TW202033478A - Method for manufacturing sputtering target component and sputtering target component capable of preventing notches on a cut surface during a mechanical processing and avoiding abnormal discharge - Google Patents

Method for manufacturing sputtering target component and sputtering target component capable of preventing notches on a cut surface during a mechanical processing and avoiding abnormal discharge Download PDF

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TW202033478A
TW202033478A TW108137275A TW108137275A TW202033478A TW 202033478 A TW202033478 A TW 202033478A TW 108137275 A TW108137275 A TW 108137275A TW 108137275 A TW108137275 A TW 108137275A TW 202033478 A TW202033478 A TW 202033478A
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sputtering target
sintered body
cut surface
target component
manufacturing
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TW108137275A
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TWI710541B (en
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久家俊洋
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日商Jx金屬股份有限公司
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B1/00Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/3407Cathode assembly for sputtering apparatus, e.g. Target
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B27/00Other grinding machines or devices
    • B24B27/06Grinders for cutting-off
    • B24B27/0675Grinders for cutting-off methods therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B27/00Other grinding machines or devices
    • B24B27/06Grinders for cutting-off
    • B24B27/0683Accessories therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B41/00Component parts such as frames, beds, carriages, headstocks
    • B24B41/04Headstocks; Working-spindles; Features relating thereto
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B55/00Safety devices for grinding or polishing machines; Accessories fitted to grinding or polishing machines for keeping tools or parts of the machine in good working condition
    • B24B55/02Equipment for cooling the grinding surfaces, e.g. devices for feeding coolant
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B11/00Apparatus or processes for treating or working the shaped or preshaped articles
    • B28B11/12Apparatus or processes for treating or working the shaped or preshaped articles for removing parts of the articles by cutting
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/3407Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32Gas-filled discharge tubes
    • H01J37/34Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3488Constructional details of particle beam apparatus not otherwise provided for, e.g. arrangement, mounting, housing, environment; special provisions for cleaning or maintenance of the apparatus
    • H01J37/3491Manufacturing of targets

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Analytical Chemistry (AREA)
  • Structural Engineering (AREA)
  • Ceramic Engineering (AREA)
  • Physical Vapour Deposition (AREA)
  • Grinding Of Cylindrical And Plane Surfaces (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)

Abstract

The present invention provides a method for manufacturing a sputtering target component that can reduce peeling during mechanical processing. The method for manufacturing the sputtering target component includes steps of: a grinding step of grinding a sintered body; a cutting step after the grinding step, wherein a rotating tool is used to cut the sintered body while cooling water is poured at the contact point between the rotating tool and the sintered body in an amount greater than 20 L/min to obtain a sintered body having at least one cut surface.

Description

濺射靶部件的製造方法以及濺射靶部件Manufacturing method of sputtering target component and sputtering target component

本發明涉及一種濺射靶部件的製造方法以及濺射靶部件。The invention relates to a method for manufacturing a sputtering target component and a sputtering target component.

由複合氧化物構成的透明導電膜,具有高導電性和可見光透過性,在透明導電膜中最普及的是被稱作ITO的由氧化銦-氧化錫構成的透明導電膜。除此之外,已知氧化銦-氧化鋅(IZO)等。製造這些透明導電膜,在濺射法中,使用由組成與透明導電膜相同的金屬複合氧化物構成的濺射靶部件。例如,關於濺射靶部件的製造具有各種各樣的報告。A transparent conductive film made of a composite oxide has high conductivity and visible light transmittance. The most popular transparent conductive film is a transparent conductive film made of indium oxide-tin oxide called ITO. In addition, indium oxide-zinc oxide (IZO) and the like are known. In the production of these transparent conductive films, a sputtering target member composed of a metal composite oxide having the same composition as the transparent conductive film is used in the sputtering method. For example, there are various reports on the manufacture of sputtering target components.

在專利文獻1中提出了一種製作長寬比(厚度/外徑)為0.01~2的燒結體,並且在與厚度正交的方向上切斷該燒結體得到多個靶的濺射靶的製造方法。另外,專利文獻1中提出了,在將燒結體切斷成規定的尺寸時,使用內周刃式切斷機,或者使用線式切斷機進行切斷。Patent Document 1 proposes the production of a sputtering target in which a sintered body having an aspect ratio (thickness/outer diameter) of 0.01 to 2 is produced, and the sintered body is cut in a direction perpendicular to the thickness to obtain multiple targets. method. In addition, Patent Document 1 proposes to cut the sintered body to a predetermined size using an inner peripheral blade cutter or a wire cutter.

現有技術文獻Prior art literature

專利文獻Patent literature

專利文獻1:日本特開2002-371354號公報Patent Document 1: Japanese Patent Application Publication No. 2002-371354

發明要解決的技術問題The technical problem to be solved by the invention

然而,在對切斷面產生了缺口(以下,稱作剝落)的燒結體進行機械加工以形成濺射靶時,在沒有完全除去剝落的情況下,存在以該剝落為起點,在濺射中靶裂開、產生異常放電的擔憂。However, when machining a sintered body with chipping (hereinafter referred to as flaking) on the cut surface to form a sputtering target, if the flaking is not completely removed, the flaking may be used as a starting point. There is a concern that the target will crack and produce abnormal discharge.

為了抑制切斷燒結體時產生的剝落,例如可列舉使用加工中心(Machining Center:MC)。然而,在使用MC作為尺寸調節機構的情況下,非常耗費功夫,因此基於生產效率上的觀點,很難說是合適的。In order to suppress peeling during cutting of the sintered body, for example, the use of a machining center (Machining Center: MC) can be cited. However, in the case of using MC as the size adjustment mechanism, it takes a lot of time and effort. Therefore, it is difficult to say that it is suitable from the viewpoint of production efficiency.

因此,本發明鑒於以上情況而完成,在一實施方式中,目的在於提供一種能夠實現在機械加工時減少剝落產生的濺射靶部件的製造方法及濺射靶部件。Therefore, the present invention has been completed in view of the above circumstances. In one embodiment, an object is to provide a method of manufacturing a sputtering target member and a sputtering target member that can reduce peeling during machining.

解決技術問題的方法Solutions to technical problems

即,本發明的一個方面提供一種濺射靶部件的製造方法,上述濺射靶部件由使用ITO或IZO形成的陶瓷燒結體形成,所述製造方法包括:磨削上述燒結體的磨削步驟;在上述磨削步驟後的切斷步驟,其中,使用旋轉刀具並且在上述旋轉刀具與上述燒結體的接點以超過20L/分鐘一邊淋冷卻水一邊切斷,得到具有至少1個切斷面的燒結體。That is, one aspect of the present invention provides a method of manufacturing a sputtering target member, the sputtering target member is formed of a ceramic sintered body formed using ITO or IZO, and the manufacturing method includes: a grinding step of grinding the sintered body; In the cutting step after the grinding step, a rotary tool is used and the contact point between the rotary tool and the sintered body is cut at a rate of more than 20 L/min while pouring cooling water to obtain at least one cut surface Sintered body.

