TW202126838A - Oxide sputtering target and oxide sputtering target production method - Google Patents
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Abstract
Description
本發明是有關由含有鋯、矽及銦作為金屬成分的氧化物所成的氧化物濺射靶、及此氧化物濺射靶的製造方法。 本案是根據在2019年12月2日申請的日本特願2019-217933號,主張優先權,且將其內容援用於此。The present invention relates to an oxide sputtering target made of an oxide containing zirconium, silicon, and indium as metal components, and a method for manufacturing the oxide sputtering target. This case is based on Japanese Special Application No. 2019-217933 filed on December 2, 2019, claiming priority and citing its content here.
含有鋯、矽及銦作為金屬成分的氧化物膜是電阻高,例如在液晶顯示器、有機EL顯示器及觸控面板等的顯示器面板中,作為用以防止液晶元件或有機EL元件等的帶電所造成的誤動作之屏蔽層使用。 在此,上述的屏蔽層被適用於內嵌(In-Cell)型的觸控面板時,屏蔽層也被要求邊排除來自外部的雜訊,邊使碰觸訊號到達面板內部的感測器部分之作用。而且,在此屏蔽層中,為了確保顯示器面板的視認性,也被要求可視光的透過性高。Oxide films containing zirconium, silicon, and indium as metal components have high electrical resistance. For example, in display panels such as liquid crystal displays, organic EL displays, and touch panels, they are used to prevent charging of liquid crystal elements or organic EL elements. The misoperation of the shielding layer is used. Here, when the above-mentioned shielding layer is applied to an in-cell type touch panel, the shielding layer is also required to remove noise from the outside while allowing touch signals to reach the sensor part inside the panel. The role. Moreover, in this shielding layer, in order to ensure the visibility of the display panel, it is also required to have high transmittance of visible light.
又,含有鋯、矽及銦作為金屬成分的氧化物膜也作為作為資訊記錄媒體使用的相變化型光碟的介電質層或保護膜利用。 在此,專利文獻1~4提案一種被用在形成含有鋯、矽及銦作為金屬成分的氧化物膜時的氧化物濺射靶。In addition, an oxide film containing zirconium, silicon, and indium as metal components is also used as a dielectric layer or a protective film of a phase change optical disc used as an information recording medium. Here, Patent Documents 1 to 4 propose an oxide sputtering target to be used when forming an oxide film containing zirconium, silicon, and indium as metal components.
可是,最近被要求以大面積且生產效率佳形成含有鋯、矽及銦作為金屬成分的氧化物膜。因此,需要對應於濺射靶的大型化及濺射成膜時的高輸出化。 然而,在含有鋯、矽及銦作為金屬成分的氧化物濺射靶中,在以高輸出濺射成膜時容易發生破裂,有無法安定進行濺射成膜的情形。特別是在大型的濺射靶中,有容易發生破裂的傾向。 [先前技術文獻] [專利文獻]However, it has recently been required to form an oxide film containing zirconium, silicon, and indium as metal components with a large area and high production efficiency. Therefore, it is necessary to cope with the increase in the size of the sputtering target and the increase in output during sputtering film formation. However, in an oxide sputtering target containing zirconium, silicon, and indium as metal components, cracks are likely to occur during sputtering film formation at high output, and sputtering film formation cannot be performed stably. Especially in large sputtering targets, cracks tend to occur easily. [Prior Technical Literature] [Patent Literature]
[專利文獻1] 日本特開2013-142194號公報 [專利文獻2] 日本特開2007-327103號公報 [專利文獻3] 日本特開2009-062585號公報 [專利文獻4] 日本特開2018-040032號公報[Patent Document 1] JP 2013-142194 A [Patent Document 2] JP 2007-327103 A [Patent Document 3] JP 2009-062585 A [Patent Document 4] Japanese Patent Application Publication No. 2018-040032
(發明所欲解決的課題)(The problem to be solved by the invention)
本發明是有鑑於前述的情事而研發者,以提供一種即使是以高輸出濺射成膜的情況,也可抑制破裂的發生,可安定且生產效率佳進行濺射成膜之氧化物濺射靶及此氧化物濺射靶的製造方法為目的。 (用以解決課題的手段)The present invention was developed in view of the foregoing circumstances to provide an oxide sputtering that can suppress the occurrence of cracks even in the case of high-output sputtering film formation, and can perform sputtering film formation with stability and high production efficiency. The target and the manufacturing method of this oxide sputtering target are the objective. (Means to solve the problem)
為了上述課題,經本發明者們深入檢討的結果,確認在含有鋯、矽及銦作為金屬成分的氧化物濺射靶中,存在氧化鋯相,此氧化鋯相會在1000℃附近相變,因為此時的體積變化而產生破裂。 又,得知成為氧化物濺射靶的原料的氧化鋯粉是若與氧化銦粉及氧化矽粉一起粉碎混合,則氧化鋯粉的粒徑會比氧化銦粉及氧化矽粉更大,形成粗大的氧化鋯相,成為破裂的發生的原因。In order to solve the above-mentioned problems, the inventors of the present invention have conducted in-depth studies and confirmed that in an oxide sputtering target containing zirconium, silicon, and indium as metal components, a zirconium oxide phase is present, and this zirconium oxide phase transforms around 1000°C. The volume at this time changed and cracks occurred. In addition, it is known that if the zirconia powder used as the raw material of the oxide sputtering target is pulverized and mixed with indium oxide powder and silicon oxide powder, the particle size of the zirconia powder will be larger than that of the indium oxide powder and silicon oxide powder. The coarse zirconia phase causes the occurrence of cracks.
本發明是根據上述的見解而研發者,本發明之一形態的氧化物濺射靶是由含有鋯、矽及銦作為金屬成分的氧化物所成的氧化物濺射靶,其特徵為:氧化鋯相的最大粒徑為10μm以下。The present invention was developed based on the above-mentioned knowledge. The oxide sputtering target of one aspect of the present invention is an oxide sputtering target made of an oxide containing zirconium, silicon and indium as metal components, and is characterized by: oxidation The maximum particle size of the zirconium phase is 10 μm or less.
若根據本發明之一形態的氧化物濺射靶,則由於是含有鋯、矽及銦作為金屬成分的氧化物,因此可形成電阻高且可視光的透過性佳的氧化物膜。 又,由於氧化鋯相的最大粒徑被限制於10μm以下,因此在以高輸出濺射成膜時,即使氧化鋯相相變而體積變化,也抑制破裂的發生。又,即使是將濺射靶大型化的情況,也抑制濺射時的破裂的發生。因此,可安定且生產效率佳進行濺射成膜。According to the oxide sputtering target according to one aspect of the present invention, since it is an oxide containing zirconium, silicon, and indium as metal components, an oxide film with high electrical resistance and good visible light permeability can be formed. In addition, since the maximum particle size of the zirconia phase is limited to 10 μm or less, during sputtering film formation at high output, even if the zirconia phase changes and the volume changes, the occurrence of cracks is suppressed. In addition, even when the sputtering target is increased in size, the occurrence of cracks during sputtering is suppressed. Therefore, sputtering film formation can be performed stably and with high production efficiency.
在此,在本發明之一形態的氧化物濺射靶中,將氧化鋯相的平均粒徑設為DZrO ,將其他的氧化物相的平均粒徑設為DMO 時,符合0.6≦DMO /DZrO ≦1.8為理想。 此情況,氧化鋯相與其他的氧化物相的粒徑差會變小,可確保靶的強度。因此,可進一步抑制以高輸出濺射成膜時的破裂的發生。Here, in the oxide sputtering target of one aspect of the present invention, when the average particle size of the zirconium oxide phase is D ZrO and the average particle size of the other oxide phases is D MO , 0.6≦D MO /D ZrO ≦1.8 is ideal. In this case, the difference in particle size between the zirconium oxide phase and other oxide phases is reduced, and the strength of the target can be ensured. Therefore, it is possible to further suppress the occurrence of cracks during sputtering film formation with high output.
