JP2018193603A - Method for manufacturing cylindrical target material, method for manufacturing cylindrical sputtering target, jig for machining cylindrical sintered body, grinding device, and cylindrical target material - Google Patents

Abstract

To provide a machining jig that has a smaller concentricity and a simple processing method, and does not generate a trouble such as dirt on a target material and an outer peripheral surface of the target material to be used.SOLUTION: In a method for manufacturing a cylindrical target material including a grinding process in which a cylindrical target material is fabricated by grinding a cylindrical sintered body, the grinding process has: a process S13-a of grinding one end face of a sintered body; a process S13-b of temporarily fastening the sintered body and installing it to a jig for machining a cylindrical sintered body via a temporarily fastening adhesive agent; a process S13-c of grinding the other end face of the sintered body; a process S13-d of grinding an outer peripheral surface and an inner peripheral surface of the sintered body; and a process S13-e of removing a target material obtained by grinding the sintered body, the jig for machining a cylindrical sintered body includes a cylindrical sleeve part, and a base provided on a bottom face of the sleeve part, the inner diameter of the sleeve part is larger than the inner diameter of the sintered body and the outer diameter of the sleeve part is smaller than the outer diameter of the sintered body, the temporarily fastening adhesive agent is applied to the top face of the sleeve part, and the sintered body is temporarily fastened.SELECTED DRAWING: Figure 5

Description

  The present invention relates to a method for manufacturing a cylindrical target material, a method for manufacturing a cylindrical sputtering target, a jig for processing a cylindrical sintered body, a grinding apparatus, and a cylindrical target material.

  Conventionally, it has been proposed to increase the usage efficiency of a target by making a flat sputtering target into a cylindrical shape. This sputtering method uses a cylindrical sputtering target consisting of a cylindrical backing tube and a cylindrical target material formed on the outer periphery thereof, and a magnetic field generating facility and a cooling facility are installed inside the backing tube to form a cylindrical shape. Sputtering is performed while rotating the sputtering target. It is said that the use efficiency of the target, which has been 20% to 30% so far, can be increased to 60% to 70% by using the cylindrical sputtering target.

  Since the sintered body of the ceramic material used for this cylindrical target has low mechanical strength and is brittle, there is a problem that it is difficult to machine the cylindrical sintered body in the process of manufacturing the cylindrical target. If the cylindrical workpiece that has been processed from a sintered body has a large misalignment between the center of the outer diameter and the center of the inner diameter (hereinafter referred to as concentricity), the cylindrical target will be decentered and rotated, making sputtering unstable. is there. In addition, a cylindrical target with multiple cylindrical workpieces joined has a large step difference in the outer diameter of the cylindrical target due to the addition of a variation in bonding accuracy to the degree of concentricity. Discharge occurs frequently.

  For this reason, in Patent Document 1, using a lathe, the inner diameter of the sintered ceramics is first processed by processing the inner diameter of the cylindrical ceramic sintered body and then processing the tapered fixing jig (with the hole for center alignment). It is described that the concentricity (eccentricity) can be reduced to 0.2 mm or less by fitting and fixing both ends of the fixing jig with a lathe to process the outer diameter.

  In Patent Document 2, grinding is performed using a rotating grindstone as a processing method, and alignment is performed by inserting a thin metal wire between a sintered body and a fixing jig, and concentricity is less than 0.5 mm (0. (04 mm to 0.4 mm) is disclosed. Unlike lathe processing, grinding processing can be performed on brittle ceramic materials while suppressing the occurrence of cracks and chips.

  Patent Document 3 discloses a method of grinding the outer diameter of a cylindrical sintered body by inserting and fixing the inner diameter of the cylindrical sintered body with three or more support claws coated with rubber.

  In Patent Document 4, a temporary fixing adhesive is applied and fixed to an end face of a cylindrical sintered body, and a concentricity is 0.30 mm or less (0.09 mm to 0.00) using a cylindrical grinding device and an inner diameter grinding device. 3 mm) is disclosed. In this processing method, since the outer diameter ground workpiece is removed from the cylindrical grinding device and attached to the rotating shaft of the inner diameter grinding device, it is necessary to perform an axis alignment operation. In general, the axis alignment operation is performed by bringing the dial gauge into contact with the outer diameter of the workpiece, rotating the inner diameter grinding device, and adjusting the attachment position of the workpiece so that the deflection of the dial gauge is reduced. By repeating this operation for different length positions of the workpiece, the deviation of the rotation axis can be reduced.

JP 2005-281862 A Japanese Patent Laid-Open No. 2015-036448 JP 2006-044333 A JP 2006-089181 A

  However, according to the manufacturing method described in Patent Document 1, when a brittle sintered body is turned, there is a possibility that cracks and chips occur frequently in the cylindrical processed body. Moreover, in the manufacturing method described in Patent Document 2, when fixing the sintered body and the fixing jig, a temporary fixing adhesive is applied to the outer peripheral surface and the inner peripheral surface having a large area. Even if it carries out, an adhesive component will remain. Furthermore, in the manufacturing method described in Patent Document 3, there is no description about the processing method of the inner diameter, and there is no description about the concentricity. In the manufacturing method described in Patent Document 4, a series of axis alignment operations require time and skill, and the production efficiency is not high.

  As described above, the processing method for adjusting the shape and size of the cylindrical workpiece used in the cylindrical target described in Patent Documents 1 to 4 is not yet sufficient.

  Therefore, in the present invention, in view of the above situation, the cylindrical sintered body used for the cylindrical target has a smaller concentricity and a simple processing method, and the outer peripheral surface of the target material and the sintered body used. New and improved method for manufacturing cylindrical target material, method for manufacturing cylindrical sputtering target, jig for processing cylindrical sintered body, grinding apparatus, and cylindrical target The purpose is to provide materials.

  That is, according to one aspect of the present invention, there is provided a manufacturing method of a cylindrical target material including a grinding step of producing a cylindrical target material by grinding a cylindrical sintered body, wherein the grinding step includes the firing step. A step of grinding one end surface of the bonded body, a step of temporarily fixing the sintered body to a cylindrical sintered body processing jig via a temporary fixing adhesive, and a second end surface of the sintered body. A step of grinding, a step of grinding an outer peripheral surface and an inner peripheral surface of the sintered body, and a step of removing the target material obtained by grinding the sintered body, the cylindrical sintered body The processing jig includes a cylindrical sleeve portion and a base provided on the bottom surface of the sleeve portion, and the inner diameter of the sleeve portion is larger than the inner diameter of the sintered body and the outer diameter of the sleeve portion. Is smaller than the outer diameter of the sintered body, and the temporary adhesive is the sleeve portion. Applied to the top surface, the sintered body is characterized in that it is temporarily fixed.

  In one embodiment of the present invention, it is preferable that the ten-point average surface roughness Rz of the top surface of the sleeve portion is 2 μm or more and 12 μm or less.

  In one embodiment of the present invention, it is preferable that a height of the sleeve portion is 30 mm or more and 100 mm or less.

  Further, in one aspect of the present invention, one end face of the sintered body is ground by an end face processing jig, the end face processing jig includes a pedestal, and a column fixed vertically from the pedestal, A pressing bolt for holding the sintered body, the number of the columns is 3 or 4, and the height of the column is 1/2 or more of the length of the sintered body. It is preferable that the end portion of the pressing bolt is an elastic body.

  In another aspect of the present invention, a cylindrical sputtering target manufacturing method for producing a cylindrical sputtering target, wherein a backing tube is formed in a hollow portion of the cylindrical target material manufactured by the above-described cylindrical target material manufacturing method. And the step of solidifying the bonding material by allowing the target material and the backing tube to cool, and the step of filling the bonding material into the gap between the target material and the backing tube, A bonding step of forming a bonding layer in the gap.

  In another aspect of the present invention, a cylindrical sintered body processing jig for grinding a cylindrical sintered body, the cylindrical sleeve portion, and a base provided on the bottom surface of the sleeve portion, A top surface of the sleeve portion is configured to be able to apply a temporary fixing adhesive for temporarily fixing the sintered body, and an inner diameter of the sleeve portion is larger than an inner diameter of the sintered body, and the sleeve portion The outer diameter is smaller than the outer diameter of the sintered body.

  In another aspect of the present invention, the ten-point average surface roughness Rz of the top surface of the sleeve portion is preferably 2 μm or more and 12 μm or less.

  In another aspect of the present invention, it is preferable that a height of the sleeve portion is 30 mm or more and 100 mm or less.

  In another aspect of the present invention, there is provided a grinding apparatus for grinding a cylindrical sintered body, the grinding means for grinding both end faces, the outer peripheral face and the inner peripheral face of the sintered body, and the above-mentioned cylindrical firing. And a ligation processing jig.

  According to another aspect of the present invention, a cylindrical target material used as a raw material for a cylindrical sputtering target, wherein the concentricity of the outer diameter and the inner diameter is 0.03 mm or less.

  According to the present invention, it is possible to produce a target material having a smaller concentricity, simple grinding means, and no defects such as dirt on the outer peripheral surface.

It is a flowchart which shows the outline of the manufacturing method of the cylindrical target material which concerns on one Embodiment of this invention. It is a schematic explanatory drawing of the grinding device concerning one embodiment of the present invention. It is a schematic sectional drawing for demonstrating the end surface processing jig | tool which concerns on one Embodiment of this invention. It is a schematic sectional drawing for demonstrating the jig | tool for cylindrical sintered compact processing concerning one Embodiment of this invention, (A) is a figure which shows grinding of the other end surface of a cylindrical sintered compact, (B ) Is a diagram showing grinding of the outer peripheral surface of the cylindrical sintered body. It is a flowchart which shows the detail of the grinding process included in the manufacturing method of the cylindrical target material which concerns on one Embodiment of this invention. BRIEF DESCRIPTION OF THE DRAWINGS It is a schematic sectional drawing which shows typically the manufacturing method of the cylindrical target material which concerns on one Embodiment of this invention, (A) is a figure which shows the grinding of the end surface used as the reference surface of a cylindrical sintered compact, (B) is a figure which shows grinding of the other end surface of a cylindrical sintered compact, (C) is a figure which shows grinding of the outer peripheral surface of a cylindrical sintered compact, (D) is a figure of cylindrical sintered compact It is a figure which shows grinding of an internal peripheral surface, (E) is a figure which shows after completion | finish of grinding of a cylindrical sintered compact. It is a flowchart which shows the outline of the manufacturing method of the cylindrical sputtering target which concerns on one Embodiment of this invention.

  Hereinafter, preferred embodiments of the present invention will be described in detail. The present embodiment described below does not unduly limit the contents of the present invention described in the claims, and all the configurations described in the present embodiment are essential as means for solving the present invention. Not necessarily.

  Moreover, the manufacturing method of the cylindrical target material which concerns on one Embodiment of this invention is demonstrated below taking the application to the cylindrical sintered compact used for a cylindrical target as an example.

