WO2016129622A1 - Cible de pulvérisation cathodique et son procédé de production - Google Patents

Cible de pulvérisation cathodique et son procédé de production Download PDF

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Publication number
WO2016129622A1
WO2016129622A1 PCT/JP2016/053897 JP2016053897W WO2016129622A1 WO 2016129622 A1 WO2016129622 A1 WO 2016129622A1 JP 2016053897 W JP2016053897 W JP 2016053897W WO 2016129622 A1 WO2016129622 A1 WO 2016129622A1
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target
base material
less
sputtering target
target members
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PCT/JP2016/053897
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English (en)
Japanese (ja)
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幸三 長田
純 梶山
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Ｊｘ金属株式会社
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Priority to JP2016574826A priority Critical patent/JP7097670B2/ja
Publication of WO2016129622A1 publication Critical patent/WO2016129622A1/fr

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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

Definitions

  • the present invention relates to a sputtering target and a manufacturing method thereof.
  • it relates to the surface roughness of the sintered body constituting the target member.
  • the cylindrical sputtering target refers to a sputtering target obtained by processing a sintered body made of a target material into a hollow cylindrical shape and joining it to a substrate called a backing plate or a backing tube.
  • Such a cylindrical sputtering target has advantages in that the use efficiency of the target is high, the generation of erosion is small, and the generation of particles due to the separation of the deposit is small compared to the flat plate type sputtering target.
  • the advantage of low generation of particles is very advantageous in reducing the occurrence of arcing due to redeposition of particles on the target.
  • a sintered body (ceramics) obtained by mixing and sintering indium oxide powder and tin oxide powder is hollow. It is processed into a cylindrical shape and bonded to a cylindrical substrate (backing tube).
  • Patent Document 1 A technique for realizing a type sputtering target has been developed.
  • the target members When a plurality of target members are arranged with no gap with respect to the base material, the target members may expand and contract due to heat during sputtering, and the target members may collide with each other, which may cause cracking or chipping. Therefore, in general, when joining a plurality of target members to a base material, it is carried out with a certain interval between the target members.
  • An object of the present invention is to provide a sputtering target capable of suppressing the occurrence of arcing during sputtering and improving the yield of a device manufacturing process using a sputtering process.
  • a sputtering target includes a plurality of target members made of ceramics bonded to a base material made of metal via a bonding material made of a low melting point metal having a melting point of 300 ° C. or lower.
  • the surface roughness (Ra) on the surface of the base material that contacts the bonding material is 1.8 ⁇ m or more (preferably 1.8 ⁇ m or more and 3.0 ⁇ m or less, more preferably 1.8 ⁇ m or more and 2.5 ⁇ m or less).
  • the plurality of target members have a hollow cylindrical shape, and face each other with a predetermined interval between adjacent target members when joined to the base material so as to surround the outer peripheral surface of the base material. It has a circular surface, and the surface roughness (Ra) on the circular surface is 1.0 ⁇ m or less.
  • the surface roughness (Ra) is preferably 0.05 ⁇ m or more and 1.0 ⁇ m or less.
  • a manufacturing method of a sputtering target includes a hollow cylinder made of ceramics bonded to a base made of metal via a bonding material made of a low melting point metal having a melting point of 300 ° C. or lower.
  • the circular surfaces of the plurality of target members having a shape are polished so that the surface roughness (Ra) is 2.0 ⁇ m or more and 8.0 ⁇ m or less, and the surface of the substrate that is in contact with the bonding material is surface roughness (Ra ) Is 1.8 ⁇ m or more (preferably 1.8 ⁇ m or more and 3.0 ⁇ m or less, more preferably 1.8 ⁇ m or more and 2.5 ⁇ m or less), with a predetermined interval between each adjacent target member.
  • the plurality of target members are bonded to the base material via the bonding material so that the circular surfaces face each other and surround an outer peripheral surface of the base material.
  • the surface roughness (Ra) is preferably 0.05 ⁇ m or more and 1.0 ⁇ m or less.
  • the target member may be made of ITO (Indium-Tin-Oxide), IZO (Indium-Zinc-Oxide), or IGZO (Indium-Gallium-Tin-Oxide).
  • the surface roughness (Ra) is measured according to ANSI standards using a non-contact type surface roughness measuring machine. The surface roughness is measured at each of the end surfaces of the target member at six locations at 60 ° intervals (12 locations per target member), and the weighted average value of all measured values is defined as the surface roughness of the target member.
  • FIG. 1 is a perspective view showing a configuration of a sputtering target according to an embodiment of the present invention.
  • FIG. 2 is sectional drawing which shows the structure of the sputtering target which concerns on one Embodiment of this invention.
