WO2016067717A1 - 円筒形セラミックススパッタリングターゲットならびにその製造装置および製造方法 - Google Patents
円筒形セラミックススパッタリングターゲットならびにその製造装置および製造方法 Download PDFInfo
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- WO2016067717A1 WO2016067717A1 PCT/JP2015/073347 JP2015073347W WO2016067717A1 WO 2016067717 A1 WO2016067717 A1 WO 2016067717A1 JP 2015073347 W JP2015073347 W JP 2015073347W WO 2016067717 A1 WO2016067717 A1 WO 2016067717A1
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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
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- 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
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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
-
- 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
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- 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
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- 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
- H01J37/3426—Material
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- 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
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
- C04B2237/40—Metallic
- C04B2237/403—Refractory metals
Definitions
- the present invention relates to a cylindrical ceramic sputtering target capable of forming a uniform thin film up to the life end by sputtering, a manufacturing apparatus and a manufacturing method thereof.
- the magnetron type rotary cathode sputtering device has a magnetic field generator inside the cylindrical sputtering target, and performs sputtering while rotating the target while cooling from the inside of the target.
- the entire surface of the target material becomes erosion and becomes uniform. It is shaved by.
- the use efficiency of the target material is 20 to 30% in the flat plate type magnetron sputtering apparatus, whereas the magnetron type rotary cathode sputtering apparatus can realize a remarkably high use efficiency of 60% or more, thereby obtaining high productivity. It is done.
- the cylindrical sputtering target is usually formed by joining a cylindrical sputtering target material to a cylindrical substrate with solder.
- Such a rotating cathode sputtering method is widely used for metal targets that can be easily processed into a cylindrical shape and have high mechanical strength.
- the ceramic target material has low strength and is brittle, cracks and deformation are likely to occur during production. For this reason, in a ceramic target, although a short cylindrical target material could be manufactured, it was difficult to manufacture a long cylindrical target material with high performance.
- a plurality of short cylindrical target materials are arranged side by side in the axial direction in ceramic targets.
- Patent Document 1 describes a long cylindrical target material produced by stacking short cylindrical target materials, and the adjacent cylindrical target materials are divided at a divided portion between adjacent cylindrical target materials.
- a technique for suppressing the generation of arcing and particles due to the step is disclosed by setting the step of the outer peripheral surface of the sheet to 0.5 mm or less.
- the entire target material is not evenly cut, and erosion progresses locally at a certain site. To do.
- the base material may be exposed at a site that is locally eroded, and as a result, the base material is sputtered, so that a homogeneous sputtered film cannot be obtained.
- the target material could not be used until the original life end. Such local erosion can occur even when a single cylindrical target material is used.
- the ceramic target has a problem that high productivity, which is a feature of a manufacturing method using a cylindrical sputtering target, cannot be ensured.
- An object of the present invention is to provide a cylindrical ceramic sputtering target capable of forming a uniform thin film up to the life end by sputtering, a manufacturing apparatus and a manufacturing method thereof.
- the inventor found that local erosion occurred during sputtering, and the base material was exposed to a specific part before reaching the original life end.
- the inventors found that eccentricity is the main cause and completed the present invention.
- the present invention is a cylindrical ceramic sputtering target including a cylindrical base material, a cylindrical ceramic target material, and solder for joining the cylindrical base material and the cylindrical ceramic target material, the cylindrical ceramic target A dial gauge is applied to the outer surface of the target material at positions 7 mm inside from both ends of the cylindrical ceramic target material, and 15 mm from the both ends of the cylindrical ceramic target material on the outer peripheral surface of the cylindrical base material.
- the difference between the maximum value and the minimum value of the dial gauge reading was 1.
- the warpage of the cylindrical ceramic sputtering target is preferably 0.6 mm or less.
- the cylindrical ceramic target material may include at least two divided cylindrical ceramic target materials.
- the cylindrical ceramic sputtering target is applied with dial gauges at positions 7 mm inside from both ends of the ceramic target material, and on the outer peripheral surface of the cylindrical base material, the positions 15 mm outside from both ends of the cylindrical ceramic target material.
- the dial gauge reading is measured by rotating the dial one time, the difference between the maximum value and the minimum value of the dial gauge reading is preferably 1.0 mm or less at any measurement location.
- the cylindrical ceramic target material includes at least two divided cylindrical ceramic target materials
- the steps between the adjacent divided cylindrical ceramic target materials are all 0.3 mm or less. Preferably there is.
- a deviation between both ends of the cylindrical base material and the cylindrical ceramic target material is 0.5 mm or less.
- the cylindrical base material is preferably made of titanium or a titanium alloy, or made of molybdenum or a molybdenum alloy.
- the length of the cylindrical ceramic target material is preferably 500 mm or more.
- the relative density of the cylindrical ceramic target material is preferably 95% or more.
- the present invention also includes a lower holding member for holding a lower end portion of an upright cylindrical ceramic target material and a lower end portion of a cylindrical base material housed in a hollow portion of the cylindrical ceramic target material, A target material holding member for holding an upper end portion of the cylindrical ceramic target material; A base material holding member for holding the upper end portion of the cylindrical base material, and a connecting member made of titanium or titanium alloy, or made of molybdenum or molybdenum alloy for connecting the lower holding member, the target material holding member and the base material holding member
- An apparatus for manufacturing a cylindrical ceramic sputtering target comprising:
- the connecting member is composed of at least two columnar members.
- the present invention is a method for manufacturing a cylindrical ceramic sputtering target using the cylindrical ceramic sputtering target manufacturing apparatus,
- the lower holding member and the target material holding member hold the lower end portion and the upper end portion of the cylindrical ceramic target material, respectively, and the lower holding member and the base material holding member are accommodated in the hollow portion of the cylindrical ceramic target material.
- the manufacturing apparatus, the cylindrical ceramic target material and the cylindrical base material are heated to a temperature equal to or higher than the melting point of solder used for joining the cylindrical ceramic target material and the cylindrical base material, Injecting the melted solder into a gap formed between the cylindrical ceramic target material and the cylindrical base material, A manufacturing method of a cylindrical ceramic sputtering target, wherein the solder injected into the manufacturing apparatus, the cylindrical ceramic target material, the cylindrical base material, and the gap is cooled to a temperature lower than the melting point of the solder. .
- the cylindrical ceramic target material may be composed of at least two divided cylindrical ceramic target materials.
- the lower end portion of the cylindrical ceramic target material is formed by the lower holding member and the target material holding member.
- the upper end and the upper end are respectively held, it is preferable to adjust so that the step between the divided cylindrical ceramic target materials is 0.3 mm or less.
- the cylindrical ceramic sputtering target of the present invention can form a homogeneous thin film through the life end by sputtering.
- the cylindrical ceramic sputtering target manufacturing apparatus and manufacturing method of the present invention can preferably manufacture the cylindrical ceramic sputtering target.
- FIG. 1 is a schematic view showing a state in which the cylindrical target 1 is placed on the target rotating device 4 in the horizontal direction.
- FIG. 2 is a schematic view showing a state in which a cylindrical target 11 made of four divided target materials is placed on the target rotating device 4 in the horizontal direction.
- FIG. 3 is a schematic partial explanatory view of a cylindrical target having a cylindrical ceramic target material composed of two divided target materials.
- FIG. 4 is a view showing one end face of the cylindrical ceramic sputtering target 31.
- FIG. 5 is a longitudinal sectional view of a manufacturing apparatus 40 which is a specific example of the manufacturing apparatus of the cylindrical ceramic sputtering target of the present invention.
- FIG. 6 is a view showing one end face of a cylindrical ceramic sputtering target.
- FIG. 7 is a longitudinal sectional view of the ITO cylindrical sputtering target manufacturing apparatus 60.
- FIG. 8 is a photograph showing the state of erosion during sputtering of the ITO cylindrical sputtering target produced in Example 1.
- FIG. 9 is a photograph showing the state of erosion during sputtering of the ITO cylindrical sputtering target produced in Comparative Example 1.