  In order to solve the problems relating to the processing means for adjusting the shape and size of the cylindrical sintered body used in the above-described cylindrical target material, the present inventors have provided a manufacturing method, a processing jig, and a manufacturing method for obtaining the cylindrical target material. We have earnestly researched about grinding equipment. As a result, one end surface of the cylindrical sintered body is temporarily fixed to the top surface of the jig via a temporary fixing adhesive, and a method for continuously grinding the outer peripheral surface and inner peripheral surface of the cylindrical target material is found. It was.

  Thereby, the process of attaching and removing the cylindrical sintered body is reduced, and the grinding time can be shortened. Moreover, as a result of grinding the outer peripheral surface and the inner peripheral surface continuously without removing the cylindrical sintered body, the concentricity of the target material is set to 0.03 mm or less so that a plurality of target materials are joined together. It was found that abnormal discharge was suppressed. This is presumably because of the small concentricity, the level difference of the cylindrical target material including the variation in joining accuracy when joining a plurality of parts becomes small, and abnormal discharge is suppressed. Hereinafter, the manufacturing method of the cylindrical target material which concerns on this embodiment is demonstrated in detail.

[1. Manufacturing method of cylindrical target material]
FIG. 1 is a flowchart showing an outline of a method for manufacturing a cylindrical target material according to an embodiment of the present invention. The manufacturing method of the cylindrical target material which concerns on one Embodiment of this invention has the formation process S11, the baking process S12, and the grinding process S13, as shown in FIG. Hereinafter, each process will be described.

(Molding process)
In the molding step S11, an oxide powder is used as a raw material, granulated, filled into a cylindrical rubber mold, and a cylindrical formed body is formed by cold isostatic pressing. The oxide powder used as the raw material of the cylindrical sintered body can be appropriately selected according to the use of the target material, and is not particularly limited. For example, it is possible to use an oxide powder mainly composed of indium (In), tin (Sn), zinc (Zn), aluminum (Al), niobium (Nb), tantalum (Ta), titanium (Ti), and the like. it can. Water, a binder, a dispersant, and the like are added to the above-described oxide powder to form a slurry, and the slurry is spray-dried to obtain a granulated powder.

  The granulated powder is filled into a rubber mold, and a cylindrical compression-molded body is produced by cold isostatic pressing (CIP). From the viewpoint of obtaining a high-density cylindrical sintered body, the pressing pressure is preferably molded at a pressure of 100 MPa or more, more preferably 200 MPa or more. If the pressure is less than 100 MPa, a high-density cylindrical sintered body cannot be obtained. The upper limit of the pressure is not particularly limited, but is preferably 500 MPa or less in consideration of the durability of the apparatus.

  As the rubber mold, one constituted by an upper and lower lid, an inner frame and an outer frame can be used. As the material of the rubber mold, for example, silicone rubber can be used for the upper and lower lids, hard plastic rubber can be used for the inner frame, and soft rubber can be used for the outer frame.

  In such compression molding, a time lag occurs when water pressure acts on each part of the rubber mold, so that the flow of the granulated powder varies within the molding mold, and the shape of the resulting cylindrical formed body may be distorted. is there.

(Baking process)
In the firing step S12, the cylindrical formed body is fired to obtain a cylindrical sintered body. Specifically, the cylindrical formed body is fired using a firing furnace and sintered to produce a cylindrical sintered body. In the firing step, first, degreasing treatment is performed to decompose and volatilize organic components such as a binder and a dispersant from the molded body. Specifically, the organic component is decomposed and volatilized by heating the cylindrical formed body at 300 ° C. to 500 ° C., preferably 350 ° C. to 450 ° C., for 50 hours to 300 hours, preferably 100 hours to 200 hours. When the heating temperature is less than 300 ° C. or the heating time is less than 50 hours, a sufficient degreasing effect cannot be obtained. On the other hand, when the heating temperature exceeds 500 ° C. or the heating time exceeds 300 hours, productivity deteriorates.

The degreasing treatment is preferably performed in an air atmosphere. Specifically, the degreasing treatment is performed in a state where the atmosphere gas (air) is circulated in the firing furnace at a rate of 100 L / min to 600 L / min, preferably 200 L / min to 400 L / min per 1 m ³ of the furnace volume. By circulating air at such a flow rate, the furnace temperature can be controlled within a range of ± 20 ° C. while sufficiently decomposing and volatilizing the organic components in the cylindrical formed body, so that the density is high and uniform. It becomes possible to obtain a simple cylindrical sintered body.

  After the degreasing treatment, it is necessary to heat and sinter the cylindrical formed body at a higher temperature. At this time, it is preferable to control the heating rate to 15 ° C./hour to 150 ° C./hour or less. Thereby, it is possible to effectively discharge the voids existing inside the cylindrical forming body to the outside. On the other hand, when the temperature rising rate is less than 15 ° C./hour, the productivity is remarkably deteriorated. On the other hand, when the rate of temperature rise exceeds 150 ° C./hour, the temperature distribution in the furnace becomes non-uniform, and it becomes difficult to obtain a uniform cylindrical sintered body. In addition, from the viewpoint of making the temperature distribution in the furnace uniform and allowing the grain growth inside the cylindrical formed body to progress uniformly, the rate of temperature rise is more preferably 130 ° C./hour or less, and 100 ° C./hour or less. More preferably.

  In the firing step S12, it is necessary to appropriately select the sintering temperature of the cylindrical formed body so that the obtained cylindrical sintered body has a sufficiently high density according to its composition. For example, when a cylindrical formed body containing indium oxide as a main component is fired, the sintering temperature is preferably 1200 ° C to 1600 ° C, and more preferably 1300 ° C to 1600 ° C. On the other hand, in the case of firing a cylindrical formed body containing zinc oxide as a main component, the sintering temperature is preferably 1200 ° C to 1400 ° C, and more preferably 1250 ° C to 1350 ° C.

  The firing time (sintering time) at the sintering temperature described above is preferably 5 to 40 hours, preferably 10 to 30 hours, considering the balance between sinterability and productivity. More preferably, it is more preferably 15 hours to 25 hours. If the sintering time is less than 5 hours, it is difficult to obtain a high-density cylindrical sintered body. On the other hand, when the sintering time exceeds 40 hours, the distortion of the cylindrical sintered body becomes large, and the reduction reaction proceeds to significantly increase the volatilization amount of the metal component.

Note that the atmosphere during firing is preferably an oxidizing atmosphere, and more preferably a pure oxygen atmosphere. Specifically, the firing is performed in a state where oxygen is circulated at 100 L / min to 600 L / min, preferably 200 L / min to 400 L / min per 1 m ³ of the furnace volume. This makes it possible to control the furnace temperature within a range of ± 20 ° C. while suppressing the occurrence of oxygen vacancies. Therefore, the cylindrical sintered body (hereinafter referred to as “ It is also possible to obtain a “sintered body”.

The shape of the cylindrical sintered body may be distorted due to variations in the sintering shrinkage rate in the cylindrical formed body, or because the free sintering shrinkage is hindered by restraint with the ground plane. The thus-obtained cylindrical sintered body may have a large strain due to the addition of the strain generated during CIP molding and the strain generated during sintering. The size of the strain is determined by measuring the outer diameter and inner diameter of the cylindrical sintered body at a plurality of locations using calipers, and calculating the outer diameter strain and inner diameter strain by the difference between the maximum value and the minimum value. 2).
Outer diameter strain = Maximum outer diameter measurement value-Minimum outer diameter measurement value (1)
Inner diameter strain = inner diameter measurement maximum value-inner diameter measurement minimum value (2)

Although it varies depending on the conditions at the time of CIP molding and the configuration of the mold, the cylindrical sintered body is distorted with a roundness α ₀ of 0.50 mm or more and a concentricity β ₀ of 1.0 mm or more. There are many cases.

Here, the roundness α ₀ means a value obtained by the diameter method. Specifically, when the outer diameter d ₀ of the cylindrical sintered body is measured at an arbitrary 8 locations, and the maximum value is d _{0 (max)} and the minimum value is d _{0 (min)} , the following formula ( 3).
Roundness: α ₀ = (d _{0 (max)} −d _{0 (min)} ) / 2 (3)

Further, the concentricity β ₀ means the thickness deviation (thickness variation), and the thickness of the cylindrical sintered body is measured at any 8 locations, and the maximum value is t _{0 (max)} and the minimum value. When the value is t _{0 (min)} , it can be obtained by the following equation (4).
Concentricity: β ₀ = t _{0 (max)} −t _{0 (min)} (4)

(Grinding process)
In the grinding step S13, the target material is obtained by grinding the sintered body. In this grinding step S13, a grinding device is used to grind the sintered body by the grinding means. Hereinafter, a grinding apparatus according to an embodiment of the present invention will be described with reference to the drawings.

  FIG. 2 is a schematic explanatory view of a grinding apparatus according to an embodiment of the present invention. As shown in FIG. 2, the grinding apparatus 100 according to the present embodiment includes a grinding unit 110 serving as a grinding unit for grinding the sintered body W, and a cylindrical sintered body processing jig 120 for fixing the sintered body W. With. Hereinafter, each component of the grinding apparatus 100 according to the present embodiment will be described.

  The grinding part 110 has a function of grinding the sintered body W into a desired shape. The grinding unit 110 includes a support shaft 111 extending in the vertical direction (Z-axis) and a cylindrical straight grindstone 112 attached to the tip of the support shaft 111. In the grinding unit 110, a support body 130 is connected to the base end portion of the support shaft 111. The grinding part 110 is driven by driving means such as a motor (not shown) built in the support 130, and the straight grindstone 112 is rotationally driven around the axis C1 via a support shaft 111 connected to the support 130. The support 130 is connected to an up-and-down moving part 131 that moves along a column 132 extending in the vertical direction (Z-axis).

  The ascending / descending moving unit 131 can move the grinding unit 110 in the vertical direction (Z axis) via the support 130 along the column 132 extending in the vertical direction (Z axis) by driving means such as a motor (not shown). It is said.

  The cylindrical sintered body processing jig 120 is used to grind the outer peripheral surface Wc and the inner peripheral surface Wd of the sintered body W with a straight grindstone 112 provided in the grinding part 110. Thereby, the outer peripheral surface Wc and the inner peripheral surface Wd of the cylindrical sintered body can be easily ground, and a target material having a low concentricity can be produced.

  The cylindrical sintered body processing jig 120 is placed on the spindle flange 140. The main shaft flange 140 is fastened to a base 122 (see FIGS. 4A and 4B) provided in a cylindrical sintered body processing jig 120 described later via a bolt or the like. Further, the spindle flange 140 is provided on the top surface side of the drive support portion 141, and is driven to rotate around the axis C2 by the drive support portion 141. The drive support portion 141 is installed on a bed 142 that moves along the horizontal direction (X axis) in order to adjust the position of the sintered body W by drive means such as a motor (not shown). For example, the grinding unit 110 rotates clockwise about the axis C1 as the central axis, while the main shaft flange 140 rotates counterclockwise about the axis C2. That is, the axis C1 and the axis C2 rotate in opposite directions. Thereby, the grinding time of the sintered compact W can be shortened.