在本發明的濺射靶部件的製造方法的一實施方式中,上述冷卻水的量為25~100L/分鐘。In one Embodiment of the manufacturing method of the sputtering target member of this invention, the quantity of the said cooling water is 25-100 L/min.

在本發明的濺射靶部件的製造方法的一實施方式中,上述旋轉刀具的砂粒的細微性是JIS R6001:1998規定的#80以上。In one embodiment of the method of manufacturing a sputtering target member of the present invention, the fineness of the sand grains of the rotating cutter is #80 or more specified in JIS R6001:1998.

在本發明的濺射靶部件的製造方法的一實施方式中,上述旋轉刀具的周速度為5~60m/秒。In one Embodiment of the manufacturing method of the sputtering target member of this invention, the peripheral speed of the said rotating blade is 5-60 m/sec.

在本發明的濺射靶部件的製造方法的一實施方式中,在上述燒結體為平板狀的情況下,在與上述燒結體的厚度垂直的一個方向上逐次移動所上述旋轉刀具,形成上述至少1個切斷面中的各個切斷面。In an embodiment of the method for manufacturing a sputtering target member of the present invention, when the sintered body is in the shape of a flat plate, the rotating cutter is successively moved in a direction perpendicular to the thickness of the sintered body to form the at least Each cut surface in one cut surface.

在本發明的濺射靶部件的製造方法的一實施方式中,在上述燒結體為圓筒狀的情況下,在與上述燒結體的軸心垂直的一個方向上逐次移動所上述旋轉刀具,形成上述至少1個切斷面中的各個切斷面。In one embodiment of the method of manufacturing a sputtering target member of the present invention, when the sintered body is cylindrical, the rotary cutter is sequentially moved in a direction perpendicular to the axis of the sintered body to form Each of the above-mentioned at least one cut surface.

另外,本發明在另一方面,提供一種濺射靶部件,上述濺射靶部件由使用ITO或IZO形成的陶瓷燒結體形成,上述射靶部件具有切斷面,在5個視野中用SEM觀察所述切斷面時,在1個視野中在內沿切斷面外緣的長度為2.5mm的範圍內以厚度方向上的深度從大到小的順序抽出5個剝落,在對各個視野進行測量後,在合計25個剝落中,厚度方向上的深度為50μm以上的剝落在11個以內。In addition, in another aspect of the present invention, there is provided a sputtering target member, the sputtering target member is formed of a ceramic sintered body formed using ITO or IZO, the target member has a cut surface, and is observed by SEM in 5 fields of view In the case of the cut surface, in a field of view, within a range of 2.5 mm in length along the outer edge of the cut surface, five peelings are extracted in the order of the depth in the thickness direction from large to small. After the measurement, out of a total of 25 peels, there were 11 peels with a depth of 50 μm or more in the thickness direction.

在本發明的濺射靶部件的一實施方式中,在5個視野中用SEM觀察上述切斷面時,在1個視野中在沿上述切斷面外緣的長度為2.5mm的範圍內按照厚度方向上的深度從大到小的順序抽出5個剝落,在對各個視野進行測量後,在合計25個剝落中,厚度方向上的深度為100μm以上的剝落在5個以內。In one embodiment of the sputtering target member of the present invention, when the cut surface is observed by SEM in five fields of view, the length along the outer edge of the cut surface is 2.5 mm in one field of view. Five peelings were extracted in descending order of the depth in the thickness direction, and after measuring each field of view, out of a total of 25 peelings, the peelings with a depth of 100 μm or more in the thickness direction were within five.

在本發明的濺射靶部件的一實施方式中,在5個視野中用SEM觀察上述切斷面時,在1個視野中在沿上述切斷面外緣的長度為2.5mm的範圍內按照厚度方向上的深度從大到小的順序抽出5個剝落,在對各個視野進行測量後,在合計25個剝落中,厚度方向上的深度為25μm以上且小於50μm的剝落在15個以內。In one embodiment of the sputtering target member of the present invention, when the cut surface is observed by SEM in five fields of view, the length along the outer edge of the cut surface is 2.5 mm in one field of view. Five peelings were extracted in descending order of the depth in the thickness direction. After measuring each field of view, in a total of 25 peelings, there were 15 peels having a depth of 25 μm or more and less than 50 μm in the thickness direction.

在本發明的濺射靶部件的一實施方式中,在上述燒結體由ITO形成的情況下,該燒結體含有0.1~70質量%的Sn。In one embodiment of the sputtering target member of the present invention, when the sintered body is formed of ITO, the sintered body contains 0.1 to 70% by mass of Sn.

在本發明的濺射靶部件的一實施方式中,在上述燒結體由IZO形成的情況下,該燒結體含有0.1~99質量%的Zn。In one embodiment of the sputtering target member of the present invention, when the sintered body is formed of IZO, the sintered body contains 0.1 to 99% by mass of Zn.

在本發明的濺射靶部件的一實施方式中,濺射靶部件是平板狀或圓筒狀。In one embodiment of the sputtering target member of the present invention, the sputtering target member has a flat plate shape or a cylindrical shape.

發明的效果Effect of invention

根據本發明的一實施方式中,能夠提供一種能夠實現在機械加工時減少剝落產生的濺射靶部件的製造方法及濺射靶部件。According to an embodiment of the present invention, it is possible to provide a method for manufacturing a sputtering target member that can reduce peeling during machining, and a sputtering target member.

以下,本發明不限於各實施方式,在不脫離其要旨的範圍內,能夠對組成要素進行變形並具體化。另外,能夠通過適當地組合各實施方式中公開的多個組成要素,從而形成各種發明。例如,可以從實施方式所示的全部組成要素中刪除若干個組成要素。進一步,可以適當組合不同的實施方式的組成要素。需要說明的是,在以下的實施方式中說明的濺射靶部件的形狀,是在平板狀的前提下進行描述,但是也可以是圓筒狀。Hereinafter, the present invention is not limited to the respective embodiments, and the constituent elements can be modified and embodied within the scope not departing from the gist thereof. In addition, various inventions can be formed by appropriately combining a plurality of constituent elements disclosed in the respective embodiments. For example, some constituent elements may be deleted from all the constituent elements shown in the embodiments. Furthermore, the constituent elements of different embodiments can be appropriately combined. It should be noted that the shape of the sputtering target member described in the following embodiments is described on the premise of a flat plate shape, but it may be a cylindrical shape.

(1.濺射靶部件)(1. Sputtering target components)

根據本發明的濺射靶部件的一實施方式中,能夠提供一種能夠實現在機械加工時減少剝落產生的燒結體的切斷方法及燒結體。According to one embodiment of the sputtering target member of the present invention, it is possible to provide a cutting method and a sintered body capable of reducing the sintered body caused by peeling during machining.