  • a cylindrical sputtering target is exemplified.
  • the cylindrical sputtering target 100 includes a base material 101 and a plurality of target members 102a and 102b.
  • the target members 102a and 102b are bonded to the base material 101 via the bonding material 103, respectively.
  • the bonding material 103 is provided so as to fill a gap provided between the base material 101 and the target members 102a and 102b.
  • the sputtering target 100 is characterized by a sintered body constituting a plurality of target members 102a and 102b. Specifically, each of the target members 102a and 102b has a circular surface 104 facing the adjacent target member at a predetermined interval, and the surface roughness Ra of the circular surface 104 is 1.0 ⁇ m or less (preferably , 0.05 ⁇ m or more and 1.0 ⁇ m or less). This point will be described later.
  • the plurality of target members 102 a and 102 b are provided so as to surround the outer peripheral surface of the base material 101.
  • the plurality of target members 102 a and 102 b are preferably provided coaxially or substantially coaxially with the central axis of the substrate 101.
  • the target members 102a and 102b are arranged at predetermined intervals.
  • the gap may be 1 mm or less, for example, 0.1 to 0.5 mm.
  • the cylindrical sputtering target 100 of the present embodiment can be formed into a long sputtering target having a length of 100 mm or more by bonding a plurality of target members 102 to the base material 101 by the bonding material 103.
  • the base material 101 has an outer surface shape along the inner surface of the target members 102a and 102b having a hollow cylindrical shape. As described above, the outer diameter of the base material 101 is slightly smaller than the inner diameters of the target members 102a and 102b, and is adjusted so that a gap is formed when the two are stacked coaxially. A bonding material 103 is provided in the gap.
  • Each target member 102a, 102b is heated by ion irradiation during film formation by sputtering, and the temperature rises.
  • the base material 101 function as a coolant (heat sink) for each target member 102a, 102b.
  • the base material 101 it is possible to configure the base material 101 to have a hollow structure so that the coolant flows through the base material 101. Therefore, it is preferable to use a material having good conductivity and thermal conductivity as the substrate 101.
  • the base material 101 is preferably a metal that has good wettability with the bonding material 103 and can provide high bonding strength. From the above, it is preferable to use, for example, copper (Cu) or titanium (Ti), or a copper alloy, titanium alloy, or stainless steel (SUS) as a material constituting the substrate 101.
  • copper alloy an alloy mainly composed of copper (Cu) such as chromium copper can be applied.
  • Ti titanium
  • a light and rigid base material can be obtained.
  • the substrate 101 is not only formed of a single metal or a metal alloy, but may also be one in which a coating of other metal is provided on the surface of the metal substrate.
  • a metal film containing titanium (Ti), copper (Cu), silver (Ag), nickel (Ni), or the like may be formed.
  • the cylindrical sputtering target 100 does not irradiate ions on the entire surface of the target members 102a and 102b at the time of sputtering, but rotates while irradiating ions only on a part of the surfaces. There will be a temperature difference between the irradiated surface and its back surface. However, since the base material 101 has a cooling function, an increase in the temperature of the target members 102a and 102b can be suppressed, and the influence of thermal distortion due to the above-described temperature difference can also be suppressed.
  • the molten bonding material 103 is injected into the space between the base material 101 and the target members 102a and 102b, and then solidified through a cooling process to bond them together. Therefore, since it becomes the structure which inserts the base material 101 in the hollow part in the hollow cylindrical target members 102a and 102b, the space
  • the base material 101 has an anchor effect with respect to the bonding material 103 because there is a possibility that the adhesiveness between the bonding surfaces of the base material 101 and the bonding material 103 may be impaired due to volume shrinkage accompanying solidification of the bonding material 103.
  • the base material 101 is preferably roughened on the surface side in contact with the bonding material 103.
  • the surface area in contact with the bonding material 103 can be increased, and the adhesion between the base material 101 and the bonding material 103 can be increased.
  • the surface of the substrate 101 can be roughened by sandblasting or the like.
  • the surface roughness (Ra) of the surface of the base material 101 is larger, the surface area is larger and the adhesion is increased, but in the gap between the target members 102a and 102b, the surface roughness of the base material 101 is increased. It is desirable not to roughen the surface excessively.
  • the surface of the base material 101 is roughened in the gap, there is an advantage that the particles generated in the gap are firmly attached to prevent re-peeling.
  • the surface is excessively roughened, The material 101 itself is sputtered, and the components of the base material 101 may become impurities in the film or become particles and cause abnormal discharge.