  In the grinding part 110, a cup grindstone 117 (see FIG. 4A) may be used instead of the straight grindstone 112 in order to grind the end face of the sintered body W. Accordingly, the other end face Wb, the outer peripheral face Wc, and the inner peripheral face Wd can be continuously ground without removing the cylindrical sintered body W from the main spindle flange 140 of the grinding apparatus. Therefore, the reference face Wa and the other end face Wb can be ground. The parallelism can be reduced, and the perpendicularity with respect to the central axis of the cylindrical sintered body W can also be reduced.

  In this embodiment, in order to form the reference surface of the sintered body W, the cylindrical sintered body processing jig 120 is replaced with an end surface processing jig 150 (see FIG. 3), and the end surface processing jig 150 is replaced. May be provided on the top surface of the spindle flange 140. Hereinafter, an end face processing jig according to an embodiment will be described with reference to the drawings.

  FIG. 3 is a schematic cross-sectional view for explaining an end face processing jig according to an embodiment of the present invention. The end face processing jig 150 according to the present embodiment is used for grinding the reference surface Wa of the cylindrical sintered body W. Here, the reference surface Wa refers to one end surface of a cylindrical sintered body that is temporarily fixed by a temporary fixing adhesive provided in a cylindrical sintered body processing jig described later.

  As shown in FIG. 3, the end surface processing jig 150 according to the present embodiment includes a pedestal 151, a column 152 fixed vertically from the pedestal 151, and a pressing bolt 153 that holds the cylindrical sintered body W. And mounted on the spindle flange 140 of the grinding apparatus. The cylindrical sintered body W is disposed between the support columns 152 and is fixed by pressing with the pressing bolts 153. Further, a grinding part 115 is provided for grinding the reference surface Wa of the cylindrical sintered body W. Hereinafter, each component of the end face processing jig 150 according to the present embodiment will be described.

  The end face processing jig 150 is fixed to a spindle flange 140 provided in the grinding apparatus. Specifically, the pedestal 151 is fixed to the spindle flange 140 via a fastening means such as a bolt. The shape of the base 151 is a columnar shape. The material of the pedestal 151 is not particularly limited, but a metal material such as stainless steel or carbon steel excellent in impact resistance can be used.

  The support column 152 is fixed to the pedestal 151 via a fastening means such as a bolt. Three or four columns 152 are preferable. When the number of the support columns 152 is two, the cylindrical sintered body W cannot be stably held. On the other hand, when the number of the support columns 152 is five, the cylindrical sintered body W can be stably held, but the number of positions to be adjusted increases and the operation becomes complicated. The fixing position of the support column 152 may be enlarged so that the fixing position of the support column can be adjusted according to the outer peripheral surface of the cylindrical sintered body W. Alternatively, a plurality of end face processing jigs having different fixing positions may be prepared.

  The height of the support column 152 is preferably equal to or lower than the height of the cylindrical sintered body W and is equal to or higher than ½ of the height of the cylindrical sintered body W. If it is higher than the height of the cylindrical sintered body W, it will come into contact with the grinding part 115. If it is lower than 1/2 of the height of the cylindrical sintered body W, the cylindrical sintered body W cannot be stably held.

  It is preferable that the pressing bolts 153 are located at two locations, the upper portion and the lower portion of the support column 152. The cylindrical sintered body W cannot be stably held at one place. Although it can be stably held at three places, the number of places to be adjusted increases, and the work becomes complicated.

  An elastic body 153 a is provided at the tip of the pressing bolt 153. In the present embodiment, the elastic body 153a is preferably silicone rubber, acrylic rubber, urethane rubber, fluorine rubber, polysulfide rubber, ethylene propylene rubber, nitrile rubber, butyl rubber, butadiene rubber, or styrene butadiene rubber, and urethane rubber. And butyl rubber are more preferred.

  A cup grindstone 117 is attached to the tip of the support shaft 116 provided in the grinding part 115. The cup grindstone 117 is preferably an electrodeposited diamond. By processing the reference surface Wa as described above, it is possible to remove a large distortion of the end surface generated during the CIP molding, and to form the reference surface Wa perpendicular to the axis C2.

  The grindstone surface 117a of the cup grindstone 117 is preferably inclined with respect to the vertical plane of the axis C1 of the grinding portion 115. Thus, since the grindstone surface 117a is inclined, there is little load and high peripheral speed grinding becomes possible. Thus, the end surface of the cylindrical sintered body can be easily ground by using the cup grindstone 117. The width of the grindstone surface 117a of the cup grindstone 117 ((outer diameter of the grindstone surface) − (inner diameter of the grindstone surface)) is equal to the width of the cylindrical sintered body W ((outer diameter of the cylindrical sintered body) − (cylindrical shape). If it is smaller than the inner diameter of the sintered body)), this can be dealt with by moving the stage of the grinding apparatus in the X-axis direction.

  In the present embodiment, by smoothing one end surface serving as the reference surface Wa of the cylindrical sintered body W with the cup grindstone 117 of the grinding device, the strain on the end surface is removed to smooth the end surface. Such a smoothed reference surface Wa is an end surface (the other end surface Wb) opposite to the reference surface Wa of the cylindrical sintered body using an after-mentioned cylindrical sintered body processing jig, and the outer peripheral surface Wc. When the inner peripheral surface Wd is ground, it is useful for reducing the concentricity of the ground target material.

  Next, a cylindrical sintered body processing jig according to one embodiment will be described with reference to the drawings.

  FIG. 4 is a schematic cross-sectional view for explaining a cylindrical sintered body processing jig according to an embodiment of the present invention, and FIG. 4 (A) shows processing of the other end face of the cylindrical sintered body. FIG. 4B is a diagram showing processing of the outer peripheral surface of the cylindrical sintered body. The cylindrical sintered body processing jig 120 is used for the other end surface grinding, inner peripheral surface grinding, and outer peripheral surface grinding of the cylindrical sintered body W.

  As shown in FIGS. 4A and 4B, the cylindrical sintered body processing jig 120 according to the present embodiment is provided on the cylindrical sleeve portion 121 and the bottom surface 121 a side of the sleeve portion 121. And a base 122. The sleeve portion 121 and the base 122 are integrated in terms of configuration.

  The sintered body W is placed on the sleeve portion 121. The top surface 121b of the sleeve portion 121 is configured to be coated with a temporary fixing adhesive 124 that temporarily fixes the sintered body W. That is, the temporary fixing adhesive 124 is placed on the top surface 121 b of the sleeve portion 121. The reference surface Wa of the cylindrical sintered body W ground with the end face processing jig described above is temporarily fixed to the sleeve portion 121 via the temporary fixing adhesive 124. This is attached to the spindle flange 140 of the grinding apparatus, and the other end face Wb of the cylindrical sintered body W is ground using the grinding part 115. In the grinding part 115, a cup grindstone 117 is attached to the tip of the support shaft 116 in the same manner as the end face processing jig described above. As described above, the other end surface Wb of the cylindrical sintered body W is ground by the grinding with the grindstone surface 117a of the cup grindstone 117, thereby removing the distortion of the other end surface Wb.

  Further, the ten-point average surface roughness Rz of the top surface 121b of the sleeve portion 121 is preferably 1 μm or more and 50 μm or less, and 2 μm or more and 12 μm or less in order to ensure the adhesive strength with the temporary fixing adhesive 124. More preferred. When the ten-point average surface roughness Rz is less than 1 μm, the adhesive strength is insufficient and the cylindrical sintered body W may come off during grinding. On the other hand, when the ten-point average surface roughness Rz exceeds 50 μm, when repeatedly used, the old adhesive remains on the top surface 121b of the sleeve portion 121 and the adhesive strength is lowered, and the cylindrical shape is reduced during grinding. The sintered body W may come off.

  Further, the width (the length obtained by subtracting the inner diameter from the outer diameter) of the top surface 121b of the sleeve portion 121 needs to be 4 mm or more in order to secure the adhesive strength through the temporary fixing adhesive 124. When the width of the top surface 121b of the sleeve portion 121 is smaller than 4 mm, the adhesive strength with the cylindrical sintered body W is insufficient, and the cylindrical sintered body W fixed during grinding may come off.

  The temporary fixing adhesive 124 is used for temporarily fixing the sleeve portion 121 and the cylindrical sintered body W to temporarily fix each other, and the cylindrical sintered body W is separated after finishing the processing. The temporary fixing adhesive 124 uses heat melting of the adhesive, uses adhesive decomposition or chemical change, uses expander (thermally expandable microcapsule, expanded graphite, etc.), etc. Is mentioned. As the temporary fixing adhesive, it is preferable that the adhesive does not easily flow during processing of the cylindrical sintered body W, has a certain degree of adhesiveness and shape retention, and can be easily peeled off after processing. For this reason, it is more preferable that the temporary fixing adhesive 124 uses thermal melting.

  The temporary fixing adhesive 124 using heat melting of the adhesive melts by heating and solidifies when the temperature falls to room temperature or the like, thereby temporarily fixing the sleeve portion 121 and the cylindrical sintered body W. For example, the temporary fixing adhesive 124 is required to be solid at room temperature (5 ° C. to 35 ° C.) and have a heat melting temperature of 50 ° C. or more and 300 ° C. or less. When the heat melting temperature is lower than 50 ° C., the adhesive strength is insufficient, and the cylindrical sintered body W falls off during processing. When the heat melting temperature is higher than 300 ° C., cracks occur in the cylindrical sintered body W when it is peeled off by heating. When peeling with a solvent, the temporary fixing adhesive 124 is not sufficiently dissolved and cannot be peeled off.

  Specifically, the temporary fixing adhesive 124 is a vinyl polymer compound, a petroleum resin, a natural resin such as rosin and its derivatives, a thermoplastic resin such as paraffin wax, or a thermosetting resin such as an epoxy resin. Etc. can be used suitably. In particular, an epoxy resin excellent in adhesive strength is more preferable. In addition, by using an epoxy resin as a temporary fixing adhesive when the average ten-point roughness Rz of the top surface 121b of the sleeve portion 121 is 2 μm or more and 12 μm or less, the top surface 121b of the sleeve portion 121 or the cylindrical firing is obtained. Even if the area of the reference surface Wa of the bonded body W is small, the sleeve portion 121 and the cylindrical sintered body W can be reliably fixed. For this reason, during the grinding of the cylindrical sintered body W, the cylindrical sintered body W does not come off due to vibration.

  The base 122 has a function of holding the sleeve portion 121. The base 122 is formed in a cylindrical shape on the bottom surface 121 a side of the sleeve portion 121. And since the base 122 is attached to the upper surface of the spindle flange 140 with which a grinding apparatus is equipped, the base 122 can be fixed to the spindle flange 140 with fastening means, such as a volt | bolt.

