WO2015004958A1 - スパッタリングターゲット及び、それの製造方法 - Google Patents
スパッタリングターゲット及び、それの製造方法 Download PDFInfo
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- WO2015004958A1 WO2015004958A1 PCT/JP2014/058987 JP2014058987W WO2015004958A1 WO 2015004958 A1 WO2015004958 A1 WO 2015004958A1 JP 2014058987 W JP2014058987 W JP 2014058987W WO 2015004958 A1 WO2015004958 A1 WO 2015004958A1
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
- B22D21/002—Castings of light metals
- B22D21/007—Castings of light metals with low melting point, e.g. Al 659 degrees C, Mg 650 degrees C
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
- B22D21/02—Casting exceedingly oxidisable non-ferrous metals, e.g. in inert atmosphere
- B22D21/027—Casting heavy metals with low melting point, i.e. less than 1000 degrees C, e.g. Zn 419 degrees C, Pb 327 degrees C, Sn 232 degrees C
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/08—Shaking, vibrating, or turning of moulds
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
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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
- 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
Definitions
- the present invention relates to a sputtering target used for sputtering, which is a technique for producing a thin film on a substrate, and a method for producing the same.
- the present invention effectively eliminates the risk of arcing when performing sputtering.
- a back electrode layer, a light absorption layer, a resistance buffer layer, and a transparent conductive layer are sequentially arranged on a substrate.
- Various studies have been made to increase the light absorption capacity of the light absorption layer of solar cells.
- a CIGS alloy having a wavelength that covers a wide spectrum range of sunlight and having a high light absorption capability may be used.
- the planar surface thereof is used in an annular shape, and the target surface The area used is reduced and the surface cannot be used effectively.
- sputtering is performed under rotation around the axis of such a cylindrical sputtering target using a cylindrical sputtering target bonded to the outer peripheral surface of a cylindrical backing tube. Sputtering technology by rotary sputtering has been put into practical use.
- a conceptual diagram of the cylindrical sputtering target is shown in FIG.
- a cylindrical sputtering target 100 shown in FIG. 1 is formed on the outer peripheral side of a cylindrical backing tube 101.
- a sputtering target made of indium has a backing plate or a backing tube or other supporting substrate disposed in a mold as described in Patent Document 1, for example, in both flat and cylindrical types.
- indium in a molten state is generally poured by casting into the casting space where the surface of the supporting substrate is exposed, and is formed by a melt casting method in which it is cooled and cured.
- this melting casting method it is difficult to make the solidification rate of indium during cooling constant throughout the casting space for forming the sputtering target, especially when manufacturing a sputtering target having a length exceeding 1 m. Since the structure of the sputtering target is not uniform and the crystal grains are coarsened, it is difficult to make the film thickness distribution of the deposition substrate sufficiently uniform when sputtering is performed using the structure.
- Patent Document 2 a tubular sputter target is disposed on a support tube by spraying molten indium toward a rotating support tube. Depending on the grain size, it had a fine grain microstructure with an average grain size of 50-500 ⁇ m. In many cases the resulting average grain size was less than 200 ⁇ m, ”and“ the book in the form of a layer. Thanks to the production of the sputter target according to the invention, the microstructure is homogeneous over the thickness of the sputter target and the exterior surface. "
- the present invention aims to solve such problems of the prior art, and the object of the present invention is to increase the target density sufficiently to enable stable sputtering, It is an object of the present invention to provide a sputtering target capable of effectively removing the cause of arcing during sputtering and realizing uniform film thickness of a film formation substrate by sputtering, and a method of manufacturing the same.
- the inventor adds a small amount of copper to indium, casts a sputtering target material by, for example, a melt casting method, and further performs a predetermined plastic processing to produce a sputtering target, thereby producing a conventional melting target. It has been found that crystal grains can be effectively refined while achieving a high density as in the casting method.
- the sputtering target of the present invention contains Cu at 5 wtppm to 10,000 wtppm, the balance is In, the relative density is 99% or more, and the average crystal grain size is 3000 ⁇ m or less.
- the average crystal grain size of the sputtering target of the present invention is preferably 10 ⁇ m to 1000 ⁇ m, more preferably 10 ⁇ m to 500 ⁇ m, and even more preferably 10 ⁇ m to 300 ⁇ m. Further, here, this sputtering target preferably has an oxygen concentration of 20 wtppm or less.