- the cylindrical ceramic sputtering target of the present invention is a cylindrical ceramic sputtering target comprising a cylindrical base material, a cylindrical ceramic target material, and solder for joining the cylindrical base material and the cylindrical ceramic target material,
- a dial gauge is applied to the outer surface of the cylindrical ceramic target material at positions 7 mm inside from both ends of the cylindrical ceramic target material, and from both ends of the cylindrical ceramic target material on the outer peripheral surface of the cylindrical base material.
- the dial gauge reading was measured by rotating the cylindrical ceramic sputtering target once with the outer 15 mm position as a fulcrum, the difference between the maximum value and the minimum value of the dial gauge reading was 1.0 It is characterized by being not more than mm.
- cylindrical ceramic sputtering target of the present invention (hereinafter also referred to as a cylindrical target)
- a cylindrical base material is accommodated in a hollow portion of a cylindrical ceramic target material (hereinafter also referred to as a cylindrical target material). And the cylindrical target material are joined by solder.
- FIG. 1 is a schematic view showing a state where the cylindrical target 1 is placed on the target rotating device 4 in the horizontal direction.
- the cylindrical target 1 includes a cylindrical base material 2 and a cylindrical target material 3 joined to the cylindrical base material 2 with solder.
- the target rotating device 4 includes rotating tools 5a and 5b.
- the cylindrical target 1 is placed on the target rotating device 4 so that the rotating tools 5a and 5b are in contact with both ends of the cylindrical base material 2.
- the locations where the rotating tools 5a and 5b come into contact with the cylindrical base material 2 become the rotation fulcrums 7a and 7b.
- the fulcrums 7a and 7b are adjusted so as to be positioned 15 mm outside from the end faces 6a and 6b of the cylindrical target material 3, respectively.
- a dial gutter gauge (not shown) is applied to a position 7 mm inside from the end face 6 a on the outer surface of the cylindrical target material 3 indicated by an arrow Xa.
- the target rotating device 4 is driven to rotate the cylindrical target 1 once.
- the reading of the dial gauge is continuously measured, and the difference Da between the maximum value and the minimum value of the reading is calculated.
- a dial rod gauge (not shown) is applied to a position 7 mm inside from the end surface 6 b on the outer surface of the cylindrical target material 3 indicated by an arrow Xb.
- the target rotating device 4 is driven to rotate the cylindrical target 1 once.
- the dial gauge reading at this time is continuously measured, and the difference Db between the maximum value and the minimum value of the reading is calculated.
- the difference between the maximum value and the minimum value is 0 mm.
- the differences Da and Db between the maximum value and the minimum value obtained at the measurement points indicated by arrows Xa and Xb are both 1.0 mm or less.
- the difference between the maximum reading and the minimum reading of the dial gauge is also referred to as “eccentricity”.
- the eccentricity obtained at each measurement location is 1.0 mm or less, erosion progresses locally at a specific portion of the cylindrical target material during sputtering, and the original life Since the base material is not exposed to the part before reaching the end, and erosion progresses uniformly over the entire surface of the target material, a uniform film can be formed up to the original life end of the target material.
- at least one eccentricity obtained at each measurement location is larger than 1.0 mm, erosion progresses locally at a specific portion of the cylindrical target material during sputtering, and before reaching the original life end, The substrate is likely to be exposed at the site.
- the cylindrical target rotates around the axis of the cylindrical substrate during the sputtering, and if the eccentricity is larger than 1.0 mm, the outer peripheral surface of the cylindrical target material, which is the sputtering surface, is different for each part.
- the energy received by the sputter surface varies greatly from site to site, and this is presumably because the site receiving particularly large energy is preferentially eroded.
- the eccentricity between the cylindrical base material and the cylindrical target material occurs because the positions of the cylindrical base material and the cylindrical target material are eccentric when the cylindrical base material and the cylindrical target material are joined. This is because even if the adjustment is made so that there is no gap, the positional relationship between the two fluctuates in the process of heating and cooling during bonding.
- This invention implement achieves the cylindrical ceramic sputtering target whose said eccentricity is 1.0 mm or less by the manufacturing apparatus and manufacturing method of a cylindrical ceramic sputtering target mentioned later.
- the eccentricity obtained at each measurement point is preferably as small as possible, and any eccentricity is 1.0 mm or less, preferably 0.6 mm or less, and 0.4 mm or less. Is more preferable.
- the warp of the cylindrical target of the present invention is preferably 0.6 mm or less, more preferably 0.4 mm or less, and further preferably 0.2 mm or less. If the warpage of the cylindrical target is 0.6 mm or less, erosion progresses evenly over the entire surface of the target material during sputtering, and it is easy to form a homogeneous film up to the original life end of the target material.
- the warpage of the cylindrical target can be measured as follows.
- the cylindrical target 1 is left in a horizontal direction, for example, on the target rotating device 4 of FIG.
- a straight edge is applied to the outer surface along the length direction of the cylindrical target material 3, and the maximum length of the gap formed between the cylindrical target material 3 and the straight edge is measured using a gap gauge.
- the measurement is performed at a total of eight measurement points determined at intervals of 45 degrees in the circumferential direction with reference to the first measurement point, and the maximum value among the eight maximum lengths obtained is warped of the cylindrical target 1.
- warpage can be obtained by such a measurement method, for example, when the entire cylindrical target is warped in a beautiful arcuate shape, the cylindrical target is left still so that the convex side is directly below the vertical target, When the measurement is performed by applying a straight edge to the surface of the cylindrical target, the measured value by the gap gauge at the center in the length direction of the cylindrical target is warped.
- the cylindrical target material may include two or more divided cylindrical ceramic target materials (hereinafter also referred to as divided target materials).
- two or more cylindrical divided target materials are joined to the cylindrical base material with a certain gap therebetween.
- the cylindrical target of the present invention when the cylindrical target material consists of only one target material, as described above, the positional relationship between the cylindrical target material and the cylindrical base material at both ends of the cylindrical target material.
- the eccentricity obtained from the above the effect that a homogeneous film can be formed until the end of the life can be obtained, but when the cylindrical target material is composed of two or more divided target materials, each divided target It is important that the eccentricity at both ends of the material is in a certain numerical range. That is, a dial gauge is applied to the outer surface of each divided target material at a position 7 mm inside from both ends of the divided target material, and the outer peripheral surface of the cylindrical base material is respectively outward from both ends of the cylindrical ceramic target material.
- FIG. 2 is a schematic view showing a state in which a cylindrical target 11 having a cylindrical target material composed of four divided target materials is placed on the target rotating device 4 in the horizontal direction.
- the cylindrical target 11 includes a cylindrical base material 12 and a cylindrical target material 13 joined to the cylindrical base material 12 with solder.
- the cylindrical target material 13 is composed of divided target materials 13-1, 13-2, 13-3, and 13-4, and the divided target materials 13-1 to 13-4 are arranged in this order at regular intervals. Yes.
- the target rotating device 4 and the fulcrums 17a and 17b are the same as described in FIG.
- a dial pad gauge (not shown) is applied at a position 7 mm from the end face 16a on the outer surface of the divided target material 13-1 indicated by an arrow X1a.
- the target rotating device 4 is driven to rotate the cylindrical target 11 once.
- the dial gauge reading at this time is continuously measured, and the difference D1a between the maximum value and the minimum value of the reading is calculated.
- a dial gage gauge (not shown) is applied to a position 7 mm inside from the end face 16b on the outer surface of the divided target material 13-1 indicated by an arrow X1b.
- the target rotating device 4 is driven to rotate the cylindrical target 11 once.
- the dial gauge reading at this time is continuously measured, and a difference D1b between the maximum value and the minimum value of the reading is calculated.
- the above operations are performed at the measurement points indicated by, and the differences D2a, D2b, D3a, D3b, D4a and D4b are obtained.
- the dial gauge reading is constant while the cylindrical target 11 is rotated once, the difference between the maximum value and the minimum value is 0 mm.
- the differences D1a, D1b, D2a, D2b, D3a, D3b, D4a, and D4b are all 1.0 mm or less. The same applies to the eccentricity when the number of divided target materials is other than four.
- the eccentricity obtained at each measurement location is as small as possible, and any eccentricity is 1.0 mm or less and 0.6 mm or less. Preferably, it is 0.4 mm or less.
