WO2012029363A1 - インジウムターゲット及びその製造方法 - Google Patents
インジウムターゲット及びその製造方法 Download PDFInfo
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- WO2012029363A1 WO2012029363A1 PCT/JP2011/061682 JP2011061682W WO2012029363A1 WO 2012029363 A1 WO2012029363 A1 WO 2012029363A1 JP 2011061682 W JP2011061682 W JP 2011061682W WO 2012029363 A1 WO2012029363 A1 WO 2012029363A1
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- indium
- grain size
- target
- indium target
- crystal grain
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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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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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
- 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
-
- 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
- H01J37/3426—Material
Definitions
- the present invention relates to a sputtering target and a manufacturing method thereof, and more particularly to an indium target and a manufacturing method thereof.
- Indium is used as a sputtering target for forming a light absorption layer of a Cu—In—Ga—Se (CIGS) thin film solar cell.
- CGS Cu—In—Ga—Se
- Patent Document 1 describes a method in which an indium thin film is formed on a backing plate, and then indium is poured onto the thin film and cast so as to be integrated with the backing plate.
- Patent Document 2 describes a predetermined amount of indium raw material is charged and dissolved in a heated mold, indium oxide floating on the surface is removed, and cooled to obtain an ingot.
- an object of the present invention is to provide an indium target capable of achieving a high sputtering rate while suppressing the occurrence of abnormal discharge, and a method for manufacturing the indium target.
- the inventor has intensively studied to solve the above problems, and indium solid obtained by adding ultrasonic vibration to the molten indium solution at least immediately before solidification in the solidification process during melting and casting of the indium ingot. It was found that the crystal grain size of the ingot can be significantly reduced. Although it is not intended that the present invention be limited by theory, this is due to the fact that a large number of crystal nuclei are formed by ultrasonic vibration, and the gaps between crystal grains are reduced, and the coarsening of crystal grains is suppressed. It is considered a thing.
- the average grain size of the whole is 10 mm or less, the crystal grains observed from a cross section parallel to the plate thickness direction, the average grain in the direction perpendicular to the plate thickness direction
- the indium target has a ratio of the average particle diameter in the direction parallel to the plate thickness direction to the diameter of 0.7 to 1.1, and a void having a hole diameter of 50 ⁇ m or more is 1 piece / cm 3 or less.
- the indium target according to the present invention has a maximum crystal grain size of 20 mm or less.
- an indium target manufacturing method including a step of melting and casting an indium raw material, wherein at least ultrasonic vibration is applied when the indium raw material is solidified.
- cooling is performed at a cooling rate of 3 to 70 ° C./min during melt casting.
- an indium target capable of maintaining a high sputter rate while suppressing the occurrence of abnormal discharge can be obtained. Further, in the present invention, since an impurity such as a crystal grain refining agent is not added to indium, there is also an effect that the target can be easily recycled.
- the average crystal grain size of the entire indium target can be controlled to 10 mm or less.
- the average crystal grain size is about 40 mm or more. And get bigger. With such a large crystal grain size, the film formation rate of sputtering is reduced.
- the growth of crystal grains can be suppressed even at such a slow cooling rate by adding ultrasonic vibration during solidification.
- the addition of ultrasonic vibration also has an effect of suppressing the void amount.
- the total average crystal grain size is preferably 1 to 6 mm, more preferably 1 because there is a limit to reducing the crystal grain size. ⁇ 3 mm.
- the indium target according to the present invention can be manufactured without performing cold rolling after melt casting, so that the crystal grains observed from a cross section parallel to the plate thickness direction are perpendicular to the plate thickness direction.
- the ratio of the average grain size in the direction parallel to the plate thickness direction to the average grain size in the direction (hereinafter also referred to as “cross-sectional aspect ratio”) is close to 1, that is, the crystal grains are not flat.
- the cross-sectional aspect ratio is 0.7 to 1.1, typically 0.8 to 1.0.
- the cross-sectional aspect ratio is measured by the following method. With reference to FIG. 1, it cut
- FIG. 1 the exposed cut surface 12 is lightly etched with a weak acid, or carbon powder is rubbed on the cut surface 12 to make the crystal grain boundary easy to see, and then, by measuring any 20 crystal grains as objects of measurement, The average particle size (a) in the direction perpendicular to the direction x and the average particle size (b) in the direction y parallel to the plate thickness direction are calculated to determine the cross-sectional aspect ratio (b / a).
- Average grain size in the direction perpendicular to the plate thickness direction is measured when the longest line perpendicular to the plate thickness direction that can be surrounded by each crystal grain is the grain size in the direction perpendicular to the plate thickness direction of each crystal grain. It is an average value about the target crystal grain.