  An opening groove 123 is formed on the bottom surface of the base 122. The opening groove 123 has a function of discharging the grinding fluid and grinding waste accumulated in the sleeve portion 121 to the outside of the cylindrical sintered body processing jig 120. Furthermore, it is preferable that a plurality of opening grooves 123 are formed radially on the bottom surface of the base 122 so that the grinding liquid and the grinding waste can be more reliably discharged by the centrifugal force generated by the rotation of the axis C2.

  Although the material of the sleeve part 121 and the base 122 is not specifically limited, Metal materials, such as stainless steel and carbon steel excellent in impact resistance, can be used.

  Next, in the cylindrical sintered body processing jig 120 according to the embodiment, as shown in FIG. 4B, after the other end face Wb is ground, the cylindrical sintered body W is attached. This is an example when the grinding part 110 is replaced with the straight grindstone 112 from the cup grindstone 117 and used for outer peripheral surface grinding and inner peripheral surface grinding concentric with the axis C2.

  The outer peripheral surface Wc and the inner peripheral surface Wd of the sintered body are ground by a straight grindstone 112 attached to the tip of the support shaft 111 of the grinding unit 110. Thereby, the concentricity between the inner diameter and the outer diameter of the sintered body can be lowered.

  The cylindrical sintered body processing jig 120 is fixed to the spindle flange 140 of the grinding apparatus. Specifically, the base 122 is fixed to the spindle flange 140 via fastening means such as bolts.

  The height of the sleeve 121 is affected by the inner peripheral surface grinding and the outer peripheral surface grinding. For this reason, the height of the sleeve portion 121 is preferably 5 mm or more and 100 mm or less, and more preferably 30 mm or more and 100 mm or less because the cylindrical sintered body W does not vibrate and break during grinding. When the height of the sleeve portion 121 is less than 5 mm, the tip of the straight grindstone 112 provided in the grinding portion 110 may come into contact with the cylindrical sintered body processing jig 120. On the other hand, when the height of the sleeve portion 121 is higher than 100 mm, the strength of the sleeve portion 121 is insufficient, and the cylindrical sintered body W may vibrate and crack during grinding.

  Since the shape of the base 122 is formed in a cylindrical shape on the bottom surface 121a side of the sleeve portion 121, grinding scraps generated when the inner peripheral surface Wd is ground with the straight grindstone 112 can be removed from the bottom surface of the base 122. It can be discharged from the groove 123. As a result, even if the inner peripheral surface Wd in the vicinity of the reference surface Wa is ground with the straight grindstone 112, the grinding debris does not come into contact with the tip of the straight grindstone 112, so that the inner peripheral surface Wd is ground to take out the grinding debris. There is no problem of having to cancel. Further, by providing a through hole (not shown) in the main shaft flange 140, it is possible to discharge grinding waste and the like from the through hole during processing.

  The inner diameter of the sleeve portion 121 is larger than the inner diameter of the cylindrical sintered body W, and the outer diameter of the sleeve portion 121 is smaller than the outer diameter of the cylindrical sintered body W. Specifically, the outer diameter of the top surface 121b of the sleeve portion 121 is made 0.2 mm or more narrower than the target grinding outer diameter of the cylindrical sintered body W. Thereby, the outer peripheral surface can be ground from the upper end to the lower end of the cylindrical sintered body W while the cylindrical sintered body W is attached to the sleeve portion 121. If the difference between the outer diameter of the top surface 121b of the sleeve portion 121 and the target grinding outer diameter of the cylindrical sintered body W is less than 0.2 mm, the straight grindstone 112 may contact the sleeve portion 121 and be damaged. .

  On the other hand, the inner diameter of the top surface 121b of the sleeve portion 121 is 0.2 mm or more wider than the target grinding inner diameter of the cylindrical sintered body W. Thereby, the inner peripheral surface can be ground from the upper end to the lower end of the cylindrical sintered body W while the cylindrical sintered body W is attached to the sleeve portion 121. If the difference between the inner diameter of the top surface 121b of the sleeve portion 121 and the target grinding inner diameter of the cylindrical sintered body W is less than 0.2 mm, the straight grindstone 112 may contact the sleeve portion 121 and be damaged.

Inevitably, the upper limit of the thickness of the top surface 121b of the sleeve portion 121 is 0.2 mm smaller than the target grinding thickness from the maximum thickness of the sleeve portion 121 defined by the following formula (5).
Maximum thickness of sleeve portion 121 = (maximum outer diameter of jig−minimum inner diameter of jig) / 2
= ((Target grinding outer diameter−0.2 mm) − (target grinding inner diameter + 0.2 mm)) / 2
= (Target grinding outer diameter-Target grinding inner diameter) /2-0.2mm
= Target grinding thickness -0.2mm (5)

  In this embodiment, by grinding the other end face, outer peripheral face, and inner peripheral face of the cylindrical sintered body without removing it from the cylindrical sintered body processing jig attached to the spindle flange of the grinding device, The perpendicularity and parallelism can be reduced, and the concentricity of the inner and outer diameters can be reduced. For this reason, in the cylindrical sputtering target produced using this ground cylindrical target material, abnormal discharge hardly occurs.

  Next, details of the grinding step S13 will be described with reference to the drawings.

  FIG. 5 is a flowchart showing details of a grinding process included in the method for manufacturing a cylindrical target material according to an embodiment of the present invention. FIG. 6 is a schematic cross-sectional view schematically showing a grinding procedure of the cylindrical sintered body according to one embodiment of the present invention, and FIG. 6A is a reference plane of the cylindrical sintered body. FIG. 6B is a diagram showing grinding of the other end surface of the cylindrical sintered body, and FIG. 6C is a diagram showing grinding of the outer peripheral surface of the cylindrical sintered body. FIG. 6D is a view showing grinding of the inner peripheral surface of the cylindrical sintered body, and FIG. 6E is a view showing after the grinding of the cylindrical sintered body. As shown in FIG. 5, the grinding step S13 includes a step S13-a for grinding one end surface of the sintered body, a step S13-b for temporarily fixing and installing the sintered body, and the other end surface of the sintered body. Step S13-c, step S13-d for grinding the outer peripheral surface and inner peripheral surface of the sintered body, and step S13-e for removing the target material obtained by grinding the sintered body. Hereinafter, each process will be described with reference to FIGS.

In addition, the manufacturing method of the cylindrical target material which concerns on this embodiment can be applied, without being restrict | limited by the size of the cylindrical sintered compact used as the object, and the distortion (roundness). In the following, the cylindrical sintered body having a roundness α ₀ exceeding 0.03 mm obtained by the molding step S11 and the firing step S12 to which the present embodiment is suitably applied is ground, As an example, a target material having a diameter of 80 mm to 200 mm, an inner diameter of 40 mm to 190 mm, a wall thickness of 5 mm to 20 mm, a total length of 50 mm to 500 mm, and a roundness α ₁ of 0.03 mm or less will be described. explain.

  First, step S13-a grinds one end surface of the sintered body. As shown in FIG. 6A, the end face processing jig 150 is installed on the spindle flange 140 of the grinding apparatus. In order to fix the end face processing jig 150 to the spindle flange 140, a fastening means may be used. The main shaft flange 140 rotates with the axis C2 as the central axis in the vertical direction.

  Next, in order to fix the cylindrical sintered body W to the end face processing jig 150, the cylindrical sintered body W is disposed between the support pillar 152 provided on the end face processing jig 150 and the support pillar 152 on the opposite side. At this time, it arrange | positions so that the center of the cylindrical sintered compact W may correspond in general with the rotation center of a main axis | shaft. Next, the cylindrical sintered body W is fixed to the end surface processing jig 150 by screwing the pressing bolt 153 and pressing the elastic body 153a at the tip of the pressing bolt 153 against the outer peripheral surface of the cylindrical sintered body W. . In addition, when the cylindrical sintered compact W has produced the big distortion by CIP shaping | molding and sintering, since the center of the cylindrical sintered compact W is not clear, if the rotation center is substantially corresponded with the axial center C2. Good. Whether one of the two end faces of the cylindrical sintered body W is used as a reference plane is not particularly limited.

  Then, the cylindrical sintered body W is ground by the cup grindstone 117 attached to the grinding unit 115 of the grinding apparatus. Since the end surface of the cylindrical sintered body W is distorted due to variations in compression molding, variations in sintering shrinkage, and the like, first, the reference surface Wa of the sintered body W is ground by the cup grindstone 117. The cylindrical sintered body W is attached to the end surface processing jig 150, and one end surface serving as the reference surface Wa is ground by the cup grindstone 117 while the main shaft flange 140 rotates about the axis C2. By doing so, it is possible to form the reference surface Wa substantially orthogonal to the central axis of the cylindrical sintered body W.

  Since the grindstone surface 117a (surface on which the workpiece is ground) of the cup grindstone 117 is inclined, the angle of the grindstone rotation axis is adjusted according to the inclination angle, and the grindstone surface 117a is adjusted to be orthogonal to the rotation axis of the main shaft. . The grain size of the cup grindstone 117 is preferably # 80 to # 400, more preferably # 150 to # 350. Further, in grinding of the reference surface Wa of the cylindrical sintered body, the depth of cut is preferably adjusted to 1 μm to 30 μm, and more preferably adjusted to 10 μm to 25 μm. Furthermore, although the abrasive grain used for the cup grindstone 117 is not particularly limited, diamond is preferable because of excellent hardness at room temperature.

  Thus, the reference surface Wa perpendicular to the axis C2 can be formed on the cylindrical sintered body W having a large strain by grinding the end face of the cylindrical sintered body W.

  Then, when the reference surface Wa perpendicular to the axis C2 of the cylindrical sintered body W can be formed, the grinding with the cup grindstone 117 is finished.

  Next, in step S13-b, the sintered body is temporarily fixed to a cylindrical sintered body processing jig via a temporary fixing adhesive. In the cylindrical sintered body W, as shown in FIG. 6B, the reference surface Wa of the cylindrical sintered body W is arranged on the top surface 121b of the sleeve portion 121 provided in the cylindrical sintered body processing jig 120. It is bonded to the temporary fixing adhesive 124 and temporarily fixed to the cylindrical sintered body processing jig 120.

  First, the cylindrical sintered body W is removed from the end face processing jig 150, and the end face processing jig 150 is removed from the spindle flange 140. Next, the reference surface Wa of the cylindrical sintered body W is turned upward so as to face downward. That is, the other end surface Wb of the cylindrical sintered body W faces upward.

  As shown in FIG. 6B, the cylindrical sintered body W is applied to the top surface 121b of the sleeve portion 121 provided in the cylindrical sintered body processing jig 120 with the reference surface Wa of the cylindrical sintered body W. Temporarily fixed to the temporary fixing adhesive 124 and temporarily fixed to the cylindrical sintered body processing jig 120. Here, the top surface 121b of the sleeve portion 121 can be adjusted so that the bonding thickness of the temporary fixing adhesive 124 becomes desired by controlling the amount of the temporary fixing adhesive 124 applied.

