WO2012015016A1 - Cible de pulvérisation cathodique et son procédé de fabrication - Google Patents

Cible de pulvérisation cathodique et son procédé de fabrication Download PDF

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Publication number
WO2012015016A1
WO2012015016A1 PCT/JP2011/067371 JP2011067371W WO2012015016A1 WO 2012015016 A1 WO2012015016 A1 WO 2012015016A1 JP 2011067371 W JP2011067371 W JP 2011067371W WO 2012015016 A1 WO2012015016 A1 WO 2012015016A1
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Prior art keywords
sputtering target
group
sintered body
powder
sputtering
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PCT/JP2011/067371
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English (en)
Japanese (ja)
Inventor
光井　彰
健 岡東
秀文 小高
川本　泰
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旭硝子株式会社
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    • 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
    • C04B35/495—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 based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G33/00—Compounds of niobium
    • 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
    • C23C14/08—Oxides
    • C23C14/088—Oxides of the type ABO3 with A representing alkali, alkaline earth metal or Pb and B representing a refractory or rare earth metal
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    • 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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    • C01P2002/52—Solid solutions containing elements as dopants
    • C01P2002/54—Solid solutions containing elements as dopants one element only
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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    • C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
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    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
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Definitions

  • the present invention relates to a sputtering target and a manufacturing method thereof.
  • Solar cells are classified into many types depending on the material of the light absorption layer and the form of the element.
  • a solar cell using a compound semiconductor made of Cu (copper), In (indium), Ga (gallium), and Se (selenium) as a material for the light absorption layer is called a CIGS solar cell.
  • CIGS type solar cells have been researched and developed in various ways because of their high energy conversion efficiency and low degradation of energy conversion efficiency due to light irradiation.
  • a Mo (molybdenum) electrode layer In general CIGS type solar cells, a Mo (molybdenum) electrode layer, a CIGS layer as a light absorption layer, a buffer layer, and a ZnO (zinc oxide) electrode layer are laminated in this order on a substrate such as glass. It is constituted by.
  • the CIGS layer is known to have an improved carrier concentration due to the presence of an alkali metal such as Na (sodium). Therefore, energy conversion efficiency improves by using the CIGS layer which has high carrier concentration for a solar cell.
  • Patent Document 1 in order to further improve the energy conversion efficiency of the solar cell, at least one selected from Na 2 S, Na 2 Se, NaCl, NaF, or soda lime glass between the Mo electrode layer and the CIGS layer. It is disclosed that a layer composed of two layers (hereinafter referred to as a sodium supply layer) is provided. By forming the sodium supply layer between the Mo electrode layer and the CIGS layer, the alkali metal can be diffused from the sodium supply layer to the CIGS layer in the manufacturing process of the solar cell. Thereby, the energy conversion efficiency of a solar cell can further be improved.
  • NaNbO 3 sodium niobate
  • NaNbO 3 sodium niobate
  • Patent Document 2 discloses that NaNbO 3 is used as a material for a piezoelectric thin film because it has a high dielectric constant.
  • the piezoelectric thin film is formed by an RF sputtering method using a sputtering target made of a sintered body containing insulating NaNbO 3 .
  • Na 1-x Sr x NbO 3 is disclosed as one of electrode layer materials used for electronic thin film components, but Na 1-x Sr x NbO 3 has conductivity. There is no description.
  • a sputtering method in which a thin film having a uniform film thickness is easily obtained and environmental pollution is small is suitable.
  • a DC (direct current) sputtering method using direct current discharge is more suitable because the film formation rate can be increased.
  • a sputtering target having conductivity is required.
  • a sputtering target having stability against moisture is required.
  • materials containing Na are generally insulative, and some of them exhibit unstable properties against moisture, such as being dissolved in water or absorbing water vapor.
  • NaNbO 3 has stability against moisture but is insulative, and therefore, when used as a sputtering target, it has been limited to application to an RF (high frequency) sputtering method.
  • An object of the present invention is to provide a sputtering target that is made of a sintered body containing NaNbO 3 and can be used in a DC sputtering method, and a method for manufacturing the sputtering target.
  • the present invention comprises a sintered body containing NaNbO 3 doped with a Group 2 element (hereinafter referred to as Group 2 element-doped NaNbO 3 ), and the electrical resistance of the sintered body is 15 k ⁇ or less.
  • a sputtering target is provided.
  • the present invention provides a sputtering target in which the Group 2 element is at least one selected from the group consisting of Ca, Sr, and Ba.
  • the present invention also provides a sputtering target in which the Group 2 element is Sr.