又,在本發明之一形態的氧化物濺射靶中,是在靶組織全體中,最大粒徑為7μm以下,且平均粒徑為4μm以下為理想。 此情況,由於在靶組織全體,粒徑均一化,且被微細化,因此可均一地進行濺射成膜。又,可確保靶的強度,進一步可抑制以高輸出濺射成膜時的破裂的發生。In addition, in the oxide sputtering target of one aspect of the present invention, it is preferable that the maximum particle size is 7 μm or less and the average particle size is 4 μm or less in the entire target structure. In this case, since the particle size is uniform and finer in the entire target structure, sputtering film formation can be performed uniformly. In addition, the strength of the target can be ensured, and the occurrence of cracks during sputtering film formation with high output can be further suppressed.
本發明之一形態的氧化物濺射靶的製造方法,係由含有鋯、矽及銦作為金屬成分的氧化物所成的氧化物濺射靶的製造方法,其特徵係具有: 預備粉碎工程,其係將氧化鋯粉予以粉碎成最大粒徑成為4μm以下; 燒結原料粉形成工程,其係取得混合最大粒徑為4μm以下的氧化鋯粉、氧化矽粉及氧化銦粉的燒結原料粉;及 燒結工程,其係邊導入氧,邊將取得的前述燒結原料粉加熱燒製,取得燒結體。The method for manufacturing an oxide sputtering target in one aspect of the present invention is a method for manufacturing an oxide sputtering target made of an oxide containing zirconium, silicon, and indium as metal components, and is characterized by: Preliminary crushing process, which is to crush the zirconia powder to a maximum particle size of 4μm or less; Sintering raw material powder formation process, which is to obtain sintering raw material powder that mixes zirconium oxide powder, silicon oxide powder and indium oxide powder with a maximum particle size of 4 μm or less; and The sintering process involves heating and firing the obtained sintering raw material powder while introducing oxygen to obtain a sintered body.
若根據此構成的氧化物濺射靶的製造方法,則由於具備將氧化鋯粉予以粉碎成最大粒徑成為4μm以下的預備粉碎工程,因此可將燒結後的氧化鋯相的最大粒徑壓在10μm以下。 因此,可抑制以高輸出濺射成膜時的破裂的發生,可製造一種能夠安定且生產效率佳進行濺射成膜的氧化物濺射靶。According to the manufacturing method of the oxide sputtering target with this configuration, since the zirconia powder is pulverized to a preliminary crushing process with a maximum particle size of 4 μm or less, the maximum particle size of the sintered zirconia phase can be reduced to 10μm or less. Therefore, the occurrence of cracks during sputtering film formation with high output can be suppressed, and an oxide sputtering target that can perform sputtering film formation with stability and high production efficiency can be manufactured.
在此,在本發明之一形態的氧化物濺射靶的製造方法中,將最大粒徑為4μm以下的氧化鋯粉的平均粒徑設為dZrO ,將氧化銦粉的平均粒徑設為dInO ,且將氧化矽粉的平均粒徑設為dSiO 時,符合0.7≦dInO /dZrO ≦1.6及0.7≦dSiO /dZrO ≦1.6為理想。 此情況,氧化鋯粉與氧化銦粉及氧化矽粉的粒徑差會變小,可製造高強度的氧化物濺射靶。Here, in the method for producing an oxide sputtering target according to one aspect of the present invention, the average particle diameter of the zirconium oxide powder having a maximum particle diameter of 4 μm or less is d ZrO , and the average particle diameter of the indium oxide powder is d InO , and when the average particle size of the silicon oxide powder is set to d SiO , 0.7≦d InO /d ZrO ≦1.6 and 0.7≦d SiO /d ZrO ≦1.6 are ideal. In this case, the particle size difference between the zirconium oxide powder and the indium oxide powder and the silicon oxide powder will be reduced, and a high-strength oxide sputtering target can be manufactured.
又,本發明之一形態的氧化物濺射靶的製造方法中,是在混合氧化鋯粉、氧化矽粉及氧化銦粉而取得的燒結原料粉全體中,最大粒徑為3μm以下,且平均粒徑為1μm以下為理想。 此情況,可製造一種在靶組織全體,粒徑會微細化及均一化,且可均一地進行濺射成膜的氧化物濺射靶。 [發明的效果]In addition, in the method for producing an oxide sputtering target according to one aspect of the present invention, in the total sintering raw material powder obtained by mixing zirconium oxide powder, silicon oxide powder, and indium oxide powder, the maximum particle size is 3 μm or less, and the average The particle size is preferably 1 μm or less. In this case, it is possible to manufacture an oxide sputtering target in which the particle size can be made finer and uniform throughout the target structure, and the sputtering film can be formed uniformly. [Effects of the invention]
若根據本發明之一形態,則可提供一種即使是以高輸出濺射成膜的情況,也可抑制破裂的發生,可安定且生產效率佳進行濺射成膜之氧化物濺射靶及此氧化物濺射靶的製造方法。According to one aspect of the present invention, it is possible to provide an oxide sputtering target capable of suppressing the occurrence of cracks even in the case of high-output sputtering film formation, and capable of performing sputtering film formation with stability and high production efficiency, and the same. Manufacturing method of oxide sputtering target.
以下,參照附圖說明有關本發明的實施形態的氧化物濺射靶及氧化物濺射靶的製造方法。 本實施形態的氧化物濺射靶是被用在形成適合作為在液晶顯示器面板、有機EL顯示器面板及觸控面板等的顯示器面板中為了防止帶電而配設的屏蔽層或資訊記錄媒體的相變化型光碟的介電質層或保護膜之氧化物膜時者。Hereinafter, the oxide sputtering target and the manufacturing method of the oxide sputtering target according to the embodiment of the present invention will be described with reference to the drawings. The oxide sputtering target of this embodiment is used to form a phase change suitable as a shielding layer or information recording medium arranged in order to prevent charging in display panels such as liquid crystal display panels, organic EL display panels, and touch panels. It is the oxide film of the dielectric layer or protective film of the type optical disc.
另外,本實施形態的氧化物濺射靶是其形狀不被特別加以限定,亦可為濺射面形成矩形狀的矩形平板型濺射靶,或亦可為濺射面形成圓形的圓板型濺射靶。或者,亦可為濺射面設為圓筒面的圓筒型濺射靶。又,濺射面的面積是不被特別加以限制,但為了在大面積的基板效率佳成膜,濺射面的面積為2.0m2 以上的大型的濺射靶為理想。In addition, the shape of the oxide sputtering target of this embodiment is not particularly limited, and it may be a rectangular flat-plate type sputtering target with a rectangular sputtering surface, or a circular plate with a circular sputtering surface. Type sputtering target. Alternatively, it may be a cylindrical sputtering target whose sputtering surface is a cylindrical surface. In addition, the area of the sputtering surface is not particularly limited, but for efficient film formation on a large-area substrate, a large sputtering target with an area of the sputtering surface of 2.0 m 2 or more is preferable.