- the sputtering target of the present invention may further contain at least one selected from S, Cd, Zn, Se, Mg, Ca, and Sn in a total amount of 100 wtppm or less, and may have a cylindrical shape. preferable.
- the sputtering target manufacturing method of the present invention is such that, for example, a sputtering target material containing Cu at 5 wtppm to 10000 wtppm and the balance being made of In is bonded to the surface of the support substrate by a melt casting method or a spraying method. Thereafter, plastic processing in the thickness direction of the sputtering target material is performed on the sputtering target material at a thickness reduction rate within a range of 10% to 80%.
- the sputtering target material may further contain at least one selected from S, Cd, Zn, Se, Mg, Ca, and Sn in a total amount of 100 wtppm or less.
- the supporting base material is preferably a cylindrical backing tube and is preferably used for manufacturing a cylindrical sputtering target.
- the sputtering target material is preferably formed by casting using a molten metal. In this case, the molten metal is preferably stirred and shaken during casting, and the casting is performed in a nitrogen or Ar atmosphere. It is preferable to carry out with.
- the sputtering target of the present invention since the relative density is 99% or more and the average crystal grain size is 3000 ⁇ m or less, the possibility of arcing at the time of sputtering can be effectively eliminated, and stable sputtering can be performed. In addition, the film thickness of the substrate thus formed can be made sufficiently uniform. Moreover, according to the sputtering target manufacturing method of the present invention, a sputtering target having a high density and a small average crystal grain size as described above can be manufactured.
- the sputtering target of the present invention has a required shape such as a flat type bonded to the surface of a disk-shaped backing plate or a cylindrical type bonded to the outer surface of a cylindrical backing tube.
- Cu is contained at 5 wtppm to 10000 wtppm, the remainder is made of In, the relative density is 99% or more, and the average crystal grain size is 3000 ⁇ m or less.
- the cylindrical sputtering target 100 as illustrated in FIG. 1 is formed on the outer peripheral side of the cylindrical backing tube 101, the target surface can be effectively used for the above-described rotary type sputtering. Can be used.
- the average crystal grain size after plastic processing as will be described later is sufficiently set to, for example, 3000 ⁇ m or less. It becomes possible to make it smaller. If the copper content decreases, it becomes difficult to obtain the effect of refining the crystal grains, so that the copper is contained in an amount of 5 wtppm or more in order to effectively make the crystal grains fine. On the other hand, when there is too much copper content, there exists a possibility that the compound of Cu and In will increase and arcing may increase. Therefore, the upper limit of the copper content is 10000 wtppm.
- a preferred range for the copper content is 25 to 5000 wtppm, particularly 50 to 1000 wtppm, and of these, 100 to 500 wtppm.
- the sputtering target of the invention may further contain at least one impurity selected from S, Cd, Zn, Se, Mg, Ca, and Sn in a total amount of 100 wtppm or less. If such impurities are 100 wtppm or less, even if they are contained in the sputtering target, there is no possibility of adversely affecting the crystal grain refining effect by adding copper as described above.
- the impurities are preferably 80 wtppm or less, more preferably 50 wtppm or less, and most preferably 10 wtppm or less.
- the backing tube or backing plate or other supporting substrate can be formed of any material, and specific examples thereof include stainless steel, titanium, copper, etc. Of these, stainless steel and titanium are preferable.
- this sputtering target has a relative density of 99% or more.
- production of arcing at the time of performing sputtering is prevented effectively, and stable film-forming can be implemented.
- the relative density of the sputtering target is preferably 99% or more, more preferably 99.2% or more, and particularly preferably 99.5% or more. .
- the average crystal grain size is 3000 ⁇ m or less.
- the average crystal grain size is preferably 1000 ⁇ m or less, particularly 500 ⁇ m or less, and more preferably 300 ⁇ m or less.
- the lower limit of the average crystal grain size of the sputtering target is, for example, about 10 ⁇ m.