本發明的濺射靶部件的一實施方式,由陶瓷燒結體(以下,簡稱為“燒結體”。)形成。更具體地,燒結體,由ITO或IZO形成,它們的組成是任意的。例如,是In2 O3 :SnO2 =90.0:10.0的ITO或In2 O3 :ZnO=89.3:10.7的IZO。另外,以氧化物換算計,可以含有10質量%以下的Ti、Zr、Al、Ta、Ca、Na等元素。One embodiment of the sputtering target member of the present invention is formed of a ceramic sintered body (hereinafter, simply referred to as “sintered body”). More specifically, the sintered body is formed of ITO or IZO, and their composition is arbitrary. For example, it is ITO with In 2 O 3 :SnO 2 =90.0:10.0 or IZO with In 2 O 3 :ZnO=89.3:10.7. In addition, in terms of oxides, elements such as Ti, Zr, Al, Ta, Ca, and Na may be contained at 10% by mass or less.

在本發明的濺射靶部件的一實施方式中,在燒結體由ITO形成的情況下,該燒結體的主要成分是In,優選含有0.1~70質量%的Sn,更優選含有0.5~50質量%的Sn,還更優選含有0.8~40質量%的Sn。In one embodiment of the sputtering target member of the present invention, when the sintered body is formed of ITO, the main component of the sintered body is In, and preferably contains 0.1 to 70% by mass of Sn, and more preferably contains 0.5 to 50% by mass. % Of Sn, and more preferably 0.8-40% by mass of Sn.

另外,在本發明的濺射靶部件的一實施方式中,在燒結體由IZO形成的情況下,該燒結體的主要成分是In,優選含有0.1~99質量%的Zn,更優選含有1~90質量%的Zn,還更優選含有3~85質量%的Zn。In addition, in one embodiment of the sputtering target member of the present invention, when the sintered body is formed of IZO, the main component of the sintered body is In, and preferably contains 0.1 to 99% by mass of Zn, and more preferably contains 1 to 90% by mass of Zn, and more preferably 3 to 85% by mass of Zn.

(剝落個數)(Number of peeling)

在本發明的濺射靶部件的一實施方式中,基於濺射中不會產生靶裂開或異常放電,穩定地提供濺射膜的觀點,用掃描型電子顯微鏡(SEM)觀察切斷面時,沿切斷面外緣的共計25個剝落中,厚度方向上的深度為50μm以上的剝落在11個以內,優選在10個以內,更優選在8個以內。In one embodiment of the sputtering target member of the present invention, based on the viewpoint that sputtering film is stably provided without causing target cracking or abnormal discharge during sputtering, when the cut surface is observed with a scanning electron microscope (SEM) Among the 25 peels in total along the outer edge of the cut surface, the peels having a depth of 50 μm or more in the thickness direction are within 11, preferably within 10, and more preferably within 8.

另外,在本發明的濺射靶部件的一實施方式中,用SEM觀察切斷面時,沿切斷面外緣的共計25個剝落中,厚度方向上的深度為100μm以上的剝落優選在5個以內,更優選在3個以內,還更優選在1個以內。In addition, in one embodiment of the sputtering target member of the present invention, when the cut surface is observed by SEM, among a total of 25 peelings along the outer edge of the cut surface, the peeling having a depth of 100 μm or more in the thickness direction is preferably 5 Within one, more preferably within three, and still more preferably within one.

另外,在本發明的濺射靶部件的一實施方式中,用SEM觀察切斷面時,沿切斷面外緣共計25個剝落中,厚度方向上的深度為25μm以上且小於50μm的剝落優選在15個以內,更優選在12個以內,還更優選在10個以內。In addition, in one embodiment of the sputtering target member of the present invention, when the cut surface is observed by SEM, a total of 25 peelings along the outer edge of the cut surface are preferably peeled with a depth of 25 μm or more and less than 50 μm in the thickness direction. It is 15 or less, more preferably 12 or less, and still more preferably 10 or less.

另外,SEM分析如下文進行說明。In addition, SEM analysis is described below.

切取燒結體作為試驗片。接著,用切斷機切斷該試驗片用作測量樣品,例如使用FE-EPMA(JXA-8500F,日本電子株式會社製造),以加速電壓15.0kV、50~100倍的倍率觀察切斷面的上端部。The sintered body was cut out as a test piece. Next, the test piece is cut with a cutting machine and used as a measurement sample. For example, using FE-EPMA (JXA-8500F, manufactured by JEOL Ltd.), the cut surface is observed at an acceleration voltage of 15.0kV and a magnification of 50 to 100 times. Upper end.

例如,在50倍的倍率下的1個視野中,在沿切斷面外緣的長度2.5mm的範圍內,在該視野中按照厚度方向上的深度從大到小的順序抽取5個剝落,測量剝落深度。在5個視野中進行同樣的操作,測量共計25個剝落深度。在1個視野中在沿切斷面外緣的長度2.5mm的範圍內完全不存在剝落的情況下,將剝落深度記做0μm。例如,在1視野中存在2個剝落的情況下,剩餘的3個剝落的剝落深度記做0μm。For example, in a field of view at a magnification of 50 times, within a range of 2.5 mm in length along the outer edge of the cut surface, in the field of view, five peelings are extracted in the order of the depth in the thickness direction, Measure the peeling depth. Perform the same operation in 5 fields of view, and measure a total of 25 peeling depths. When there was no peeling within a range of 2.5 mm in length along the outer edge of the cut surface in one field of view, the peeling depth was recorded as 0 μm. For example, in the case where there are two peelings in one field of view, the peeling depth of the remaining three peelings is recorded as 0 μm.

這裡,剝落的深度是指,在垂直於濺射面的方向上,從切斷面外緣開始到切口的最深部位為止的長度D(參照圖6)。Here, the depth of peeling refers to the length D from the outer edge of the cut surface to the deepest part of the cut in the direction perpendicular to the sputtering surface (see FIG. 6).

濺射靶部件,沒有限定,能夠加工成平板狀、圓筒狀等形狀並使用。The sputtering target member is not limited, and it can be processed into a shape such as a flat plate or a cylindrical shape and used.

(2. 濺射靶部件的製造方法)(2. Manufacturing method of sputtering target components)

接著,使用附圖說明濺射靶部件的製造方法。圖1是用於說明本發明的濺射靶部件的製造方法的一實施方式的流程圖。圖2是用於說明本發明的濺射靶部件的製造方法所包括的機械加工步驟的一示例的流程圖。圖3是示出本發明的供在濺射靶部件的製造方法中使用的切斷裝置的示意性的概略結構圖。圖4(A)是在本發明的濺射靶部件的製造方法所包括的切斷步驟中,對切斷燒結體的方法的一示例進行說明的示意性的概略平面圖,圖4(B)是用於說明切斷後的燒結體的示意性的立體圖。Next, a method of manufacturing a sputtering target member will be described using the drawings. FIG. 1 is a flowchart for explaining one embodiment of the method of manufacturing a sputtering target member of the present invention. 2 is a flowchart for explaining an example of machining steps included in the method of manufacturing a sputtering target member of the present invention. Fig. 3 is a schematic schematic configuration diagram showing a cutting device used in a method of manufacturing a sputtering target member of the present invention. 4(A) is a schematic plan view illustrating an example of a method of cutting a sintered body in the cutting step included in the method of manufacturing a sputtering target member of the present invention, and FIG. 4(B) is A schematic perspective view for explaining the sintered body after cutting.

