CN114651086A - Sputtering target and method for producing same - Google Patents
Sputtering target and method for producing same Download PDFInfo
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- CN114651086A CN114651086A CN202080078115.6A CN202080078115A CN114651086A CN 114651086 A CN114651086 A CN 114651086A CN 202080078115 A CN202080078115 A CN 202080078115A CN 114651086 A CN114651086 A CN 114651086A
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
- C04B37/023—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used
- C04B37/026—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used consisting of metals or metal salts
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
- H01J37/3411—Constructional aspects of the reactor
- H01J37/3414—Targets
- H01J37/3423—Shape
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
- H01J37/3488—Constructional details of particle beam apparatus not otherwise provided for, e.g. arrangement, mounting, housing, environment; special provisions for cleaning or maintenance of the apparatus
- H01J37/3491—Manufacturing of targets
Abstract
The present invention relates to a sputtering target capable of using a warped cylindrical base material as a constituent material and a method for manufacturing the same, and provides a novel method for manufacturing a sputtering target capable of eliminating warping of a cylindrical base material even if the axial length of a cylindrical target material is long or even if the cylindrical target material is heated during filling with a bonding material. The present invention provides a method for manufacturing a sputtering target, characterized in that a warpage width of a cylindrical base material is measured, a processing for warping the cylindrical base material in a direction opposite to the warpage direction is performed, a plurality of cylindrical target materials are arranged at intervals in an axial direction on the outer side of the processed cylindrical base material, and the cylindrical base material and the cylindrical target materials are bonded by a bonding material.
Description
Technical Field
The present invention relates to a sputtering target including a cylindrical base material and a plurality of cylindrical target materials and a method for manufacturing the same, and more particularly to a method for manufacturing a sputtering target capable of using a cylindrical base material warped by bending deformation as a material.
Background
In the manufacture of organic EL, liquid crystal displays, touch panels, and other display devices, magnetron sputtering using a flat sputtering target in which a target material is joined to a flat base material is the mainstream for sputtering for forming a transparent conductive thin film made of ITO or the like.
In recent years, rotary sputtering has been put into practical use in which a cylindrical sputtering target in which a target material is joined to an outer peripheral surface of a cylindrical base material is rotated around an axis to perform sputtering. The above-described rotary sputtering has an advantage that high productivity can be obtained because it can achieve an extremely high use efficiency as compared with a flat plate sputtering target.
As glass substrates used in flat panel displays and solar cells have been increased in size, long cylindrical sputtering targets having a length of 2m or more are required to form thin films on the increased size substrates. However, since it is difficult to manufacture a cylindrical target having a length of 2m or more, a plurality of cylindrical targets (also referred to as "divided targets") are arranged outside a long cylindrical substrate in the axial direction.
For example, patent documents 1 and 2 disclose the following: the sputtering target is produced by preparing a plurality of target materials obtained by dividing a target material into a plurality of pieces in the axial direction, arranging the plurality of target materials in an axial direction on the outer peripheral side of a cylindrical base material, and bonding the plurality of target materials to each other with a bonding material.
As the cylindrical sputtering target becomes long as described above, if the cylindrical base material also becomes long, the influence of the cylindrical base material on the warpage becomes non-negligible. In particular, a long cylindrical substrate having a thickness of more than 2m has a problem that the substrate is warped to a large extent and the warpage width is large. If the warpage of the cylindrical base material is large, the thickness of the bonding material becomes uneven, and cooling becomes insufficient in the thin portion of the bonding material, which causes a problem such as cracking during sputtering.
In recent years, sputtering apparatuses for forming a film on a larger 10 th generation glass substrate have been used, and the total length of the target exceeds 3 m. When the total length of the target exceeds 3m, the problem of the warpage as described above becomes more significant.
Therefore, patent document 2 focuses on the eccentricity between the substrate and the target, and proposes the following method for suppressing the eccentricity: the warpage of the cylindrical base material is confirmed before the cylindrical target is manufactured, and when the warpage is large, the warpage of the cylindrical base material is corrected using a press or the like.
Further, patent document 3 presupposes that the cylindrical base material is bent, and a plurality of cylindrical targets are arranged in accordance with the bending deformation of the cylindrical base material. Namely, the following methods are disclosed: the center axis of each cylindrical target is inclined or displaced in the radial direction at an arbitrary position in the circumferential direction, thereby ensuring a required bonding material thickness between the inner circumferential surface of the cylindrical target and the outer circumferential surface of the cylindrical base.
Documents of the prior art
Patent document
Patent document 1: japanese patent laid-open publication No. 2010-100930
Patent document 2: international publication No. 2016/067717
Patent document 3: japanese patent laid-open publication No. 2018-159105
Disclosure of Invention
Problems to be solved by the invention
The invention described in patent document 2 proposes the following problems: when the warpage of the cylindrical base material is measured in advance and the warpage is large, the warpage is corrected using a press or the like. However, if the cylindrical base material is heated in advance or the cylindrical base material is heated by filling a bonding material that is heated and melted between the cylindrical base material and the target material at the time of filling the bonding material, there is a problem of recovery of the corrected warpage (also referred to as "recovery of warpage").
In addition, the invention described in patent document 3 is premised on the use of a curved cylindrical base material, and therefore, when the axial length of the cylindrical target is less than 750mm, a required bonding material thickness can be secured, whereas if the axial length of the cylindrical target is not less than 750mm, it is difficult to secure the required bonding material thickness.