- FIG. 3 is a schematic partial explanatory view of a cylindrical target having a cylindrical target material composed of two divided target materials.
- the outer peripheral surface 22a of the cylindrical base member 22 in the direction perpendicular to the axis Z of the cylindrical base member 22 A point X where the distance is maximum is determined.
- the distance from the outer peripheral surface 22a of the point X in the direction D perpendicular to the axis Z including the point X is L X.
- a point Y in the direction D on the outer periphery of the end surface 23b facing the end surface 23a including the point X is obtained.
- the distance from the outer peripheral surface 22a in the direction D at the point Y is defined as L Y.
- the difference L X -L Y of L X and L Y is the step between the divided target material.
- the cylindrical target material is composed of N divided target materials
- all the N ⁇ 1 steps are 0.3 mm or less.
- the step is more preferably 0.2 mm or less, and most preferably 0 mm.
- At least one of the steps of the cylindrical target is larger than 0.3 mm, as in the case of the eccentricity, energy concentrates on a specific part of the target material during sputtering, and abnormal discharge occurs in the part, Erosion can progress.
- the base material such as solder used for the bonding material is sputtered. End up.
- the deviation between both ends of the cylindrical base material and the cylindrical target material is 0.5 mm or less.
- the deviations at both ends of the cylindrical base material and the cylindrical target material are the center point with respect to the outer peripheral line of the cylindrical target material and the center point with respect to the outer peripheral line of the cylindrical base material at both end surfaces of the cylindrical target.
- FIG. 4 is a view showing one end face of the cylindrical target 31.
- the cylindrical target 31 includes a cylindrical base material 32, a cylindrical target material 33, and solder 34 that joins the cylindrical base material 32 and the cylindrical target material 33.
- the distance between the center point 32b with respect to the outer peripheral line 32a of the cylindrical base material 32 and the center point 33b with respect to the outer peripheral line 33a of the cylindrical target material 33 is L A.
- the distance between the center point with respect to the outer peripheral line of the cylindrical base material 32 and the center point with respect to the outer peripheral line of the cylindrical target material 33 is L B.
- Deviations at both ends of the cylindrical base material and the cylindrical target material are obtained by determining the center point with respect to the outer peripheral line of the cylindrical target material and the center point with respect to the outer peripheral line of the cylindrical base material at the end face, and measuring the distance. It can also be obtained by the method shown in the embodiment.
- both the deviations L A and L B are 0.5 mm or less.
- the deviation is preferably as small as possible, more preferably 0.3 mm or less, still more preferably 0.1 mm or less, and most preferably 0 mm.
- the length of the cylindrical target material is not particularly limited as long as the eccentricity can be evaluated, and is generally 500 to 4000 mm.
- the cylindrical target material is composed of a plurality of divided target materials, the sum of the total length of the divided target materials and the total length of the gaps between the divided target materials is the length of the cylindrical target material.
- the cylindrical base material and the cylindrical target material are joined by solder containing metal indium or the like as a component, when the cylindrical target material is composed of a divided cylindrical target material, the number of the divided cylindrical target materials is determined. If it is used too much, it may cause eccentricity or steps. For this reason, the number of divided target materials to be bonded to one cylindrical base material is preferably 10 or less, more preferably 7 or less, and even more preferably 3 or less.
- the length of the divided target material is preferably 300 mm or more, more preferably 450 mm or more, still more preferably 600 mm or more, and particularly preferably 850 mm or more.
- the lengths of the divided target materials do not have to be the same as each other, and divided target materials having different lengths may be used in combination.
- one or two divided target materials shorter than 300 mm may be used in combination with a long divided target material.
- the gap between the divided target materials is usually 0.1 to 0.5 mm.
- the outer diameter of the cylindrical target material is usually 145 to 177 mm, and the inner diameter is usually 134 to 136 mm.
- indium oxide-tin oxide material ITO
- aluminum oxide-zinc oxide material AZO
- indium oxide-gallium oxide-zinc oxide examples thereof include system materials (IGZO).
- the relative density of the cylindrical target material is preferably 95% or more, more preferably 99% or more, and further preferably 99.5% or more. As the relative density of the target material is higher, the target material can be prevented from cracking due to thermal shock or temperature difference during sputtering, and the target material thickness can be effectively utilized without waste. In addition, generation of particles and arcing is reduced, and good film quality can be obtained.
- the upper limit of the relative density is not particularly limited, but is usually 100%.
- the cylindrical base material is longer than the cylindrical target material, has a size capable of joining the cylindrical target material, and is capable of evaluating the eccentricity.
- the length is not particularly limited.
- the material of the cylindrical base material is preferably titanium or a titanium alloy, or molybdenum or a molybdenum alloy in terms of a thermal expansion coefficient close to that of the ceramic used for the target material.
- the titanium alloy is an alloy containing titanium as a main component, and generally refers to an alloy having a titanium content of 90 to 99% by mass. ASTM standard Gr. 5, Gr. 7, Gr. 9, Gr. 11, Gr. 12 is known.
- Molybdenum alloy is an alloy containing molybdenum as a main component, and usually refers to an alloy having a molybdenum content of 50 to 99.95% by mass, such as TZM, HMC, Mo—W, Mo—Re, and Mo—La. Are known.
- TZM molybdenum content of 50 to 99.95% by mass
- HMC molybdenum content of 50 to 99.95% by mass
- Mo—W molybdenum content of 50 to 99.95% by mass
- Mo—W molybdenum content of 50 to 99.95% by mass
- the type of the solder is not particularly limited, and can be appropriately selected from conventionally used solders according to the target material, and examples thereof include indium solder.
- the cylindrical ceramic sputtering target can be manufactured by the following cylindrical ceramic sputtering target manufacturing apparatus and manufacturing method.
- the cylindrical ceramic sputtering target manufacturing apparatus (hereinafter also referred to as a cylindrical target manufacturing apparatus) A lower holding member for holding a lower end portion of a cylindrical ceramic target material that is upright and a lower end portion of a cylindrical base material that is accommodated in a hollow portion of the cylindrical ceramic target material; A target material holding member for holding an upper end portion of the cylindrical ceramic target material; A base material holding member for holding the upper end portion of the cylindrical base material, and a connecting member made of titanium or titanium alloy, or made of molybdenum or molybdenum alloy for connecting the lower holding member, the target material holding member and the base material holding member And have.
- the manufacturing method of the cylindrical ceramic sputtering target (hereinafter also referred to as the manufacturing method of the cylindrical target) is: A method for manufacturing a cylindrical ceramic sputtering target using the cylindrical ceramic sputtering target manufacturing apparatus, The lower end portion and the upper end portion of the cylindrical ceramic target material are respectively held by the holding member and the target material holding member, and are made of titanium accommodated in the hollow portion of the cylindrical ceramic target material by the holding member and the base material holding member.
- the lower end and the upper end of the cylindrical base material made of titanium alloy, or molybdenum or molybdenum alloy are respectively held,
- the manufacturing apparatus, the cylindrical ceramic target material and the cylindrical base material are heated to a temperature equal to or higher than the melting point of the solder used for joining the cylindrical ceramic target material and the cylindrical base material, and the cylindrical ceramic target material And injecting the melted solder into a gap formed between the cylindrical base material and The solder injected into the manufacturing apparatus, the cylindrical ceramic target material, the cylindrical base material, and the gap is cooled to a temperature lower than the melting point of the solder.
- the manufacturing apparatus of the cylindrical target of this invention is not restrict
- FIG. 5 is a longitudinal sectional view of a manufacturing apparatus 40, which is a specific example of the cylindrical target manufacturing apparatus.
- FIG. 5 shows the manufacturing apparatus 40 with the cylindrical base material 41 and the cylindrical target material 42 attached to the manufacturing apparatus 40.
- the cylindrical target material 42 is formed by three cylindrical divided target materials 42a.
- the manufacturing apparatus 40 includes a lower holding member 43, a target material holding member 44, a base material holding member 45, and a connecting member 46.