本發明的濺射靶部件的製造方法,在一實施方式中,如圖1所示包括混合步驟S10、加壓成型步驟S20、燒結步驟S30和機械加工步驟S40。以下,使用附圖說明機械加工步驟S40,且混合步驟S10、加壓成型步驟S20和燒結步驟S30可以使用現有的方法。另外,省略與上文重複的內容。The manufacturing method of the sputtering target component of the present invention, in one embodiment, includes a mixing step S10, a pressure forming step S20, a sintering step S30, and a machining step S40 as shown in FIG. 1. Hereinafter, the machining step S40 will be described with reference to the drawings, and the mixing step S10, the press molding step S20, and the sintering step S30 can use existing methods. In addition, the content overlapping with the above is omitted.

(混合步驟,加壓成型步驟,燒結步驟)(Mixing step, press molding step, sintering step)

在混合步驟S10中,稱量所需的原料粉後,進行混合・微粉碎,之後,使用噴霧乾燥機進行乾燥・造粒,得到混合粉末。例如,在得到由ITO形成的燒結體的情況下,可以使用In2 O3 粉末及SnO2 粉末作為原料粉。另外,在得到由IZO形成的燒結體的情況下,可以使用In2 O3 粉末及ZnO2 粉末作為原料粉。In the mixing step S10, the required raw material powder is weighed, mixed and finely pulverized, and then dried and granulated using a spray dryer to obtain a mixed powder. For example, when a sintered body made of ITO is obtained, In 2 O 3 powder and SnO 2 powder can be used as raw material powders. In addition, when a sintered body made of IZO is obtained, In 2 O 3 powder and ZnO 2 powder can be used as raw material powders.

之後,在加壓成型步驟S20中,將混合粉末填充到所需的形狀的模具中,進行擠壓得到成型體。得到成型體後,還可以通過冷等靜壓加壓(CIP)進行成型。After that, in the press molding step S20, the mixed powder is filled in a mold of a desired shape and pressed to obtain a molded body. After obtaining the molded body, it can also be molded by cold isostatic pressing (CIP).

在燒結步驟S30中,在含氧氣氛下燒結成型體得到燒結體。燒結步驟的條件,根據每個組成而不同。In the sintering step S30, the molded body is sintered in an oxygen-containing atmosphere to obtain a sintered body. The conditions of the sintering step vary according to each composition.

(機械加工步驟)(Machining steps)

通過機械加工步驟S40,機械加工成所需的形狀,能夠得到濺射靶。機械加工步驟S40,如圖2所示,包括磨削步驟S41、切斷步驟S42和精加工步驟S43,濺射靶部件是指通過各個加工步驟得到的部件。Through the machining step S40, the sputtering target can be obtained by machining into a desired shape. The machining step S40, as shown in FIG. 2, includes a grinding step S41, a cutting step S42, and a finishing step S43. The sputtering target component refers to a component obtained through each processing step.

(磨削步驟)(Grinding step)

磨削步驟S41,對上述得到的燒結體進行磨削。在該磨削步驟S41中,可以使用磨削裝置以通過磨削手段磨削燒結體。In the grinding step S41, the sintered body obtained above is ground. In this grinding step S41, a grinding device may be used to grind the sintered body by grinding means.

(切斷步驟)(Cutting step)

切斷步驟S42,在磨削步驟S41之後,使用切斷裝置上配備的旋轉刀具並且在旋轉刀具與燒結體的接點c(參照圖3),一邊通過供應泵P從供應罐121淋冷卻水一邊切斷燒結體138,得到具有至少1個切斷面的燒結體。在本發明的一實施方式中,通過在旋轉刀具與燒結體的接點淋冷卻水,在燒結體與旋轉刀具接觸時,可減少燒結體發熱。接下來,針對使用切斷裝置的情況,示例了切斷步驟S42。Cutting step S42, after the grinding step S41, use the rotary cutter provided on the cutting device and at the contact point c (refer to FIG. 3) between the rotary cutter and the sintered body, the cooling water is poured from the supply tank 121 through the supply pump P While cutting the sintered body 138, a sintered body having at least one cut surface is obtained. In one embodiment of the present invention, by pouring cooling water at the contact point between the rotating tool and the sintered body, heat generation of the sintered body can be reduced when the sintered body is in contact with the rotating tool. Next, for the case of using the cutting device, the cutting step S42 is exemplified.

(切斷裝置)(Cutting device)

如圖3所示,切斷裝置100具備:切斷部110、供應部120、工作臺130、控制機構140。As shown in FIG. 3, the cutting device 100 includes a cutting unit 110, a supply unit 120, a table 130, and a control mechanism 140.

切斷部110具有:旋轉刀具111,插在旋轉刀具111的孔部111a中的旋轉軸112,用於將旋轉刀具111固定在旋轉軸112上的法蘭113。The cutting part 110 has a rotating tool 111, a rotating shaft 112 inserted in the hole 111 a of the rotating tool 111, and a flange 113 for fixing the rotating tool 111 to the rotating shaft 112.

關於旋轉刀具111的形狀,只要能夠切斷燒結體138,就沒有特別的限定,但是基於避免在切斷時將劇烈的負荷施加給燒結體的觀點,優選為圓形。另外,旋轉刀具111的砂粒的細微性,優選為#80以上,例如為#80~800。需要說明的是,該砂粒的細微性,遵照JIS R6001:1998規格。The shape of the rotary cutter 111 is not particularly limited as long as it can cut the sintered body 138. However, from the viewpoint of avoiding applying a severe load to the sintered body during cutting, it is preferably circular. In addition, the fineness of the sand grains of the rotary cutter 111 is preferably #80 or more, for example, #80 to 800. It should be noted that the fineness of the sand particles complies with JIS R6001: 1998 standards.

旋轉刀具111的周速度,基於施加於該旋轉刀具111的負荷的觀點,優選為5m/秒以上,更優選為10m/秒以上,還更優選為15m/秒以上。另外,旋轉刀具111的周速度,基於施加於裝置的負荷的觀點,優選為60m/秒以下,更優選為45m/秒以下,還更優選為35m/秒以下。From the viewpoint of the load applied to the rotating cutter 111, the circumferential speed of the rotating cutter 111 is preferably 5 m/sec or more, more preferably 10 m/sec or more, and still more preferably 15 m/sec or more. In addition, the peripheral speed of the rotary cutter 111 is preferably 60 m/sec or less, more preferably 45 m/sec or less, and still more preferably 35 m/sec or less from the viewpoint of the load applied to the device.

切斷速度,基於提高加工效率的觀點,優選為0.025mm/秒以上,更優選為0.05mm/秒以上,還更優選為0.1mm/秒以上,進一步優選為0.30mm/秒以上。上述切斷速度,基於減少施加於燒結體138及旋轉刀具111的負荷的觀點,優選為5mm/秒以下,更優選為2.5mm/秒以下,還更優選為1mm/秒以下。From the viewpoint of improving the processing efficiency, the cutting speed is preferably 0.025 mm/sec or more, more preferably 0.05 mm/sec or more, still more preferably 0.1 mm/sec or more, and even more preferably 0.30 mm/sec or more. From the viewpoint of reducing the load applied to the sintered body 138 and the rotary cutter 111, the cutting speed is preferably 5 mm/sec or less, more preferably 2.5 mm/sec or less, and still more preferably 1 mm/sec or less.