- the average grain size in the direction parallel to the plate thickness direction is measured when the longest line segment parallel to the plate thickness direction that can be surrounded by each crystal grain is the grain size in the direction parallel to the plate thickness direction of each crystal grain. It is an average value about the target crystal grain.
- the indium target according to the present invention has a maximum crystal grain size of 20 mm or less.
- the maximum crystal grain size is preferably 15 mm or less, more preferably 10 mm or less, for example, 5 to 10 mm.
- the maximum crystal grain size of the indium target is measured by the following method.
- the number of voids having a pore diameter of 50 ⁇ m or more is 1 / cm 3 or less. It is desirable to minimize the gaps present in the target, particularly large gaps having a pore diameter of 50 ⁇ m or more, because they cause abnormal discharge during sputtering. According to the present invention, since the effect of suppressing crystal grain coarsening due to ultrasonic vibration works, cooling can be performed at a slow cooling rate that suppresses the generation of voids during melting and casting of ingots. It is possible to prevent both occurrences.
- the voids having a pore diameter of 50 ⁇ m or more are preferably 0.5 pieces / cm 3 or less, more preferably 0.3 pieces / cm 3 or less, for example, 0 to 0.3 pieces / cm 3 .
- the number ratio of voids having a pore diameter of 50 ⁇ m or more is measured with an electronic scanning ultrasonic flaw detector.
- the ratio of the number of voids is obtained from the volume of the target to be measured.
- the hole diameter is defined by the diameter of the smallest circle surrounding the hole of the image image.
- indium which is a raw material is dissolved and poured into a mold.
- the raw material indium to be used preferably has a high purity because the conversion efficiency of a solar cell produced from the raw material is reduced when impurities are contained, for example, 99.99 mass.
- a raw material with a purity of at least% can be used. Then, it cools to room temperature and forms an indium ingot. From the viewpoint of encouraging the generation of a large number of crystal nuclei during the initial crystallization, it is necessary to add ultrasonic waves at least during solidification of the indium raw material.
- the temperature is gradually decreased from the melting temperature of indium, and is started when the temperature is at least directly above 156 ° C. (eg, 157 to 160 ° C.) which is the melting point of indium.
- Ultrasonic vibration may be added at a time when the temperature is higher than that, that is, when the indium is in a molten state, but it does not make much sense. It is important to add ultrasonic vibration just before solidification. Further, the addition may be continued until the indium solidification is completed, but this is not necessary. For example, when the indium temperature is lowered to about 159 ° C., typically to about 157 ° C., the ultrasonic wave is used. The addition of vibration may be stopped.
- the ultrasonic vibration is performed using a device based on the principle that an electrostrictive vibrator vibrates at a high frequency.
- the method of applying ultrasonic vibration to the indium melt just before solidification by amplifying the vibration of the vibrator with an magnifying device and transmitting it to the ultrasonic vibration horn and inserting this ultrasonic vibration horn directly into the molten indium is indium. It is preferable because ultrasonic vibration can be directly added inside.
- Cooling at the time of solidification may be natural cooling by air (about 10 ° C./min), but by cooling at a slow cooling rate, for example, 9 ° C./min or less, preferably 8 ° C./min or less, there are voids in the ingot An effect of further suppressing the generation is obtained. However, if it is too slow, the effect of suppressing crystal coarsening due to ultrasonic vibration cannot be obtained sufficiently, and therefore it is preferably 3 ° C./min or more, more preferably 5 ° C./min or more. On the other hand, when importance is attached to preventing the growth of crystal grain size, the cooling rate can be increased. For example, it can be set to 20 ° C./min or more, preferably 50 ° C./min.
- the increase rate of the void amount is smaller than the increase rate of the cooling rate. Therefore, by setting the cooling rate high, it is possible to achieve a high level of high sputtering rate and suppression of abnormal discharge.
- the cooling rate can be adjusted by heating the mold with a heater or the like when reducing the cooling rate, and conversely when increasing the cooling rate, such as water cooling by supplying cooling water around the mold. Can be done by the method.
- the cooling rate is calculated by (indium melting temperature ⁇ 25 ° C.) / (Time from the start of cooling until the indium temperature decreases from the melting temperature to 25 ° C.). After melt casting, shape processing and surface polishing are performed as necessary to obtain an indium target.
- the thickness of the target is not particularly limited and may be appropriately set according to the sputtering apparatus to be used, the film formation use time, etc., but is usually about 3 to 20 mm, and typically about 5 to 10 mm.
- the indium target thus obtained can be suitably used as a sputtering target for preparing a light absorption layer for a CIGS thin film solar cell.