- the oxygen concentration in such a sputtering target is too high, there is a concern that arcing may occur during sputtering, as in the case where the density is low. Therefore, the oxygen concentration is preferably 20 wtppm or less. When the content is 15 wtppm or less, particularly 10 wtppm or less, the possibility of arcing can be sufficiently removed. On the other hand, as the oxygen concentration is lowered, the investment for the facility increases. However, since the effect per cost decreases, the lower limit value of the oxygen concentration can be set to 10 wtppm, for example.
- a cylindrical sputtering target can be produced as follows. First, copper is added to the dissolved indium at 5 wtppm to 10000 wtppm, and the molten metal is poured into the casting space of the mold. Here, prior to pouring the molten metal, a cylindrical backing tube is previously arranged on the inner peripheral side of the casting space of the mold so that the outer peripheral surface thereof is exposed to the casting space. If necessary, in order to remove oxide slag present in the molten metal, the molten metal is agitated and rocked using a stirring rod or the like, or cast in an atmosphere in which the amount of oxygen such as nitrogen and Ar is reduced in advance.
- the sputtering target material is formed in a posture that surrounds the backing tube by cooling and hardening the molten metal in the casting space, for example, with a cooling facility or the like disposed around the mold. At this time, the sputtering target material is bonded to the outer peripheral surface of the backing tube.
- the cylindrical joined body of the sputtering target material and the backing tube is subjected to plastic working in the direction of reducing the thickness in the thickness direction of the sputtering target material, in this case, inward in the radial direction.
- the amount of processing at this time is 10% to 80% in terms of the thickness reduction rate of the sputtering target material.
- Sputtering target after casting generally has a lot of coarse particles, and the crystal grains become coarse, and it is a sputtering target material formed by containing Cu in indium that can be sufficiently recrystallized during plastic processing even at room temperature.
- the plastic processing as described above, recrystallization of the sputtering target material is promoted, and the crystal structure becomes finer, so that the crystal grains of the sputtering target to be manufactured are refined. be able to.
- the spraying method can be used instead of the melting casting method described above, the melting casting method can increase the density of the sputtering target material to be formed and can reduce the cost. Since it can suppress, it is preferable at the point which can implement
- the sputtering target manufactured as described above can have a relative density of 99% or more and an average crystal grain size of 3000 ⁇ m or less, and its thickness is measured along the radial direction, for example, 5 mm to 20 mm. And generally about 8 mm to 15 mm.
- the plastic working is a rolling process, an extrusion process, a press process, etc., as long as pressure is applied to the sputtering target material inward in the radial direction (in the direction of decreasing the thickness in the case of a flat sputtering target), Regardless of the means used, and since the temperature condition during the processing does not matter, it may be either cold or hot.
- a mandrel 10 having an outer diameter slightly smaller than the inner diameter is provided inside the backing tube 2 joined to the inner peripheral side of the sputtering target material 1 after casting as necessary. Further, the sputtering target material 1 is inserted and the inclined surfaces 21a of the two support portions 21 arranged on the base 20, and the pressing means 22 that is spaced apart from the support portions 21 on the upper side in the figure. The flat surface 22a is sandwiched between and supported. In that state, the pressing means 22 is moved toward the base 20 side as indicated by an arrow in the drawing until it reaches a predetermined thickness reduction rate, and the sputtering target material 1 is pressed to reduce the thickness. This is performed with the same processing amount over the entire circumference.
- each of the support portion and the pressing means follows the outer peripheral surface of the sputtering target material 1 although not shown in the drawing, instead of the flat surface-like inclined surface 21a and the flat surface 22a. It can be of a curved surface.
- the material of the mandrel 10 that functions to support the sputtering target material at the time of pressing from the inner peripheral side and maintain the cylindrical shape thereof is, for example, hard enough not to be deformed even by the action of pressure applied by the press.
- Stainless steel, cast iron, and the like can be used, but stainless steel is preferable from the viewpoint of preventing contamination due to rust and the like.
- interposes between several rolls and presses by rotating a sputtering target raw material to the surroundings of a center axis line direction or not rotating can be implemented.
- the sputtering target material is inserted into a tubular space having a predetermined shape such as a taper of an extruder, and is passed through it at a predetermined extrusion speed, thereby performing an extrusion process for plastic processing to a desired thickness. It is also possible.
- the processing amount is within the above range in terms of thickness reduction rate.