冷卻水量,基於減少施加於燒結體138及旋轉刀具111的熱負荷的觀點,優選以大於20L/分鐘進行供應,更優選以25L/分鐘以上進行供應,還更優選為30L/分鐘以上進行供應。另外,上述冷卻水,基於減少裝置容量的觀點,優選以100L/分鐘以下,更優選以75L/分鐘以下,還更優選以50L/分鐘以下進行供應。From the viewpoint of reducing the heat load applied to the sintered body 138 and the rotary cutter 111, the amount of cooling water is preferably supplied at more than 20 L/min, more preferably at 25 L/min or more, and still more preferably at 30 L/min or more. In addition, the above-mentioned cooling water is preferably supplied at 100 L/min or less, more preferably 75 L/min or less, and still more preferably 50 L/min or less from the viewpoint of reducing the device capacity.

作為切斷燒結體138的方法,基於減少在切斷時產生的剝落的觀點,可列舉使用切斷裝置100上配備的旋轉刀具111,作為切斷方向沿著一個方向切斷燒結體138的方法。更具體地,在燒結體138為平板狀的情況下,在與燒結體138的厚度垂直的一個方向上逐次移動旋轉刀具111,形成至少1個切斷面中的各個切斷面。另外,在燒結體138為圓筒狀的情況下,在與燒結體138的軸心垂直的一個方向上逐次移動旋轉刀具111,形成至少1個切斷面中的各個切斷面。As a method of cutting the sintered body 138, based on the viewpoint of reducing peeling during cutting, a method of cutting the sintered body 138 in one direction as the cutting direction using the rotary cutter 111 provided in the cutting device 100 can be mentioned. . More specifically, when the sintered body 138 has a flat plate shape, the rotary cutter 111 is successively moved in one direction perpendicular to the thickness of the sintered body 138 to form each of at least one cut surface. In addition, when the sintered body 138 is cylindrical, the rotary cutter 111 is successively moved in one direction perpendicular to the axis of the sintered body 138 to form each of at least one cut surface.

(精加工步驟)(Finishing steps)

精加工步驟S43,使用車床、加工中心等機械加工設備,對加工品等進行精研磨。由此,得到濺射靶部件。In the finishing step S43, the finished product is subjected to finishing grinding using machining equipment such as a lathe and a machining center. Thus, a sputtering target member was obtained.

〔實施例〕[Example]

基於實施例及比較例具體說明本發明。以下的實施例及比較例的記載,僅僅是為了容易理解本發明的技術內容而列舉的具體例,本發明的技術範圍不限於這些具體例。另外,在表1中示出濺射靶部件的製造條件。The present invention will be specifically described based on Examples and Comparative Examples. The description of the following examples and comparative examples are merely specific examples for easy understanding of the technical content of the present invention, and the technical scope of the present invention is not limited to these specific examples. In addition, Table 1 shows the manufacturing conditions of the sputtering target member.

(實施例1)(Example 1)

作為原料,混合90質量%的In2 O3 粉末,10質量%的SnO2 粉末得到混合粉末。用珠磨的濕式介質攪拌磨將混合粉末混合粉碎後,將這些粉末分別混合在純水中,製作粉碎漿料。接著,在該粉碎漿料中添加粘合劑,通過噴霧乾燥機進行造粒及乾燥。然後,將該混合粉末填充到擠壓用磨具中後,在20MPa的壓力下成型。進一步通過通過冷等靜壓加壓(CIP)進行成型,得到成型體。接著,以1540℃的燒結溫度、在氧氣氣氛下對該成型體進行20小時的常壓燒結,得到燒結體。As a raw material, 90% by mass of In 2 O 3 powder and 10% by mass of SnO 2 powder were mixed to obtain a mixed powder. After mixing and pulverizing the mixed powders with a wet media stirring mill of a bead mill, the powders are mixed in pure water to prepare pulverized slurry. Next, a binder is added to the pulverized slurry, and granulated and dried by a spray dryer. Then, the mixed powder was filled in an extrusion abrasive tool, and then molded under a pressure of 20 MPa. Further, molding is performed by cold isostatic pressing (CIP) to obtain a molded body. Next, the molded body was subjected to normal pressure sintering at a sintering temperature of 1540° C. in an oxygen atmosphere for 20 hours to obtain a sintered body.

通過平面銑床使用金剛石磨石對燒結體的表面進行平面磨削,以使得燒結體的厚度為3mm。接著,使用切斷裝置(DAS-W65N,株式會社YAC DAStech製造),以外表面為燒結體的方式將上述結構體放置在切斷裝置的工作臺上。接著,用圓形的旋轉刀具(周速度:25m/秒,砂粒的細微性:#270)切斷結構體,並如圖4(A)所示切斷燒結體以使得燒結體的尺寸為全長45mm、寬度4.0mm、厚度3.0mm,得到16個具有如圖4(B)所示的切斷面的燒結體。需要說明的是,在垂直於燒結體的厚度的一個方向上逐次移動旋轉刀具,由此形成上述各個切斷面。在切斷時,以30L/分鐘在燒結體與旋轉刀具的接點淋冷卻水(20℃)。如表2所示實施評價。The surface of the sintered body was surface ground using a diamond grindstone by a plane milling machine so that the thickness of the sintered body was 3 mm. Next, using a cutting device (DAS-W65N, manufactured by YAC DAStech Co., Ltd.), the above-mentioned structure was placed on the table of the cutting device so that the outer surface was a sintered body. Next, cut the structure with a circular rotating tool (peripheral speed: 25m/sec, fineness of sand: #270), and cut the sintered body as shown in Figure 4(A) so that the size of the sintered body is the full length 45 mm, width 4.0 mm, thickness 3.0 mm, and 16 sintered bodies having cut surfaces as shown in FIG. 4(B) were obtained. It should be noted that the rotary cutter is successively moved in a direction perpendicular to the thickness of the sintered body, thereby forming each of the above-mentioned cut surfaces. When cutting, spray cooling water (20°C) at the junction between the sintered body and the rotating tool at 30L/min. The evaluation was performed as shown in Table 2.

(剝落評價)(Peeling evaluation)

按照上文所述的方法,用FE-EPMA(JXA-8500F,日本電子株式會社製造)觀察燒結體的切斷面的上端部,在基於圖5得到的SEM畫像(倍率×50)對5個視野進行觀察時,在1個視野中在沿切斷面外緣的長度為2.5mm的範圍內,按照厚度方向上的深度從大到小的順序抽出5個剝落,並在對各個視野進行測量後的情況下,判斷厚度方向上的各剝落的大小的數值(25個)。另外,其結果在表2中示出。According to the method described above, observe the upper end of the cut surface of the sintered body with FE-EPMA (JXA-8500F, manufactured by JEOL Co., Ltd.), and compare 5 pieces on the SEM image (magnification×50) obtained based on Fig. 5 When observing the field of view, in a field of view, within a range of 2.5mm along the outer edge of the cut surface, extract 5 peels in the order of the depth in the thickness direction from largest to smallest, and measure each field of view In the latter case, determine the numerical value (25) of the size of each peeling in the thickness direction. In addition, the results are shown in Table 2.