  • the present invention also provides a sputtering target in which the ratio R / Rn of the amount R of atoms of the Group 2 element to the amount of atoms Rn of Na contained in the sintered body is 0.005 to 0.25. To do.
  • the present invention also provides a sputtering target in which the bulk density of the sintered body is 4.0 to 4.8 g / cm 3 .
  • this invention provides the sputtering target used for DC sputtering method.
  • this invention provides the sputtering target whose electrical resistance of the said sintered compact is 1 kohm or less.
  • the present invention provides a sintering process in which a composite oxide powder containing a Group 2 element, Na, and Nb as metal cations is fired at a firing temperature of 1150 ° C. or higher and 1350 ° C. or lower in an atmosphere having a lower oxygen concentration than the atmosphere.
  • a method for producing a sputtering target is provided.
  • the present invention provides an oxide powder containing a Group 2 element, Na, and Nb as metal cations as a molded body by a molding means, and a sheath material with a lid is filled with the graphite particle powder.
  • a method for producing a sputtering target characterized by having a firing step of filling a compact and firing at 1150 ° C.
  • the present invention provides a powder obtained by mixing oxide powder containing Group 2 elements, Na, and Nb as metal cations with niobium pentoxide powder, sodium carbonate powder, and compound powder having Group 2 elements.
  • a method for producing a sputtering target which is an oxide powder obtained by calcining at 900 to 1000 ° C.
  • the present invention which can be used for DC sputtering method, it is possible to provide a sputtering target and its manufacturing method of a sintered body containing NaNbO 3.
  • the sputtering target of the present invention is made of a sintered body containing a Group 2 element-doped NaNbO 3, and the electric resistance of the sintered body is 15 k ⁇ or less.
  • the sintered body contains the Group 2 element-doped NaNbO 3 , and the Group 2 element-doped NaNbO 3 is preferably contained in the sintered body in an amount of 70% by mass or more, particularly 90% by mass or more. More preferably it is included. It may be 100% by mass. If the group 2 element-doped NaNbO 3 is contained in the sintered body in an amount of 70% or more, it is preferable for maintaining effective conductivity of the sputtering target. Further, since NaNbO 3 is contained in the sintered body, the sputtering target is stable against moisture.
  • the Group 2 element-doped NaNbO 3 is represented by the chemical formula of (Na 1-X , M X ) NbO 3 + ⁇ where the Group 2 element is M, and a Group 2 element replaces a part of the sodium atom. ing. Note that ⁇ in the chemical formula is 0 ⁇ ⁇ ⁇ X / 2.
  • the electric resistance of the sintered body is 15 k ⁇ or less.
  • the electrical resistance of the sintered body is preferably 1 k ⁇ or less. If it is 15 k ⁇ or less, stable discharge can be maintained in the sputtering method, particularly the DC sputtering method.
  • the Group 2 element contained in the sintered body is contained as a NaNbO 3 dopant in the sintered body containing NaNbO 3 for the purpose of causing the sputtering target to exhibit conductivity.
  • the Group 2 element may be any of Be (beryllium), Mg (magnesium), Ca (calcium), Sr (strontium), Ba (barium), and Ra (radium). However, at least one selected from the group consisting of Ca, Sr, and Ba is preferable. In particular, Sr is more preferable in terms of improving conductivity.
  • the atomic ratio R / Rn which is the ratio of the amount R of atoms of the Group 2 element to the amount Rn of Na (sodium) atoms contained in the sintered body, is preferably 0.005 to 0.25, More preferably, it is 0.02 to 0.20. If R / Rn is 0.005 or more and 0.25 or less, the electrical resistance of the sintered body can be lowered.
  • a method for manufacturing a sputtering target comprising a sintered body containing a Group 2 element doped NaNbO 3.
  • the sintering temperature is preferably 1150 ° C. or higher and 1350 ° C. or lower, more preferably 1200 ° C. or higher and 1300 ° C. or lower. If a calcination temperature is 1150 degreeC or more, the bulk density (bulk density) of a sintered compact can be made high and an electrical resistance can be reduced.
  • the evaporation component from a sintered compact is suppressed as it is 1350 degrees C or less.
  • the holding time is preferably 0.5 hours to 10 hours, and more preferably 1 hour to 5 hours.
  • the bulk density of the sintered body is preferably 4.0 to 4.8 g / cm 3 , and more preferably 4.1 to 4.7, 4.2 to 4.6 g / cm 3 .
  • the oxygen concentration of the atmosphere when firing the oxide powder is preferably lower than the oxygen concentration in the atmosphere, that is, less than 21%.
  • the oxygen concentration is more preferably 1% or less. If the oxygen concentration in the firing step is less than 21%, the electrical resistance of the sintered body can be reduced.
  • the method for firing the sintered body is not particularly limited, and examples thereof include a normal pressure sintering method, a pressure sintering method, a hot pressing method, a HIP (hot isostatic pressing) method, and a spark plasma method.
  • the sputtering target of the present invention is preferably manufactured as follows.
  • the raw material niobium pentoxide powder, sodium carbonate powder, and compound powder having a Group 2 element were mixed using a dry ball mill, and the mixed powder was put into a crucible and 1-10 in air at 900-1000 ° C. It is preferable to perform calcination by holding for 5 hours, for example.
  • the carbonate in the raw material is decomposed, the powders undergo a solid phase reaction, and the Group 2 element-doped NaNbO 3 is synthesized.