  The adhesion thickness of the temporary fixing adhesive 124 is preferably adjusted to 0.005 mm to 0.5 mm. If the adhesive thickness is thinner than 0.005 mm, the adhesive strength is insufficient and the cylindrical sintered body W falls off during grinding. On the other hand, if the adhesion thickness is thicker than 0.5 mm, the cylindrical sintered body W vibrates during grinding and falls off significantly. Next, the cylindrical sintered body processing jig 120 with the cylindrical sintered body W is installed on the spindle flange 140. Tightening means may be used to fix the cylindrical sintered body processing jig 120 to the spindle flange 140. The cylindrical sintered body processing jig 120 with the cylindrical sintered body W is a temporary fixing adhesive 124 disposed on the top surface 121b of the sleeve portion 121 provided in the cylindrical sintered body processing jig 120. It means that the cylindrical sintered body W is temporarily fixed via

  Next, process S13-c grinds the other end surface of a sintered compact. Then, after the cylindrical sintered body W on which the reference surface Wa is formed is temporarily fixed to the cylindrical sintered body processing jig via the temporary fixing adhesive 124, the other end surface Wb of the cylindrical sintered body is: Grinding is performed by the grinding unit 115.

  The other end face Wb of the cylindrical sintered body W is ground by the cup grindstone 117 attached to the grinding portion 115 of the grinding apparatus. When the other end face Wb of the cylindrical sintered body W is perpendicular to the axis C2, grinding by the cup grindstone 117 is finished.

  In step S13-a, in order to improve work efficiency, the cup grindstone 117 may be attached to the grinding portion 115 of the grinding device before the end face processing jig 150 is fixed.

  Further, without removing the cup grindstone 117 shown in FIG. 6A described above, the cup grindstone 117 used in grinding the sintered body W shown in FIG. 6B may not be replaced as it is. In such a case, since the cup grindstone 117 is not replaced, the grinding time of the sintered body W can be shortened. Furthermore, the cup grindstone 117 may be newly replaced in order to eliminate the distortion of the other end face Wb of the cylindrical sintered body W and smoothen it better.

  Next, process S13-d grinds the outer peripheral surface and inner peripheral surface of a sintered compact. As shown in FIG. 6C, the outer peripheral surface Wc of the cylindrical sintered body is ground by the straight grindstone 112 attached to the grinding portion 110 of the grinding apparatus. Since the outer peripheral surface Wc and the inner peripheral surface Wd of the cylindrical sintered body W are distorted due to variations in compression molding, variations in sintering shrinkage, etc., first, the spindle flange 140 rotates around the axis C2 as the central axis. However, the outer peripheral surface Wc of the sintered body W is ground by the straight grindstone 112. The rotation center axis of the outer peripheral surface Wc coincides with the axis C2 of the main shaft flange 140 with high accuracy.

  Further, when the outer peripheral surface Wc of the cylindrical sintered body W is ground, the movable region to be ground by the straight grindstone 112 provided in the grinding part 110 is formed by the sleeve part 121 having a predetermined height, so that the sintered body W Extends to the lower edge of the outer circumferential surface Wc. Thereby, it can grind to the reference surface Wa vicinity of the outer peripheral surface Wc of the sintered compact W. FIG.

  The grain size of the straight grindstone 112 is preferably # 80 to # 200 for rough grinding, preferably # 200 to # 400 for final grinding, and # 150 to # 200 for rough grinding. It is more preferable to use one having a grinding of # 300 to # 400. The abrasive grains used for the straight grindstone 112 are not particularly limited, but diamond is preferred because of excellent hardness at room temperature. It is preferable to perform finish grinding after roughly grinding the outer peripheral surface Wc.

  In rough grinding, the depth of cut is preferably adjusted to 1 μm to 30 μm, and more preferably adjusted to 10 μm to 25 μm. On the other hand, the depth of cut by finish grinding is preferably adjusted to 10 μm or less, and more preferably adjusted to 6 μm or less. Furthermore, the grinding amount in finish grinding is preferably 5 μm or more, and more preferably 10 μm or more.

  When the distortion of the outer peripheral surface Wc of the cylindrical sintered body W is removed and smoothed, the grinding of the outer peripheral surface Wc with the straight grindstone 112 is finished.

  Next, as shown in FIG. 6D, the straight grindstone 112 is put into the hollow portion Wh of the sintered body W because the straight grindstone 112 provided in the grinding portion 110 grinds the inner peripheral surface Wd. Then, the inner peripheral surface Wd of the sintered body W is ground by the straight grindstone 112 while rotating the main shaft flange 140 around the axis C2. Similarly to the outer peripheral surface Wc, the inner peripheral surface Wd may be subjected to rough grinding and then finish grinding.

  Moreover, it is good also as only rough grinding, without finishing the internal peripheral surface Wd. Since the inner peripheral surface Wd is not a sputtering surface but a bonding surface with the backing tube, when the bonding material is poured, the bonding area between the inner peripheral surface Wd and the backing tube is increased, and the inner peripheral surface Wd and the backing surface are increased. The joining rate with the tube can be improved.

  The order of the outer peripheral surface grinding and the inner peripheral surface grinding is not limited, and the outer peripheral surface grinding may be performed after the inner peripheral surface grinding. Furthermore, after performing outer peripheral surface grinding and inner peripheral surface grinding using a grinding wheel for rough grinding, a grinding wheel for finish grinding with the cylindrical sintered body W attached to the cylindrical sintered body processing jig 120 Alternatively, the outer peripheral surface grinding and the inner peripheral surface grinding may be performed.

  Further, after the outer peripheral surface Wc and the inner peripheral surface Wd of the sintered body W are ground with the straight grindstone 112, the other end surface Wb of the sintered body W may be ground with the cup grindstone 117.

  When the distortion of the inner peripheral surface Wd of the cylindrical sintered body W is removed and smoothed, the grinding with the straight grindstone 112 is finished.

  In this manner, the reference surface Wa of the cylindrical sintered body W is temporarily fixed to the cylindrical sintered body processing jig 120 with the temporary fixing adhesive 124, and the other end surface Wb, the inner peripheral surface Wc, and the outer peripheral surface Wd are formed. Since the grinding is performed, the parallelism between the reference surface Wa and the other end surface Wb can be reduced, and the perpendicularity with respect to the central axis of the cylindrical sintered body Wa can also be reduced. Further, the other end face Wb, the inner peripheral face Wc, and the outer peripheral face Wd can be continuously ground without removing the cylindrical sintered body W from the main spindle flange 140 of the grinding apparatus. Generation of deviation can be suppressed, and a cylindrical target material excellent in concentricity can be ground.

  Here, the degree of parallelism means the degree of parallelism of the other end face Wb with respect to the reference plane Wa, and can be obtained by, for example, a height gauge. In addition, the squareness means that the target material is fixed to the scale placed on the surface plate so that the outer peripheral surface thereof is parallel to the regular plate, and at least four reference surfaces in the circumferential direction using a height gauge or the like. It can be obtained by measuring the height on the Wa side and the other end face Wb side and calculating the maximum value of the difference.

  Next, in step S13-e, the target material obtained by grinding the sintered body W is removed. That is, by grinding the outer peripheral surface Wc and the inner peripheral surface Wd of the sintered body W described above, the distortion of the outer peripheral surface Wc and the inner peripheral surface Wd is eliminated, and the grinding of the sintered body W is completed.

  Examples of the peeling means for peeling the temporary fixing adhesive from the sintered body W include a means for dissolving the temporary fixing adhesive 124 with an organic solvent or heating and melting it. However, if impurities remain on the other end face Wb of the cylindrical sintered body W after peeling or the surface roughness of the other end face Wb deteriorates, arcing and nodules are caused during sputtering. For this reason, it is necessary to appropriately select the type of organic solvent or the heating temperature in consideration of the material of the cylindrical sintered body.

  For example, when peeling using an organic solvent, it is preferable to use an organic solvent such as alcohol, methyl ethyl ketone, or ethyl acetate. In the case of peeling by heating and melting, the heating temperature is preferably set to a temperature higher by about 10 ° C. to 50 ° C. than the heat melting temperature of the temporary fixing adhesive 124.

  In the case of peeling by heating and melting, if heated rapidly, the cylindrical sintered body W is caused by the difference in thermal expansion coefficient between the cylindrical sintered body W and the cylindrical sintered body processing jig 120. May crack or chip. For this reason, it is preferable to adjust a heating rate suitably, and it is more preferable to adjust to about 5 to 50 degree-C / min. Furthermore, in order to suppress the remaining of impurities, it is preferable to polish the reference surface Wa of the peeled cylindrical sintered body W.

  As shown in FIG. 6 (E), by removing the cylindrical sintered body W from which both end faces Wa and Wb, the outer peripheral face Wc, and the inner peripheral face Wd have been ground from the cylindrical sintered body processing jig 120. A target material is obtained.

  Therefore, the cylindrical target material manufactured by this embodiment is completed by performing each said process. Thereby, the attachment removal of a cylindrical sintered compact and a centering process are reduced, and the grinding time of 20 to 30% can be shortened. In addition, after grinding the reference surface, the other end face, outer peripheral face and inner peripheral face are ground continuously without removing the sintered body. The concentricity between the outer peripheral surface and the inner peripheral surface can be 0.03 mm or less. In this embodiment, unlike Patent Document 2, by not using an adhesive on the outer peripheral surface of the sintered body, the outer peripheral surface of the cylindrical target material to be sputtered is not contaminated by the adhesive, and at the time of sputtering. Abnormal discharge can be reduced.

  Further, in the present embodiment, grinding using the end face processing jig or the cylindrical sintered body processing jig according to the above-described embodiment is used, and in particular, a cylinder provided in a grinding apparatus having a spindle flange in a vertical direction. A method for manufacturing a cylindrical target material using a jig for processing a shaped sintered body is preferable because it has less distortion and is excellent in workability. Unlike the lathe process, the grinding by such a processing jig has a small grinding load, so that the generation of cracks and chips can be effectively suppressed even when grinding a brittle oxide sintered body.

  Furthermore, in this embodiment, since the large distortion is eliminated from the manufacturing method of the cylindrical target material for which a high sintering density is required, it does not become a big problem at the time of axial alignment work with a backing tube described later.

[3. Target material]
The target material which concerns on one Embodiment of this invention is manufactured by the manufacturing method of the cylindrical target material which concerns on this embodiment mentioned above, and is used for a cylindrical sputtering target. In this cylindrical sputtering target, a target material made of a hollow cylindrical ceramic sintered body is formed on the outer peripheral surface of a cylindrical base material made of Ti material or SUS material, and a low melting point solder joint material, for example, indium containing indium as a main component. A ceramic sintered body and a cylindrical base material are connected with an alloy or the like.

The material of the target material is not particularly limited. For example, ITO (In ₂ O ₃ —SnO ₂ ) and IGZO (In ₂ O ₃ —Ga ₂ O), which are optical film materials used for transparent conductive films and the like, are used. _{3 -ZnO), AZO (Al 2} O 3 -ZnO), and a ZTO (ZnO-SnO ₂₎ or the like.