(平均彎曲強度)(Average bending strength)

切割濺射靶部件,準備10個試驗片。對於該試驗片,按照下述的測量條件測量3點彎曲強度,算出其平均值。The sputtering target part was cut to prepare 10 test pieces. For this test piece, the three-point bending strength was measured under the following measurement conditions, and the average value was calculated.

<測量條件><Measurement conditions>

裝置名:今田製作所拉伸壓縮試驗機(SV-201NA-50SL型)Device name: Tensile and Compression Testing Machine (SV-201NA-50SL) by Imada Manufacturing Co., Ltd.

試驗冶具:3p-30Test fixture: 3p-30

試驗片尺寸:3×4×45mmTest piece size: 3×4×45mm

試驗速度:0.5mm/minTest speed: 0.5mm/min

支點間距離L:30mmDistance between fulcrums L: 30mm

(標準差)(Standard deviation)

基於上文所述的10個試驗片的3點彎曲強度測量值,算出標準差。這裡,平均彎曲強度的標準差S通過下式1算出。Based on the three-point bending strength measurement values of the 10 test pieces described above, the standard deviation was calculated. Here, the standard deviation S of the average bending strength is calculated by Equation 1 below.

Figure 02_image001
・・・式(1)
Figure 02_image001
···Formula 1)

S:標準偏差S: standard deviation

n:試驗片的總數n: the total number of test pieces

X:每個的數值X: the value of each

x:平均值x: average

(尺度參數)(Scale parameter)

按照精細陶瓷的強度資料的韋伯統計分析法(JIS R 1625:2010),將上述的10個試驗片的3點彎曲強度σ按照值從低到高的順序進行排序,並按照下式(2)通過平均等級法求出資料的累積破壞概率。According to the Weber statistical analysis method (JIS R 1625:2010) of the strength data of fine ceramics, the three-point bending strength σ of the above 10 test pieces are sorted in the order of value from low to high, and according to the following formula (2) Obtain the cumulative destruction probability of the data by the average grade method.

F=i/(n+1)・・・式(2)F=i/(n+1)・・・Formula (2)

式中,n為樣本數,i表示從小到大排序的位數(排序位數)。In the formula, n is the number of samples, and i represents the number of digits sorted from small to large (sorting digits).

接著,分別計算出lnσ及ln[ln{1/(1-F)}]。然後,以lnσ為橫軸、ln[ln{1/(1-Fi)}]為縱軸繪圖,畫出適合資料的直線,基於該截距算出尺度參數。Then, respectively calculate lnσ and ln[ln{1/(1-F)}]. Then, draw lnσ as the horizontal axis and ln[ln{1/(1-Fi)}] as the vertical axis, draw a straight line suitable for the data, and calculate the scale parameter based on the intercept.

(韋伯係數)(Weber coefficient)

按照精細陶瓷的強度資料的韋伯統計分析法(JIS R 1625:2010),將上述的10個試驗片的3點彎曲強度σ按照值從低到高的順序進行排序,並按照下式(3)通過平均等級法求出資料的累積破壞概率。According to the Weber statistical analysis method of the strength data of fine ceramics (JIS R 1625: 2010), the three-point bending strength σ of the above 10 test pieces are sorted in order of value from low to high, and according to the following formula (3) Obtain the cumulative destruction probability of the data by the average grade method.

F=i/(n+1)・・・式(3)F=i/(n+1)・・・Formula (3)

式中,n為樣本數,i表示從小到大排序的位數(排序位數)。In the formula, n is the number of samples, and i represents the number of digits sorted from small to large (sorting digits).

接著,分別計算出lnσ及ln[ln{1/(1-F)}]。然後,以lnσ為橫軸、ln[ln{1/(1-Fi)}]為縱軸繪圖,畫出適合資料的直線,基於該斜率算出韋伯係數。需要說明的是,可以說韋伯係數的數值越大,強度分佈的寬度越窄,穩定性越高。Then, respectively calculate lnσ and ln[ln{1/(1-F)}]. Then, draw lnσ as the horizontal axis and ln[ln{1/(1-Fi)}] as the vertical axis to draw a straight line suitable for the data, and calculate the Weber coefficient based on the slope. It should be noted that the larger the value of the Weber coefficient, the narrower the width of the intensity distribution and the higher the stability.

(實施例2)(Example 2)

除了混合89.3質量%的In2 O3 粉末、10.7質量%的ZnO粉末得到混合粉末以外,與實施例1同樣地得到燒結體。另外,剝落的評價是,基於得到的SEM圖像對5個視野進行觀察時,在1個視野中在沿所述切斷面外緣的長度為2.5mm的範圍內按照厚度方向上的深度從大到小的順序抽出5個剝落,在對各個視野進行測量後,對厚度方向上的各個剝落的大小的數值(25個)進行判斷。另外,燒結體的評價結果在表2中示出。A sintered body was obtained in the same manner as in Example 1, except that 89.3% by mass of In 2 O 3 powder and 10.7% by mass of ZnO powder were mixed to obtain a mixed powder. In addition, the evaluation of peeling is based on the observation of 5 fields of view based on the obtained SEM images, in one field of view, within a range of 2.5 mm along the outer edge of the cut surface according to the depth in the thickness direction Five peelings are extracted in order of large to small, and after measuring each field of view, the value (25) of the size of each peeling in the thickness direction is judged. In addition, the evaluation results of the sintered body are shown in Table 2.

(比較例1)(Comparative example 1)

除了旋轉刀具的砂粒的細微性選用#80,切斷速度選用0.25mm/秒,周速度選用10m/秒,冷卻水量選用5L/分,固定方法選用冶具以外,與實施例1同樣地得到燒結體。另外,剝落的評價是,基於圖6中得到的SEM圖像(倍率×50)對5個視野進行觀察時,在1個視野中在沿所述切斷面外緣的長度為2.5mm的範圍內按照厚度方向上的深度從大到小的順序抽出5個剝落,在對各個視野進行測量後,對厚度方向上的各個剝落的大小的數值(25個)進行判斷。另外,燒結體的評價結果在表2中示出。The sintered body is obtained in the same manner as in Example 1 except that the fineness of the sand of the rotating tool is #80, the cutting speed is 0.25mm/sec, the circumferential speed is 10m/sec, the cooling water volume is 5L/min, and the fixing method is selected as the fixture. . In addition, the evaluation of peeling is based on the SEM image (magnification × 50) obtained in FIG. 6 when observing 5 fields of view, the length along the outer edge of the cut surface in one field of view is within a range of 2.5 mm Five peelings are extracted in the order of the depth in the thickness direction from largest to smallest. After measuring each field of view, the value (25) of the size of each peeling in the thickness direction is judged. In addition, the evaluation results of the sintered body are shown in Table 2.