In the case of forming a cylindrical sputtering target by arranging a plurality of cylindrical target materials outside a cylindrical base material, it is preferable to reduce the number of divisions of the cylindrical target materials as much as possible because a gap between the cylindrical target materials causes nodules (nodule) during sputtering. Therefore, as the length of the cylindrical sputtering target increases year by year as described above, the axial length of the cylindrical target material also increases year by year, and the cylindrical target material also tends to increase in length, and thus cannot be limited to less than 750 mm.
Accordingly, the present invention relates to a sputtering target and a method for manufacturing the same, which can use a warped cylindrical base material as a constituent material, and provides a novel method for manufacturing a sputtering target and a novel sputtering target, which can suppress the effect of warping of the cylindrical base material used even when the axial length of the cylindrical target material is long, or even when the cylindrical base material is heated by heating at the time of filling a bonding material, that is, when the bonding material is previously heated at the time of filling the bonding material, or even when the cylindrical base material is heated by filling a heating-melted bonding material between the cylindrical base material and the target material, and as a result, the thickness of the bonding material is uniform, the difference in height between adjacent cylindrical target materials is small, and the axial distance between adjacent cylindrical target materials is uniform.
Means for solving the problems
The present invention provides a method for manufacturing a sputtering target including a cylindrical base material and a cylindrical target material, the method including:
the warpage amplitude of the cylindrical base material was measured,
the cylindrical base material is warped in the direction opposite to the warped direction,
a plurality of cylindrical targets are arranged outside the processed cylindrical substrate at intervals in the axial direction, and the cylindrical substrate and the cylindrical targets are bonded by a bonding material.
The present invention also provides a sputtering target comprising a cylindrical base material and a cylindrical target material, wherein the cylindrical base material and the cylindrical target material are bonded to each other with a bonding material,
at least one of the cylindrical targets has an axial length of 750mm or more, a difference between a maximum value and a minimum value of the thickness of the bonding material is 1.0mm or less, a maximum value of a height difference between outer peripheral surfaces of adjacent cylindrical targets is 0.5mm or less, and a difference between a maximum value and a minimum value of an axial distance between adjacent cylindrical targets is 0.2mm or less.
Effects of the invention
The manufacturing method proposed by the present invention is a method of processing a cylindrical base material so as to warp a predetermined width in a reverse direction opposite to the original warped direction in consideration of the restoration of the warp, which is the re-deformation by heating after the processing of the cylindrical base material. Therefore, even if the axial length of the cylindrical target material is long or the cylindrical target material is heated during filling with the bonding material, the influence of warpage of the cylindrical base material used can be eliminated, and a sputtering target in which the thickness of the bonding material is uniform, the height difference between the adjacent cylindrical target materials is small, and the axial distance between the adjacent cylindrical target materials is uniform can be manufactured.
Therefore, according to the manufacturing method proposed by the present invention, the following sputtering target can be manufactured: the sputtering target is provided with a cylindrical base material and a plurality of cylindrical target materials, wherein the axial length of at least one of the cylindrical target materials is more than 750mm, the difference between the maximum value and the minimum value of the thickness of a bonding material is less than 1.0mm, the maximum value of the height difference between the outer peripheral surfaces of adjacent cylindrical target materials is less than 0.5mm, and the difference between the maximum value and the minimum value of the axial distance between adjacent cylindrical target materials is less than 0.2 mm.
In addition, in the sputtering target described above, since the thickness of the bonding layer is ensured to be uniform, cracks are not easily generated during sputtering, the difference in height between the outer peripheral surfaces of the adjacent cylindrical target materials is small, and the gap interval is uniform, so that the probability of occurrence of an abnormality during sputtering can be significantly reduced. Further, since warpage, that is, warpage is small, the target is rotated with little shaking (japanese text "ブレ"), the distance between the cylindrical target and the substrate can be kept constant, and the quality of the film formed by sputtering can be made uniform.
Drawings
Fig. 1 is a perspective view schematically showing an example of a sputtering target.
Fig. 2 is a perspective view schematically showing an example of a warped cylindrical base material.
Fig. 3 is a diagram schematically showing an example of a method for measuring the warpage width of a cylindrical base material.
Fig. 4 is a side view schematically showing an example of a method of processing a cylindrical base material, where (a) is a view showing a state before processing, and (B) is a view showing a state after processing.
Fig. 5 is a longitudinal sectional view showing an enlarged main part of an example of the manufactured sputtering target.
Fig. 6 is an enlarged cross-sectional view of a main portion for explaining the amount of height difference h and the axial distance d between adjacent targets.
FIG. 7 is a longitudinal sectional view showing an apparatus for producing a sputtering target used in examples.
Detailed Description
The present invention will be described below based on embodiment examples. However, the present invention is not limited to the embodiments described below.
< method for producing main target >
A method for manufacturing a sputtering target according to an embodiment of the present invention (referred to as a "main target manufacturing method") is a method for manufacturing a sputtering target including a cylindrical base material 2 and a plurality of cylindrical target materials 3 and 3 … …, and includes:
the extent of the warpage or the direction of warpage of the cylindrical base material 2 is measured (referred to as "measuring step"),
the cylindrical base material 2 is warped in the direction opposite to the warped direction (referred to as "processing step"),
a plurality of cylindrical targets 3 and 3 … … are arranged outside the processed cylindrical base 2 at intervals in the axial direction, and the cylindrical base 2 and the cylindrical target 3 are bonded by a bonding material 4.