  The target material according to this embodiment is not particularly limited in size as long as it has a hollow cylindrical shape. In particular, the outer diameter is 80 mm to 200 mm, the inner diameter is 40 mm to 190 mm, the wall thickness is 5 mm to 20 mm, and the overall length is 50 mm to 500 mm is preferred.

  Further, the parallelism and perpendicularity of the end face of the target material are each 0.1 mm or less. In the conventional manufacturing method, a cylindrical target having a large parallelism and perpendicularity of the end face of the target material has a large change in the division gap dimension, resulting in unstable sputtering, and abnormal discharge frequently occurs in some cases. This can be improved.

  Further, the concentricity of the outer diameter and the inner diameter is 0.03 mm or less. By performing the processing jig and the grinding method described above, the concentricity can be made 0.03 mm or less. In the conventional manufacturing method, a cylindrical target having a large concentricity between the center of the outer diameter and the center of the inner diameter of the target material is eccentric and rotated, resulting in unstable sputtering, and abnormal discharge frequently occurs in some cases. This can be improved. Further, this target material can have an outer diameter roundness of 0.04 mm or less and an inner diameter roundness of 0.03 mm or less. In addition, since this target material is excellent in concentricity and roundness, it is suitable for producing a cylindrical sputtering target.

[4. Manufacturing method of cylindrical sputtering target]
FIG. 7 is a flowchart showing an outline of a method for manufacturing a cylindrical sputtering target according to an embodiment of the present invention. As shown in FIG. 7, the manufacturing method of the cylindrical sputtering target according to the present embodiment forms an arrangement step S21 in which the target material and the backing tube are arranged, a filling step S22 in which the bonding material is filled, and a bonding layer. Joining process S23.

  The arranging step S21 prepares a target material produced by the above-described target material manufacturing method and a cylindrical base material (backing tube) made of Ti material or SUS material, and coaxially arranges the backing tube in the hollow portion of the target material. Assemble to become.

  In the filling step S22, the bonding material is filled in the gap between the target material and the backing tube. As the bonding material, in addition to the indium-based low-melting-point bonding material, a resin paste containing indium powder, a conductive resin, or the like can be used. From the viewpoint of conductivity and spreadability, an indium-based low-melting-point bonding material is used. Preferably, an indium-based low melting point bonding material having a melting point of 130 ° C. to 160 ° C. is more preferable. In addition, as a means for filling the gap between the target material and the backing tube with the bonding material, the target material and the backing tube are placed in an upright state, inclined state, or horizontally laid, and the bonding material is inserted into these gaps. Can be filled.

  Joining process S23 solidifies a joining material by allowing a target material and a backing tube to cool, and forms a joining layer in a crevice. By allowing the target material and the backing tube to cool, the bonding material filled in the gap between the target material and the backing tube is cooled, so that a bonding layer in the cylindrical sputtering target is formed.

  Next, after confirming that the bonding material is completely solidified and a bonding layer is formed, the used masking tape and the like are removed, and a cylindrical sputtering target is obtained. Since the obtained cylindrical sputtering target uses a target material made of a sintered body excellent in concentricity, a bonding layer having a high bonding rate is formed, and there are problems such as cracking, chipping and peeling during sputtering. It does not occur.

  By performing the above steps, a bonding layer having a high bonding rate can be formed when a cylindrical sputtering target is manufactured. And in the manufacturing method of a cylindrical sputtering target, the cylindrical sputtering target which does not generate | occur | produce troubles, such as a crack, a chip | tip, and peeling at the time of sputtering, can be obtained. Moreover, in the manufacturing method of a cylindrical sputtering target, since such a cylindrical sputtering target can be obtained easily in industrial scale production, the industrial significance is very large.

  EXAMPLES Hereinafter, although this invention is demonstrated further in detail using an Example and a comparative example, this invention is not limited to these Examples and a comparative example.

Example 1
Water, a binder, and a dispersing agent were added to a mixed powder composed of indium oxide powder and tin oxide powder to form a slurry, and then granulated powder was obtained by spray drying. Next, this granulated powder is filled into a mold comprising an upper lid made of silicone rubber, an outer frame made of soft rubber, and an inner frame made of hard plastic rubber, and a pressure of 294 MPa is applied by the CIP method to form a cylinder. A formed form was obtained. The cylindrical formed body was degreased by raising the temperature to 500 ° C. over 200 hours in an air atmosphere. After that, by switching to a pure oxygen atmosphere, raising the temperature to 1550 ° C. and holding it at this temperature for 20 hours, it is fired to form a cylindrical indium tin oxide (ITO) sintered body having a relative density of 99% (below) , Also referred to as “cylindrical sintered body”).

  As a result of measuring the height, outer diameter and inner diameter of this cylindrical sintered body with calipers, the length was 202.1 to 203.4 mm, the outer diameter was 152.4 mm to 154.6 mm, and the inner diameter was 131.0 mm to 132. As shown in Table 1, the length strain was 1.3 mm, the outer diameter strain was 2.2 mm, and the inner diameter strain was 1.8 mm. The target grinding dimensions were a height of 201 mm, an outer diameter of 151 mm, and an inner diameter of 135 mm.

  In order to grind the cylindrical sintered body, a vertical grinding apparatus (company name: Toyo Advanced Technologies Co., Ltd., product name: TVG) was prepared as a grinding apparatus.

  The end face processing jig shown in FIG. 3 was fixed to the spindle flange of the grinding apparatus by bolting. The end face processing jig has a pedestal outer diameter of 350 mm, a column height of 200 mm, the number of columns is four, the number of pressing bolts is two for each column, and the pedestal, column and pressing bolts are chrome molybdenum steel. Made of urethane rubber at the tip of the pressing bolt.

  Next, the cylindrical sintered body was placed on an end face processing jig. Specifically, as shown in FIG. 3, a cylindrical sintered body was disposed between the columns. At this time, since the sintered body has a large strain, the center of the sintered body is not clear, but it is arranged so as to substantially coincide with the rotation center of the spindle flange. Next, the tip of the pressing bolt was pressed against the outer diameter portion of the sintered body and fixed and installed.

  Next, a cup grindstone was installed in the vertical grinding apparatus. As the cup grindstone, an electrodeposited diamond grindstone having a particle size of # 170 was prepared. Since the cup grindstone is inclined as shown in FIG. 3, the grindstone surface of the cup grindstone was adjusted to be perpendicular to the axis C <b> 2.

  Next, the reference surface of the sintered body was ground. A cylindrical sintered body having a reference surface was prepared by grinding under conditions of a spindle flange rotation speed of 100 rpm, a grinding wheel rotation speed of 3000 rpm, and a cutting depth of 0.02 mm.

  Thereafter, the cylindrical sintered body was removed from the end face processing jig, and the end face processing jig was removed from the spindle flange. Then, the reference surface of the cylindrical sintered body was turned upward so as to face downward.

  Next, in order to grind the other end surface of the cylindrical sintered body, a cylindrical sintered body processing jig shown in FIGS. 4A and 4B was prepared. The cylindrical sintered body processing jig has an outer diameter of the pedestal of 300 mm, an outer diameter of the sleeve portion of 150 mm, an inner diameter of the sleeve portion of 136 mm, a width between the outer diameter of the sleeve portion and the inner diameter of 7 mm, and a high height of the sleeve portion. A chrome molybdenum steel having a thickness of 30 mm and a 10-point average surface roughness Rz of 12 μm on the top surface of the sleeve portion was prepared.

  Next, the reference surface of the cylindrical sintered body was bonded to a temporary adhesive with a heat melting temperature of 120 ° C. (company name: Nikka Seiko Co., Ltd., product name: Adfix) with a thickness of 0. It adjusted so that it might be set to 05 mm, and it fixed to the top face of the sleeve part of the jig for cylindrical sintered compact processing.

  A cylindrical sintered body processing jig to which the cylindrical sintered body was fixed was disposed on the spindle flange of the vertical grinding apparatus. Since the cylindrical sintered body has a large strain, the center of the sintered body is not clear, but after adjusting the position of the cylindrical sintered body processing jig so that it almost coincides with the center of rotation of the main shaft flange, bolts are attached to the main shaft flange. It was fixed by tightening.

  Next, a cup grindstone was installed in the grinding part. In addition, since the cup grindstone is the same as that used for the above-mentioned reference surface grinding, details are omitted.

  Next, the other end surface of the cylindrical sintered body was ground. The grinding conditions were the same as those for the reference surface grinding described above, and grinding was performed until the length between the reference surface and the other end surface reached 200 mm. As a result, the length between the reference surface and the other end surface is the length of the target material.

  Next, instead of the cup grindstone, the straight grindstone was installed in the grinding part. The grinding wheel was replaced by an automatic grinding wheel exchange device of a vertical grinding machine. Two straight grindstones for rough grinding and finish grinding were prepared. For rough grinding, an electrodeposited diamond grindstone with a grain size of # 170 was used, and after grinding the outer peripheral surface under conditions of a spindle flange rotation speed of 100 rpm, a grinding wheel rotation speed of 3000 rpm, and a cutting depth of 0.02 mm, the inner peripheral surface was continuously ground. did. Subsequently, as the finish grinding, only the outer peripheral surface is finish-ground using the electrodeposited diamond grindstone of particle size # 325 under the conditions of the spindle flange rotation speed of 100 rpm, the grindstone rotation speed of 3000 rpm, and the cutting depth of 0.005 mm. And ground to inner diameter.

  Next, the cylindrical sintered body processing jig to which the ground cylindrical sintered body was fixed was removed from the spindle flange, put into an oven, and heated to 150 ° C. When the temporary fixing adhesive was melted, the target material was peeled from the cylindrical sintered body processing jig. The adhesive remaining on the peeled surface of the target material was removed by grinding with emery paper having a particle size of # 320.

  The time rate (grinding time rate) required from the start of the temporary bonding operation to the end of the peeling operation after grinding of the end faces and the inner and outer peripheral surfaces, as shown in Table 2, is the inner and outer peripheral surface grinding of Comparative Example 1 described later. The relative value when the time was 100 was 72, and the grinding time reduction was 28%.

  As a result of measuring the shape of the obtained target material with a three-dimensional measuring machine (company name: Mitutoyo Corporation, product name: Crysta-Apex), as shown in Table 2, the length was 200.01 mm and the outer diameter was 151.02 mm, inner diameter 134.98 mm, end face parallelism 0.05 mm, perpendicularity 0.03 mm, outer diameter roundness 0.008 mm, inner diameter roundness 0.010 mm, outer diameter and The concentricity of the inner diameter was 0.006 mm.

Similarly, another ITO target material was produced, and the two target materials were joined to a backing tube using metal In solder to produce a cylindrical sputtering target. This cylindrical target is attached to a rotary cathode (company name: SCI company, product name: QRM) of a sputtering device, and Ar-2% O ₂ mixed gas, gas pressure 0.6 Pa, DC input power 15 kW / m. Sputter discharge was performed for 1 hour, and the number of abnormal discharges was evaluated. As a result, the number of abnormal discharges was less than 1 time / minute, which was very small and good.