- the lower holding member 43 has a connecting member mounting portion 43a having four mounting holes 43e for mounting the connecting member 46, a target material holding portion 43b for holding the divided target material 42a in an upright state, and a cylindrical base material 41 standing upright. It is comprised from the base-material holding
- the connecting member mounting portion 43a, the target material holding portion 43b, and the base material holding portion 43c are ring-shaped and are integrally formed in this order from the outside, and are made of, for example, titanium.
- the cylindrical target material 42 is inserted into the target material holding portion 43b, and a state in which an O-ring 47 made of, for example, Teflon (registered trademark) is interposed between the lower end surface of the cylindrical target material 42 and the target material holding portion 43b. And attached to the target material holding portion 43b.
- the cylindrical base material 41 is accommodated in a hollow portion of the cylindrical target material 42, and an O-ring 48 made of, for example, Teflon (registered trademark) is interposed between the lower end surface of the cylindrical base material 41 and the base material holding portion 43c. In this state, it is attached to the base material holding part 43c.
- the lower holding member 43 holds the lower ends of the cylindrical target material 42 and the cylindrical base material 41.
- the cylindrical target material 42 and the cylindrical base material 41 are held by the lower holding member 43 in this way, whereby a gap 49 is formed between the cylindrical target material 42 and the cylindrical base material 41. .
- the connecting member 46 includes four columnar members 46a.
- FIG. 5 shows only two columnar members 46a out of the four.
- the four columnar members 46a are inserted into mounting holes 43e provided in the lower holding member 43, and are fixed to the lower holding member 43 by a fixture 43d such as a nut.
- a target material holding member 44 and a base material holding member 45 are mounted on the four columnar members 46a.
- the connecting member 46 connects the lower holding member 43, the target material holding member 44, and the base material holding member 45.
- the number of columnar members 46a may be two, three, or five or more. When the number of the columnar members 46a is larger, the lower holding member 43, the target material holding member 44, and the base material holding member 45 can be connected more firmly, and the manufacturing apparatus 40 is stabilized.
- the material of the connecting member 46 is selected according to the material of the cylindrical base material.
- the cylindrical target manufacturing apparatus of the present invention is used for a cylindrical base material made of titanium or titanium alloy, or molybdenum or molybdenum alloy.
- the connecting member 46 is also made of titanium or a titanium alloy.
- the connecting member 46 is also made of molybdenum or a molybdenum alloy.
- the titanium alloy and the molybdenum alloy are the same as those described above for the cylindrical base material. The significance of the connecting member 46 being made of titanium or titanium alloy, or molybdenum or molybdenum alloy will be described later.
- the target material holding member 44 includes a connecting member mounting portion 44a, a target material holding portion 44b, and a fixture 44c.
- the connecting member mounting portion 44a and the target material holding portion 44b are ring-shaped and are integrally formed in this order from the outside, and are made of, for example, titanium.
- the connecting member mounting portion 44a has four mounting holes 44d.
- a columnar member 46a is inserted into each mounting hole 44d, and is fixed to the connecting member 46 by a fixing tool 44c such as a nut. The position of the target material holding member 44 can be freely adjusted along the connecting member 46.
- the cylindrical target material 42 is inserted into the target material holding portion 44b, and a state where, for example, an O-ring 50 made of Teflon (registered trademark) is interposed between the upper end surface of the cylindrical target material 42 and the target material holding portion 44b. And attached to the target material holding portion 44b. That is, the target material holding part 44b holds the cylindrical target material 42 so as to be pressed from above. In this way, the target material holding member 44 holds the upper end portion of the cylindrical target material 42.
- the base material holding member 45 includes a connecting member mounting portion 45a, a base material pressing portion 45b, and a fixture 45c.
- the connecting member mounting portion 45a has four mounting holes 45d.
- a columnar member 46a is inserted into each mounting hole 45d, and the base material holding member 45 is fixed to the connecting member 46 by a fixture 45c such as a nut.
- the position of the substrate holding member 45 can be freely adjusted along the connecting member 46.
- the base material pressing portion 45b is provided on the lower side of the connecting member mounting portion 45a and has a disk shape, and holds the upper end portion of the cylindrical base material 41 so as to press the upper end surface of the cylindrical base material 41 from above.
- the substrate holding member only needs to be able to be fixed without shifting the position of the cylindrical substrate. Good.
- the cylindrical target of the present invention can be manufactured using the manufacturing apparatus 40 by a manufacturing method including the following assembly process, heating process, solder injection process, and cooling process, for example.
- Assembly process As shown in FIG. 5, a cylindrical base material 41 and a cylindrical target material 42 are attached to the manufacturing apparatus 40.
- the cylindrical base material 41 made of titanium or titanium alloy, or molybdenum or molybdenum alloy is installed in the manufacturing apparatus 40.
- the titanium alloy and the molybdenum alloy are the same as those described above for the cylindrical base material.
- the cylindrical base material 41 is attached to the base material holding portion 43c of the lower holding member 43 on which an O-ring 48 made of, for example, Teflon (registered trademark) is attached.
- an O-ring 48 made of, for example, Teflon (registered trademark) is attached.
- the cylindrical base material 41 is warped, it is reflected in the eccentricity or warpage of the manufactured cylindrical target. Therefore, check the warpage of the cylindrical base material 41 before attaching it to the manufacturing apparatus 40. Is preferred. Although there is no restriction
- the cylindrical base material is left in the horizontal direction on the target rotating device 4 of FIG. A straight edge is placed on the cylindrical substrate, and the maximum length of the gap formed between the cylindrical substrate and the straight edge is measured using a gap gauge.
- the measurement is performed at a total of eight measurement points determined at intervals of 45 degrees in the circumferential direction, and the maximum value among the eight maximum lengths obtained is the warp of the cylindrical base material. It can be. Further, the warp may be obtained using a three-dimensional shape measuring machine.
- the warp of the cylindrical base material 41 is preferably 0.6 mm or less, more preferably 0.4 mm or less, still more preferably 0.2 mm or less, and most preferably 0 mm.
- a step of correcting the warpage of the cylindrical base material 41 may be included.
- limiting in particular in the correction method of the curvature of the said cylindrical base material 41 For example, there exists a method of correcting a curvature using a press machine.
- a cylindrical target material 42 is attached to the outside of the cylindrical base material 41.
- an O-ring 47 made of, for example, Teflon (registered trademark) is attached to the target material holding portion 43b of the lower holding member 43, and the divided target material 42a is attached to the target material holding portion 43b.
- the target material holding portion 43b and the base material holding portion 43c have a bottom surface and a side surface that are vertical, and the outer diameter of the cylindrical base material 41, the inner diameter of the base material holding portion 43c, the outer diameter of the divided target material 42a, and the target The inner diameter of the material holding portion 43b is almost the same size.
- the lower holding member 43 erects the cylindrical base material 41 and the split target material 42a, and creates a gap 49 between the cylindrical base material 41 and the split target material 42a. It also plays the role of a jig such that the deviation of the lower end from the material 42a is 0.5 mm or less.
- the other two divided target materials 42a are stacked on the divided target material 42a attached to the target material holding portion 43b.
- the step between the divided target materials 42a to be stacked is adjusted.
- an O-ring 51 made of Teflon (registered trademark) is interposed between the divided target materials 42a.
- An O-ring 50 made of, for example, Teflon (registered trademark) is mounted on the divided target material 42 a placed on the top, and the upper divided target material 42 a is used as the target material holding portion 44 b of the target material holding member 44.
- the cylindrical target material 42 is pressed from the upper side by the attachment and target material holding portion 44b.
- the positions of the three divided target materials 42a are adjusted so that the eccentricity between the divided target material 42a and the cylindrical base material 41 is reduced, for example, the eccentricity in the cylindrical target is 1.0 mm or less. To do. Moreover, it should be, for example, 0.3 mm or less so that the level difference between the divided target materials 42a is reduced. Thus, the upper end portion of the cylindrical target material 42 is held by the target material holding member 44.
- the base material pressing portion 45 b of the base material holding member 45 is pressed against the upper end surface of the cylindrical base material 41.
- the base material pressing portion 45 b of the base material holding member 45 is pressed against the upper end surface of the cylindrical base material 41.