  • the surface roughness (Ra) on the surface of the base material 101 that contacts the bonding material 103 is 1.8 ⁇ m or more (preferably 1.8 ⁇ m or more and 3.0 ⁇ m or less, more preferably 1.8 ⁇ m or more and 2. 5 ⁇ m or less).
  • the surface roughness (Ra) on the surface of the base material 101 in contact with the bonding material 103 is preferably set to 1.8 ⁇ m or more.
  • the upper limit is preferably set to 3.0 ⁇ m (more preferably 2.5 ⁇ m).
  • the bonding material 103 is provided between the base material 101 and the target members 102a and 102b.
  • the bonding material 103 preferably bonds the base material 101 and the target members 102a and 102b and has good heat resistance and thermal conductivity. Further, since it is placed under vacuum during sputtering, it is preferable that it has a characteristic that gas emission is small in vacuum.
  • the bonding material 103 has fluidity when the base material 101 and the target members 102a and 102b are bonded.
  • a low melting point metal material having a melting point of 300 ° C. or lower can be used as the bonding material 103.
  • a metal such as indium or tin, or a metal alloy material containing any one of these elements may be used.
  • indium or tin alone, an alloy of indium and tin, a solder alloy containing tin as a main component, or the like may be used.
  • each target member 102a, 102b is formed into a hollow cylindrical shape.
  • Each target member 102a, 102b has a thickness of at least several millimeters to several tens of millimeters, and the entire thickness portion can be used as a target member.
  • the base material 101 is inserted into the hollow portions of the target members 102 a and 102 b, and then both are joined by the joining material 103. That is, the outer diameter of the base material 101 is smaller than the inner diameter (the diameter of the hollow portion) of each of the target members 102a and 102b, both are arranged at a predetermined interval, and the bonding material 103 is filled so as to fill this gap. Is provided. In order to stably hold the target members 102a and 102b and the base material 101, the bonding material 103 is provided with no gap in the gap.
  • Each of the target members 102a and 102b has a cylindrical outer surface as a target surface, and a cylindrical inner surface that faces the base material 101 and comes into contact with the bonding material 103. For this reason, at the time of manufacture, the outer surface of each target member 102a, 102b may be formed into a smooth surface, and the inner surface of the cylinder may be roughened to enhance the adhesion.
  • the target members 102a and 102b are formed using various materials that can be formed by sputtering.
  • the target members 102a and 102b may be ceramics.
  • a metal oxide, a metal nitride, a sintered body of metal oxynitride, or the like can be used.
  • the metal oxide an oxide of a metal belonging to a typical element such as indium oxide, tin oxide, zinc oxide, or gallium oxide can be used.
  • a compound of tin oxide and indium oxide Indium Tin Oxide: ITO
  • zinc oxide Zinc Oxide: ZnO
  • a compound of indium oxide and zinc oxide Indium Zinc Oxide: IZO
  • indium oxide, zinc oxide and
  • a sintered body of a compound selected from a compound of gallium oxide Indium Gallium Zinc Oxide: IGZO
  • IGZO Indium Gallium Zinc Oxide
  • said specific example is an example and the sputtering target which concerns on this embodiment can use various sputtering materials as a target member.
  • a gap having a predetermined interval (preferably 1 mm or less, for example, 0.1 to 0.5 mm) is provided between the target member 102a and the target member 102b.
  • This gap is a safety measure for preventing the target members from colliding with each other, and as described above, the present inventors have found that the thin film re-deposited in this gap leads to the occurrence of arcing. .
  • the present inventors have determined that the surface roughness of the surface where the target member 102a and the target member 102b face each other (ie, the circular surface 104 shown in FIGS. 1 and 2) is 1.0 ⁇ m or less. Thus, it was found that the occurrence of arcing can be suppressed. That is, in the sputtering target 100 according to this embodiment, the surface roughness of the surface where the target member 102a and the target member 102b face each other is set to 1.0 ⁇ m or less (preferably 0.05 ⁇ m to 1.0 ⁇ m).
  • FIG. 3 is a cross-sectional view showing the vicinity of a gap between adjacent target members.
  • a schematic diagram in which the inside of the frame indicated by reference numeral 105 is enlarged is shown.
  • a gap of 0.2 to 0.5 mm is provided between the target member 102a and the target member 102b, and the surface 104 on which each target member faces is intentionally rough. It is processed to become. That is, each of the target members 102a and 102b has a circular surface 104 facing the adjacent target member at a predetermined interval when bonded to the base material 101, and the surface roughness (Ra ) Is 1.0 ⁇ m or less (preferably 0.05 ⁇ m or more and 1.0 ⁇ m or less).