- the thickness reduction rate is preferably 10 to 80%, more preferably 15 to 70%.
- the sputtering target manufactured as described above can be suitably used for the production of a light absorption layer of a CIGS thin film solar cell.
- the target of Example 1 was manufactured by the following method. Indium with a purity of 4N is dissolved and copper of 5 wtppm is added thereto, and the molten metal is poured into a cylindrical casting space of a SUS304 mold in which a backing tube is arranged inside, and then cooled and hardened there to form a sputtering target material. Formed.
- a heater was arranged around the mold, and when the molten metal was poured into the casting space, the mold was heated to 180 ° C. by the heater, and when cooling and curing was performed, the heater was turned off and allowed to cool to the atmosphere. .
- a tube made of SUS304 having an axial length of 640 mm, an inner diameter of 125 mm, and an outer diameter of 133 mm was used.
- the sputtering target material is placed as shown in FIG. 2 with the SUS304 mandrel inserted inside, and cold-pressed by pressing means every time it is rotated around the axis by 5 °.
- Plastic working with a working amount with a thickness reduction rate of 14.3% was performed under normal temperature conditions.
- This processing amount was an average value of thickness reduction rates measured at four measurement points set at 90 ° intervals in the circumferential direction at one end portion (end portion A) of the sputtering target material.
- the target thus obtained was cut with a lathe into dimensions of an axial length of 600 mm, an inner diameter of 133 mm, and an outer diameter of 151 mm to produce the target of Example 1.
- Example 2 to 6 was the same as Example 1 except that the amount of Cu added was 20, 50, 100, 1000, and 10000 wtppm, respectively.
- Example 7 was the same as Example 1 except that the Cu addition amount was 100 wtppm and the processing amount was 50%.
- Examples 8 and 9 were the same as Example 1 except that Cu was added at 100 wtppm, S was added at 100 wtppm in Example 8, and Zn was further added at 100 wtppm in Example 9.
- Each of Examples 10 and 11 was the same as each of Examples 4 and 6 except that the target type was a round disk-shaped flat sputtering target and the processing amount was 80%.
- Example 12 was the same as Example 1 except that it was cast in a nitrogen atmosphere.
- Comparative Example 1 was the same as Example 1 except that Cu was not added, and Comparative Example 2 was the same as Example 1 except that Cu was not added and plastic working was not performed.
- Comparative Example 3 was the same as Example 1 except that Cu was not added, the sputtering target was formed by thermal spraying instead of casting, and plastic processing was not performed.
- Comparative Example 4 was the same as Example 1 except that the Cu addition amount was 100 wtppm, the sputtering target was formed by thermal spraying instead of casting, and plastic processing was not performed.
- Comparative Example 5 was the same as Example 1 except that the amount of Cu added was 100 wtppm and plastic processing was not performed.
- the average crystal grain size, relative density, and oxygen concentration are measured, and sputtering is performed using each sputtering target, and the film thickness of the deposition substrate and sputtering are measured. The number of occurrences of arcing per hour was measured.
- the sputtering conditions are as follows. ⁇ Sputtering gas: Ar ⁇ Sputtering gas pressure: 0.5Pa ⁇ Sputtering gas flow rate: 50 SCCM Sputtering temperature: T. T. et al. (No heating) ⁇ Sputtering power density: 1.3 W / cm 2 -Substrate: Corning Eagle 2000, ⁇ 4 inch x 0.7 mmt (placed opposite the film thickness measurement location) ⁇ Deposition time: 1 min ⁇ Pre-sputtering: 1h under the above conditions Further, here, in measuring the film thickness of the film formation substrate, the film thickness at the position corresponding to the central region in the longitudinal direction of the sputtering target and the position corresponding to one end portion (end portion A) in the longitudinal direction. Each of the film thickness and the film thickness at the position corresponding to the other end portion (end portion B) in the longitudinal direction were measured, and the standard deviation of the film thicknesses was also obtained. The results are shown in Table 1.
- the present invention is not limited to a cylindrical sputtering target, but is also a round disk, a rectangular or other flat sputtering target. It can be seen that this is also applicable.
- Example 12 it turns out that oxygen concentration is reducing to 10 wtppm by casting in nitrogen atmosphere.