(Example 2)
In Example 2, a cylindrical sintered body was produced in the same manner as in Example 1. As a result, as shown in Table 1, an ITO cylindrical sintered body having a relative density of 99%, a length strain of 1.0 mm, an outer diameter strain of 1.8 mm, and an inner diameter strain of 1.9 mm was obtained. A target material was prepared in the same manner as in Example 1 except that the outer peripheral surface was continuously ground after the inner peripheral surface was ground. The time rate (grinding time rate) required from the start of the temporary bonding operation to the end of the peeling operation after grinding of the end faces and the inner and outer peripheral surfaces, as shown in Table 2, is the inner and outer peripheral surface grinding of Comparative Example 1 described later. The relative value when the time was 100 was 73, and the grinding time reduction was 27%.

  As a result of measuring the shape of the obtained target material with a three-dimensional measuring machine, as shown in Table 2, the parallelism of the end face was 0.07 mm, the perpendicularity was 0.05 mm, and the roundness of the outer diameter was 0.010 mm. The roundness of the inner diameter was 0.009 mm, and the concentricity of the outer diameter and the inner diameter was 0.009 mm. Further, another target material was prepared in the same manner as in Example 1, a cylindrical sputtering target was prepared, and abnormal discharge was evaluated by sputter discharge. As a result, the number of abnormal discharges was less than 1 time / minute. Very good.

Example 3
In Example 3, a cylindrical sintered body was produced in the same manner as in Example 1 except that zinc oxide powder and aluminum oxide powder were used and sintered at 1340 ° C. in an air atmosphere. As a result, as shown in Table 1, an AZO cylindrical sintered body having a relative density of 97%, a length strain of 1.9 mm, an outer diameter strain of 2.0 mm, and an inner diameter strain of 1.8 mm was obtained. A target material was produced in the same manner as in Example 1 except that the column height was 120 mm. The time rate (grinding time rate) required from the start of the temporary bonding operation to the end of the peeling operation after grinding of the end faces and the inner and outer peripheral surfaces, as shown in Table 2, is the inner and outer peripheral surface grinding of Comparative Example 1 described later. The relative value when the time was 100 was 74, and the grinding time reduction was 26%.

  As a result of measuring the shape of the obtained target material with a three-dimensional measuring machine, as shown in Table 2, the parallelism of the end face was 0.04 mm, the perpendicularity was 0.07 mm, and the roundness of the outer diameter was 0.015 mm. The roundness of the inner diameter was 0.020 mm, and the concentricity of the outer diameter and the inner diameter was 0.011 mm. Further, another target material was prepared in the same manner as in Example 1, a cylindrical sputtering target was prepared, and abnormal discharge was evaluated by sputter discharge. As a result, the number of abnormal discharges was less than 1 time / minute. Very good.

(Example 4)
In Example 4, a cylindrical sintered body was produced in the same manner as in Example 1 except that zinc oxide powder and aluminum oxide powder were used and sintered at 1340 ° C. in an air atmosphere. As a result, as shown in Table 1, an AZO cylindrical sintered body having a relative density of 97%, a length strain of 2.0 mm, an outer diameter strain of 2.1 mm, and an inner diameter strain of 1.9 mm was obtained. A target material was produced in the same manner as in Example 1 except that the surface width of the sleeve portion of the cylindrical sintered body processing jig was 4 mm. The time rate (grinding time rate) required from the start of the temporary bonding operation to the end of the peeling operation after grinding of the end faces and the inner and outer peripheral surfaces, as shown in Table 2, is the inner and outer peripheral surface grinding of Comparative Example 1 described later. The relative value when the time was 100 was 74, and the grinding time reduction was 26%.

  As a result of measuring the shape of the obtained target material with a three-dimensional measuring machine, as shown in Table 2, the parallelism of the end face was 0.03 mm, the perpendicularity was 0.05 mm, and the roundness of the outer diameter was 0.022 mm. The roundness of the inner diameter was 0.015 mm, and the concentricity of the outer diameter and the inner diameter was 0.010 mm. Further, another target material was prepared in the same manner as in Example 1, a cylindrical sputtering target was prepared, and abnormal discharge was evaluated by sputter discharge. As a result, the number of abnormal discharges was less than 1 time / minute. Very good.

(Example 5)
In Example 5, a cylindrical sintered body was produced in the same manner as in Example 1 except that zinc oxide powder and aluminum oxide powder were used and sintered at 1340 ° C. in an air atmosphere. As a result, as shown in Table 1, an AZO cylindrical sintered body having a relative density of 97%, a length strain of 1.5 mm, an outer diameter strain of 2.4 mm, and an inner diameter strain of 2.1 mm was obtained. A target material was produced in the same manner as in Example 1 except that the height of the sleeve portion of the cylindrical sintered body processing jig was set to 100 mm. The time rate (grinding time rate) required from the start of the temporary bonding operation to the end of the peeling operation after grinding of the end faces and the inner and outer peripheral surfaces, as shown in Table 2, is the inner and outer peripheral surface grinding of Comparative Example 1 described later. The relative value when the time was 100 was 76, and the grinding time reduction was 24%.

  As a result of measuring the shape of the obtained target material with a three-dimensional measuring machine, as shown in Table 2, the parallelism of the end face was 0.09 mm, the perpendicularity was 0.09 mm, and the roundness of the outer diameter was 0.026 mm. The roundness of the inner diameter was 0.018 mm, and the concentricity of the outer diameter and the inner diameter was 0.020 mm. Further, another target material was prepared in the same manner as in Example 1, a cylindrical sputtering target was prepared, and abnormal discharge was evaluated by sputter discharge. As a result, the number of abnormal discharges was less than 1 time / minute. Very good.

(Example 6)
In Example 6, a cylindrical sintered body was produced in the same manner as in Example 1 except that zinc oxide powder and tin oxide powder were used and sintered at 1340 ° C. in an oxygen atmosphere. As a result, as shown in Table 1, a ZTO cylindrical sintered body having a relative density of 95%, a length strain of 1.6 mm, an outer diameter strain of 2.0 mm, and an inner diameter strain of 2.0 mm was obtained. A target material was prepared in the same manner as in Example 1 except that the ten-point average surface roughness Rz of the top surface of the sleeve portion of the cylindrical sintered body processing jig was 2 μm. The time rate (grinding time rate) required from the start of the temporary bonding operation to the end of the peeling operation after grinding of the end faces and the inner and outer peripheral surfaces, as shown in Table 2, is the inner and outer peripheral surface grinding of Comparative Example 1 described later. The relative value when the time was 100 was 73, and the grinding time reduction was 27%.

  As a result of measuring the shape of the obtained target material with a three-dimensional measuring machine, as shown in Table 2, the parallelism of the end face was 0.05 mm, the perpendicularity was 0.04 mm, and the roundness of the outer diameter was 0.032 mm. The roundness of the inner diameter was 0.022 mm, and the concentricity of the outer diameter and the inner diameter was 0.015 mm. Further, another target material was prepared in the same manner as in Example 1, a cylindrical sputtering target was prepared, and abnormal discharge was evaluated by sputter discharge. As a result, the number of abnormal discharges was less than 1 time / minute. Very good.

(Example 7)
In Example 7, a cylindrical sintered body was produced in the same manner as in Example 1 except that zinc oxide powder and tin oxide powder were used and sintered at 1340 ° C. in an oxygen atmosphere. As a result, as shown in Table 1, a ZTO cylindrical sintered body having a relative density of 95%, a length strain of 1.8 mm, an outer diameter strain of 2.3 mm, and an inner diameter strain of 2.2 mm was obtained. Example 1 except that an epoxy resin (company name: manufactured by Nikka Seiko Co., Ltd., product name: B bond) was used as a temporary fixing adhesive at a heat melting temperature of 280 ° C., and it was peeled off by heating to 310 ° C. in an oven. A target material was produced in the same manner as described above. The time rate (grinding time rate) required from the start of the temporary bonding operation to the end of the peeling operation after grinding of the end faces and the inner and outer peripheral surfaces, as shown in Table 2, is the inner and outer peripheral surface grinding of Comparative Example 1 described later. The relative value when the time was 100 was 75, and the grinding time reduction was 25%.

  As a result of measuring the shape of the obtained target material with a three-dimensional measuring machine, as shown in Table 2, the parallelism of the end face was 0.04 mm, the perpendicularity was 0.06 mm, and the roundness of the outer diameter was 0.006 mm. The roundness of the inner diameter was 0.004 mm, and the concentricity of the outer diameter and the inner diameter was 0.002 mm. Further, another target material was prepared in the same manner as in Example 1, a cylindrical sputtering target was prepared, and abnormal discharge was evaluated by sputter discharge. As a result, the number of abnormal discharges was less than 1 time / minute. Very good.

(Comparative Example 1)
In Comparative Example 1, a cylindrical sintered body was produced in the same manner as in Example 1. As a result, as shown in Table 1, an ITO cylindrical sintered body having a relative density of 99%, a length strain of 1.4 mm, an outer diameter strain of 2.1 mm, and an inner diameter strain of 2.2 mm was obtained. After fixing the cylindrical sintered body on the table of the surface grinding machine with a magnet and grinding the reference surface, the fixing was removed and the sintered body was turned upside down, and the other end surface of the cylindrical sintered body was ground. . Next, after bonding one end surface to the flat fixture using a temporary fixing adhesive having a heat melting temperature of 120 ° C., the outer peripheral surface was ground using a cylindrical grinding apparatus having a horizontal rotation axis. . The flat plate-shaped fixing jig in which the ground cylindrical sintered body was fixed was removed from the cylindrical grinding apparatus, put into an oven, and heated to 150 ° C. When the temporary fixing adhesive was melted, the cylindrical sintered body was peeled off from the flat fixture and removed. This cylindrical sintered body is attached to the three-jaw scroll chuck of the internal grinding device, and rotated while the dial gauge is in contact with the outer peripheral surface, so that the rotation axis of the internal grinding device and the central axis of the outer peripheral surface are aligned. The work was done. The same operation was repeated at different positions of the cylindrical sintered body at the position of the dial gauge to reduce the displacement of the rotating shaft, and then the inner peripheral surface was ground and removed to obtain a cylindrical target material. The time rate (grinding time rate) required from the start of the temporary bonding operation for grinding the outer peripheral surface to the end of the removal operation after grinding the inner peripheral surface was taken as a relative value of 100 and is shown in Table 2.

  As a result of measuring the shape of the obtained target material with a three-dimensional measuring machine, as shown in Table 2, the parallelism of the end face was as large as 0.36 mm and the perpendicularity was as large as 0.67 mm. The roundness of the outer diameter was 0.008 mm and the roundness of the inner diameter was 0.010 mm. However, the concentricity of the outer diameter and the inner diameter was 0.200 mm, and the center positions of the outer diameter and the inner diameter were misaligned. It was. Further, another target material was produced in the same manner as in Example 1, and a cylindrical sputtering target was produced in the same manner as in Example 1. As a result of performing abnormal discharge evaluation by performing sputter discharge, abnormal discharge was performed once / Occurs for over a minute.