(Main sputtering target)
As shown in fig. 1, a sputtering target ("main sputtering target") 1 produced by the main target production method is a sputtering target as follows: a sputtering target is obtained by arranging a plurality of cylindrical target materials 3 outside one cylindrical base material 2 at intervals in the axial direction of the cylindrical base material 2, and bonding the cylindrical base material 2 and the cylindrical target materials 3 with a bonding material 4 (not shown).
The details of the main sputtering target 1 will be described later. Here, first, the constituent members will be explained.
(target material)
The target is formed of a plurality of cylindrical targets 3, 3 … …, and the plurality of cylindrical targets 3 are disposed on the outer peripheral side of the cylindrical substrate 2 at appropriate intervals in the axial direction of the cylindrical substrate 2.
Each cylindrical target 3 may have an inner diameter larger than the outer diameter of the cylindrical substrate 2.
The following problems have been pointed out: the length of the cylindrical target tends to increase year by year, and if the length of the cylindrical target increases, particularly to 750mm or more, the thickness of the bonding material cannot be secured. However, according to the main target manufacturing method, the above-described problems can be solved, and the effects of the present invention can be further exhibited.
Therefore, from the viewpoint of further exhibiting the effects of the present invention, the axial length L of at least one of the plurality of cylindrical targets 3 and 3 … … is set to be longer3Preferably 750mm or more, more preferably 850mm or more, still more preferably 950mm or more, and still more preferably 1400mm or more.
The material of the cylindrical target 3 is not particularly limited. Examples thereof include oxides containing at least one of Cu, Al, In, Sn, Ti, Ba, Ca, Zn, Mg, Ge, Y, La, Al, Si, Ga and W.
Examples of the oxide include: In-Sn-O, In-Ti-O, In-Ga-Zn-O, In-Zn-Sn-O, In-Ga-Zn-Sn-O, Ga-Zn-O, In-Zn-O, In-Ga-O, I-W-O, I-Zn-W-O, Zn-O, Sn-Ba-O, Sn-Zn-O, Sn-Ti-O, Sn-Ca-O, Sn-Mg-O, Zn-Mg-O, Zn-Ge-O, Zn-Ca-O, Zn-Sn-Ge-O, Cu2O、CuAlO2、CuGaO2、CuInO2And the like.
(cylindrical substrate)
The cylindrical base material 2 is preferably formed in a cylindrical shape having a straight central axis and an outer peripheral surface parallel to the axis. However, as shown in fig. 2, the newly used cylindrical base material or the recycled cylindrical base material 2 is warped in a curved shape, in other words, an arch shape, and the outer peripheral surface of the cylindrical base material 2 has a deviation from the linear axis direction.
The material of the cylindrical substrate 2 may be any metal such as Ti, SUS, or Cu. However, they are not limited thereto.
(bonding Material)
The bonding material 4 is the following material: which is a material obtained by supplying a material in a molten state to a gap between a cylindrical base material 2 and each cylindrical target material 3 arranged at a predetermined position on the outer peripheral side thereof during the production of a sputtering target, filling the gap with the material, solidifying the material, and bonding the cylindrical base material 2 and the cylindrical target material 3 to each other.
The material of the bonding material 4 is not particularly limited as long as it can be used for bonding the target and the base material. Examples thereof include: low melting point solder such as In metal, In — Sn metal, or In alloy metal In which a trace amount of metal component is added to In.
Since the low melting point solder has a melting point of 150 to 250 ℃, the bonding material 4 is usually heated to 150 to 300 ℃ and melted when the bonding material 4 is filled.
< measurement procedure >
In the measurement step, the magnitude of the warpage or the direction of warpage of the cylindrical base material 2 used as a constituent material is measured.
The method for measuring the warpage width is not particularly limited. For example, the displacement width, that is, the warpage width of the outer peripheral surface may be measured by rotating the cylindrical base material 2 around the axis, or the displacement width, that is, the warpage width may be measured along a perpendicular line standing on a flat table with respect to the distance between the flat surface of the flat table and the outer peripheral surface 2a of the cylindrical base material 2 by placing the cylindrical base material 2 on the flat table in the lateral direction. Other methods may also be used.
The position of the measurement of the warpage width may be one or two or more positions in the longitudinal direction of the cylindrical base material 2.
Since the cylindrical base material 2 is often warped in an arch shape, if the warp width is measured in the vicinity of the center portion in the longitudinal direction, the maximum warp width and the warp direction thereof can be measured.
However, the warp is not limited to a constant arch shape, and therefore, the warp width is preferably measured at a plurality of positions at intervals in the longitudinal direction. For example, the measurement is preferably performed at intervals of 100mm to 1000mm, more preferably at intervals of 200mm or more and 800mm or less, and particularly preferably at intervals of 500mm or less.
An example of a specific measurement method for measuring the warpage width will be described.
As shown in fig. 3, the cylindrical base material 2 is set horizontally and axially rotatable, a dial indicator 5 is pressed against the outer peripheral surface 2a of the cylindrical base material 2, the cylindrical base material 2 is rotated once, and the reading of the dial indicator 5 is measured. The maximum value H of the reading of the dial indicator 5 can then be determinedmaxAnd minimum value HminDifference (H)max-Hmin) As the magnitude of the warpage.