- it should be adjusted to 0 mm.
- the upper end portion of the cylindrical base material 41 is held by the base material holding member 45.
- the upper end portion thereof is designed to protrude from the upper opening of the cylindrical target material 42.
- the cylindrical base material 44 and the cylindrical target material 42 are firmly fixed to the manufacturing apparatus 40 by fixing the target material holding member 44 to the connecting member 46 with the fixing tool 44C and the base material holding member 45 with the fixing tool 45C.
- the manufacturing apparatus 40 that is, the lower holding member 43, the target material holding member 44, the base material holding member 45 and the connecting member 46, and the cylindrical base material 41 and the cylindrical target material 42 attached to the manufacturing apparatus 40 are connected to the cylindrical target. Heating is performed to a temperature equal to or higher than the melting point of the solder used for joining the material 42 and the cylindrical base material 41. For example, when indium solder is used as the solder, it is heated to 160 to 250 ° C.
- the injection amount is an amount sufficient for joining the cylindrical target material 42 and the cylindrical base material 41.
- the molten solder injected into the manufacturing apparatus 40, the cylindrical base material 41, the cylindrical target material 42, and the gap portion 49 is cooled to a temperature lower than the melting point of the solder. For example, when indium solder is used as the solder, it is cooled to 150 ° C. or lower.
- the cylindrical base material 41 and the cylindrical target material 42 are joined by solder, and a cylindrical target is manufactured.
- the manufactured cylindrical target is removed from the manufacturing apparatus 40, and the O-ring 51 is also removed.
- the portion where the O-ring 51 was interposed becomes a gap between the divided target materials.
- the cylindrical base material 41 and the cylindrical target material 42 are firmly fixed to the manufacturing apparatus 40, so that the relative positions of the cylindrical base material 41 and the cylindrical target material 42 that can occur at the time of joining are obtained. Deviation can be suppressed within a certain range.
- the connecting member has a thermal expansion coefficient that is significantly different from that of the cylindrical base material or the cylindrical target material
- the degree of expansion in the heating process and the degree of shrinkage in the cooling process are Since it differs greatly depending on the base material and the cylindrical target material, particularly when the cylindrical base material and the cylindrical target material are firmly fixed to the manufacturing apparatus, a large stress is generated in the cylindrical base material in the cooling process.
- a relatively large positional deviation between the cylindrical base material and the cylindrical target material occurs, and even if the eccentricity and the deviation between the cylindrical base material and the cylindrical target material are adjusted in the assembly process, In the manufactured cylindrical target, the eccentricity between the cylindrical base material and the cylindrical target material cannot be 1.0 mm or less, and the deviation cannot be 0.5 mm or less.
- the divided cylindrical target is divided.
- the step between the target materials cannot be maintained at 0.3 mm or less.
- the manufactured cylindrical target may be cracked or warped.
- the connecting member is made of SUS
- the cylindrical base material made of titanium or titanium alloy, or molybdenum or molybdenum alloy, and the cylindrical target material made of ceramics and the connecting member have a large coefficient of thermal expansion.
- the eccentricity between the cylindrical base material and the cylindrical target material cannot be 1.0 mm or less, and the deviation cannot be 0.5 mm or less, and the step between the divided target materials is 0. It is also impossible to make it 3 mm or less.
- the connecting member 46 is made of titanium or a titanium alloy, or made of molybdenum or a molybdenum alloy.
- the cylindrical base material 41 used in the manufacturing method is also made of titanium or a titanium alloy, or molybdenum or a molybdenum alloy.
- the connecting member 46 is made of titanium or titanium alloy when the cylindrical base material 41 is made of titanium or a titanium alloy, and made of molybdenum when the cylindrical base material 41 is made of molybdenum or a molybdenum alloy. Or made of molybdenum alloy. Therefore, the thermal expansion coefficient of the connecting member 46 is equal to or close to the thermal expansion coefficient of the cylindrical base material 41.
- the thermal expansion coefficient of ceramics approximates the thermal expansion coefficient of titanium or titanium alloy, or molybdenum or molybdenum alloy
- the thermal expansion coefficient of the cylindrical target material 42 is equal to the thermal expansion coefficient of the connecting member 46 and the cylindrical base material 41. Approximate.
- the degree of expansion in the heating process and the degree of contraction in the cooling process are greatly different in the connecting member 46, the cylindrical base material 41, and the cylindrical target material 42. Therefore, even when the cylindrical base material and the cylindrical target material are firmly fixed to the manufacturing apparatus, no great stress is generated on the cylindrical base material in the cooling process. As a result, the relative displacement between the cylindrical base material 41 and the cylindrical target material 42 does not occur, and adjustment is performed so that the eccentricity and the deviation between the cylindrical base material 41 and the cylindrical target material 42 are reduced in the assembly process. If it is made, eccentricity and deviation are reduced even in the manufactured cylindrical target. Therefore, by appropriately adjusting the positional relationship between the cylindrical base material 41 and the cylindrical target material 42 in the assembly process, the eccentricity is 1.0 mm or less and the deviation is 0.5 mm or less. You can get a target.
- the manufactured cylindrical target can be reduced to 0.3 mm or less. Furthermore, it is possible to prevent the manufactured cylindrical target from being cracked or warped.
- a dial gauge was applied to a position 7 mm inside from one end on the outer surface, and the target rotating device 4 was driven to rotate the cylindrical target once. The reading of the dial gauge at this time was continuously measured, and the eccentricity, which is the difference between the maximum value and the minimum value of the reading, was calculated. Similarly, a dial gauge was applied to a position 7 mm inside from the other end of the divided target material, the target rotating device 4 was driven, the cylindrical target 1 was rotated once, and the eccentricity was similarly calculated. The same operation was performed on all the divided target materials, and the eccentricity at each end portion was calculated. (Measurement of deviation between cylindrical base material and cylindrical target material) The deviation between the cylindrical base material and the cylindrical target material was measured as follows.
- the ITO cylindrical sputtering target is allowed to stand on a surface plate, and as shown in FIG. 6, the maximum length of line segments connecting two points on the outer peripheral line (circle) of the cylindrical target material at one end face.
- the line segment L having (the diameter of the circle) the lengths of the two laminated portions of the cylindrical target material and the solder layer (the length between AB and the length between CD shown in FIG. 6) are depth gauges.
- the difference d between the two measured values ((length between CDs) ⁇ (length between ABs) in FIG. 6) was obtained.
- a value X obtained by dividing the difference d obtained in the line segment L giving the maximum difference d by 2 was obtained.
- FIG. 6 is a view similar to FIG. (Measurement of level difference between split target materials)
- the level difference between adjacent divided target materials the height difference between the adjacent end faces of these divided target materials is measured at eight points equally spaced in the circumferential direction with a depth gauge, and the maximum value of the difference is defined as the level difference. did. (Measurement of warpage of cylindrical sputtering target)
- the ITO cylindrical sputtering target was left in the horizontal direction on the target rotating device 4 of FIG.
- a straight edge was applied to the outer peripheral surface of the cylindrical target material joined to the cylindrical base material, and a gap formed between the cylindrical target material and the straight edge was measured using a gap gauge.
- the above-mentioned measurement was performed at eight positions that are equally spaced in the circumferential direction, and the maximum value of the gap was defined as the warpage of the ITO cylindrical sputtering target.
- the cylindrical target material of the ITO cylindrical sputtering target was visually observed, and the number of divided target materials in which cracks occurred among the nine divided target materials was measured.
- evaluation of erosion during sputtering Sputtering was performed using the manufactured ITO cylindrical sputtering target under the following conditions. The state of erosion of the cylindrical target material after sputtering was observed visually.
- ⁇ Sputtering conditions Substrate temperature 100 ° C Sputtering pressure 0.2Pa Power 20KW Target speed 10rpm (Measurement of the number of split target materials that have cracked by sputtering) After the sputtering, the cylindrical target material of the ITO cylindrical sputtering target was visually observed, and the number of divided target materials in which cracks occurred among the nine divided target materials was measured. [Example 1]
- the ITO cylindrical sputtering target was manufactured as follows using the manufacturing apparatus 40 shown in FIG.