本實施形態的氧化物濺射靶是以含有鋯、矽及銦作為金屬成分的氧化物所構成。
在此氧化物濺射靶中,如圖1所示般,具有:氧化鋯相11、氧化銦相12、及含有上述的金屬元素的至少一部分的複合氧化物相13。在本實施形態中,複合氧化物相13是為In及Si的複合氧化物(例如In2
Si2
O7
相)。The oxide sputtering target of this embodiment is composed of an oxide containing zirconium, silicon, and indium as metal components. As shown in FIG. 1, this oxide sputtering target has a
而且,在本實施形態的氧化物濺射靶中,氧化鋯相11的最大粒徑為10μm以下。
又,在本實施形態中,氧化鋯相11的平均粒徑DZrO
與其他的氧化物相的氧化銦相12的平均粒徑DInO
的比DInO
/DZrO
及氧化鋯相11的平均粒徑DZrO
與其他的氧化物相的複合氧化物相13的平均粒徑DInSiO
的比DInSiO
/DZrO
分別為0.6以上1.8以下的範圍內為理想。
而且,在本實施形態中,在靶組織全體,最大粒徑為7μm以下,且平均粒徑為4μm以下為理想。In addition, in the oxide sputtering target of this embodiment, the maximum particle size of the
以下,顯示在本實施形態的氧化物濺射靶中,將氧化物的組成、氧化鋯相11的最大粒徑、氧化鋯相11與其他的氧化物相(氧化銦相12及複合氧化物相13)的平均粒徑比、靶組織全體的最大粒徑及平均粒徑規定為如上述般的理由。The following shows that in the oxide sputtering target of this embodiment, the composition of the oxide, the maximum particle size of the
(氧化物組成) 本實施形態的氧化物濺射靶是以含有鋯、矽及銦的氧化物作為金屬成分的氧化物所構成。如此的組成的氧化物濺射靶是可形成電阻值十分高,且可視光的透過性佳的氧化物膜。 在此,在本實施形態中,將金屬成分的合計設為100 mass%,Zr的含有量為2mass%以上27mass%以下的範圍內,In的含有量為65mass%以上95mass%以下的範圍內,Si的含有量為0.5mass%以上15mass%以下的範圍內,剩餘部分為不可避免雜質金屬元素(不可避免金屬)為理想。又,Zr、In及Si的合計含有量是95mass%以上為理想,99mass%以上更加理想。 詳細,本實施形態的氧化物濺射靶是由氧化物及不可避免雜質所成,該氧化物是由金屬成分及氧所成,金屬成分是將金屬成分的合計含有量設為100mass%,含Zr:2mass%以上27mass%以下,In:65mass%以上95mass%以下,及Si:0.5mass%以上15mass%以下,剩餘部分為不可避免金屬為理想。 不可避免雜質是氧與金屬成分以外的元素。不可避免金屬是上述的含有量特定的元素以外的金屬元素。 Hf是與Zr化學性質相似,難以分離Hf與Zr。因此,在工業用原料的ZrO2 粉末中是不可避免地含有HfO2 。因此,可舉Hf作為不可避免金屬。Hf的含有量是0mass%以上0.9 mass%以下。又,可舉Fe,Ti,Na,作為不可避免金屬,該等的合計是0mass%以上0.1mass%以下。(Oxide composition) The oxide sputtering target of this embodiment is composed of an oxide containing oxides of zirconium, silicon, and indium as metal components. The oxide sputtering target of such a composition can form an oxide film with a very high resistance value and good visible light transmittance. Here, in this embodiment, the total of the metal components is 100 mass%, the content of Zr is within the range of 2 mass% to 27 mass%, and the content of In is within the range of 65 mass% to 95 mass%. It is preferable that the Si content is in the range of 0.5 mass% or more and 15 mass% or less, and the remainder is an unavoidable impurity metal element (unavoidable metal). In addition, the total content of Zr, In, and Si is preferably 95 mass% or more, and more preferably 99 mass% or more. In detail, the oxide sputtering target of this embodiment is made of oxide and unavoidable impurities. The oxide is made of a metal component and oxygen. Zr: 2mass% or more and 27mass% or less, In: 65mass% or more and 95mass% or less, and Si: 0.5mass% or more and 15mass% or less, and the remainder is ideal for unavoidable metals. The inevitable impurities are elements other than oxygen and metal components. The inevitable metal is a metal element other than the above-mentioned elements with a specific content. Hf is chemically similar to Zr, and it is difficult to separate Hf and Zr. Therefore, HfO 2 is inevitably contained in the ZrO 2 powder as an industrial raw material. Therefore, Hf can be cited as an inevitable metal. The Hf content is 0 mass% or more and 0.9 mass% or less. In addition, Fe, Ti, and Na can be cited. As unavoidable metals, the total of these is 0 mass% or more and 0.1 mass% or less.
將Zr的含有量設為2mass%以上時,可使成膜後的氧化物膜的耐久性提升,且硬度變硬,耐刮擦。另一方面,將Zr的含有量設為27mass%以下時,可抑制折射率増大,可抑制不要的反射的發生,因此可抑制可視光的透過率降低。 另外,將金屬成分的合計設為100mass%,Zr的含有量的下限是設為3mass%以上為理想,設為5mass%以上更加理想。Zr的含有量的上限是設為21mass%以下為理想,20mass%以下更加理想。When the content of Zr is 2 mass% or more, the durability of the oxide film after film formation can be improved, and the hardness can be hardened and scratch resistance can be made. On the other hand, when the content of Zr is 27 mass% or less, the increase in refractive index can be suppressed, and the occurrence of unnecessary reflection can be suppressed, and therefore the decrease in the transmittance of visible light can be suppressed. In addition, the total of the metal components is 100 mass%, and the lower limit of the Zr content is preferably 3 mass% or more, and more preferably 5 mass% or more. The upper limit of the content of Zr is preferably 21 mass% or less, and more preferably 20 mass% or less.
將In的含有量設為65mass%以上時,可確保氧化物濺射靶的導電性,可藉由直流(DC)濺射來安定形成氧化物膜。另一方面,將In的含有量設為95mass%以下時,可抑制短波長的透過率降低,可確保視認性。 另外,將金屬成分的合計設為100mass%,In的含有量的下限設為75mass%以上為理想,設為80mass%以上更加理想。In的含有量的上限是設為90mass%以下為理想。When the In content is 65 mass% or more, the conductivity of the oxide sputtering target can be ensured, and the oxide film can be formed stably by direct current (DC) sputtering. On the other hand, when the content of In is 95 mass% or less, the decrease in the transmittance of short wavelengths can be suppressed, and visibility can be ensured. In addition, the total of the metal components is 100 mass%, and the lower limit of the In content is preferably 75 mass% or more, and more preferably 80 mass% or more. The upper limit of the content of In is preferably 90 mass% or less.
將Si的含有量設為0.5mass%以上時,可確保氧化物濺射靶的柔軟性,提升膜的破裂耐性。另一方面,將Si的含有量設為15mass%以下時,可抑制膜的導電性降低,可藉由直流(DC)濺射來安定形成氧化物膜。 另外,將金屬成分的合計設為100mass%,Si的含有量的下限是設為2mass%以上為理想,設為3mass%以上更加理想。Si的含有量的上限是設為12mass%以下為理想,設為7mass%以下更加理想。When the Si content is 0.5 mass% or more, the flexibility of the oxide sputtering target can be ensured, and the fracture resistance of the film can be improved. On the other hand, when the Si content is 15 mass% or less, the decrease in conductivity of the film can be suppressed, and the oxide film can be stably formed by direct current (DC) sputtering. In addition, the total of the metal components is 100 mass%, and the lower limit of the Si content is preferably 2 mass% or more, and more preferably 3 mass% or more. The upper limit of the Si content is preferably 12 mass% or less, and more preferably 7 mass% or less.