- Indium raw material (purity 5N) was dissolved at 170 ° C., and this solution was poured into a cylindrical mold having a diameter of 250 mm and a height of 7 mm, and cooled to the room temperature (25 ° C.) at the cooling rate shown in Table 1. An indium ingot was produced. At this time, in the inventive example, addition of ultrasonic vibration was started at 160 ° C. just above the solidification temperature of indium. Ultrasonic vibration uses a device based on the principle that an electrostrictive vibrator vibrates at a high frequency, and the vibration of the vibrator is amplified by an enlarger and then transmitted to the ultrasonic vibration horn. The ultrasonic vibration was given to the indium melt immediately before solidification.
- the indium targets of the inventive example and the comparative example were sputtered by an ANELVA SPF-313H apparatus with an ultimate vacuum pressure in the chamber before sputtering start of 1 ⁇ 10 ⁇ 4 Pa and argon gas flowed at 5 sccm.
- the pressure was 0.5 Pa
- the sputtering power was 650 W
- Corning # 1737 glass was used as a substrate for 5 minutes without heating the substrate.
- Table 2 lists the sputtering rate and the number of abnormal discharges during sputtering. The sputtering rate was calculated from the film formation time and the result of film thickness measurement using a step gauge, and the number of abnormal discharges was measured by a visual method.
- Comparative Example 1 was an example of natural cooling without ultrasonic vibration, and the average crystal grain size was excessive. As a result, the sputter rate became slow. Invention Example 1 was naturally cooled in the same manner as Comparative Example 1, but the addition of ultrasonic vibration reduced the average crystal grain size and improved the sputtering rate. In Comparative Example 2, the average crystal grain size was reduced by high-speed cooling, but the amount of voids increased because no ultrasonic vibration was added. As a result, the number of abnormal discharges increased. In Invention Example 2, since the cooling rate was slightly lower than that in Invention Example 1, the average particle size was slightly larger, but since ultrasonic vibration was added, the average crystal particle size was smaller than in Comparative Example 1.
- Invention Example 3 is an example in which the sputtering rate is increased by increasing the cooling rate. Although the cooling rate was quite high, the increase in void volume was suppressed and no abnormal discharge was observed.
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Abstract
Description
特公昭63-44820号公報(特許文献1)にはバッキングプレートにインジウムの薄膜を形成した後、該薄膜の上にインジウムを流し込み鋳造することでバッキングプレートと一体に形成する方法が記載されている。
また、特開2010-24474号公報(特許文献2)では、加熱された鋳型に所定量のインジウム原料を投入して溶解し、表面に浮遊する酸化インジウムを除去し、冷却してインゴットを得、得たインゴット表面を研削してインジウムターゲットを得るに際し、所定量のインジウム原料を一度に鋳型に投入せずに複数回に分けて投入し、都度生成した溶湯表面の酸化インジウムを除去し、その後、冷却して得られたインゴットを表面研削して得る方法が記載されている。
その結果、異常放電の原因となるターゲット内の空隙発生を防止するために溶解鋳造時の冷却速度を遅くしても、結晶粒の粗大化が抑制されるため、高いスパッタレートをもつターゲットが得られる。
A=2(s/π)1/2
板厚方向に直角方向の平均粒径は、各結晶粒が取り囲むことの出来る板厚方向に直角な最も長い線分を各結晶粒における板厚方向に直角方向の粒径としたときの、測定対象となる結晶粒についての平均値である。
板厚方向に平行方向の平均粒径は、各結晶粒が取り囲むことの出来る板厚方向に平行な最も長い線分を各結晶粒における板厚方向に平行方向の粒径としたときの、測定対象となる結晶粒についての平均値である。
上記のインジウムターゲット全体の平均粒径測定時の測定対象面積内の結晶粒の中で最大の結晶粒の面積(smax)について、結晶粒を球と仮定して、最大粒径(B)を以下の式で算出する。
B=2(smax/π)1/2