(比較例2)(Comparative example 2)

除了旋轉刀具的砂粒的細微性選用#80,切斷速度選用0.25mm/秒,周速度選用10m/秒,冷卻水量選用5L/分鐘,固定方法選用冶具以外,與實施例2同樣地得到濺射靶部件。另外,剝落的評價是,基於得到的SEM圖像對5個視野進行觀察時,在1個視野中在沿所述切斷面外緣的長度為2.5mm的範圍內按照厚度方向上的深度從大到小的順序抽出5個剝落,在對各個視野進行測量後,對厚度方向上的各個剝落的大小的數值(25個)進行判斷。另外,燒結體的評價結果在表2中示出。Except that the fineness of the grit of the rotating tool is #80, the cutting speed is 0.25mm/sec, the circumferential speed is 10m/sec, the cooling water volume is 5L/min, and the fixing method is selected as the fixture, the sputtering is obtained in the same manner as in Example 2. Target parts. In addition, the evaluation of peeling is based on the observation of 5 fields of view based on the obtained SEM images, in one field of view, within a range of 2.5 mm along the outer edge of the cut surface according to the depth in the thickness direction Five peelings are extracted in order of large to small, and after measuring each field of view, the value (25) of the size of each peeling in the thickness direction is judged. In addition, the evaluation results of the sintered body are shown in Table 2.

(比較例3)(Comparative example 3)

除了混合44.2質量%的In2 O3 粉末、25.9質量%的ZnO粉末和29.9質量%的Ga2 O3 得到混合粉末作為原料,並且旋轉刀具的砂粒的細微性選用#80,切斷速度選用0.25mm/秒,周速度選用10m/秒,冷卻水量選用5L/分鐘,固定方法選用冶具以外,與實施例1同樣地得到濺射靶部件。另外,剝落的評價是,基於得到的SEM圖像對5個視野進行觀察時,在1個視野中在沿所述切斷面外緣的長度為2.5mm的範圍內按照厚度方向上的深度從大到小的順序抽出5個剝落,在對各個視野進行測量後,對厚度方向上的各個剝落的大小的數值(25個)進行判斷。另外,燒結體的評價結果在表2中示出。In addition to mixing 44.2% by mass of In 2 O 3 powder, 25.9% by mass of ZnO powder and 29.9% by mass of Ga 2 O 3 to obtain mixed powder as raw materials, and the fineness of the grit of the rotating tool is #80, and the cutting speed is 0.25 mm/sec, the circumferential speed is 10m/sec, the amount of cooling water is 5L/min, and the fixing method is selected from the fixture, the sputtering target component is obtained in the same manner as in Example 1. In addition, the evaluation of peeling is based on the observation of 5 fields of view based on the obtained SEM images, in one field of view, within a range of 2.5 mm along the outer edge of the cut surface according to the depth in the thickness direction Five peelings are extracted in order of large to small, and after measuring each field of view, the value (25) of the size of each peeling in the thickness direction is judged. In addition, the evaluation results of the sintered body are shown in Table 2.

(比較例4)(Comparative Example 4)

除了混合44.2質量%的In2 O3 粉末、25.9質量%的ZnO粉末和29.9質量%的Ga2 O3 得到混合粉末作為原料,並且旋轉刀具的砂粒的細微性選用#80以外,實施例1同樣地得到濺射靶部件。另外,剝落的評價是,基於得到的SEM圖像對5個視野進行觀察時,在1個視野中在沿所述切斷面外緣的長度為2.5mm的範圍內按照厚度方向上的深度從大到小的順序抽出5個剝落,在對各個視野進行測量後,對厚度方向上的各個剝落的大小的數值(共計25個)進行判斷。另外,燒結體的評價結果在表2中示出。Except that 44.2% by mass of In 2 O 3 powder, 25.9% by mass of ZnO powder, and 29.9% by mass of Ga 2 O 3 were mixed to obtain a mixed powder as raw materials, and #80 was selected for the fineness of the grit of the rotating tool, the same as in Example 1 The sputtering target part was obtained. In addition, the evaluation of peeling is based on the observation of 5 fields of view based on the obtained SEM images, in one field of view, within a range of 2.5 mm along the outer edge of the cut surface according to the depth in the thickness direction Five peelings are extracted in order of large to small, and after measuring each field of view, the value of the size of each peeling in the thickness direction (a total of 25) is judged. In addition, the evaluation results of the sintered body are shown in Table 2.

Figure 02_image003
表1
Figure 02_image003
Table 1

Figure 02_image005
表2
Figure 02_image005
Table 2

(實施例的考察)(Examination of Examples)

如表2所示,與比較例1~2相比較,實施例1~2的厚度方向上為50μm以上的剝落個數更少,因此作為濺射靶部件更優選。進一步,與比較例1相比較,實施例1的彎曲強度及韋伯係數更高,因此可確認能夠用作濺射靶部件。需要說明的是,不同於由ITO或IZO形成的濺射靶部件,在比較例3~4中,可認為材料導致彎曲強度低,因此與切斷時的剝落沒有關係,強度仍然低。As shown in Table 2, compared with Comparative Examples 1 and 2, the number of peelings of 50 μm or more in the thickness direction of Examples 1 and 2 is smaller, and therefore more preferable as a sputtering target member. Furthermore, compared with Comparative Example 1, the bending strength and Weber coefficient of Example 1 are higher, and therefore it can be confirmed that it can be used as a sputtering target member. It should be noted that, unlike the sputtering target member formed of ITO or IZO, in Comparative Examples 3 to 4, it is considered that the material causes low bending strength, so it has nothing to do with peeling during cutting, and the strength is still low.

以上所述僅為本發明較佳可行實施例而已,舉凡應用本發明說明書及申請專利範圍所為之等效變化,理應包含在本發明之專利範圍內。The above are only the preferred and feasible embodiments of the present invention. Any equivalent changes made by applying the specification of the present invention and the scope of the patent application should be included in the patent scope of the present invention.

[本發明] 100:切斷裝置 110:切斷部 111:旋轉刀具 111a:孔部 112:旋轉軸 113:法蘭 120:供應部 121:供應罐 130:工作臺 138:燒結體 140:控制機構 C:接點 S10:混合步驟 S20:加壓成型步驟 S30:燒結步驟 S40:機械加工步驟 S41:磨削步驟 S42:切斷步驟 S43:精加工步驟[this invention] 100: cutting device 110: Cutting part 111: Rotating tool 111a: Hole 112: Rotation axis 113: Flange 120: Supply Department 121: supply tank 130: workbench 138: Sintered body 140: control mechanism C: Contact S10: mixing steps S20: pressure forming step S30: Sintering step S40: Machining steps S41: Grinding steps S42: Cut off step S43: Finishing step