(氧化鋯相11的最大粒徑)
在此氧化鋯相11中,在1000℃附近相變而體積變化。因此,粗大的氧化鋯相11存在的情況,在以高輸出濺射成膜時,因此為相變而產生大的體積變化,恐有發生破裂之虞。
於是,在本實施形態中,將氧化鋯相11的最大粒徑限制於10μm以下。
另外,為了進一步抑制氧化物濺射靶的破裂的發生,而將氧化鋯相11的最大粒徑設為8μm以下為理想,設為7μm以下更理想。(Maximum particle size of zirconia phase 11)
In this
(氧化鋯相11與其他的氧化物相的平均粒徑比)
在本實施形態的氧化物濺射靶中,藉由縮小氧化鋯相11與其他的氧化物相(氧化銦相12及複合氧化物相13)的粒徑差,可使氧化物濺射靶的強度提升,可進一步抑制破裂的發生。
於是,在本實施形態中,將氧化鋯相11的平均粒徑DZrO
與其他的氧化物相的氧化銦相12的平均粒徑DInO
的比DInO
/DZrO
及氧化鋯相11的平均粒徑DZrO
與其他的氧化物相的複合氧化物相13的平均粒徑DInSiO
的比DInSiO
/DZrO
分別設為0.6以上1.8以下的範圍內為理想。
另外,DInO
/DZrO
及DInSiO
/DZrO
的下限是0.63以上更理想,0.65以上更加理想。另一方面,DInO
/DZrO
及DInSiO
/ DZrO
的上限是1.75以下更理想,1.7以下更加理想。(The ratio of the average particle size of the
(靶組織全體的最大粒徑及平均粒徑) 在本實施形態的氧化物濺射靶中,藉由在靶組織全體,粒徑微細化及均一化,可均一地進行濺射成膜,且可確保靶的強度,可進一步抑制以高輸出濺射成膜時的破裂的發生。 於是,在本實施形態中,在靶組織全體,最大粒徑而7μm以下,且平均粒徑為4μm以下為理想。 另外,在靶組織全體的最大粒徑是6.5μm以下更理想,6μm以下更加理想。又,在靶組織全體的平均粒徑是3μm以下更理想,2μm以下更加理想。(Maximum particle size and average particle size of the entire target tissue) In the oxide sputtering target of this embodiment, by making the particle size finer and uniform in the entire target structure, the sputtering film can be formed uniformly, the strength of the target can be ensured, and the sputtering with high output can be further suppressed. The occurrence of rupture during film formation. Therefore, in the present embodiment, it is preferable that the maximum particle size of the entire target tissue is 7 μm or less, and the average particle size is 4 μm or less. In addition, the maximum particle size in the entire target tissue is more preferably 6.5 μm or less, and more preferably 6 μm or less. In addition, the average particle size of the entire target tissue is more preferably 3 μm or less, and more preferably 2 μm or less.
其次,參照圖2說明上述的本實施形態的氧化物濺射靶的製造方法。Next, the method of manufacturing the oxide sputtering target of this embodiment described above will be described with reference to FIG. 2.
(預備粉碎工程S01) 首先,準備氧化鋯粉(ZrO2 粉)。在此,此氧化鋯粉是去除Fe2 O3 ,SiO2 ,TiO2 ,Na2 O等的不可避免雜質後的純度為99.9mass%以上為理想。另外,ZrO2 是與HfO2 的連結非常強,即使是高純度的ZrO2 粉,也在不可避免雜質之中含有氧化鉿(HfO2 )最大2.5mass%。因此,通常ZrO2 的純度是測定HfO2 以外的雜質的含有量,利用得到的雜質的合計量,藉由差數法來算出。上述的ZrO2 粉的純度是測定雜質的Fe2 O3 、SiO2 、TiO2 、Na2 O的含有量,從100mass%扣除該等化合物的含有量的合計而算出者。 將此氧化鋯粉(ZrO2 粉)粉碎,最大粒徑設為4μm以下。另外,有關粉碎方法是無特別加以限定,只要從既存的粉碎方法適當選擇即可。(Preliminary grinding process S01) First, zirconia powder (ZrO 2 powder) is prepared. Here, it is desirable that the zirconia powder has a purity of 99.9 mass% or more after removing inevitable impurities such as Fe 2 O 3 , SiO 2 , TiO 2 , and Na 2 O. In addition, ZrO 2 has a very strong connection with HfO 2 and even high-purity ZrO 2 powder contains hafnium oxide (HfO 2 ) at a maximum of 2.5 mass% among inevitable impurities. Therefore, the purity of ZrO 2 is usually measured by measuring the content of impurities other than HfO 2 and calculating by the difference method using the total amount of impurities obtained. The purity of the above-mentioned ZrO 2 powder is calculated by measuring the contents of Fe 2 O 3 , SiO 2 , TiO 2 , and Na 2 O as impurities, and subtracting the sum of the contents of these compounds from 100 mass%. This zirconia powder (ZrO 2 powder) is pulverized, and the maximum particle size is set to 4 μm or less. In addition, the pulverization method is not particularly limited, as long as it is appropriately selected from existing pulverization methods.
(燒結原料粉形成工程S02) 其次,準備氧化矽粉(SiO2 粉)及氧化銦粉(In2 O3 粉)。在此,氧化矽粉(SiO2 粉)及氧化銦粉(In2 O3 粉)是分別純度為99.9mass%以上為理想。 將該等氧化矽粉(SiO2 粉)及氧化銦粉(In2 O3 粉)及藉由預備粉碎而最大粒徑為4μm以下的氧化鋯粉(ZrO2 粉)予以秤量成為預定的組成比。使用濕式的粉碎混合裝置來將秤量後的原料粉予以粉碎、混合,形成燒結原料粉(燒結用原料粉)。在此,溶媒可舉水等。 另外,粉碎混合而取得的糊狀物的乾燥方法是無特別加以限制,可用通常的乾燥機或噴霧乾燥等來實施。由取得均質的混合粉的觀點,使用噴霧乾燥為理想。(Sintering raw material powder formation process S02) Next, silica powder (SiO 2 powder) and indium oxide powder (In 2 O 3 powder) are prepared. Here, it is desirable that silicon oxide powder (SiO 2 powder) and indium oxide powder (In 2 O 3 powder) each have a purity of 99.9 mass% or more. The silicon oxide powder (SiO 2 powder) and indium oxide powder (In 2 O 3 powder) and zirconia powder (ZrO 2 powder) with a maximum particle size of 4 μm or less by preliminary grinding are weighed to a predetermined composition ratio . A wet pulverizing and mixing device is used to pulverize and mix the weighed raw material powder to form sintering raw material powder (raw material powder for sintering). Here, the solvent can be water or the like. In addition, the drying method of the paste obtained by pulverization and mixing is not particularly limited, and it can be carried out by a normal dryer, spray drying, or the like. From the viewpoint of obtaining a homogeneous mixed powder, spray drying is ideal.
