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WO2000040769A1 - Cible de pulverisation cathodique - Google Patents

Cible de pulverisation cathodique Download PDF

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Publication number
WO2000040769A1
WO2000040769A1 PCT/JP1999/006566 JP9906566W WO0040769A1 WO 2000040769 A1 WO2000040769 A1 WO 2000040769A1 JP 9906566 W JP9906566 W JP 9906566W WO 0040769 A1 WO0040769 A1 WO 0040769A1
Authority
WO
WIPO (PCT)
Prior art keywords
sputtering target
target
sputtering
less
ceramic
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP1999/006566
Other languages
English (en)
Japanese (ja)
Inventor
Koichi Nakashima
Yoshikazu Kumahara
Keiichi Ishizuka
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Eneos Corp
Original Assignee
Japan Energy Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Japan Energy Corp filed Critical Japan Energy Corp
Publication of WO2000040769A1 publication Critical patent/WO2000040769A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • 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
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics

Definitions

  • the present invention is a sputtering target manufactured by a powder metallurgy method made of ceramics such as "indium tin oxide" called IT ⁇ , which generates a small amount of nodules on the target during film formation by sputtering. It relates to a sputtering target in which abnormal discharge and particles are unlikely to occur. Background art
  • “Indium tin oxide” film called “ ⁇ ⁇ ⁇ film” has high conductivity and visible light transmission
  • a sputtering target composed of ceramics having the same composition is generally used, and an oxide powder is usually used as the ceramic sputtering target.
  • the material is integrated by powder metallurgy and densified.
  • a target composed of indium oxide and tin oxide is used when forming an I-O film, and a powder mixture of indium oxide and tin oxide or a dopant is used for this ITO target.
  • the added powder mixture is press-molded at room temperature, sintered in air at 125 ° C to 160 ° C, and then subjected to further machining such as surface grinding.
  • Nodules increase in number and increase as the sputtering time increases, gradually covering the target surface. Nodules have poor conductivity compared to other parts. If the nodules are generated in a large amount, abnormal discharge (arcing) occurs frequently during sputtering, particles are generated in the IT ⁇ film, and the sputtering is maintained. There was a problem that it was difficult to continue.
  • this nodule is caused by the adhesion of the initial particles to the target, but in either case, both increase rapidly with the progress of film formation by sputtering, and abnormal discharge occurs. Tend to increase.
  • the generation of nodules is a problem that appears particularly strongly in ITO sputtering targets for forming transparent conductive films. If the nodules increase abnormally on the target surface, the sputtering operation is temporarily stopped to generate on the target surface. Regeneration treatment, such as scraping off the nodules, has been performed, but such interruption of sputtering has been a factor that significantly reduces productivity in continuous operation. And while this regeneration work itself is simple, it requires a certain amount of skill and time, and is inevitably complicated.
  • An ITO sputtering target is generally obtained by grinding a sintered body with a surface grinder or the like, but grinding powder of I ⁇ adhering to the target surface is generated by nodules. It is presumed to be one of the raw causes. Therefore, it is expected that reducing the amount of ITO grinding powder could reduce the amount of nodules generated. In addition, it was difficult to know and to reduce the amount of ITO grinding powder to its limit on the scale of actual operation.
  • the present invention remarkably improves the above-mentioned problems by adjusting the roughness of the target surface, and more preferably adjusts the density, bulk resistance value and average crystal grain size of the target within an appropriate range to clean the surface.
  • Ceramic sputter which suppresses the generation of nodules during film formation by sputtering and prevents abnormal discharge and particles. Provide the target.
  • the present invention is a.
  • a sputtering target which is a ceramic sputtering target manufactured by a powder metallurgy method, wherein the sputtering target has a center line average roughness Ra of 0.1 ⁇ or less.
  • “Surface center line surface roughness Ra” refers to the surface roughness defined by JIS B0601. Needless to say, in the ceramic sputtering target according to the present invention, the center line surface roughness Ra of the sputter surface is 0.1 ⁇ or less, preferably 0.05 ⁇ or less, more preferably 0.005 / Adjusted to m or less.
  • the “sintering of the compression-molded oxide powder mixture” must be performed using a high oxygen content of 0.1 MPa (1 atm) or more.
  • the density of the target can be increased to a level exceeding 7 gZcm 3 (about 97 to 99% of the theoretical density), and the effect of further suppressing the generation of nodules is brought about.