  • the synthesized Group 2 element-doped NaNbO 3 is preferably pulverized and pulverized using a wet ball mill.
  • the pulverized ball is preferably 80 to 150 hours.
  • the grinding means is not limited to a ball mill, and various mills such as a bead mill, a sand mill, and a roll mill can be used.
  • the grinding time may be selected according to the characteristics of various mills.
  • the pulverized Group 2 element-doped NaNbO 3 powder is molded using a molding means so as to have a predetermined size to obtain a molded body.
  • the atmosphere during firing has a lower oxygen concentration than air.
  • the means for reducing the oxygen concentration can be realized, for example, by filling a sheath material with a lid with graphite particles, filling a molded body in the sheath material, and filling and burning with graphite particles.
  • air in the atmosphere may be exhausted using a vacuum pump, and a vacuum state or an inert gas such as argon gas may be filled.
  • the firing temperature of the molded body is preferably 1150 ° C. to 1350 ° C., more preferably 1200 to 1300 ° C.
  • the holding time is preferably 0.5 hours to 10 hours, and more preferably 1 hour to 5 hours.
  • a sintered body can be obtained through the above steps.
  • the obtained sintered body is processed into a predetermined size by a processing means, and is metal-bonded on a metal backing plate such as copper using a low melting point metal such as indium to form a sputtering target.
  • the number of the sintered bodies bonded to the backing plate is not limited, and may be single or plural.
  • Examples 1 to 5 (Production of sintered body) Niobium pentoxide powder (Nb 2 O 5 , 3N grade, average particle size 1 ⁇ m), sodium carbonate powder (Na 2 CO 3 , manufactured by Kanto Chemical Co., Ltd., special grade) As a compound containing a group 2 element, strontium carbonate powder (SrCO 3 , manufactured by Kojundo Chemical Laboratory Co., Ltd., 99% grade) was measured with an electronic balance so that the content shown in Table 1 was obtained.
  • the compact was fired to produce a sintered body.
  • high-purity graphite particles particles (particle size of about 1 to 3 mm) are filled in the sheath material made of alumina with a lid, and the compact is embedded in the sheath material. It was.
  • the sheath material was placed in an electric furnace (manufactured by Motoyama, NH-3035F) and fired.
  • the firing temperature was 1240 ° C. and the holding time was 2 hours.
  • the sintered body was taken out from the sheath material. An altered portion on the surface of the sintered body was removed from the obtained sintered body to obtain a sintered body serving as a sputtering target.
  • the size of the sintered body was about 20 mm in diameter and about 7 mm in thickness.
  • the bulk density of the sintered body serving as the sputtering target was measured by the Archimedes method.
  • the bulk density is a density when a container of a certain volume is filled with powder and the volume is taken as the volume.
  • the electrical resistance of the sintered body was measured using a digital multimeter (CDM-12M, manufactured by Custom Corp.). The electrical resistance was measured under the condition that the distance between the terminals of the digital multimeter was 5 mm on the same surface of the sintered body.
  • the specific resistance was measured by a four-terminal method by cutting a 3 ⁇ 3 ⁇ 15 mm 3 prism sample. Table 1 shows the evaluation results of the bulk density, electrical resistance and specific resistance of the sintered body.
  • Example 6 to 11 In place of strontium carbonate in Examples 1 to 5, calcium carbonate (CaCO 3 , 99% grade, manufactured by Kojundo Chemical Laboratory Co., Ltd.) was used, and the contents of the raw materials were changed. Similarly, a sintered body was produced and evaluated. The evaluation results are shown in Table 1.
  • Example 12 to 17 Except for using strontium carbonate in Examples 1 to 5 and using barium carbonate (BaCO 3 , manufactured by Junsei Chemical Co., Ltd. grade for high-purity ceramics) and changing the content of raw materials, the same as in Examples 1 to 5 Thus, a sintered body was produced and evaluated. The evaluation results are shown in Table 1. In Examples 1 to 17, the atomic ratio R / Rn between Na contained in the sintered body and the Group 2 element was 0.005 to 0.25. In addition, the sintered body had an electric resistance of 15 k ⁇ or less. Therefore, the sintered bodies in Examples 1 to 17 can be used as a sputtering target having conductivity suitable for the DC sputtering method.
  • barium carbonate BaCO 3 , manufactured by Junsei Chemical Co., Ltd. grade for high-purity ceramics
  • Example 1 A sintered body was produced and evaluated in the same manner as in Example 4 except that the atmosphere during firing was changed from a low oxygen atmosphere to air (oxygen concentration of about 21%). The evaluation results are shown in Table 1.
  • Comparative Example 2 Sintered bodies were produced and evaluated in the same manner as in Examples 1 to 5 except that the ratio of the raw materials shown in Table 1 was changed without using the Group 2 element. The evaluation results are shown in Table 1. The electric resistances of the sintered bodies of Comparative Examples 1 and 2 were 2 M ⁇ or more exceeding the measurement range of the digital multimeter, and were substantially insulating.
  • the sputtering target of the present invention can be used not only for forming a thin film of a CIGS type solar cell but also for forming a dielectric layer of a piezoelectric element. It should be noted that the entire contents of the specification, claims, and abstract of Japanese Patent Application No. 2010-171827 filed on July 30, 2010 are incorporated herein as the disclosure of the specification of the present invention. Is.