在此,在燒結原料粉中,將在預備粉碎工程S01最大粒徑為4μm以下的氧化鋯粉(ZrO2 粉)的平均粒徑設為dZrO ,且將氧化銦粉(In2 O3 粉)的平均粒徑設為dInO ,將氧化矽粉(SiO2 粉)的平均粒徑設為dSiO 時,符合0.7≦dInO / dZrO ≦1.6及0.7≦dSiO /dZrO ≦1.6為理想。 另外,上述的平均粒徑比dInO /dZrO 及dSiO /dZrO 的下限是設為0.7以上更理想,設為0.75以上更加理想。又,上述的平均粒徑比dInO /dZrO 及dSiO /dZrO 的上限是設為1.55以下更理想,設為1.5以下更加理想。Here, in the sintering raw material powder, the average particle size of the zirconia powder (ZrO 2 powder) whose maximum particle size is 4 μm or less in the preliminary grinding process S01 is set to d ZrO , and the indium oxide powder (In 2 O 3 powder When the average particle size of) is set to d InO and the average particle size of silicon oxide powder (SiO 2 powder) is set to d SiO , 0.7≦d InO / d ZrO ≦1.6 and 0.7≦d SiO /d ZrO ≦1.6 are ideal. In addition, the lower limit of the average particle diameter ratio d InO /d ZrO and d SiO /d ZrO is more preferably 0.7 or more, and more preferably 0.75 or more. In addition, the upper limit of the average particle diameter ratio of d InO /d ZrO and d SiO /d ZrO is more preferably 1.55 or less, and more preferably 1.5 or less.
又,在取得的燒結原料粉全體中,最大粒徑為3μm以下,且平均粒徑設為1μm以下為理想。 另外,燒結原料粉全體的最大粒徑是2.8μm以下更理想,2.6μm以下更加理想。又,燒結原料粉全體的平均粒是0.9μm以下更理想,0.8μm以下更加理想。In addition, in the entire obtained sintering raw material powder, the maximum particle size is preferably 3 μm or less, and the average particle size is preferably 1 μm or less. In addition, the maximum particle size of the entire sintering raw material powder is more preferably 2.8 μm or less, and more preferably 2.6 μm or less. In addition, the average particle size of the entire sintering raw material powder is more preferably 0.9 μm or less, and more preferably 0.8 μm or less.
(成形工程S03) 其次,將取得的燒結原料粉充填於成形模而加壓,藉此取得預定形狀的成形體。此時的加壓壓力是設為20MPa以上35MPa以下的範圍內為理想。又,溫度是亦可為常溫,但以900℃以上950℃以下的範圍的溫度進行加壓成形為理想。藉此,促進頸口成形,提升成形體的強度。(Forming process S03) Next, the obtained sintering raw material powder is filled in a forming mold and pressurized, thereby obtaining a molded body of a predetermined shape. The pressurizing pressure at this time is preferably in the range of 20 MPa or more and 35 MPa or less. In addition, the temperature may be normal temperature, but it is desirable to perform press molding at a temperature in the range of 900°C or more and 950°C or less. Thereby, the neck opening is promoted, and the strength of the molded body is improved.
(燒結工程S04) 將此成形體裝入具有氧導入機能的燒製裝置內,邊導入氧邊加熱燒結,取得燒結體。 此時,氧的導入量是設為3L/分以上10L/分以下的範圍內為理想。又,昇溫速度設為50℃/h以上200℃/h以下的範圍內為理想。 燒製工程S04是由保持工程及正式燒製工程所成為理想。首先,將成形體保持3~5小時於1200℃以上1400℃以下的溫度為理想(保持工程)。其次,將成形體保持5~10小時於1450℃以上1600℃以下的溫度為理想(正式燒製工程)。 在保持工程中,溫度未滿1200℃的情況,或加熱時間未滿3小時的情況,複合氧化物的生成不夠充分,恐有在正式燒製工程發生破裂之虞。在保持工程中,溫度超過1400℃的情況,或加熱時間超過5小時的情況,恐有在燒結體產生彎曲之虞。 在正式燒製工程中,溫度未滿1450℃的情況,或加熱時間未滿5小時的情況,恐有燒結體的密度降低之虞。在正式燒製工程中,溫度超過1600℃的情況,或加熱時間超過10小時的情況,恐有導致過度地粒成長之虞。(Sintering Engineering S04) This compact is put into a sintering device with oxygen introduction function, and the sintered body is obtained by heating and sintering while introducing oxygen. At this time, the amount of oxygen introduced is preferably within the range of 3 L/min or more and 10 L/min or less. In addition, it is desirable that the temperature increase rate is within the range of 50°C/h or more and 200°C/h or less. The firing process S04 is an ideal from the maintenance process and the formal firing process. First, it is desirable to keep the molded body at a temperature of 1200°C or higher and 1400°C or lower for 3 to 5 hours (maintenance process). Next, it is ideal to keep the molded body at a temperature of 1450°C or higher and 1600°C or lower for 5-10 hours (main firing process). In the maintenance process, if the temperature is less than 1200°C, or if the heating time is less than 3 hours, the formation of the composite oxide is insufficient, and there is a risk of cracking in the actual firing process. In the holding process, if the temperature exceeds 1400°C, or if the heating time exceeds 5 hours, there is a possibility that the sintered body may be bent. In the main firing process, if the temperature is less than 1450°C, or if the heating time is less than 5 hours, the density of the sintered body may decrease. In the actual firing process, if the temperature exceeds 1600°C, or if the heating time exceeds 10 hours, there is a risk of excessive grain growth.
(機械加工工程S05) 其次,對於上述的燒結體進行車床加工等的機械加工,取得預定大小的氧化物濺射靶。(Machining Engineering S05) Next, the above-mentioned sintered body is subjected to mechanical processing such as lathe processing to obtain an oxide sputtering target of a predetermined size.
藉由上述的工程,製造本實施形態的氧化物濺射靶。Through the above-mentioned process, the oxide sputtering target of this embodiment is manufactured.
若根據以上般的構成的本實施形態的氧化物濺射靶,則由於以含有鋯、矽及銦作為金屬成分的氧化物所構成,因此可形成電阻值高且可視光的透過率佳的氧化物膜。According to the oxide sputtering target of this embodiment constructed as above, since it is composed of an oxide containing zirconium, silicon, and indium as metal components, an oxide with high resistance and good visible light transmittance can be formed.物膜。 Material film.
而且,氧化鋯相11的最大粒徑被限制於10μm以下,因此在以高輸出濺射成膜時,即使是氧化鋯相11相變而體積變化的情況,也可抑制破裂的發生。因此,可安定且生產效率佳進行濺射成膜。In addition, the maximum particle size of the
又,本實施形態中,氧化鋯相11的平均粒徑DZrO
與其他的氧化物相的氧化銦相12的平均粒徑DInO
的比DInO
/DZrO
及氧化鋯相11的平均粒徑DZrO
與其他的氧化物相的複合氧化物相13的平均粒徑DInSiO
的比DInSiO
/DZrO
分別為0.6以上1.8以下的範圍內的情況,是氧化鋯相11與其他的氧化物相的氧化銦相12及複合氧化物相13的粒徑差變小,可確保靶的強度。因此,可進一步抑制以高輸出濺射成膜時的破裂的發生。Also, in this embodiment, the ratio of the average particle size D ZrO of the zirconium oxide phase 11 to the average particle size D InO of the
又,本實施形態中,靶組織全體的最大粒徑為7μm以下,且平均粒徑為4μm以下的情況,由於在靶組織全體,粒徑會均一化,且被微細化,因此可均一地進行濺射成膜。又,可確保靶的強度,可進一步抑制以高輸出濺射成膜時的破裂的發生。Also, in this embodiment, when the maximum particle size of the entire target tissue is 7 μm or less, and the average particle size is 4 μm or less, since the particle size is uniform and finer throughout the target tissue, it can be uniformly processed. Sputtering film formation. In addition, the strength of the target can be ensured, and the occurrence of cracks during sputtering film formation with high output can be further suppressed.
