FIG. 11 shows a case where two adapters are used, and FIG. 12 shows a case where four adapters are used. In any case, since the space where the adapter is not installed becomes the air vent opening 80, the joining material is more smoothly injected, the joining material does not take in air bubbles, and in the vicinity of the target end. The bonding material does not solidify.

  According to the present invention, it becomes easy to inject a bonding material such as a low melting point solder between the cylindrical target material and the cylindrical base material, and it is possible to continuously inject smoothly, It is difficult for voids and sink marks to occur in the bonding layer, and a uniform bonding layer is formed, so that cracking and peeling due to non-uniform heat distribution during manufacturing and sputtering can be reduced. Furthermore, the adapter has a tapered shape, or the adapter is installed so that an air vent opening exists when the bonding material is injected, so that the bonding material does not further capture the air layer, and pulsation, etc. Therefore, it is possible to smoothly and quickly inject a space formed between the cylindrical target material and the cylindrical base material in a short time, thereby forming a uniform bonding layer.

It is a figure which shows the usage example of the adapter which has a taper shape. It is an assembly figure at the time of inject | pouring joining material using an adapter. It is a figure which shows the adapter which has a taper shape and a groove | channel. It is a top view of the adapter which has a taper shape and a groove | channel. FIG. 6 is a top view of an adapter having tapered and helical grooves. It is a figure which shows the adapter which has a taper shape. It is a figure which shows a sector adapter. It is a figure which shows the usage example of the adapter of FIG. It is a figure which shows the fan-shaped adapter which has a groove | channel. It is a top view of the fan-shaped adapter which has a groove | channel. It is a figure which shows the usage example of two adapters. It is a figure which shows the usage example of four adapters. It is a figure which shows the joining state of the cylindrical sputtering target in Example 1. FIG. It is a figure which shows the joining state of the cylindrical sputtering target in the comparative example 1.

  Examples of the present invention will be described below, but the present invention is not limited thereto.

Example 1
Two cylindrical ITO target materials having an outer diameter of 88 mmφ, an inner diameter of 68 mmφ, and a length of 180 mm were prepared, and the surfaces other than the joint surfaces of the respective cylindrical ITO target materials were masked with heat-resistant tape. In order to prevent the bonding material from adhering, a surface other than the bonding surface of the cylindrical substrate made of SUS304 having an outer diameter of 65 mmφ, an inner diameter of 61 mmφ, and a length of 400 mm is masked with heat-resistant tape, as shown in FIG. And it hold | maintained with the jig | tool so that the lower end of cylindrical ITO target material may come to the position of 20 mm from the lower part. An annular Teflon (registered trademark) sheet (outer diameter: 100 mmφ, inner diameter 68.1 mmφ, 0.4 mmt) is fitted into a cylindrical base material as a sealing material 50 at the connection portion between two target materials, and the annular sheet Two cylindrical target materials were overlapped with each other. As shown in FIG. 1, a semicircular adapter having an outer diameter of 100 mmφ, an inner diameter of 68 mmφ, and a height of 20 mm (an angle formed by the adapter bottom surface and the taper surface of 60 degrees) is cylindrical so as to match the inner diameter of the cylindrical ITO target material. The upper end of the target material was fixed with an adhesive, and molten In was injected and filled as a bonding material through an adapter. There was no pulsation during injection and filling, and a predetermined amount of In was smoothly injected and filled. Next, In was cooled and solidified, and the heat-resistant tape, Teflon (registered trademark) sheet, and the like were removed to obtain a cylindrical ITO sputtering target.

With respect to the cylindrical target thus obtained, an X-ray source was placed inside the cylindrical base material, a film was placed outside the target, and the state of In as a bonding material was confirmed by X-ray transmission imaging. As a result, as shown in FIG. 13 (X-ray transmission photograph), voids and sink marks (dents) were not recognized. Further, a 48-hour continuous discharge test (target rotation speed: 6 rpm, sputtering pressure: 0.4 Pa, power density: 4.0 W / cm 2 ) was carried out. Even after 48 hours, cracks, cracks and peeling were observed on the target. I couldn't.

Example 2
The molten In was injected and filled in the same manner as in Example 1 except that the adapter was changed to an adapter having grooves (depth: 0.8 mm, 16) as shown in FIG. There was no pulsation during injection and filling, and a predetermined amount of In was smoothly injected and filled. Next, In was cooled and solidified to obtain a cylindrical ITO sputtering target.