Abstract

L'invention concerne une cible de pulvérisation cathodique qui comprend un matériau fritté contenant du NaNbO3 et qui peut être utilisée dans un procédé de pulvérisation en courant continu. L'invention concerne également un procédé de fabrication de ladite cible. La cible de pulvérisation cathodique comprend un matériau fritté dopé avec un élément du groupe 2 et contenant du NaNbO3, ledit matériau fritté ayant une résistance électrique inférieure ou égale à 15 kΩ.
PCT/JP2011/067371 2010-07-30 2011-07-28 Cible de pulvérisation cathodique et son procédé de fabrication WO2012015016A1 (fr)

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JP2010-171827 2010-07-30

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JP2020143359A (ja) * 2019-03-08 2020-09-10 Ｊｘ金属株式会社 スパッタリングターゲット部材の製造方法及びスパッタリングターゲット部材

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09165262A (ja) * 1995-12-19 1997-06-24 Matsushita Electric Ind Co Ltd 圧電体磁器組成物
JP2003063877A (ja) * 2001-08-28 2003-03-05 National Institute Of Advanced Industrial & Technology 多成分系圧電材料の製造方法
JP2007055864A (ja) * 2005-08-26 2007-03-08 National Institute Of Advanced Industrial & Technology 圧電磁器組成物
JP2010161330A (ja) * 2008-12-08 2010-07-22 Hitachi Cable Ltd 圧電薄膜素子

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09165262A (ja) * 1995-12-19 1997-06-24 Matsushita Electric Ind Co Ltd 圧電体磁器組成物
JP2003063877A (ja) * 2001-08-28 2003-03-05 National Institute Of Advanced Industrial & Technology 多成分系圧電材料の製造方法
JP2007055864A (ja) * 2005-08-26 2007-03-08 National Institute Of Advanced Industrial & Technology 圧電磁器組成物
JP2010161330A (ja) * 2008-12-08 2010-07-22 Hitachi Cable Ltd 圧電薄膜素子

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