At this time, means for rotating the cylindrical base material 2 is arbitrary. For example, the substrate may be rotated by placing it between two rotating rollers, or by placing the cylindrical substrate near both ends thereof in a groove of a support table having a v-shaped groove and rotating it by hand or a roller.
In the measurement step, the original warpage width X or warpage direction of the obtained cylindrical base material 2 may be measured as described above, or the obtained cylindrical base material 2 may be heated, and then the warpage width Y or warpage direction of the heated cylindrical base material 2 may be measured as described above.
When the cylindrical base material 2 is heated and the warpage width Y or warpage direction of the heated cylindrical base material is measured, the heating temperature of the cylindrical base material 2 is preferably set to a temperature at which the cylindrical base material 2 is heated when the bonding material is filled, that is, when the bonding material 4 melted by heating is filled between the cylindrical base material 2 and the cylindrical target 3, or a temperature at which the cylindrical base material 2 is heated by the filled bonding material 4. However, if the temperature is too high, surface oxidation of the cylindrical base material 2 is likely to occur. From this viewpoint, the heating temperature of the cylindrical substrate 2 at this time is preferably to 150 to 300 ℃ in surface temperature, more preferably to 160 ℃ or higher or 240 ℃ or lower, and still more preferably to 170 ℃ or higher or 230 ℃ or lower.
The method of heating the cylindrical base material 2 is not particularly limited. For example, the substrate may be placed in an electric furnace or the like and heated from the outside, or a heater may be provided inside the substrate and heated from the inside.
< working procedure >
In the machining step, the cylindrical base material 2 is machined so as to be warped by a predetermined width α in a reverse direction to the original warped direction.
For example, as shown in fig. 4, the cylindrical base material 2 may be bent by pressing the measurement position in the measurement step in the direction opposite to the warping direction measured in the measurement step, and as shown in fig. 4(B), the cylindrical base material 2 may be processed so as to reverse the warping direction by only the warping width α, in other words, so as to displace only α from the linear axis.
The pressing position may be a position where one point of the axial center portion is pressed and deformed, for example, when the cylindrical base material 2 is warped in an arch shape. Further, it is preferable to pressurize the position measured in the measuring step. For example, the measurement is performed at intervals of 100mm to 1000mm, and it is preferable to deform the sample by applying pressure to each measurement point.
The width α (mm) of the cylindrical base material 2 warped in the direction opposite to the warped direction is preferably determined based on the warp width X or Y measured in the above-described measurement step. This is because the larger the warpage width X or Y is, the larger the magnitude of the warpage recovery caused by heating after processing is.
For example, in the measurement step, when the original warpage width of the cylindrical base material 2 obtained is measured to obtain the warpage width X, the warpage width α (mm) is preferably X (mm) X (0.10 to 2.00), more preferably X (mm) X0.50 or more or X (mm) X1.50 or less, still more preferably X (mm) X0.80 or more or X (mm) X1.40 or less, and still more preferably X (mm) X0.90 or more or X (mm) X1.30 or less.
In the measurement step, when the obtained cylindrical base material 2 is heated and the warpage width of the heated cylindrical base material 2 is measured to obtain the warpage width, the warpage width α (mm) is preferably y (mm) x (0.50 to 1.50), more preferably y (mm) x 0.80 or more, even more preferably y (mm) x 0.90 or more, or y (mm) x 1.30 or less, even more preferably y (mm) x 0.95 or more, or y (mm) x 1.25 or less.
If the warpage width Y after heating is actually measured and the warpage width α is determined based on the warpage width Y, the warpage recovery can be further reduced because the width α can be determined in consideration of the heating behavior of the cylindrical base material 2 obtained.
As a processing method for warping the cylindrical base material 2 by pressing, for example, as shown in fig. 4(a), a method of pressing the cylindrical base material 2 in a direction opposite to the warped direction at the measurement position (1 or more) in the measurement step is exemplified. In fig. 4(a), P represents the pressing direction. In this case, examples of the means for pressing include mechanical press working and forging working.
However, any means may be employed if the cylindrical base material 2 can be warped only by a desired extent.
In this case, in order not to change the roundness of the cylindrical base material, an arc-shaped terminal or the like corresponding to the shape of the cylindrical base material 2 may be used as a terminal to which pressure is applied.
Further, heat treatment (annealing) may be further performed as necessary.
Further, the processing method of pressing and warping the cylindrical base material 2 may be repeated. That is, the cylindrical base material 2 may be warped by applying pressure such as pressing the cylindrical base material 2 to warp it and further pressing the cylindrical base material to warp it, and finally the cylindrical base material 2 may be warped by the predetermined width α.
Further, the cylindrical base material 2 may be warped by heating and pressing (measuring the warping width Y) and then warping, or by heating and pressing such as further heating and pressing and then warping, and finally the cylindrical base material 2 may be warped by the predetermined width α. In this case, the warpage width Y may be measured after heating.
< arrangement of cylindrical target >
Using the cylindrical substrate 2 processed as described above, a plurality of cylindrical targets 3, 3 … … are arranged at appropriate intervals in the axial direction on the outer circumferential side of the cylindrical substrate 2.
The cylindrical targets 3 are preferably arranged in parallel at an interval of 0.15mm to 0.50mm in the axial direction.