冷却速度の調整は、冷却速度を小さくする場合は、鋳型をヒーター等で加熱保温することで、逆に、冷却速度を大きくする場合は、鋳型の周辺に冷却水を供給することによる水冷等の方法で行うことができる。ここでの冷却速度は、(インジウムの溶解温度-25℃)/(冷却開始後、インジウムの温度が溶解温度から25℃に低下するまでの時間)で計算される。溶解鋳造後、必要に応じて形状加工や表面研磨してインジウムターゲットとする。
A~Cの測定には表面研磨用に市販のカーボン粉を使用し、目視観察により測定した。
Dの測定には日本クラウトクレーマー株式会社製の電子走査式超音波探傷システムPA-101を使用した。
結果を表1に示す。
A:全体の平均結晶粒径
B:最大結晶粒径
C:結晶粒の断面アスペクト比
D:孔径50μm以上の空隙の個数割合
スパッタレートは、成膜時間と段差計による膜厚測定の結果から算出し、異常放電の回数は目視の方法により測定した。
比較例1は超音波振動なしで自然冷却した例であり、平均結晶粒径が過大となった。その結果、スパッタレートが遅くなった。
発明例1は比較例1と同様に自然冷却したが、超音波振動を付加したことで、平均結晶粒径が小さくなり、スパッタレートが向上した。
比較例2では、高速冷却により平均結晶粒径を小さくしたが、超音波振動を付加していないために空隙の量が増加した。その結果、異常放電の回数が増えた。
発明例2では、冷却速度を発明例1より少し小さくしたために、平均粒径はやや大きくなったが、超音波振動を付加しているため、比較例1よりも平均結晶粒径は小さい。
比較例3は超音波振動を付加したものの、冷却速度を遅くし過ぎたことで平均結晶粒径が過大となった例である。
発明例3は冷却速度を高めることでスパッタレートを高くした例である。冷却速度はかなり高いが空隙量の増加は抑制され、異常放電は見られなかった。
11 中心軸
12 切断面
x 直角方向
y 平行方向
Claims (4)
- 全体の平均結晶粒径が10mm以下であり、板厚方向に平行な断面から観察した結晶粒について、板厚方向に直角方向の平均粒径に対する板厚方向に平行方向の平均粒径の比が0.7~1.1であり、孔径50μm以上の空隙が1個/cm3以下のインジウムターゲット。
- 最大結晶粒径が20mm以下である請求項1に記載のインジウムターゲット。
- インジウム原料を溶解鋳造する工程を含むインジウムターゲットの製造方法であって、少なくともインジウム原料の凝固時に超音波振動を付加するインジウムターゲットの製造方法。
- 溶解鋳造時の冷却速度を3~70℃/分として冷却する請求項3に記載のインジウムターゲットの製造方法。
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
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US13/704,086 US9490108B2 (en) | 2010-09-01 | 2011-05-20 | Indium target and method for manufacturing same |
EP11821381.8A EP2612953A4 (en) | 2010-09-01 | 2011-05-20 | INDUSTRIAL OBJECT AND MANUFACTURING METHOD THEREFOR |
KR1020127013157A KR101202232B1 (ko) | 2010-09-01 | 2011-05-20 | 인듐 타깃 및 그 제조 방법 |
CN2011800049830A CN102656291B (zh) | 2010-09-01 | 2011-05-20 | 铟靶材及其制造方法 |
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JP2010-196213 | 2010-09-01 | ||
JP2010196213A JP4948634B2 (ja) | 2010-09-01 | 2010-09-01 | インジウムターゲット及びその製造方法 |
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WO2012029363A1 true WO2012029363A1 (ja) | 2012-03-08 |
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US (1) | US9490108B2 (ja) |
EP (1) | EP2612953A4 (ja) |
JP (1) | JP4948634B2 (ja) |
KR (1) | KR101202232B1 (ja) |
CN (1) | CN102656291B (ja) |
TW (1) | TW201211284A (ja) |
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US9758860B2 (en) | 2012-01-05 | 2017-09-12 | Jx Nippon Mining & Metals Corporation | Indium sputtering target and method for manufacturing same |
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JP5140169B2 (ja) | 2011-03-01 | 2013-02-06 | Jx日鉱日石金属株式会社 | インジウムターゲット及びその製造方法 |
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US9758860B2 (en) | 2012-01-05 | 2017-09-12 | Jx Nippon Mining & Metals Corporation | Indium sputtering target and method for manufacturing same |
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US9922807B2 (en) | 2013-07-08 | 2018-03-20 | Jx Nippon Mining & Metals Corporation | Sputtering target and method for production thereof |
Also Published As
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US20130153414A1 (en) | 2013-06-20 |
US9490108B2 (en) | 2016-11-08 |
JP2012052193A (ja) | 2012-03-15 |
CN102656291B (zh) | 2013-11-06 |
KR101202232B1 (ko) | 2012-11-16 |
EP2612953A4 (en) | 2014-01-22 |
JP4948634B2 (ja) | 2012-06-06 |
TWI372185B (ja) | 2012-09-11 |
KR20120079149A (ko) | 2012-07-11 |
CN102656291A (zh) | 2012-09-05 |
TW201211284A (en) | 2012-03-16 |
EP2612953A1 (en) | 2013-07-10 |
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