又,若根據本實施形態的氧化物濺射靶的製造方法,則由於具備將氧化鋯粉予以粉碎成最大粒徑成為4μm以下的預備粉碎工程S01,因此可將燒結後的氧化鋯相11的最大粒徑壓在10μm以下。
因此,可抑制以高輸出濺射成膜時的破裂的發生,可製造一種可安定且生產效率佳進行濺射成膜的氧化物濺射靶。In addition, according to the method of manufacturing the oxide sputtering target of this embodiment, since the zirconia powder is pulverized to a maximum particle size of 4 μm or less, the preliminary pulverization process S01 is provided, so that the
又,本實施形態中,將最大粒徑為4μm以下的氧化鋯粉的平均粒徑設為dZrO ,將氧化銦粉的平均粒徑設為dInO ,且將氧化矽粉的平均粒徑設為dSiO 時,符合0.7≦dInO /dZrO ≦1.6及0.7≦dSiO /dZrO ≦1.6的情況,氧化鋯粉與氧化銦粉及氧化矽粉的粒徑差會變小,可製造高強度的氧化物濺射靶。In addition, in this embodiment, the average particle size of zirconia powder with a maximum particle size of 4 μm or less is set to d ZrO , the average particle size of indium oxide powder is set to d InO , and the average particle size of silica powder is set to When it is d SiO , if it meets the conditions of 0.7≦d InO /d ZrO ≦1.6 and 0.7≦d SiO /d ZrO ≦1.6, the particle size difference between zirconium oxide powder and indium oxide powder and silicon oxide powder will be small, and high manufacturing can be achieved. Strong oxide sputtering target.
而且,在本實施形態中,在將氧化鋯粉、氧化矽粉及氧化銦粉混合而取得的燒結原料粉全體,最大粒徑為3μm以下,且平均粒徑為1μm以下的情況,可製造一種在靶組織全體,粒徑會微細化及均一化,可均一地進行濺射成膜的氧化物濺射靶。Furthermore, in this embodiment, in the case where the total sintering raw material powder obtained by mixing zirconium oxide powder, silicon oxide powder and indium oxide powder has a maximum particle size of 3 μm or less and an average particle size of 1 μm or less, one type can be produced An oxide sputtering target in which the particle size is refined and uniform in the entire target structure, and can be sputtered and formed uniformly.
以上,說明有關本發明的實施形態,但本發明是不被限定於此,可在不脫離發明的技術要件的範圍適當變更。 [實施例]As mentioned above, although the embodiment of this invention was described, this invention is not limited to this, It can change suitably in the range which does not deviate from the technical requirement of the invention. [Example]
以下,說明有關為了確認本實施形態的有效性而進行的確認實驗的結果。Hereinafter, the results of the confirmation experiment performed to confirm the effectiveness of the present embodiment will be explained.
<氧化物濺射靶> 準備氧化銦粉末(In2 O3 粉末:純度99.9mass%以上,平均粒徑1μm),氧化矽粉末(SiO2 粉末:純度99.8mass%以上,平均粒徑2μm)及氧化鋯粉末(ZrO2 粉末:純度99.9 mass%以上,平均粒徑2μm),作為原料粉末。然後,將該等秤量成為表1所示的混合比。另外,氧化鋯粉末的純度是測定Fe2 O3 ,SiO2 ,TiO2 ,Na2 O等的HfO2 以外的雜質的含有量,從100mass%扣除該等化合物的含有量的合計而算出。在氧化鋯粉末之中是HfO2 最大含有2.5mass%。<Oxide sputtering target> Prepare indium oxide powder (In 2 O 3 powder: purity 99.9 mass% or more, average particle size 1μm), silicon oxide powder (SiO 2 powder: purity 99.8 mass% or more, average particle size 2μm) and Zirconia powder (ZrO 2 powder: purity 99.9 mass% or more, average particle size 2 μm) was used as the raw material powder. Then, the equivalent was weighed to the mixing ratio shown in Table 1. The purity of the zirconia powder is calculated by measuring the content of impurities other than HfO 2 such as Fe 2 O 3 , SiO 2 , TiO 2 , and Na 2 O, and subtracting the total content of these compounds from 100 mass%. Among zirconia powders, HfO 2 contains a maximum of 2.5 mass%.
作為預備粉碎工程,是使用以直徑0.5mm的氧化鋯球作為粉碎媒體的珠磨機裝置,以表1所示的條件來濕式粉碎上述的氧化鋯粉末。 針對粉碎後的氧化鋯粉,藉由雷射繞射散射法來測定最大粒徑及中值徑(D50)。 具體而言,將六偏磷酸鈉濃度0.2mol%的水溶液調製100mL,在此水溶液中加入10mg氧化鋯粉末,使用雷射繞射散射法(測定裝置:NIKKISO CO.,LTD.製、Microtrac MT3000)來測定粒子徑分佈。從取得的粒子徑分佈作成累積粒度分佈曲線,取得最大粒徑及平均粒徑(中值徑(D50))。 在此所為的中值徑(D50)是表示體積累積成為50%的粒子徑。As the preliminary pulverization process, a bead mill device using zirconia balls with a diameter of 0.5 mm as a pulverizing medium was used to wet pulverize the above-mentioned zirconia powder under the conditions shown in Table 1. For the pulverized zirconia powder, the maximum particle diameter and median diameter (D50) are measured by the laser diffraction scattering method. Specifically, 100 mL of an aqueous solution with a concentration of 0.2 mol% of sodium hexametaphosphate was prepared, 10 mg of zirconia powder was added to this aqueous solution, and the laser diffraction scattering method was used (measurement device: manufactured by NIKKISO CO., LTD., Microtrac MT3000) To determine the particle size distribution. Create a cumulative particle size distribution curve from the obtained particle size distribution, and obtain the maximum particle size and the average particle size (median diameter (D50)). The median diameter (D50) referred to here refers to the particle diameter at which the cumulative volume becomes 50%.
如表1所示般,使用以直徑2mm的氧化鋯球作為粉碎媒體的籃式研磨機(basket mill)裝置、或以直徑0.5mm的氧化鋯球作為粉碎媒體的珠磨機(Bead mill)裝置,60分鐘,將粉碎後的氧化鋯粉末、氧化銦粉末及氧化矽粉末的各原料粉末予以濕式粉碎混合。 利用乾燥機來使取得的糊狀物乾燥,取得燒結原料粉。另外,將取得的燒結原料粉的最大粒徑及平均粒徑(中值徑(D50))顯示於表1。測定方法是與氧化鋯粉末的情況同樣。As shown in Table 1, use a basket mill device using zirconia balls with a diameter of 2 mm as the pulverizing medium, or a bead mill device using zirconia balls with a diameter of 0.5 mm as the pulverizing medium , 60 minutes, the pulverized zirconia powder, indium oxide powder and silicon oxide powder each raw material powder is wet pulverized and mixed. A dryer is used to dry the obtained paste to obtain sintering raw material powder. In addition, Table 1 shows the maximum particle size and average particle size (median diameter (D50)) of the obtained sintering raw material powder. The measurement method is the same as in the case of zirconia powder.