< engagement >
After the cylindrical targets 3 are arranged as described above, the cylindrical base 2 and the cylindrical targets 3 are heated, the bonding material 4 in a molten state is filled in the gap between the cylindrical base 2 and the cylindrical targets 3, the bonding material 4 is cooled, and the cylindrical targets 3 are bonded to the periphery of the cylindrical base 2 by the bonding material 4.
The temperature at which the cylindrical base 2 and the cylindrical target 3 are heated before the bonding material 4 is filled is preferably set to be equal to or higher than the temperature of the bonding material 4.
The temperature of the bonding material 4 when the bonding material 4 is filled is a temperature equal to or higher than the melting point of the bonding material, and is preferably heated to 150 to 300 ℃, more preferably 160 ℃ or higher or 240 ℃ or lower, and still more preferably 170 ℃ or higher or 230 ℃ or lower.
The method of filling and cooling the bonding material may be a known method.
< main sputtering target >
According to the main target manufacturing method, even if the heating at the time of filling the bonding material is performed, the influence of the warpage of the cylindrical base material 2 can be eliminated, and therefore, a main sputtering target as described below can be manufactured.
As a preferable example of the main sputtering target, a sputtering target having a cylindrical shape can be mentionedA sputtering target comprising a base material 2 and a plurality of cylindrical target materials 3 and 3 … …, wherein at least one of the cylindrical target materials 3 and 3 … … has an axial length L3750mm or more, the difference between the maximum value and the minimum value of the thickness of the bonding material 4 is 1.0mm or less, the maximum value of the height difference h between the outer peripheral surfaces 3a, 3a of the adjacent cylindrical targets 3, 3 is 0.5mm or less, and the difference between the maximum value and the minimum value of the axial distance d between the adjacent cylindrical targets 3, 3 is 0.2mm or less.
From the viewpoint of further exhibiting the effects of the present invention, the length of the cylindrical base material 2 is preferably 2.0m to 4m, more preferably 3.0m or more or 3.8m or less, and still more preferably 3.3m or more or 3.7m or less.
The outer diameter of the cylindrical substrate 2 is preferably 125mm to 140mm, more preferably 130mm or more or 135mm or less, and still more preferably 132mm or more or 134mm or less.
The inner diameter of the cylindrical target 3 is preferably 127mm to 142mm, more preferably 132mm or more and 137mm or less, and still more preferably 134mm or more and 136mm or less.
The thickness of the cylindrical target 3 is preferably 5mm to 20mm, more preferably 6mm or more and 16mm or less, and still more preferably 8mm or more and 13mm or less.
From the viewpoint of further exhibiting the effects of the present invention, the axial length L of at least 1 of the cylindrical targets 3 is set to be longer3Preferably 750mm to 1500mm, more preferably 850mm or more or 1450mm or less, and still more preferably 950mm or more or 1450mm or less.
If the difference between the maximum value and the minimum value of the thickness of the bonding material 4 is 1.0mm or less, the thickness of the bonding material 4 is ensured to be uniform, and therefore, for example, the target can be prevented from being broken due to insufficient cooling at a portion where the thickness of the bonding material is thin, and the occurrence of cracks during sputtering can be suppressed.
From this viewpoint, the difference between the maximum value and the minimum value of the thickness of the bonding material 4 is more preferably 0.5mm or less, and still more preferably 0.3mm or less.
In this case, the thickness of the bonding material 4 is preferably 0.5mm or more, more preferably 0.7mm or more, and still more preferably 1mm or more.
The thickness of the joining material 4 can be measured by an ultrasonic flaw detector.
If the maximum value of the difference h between the heights of the outer peripheral surfaces 3a and 3a of the adjacent cylindrical targets 3 and 3, that is, the maximum value of the difference h between the heights of the outer peripheral surfaces 3a and 3a of the adjacent pair of cylindrical targets 3 and 3 in the axial direction is 0.5mm or less, it is possible to reduce the probability of occurrence of an abnormality during sputtering, specifically, the occurrence of an arc and the occurrence of chipping and cracking associated therewith. On the other hand, if the maximum value of the height difference h is larger than 0.5mm, the cylindrical target 3 on one side may have a protruding shape, and an adverse effect such as abnormal discharge may occur at the protruding edge portion.
From this viewpoint, the maximum value of the height difference h is more preferably 0.3mm or less, and still more preferably 0.2mm or less.
The height difference h can be measured using, for example, a depth gauge.
Further, if the difference between the maximum value and the minimum value of the axial distance (interval) d between the adjacent cylindrical targets 3, 3 is 0.2mm or less, it is possible to further reduce the probability of occurrence of chipping, cracking, or the like due to occurrence of an abnormality at the time of sputtering, for example, contact between the end portions due to thermal expansion at the time of sputtering. For example, in a portion where the axial distance d is large, the cylindrical base material 2 is exposed, and there is a possibility that a base material component is splashed and mixed as an impurity into the film. On the other hand, in a portion where the axial distance d is small, the adjacent cylindrical targets 3 and 3 collide with each other when thermally expanded by the heat of sputtering, and there is a possibility that the cylindrical target 3 is broken.
From this viewpoint, the difference between the maximum value and the minimum value of the axial distance d between the adjacent cylindrical targets 3, 3 is more preferably 0.15mm or less, and still more preferably 0.1mm or less.
The axial distance (interval) d can be measured using a feeler gauge or the like, for example.