- Comparative Example 1 the crystal grain size was large because Cu was not added, and there was room for further improvement in the film thickness distribution. Since Comparative Example 2 was formed by a casting method and was not subjected to plastic working, the particle size was large and the film thickness distribution was non-uniform. In Comparative Example 3, although the crystal grain size was reduced by being formed by thermal spraying, the relative density was low and arcing occurred. Comparative Example 4 was formed by thermal spraying and was not subjected to plastic working. However, although the crystal grain size was small and the film thickness distribution was uniform, the relative density was small. It became stable sputtering. Although the comparative example 5 contained Cu, since the plastic processing was not performed after casting, the crystal grains were coarse and the film thickness distribution became non-uniform. Therefore, according to the present invention, it is clear that the film thickness by sputtering can be made uniform while eliminating the risk of arcing.
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Abstract
Description
ここで、光吸収層を形成するには、太陽光のスペクトルの範囲を広くカバーする波長を有し、光吸収能力の高いものとして知られているCIGS系合金を用いることがあり、具体的には、Cu、In、Ga、Se等からなるこのCIGS系合金をスパッタリングターゲットとして、ガラス基板等の基板に対し、スパッタリングすることにより行うことができる。
この溶解鋳造法では、冷却時のインジウムの凝固速度を、スパッタリングターゲットを形成するための鋳造空間の全体で一定にすることが難しく、特に、長さが1mを超えるようなスパッタリングターゲットを製造する場合は、スパッタリングターゲットの組織が不均一になるとともに結晶粒が粗大化するので、それを用いてスパッタリングを実施すると、成膜基板の膜厚分布を十分に均一なものとすることが困難となる。
ここで、この発明のスパッタリングターゲットの平均結晶粒径は、10μm~1000μmであることが好ましく、より好ましくは10μm~500μmであり、さらには10μm~300μmであることが一層好適である。
またここで、このスパッタリングターゲットは、酸素濃度が20wtppm以下であることが好ましい。
そしてまた、前記スパッタリングターゲット素材は、溶湯を用いた鋳造により形成することが好適であり、この場合は、鋳造時に溶湯の撹拌、揺動を行うことが好ましく、また、鋳造を窒素もしくはAr雰囲気下で行うことが好ましい。
またこの発明の、スパッタリングターゲットの製造方法によれば、上記のような、密度が高く、かつ平均結晶粒径の小さいスパッタリングターゲットを製造することができる。
この発明のスパッタリングターゲットは、たとえば、円盤状のバッキングプレートの表面に接合される平型または、円筒状のバッキングチューブの外表面に接合される円筒型等の所要の形状を有し、基板上への薄膜形成のスパッタリングに供されるものであって、Cuを5wtppm~10000wtppmで含有し、残部がInからなり、相対密度が99%以上、かつ、平均結晶粒径が3000μm以下であるものである。
なお、図1に例示するような円筒型スパッタリングターゲット100とし、これを円筒状のバッキングチューブ101の外周側に形成したときは、先述のロータリー型スパッタリングに供することができて、ターゲット表面を有効に利用することができる。
銅の含有量が少なくなると、それによる結晶粒の微細化効果を得ることが難しくなることから、結晶粒を有効に微細なものとするため、銅は5wtppm以上含有させるものとする。一方、銅の含有量が多すぎる場合は、CuとInの化合物が多くなり、アーキングが増加する懸念がある。従って、銅の含有量の上限値は、10000wtppmとする。銅の含有量の好ましい範囲は、25~5000wtppm、特に、50~1000wtppm、そのなかでも、100~500wtppmである。