又,測定氧化鋯粉末、氧化銦粉末、氧化矽粉末的平均粒徑比。將測定結果顯示於表1。 針對燒結原料粉,使用電子探針顯微分析(EPMA)裝置來攝取3張倍率3000倍的COMPO像(反射電子組成像),藉由畫像解析,求取氧化鋯粉末、氧化銦粉末、氧化矽粉末的平均粒徑,算出平均粒徑比。詳細是測定圓近似徑(成為粒子的面積S=πD2 /4的D),作為各粒子的粒徑。算出粒子的圓近似徑的個數平均,作為平均粒徑。In addition, the average particle size ratio of the zirconium oxide powder, indium oxide powder, and silicon oxide powder was measured. The measurement results are shown in Table 1. For the sintering raw material powder, an electron probe microanalysis (EPMA) device was used to capture 3 COMPO images (reflected electron composition images) with a magnification of 3000 times, and the zirconia powder, indium oxide powder, and silicon oxide were obtained by image analysis. The average particle diameter of the powder is calculated, and the average particle diameter ratio is calculated. In detail, the approximate diameter of the circle ( D where the area S=πD 2 /4 becomes the particle) is measured as the particle diameter of each particle. The number average of the approximate circle diameters of the particles is calculated and used as the average particle diameter.
然後,在本發明例1~6,10~12及比較例1中,將取得的燒結原料粉予以沖壓成形而取得矩形平板型的成形體。另外,成形模的大小是設為165mm×298mm。並且,將加壓壓力設為98MPa。 在本發明例7~9及比較例2中,將取得的燒結原料粉予以CIP(冷均壓(Cold Isostatic Pressing))而取得圓筒型的成形體。另外,成形模的大小是設為外徑205mm、內徑165 mm、高度200mm。並且,將加壓壓力設為98MPa。Then, in Examples 1 to 6, 10 to 12, and Comparative Example 1 of the present invention, the obtained sintered raw material powder was press-formed to obtain a rectangular flat-shaped molded body. In addition, the size of the forming mold is 165 mm×298 mm. In addition, the pressurizing pressure was set to 98 MPa. In Examples 7 to 9 of the present invention and Comparative Example 2, the obtained sintering raw material powder was subjected to CIP (Cold Isostatic Pressing) to obtain a cylindrical molded body. In addition, the size of the forming mold is set to have an outer diameter of 205 mm, an inner diameter of 165 mm, and a height of 200 mm. In addition, the pressurizing pressure was set to 98 MPa.
然後,將取得的成形體裝入至具有氧導入機能的燒製裝置內(裝置內容積27000cm3 ),邊導入氧,邊加熱燒結。此時,氧的導入量是設為6L/分。又,將昇溫速度是設為120℃/h。 然後,在燒結的昇溫時,以記載於表2所示的項目“保持”的條件來進行溫度保持。其次,以記載於表2所示的項目“正式燒製”的條件來正式燒製,取得燒結體。Then, the obtained molded body was put into a sintering device having an oxygen introduction function (the internal volume of the device was 27000 cm 3 ), and the oxygen was introduced while heating and sintering. At this time, the amount of oxygen introduced was 6 L/min. In addition, the temperature increase rate was 120°C/h. Then, during the temperature increase of the sintering, the temperature was maintained under the conditions described in the item "Hold" shown in Table 2. Next, main firing was performed under the conditions of the item "main firing" shown in Table 2 to obtain a sintered body.
如上述般,對於取得的燒結體,實施機械加工,在本發明例1~6,10~12及比較例1中是取得126mm×178mm×厚度6mm的矩形平板型濺射靶。又,在本發明例7~9及比較例2中是取得外徑155mm、內徑135mm、高度150mm的圓筒型濺射靶。As described above, the obtained sintered body was subjected to mechanical processing. In Examples 1 to 6, 10 to 12 and Comparative Example 1 of the present invention, a rectangular flat sputtering target of 126 mm×178 mm×thickness 6 mm was obtained. In addition, in Examples 7 to 9 and Comparative Example 2 of the present invention, cylindrical sputtering targets with an outer diameter of 155 mm, an inner diameter of 135 mm, and a height of 150 mm were obtained.
另外,在比較例3中是將取得的燒結原料粉充填於直徑200mm的金屬模,以15MPa的壓力來沖壓,藉此製作2片直徑200mm、厚度10mm的圓板狀的成形體。 將取得的2片的成形體投入至電爐(爐內容積27000 cm3 ),邊以每分4L的流量來使氧流通至電爐內,邊以表2所示的燒製溫度來保持7小時,藉此燒製而使產生燒結體。其次,邊使氧繼續流通至電爐內,邊將燒結體冷卻至600℃。然後,停止氧的流通,藉由爐內放冷來冷卻至室溫。其次,從電爐取出燒結體。 對於上述般取得的燒結體,實施機械加工,取得直徑152.4mm、厚度6mm的2片的圓板狀的濺射靶。In Comparative Example 3, the obtained sintered raw material powder was filled in a mold with a diameter of 200 mm and punched with a pressure of 15 MPa to produce two disc-shaped molded bodies with a diameter of 200 mm and a thickness of 10 mm. The obtained two pieces of molded body were put into an electric furnace (furnace inner volume 27000 cm 3 ), and oxygen was circulated into the electric furnace at a flow rate of 4 L per minute, and the firing temperature shown in Table 2 was maintained for 7 hours. By this firing, a sintered body is produced. Next, while continuing to circulate oxygen into the electric furnace, the sintered body was cooled to 600°C. Then, the flow of oxygen was stopped, and the furnace was allowed to cool down to room temperature. Next, the sintered body is taken out from the electric furnace. The sintered body obtained as described above was subjected to machining to obtain two disc-shaped sputtering targets having a diameter of 152.4 mm and a thickness of 6 mm.
針對取得的氧化物濺射靶,評價有關以下的項目。將評價結果顯示於表2。For the obtained oxide sputtering target, the following items were evaluated. The evaluation results are shown in Table 2.
(金屬成分組成) 從被製作的氧化物濺射靶切出樣品而粉碎,以酸進行前處理。其次,藉由ICP-AES來分析Zr,Si,In的金屬成分,從取得的結果計算金屬成分的含有量。 另外,在表1中的“氧化物粉的混合組成”是將ZrO2 ,In2 O3 ,SiO2 的合計量設為100%,記載ZrO2 ,In2 O3 ,SiO2 的量。在表2中的“靶的金屬組成”是將Zr,Si,In的合計量設為100%,記載Zr,Si,In的量。(Metal component composition) A sample was cut out from the produced oxide sputtering target, pulverized, and pre-treated with acid. Next, the metal components of Zr, Si, and In are analyzed by ICP-AES, and the content of the metal components is calculated from the obtained results. In addition, in the "mixed composition of oxide powder" in Table 1, the total amount of ZrO 2 , In 2 O 3 , and SiO 2 is set to 100%, and the amounts of ZrO 2 , In 2 O 3 , and SiO 2 are described. The "metal composition of the target" in Table 2 is that the total amount of Zr, Si, and In is set to 100%, and the amounts of Zr, Si, and In are described.
(燒結體的粒徑) 從被製作的氧化物濺射靶切出樣品,以濕式研磨來進行研磨加工。其次,使用電子探針顯微分析(EPMA (electron probe micro analysis)裝置來攝取倍率3000倍(30 μm×40μm)的COMPO像。攝影是實施3片,根據攝影後的COMPO畫像,利用畫像處理來算出對於3片全體的各相(ZrO2 相、In2 O3 相、In2 SiO7 相)的結晶粒的最大粒徑及平均粒徑、靶全體的結晶粒的最大粒徑及平均粒徑。平均粒徑比是表示以In2 O3 相或In2 Si2 O7 相的平均粒徑除以ZrO2 相的平均粒徑的值。 在此所謂的粒徑是表示圓近似徑(成為結晶粒的面積S=πD2 /4的D)。平均粒徑是結晶粒的圓近似徑的個數平均。(Particle diameter of sintered body) A sample was cut out from the produced oxide sputtering target, and the polishing process was performed by wet polishing. Second, use an electron probe micro analysis (EPMA) device to capture a COMPO image with a magnification of 3000 times (30 μm×40 μm). The photography is performed on 3 pieces. Based on the COMPO image after shooting, the image processing is used. Calculate the maximum particle size and average particle size of the crystal grains of each phase (ZrO 2 phase, In 2 O 3 phase, In 2 SiO 7 phase) for the entire 3 pieces, and the maximum particle size and average particle size of the crystal grains of the entire target The average particle diameter ratio is a value obtained by dividing the average particle diameter of the In 2 O 3 phase or the In 2 Si 2 O 7 phase by the average particle diameter of the ZrO 2 phase. The area of the crystal grains S=πD 2 /4 D). The average particle size is the number average of the approximate circle diameter of the crystal grains.