  • the occurrence of arcing was confirmed in the range where the surface roughness (Ra) of the circular surface 104 of each target member 102a, 102b exceeded 1.0 ⁇ m, but it was 1.0 ⁇ m or less. It was not confirmed.
  • the reason why the occurrence of arcing is suppressed when the surface roughness (Ra) is 1.0 ⁇ m or less is that the adhesion of the redeposited film to the circular surface 104 is weakened due to the smooth surface, and thus the sputtered film This is considered to be because the abnormal discharge of plasma due to the peeling of the redeposited film is reduced as a result.
  • Ra 0.05 ⁇ m, which is so-called mirror finish, is preferable. It is not practical from the viewpoint of manufacturing cost to be less than 0.05 ⁇ m, and the surface roughness (Ra) may be 0.05 ⁇ m or more and 1.0 ⁇ m or less in order to improve the throughput of the device manufacturing process. preferable.
  • the surface roughness (Ra) of the circular surface 104 in each of the target members 102a and 102b is 1.0 ⁇ m or less (preferably 0.05 ⁇ m or more and 1.0 ⁇ m or less).
  • FIG. 4 is a process flow diagram showing a method for manufacturing the sputtering target 100 according to an embodiment of the present invention.
  • ITO indium tin oxide
  • raw materials constituting the target members 102a and 102b are prepared.
  • an indium oxide powder and a tin oxide powder are prepared (S401, S402).
  • the purity of these raw materials is usually 2N (99% by mass) or more, preferably 3N (99.9% by mass) or more, more preferably 4N (99.99% by mass) or more. If the purity is lower than 2N, the target members 102a and 102b contain a large amount of impurities, so that desired physical properties cannot be obtained (for example, the transmittance of the formed thin film is increased, the resistance value is increased, the particle size associated with arcing is reduced). Problem).
  • these raw material powders are pulverized and mixed (S403).
  • the raw material powder is pulverized and mixed using a dry method using balls and beads (so-called media) of zirconia, alumina, nylon resin, etc., media agitating mills using the balls and beads, and medialess containers
  • Wet methods such as a rotary mill, a mechanical stirring mill, and an airflow mill can be used.
  • the wet method is generally superior in pulverization and mixing ability compared to the dry method, it is preferable to perform the mixing using the wet method.
  • the raw material powders may be pulverized before mixing, or may be simultaneously pulverized by the powder processing during mixing.
  • the densification of the sintered compact used as the target members 102a and 102b can be achieved.
  • the amount of media (zirconia, etc.) used during pulverization also increases, and the impurity concentration in the target members 102a and 102b may increase. is there.
  • it is necessary to optimize the pulverization conditions while observing the balance between the high density of the sintered body and the impurity concentration in the target members 102a and 102b.
  • the raw material powder slurry is dried and granulated (S404).
  • the slurry may be rapidly dried using rapid drying granulation.
  • the rapid drying granulation may be performed by using a spray dryer and adjusting the temperature and air volume of hot air.
  • the mixture obtained by mixing and granulating as described above is pressure-molded to form a cylindrical shaped body (S405).
  • the target member 102a or 102b is formed into a suitable shape.
  • the molding process include mold molding, cast molding, injection molding, and the like.
  • CIP cold isostatic pressing
  • a rubber mold is filled with raw materials weighed to a predetermined weight. At this time, by filling the rubber mold while swinging or tapping, filling irregularities and voids of the raw material in the rubber mold can be eliminated. What is necessary is just to set suitably the pressure of shaping
  • the cylindrical molded body obtained in the molding process is sintered (S406).
  • An electric furnace is used for sintering.
  • the sintering conditions can be appropriately selected depending on the composition of the sintered body.
  • SnO 2 is 10 wt. % ITO can be sintered by placing it in an oxygen gas atmosphere at a temperature of 1500 to 1600 ° C. for 10 to 26 hours.
  • the sintering temperature is less than 1500 ° C., the density of the target members 102a and 102b is reduced.
  • the temperature exceeds 1600 ° C. the electric furnace and the furnace material are greatly damaged and frequent maintenance is required, so that the work efficiency is remarkably lowered.
  • the pressure during sintering may be atmospheric pressure, or a reduced pressure or pressurized atmosphere.
  • the temperature rising rate of the electric furnace during sintering is preferably 300 ° C./hour or less, more preferably 180 ° C./hour or less.
  • the temperature lowering rate of the electric furnace during sintering is preferably 5 ° C./hour or less. Note that the rate of temperature increase or the rate of temperature decrease may be adjusted to change stepwise.
  • the formed cylindrical sintered body is machined into a desired cylindrical shape using a machining machine such as a surface grinding machine, a cylindrical grinding machine, a lathe, a cutting machine, or a machining center (S407).