A=2(s/π)1/2
はじめに、溶解させたインジウムに銅を5wtppm~10000wtppmで添加し、その溶湯を鋳型の鋳造空間へ流し込む。ここでは、溶湯の流し込みに先立って、鋳型の鋳造空間の内周側に、円筒形状のバッキングチューブを、その外周面が鋳造空間に露出する姿勢で予め配置しておく。なお必要に応じて、溶湯内に存在する酸化物スラグを取り除くため、溶湯を、撹拌棒などを使用して撹拌、揺動させることや、あらかじめ窒素、Arなどの酸素量を低減した雰囲気で鋳造を行うことが重要である。
そして溶湯を鋳造空間に流し込んだ後、たとえば鋳型の周囲に配置した冷却設備等により、鋳造空間で溶湯を冷却硬化させることで、スパッタリングターゲット素材を、バッキングチューブの周囲を取り囲む姿勢で形成する。この際に、スパッタリングターゲット素材はバッキングチューブの外周面に接合されることになる。
上記のようにして製造されるスパッタリングターゲットは、相対密度を99%以上かつ、平均結晶粒径を3000μm以下とすることができ、また、その厚みは半径方向に沿って測って、たとえば5mm~20mm程度、一般には8mm~15mm程度とすることができる。
なおここで、プレス時のスパッタリングターゲット材を内周側から支持してその円筒形状を維持するべく機能する心棒10の材質は、たとえば、プレスによる加圧力の作用によっても変形しない程度の硬さを有するステンレス、鋳鉄等とすることができるが、錆等によるコンタミを防止するとの観点からはステンレスが好ましい。
実施例8、9は、いずれもCuを100wtppm添加するとともに、実施例8ではSを100wtppm、実施例9ではZnを100wtppmでさらに添加したことを除いて、実施例1と同様とした。
実施例10、11のそれぞれは、ターゲットのタイプを丸盤状の平型スパッタリングターゲットとし、加工量を80%としたことを除いて、実施例4、6のそれぞれと同様とした。
実施例12は、窒素雰囲気で鋳造したことを除いて、実施例1と同様とした。
また、比較例4は、Cu添加量を100wtppmとし、かつ、スパッタリングターゲットを、鋳造に代えて溶射により形成するとともに、塑性加工を施さなかったことを除いて、実施例1と同様とした。比較例5は、Cu添加量を100wtppmとし、塑性加工を施さなかったことを除いて、実施例1と同様とした。
・スパッタガス: Ar
・スパッタガス圧: 0.5Pa
・スパッタガス流量: 50SCCM
・スパッタリング温度: R.T.(無加熱)
・投入スパッタパワー密度: 1.3W/cm2
・基板: コーニング社製イーグル2000、φ4インチ×0.7mmt(膜厚測定箇所の対面に配置)
・成膜時間: 1min
・プレスパッタ: 上記条件で1h
またここで、成膜基板の膜厚を測定するに当っては、スパッタリングターゲットの長手方向の中央域に対応する位置の膜厚と、長手方向の一端部(端部A)に対応する位置の膜厚と、長手方向の他端部(端部B)に対応する位置の膜厚のそれぞれを測定し、そして、それらの膜厚の標準偏差も求めた。
それらの結果を表1に示す。
そしてまた、実施例8、9のように、100wtppm以下のSやZn等の不純物を含んでいても、結晶粒の微細化効果を十分に発揮されることが明らかである。なお、実施例10、11のような丸盤形状のスパッタリングターゲットでも、結晶粒が小さくなっていることから、この発明は、円筒型スパッタリングターゲットのみならず、丸盤や矩形その他の平型スパッタリングターゲットにも適用可能であることが解かる。実施例12では、窒素雰囲気で鋳造することで、酸素濃度が10wtppmまで低減していることがわかる。
従って、この発明によれば、アーキングのおそれを取り除きつつ、スパッタリングによる成膜の膜厚を均一化できることが明らかである。
2 バッキングチューブ
10 心棒
20 土台
21 支持部
21a 傾斜面
22 押圧手段
22a 平坦面
Claims (13)
- Cuを5wtppm~10000wtppmで含有し、残部がInからなり、相対密度が99%以上、かつ、平均結晶粒径が3000μm以下である、スパッタリングターゲット。
- 平均結晶粒径が10μm~1000μmである、請求項1に記載のスパッタリングターゲット。
- 平均結晶粒径が10μm~500μmである、請求項2に記載のスパッタリングターゲット。
- 平均結晶粒径が10μm~300μmである、請求項3に記載のスパッタリングターゲット。
- 酸素濃度が20wtppm以下である、請求項1~4のいずれか一項に記載のスパッタリングターゲット。
- S、Cd、Zn、Se、Mg、Ca、Snから選択される少なくとも一種を100wtppm以下でさらに含有してなる、請求項1~5のいずれか一項に記載のスパッタリングターゲット。
- 円筒型の形状を有する、請求項1~6のいずれか一項に記載のスパッタリングターゲット。
- Cuを5wtppm~10000wtppmで含有するとともに残部がInからなるスパッタリングターゲット素材を、支持基材の表面に接合させて形成し、その後、前記スパッタリングターゲット素材に対し、該スパッタリングターゲット素材の厚み方向の塑性加工を、10%~80%の範囲内の厚み減少率で施す、スパッタリングターゲットの製造方法。
- 前記スパッタリングターゲット素材が、S、Cd、Zn、Se、Mg、Ca、Snから選択される少なくとも一種を合計100wtppm以下でさらに含有するものとする、請求項8に記載のスパッタリングターゲットの製造方法。
- 前記支持基材を円筒形状のバッキングチューブとし、円筒型スパッタリングターゲットを製造する、請求項8または9に記載のスパッタリングターゲットの製造方法。