  • the bulk resistance of the target is also closely related to the sputtering workability, and if the density and the Banolek resistance are adjusted to specific areas, the stability of the film forming operation is further improved, and the high performance IT ⁇ The formability of the film is further improved.
  • the density D of the IT sputtering target is less than 6.70 g / cm 3 , the above effect cannot be sufficiently obtained, while the density is increased to a region exceeding 7.30 g / cm 3 because The sintering method in a high oxygen partial pressure atmosphere is also very difficult, resulting in cost disadvantages.
  • the bulk resistance value p of the ITO sputtering target tends to greatly depend on the density D, and tends to sharply decrease as the density increases.
  • Balta resistance the less the occurrence of peaking during sputtering is preferable.
  • P ⁇ 0.10761 D Achieving +0.66 can be achieved in a high oxygen partial pressure atmosphere.
  • the sintering method is also very difficult.
  • the Balta resistance value p of the ITO sputtering target is in the range of p> —0.067 6D + 0.887, not only the occurrence of abnormal discharge during sputtering increases, but also the stability of the film forming operation is impaired, The phenomenon that the film forming rate becomes unstable and the film forming rate decreases with the progress of sputtering becomes remarkable.
  • the density and bulk resistance of the ITO sputtering target can be adjusted by adjusting the pressing pressure during press molding of the raw material powder, the atmosphere during sintering (oxygen partial pressure), and the sintering temperature. is there.
  • the average crystal grain size of the ITO sputtering target is 4 ⁇ or more, the amount of nodules generated during sputtering cannot be suppressed to a satisfactory level, and abnormal discharge cannot be sufficiently suppressed, and the desired film formation operation and film quality can be improved. Can not secure.
  • a close examination of the ITO sputtering target with an average grain size of 4 ⁇ m or more reveals that there are many voids with an average diameter of 10 ⁇ m or more in the target.
  • the average crystal grain size of the ITO sputtering target is particularly reduced to less than 4 ⁇ , nodule generation and abnormal discharge on the target surface are drastically reduced, and the gas adsorption amount is also reduced. Extremely small, significantly improving film forming operability and film quality.
  • the average crystal grain size of the ITO sputtering target was limited to less than 4 ⁇ .
  • the average crystal grain size will be increased after sintering. Although less than 4 m cannot be achieved, the average particle size is smaller, By sintering with the holding time set to about 10 hours or less or 0, it is possible to achieve an average grain size of less than 4 / im (the maximum grain size at this time is only 8 m) become.
  • Figure 1 shows the integrated power (Wh / cm 2 ) and the nodule coverage. It is a figure (graph) which shows the relationship of / 0 .
  • Figure 2 is an enlarged view of up integrated electricity 40 Wh / cm 2 in FIG. 1 (graph).
  • Fig. 3 is a graph (graph) showing the relationship between the accumulated power (WhZcm 2 ) and the number of abnormal discharges (times).
  • Fig. 4 is an enlarged view (graph) up to the integrated electric energy 4 OWhZcni 2 in Fig. 3.
  • Figure 5 is a diagram showing the relationship between integrated electricity (WhZcm 2) and particle generation number (X 10 2 Quai Zm m 2) (graph).
  • Figure 6 is an enlarged view of up integrated electricity 4 OWhZcm 2 in FIG. 5 (graph).
  • ITO sputtering target for example, indium oxide powder having an average particle size of 2 m and tin oxide powder having the same particle size are weighed so as to have a weight ratio of 90:10, and a molding binder is added thereto. Mix evenly. Next, the mixed powder is filled in a mold, pressed, and sintered at a high temperature.
  • the sintered body of the ITO sputtering target thus obtained is ground with a surface grinder to obtain an ITO target material.
  • the sputter surface of the ITO sputtering target is mirror-finished to have an average surface roughness Ra of 0.1 // m or less, preferably 0.05 m or less, more preferably 0.005 ⁇ or less. .
  • polishing techniques such as mechanical polishing, chemical polishing, and mechanochemical polishing (combination of mechanical polishing and chemical polishing) can be used.
  • abrasive is diamond It can be obtained by wrapping instead of pasting.
  • polishing method There is no particular limitation on such a polishing method, and other polishing methods may be employed as long as the average surface roughness Ra of the present invention can be achieved.
  • the adhering particles (IT ⁇ ground powder) with an average diameter of 0.2 m or more in the 1 mm XI mm area (1 mm square surface) of the sputtered surface of the IT ⁇ sputtering target , The number of which can be 50 or less.
  • the ⁇ average diameter '' means that the attached particles themselves are not circular but have an irregular shape in many cases. I do.
  • the I ⁇ sputtering target obtained by the above operation can significantly reduce the nodule coverage, particles, and abnormal discharge.