< description of sentence >
In the present specification, unless otherwise specified, the expressions "a to B" (A, B is an arbitrary number) include the meaning of "a or more and B or less" and the meaning of "preferably more than a" or "preferably less than B".
In addition, when the expression "a or more" (a is an arbitrary number) or "B or less" (B is an arbitrary number), the meaning of "preferably more than a" or "preferably less than B" is also included.
Examples
The present invention will be further illustrated by the following examples. However, the following examples are not intended to limit the present invention.
< example 1 >
A cylindrical base material (length 3400mm, diameter 133mm, wall thickness 4mm) as a recovered product was placed on a pedestal supported to be rotatable axially, the base material was set to be horizontal and rotatable axially, a dial gauge fixed to hang from above was brought into contact with the outer surface of the central portion in the longitudinal direction of the cylindrical base material, the cylindrical base material was rotated once, the reading of the dial gauge was measured, and the maximum value H of the reading was measuredmaxAnd minimum value HminDifference (H)max-Hmin) The warpage amplitude X (initial) was measured.
Subsequently, the cylindrical base material was placed in an electric furnace, heated so that the surface temperature thereof was maintained at 230 ℃ for 1 hour, and the warpage width Y after heating (after heating) was measured in the same manner as described above.
Next, the longitudinal center portion of the cylindrical base material was pressed in a direction (-direction) opposite to the direction of warping (+ direction) using a press machine, and was processed so as to warp in the opposite direction (-direction) by a warp width α (═ Y × 1.0).
Next, using the cylindrical base material processed as described above, an ITO cylindrical sputtering target was produced as described below using the production apparatus 40 shown in fig. 7.
That is, 4 cylindrical split targets of ITO having an outer diameter of 153mm, an inner diameter of 133mm, and lengths of 300mm, 750mm, and 300mm were prepared, the outer peripheral surfaces of the cylindrical split targets were covered with a heat-resistant film and a tape, and In solder was primed on the bonding surfaces (inner peripheral surfaces) using an ultrasonic soldering iron.
On the other hand, In solder is also undercoated on the bonding surface (outer peripheral surface) of the cylindrical base material processed as described above using an ultrasonic soldering iron.
The cylindrical substrate was attached to the substrate holding portion 43c equipped with an O-ring 48 made of teflon (registered trademark).
Next, an O-ring 47 made of teflon (registered trademark) was attached to the target holding portion 43b, and 1 of the above-described cylindrical divided targets were attached to the target holding portion 43 b. At this time, the lower end of the cylindrical base material and the lower end of the cylindrical divided target were adjusted to be offset by 0.1mm by the lower holding member 43. Further, a gap 49 is formed between the cylindrical base material and the cylindrical divided target.
Further, the remaining cylindrical divided target material is deposited on the cylindrical divided target material. An O-ring 51 made of Teflon (registered trademark) having a thickness of 0.5mm was interposed between the cylindrical divided targets. The O-ring 50 is attached to the uppermost cylindrical divided target, the uppermost cylindrical divided target is attached to the target holding portion 44b, and the cylindrical target is pressed from above by the target holding portion 44 b. At this time, the positions of the 9 cylindrical divided targets were adjusted so that all the height differences between the cylindrical divided targets were 0.2mm or less. In this way, the upper end portion of the cylindrical target is held by the target holding member 44.
Next, the base material pressing portion 45b is pressed against the upper end portion of the cylindrical base material, and the upper end portion of the cylindrical base material is held by the base material holding member 45. At this time, the position of the jig was adjusted while measuring the distance between the surface of the cylindrical target and the surface of the cylindrical substrate with a depth gauge so that the offset between the upper end of the cylindrical substrate and the upper end of the cylindrical target became 0.1mm or less.
Finally, the lower holding member 43 is fixed to the titanium coupling member 46 by the fixing member 43d, the target holding member 44 is fixed to the titanium coupling member 46 by the fixing member 44c, and the substrate holding member 45 is fixed to the titanium coupling member 46 by the fixing member 45c, whereby the cylindrical substrate and the cylindrical target are firmly fixed to the manufacturing apparatus 40.
The manufacturing apparatus 40, the cylindrical substrate, and the cylindrical target were heated to 180 ℃.
Melted In solder of 175 deg.c, which is an amount sufficient for bonding the cylindrical target and the cylindrical base material, is injected into the void portion 49 from the upper side of the target holding member 44.
The molten solder poured into the manufacturing apparatus 40, the cylindrical base material, the cylindrical target material, and the void portion 49 is cooled.
After the solidification of the In solder was confirmed, the prepared ITO cylindrical sputtering target (sample) was removed from the manufacturing apparatus 40, the O-ring was removed, and the In solder remaining between the cylindrical divided target materials was scraped off.
In the ITO cylindrical sputtering target (sample) obtained as described above, the thickness of the bonding material was measured by an ultrasonic flaw detector (manufactured by Hitachi Power Solutions, Inc.: FS LINE) as described below. Specifically, the thickness of the bonding layer is calculated from the difference between the detection times of the reflected wave at the interface between the target and the bonding layer and the reflected wave at the interface between the bonding layer and the base material, and the propagation velocity of the ultrasonic wave in the bonding layer. In addition, a probe of 10MHz was used as the probe, and the propagation speed of the ultrasonic wave In the bonding layer (In metal) was set to 2700 m/s.