圖1是用於說明本發明的濺射靶部件的製造方法的一實施方式的流程圖。 圖2是用於說明本發明的濺射靶部件的製造方法所包括的機械加工步驟的一示例的流程圖。 圖3是示出本發明的供在濺射靶部件的製造方法中使用的切斷裝置的示意性概略結構圖。 圖4(A)是在本發明的濺射靶部件的製造方法所包括的切斷步驟中,對切斷燒結體的方法的一示例進行說明的示意性的概略平面圖,圖4(B)是用於說明切斷後的燒結體的示意性的立體圖。 圖5是實施例1得到的SEM圖像。 圖6是比較例1得到的SEM圖像FIG. 1 is a flowchart for explaining one embodiment of the method of manufacturing a sputtering target member of the present invention. 2 is a flowchart for explaining an example of the machining steps included in the method of manufacturing the sputtering target member of the present invention. FIG. 3 is a schematic diagram showing a schematic configuration of a cutting device used in a method of manufacturing a sputtering target member of the present invention. 4(A) is a schematic plan view illustrating an example of a method of cutting a sintered body in the cutting step included in the method of manufacturing a sputtering target member of the present invention, and FIG. 4(B) is A schematic perspective view for explaining the sintered body after cutting. Fig. 5 is an SEM image obtained in Example 1. Figure 6 is the SEM image obtained in Comparative Example 1

Claims (12)

一種濺射靶部件的製造方法,所述濺射靶部件由使用ITO或IZO形成的陶瓷燒結體形成,其中,所述製造方法包括: 磨削所述燒結體的磨削步驟; 在所述磨削步驟後的切斷步驟,其中,使用旋轉刀具並且在所述旋轉刀具與所述燒結體的接點以超過20L/分鐘一邊淋冷卻水一邊切斷,得到具有至少1個切斷面的燒結體。A method for manufacturing a sputtering target component, the sputtering target component is formed of a ceramic sintered body formed using ITO or IZO, wherein the manufacturing method includes: A grinding step of grinding the sintered body; In the cutting step after the grinding step, a rotary tool is used and the contact point between the rotary tool and the sintered body is cut while being poured with cooling water at a rate of more than 20 L/min to obtain at least one cut Sintered body with cross section. 如請求項1所述之濺射靶部件的製造方法,其中,所述冷卻水的量為25~100L/分鐘。The method for manufacturing a sputtering target component according to claim 1, wherein the amount of the cooling water is 25-100 L/min. 如請求項1或2所述之濺射靶部件的製造方法,其中,所述旋轉刀具的砂粒的細微性,是JIS R6001:1998規定的#80以上。The method of manufacturing a sputtering target component according to claim 1 or 2, wherein the fineness of the grit of the rotating tool is #80 or more specified in JIS R6001:1998. 如請求項1或2所述之濺射靶部件的製造方法,其中,所述旋轉刀具的周速度為5~60m/秒。The method of manufacturing a sputtering target member according to claim 1 or 2, wherein the peripheral speed of the rotating tool is 5-60 m/sec. 如請求項1或2所述之濺射靶部件的製造方法,其中,在所述燒結體為平板狀的情況下,在與所述燒結體的厚度垂直的一個方向上逐次移動所述旋轉刀具,形成所述至少1個切斷面中的各個切斷面。The method of manufacturing a sputtering target component according to claim 1 or 2, wherein, in the case where the sintered body is a flat plate, the rotating tool is successively moved in a direction perpendicular to the thickness of the sintered body , Each of the at least one cut surface is formed. 如請求項1或2所述之濺射靶部件的製造方法,其中,在所述燒結體為圓筒狀的情況下,在與所述燒結體的軸心垂直的一個方向上逐次移動所述旋轉刀具,形成所述至少1個切斷面中的各個切斷面。The method of manufacturing a sputtering target component according to claim 1 or 2, wherein, when the sintered body is cylindrical, the sintered body is sequentially moved in a direction perpendicular to the axis of the sintered body. The rotating tool forms each of the at least one cut surface. 一種濺射靶部件,所述濺射靶部件由使用ITO或IZO形成的陶瓷燒結體形成,其中,所述射靶部件具有切斷面,在5個視野中用SEM觀察所述切斷面時,在1個視野中在沿切斷面外緣的長度為2.5mm的範圍內按照厚度方向上的深度從大到小的順序抽出5個剝落,在對各個視野進行測量後,在合計25個剝落中,所述厚度方向上的深度為50μm以上的剝落在11個以內。A sputtering target component formed of a ceramic sintered body formed by using ITO or IZO, wherein the target component has a cut surface, and when the cut surface is observed with SEM in 5 fields of view , In a field of view, within the range of 2.5mm along the outer edge of the cut surface, 5 peelings are extracted in the order of the depth in the thickness direction, and after measuring each field of view, a total of 25 Among the peelings, the number of peelings with a depth of 50 μm or more in the thickness direction was within 11. 如請求項7所述之濺射靶部件,其中,在5個視野中用SEM觀察所述切斷面時,在1個視野中在沿所述切斷面外緣的長度為2.5mm的範圍內按照厚度方向上的深度從大到小的順序抽出5個剝落,在對各個視野進行測量後,在合計25個剝落中,所述厚度方向上的深度為100μm以上的剝落在5個以內。The sputtering target member according to claim 7, wherein when the cut surface is observed by SEM in 5 fields of view, the length along the outer edge of the cut surface is in a range of 2.5 mm in one field of view Five peels were extracted in the order of the depth in the thickness direction from the largest to the smallest. After measuring each field of view, out of a total of 25 peels, the peels with a depth of 100 μm or more in the thickness direction were within five. 如請求項7或8所述之濺射靶部件,其中,在5個視野中用SEM觀察所述切斷面時,在1個視野中在沿所述切斷面外緣的長度為2.5mm的範圍內按照厚度方向上的深度從大到小的順序抽出5個剝落,在對各個視野進行測量後,在合計25個剝落中,所述厚度方向上的深度為25μm以上且小於50μm的剝落在15個以內。The sputtering target component according to claim 7 or 8, wherein when the cut surface is observed by SEM in 5 fields of view, the length along the outer edge of the cut surface in one field of view is 2.5 mm In the range of, 5 peelings are extracted in order of the depth in the thickness direction from largest to smallest. After measuring each field of view, in a total of 25 peels, the depth in the thickness direction is 25μm or more and less than 50μm. Within 15. 如請求項7或8所述之濺射靶部件,其中,在所述燒結體由ITO形成的情況下,所述燒結體含有0.1~70質量%的Sn。The sputtering target member according to claim 7 or 8, wherein, when the sintered body is formed of ITO, the sintered body contains Sn in an amount of 0.1 to 70% by mass. 如請求項7或8所述之濺射靶部件,其中,在所述燒結體由IZO形成的情況下,所述燒結體含有0.1~99質量%的Zn。The sputtering target component according to claim 7 or 8, wherein when the sintered body is formed of IZO, the sintered body contains 0.1 to 99% by mass of Zn. 如請求項7或8所述之濺射靶部件,其中,所述濺射靶部件是平板狀或圓筒狀。The sputtering target member according to claim 7 or 8, wherein the sputtering target member has a flat plate shape or a cylindrical shape.
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JP6267297B1 (en) * 2016-08-29 2018-01-24 Jx金属株式会社 Sintered body, sputtering target and manufacturing method thereof

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