  • the sputtering operation is temporarily stopped, and the nodules generated on the target surface are scraped off and regenerated. Even if the treatment is no longer necessary or necessary, the number of such treatments can be reduced, and the productivity can be significantly increased. Examples and comparative examples
  • tin oxide powder having the same particle size as indium oxide powder having an average particle size of 2 / xm was weighed so as to have a weight ratio of 90:10, and this was used for molding.
  • the binder was added and mixed uniformly.
  • this raw material mixed powder was uniformly filled in a mold (165 WX 520 L), and was molded under a pressure of 78.5 MPa (800 kgf / cm 2 ) using a hydraulic press.
  • the compact thus obtained was sintered at 1640 ° C. for 7 hours in a pure oxygen gas atmosphere of 0.1 IMP a (1 atm: absolute pressure) in a high-pressure low-pressure sintering furnace.
  • the sputtered surface of the sintered body thus obtained was ground with a surface grinder, and the sides were cut with a diamond cutter to obtain an ITO target material.
  • the density of this IT target material was 7.05 g / cm 3 .
  • this ITO target material is bonded to a backing plate.
  • polishing was performed with a fixed abrasive polisher (polish liquid: water) to # 2000 or more to obtain an average surface roughness Ra of 0.05 ⁇ .
  • lapping was performed by changing the abrasive material to diamond paste to obtain an average surface roughness Ra of 0.005 m. .
  • the sputter surface was blown with air, and ultrasonic cleaning was performed for 3 minutes by oscillating 12 types of frequencies at 25 kHz intervals in a frequency range of 25 to 300 kHz.
  • the respective frequencies are 25, 50, 75, 100, 125, 150, 175, 200, 225, 250, 275, 300 kHz.
  • it was air-dried to obtain an IT sputtering target of Examples 1 and 2 of the present invention.
  • a sputtering test was performed on the sputtering target under the following conditions.
  • Sputtering was performed under the above conditions, and changes in the nodule coverage, the number of abnormal discharges, and the number of particles were observed for each integrated power (WhZcm 2 ).
  • Table 1 shows the results of the nodule coverage.
  • “nodule coverage” is the percentage of “nodule area Z erosion area” on the sputtering target surface. Also, this table
  • FIG. 1 To make the results easier to understand, they are shown in Figures 1 and 2.
  • the vertical axis shows the nodule coverage%, and the horizontal axis shows the integrated electric energy (WhZcm 2 ).
  • FIG. 2 is an enlarged view of FIG. 1 in which the integrated power amount is between 0 and 4 OWh / cm 2 .
  • Table 2 shows the results of the abnormal discharge occurrence frequency.
  • the number of times of occurrence of abnormal discharge indicates the number of times of integration at each integrated power amount (Wh / cm 2 ).
  • FIGS. 3 and 4 show the results in Table 2 easier to understand.
  • the vertical axis shows the number of abnormal discharge occurrences (times), and the horizontal axis shows the integrated electric energy (WhZ cm 2 ).
  • FIG. 4 is an enlarged view of FIG. 3 in which the integrated electric energy is between 0 and 4 OWh / cm 2 .
  • Table 3 shows the results of the number of generated particles.
  • the number of generated particles is the number of particles of a size larger than 0.1 observed on the film surface when a film with a thickness of 1 ⁇ is formed at each integrated power (Wh / cm 2 ). Is shown. Similarly, to make the results of Table 3 easier to understand, they are shown in Figs. 5 and 6.
  • the vertical axis Party cycle generation number (X 10 2 Ke / mm 2), the horizontal axis represents the cumulative amount of power (Wh / cm 2).
  • FIG. 6 is an enlarged view of FIG. 5 in which the integrated electric energy is between 0 and 4 OWh / cm 2 .
  • Examples 1 and 2 of the present invention and Comparative Examples 1 and 2 were compared from the initial stage of sputtering. There is a large difference in the number of abnormal discharge occurrences, and Examples 1 and 2 It can be seen that the number of generated particles is suppressed.
  • the characteristics of the example are excellent, but the superiority is particularly remarkable in the target integrated initial electric energy (40 WhZcm 2 or less).
  • the density, the Balta resistance value and the average crystal grain size of the ITO sputtering target are adjusted to appropriate ranges, a more uniform and dense sputtering surface can be obtained, so that the effect of the present invention can be further enhanced.
  • the multi-oscillation ultrasonic cleaning method in which the sputter surface of the ITO sputtering target used in the embodiment of the present invention oscillates multiple times at a frequency of 25 to 300 kHz is effective in suppressing nodules, abnormal discharge, and particles. It has a great effect. The combined use of this is even more effective.
  • the film is formed by sputtering. It is possible to obtain an ITO sputtering target for forming a transparent conductive film, which suppresses the generation of nodules and is resistant to abnormal discharge and particles.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Structural Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Physical Vapour Deposition (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