(Comparative Example 2)
In Comparative Example 2, a cylindrical sintered body was produced in the same manner as in Example 1. As a result, as shown in Table 1, an ITO cylindrical sintered body having a relative density of 99%, a length strain of 1.7 mm, an outer diameter strain of 1.9 mm, and an inner diameter strain of 2.4 mm was obtained. When the reference surface was ground in the same manner as in Example 1 except that the column height of the end surface processing jig was 70 mm, the cylindrical sintered body was detached from the end surface processing jig and damaged. As shown in Table 2, the shape was not measured with a three-dimensional measuring machine, and a cylindrical target material was not produced.

(Comparative Example 3)
In Comparative Example 3, a cylindrical sintered body was produced in the same manner as in Example 1. As a result, as shown in Table 1, an ITO cylindrical sintered body having a relative density of 99%, a length strain of 1.2 mm, an outer diameter strain of 2.5 mm, and an inner diameter strain of 1.7 mm was obtained. When the outer peripheral surface of the cylindrical sintered body was fixed in a state where no urethane rubber was provided at the end of the pressing bolt of the end face processing jig, a crack occurred in the sintered body, and thus grinding was not performed. As shown in Table 2, the shape was not measured with a three-dimensional measuring machine, and a cylindrical target material was not produced.

(Comparative Example 4)
In Comparative Example 4, a cylindrical sintered body was produced in the same manner as in Example 1. As a result, as shown in Table 1, an ITO cylindrical sintered body having a relative density of 99%, a length strain of 1.1 mm, an outer diameter strain of 2.2 mm, and an inner diameter strain of 2.0 mm was obtained. Except that the end face width of the sleeve portion of the cylindrical sintered body processing jig is 3 mm, the cylindrical sintered body is removed from the cylindrical sintered body processing jig when ground in the same manner as in Example 1. It was detached and damaged. As shown in Table 2, the shape was not measured with a three-dimensional measuring machine, and a cylindrical target material was not produced.

(Comparative Example 5)
In Comparative Example 5, a cylindrical sintered body was produced in the same manner as in Example 1 except that zinc oxide powder and aluminum oxide powder were used and sintered at 1340 ° C. in an air atmosphere. As a result, as shown in Table 1, an AZO cylindrical sintered body having a relative density of 97%, a length strain of 2.2 mm, an outer diameter strain of 1.9 mm, and an inner diameter strain of 2.1 mm was obtained. Grinding was performed in the same manner as in Example 1 except that the height of the sleeve portion of the jig for processing the cylindrical sintered body was set to 120 mm. Canceled. As shown in Table 2, the shape was not measured with a three-dimensional measuring machine, and a cylindrical target material was not produced.

(Comparative Example 6)
In Comparative Example 6, a cylindrical sintered body was produced in the same manner as in Example 1 except that zinc oxide powder and aluminum oxide powder were used and sintered at 1340 ° C. in an air atmosphere. As a result, as shown in Table 1, an AZO cylindrical sintered body having a relative density of 97%, a length strain of 1.5 mm, an outer diameter strain of 2.1 mm, and an inner diameter strain of 2.1 mm was obtained. Grinding in the same manner as in Example 1 except that the ten-point average surface roughness Rz of the top surface of the sleeve portion of the cylindrical sintered body processing jig was 1 μm. It broke off from the binding tool. For this reason, as shown in Table 2, the shape was not measured with a three-dimensional measuring machine, and a cylindrical target material was not produced.

(Comparative Example 7)
In Comparative Example 7, a cylindrical sintered body was produced in the same manner as in Example 1 except that zinc oxide powder and aluminum oxide powder were used and sintered at 1340 ° C. in an air atmosphere. As a result, as shown in Table 1, an AZO cylindrical sintered body having a relative density of 97%, a length strain of 2.6 mm, an outer diameter strain of 1.9 mm, and an inner diameter strain of 1.8 mm was obtained. Grinding was performed in the same manner as in Example 1 except that the ten-point average surface roughness Rz of the top surface of the sleeve portion of the cylindrical sintered body processing jig was 50 μm. It was detached from the jig for processing the shaped sintered body and damaged. The temporary tacking adhesive from the previous time remained on the top surface of the sleeve, and was peeled off at the interface with the new adhesive. For this reason, as shown in Table 2, the shape was not measured with a three-dimensional measuring machine, and a cylindrical target material was not produced.

(Comparative Example 8)
In Comparative Example 8, a cylindrical sintered body was produced in the same manner as in Example 1 except that zinc oxide powder and aluminum oxide powder were used and sintered at 1340 ° C. in an air atmosphere. As a result, as shown in Table 1, an AZO cylindrical sintered body having a relative density of 97%, a length strain of 2.4 mm, an outer diameter strain of 2.3 mm, and an inner diameter strain of 2.4 mm was obtained. Except for using a temporary adhesive with a heat melting temperature of 40 ° C., grinding was performed in the same manner as in Example 1. As a result, the cylindrical sintered body was detached from the cylindrical sintered body processing jig and damaged. For this reason, as shown in Table 2, the shape was not measured with a three-dimensional measuring machine, and a cylindrical target material was not produced.

(Comparative Example 9)
In Comparative Example 9, a cylindrical sintered body was produced in the same manner as in Example 1 except that zinc oxide powder and aluminum oxide powder were used and sintered at 1340 ° C. in an air atmosphere. As a result, as shown in Table 1, an AZO cylindrical sintered body having a relative density of 97%, a length strain of 1.2 mm, an outer diameter strain of 2.2 mm, and an inner diameter strain of 2.2 mm was obtained. Grinding was carried out in the same manner as in Example 1 except that it was temporarily fixed with an epoxy adhesive having a heat melting temperature of 320 ° C. In order to peel off from the cylindrical sintered body processing jig, it was put in an oven and heated to 350 ° C., but could not be peeled off while partly fixed. The cylindrical target material was damaged when it was strongly peeled off. For this reason, as shown in Table 2, the shape was not measured with a three-dimensional measuring machine, and a cylindrical target material was not produced.

(Consideration based on Examples)
From the results shown in Table 2 obtained by Examples 1 to 7, the manufacturing method of the cylindrical target material according to Examples 1 to 7, the inner diameter of the sleeve portion is larger than the inner diameter of the cylindrical sintered body, In addition, the outer diameter of the sleeve portion is made smaller than the outer diameter of the cylindrical sintered body, and a temporary fixing adhesive is applied to the top surface of the sleeve portion to temporarily fix the sintered body. The concentricity between the diameter and the inner diameter was 0.030 mm or less, which was confirmed to be useful. Moreover, when the processing time of Example 1- Example 7 and the comparative example 1 was compared, it was confirmed that it was shortened by about 30%. And since generation | occurrence | production of abnormal discharge hardly generate | occur | produced in the cylindrical target material obtained by Example 1- Example 7, it was also confirmed that such a cylindrical target material has high industrial value. .

DESCRIPTION OF SYMBOLS 100 Grinding device, 110 Grinding part, 111 Support shaft, 112 Straight grindstone, 115 Grinding part, 116 Support shaft, 117 Cup grindstone, 117a Grinding wheel surface, 120 Cylindrical sintered compact processing jig, 121 Sleeve part, 121a Bottom surface, 121b Top surface, 122 Base, 123 Opening groove, 124 Temporary adhesive, 130 Support, 131 Lifting / moving part, 132 Column, 140 Spindle flange, 141 Rotating / moving part, 142 Bed, 150 End face processing jig, 151 Pedestal, 152 support, 153 pressing bolt, 153a elastic body, C2, C1 axis, W sintered body, Wa reference surface, Wb other end surface, Wc outer peripheral surface, Wd inner peripheral surface, Wh hollow part

Claims (10)

A method for producing a cylindrical target material comprising a grinding step of producing a cylindrical target material by grinding a cylindrical sintered body,
The grinding step includes a step of grinding one end surface of the sintered body, a step of temporarily fixing the sintered body to a cylindrical sintered body processing jig via a temporary fixing adhesive, A step of grinding the other end face of the sintered body, a step of grinding the outer peripheral surface and the inner peripheral surface of the sintered body, and a step of removing the target material obtained by grinding the sintered body. ,
The cylindrical sintered body processing jig includes a cylindrical sleeve portion and a base provided on the bottom surface of the sleeve portion,
An inner diameter of the sleeve portion is larger than an inner diameter of the sintered body, and an outer diameter of the sleeve portion is smaller than an outer diameter of the sintered body,
The method for producing a cylindrical target material, wherein the temporary fixing adhesive is applied to a top surface of the sleeve portion, and the sintered body is temporarily fixed.   2. The method for producing a cylindrical target material according to claim 1, wherein a ten-point average surface roughness Rz of the top surface of the sleeve portion is 2 μm or more and 12 μm or less.   3. The method for manufacturing a cylindrical target material according to claim 1, wherein the sleeve portion has a height of 30 mm to 100 mm. Grinding one end face of the sintered body with an end face processing jig,
The jig for end face processing includes a pedestal, a column fixed vertically from the pedestal, and a pressing bolt for holding the sintered body,
The number of the columns is 3 or 4,
The height of the column is not less than 1/2 of the length of the sintered body and not more than the length of the sintered body,
The method for manufacturing a cylindrical target material according to any one of claims 1 to 3, wherein an end of the pressing bolt is an elastic body. A method of manufacturing a cylindrical sputtering target,
An arrangement step of coaxially arranging a backing tube in a hollow portion of a cylindrical target material manufactured by the method for manufacturing a cylindrical target material according to any one of claims 1 to 4,
A filling step of filling a bonding material into a gap between the target material and the backing tube;
A method of manufacturing a cylindrical sputtering target, comprising: a bonding step of solidifying the bonding material by allowing the target material and the backing tube to cool, and forming a bonding layer in the gap. A cylindrical sintered body processing jig for grinding a cylindrical sintered body,
A cylindrical sleeve portion;
A base provided on the bottom surface of the sleeve portion,
The top surface of the sleeve portion is configured to be capable of applying a temporary fixing adhesive for temporarily fixing the sintered body,
A cylindrical sintered body processing jig, wherein an inner diameter of the sleeve portion is larger than an inner diameter of the sintered body, and an outer diameter of the sleeve portion is smaller than an outer diameter of the sintered body.   The cylindrical sintered body processing jig according to claim 6, wherein a ten-point average surface roughness Rz of the top surface of the sleeve portion is 2 μm or more and 12 μm or less.   The cylindrical sintered body processing jig according to claim 6, wherein a height of the sleeve portion is 30 mm or more and 100 mm or less. A grinding apparatus for grinding a cylindrical sintered body,
Grinding means for grinding both end surfaces, outer peripheral surface, and inner peripheral surface of the sintered body;
A grinding apparatus comprising: the cylindrical sintered body processing jig according to any one of claims 6 to 8. A cylindrical target material used as a raw material for a cylindrical sputtering target,
A cylindrical target material having an outer diameter and an inner diameter of 0.03 mm or less.

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