The thickness measurement positions of the bonding material were: each target segment is divided into 2 points separated from both ends of the target segment by 10mm inward in the axial direction and each point divided equally so that the value obtained by dividing equally between the 2 points becomes 50mm or less, and the following are set as follows: at each of the measurement points in the axial direction, 12 points (respective positions of 0 °, 30 °, 60 ° … …, and 330 °) are provided at intervals of 30 ° in the circumferential direction. For each target segment after bonding, the measurement was performed at the aforementioned position in 1 base material, and the difference between the maximum value and the minimum value was taken as the difference in thickness of the bonding material.
Further, all the height differences h between adjacent targets were measured by a depth gauge, and the maximum value of the height differences h was obtained.
Further, all axial distances d between adjacent targets were measured using a feeler gauge, and the difference between the maximum value and the minimum value thereof was determined.
All the height-to-height difference amounts h and the axial distances d between adjacent targets were measured at 12 points (positions of 0 °, 30 °, 60 ° … …, and 330 °) spaced at 30 ° intervals in the circumferential direction.
< example 2 >
An ITO cylindrical sputtering target (sample) was produced and each value was measured in the same manner as in example 1, except that the longest cylindrical target material in example 1 was changed to 850 mm.
< example 3 >
An ITO cylindrical sputtering target (sample) was produced and each value was measured in the same manner as in example 1, except that the longest cylindrical target material in example 1 was changed to 1100 mm.
< example 4 >
An ITO cylindrical sputtering target (sample) was produced in the same manner as in example 1 except that the longest cylindrical target material was changed to 1450mm in example 1, and the respective values were measured.
< example 5 >
In example 4, the heating of the cylindrical base material was changed to be not performed. That is, an ITO cylindrical sputtering target (sample) was produced and each value was measured in the same manner as in example 4 except that, instead of placing the cylindrical base material in an electric furnace and heating, and measuring the warpage width Y after heating, the longitudinal direction central portion of the cylindrical base material was processed by pressing the longitudinal direction central portion of the cylindrical base material in the direction (-direction) opposite to the warpage direction (+ direction) without heating to have only the warpage width α (═ X × 1.0) in the opposite direction (-direction).
< example 6 >
A cylindrical IGZO sputtering target (sample) was produced in the same manner as in example 3, except that the material of the cylindrical target material was changed to IGZO in example 3, and the respective values were measured.
< comparative example 1 >
A cylindrical sputtering target (sample) of ITO was produced and each value was measured in the same manner as in example 2, except that in example 2, the process for warping the cylindrical base material was changed to non-processing.
< comparative example 2 >
An ITO cylindrical sputtering target (sample) was produced and each value was measured in the same manner as in example 2, except that in the processing step of warping the cylindrical base material, the cylindrical base material was not warped to the opposite side of the original warped direction.
TABLE 1
By measuring the warpage width of the cylindrical base material to be used and pressing the cylindrical base material in the direction opposite to the original warped direction to perform processing so that the cylindrical base material is warped in the direction opposite to the warped direction, even if the axial length of the cylindrical target material is long, that is, even if the axial length of at least one cylindrical target material is 750mm or more, or even if the cylindrical base material is heated in advance by heating at the time of filling the bonding material, that is, at the time of filling the bonding material, or the cylindrical base material is heated by filling the bonding material melted by heating between the cylindrical base material and the target material, the influence of the warpage of the cylindrical base material can be eliminated, and as a result, it is known that: the difference between the maximum value and the minimum value of the thickness of the bonding material can be reduced, the difference in height between the outer peripheral surfaces of the adjacent cylindrical targets can be reduced, and the difference between the maximum value and the minimum value of the axial distance between the adjacent cylindrical targets can be reduced.
Description of the symbols
1 sputtering target
2 base Material
2a outer peripheral surface
3 target material
4 bonding material
5 dial gauge
40 manufacturing device
43 lower holding member
43b target holding part
43c base material holding part
43d fixing piece
44 target holding member
44b target holding part
44c fixing piece
45 base material holding member
45b substrate pressing part
45c fixing piece
46 connecting member
47O ring
48O ring
49 space part
50O ring
51O ring
Claims (10)
1. A method for manufacturing a sputtering target comprising a cylindrical base material and a cylindrical target material, the method comprising the steps of:
the warpage width of the cylindrical base material was measured (referred to as "measurement step"),
a process (referred to as a "processing step") of warping the cylindrical base material in a direction opposite to the warped direction is performed,
a plurality of cylindrical targets are arranged outside the processed cylindrical substrate at intervals in the axial direction, and the cylindrical substrate and the cylindrical targets are bonded by a bonding material.
2. The method of manufacturing a sputtering target according to claim 1, wherein in the machining step, a width of warping the cylindrical base material in a direction opposite to a direction of warping is determined based on the warping width measured in the measuring step.
3. The method of manufacturing a sputtering target according to claim 1 or 2, wherein in the processing step, when the warpage width X is measured in the measuring step, the cylindrical base material is warped in a direction opposite to the warped direction by a width of X0.10 to 2.00.
4. The method of manufacturing a sputtering target according to claim 1 or 2, wherein in the measuring step, after the cylindrical base material is heated, a warpage width of the heated cylindrical base material is measured,
in the processing step, when the warpage width Y is measured in the measuring step, the cylindrical base material is warped in a direction opposite to the warped direction by a width of Y x 0.50 to 1.50.