- solder was also undercoated with an ultrasonic soldering iron on the joint surface (outer peripheral surface) of a titanium cylindrical substrate having an outer diameter of 133.0 mm, an inner diameter of 125.0 mm, and a length of 3000.0 mm.
- the cylindrical base material was attached to a base material holding part 43c on which a Teflon (registered trademark) O-ring 48 was mounted.
- a Teflon (registered trademark) O-ring 47 was attached to the target material holding portion 43b, and one cylindrical divided target material was attached to the target material holding portion 43b.
- the lower holding member 43 was adjusted so that the deviation between the lower end portion of the cylindrical base material and the lower end portion of the cylindrical divided target material was 0.1 mm.
- a gap portion 49 was formed between the cylindrical base material and the cylindrical divided target material.
- the remaining eight cylindrical divided target materials were stacked on the cylindrical divided target material.
- a 0.5 mm thick Teflon (registered trademark) O-ring 51 was interposed between the cylindrical divided target materials.
- the O-ring 50 is mounted on the cylindrical divided target material placed on the top, the uppermost cylindrical divided target material is attached to the target material holding portion 44b, and the cylindrical target material is formed by the target material holding portion 44b.
- the positions of the nine cylindrical divided target materials were adjusted so that all the steps between the cylindrical divided target materials were 0.2 mm or less.
- the upper end part of the cylindrical target material was held by the target material holding member 44.
- the base material pressing portion 45 b was pressed against the upper end portion of the cylindrical base material, and the upper end portion of the cylindrical base material was held by the base material holding member 45. At this time, while measuring the distance between the surface of the cylindrical target material and the surface of the cylindrical base material with a depth gauge so that the deviation between the upper end of the cylindrical base material and the upper end of the cylindrical target material is 0.1 mm or less, The position was adjusted.
- the lower holding member 43 is fixed to the titanium connecting member 46 by the fixing tool 43d, the target material holding member 44 by the fixing tool 44c, and the base material holding member 45 by the fixing tool 45c.
- the cylindrical target material was firmly fixed to the manufacturing apparatus 40.
- the manufacturing apparatus 40, the cylindrical base material, and the cylindrical target material were heated to 180 ° C.
- the melted solder injected into the manufacturing apparatus 40, the cylindrical base material, the cylindrical target material, and the gap 49 was cooled to 140 ° C.
- the manufactured ITO cylindrical sputtering target 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.
- Table 1 shows the results of the measurement of the eccentricity, the measurement of the deviation, the measurement of the step, the measurement of the warpage, and the measurement of the number of the divided target materials in which cracking occurred, which was performed on the manufactured ITO cylindrical sputtering target.
- a photograph showing the state of erosion at the end of sputtering is shown in FIG. As can be seen from FIG. 8, in the cylindrical target of Example 1, the substrate was not exposed due to local erosion of the cylindrical target material.
- the eccentricity shown in Table 1 is the maximum value among all the eccentricities calculated at each measurement location.
- Example 2 An ITO cylindrical sputtering target was manufactured by the same operation as in Example 1 except that the manufacturing apparatus 40 in which the connecting member 46 was made of a titanium alloy (Ti-6AL-4V ASTM standard Gr. 5) was used.
- Table 1 shows the results of the measurement of the eccentricity, the measurement of the deviation, the measurement of the step, the measurement of the warpage, and the measurement of the number of the divided target materials in which cracks occurred, which were performed on the manufactured ITO cylindrical sputtering target.
- the erosion state at the end of sputtering was the same as the photograph shown in FIG. [Example 3]
- An ITO cylindrical sputtering target was manufactured by the same operation as in Example 1 except that the cylindrical base material was made of molybdenum and the manufacturing apparatus 40 in which the connecting member 46 was made of molybdenum was used.
- Table 1 shows the results of the measurement of the eccentricity, the measurement of the deviation, the measurement of the step, the measurement of the warpage, and the measurement of the number of the divided target materials in which cracks occurred, which were performed on the manufactured ITO cylindrical sputtering target.
- the erosion state at the end of sputtering was the same as the photograph shown in FIG.
- An ITO cylindrical sputtering target was manufactured in the same manner as in Example 1 except that a manufacturing apparatus different from the manufacturing apparatus 40 was used only in that the connecting member was made of SUS304.
- Table 1 shows the results of the measurement of the eccentricity, the measurement of the deviation, the measurement of the step, the measurement of the warpage, and the measurement of the number of the divided target materials in which cracking occurred after the sputtering performed on the manufactured ITO cylindrical sputtering target.
- a photograph showing the state of erosion at the end of sputtering is shown in FIG. 9 is a portion where the cylindrical base material under the cylindrical target material is exposed by sputtering. That is, in the cylindrical target of Comparative Example 1, the cylindrical target material was not sputtered uniformly, and local erosion occurred in the cylindrical target material.
- An ITO cylindrical sputtering target was manufactured using the manufacturing apparatus 60 shown in FIG.
- the manufacturing apparatus 60 is different from the manufacturing apparatus 40 in that the connecting member is made of SUS304, the base material holding member 45 is not provided, and the four cylindrical target material pressing members 62 are provided.
- One cylindrical target material pressing member 62 is provided for each of the four columnar members 46a.
- the cylindrical target material pressing member 62 includes a coupling portion 62a that is coupled to the columnar member 46a and a pressing portion 62b that presses the cylindrical target material.
- the holding portion 62b is rod-shaped and has a function of holding down the cylindrical target material from the side face across all the divided portions between the cylindrical divided target materials and suppressing the movement of the cylindrical target material in the side face direction.
- An ITO cylindrical sputtering target was manufactured by the same operation as in Example 1 except that the cylindrical base material was not held by the base material holding member 45 and the cylindrical target material was pressed by the cylindrical target material pressing member 62. .
- Table 1 shows the results of the measurement of the eccentricity, the measurement of the deviation, the measurement of the step, the measurement of the warpage, and the measurement of the number of the divided target materials in which cracking occurred, which was performed on the manufactured ITO cylindrical sputtering target.
- the erosion state at the end of sputtering was the same result as the photograph shown in FIG.
- the ITO cylinders obtained in Examples 1 to 3 were used in spite of all the positional relationships of the respective divided cylindrical target materials and cylindrical base materials being adjusted in the same manner during the production of the cylindrical target.
- the type sputtering target has eccentricity, a deviation between the cylindrical base material and the cylindrical target material, and a step between the divided target materials is smaller than the ITO cylindrical sputtering target obtained in Comparative Examples 1 and 2, and the ITO cylindrical sputtering target.
- the warpage of the target was also smaller than that of the ITO cylindrical sputtering target obtained in Comparative Example 1.
- the number of cracks generated in the divided cylindrical target material after sputtering was smaller than that of the ITO cylindrical sputtering target obtained in Comparative Example 1.
- Example 2 This is the same material as the cylindrical base material in Example 1, and the cylindrical target was manufactured using a manufacturing apparatus having a connecting member made of titanium having a thermal expansion coefficient close to that of the ceramic target material.
- the cylindrical target was manufactured using a manufacturing apparatus having a connecting member made of a titanium alloy that is similar to the cylindrical base material and has a thermal expansion coefficient close to that of the ceramic target material.
- Cylindrical target material produced during manufacture by manufacturing a cylindrical target using a manufacturing apparatus having a molybdenum-made connecting member that is the same material as the cylindrical base material and has a thermal expansion coefficient close to that of the ceramic target material, The degree of thermal expansion and contraction of the cylindrical base material and connecting member is approximated, reducing the stress on the cylindrical base material and the cylindrical target material. It is considered to the be due.
- the cylindrical target was manufactured using a manufacturing apparatus having a connection member made of SUS having a thermal expansion coefficient significantly different from that of the cylindrical base material and the ceramic target material.
- the degree of thermal expansion and contraction of the cylindrical target material, the cylindrical base material, and the connecting member is greatly different.
- a shrinkage stress is generated in the connecting member, and the stress is mainly applied to the cylindrical base material.
- the material was greatly warped, and as a result, eccentricity, level difference and warpage were increased.