  As for the cylindrical target thus obtained, the state of In as a bonding material was confirmed by X-ray transmission imaging in the same manner as in Example 1, but no voids or sink marks (dents) were observed. Further, a 48-hour continuous discharge test was conducted in the same manner as in Example 1, but no cracks, cracks, or peeling occurred on the target even after 48 hours.

Example 3
As shown in Fig. 12, an adapter with a groove (depth: 0.8 mm, 7 pieces) (sector shape of a size corresponding to 80 degrees of a circle with an outer diameter of 100 mmφ and an inner diameter of 65 mmφ, height 20 mm. Adapter bottom surface and groove Example 1 except that the cylindrical target material is disposed evenly at the upper end of the cylindrical target material so that the inner circumference of the cylindrical target material and the adapter outlet portion (bottom of the groove) coincide with each other using four angles of 60 degrees In the same manner, molten solder was injected and filled. There was no pulsation during injection and filling, and a predetermined amount of In was smoothly injected and filled. Next, In was cooled and solidified to obtain a cylindrical ITO sputtering target.

  As for the cylindrical target thus obtained, the state of In as a bonding material was confirmed by X-ray transmission imaging in the same manner as in Example 1, but no voids or sink marks (dents) were observed. Further, a continuous discharge test for 48 hours was carried out in the same manner as in Example 1, but no cracks, cracks or peeling occurred on the target even after 48 hours.

Comparative Example 1
In the same manner as in Example 1, but without using an adapter, molten solder was directly injected and filled into the space between the cylindrical ITO target material and the cylindrical base material. Unless a film was formed and the oxide film was not removed, it was difficult to inject molten In. A part of In overflowed from the space between the target material and the substrate.

  For the cylindrical target thus obtained, the state of In as a bonding material was confirmed by X-ray transmission imaging in the same manner as in Example 1. As shown in FIG. 14 (X-ray transmission photograph), molten In A void was observed on the side of the injection. Further, in the same manner as in Example 1, however, a continuous discharge test for 6 hours was performed. As a result, surface roughness was generated on the surface of the target material corresponding to the void, and cracks were generated from the surface.

10: Cylindrical base material 20: Cylindrical target material 30: Adapter 40: Sealing jig 50: Sealing material 60: Groove 70: Space 80: Opening part for air vent

Claims (3)

  1. In a method of manufacturing a cylindrical sputtering target by bonding a cylindrical target material made of a ceramic sintered body and a cylindrical base material using a bonding material, the inner surface of the cylindrical target material and the outer surface of the cylindrical base material are formed. A method of manufacturing a cylindrical sputtering target, comprising filling a bonding material into a space to be filled by injecting the bonding material through an adapter installed at an upper end portion of the cylindrical target material .
  2. The manufacturing method according to claim 1, wherein the adapter has a tapered shape.
  3. When injecting the bonding material, the manufacturing method according to claim 1 or 2, characterized in that placing the adapter in the presence of a air vent opening.
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JP6089983B2 (en) * 2012-07-18 2017-03-08 三菱マテリアル株式会社 Cylindrical sputtering target and manufacturing method thereof
CN105378141B (en) 2013-07-05 2018-05-18 旭硝子工业陶瓷株式会社 Sputtering target material and its manufacturing method
JP2015017297A (en) * 2013-07-10 2015-01-29 三菱マテリアル株式会社 In-BASED CYLINDRICAL SPUTTERING TARGET, AND MANUFACTURING METHOD OF THE SAME
JP6332155B2 (en) * 2014-08-28 2018-05-30 住友金属鉱山株式会社 Manufacturing method of cylindrical sputtering target
KR20170074823A (en) * 2014-10-28 2017-06-30 미쓰이금속광업주식회사 Cylindrical ceramic sputtering target and manufacturing device and manufacturing method therefor
JP6341146B2 (en) * 2015-06-17 2018-06-13 住友金属鉱山株式会社 Manufacturing method of cylindrical sputtering target
CN106270866B (en) * 2016-08-30 2018-08-21 常州苏晶电子材料有限公司 A kind of welding method of rotation molybdenum target material

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JP5194460B2 (en) * 2007-01-26 2013-05-08 東ソー株式会社 Cylindrical sputtering target and manufacturing method thereof
JP5103911B2 (en) * 2007-01-29 2012-12-19 東ソー株式会社 Cylindrical sputtering target and manufacturing method thereof
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