(密度) 在矩形平板型濺射靶中,針對從中心部切出的10mm×10mm的試料測定尺寸密度。 在圓筒型濺射靶中,針對從軸線方向中心部切出的10mm×10mm的試料測定尺寸密度。將測定結果顯示於表2。(density) In a rectangular flat sputtering target, the dimensional density was measured for a sample of 10 mm×10 mm cut out from the center. In the cylindrical sputtering target, the dimensional density was measured for a sample of 10 mm×10 mm cut out from the center in the axial direction. The measurement results are shown in Table 2.
(強度) 與密度測定的情況同樣,從各濺射靶採取測定試料,根據JIS R 1601規格來測定三點彎曲強度。將評價結果顯示於表2。(strength) As in the case of density measurement, measurement samples were collected from each sputtering target, and the three-point bending strength was measured in accordance with the JIS R 1601 standard. The evaluation results are shown in Table 2.
(濺射成膜的破裂) 將濺射靶焊接於無氧銅製的支承板,予以安裝於磁控管式的濺射裝置(ULVAC公司製,SIH-450H)內。其次,以真空排氣裝置來將濺射裝置內排氣至5×10-5 Pa以下。其次,導入Ar氣體及O2 氣體,將濺射氣體壓調整成0.67Pa,實施1小時的預濺射。藉此,除去靶表面的加工層。此時的Ar氣體與O2 氣體的流量比是47對3,電力是設為DC1200W。 其次,以同樣的濺射條件,在玻璃基板上形成氧化物膜。然後,將濺射裝置大氣開放。然後,從濺射裝置取出濺射靶,目視觀察其外觀,確認破裂的發生的有無。將其結果顯示於表2。(Cracking of sputtering film formation) The sputtering target was welded to a support plate made of oxygen-free copper and installed in a magnetron-type sputtering device (manufactured by ULVAC, SIH-450H). Next, the inside of the sputtering device is evacuated to 5×10 -5 Pa or less with a vacuum exhaust device. Next, Ar gas and O 2 gas were introduced, the sputtering gas pressure was adjusted to 0.67 Pa, and pre-sputtering was performed for 1 hour. Thereby, the processed layer on the surface of the target is removed. The flow ratio of Ar gas to O 2 gas at this time is 47 to 3, and the electric power is set to DC1200W. Next, under the same sputtering conditions, an oxide film was formed on the glass substrate. Then, the sputtering device was opened to the atmosphere. Then, the sputtering target was taken out from the sputtering device, and its appearance was visually observed to confirm the occurrence of cracks. The results are shown in Table 2.
在比較例1~3是未實施預備粉碎工程,氧化鋯粉的最大粒徑超過4μm。在該等比較例1~3中,皆是ZrO2 相的最大粒徑超過10μm,在濺射成膜時發生破裂。In Comparative Examples 1 to 3, the preliminary pulverization process was not implemented, and the maximum particle size of the zirconia powder exceeded 4 μm. In these Comparative Examples 1 to 3, the maximum particle size of the ZrO 2 phase exceeded 10 μm, and cracks occurred during sputtering film formation.
相對於此,在本發明例1~12中,實施預備粉碎工程,氧化鋯粉的最大粒徑為4μm以下。在該等本發明例1~12中,皆是ZrO2 相的最大粒徑為10μm以下,在濺射成膜時不發生破裂,可安定進行成膜。 又,本發明例2~7,9~11中,氧化鋯相的平均粒徑DZrO 與其他的氧化物相的氧化銦相的平均粒徑DInO 的比DInO /DZrO 及氧化鋯相的平均粒徑DZrO 與其他的氧化物相的複合氧化物相的平均粒徑DInSiO 的比DInSiO /DZrO 分別為0.6以上1.8以下的範圍內,且在靶組織全體的最大粒徑為7μm以下,平均粒徑為4μm以下。在該等本發明例2~7,9~11中,靶的強度會更提升。In contrast, in Examples 1 to 12 of the present invention, the preliminary grinding process was performed, and the maximum particle size of the zirconia powder was 4 μm or less. In the examples 1 to 12 of the present invention, the maximum particle size of the ZrO 2 phase is 10 μm or less, and the film does not crack during sputtering film formation, and the film can be formed stably. In addition, in Examples 2-7 and 9-11 of the present invention, the ratio of the average particle size D ZrO of the zirconia phase to the average particle size D InO of the indium oxide phase of the other oxide phase D InO /D ZrO and the zirconia phase The ratio of the average particle size of D ZrO to the average particle size of the composite oxide phase D InSiO of other oxide phases D InSiO /D ZrO is in the range of 0.6 or more and 1.8 or less, and the maximum particle size of the entire target structure is 7μm or less, the average particle size is 4μm or less. In the examples 2-7, 9-11 of the present invention, the strength of the target will be more improved.
以上,若根據本發明例,則被確認可提供一種即使是以高輸出濺射成膜的情況,也可抑制破裂的發生,可安定且生產效率佳進行濺射成膜之氧化物濺射靶及此氧化物濺射靶的製造方法。 [產業上的利用可能性]As mentioned above, according to the example of the present invention, it has been confirmed that it is possible to provide an oxide sputtering target capable of suppressing the occurrence of cracks even in the case of high-output sputtering film formation, and capable of performing sputtering film formation with stability and high production efficiency. And the manufacturing method of the oxide sputtering target. [Industrial Utilization Possibility]
本實施形態的氧化物濺射靶是可適用在以濺射法來製造作為液晶顯示器面板、有機EL顯示器面板、觸控面板等的顯示器面板的屏蔽層或相變化型光碟的介電質層或保護膜使用的含有鋯、矽及銦的氧化物膜之工程。The oxide sputtering target of this embodiment is applicable to the production of a shielding layer of a display panel such as a liquid crystal display panel, an organic EL display panel, a touch panel, or the dielectric layer of a phase change optical disc by a sputtering method. Process of oxide film containing zirconium, silicon and indium used in protective film.
11:氧化鋯相 12:氧化銦相 13:複合氧化物相 S01:預備粉碎工程 S02:燒結原料粉形成工程 S03:成形工程 S04:燒結工程 S05:機械加工工程11: Zirconia phase 12: Indium oxide phase 13: Complex oxide phase S01: Preparatory crushing project S02: Sintering raw material powder formation process S03: Forming Engineering S04: Sintering Engineering S05: Mechanical Processing Engineering
[圖1]是本發明之一實施形態的氧化物濺射靶的組織觀察照片。 [圖2]是表示本發明之一實施形態的氧化物濺射靶的製造方法的流程圖。[Fig. 1] is a photograph of the structure observation of an oxide sputtering target according to an embodiment of the present invention. Fig. 2 is a flowchart showing a method of manufacturing an oxide sputtering target according to an embodiment of the present invention.
11:氧化鋯相 11: Zirconia phase
12:氧化銦相 12: Indium oxide phase
13:複合氧化物相 13: Complex oxide phase
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