- stress is also applied to the cylindrical target material, and as the thickness is reduced by sputtering, the residual stress is strongly received, and it is considered that the split target material is cracked during sputtering.
- Comparative Example 2 the base material holding member 45 was removed from the manufacturing apparatus used in Comparative Example 1, and a cylindrical target was manufactured using a manufacturing apparatus to which a cylindrical target material pressing member was added. In this apparatus, since there is no base material holding member 45, it is considered that deviation and eccentricity occurred in the upper part of the cylindrical base material and the upper part of the cylindrical sputtering target material during In solder cooling.
- the ITO cylindrical sputtering target obtained in Examples 1 to 3 can perform sputtering to the end of life as shown in FIG. could be formed.
- an oversputtering portion (portion indicated by an arrow attached to FIG. 9) is generated as shown in FIG.
- a homogeneous thin film could not be formed.
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Abstract
Description
前記円筒形セラミックスターゲット材の上端部を保持するターゲット材保持部材と、
前記円筒形基材の上端部を保持する基材保持部材と
前記下部保持部材、ターゲット材保持部材および基材保持部材を連結するチタン製もしくはチタン合金製、またはモリブデン製もしくはモリブデン合金製の連結部材と
を有することを特徴とする円筒形セラミックススパッタリングターゲットの製造装置である。
前記下部保持部材およびターゲット材保持部材によって前記円筒形セラミックスターゲット材の下端部及び上端部をそれぞれ保持し、前記下部保持部材および基材保持部材によって前記円筒形セラミックスターゲット材の中空部に収容されたチタン製もしくはチタン合金製、またはモリブデン製もしくはモリブデン合金製の前記円筒形基材の下端部および上端部をそれぞれ保持し、
前記製造装置、円筒形セラミックスターゲット材および円筒形基材を、前記円筒形セラミックスターゲット材と円筒形基材との接合に使用する半田の融点以上の温度に加温し、
前記円筒形セラミックスターゲット材と前記円筒形基材との間に形成される空隙部に、融解した前記半田を注入し、
前記製造装置、円筒形セラミックスターゲット材、円筒形基材および前記空隙部に注入された半田を、前記半田の融点より低い温度に冷却することを特徴とする円筒形セラミックススパッタリングターゲットの製造方法である。
本発明の円筒形セラミックススパッタリングターゲットは、円筒形基材、円筒形セラミックスターゲット材、および前記円筒形基材と円筒形セラミックスターゲット材とを接合する半田を備えた円筒形セラミックススパッタリングターゲットであって、前記円筒形セラミックスターゲット材の外表面における、該円筒形セラミックスターゲット材の両端からそれぞれ内側7mmの位置にダイヤル ゲージを当て、前記円筒形基材の外周面における、前記円筒形セラミックスターゲット材の両端からそれぞれ外側15mmの位置を支点として前記円筒形セラミックススパッタリングターゲットを1回転させて前記ダイヤルゲージの読みを測定したときに、前記ダイヤルゲージの読みの最大値と最小値との差が、いずれの測定箇所においても1.0mm以下であることを特徴とする。
[円筒形セラミックススパッタリングターゲットの製造装置および製造方法]
上記円筒形セラミックススパッタリングターゲットは、以下の円筒形セラミックススパッタリングターゲットの製造装置および製造方法により製造することができる。
直立した円筒形セラミックスターゲット材の下端部および該円筒形セラミックスターゲット材の中空部に収容された円筒形基材の下端部を保持する下部保持部材と、
前記円筒形セラミックスターゲット材の上端部を保持するターゲット材保持部材と、
前記円筒形基材の上端部を保持する基材保持部材と
前記下部保持部材、ターゲット材保持部材および基材保持部材を連結するチタン製もしくはチタン合金製、またはモリブデン製もしくはモリブデン合金製の連結部材と
を有する。
前記円筒形セラミックススパッタリングターゲットの製造装置を用いた円筒形セラミックススパッタリングターゲットの製造方法であって、
前記保持部材およびターゲット材保持部材によって前記円筒形セラミックスターゲット材の下端部及び上端部をそれぞれ保持し、前記保持部材および基材保持部材によって前記円筒形セラミックスターゲット材の中空部に収容されたチタン製もしくはチタン合金製、またはモリブデン製もしくはモリブデン合金製の前記円筒形基材の下端部および上端部をそれぞれ保持し、
前記製造装置、円筒形セラミックスターゲット材および円筒形基材を、前記円筒形セラミックスターゲット材と円筒形基材との接合に使用する半田の融点以上の温度に加温し、前記円筒形セラミックスターゲット材と前記円筒形基材との間に形成される空隙部に、融解した前記半田を注入し、
前記製造装置、円筒形セラミックスターゲット材、円筒形基材および前記空隙部に注入された半田を、前記半田の融点より低い温度に冷却する。
(組立工程)
図5に示したように、製造装置40に円筒形基材41及び円筒形ターゲット材42を取り付ける。まず、チタン製もしくはチタン合金製、またはモリブデン製もしくはモリブデン合金製の円筒形基材41を製造装置40に設置する。チタン合金及びモリブデン合金については前述の円筒形基材についての説明と同じである。円筒形基材41をたとえばテフロン(登録商標)製のOリング48が装着された下部保持部材43の基材保持部43cに取り付ける。これにより円筒形基材41と円筒形ターゲット材42との間に形成される空隙部49下端からのボンディング材の漏れ、及び円筒形基材41へのキズを防止することができる。
(加温工程)
製造装置40、すなわち下部保持部材43、ターゲット材保持部材44、基材保持部材45および連結部材46、ならびに製造装置40に取り付けられた円筒形基材41および円筒形ターゲット材42を、円筒形ターゲット材42と円筒形基材41との接合に使用する半田の融点以上の温度に加温する。たとえば、半田としてインジウム半田を使用する場合には160~250℃に加温する。
(半田注入工程)
ターゲット材保持部材44の上側から融解した半田を空隙部49に注入する。注入方法には、特に制限はなく空隙部49が溶融半田によって満たされるように注入すればよい。
(冷却工程)
製造装置40、円筒形基材41、円筒形ターゲット材42および空隙部49に注入された融解した半田を、半田の融点より低い温度に冷却する。たとえば、半田としてインジウム半田を使用する場合には150℃以下に冷却する。
(円筒形ターゲットの偏心の測定)
図1に示したターゲット回転装置4上に円筒形ターゲットを水平方向に置いた。回転具5aおよび5bが円筒形基材に当接する支点7aおよび7bを、円筒形ターゲット材の両端からそれぞれ外側15mmの位置になるように調整した。
(円筒形基材と円筒形ターゲット材とのズレの測定)
次のように円筒形基材と円筒形ターゲット材とのズレを測定した。
(分割ターゲット材間の段差の測定)
隣り合った分割ターゲット材の段差については、デプスゲージで、これら分割ターゲット材の隣り合う端面間の高低差を、円周方向において等間隔となる8箇所で測定し、その差の最大値を段差とした。
(円筒形スパッタリングターゲットの反りの測定)
ITO円筒形スパッタリングターゲットを、図1のターゲット回転装置4上に水平方向に静置した。ここで、円筒形基材に接合されている円筒形ターゲット材の外周面にストレートエッジを当て、円筒形ターゲット材とストレートエッジの間にできる隙間を、隙間ゲージを用いて測定した。円周方向において等間隔となる8箇所について前記測定を行い、隙間の最大値をITO円筒形スパッタリングターゲットの反りとした。
(接合時に割れが発生した分割ターゲット材の個数の測定)
ITO円筒形スパッタリングターゲットの円筒形ターゲット材を目視により観察し、9個の分割ターゲット材のうち割れが発生した分割ターゲット材の個数を計測した。