- 前記スパッタリングターゲット素材を、溶湯を用いた鋳造により形成する、請求項8~10のいずれか一項に記載のスパッタリングターゲットの製造方法。
- 鋳造時に溶湯の撹拌、揺動を行う、請求項11に記載のスパッタリングターゲットの製造方法。
- 鋳造を窒素もしくはAr雰囲気下で行う、請求項11または12に記載のスパッタリングターゲットの製造方法。
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US9748079B2 (en) | 2014-04-22 | 2017-08-29 | Mitsubishi Materials Corporation | Cylindrical sputtering target material |
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EP3211116A4 (en) * | 2015-03-04 | 2018-06-27 | JX Nippon Mining & Metals Corporation | Magnetic-material sputtering target and method for producing same |
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JP2016191087A (ja) * | 2015-03-30 | 2016-11-10 | Jx金属株式会社 | 積層構造体及びその製造方法 |
CN107636188A (zh) * | 2015-04-20 | 2018-01-26 | 万腾荣先进材料德国有限责任公司 | 用于制备管状制品的方法 |
WO2016169786A1 (en) * | 2015-04-20 | 2016-10-27 | Heraeus Deutschland GmbH & Co. KG | Process for preparing a tubular article |
JP2018517842A (ja) * | 2015-04-20 | 2018-07-05 | マテリオン アドバンスド マテリアルズ ジャーマニー ゲーエムベーハー | チューブ状物品の製作方法 |
EP3085809A1 (en) * | 2015-04-20 | 2016-10-26 | Heraeus Deutschland GmbH & Co. KG | Process for preparing a tubular article |
CN107636188B (zh) * | 2015-04-20 | 2020-08-11 | 万腾荣先进材料德国有限责任公司 | 用于制备管状制品的方法 |
JP2017106091A (ja) * | 2015-12-11 | 2017-06-15 | Jx金属株式会社 | In−Cu合金スパッタリングターゲット及びその製造方法 |
WO2017135349A1 (ja) * | 2016-02-05 | 2017-08-10 | 住友化学株式会社 | 円筒型ターゲットの製造方法および円筒型ターゲット |
TWI647023B (zh) * | 2016-02-05 | 2019-01-11 | 日商住友化學股份有限公司 | 圓筒型靶材的製造方法、圓筒型靶材及圓筒型靶材組 |
US10670384B2 (en) | 2016-02-05 | 2020-06-02 | Sumitomo Chemical Company, Limited | Cylindrical target production method and cylindrical target |
JP2018006685A (ja) * | 2016-07-07 | 2018-01-11 | Jx金属株式会社 | インジウムターゲット部材及びその製造方法 |
WO2020066957A1 (ja) * | 2018-09-26 | 2020-04-02 | 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 |
JPWO2020066957A1 (ja) * | 2018-09-26 | 2021-09-24 | 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 |
JP7145963B2 (ja) | 2018-09-26 | 2022-10-03 | 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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CN104919080A (zh) | 2015-09-16 |
US9922807B2 (en) | 2018-03-20 |
TW201506184A (zh) | 2015-02-16 |
JP5855319B2 (ja) | 2016-02-09 |
JPWO2015004958A1 (ja) | 2017-03-02 |
TWI558833B (zh) | 2016-11-21 |
US20160126072A1 (en) | 2016-05-05 |
CN104919080B (zh) | 2018-10-16 |
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