  • a machining machine such as a surface grinding machine, a cylindrical grinding machine, a lathe, a cutting machine, or a machining center (S407).
  • the machining performed here is a step of processing a cylindrical sintered body to have a desired shape and surface roughness, and finally, the target members 102a and 102b are formed through this step.
  • the surface roughness (Ra) is preferably 0.5 ⁇ m or less.
  • the circular surfaces 104 of the target members 102a and 102b are ground using a grindstone so that the surface roughness (Ra) of the circular surfaces 104 is 1.0 ⁇ m or less (preferably 0. 05 ⁇ m or more and 1.0 ⁇ m or less).
  • Ra surface roughness
  • the machined cylindrical sintered body (that is, the target members 102a and 102b) is bonded to the substrate 101 (S408).
  • the target members 102a and 102b are bonded to a cylindrical base material 101 called a backing tube using the bonding material 103 as an adhesive, as shown in FIGS.
  • the base material 101 is inserted into the hollow portions of the hollow cylindrical target members 102a and 102b, and the molten bonding material 103 is injected into the space between the base material 101 and the target members 102a and 102b. Then, the two are joined by solidifying through a cooling process.
  • the cylindrical sputtering target 100 according to this embodiment can be obtained through the above steps.
  • Example 3 The inventors prepared target members using three different materials (ITO, IZO, and IGZO), and investigated the relationship between the surface roughness and the occurrence of arcing. The results are shown in Tables 1 to 3. Each experimental condition was as follows: target thickness: 9 mm, sputtering pressure: 0.6 Pa, Ar (argon) flow rate: 300 sccm, input power: 4 kW / m, sputtering time: 70 hours. Moreover, since it was target durability evaluation at the time of performing continuous discharge, discharge was performed without setting the substrate or the like.
  • the surface roughness (Ra) was measured according to ANSI standards using a small surface roughness measuring machine (Surf Test SJ-301: manufactured by Mitutoyo Corporation). The surface roughness was measured at six locations on the end surface of the target member at 60 ° intervals (12 locations per target member), and the weighted average value of all measured values was the surface roughness of the target member.
  • the surface roughness (Ra) of the circular surface of each target member in the plurality of target members constituting the cylindrical sputtering target is 1.0 ⁇ m or less (preferably, 0 .05 ⁇ m or more and 1.0 ⁇ m or less), it was found that the occurrence of arcing during sputtering can be reduced.
  • SYMBOLS 100 Cylindrical type sputtering target 101: Base material 102a, 102b: Target member 103: Joining material 104: Circular surface 105: Frame line
  • S401 The process of preparing an indium oxide powder
  • S402 The process of preparing a tin oxide powder
  • S403 Raw material Step of crushing and mixing powder
  • S404 Step of drying and granulating raw material powder slurry
  • S405 Step of forming cylindrical shaped body
  • S406 Step of sintering cylindrical shaped body
  • S407 Desired cylindrical shape
  • Step S408 Step of bonding cylindrical sintered body to base material

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Abstract

La présente invention vise à réduire l'apparition d'un arc électrique au cours d'un procédé de production, ce qui permet d'améliorer le rendement du procédé de production. La cible de pulvérisation cathodique selon l'invention est caractérisée en ce qu'elle comprend une pluralité d'éléments de cible qui faits à partir d'une céramique et sont liés à une base qui est faite à partir d'un métal, un matériau de liaison étant interposé entre ceux-ci, ledit matériau de liaison fait à partir d'un métal à point de fusion bas qui a un point de fusion inférieur ou égal à 300 °C. Ladite cible de pulvérisation cathodique est également caractérisée en ce que : une surface de la base, avec laquelle le matériau de liaison est en contact, présente une rugosité de surface (Ra) supérieure ou égale à 1,8 µm ; et chacun de la pluralité d'éléments de cible présente une forme cylindrique creuse, tout en ayant une surface circulaire qui fait face à un élément cible adjacent à une distance prédéterminée si la pluralité d'éléments de cible sont liés à la base de manière à entourer la surface circonférentielle externe de la base ; et la surface circulaire présente une rugosité de surface (Ra) inférieure ou égale à 1,0 µm.
PCT/JP2016/053897 2015-02-13 2016-02-10 Cible de pulvérisation cathodique et son procédé de production WO2016129622A1 (fr)

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JP6220091B1 (ja) * 2017-03-22 2017-10-25 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
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
JP2020143327A (ja) * 2019-03-05 2020-09-10 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
JP7158316B2 (ja) 2019-03-05 2022-10-21 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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