L'invention concerne une cible de pulvérisation cathodique sur laquelle peu de nodules se forment au cours de la formation du film par pulvérisation cathodique, et qui ne produit guère de décharges et de particules anormales. La surface à pulvériser présente une rugosité moyenne de surface Ra égale ou inférieure à 0,1 νm, de préférence égale ou inférieure à 0,05 νm, ou idéalement égale ou inférieure à 0,005 νm.
PCT/JP1999/006566 1998-12-28 1999-11-25 Cible de pulverisation cathodique Ceased WO2000040769A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP37200298 1998-12-28
JP10/372002 1998-12-28

Publications (1)

Publication Number Publication Date
WO2000040769A1 true WO2000040769A1 (fr) 2000-07-13

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ID=18499677

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PCT/JP1999/006566 Ceased WO2000040769A1 (fr) 1998-12-28 1999-11-25 Cible de pulverisation cathodique

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WO (1) WO2000040769A1 (fr)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002069627A (ja) * 2000-08-30 2002-03-08 Toshiba Corp スパッタリングターゲットとそれを用いたスパッタリング装置
WO2003014409A1 (fr) * 2001-08-02 2003-02-20 Idemitsu Kosan Co., Ltd. Cible de pulverisation, film conducteur transparent et leur procede de fabrication
JP2003073819A (ja) * 2001-09-07 2003-03-12 Vacuum Metallurgical Co Ltd 錫−アンチモン酸化物焼結体ターゲット及びその製造方法
JPWO2006059429A1 (ja) * 2004-11-30 2008-08-07 日鉱金属株式会社 Ｓｂ−Ｔｅ系合金焼結体スパッタリングターゲット
EP2096188A1 (fr) 2006-12-13 2009-09-02 Idemitsu Kosan Co., Ltd. Cible de sublimation et film semi-conducteur à base d'oxyde
WO2012014688A1 (fr) * 2010-07-30 2012-02-02 Jx日鉱日石金属株式会社 Matériau fritté pour une cible de pulvérisation cathodique à base de zno-mgo
JP2014029032A (ja) * 2007-12-13 2014-02-13 Idemitsu Kosan Co Ltd スパッタリングターゲット及びその製造方法
US8882975B2 (en) 2006-10-13 2014-11-11 Jx Nippon Mining & Metals Corporation Sb-Te base alloy sinter sputtering target
WO2019177086A1 (fr) * 2018-03-15 2019-09-19 宇部マテリアルズ株式会社 CORPS FRITTÉ EN MgO ET CIBLE DE PULVÉRISATION