(スパッタリング時の侵食の評価)
製造されたITO円筒形スパッタリングターゲットを用いて以下の条件でスパッタリングを行った。スパッタリングを行った後の円筒形ターゲット材の侵食の状態を目視により観察した。
基板温度 100℃
スパッタ圧力 0.2Pa
パワー 20KW
ターゲット回転数 10rpm
(スパッタリングにより割れが発生した分割ターゲット材の個数の測定)
前記スパッタリング後にITO円筒形スパッタリングターゲットの円筒形ターゲット材を目視により観察し、9個の分割ターゲット材のうち割れが発生した分割ターゲット材の個数を計測した。
[実施例1]
図5に示した製造装置40を用いて、以下のようにITO円筒形スパッタリングターゲットを製造した。
[実施例2]
連結部材46がチタン合金(Ti-6AL-4V ASTM規格Gr.5)製である製造装置40を用いたこと以外は実施例1と同様の操作によりITO円筒形スパッタリングターゲットを製造した。
[実施例3]
円筒形基材がモリブデン製であること、および連結部材46がモリブデン製である製造装置40を用いたこと以外は実施例1と同様の操作によりITO円筒形スパッタリングターゲットを製造した。
[比較例1]
連結部材がSUS304製である点のみが製造装置40と異なる製造装置を用いたこと以外は実施例1と同様の操作によりITO円筒形スパッタリングターゲットを製造した。
[比較例2]
図7に示した製造装置60を用いてITO円筒形スパッタリングターゲットを製造した。製造装置60は、連結部材がSUS304製である点、基材保持部材45を有していない点、および4つの円筒形ターゲット材押え部材62を有する点において製造装置40と異なる。円筒形ターゲット材押え部材62は、4本の柱状部材46aに1つずつ設けられている。円筒形ターゲット材押え部材62は、柱状部材46aに結合する結合部62aおよび円筒形ターゲット材を押える押え部62bから構成される。押え部62bは棒状であり、円筒形分割ターゲット材間のすべての分割部を跨いで円筒形ターゲット材を側面から押え、円筒形ターゲット材の側面方向の動きを抑制する機能を有する。
2、12 円筒形基材
3、13 円筒形ターゲット材
4 ターゲット回転装置
5a、5b 回転具
6a、6b、16a、16b 端面
7a、7b、17a、17b 支点
40、60 製造装置
41 円筒形基材
42 円筒形ターゲット材
43 下部保持部材
44 ターゲット材保持部材
45 基材保持部材
46 連結部材
47、48、50、51 Oリング
49 空隙部
62 円筒形ターゲット材押え部材
Claims (12)
- 円筒形基材、円筒形セラミックスターゲット材、および前記円筒形基材と円筒形セラミックスターゲット材とを接合する半田を備えた円筒形セラミックススパッタリングターゲットであって、前記円筒形セラミックスターゲット材の外表面における、該円筒形セラミックスターゲット材の両端からそれぞれ内側7mmの位置にダイヤルゲージを当て、前記円筒形基材の外周面における、前記円筒形セラミックスターゲット材の両端からそれぞれ外側15mmの位置を支点として前記円筒形セラミックススパッタリングターゲットを1回転させて前記ダイヤルゲージの読みを測定したときに、前記ダイヤルゲージの読みの最大値と最小値との差が、いずれの測定箇所においても1.0mm以下である円筒形セラミックススパッタリングターゲット。
- 反りが0.6mm以下である請求項1に記載の円筒形セラミックススパッタリングターゲット。
- 前記円筒形セラミックスターゲット材が少なくとも2個の分割円筒形セラミックスターゲット材を含み、前記各分割円筒形セラミックスターゲット材の外表面における、該分割円筒形セラミックスターゲット材の両端からそれぞれ内側7mmの位置にダイヤル ゲージを当て、前記円筒形基材の外周面における、前記円筒形セラミックスターゲット材の両端からそれぞれ外側15mmの位置を支点として前記円筒形セラミックススパッタリングターゲットを1回転させて前記ダイヤルゲージの読みを測定したときに、前記ダイヤルゲージの読みの最大値と最小値との差が、いずれの測定箇所においても1.0mm以下である請求項1または2に記載の円筒形セラミックススパッタリングターゲット。
- 隣り合う前記分割円筒形セラミックスターゲット材間の段差がいずれも0.3mm以下である請求項3に記載の円筒形セラミックススパッタリングターゲット。
- 前記円筒形基材と前記円筒形セラミックスターゲット材との両端におけるズレが0.5mm以下である請求項1~4のいずれかに記載の円筒形セラミックススパッタリングターゲット。
- 前記円筒形基材がチタン製もしくはチタン合金製、またはモリブデン製もしくはモリブデン合金製である請求項1~5のいずれかに記載の円筒形セラミックススパッタリングターゲット。
- 前記円筒形セラミックスターゲット材の長さが500mm以上である請求項1~6のいずれかに記載の円筒形セラミックススパッタリングターゲット。
- 前記円筒形セラミックスターゲット材の相対密度が95%以上である請求項1~7のいずれかに記載の円筒形セラミックススパッタリングターゲット。
- 直立した円筒形セラミックスターゲット材の下端部および該円筒形セラミックスターゲット材の中空部に収容された円筒形基材の下端部を保持する下部保持部材と、
前記円筒形セラミックスターゲット材の上端部を保持するターゲット材保持部材と、
前記円筒形基材の上端部を保持する基材保持部材と
前記下部保持部材、ターゲット材保持部材および基材保持部材を連結するチタン製もしくはチタン合金製、またはモリブデン製もしくはモリブデン合金製の連結部材と
を有する円筒形セラミックススパッタリングターゲットの製造装置。 - 前記連結部材が少なくとも2本の柱状部材からなる請求項9に記載の円筒形セラミックススパッタリングターゲットの製造装置。
- 請求項9または10に記載の円筒形セラミックススパッタリングターゲットの製造装置を用いた円筒形セラミックススパッタリングターゲットの製造方法であって、
前記下部保持部材およびターゲット材保持部材によって前記円筒形セラミックスターゲット材の下端部及び上端部をそれぞれ保持し、前記下部保持部材および基材保持部材によって、前記円筒形セラミックスターゲット材の中空部に収容されたチタン製もしくはチタン合金製、またはモリブデン製もしくはモリブデン合金製の前記円筒形基材の下端部および上端部をそれぞれ保持し、
前記製造装置、円筒形セラミックスターゲット材および円筒形基材を、前記円筒形セラミックスターゲット材と円筒形基材との接合に使用する半田の融点以上の温度に加温し、
前記円筒形セラミックスターゲット材と前記円筒形基材との間に形成される空隙部に、融解した前記半田を注入し、
前記製造装置、円筒形セラミックスターゲット材、円筒形基材および前記空隙部に注入された半田を、前記半田の融点より低い温度に冷却する円筒形セラミックススパッタリングターゲットの製造方法。 - 請求項11に記載の円筒形セラミックススパッタリングターゲットの製造方法であって、
前記円筒形セラミックスターゲット材が少なくとも2個の分割円筒形セラミックスターゲット材からなり、前記下部保持部材およびターゲット材保持部材によって円筒形セラミックスターゲット材の下端部及び上端部をそれぞれ保持するとき、前記分割円筒形セラミックスターゲット材間の段差が0.3mm以下になるように調整する円筒形セラミックススパッタリングターゲットの製造方法。
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JP2018159105A (ja) * | 2017-03-22 | 2018-10-11 | Jx金属株式会社 | スパッタリングターゲット及び、その製造方法 |
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JPWO2021100233A1 (ja) * | 2019-11-21 | 2021-11-25 | 三井金属鉱業株式会社 | スパッタリングターゲット及びその製造方法 |
KR20220104150A (ko) | 2019-11-21 | 2022-07-26 | 미쓰이금속광업주식회사 | 스퍼터링 타깃 및 그 제조 방법 |
JP7139453B2 (ja) | 2019-11-21 | 2022-09-20 | 三井金属鉱業株式会社 | スパッタリングターゲット及びその製造方法 |
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JP6568867B2 (ja) | 2019-08-28 |
TWI710652B (zh) | 2020-11-21 |
CN106232860A (zh) | 2016-12-14 |
CN106232860B (zh) | 2021-07-13 |
KR20170074823A (ko) | 2017-06-30 |
JPWO2016067717A1 (ja) | 2017-08-10 |
JP2019183285A (ja) | 2019-10-24 |
KR102288720B1 (ko) | 2021-08-13 |
TW201615873A (zh) | 2016-05-01 |
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