5. The method of manufacturing a sputtering target according to claim 4, wherein in the measuring step, the cylindrical base material is heated to 150 to 300 ℃, and then the warpage width Y of the heated cylindrical base material is measured.
6. The method of manufacturing a sputtering target according to any one of claims 1 to 5, wherein in the measuring step, a width of displacement of the outer peripheral surface of the cylindrical base material is measured as a width of warpage.
7. The method of manufacturing a sputtering target according to any one of claims 1 to 6, wherein at least one of the cylindrical target materials has an axial length of 750mm or more.
8. The method of manufacturing a sputtering target according to any one of claims 1 to 7, wherein the difference between the maximum value and the minimum value of the thickness of the bonding material of the manufactured sputtering target is 1.0mm or less, the maximum value of the height difference between the outer peripheral surfaces of the adjacent cylindrical target materials is 0.5mm or less, and the difference between the maximum value and the minimum value of the axial distance between the adjacent cylindrical target materials is 0.2mm or less.
9. A sputtering target comprising a cylindrical base material and a cylindrical target material, wherein the cylindrical base material and the cylindrical target material are bonded to each other with a bonding material,
at least one of the cylindrical targets has an axial length of 750mm or more, a difference between a maximum value and a minimum value of a thickness of the bonding material is 1.0mm or less, a maximum value of a height difference between outer peripheral surfaces of adjacent cylindrical targets is 0.5mm or less, and a difference between a maximum value and a minimum value of an axial distance between adjacent cylindrical targets is 0.2mm or less.
10. The sputtering target according to claim 9, wherein the length of the cylindrical base material is 2m or more.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2019210822 | 2019-11-21 | ||
| JP2019-210822 | 2019-11-21 | ||
| PCT/JP2020/024891 WO2021100233A1 (en) | 2019-11-21 | 2020-06-24 | Sputtering target and method for manufacturing same |
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| Publication Number | Publication Date |
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| CN114651086A true CN114651086A (en) | 2022-06-21 |
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| CN202080078115.6A Pending CN114651086A (en) | 2019-11-21 | 2020-06-24 | Sputtering target and method for producing same |
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| JP (1) | JP7139453B2 (en) |
| KR (1) | KR20220104150A (en) |
| CN (1) | CN114651086A (en) |
| TW (1) | TWI815025B (en) |
| WO (1) | WO2021100233A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116143547A (en) * | 2022-12-15 | 2023-05-23 | 先导薄膜材料（广东）有限公司 | Method for reducing warping of ITO planar target after sintering |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02122071A (en) * | 1988-10-28 | 1990-05-09 | Tanaka Kikinzoku Kogyo Kk | Manufacture of sputtering target |
| US20160211124A1 (en) * | 2013-09-12 | 2016-07-21 | Tanaka Kikinzoku Kogyo K.K. | Warp correction method for sputtering target with backing plate |
| CN106232860A (en) * | 2014-10-28 | 2016-12-14 | 三井金属矿业株式会社 | Cylinder-shaped ceramic sputtering target and manufacture device and manufacture method |
| CN108624850A (en) * | 2017-03-22 | 2018-10-09 | Ｊｘ金属株式会社 | Sputtering target and its manufacturing method |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3937085B2 (en) * | 1999-11-12 | 2007-06-27 | 株式会社高純度化学研究所 | Method for producing sputtering target assembly |
| JP5482020B2 (en) | 2008-09-25 | 2014-04-23 | 東ソー株式会社 | Cylindrical sputtering target and manufacturing method thereof |
-
2020
- 2020-06-24 CN CN202080078115.6A patent/CN114651086A/en active Pending
- 2020-06-24 KR KR1020227014428A patent/KR20220104150A/en unknown
- 2020-06-24 WO PCT/JP2020/024891 patent/WO2021100233A1/en active Application Filing
- 2020-06-24 JP JP2020560296A patent/JP7139453B2/en active Active
- 2020-07-17 TW TW109124278A patent/TWI815025B/en active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02122071A (en) * | 1988-10-28 | 1990-05-09 | Tanaka Kikinzoku Kogyo Kk | Manufacture of sputtering target |
| US20160211124A1 (en) * | 2013-09-12 | 2016-07-21 | Tanaka Kikinzoku Kogyo K.K. | Warp correction method for sputtering target with backing plate |
| CN106232860A (en) * | 2014-10-28 | 2016-12-14 | 三井金属矿业株式会社 | Cylinder-shaped ceramic sputtering target and manufacture device and manufacture method |
| CN108624850A (en) * | 2017-03-22 | 2018-10-09 | Ｊｘ金属株式会社 | Sputtering target and its manufacturing method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116143547A (en) * | 2022-12-15 | 2023-05-23 | 先导薄膜材料（广东）有限公司 | Method for reducing warping of ITO planar target after sintering |
| CN116143547B (en) * | 2022-12-15 | 2023-12-05 | 先导薄膜材料（广东）有限公司 | Method for reducing warping of ITO planar target after sintering |
Also Published As
| Publication number | Publication date |
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| TW202120721A (en) | 2021-06-01 |
| KR20220104150A (en) | 2022-07-26 |
| TWI815025B (en) | 2023-09-11 |
| JPWO2021100233A1 (en) | 2021-11-25 |
| JP7139453B2 (en) | 2022-09-20 |
| WO2021100233A1 (en) | 2021-05-27 |
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