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0374931A2 (fr) * 1988-12-21 1990-06-27 Kabushiki Kaisha Toshiba Cible de pulvérisation et procédé pour sa fabrication
JPH03257158A (ja) * 1990-03-07 1991-11-15 Toshiba Corp スパッタリングターゲット
JPH05148635A (ja) * 1991-11-26 1993-06-15 Nikko Kyodo Co Ltd Ｉｔｏスパツタリングタ−ゲツト
JPH07243036A (ja) * 1994-03-07 1995-09-19 Japan Energy Corp Ｉｔｏスパッタリングタ−ゲット
JPH09104973A (ja) * 1995-05-30 1997-04-22 Japan Energy Corp スパッタリングタ−ゲット及びその製造方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0374931A2 (fr) * 1988-12-21 1990-06-27 Kabushiki Kaisha Toshiba Cible de pulvérisation et procédé pour sa fabrication
JPH03257158A (ja) * 1990-03-07 1991-11-15 Toshiba Corp スパッタリングターゲット
JPH05148635A (ja) * 1991-11-26 1993-06-15 Nikko Kyodo Co Ltd Ｉｔｏスパツタリングタ−ゲツト
JPH07243036A (ja) * 1994-03-07 1995-09-19 Japan Energy Corp Ｉｔｏスパッタリングタ−ゲット
JPH09104973A (ja) * 1995-05-30 1997-04-22 Japan Energy Corp スパッタリングタ−ゲット及びその製造方法

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002069627A (ja) * 2000-08-30 2002-03-08 Toshiba Corp スパッタリングターゲットとそれを用いたスパッタリング装置
WO2003014409A1 (fr) * 2001-08-02 2003-02-20 Idemitsu Kosan Co., Ltd. Cible de pulverisation, film conducteur transparent et leur procede de fabrication
JP2003073819A (ja) * 2001-09-07 2003-03-12 Vacuum Metallurgical Co Ltd 錫−アンチモン酸化物焼結体ターゲット及びその製造方法
JP4708361B2 (ja) * 2004-11-30 2011-06-22 Ｊｘ日鉱日石金属株式会社 Ｓｂ−Ｔｅ系合金焼結体スパッタリングターゲット
US7803209B2 (en) 2004-11-30 2010-09-28 Nippon Mining & Metals Co., Ltd Sb-Te alloy sintered compact sputtering target
JPWO2006059429A1 (ja) * 2004-11-30 2008-08-07 日鉱金属株式会社 Ｓｂ−Ｔｅ系合金焼結体スパッタリングターゲット
US8882975B2 (en) 2006-10-13 2014-11-11 Jx Nippon Mining & Metals Corporation Sb-Te base alloy sinter sputtering target
EP2096188A1 (fr) 2006-12-13 2009-09-02 Idemitsu Kosan Co., Ltd. Cible de sublimation et film semi-conducteur à base d'oxyde
US8784700B2 (en) 2006-12-13 2014-07-22 Idemitsu Kosan Co., Ltd. Sputtering target and oxide semiconductor film
JP2014029032A (ja) * 2007-12-13 2014-02-13 Idemitsu Kosan Co Ltd スパッタリングターゲット及びその製造方法
WO2012014688A1 (fr) * 2010-07-30 2012-02-02 Jx日鉱日石金属株式会社 Matériau fritté pour une cible de pulvérisation cathodique à base de zno-mgo
JPWO2012014688A1 (ja) * 2010-07-30 2013-09-12 Jx日鉱日石金属株式会社 ＺｎＯ−ＭｇＯ系スパッタリングターゲット用焼結体
WO2019177086A1 (fr) * 2018-03-15 2019-09-19 宇部マテリアルズ株式会社 CORPS FRITTÉ EN MgO ET CIBLE DE PULVÉRISATION

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