TW201636444A - Ruthenium-based target and intermediate layer for magnetic recording media - Google Patents

Ruthenium-based target and intermediate layer for magnetic recording media Download PDF

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TW201636444A
TW201636444A TW104110704A TW104110704A TW201636444A TW 201636444 A TW201636444 A TW 201636444A TW 104110704 A TW104110704 A TW 104110704A TW 104110704 A TW104110704 A TW 104110704A TW 201636444 A TW201636444 A TW 201636444A
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ruthenium
based target
oxide
magnetic recording
target
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TW104110704A
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黃至良
薛永浚
蔡登安
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光洋應用材料科技股份有限公司
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Abstract

Provided is a ruthenium-based target, comprising a base phase of ruthenium and an amorphous phase of a first oxide selected from the group consisting of: MgB4O7, Mg2B2O5, Mg3B2O6, and any combination thereof. An intermediate layer sputtered from the ruthenium-based target is also provided for magnetic recording media. Since a recording layer formed on the intermediate layer has been proved to have an excellent crystalline orientation texture, the magnetocrystalline anisotropy and coercivity of the recording layer are improved, and the signal to noise ratio and the areal recording density of the magnetic recording media are also increased. Accordingly, the demands of high-density magnetic recording media are met.

Description

釕基靶材及用於磁記錄媒體的中間膜Thiol-based target and interlayer film for magnetic recording medium

本發明係關於一種釕基靶材及用於磁記錄媒體的中間膜。The present invention relates to a ruthenium-based target and an intermediate film for a magnetic recording medium.

由含有鈷、鉻、鈦、鉭、矽、鎢、銅、鎂、鋯、錳、釔、鋁、鐵、鉬及硼中至少一者與釕的釕基合金或純釕,進一步與含有二氧化矽(SiO2 )、二氧化鈦(TiO2 )、一氧化鈷(CoO)、二氧化鈷(CoO2 )、二氧化鎢(WO2 )及五氧化二鉭(Ta2 O5 )中至少一者的氧化物所構成的釕基材料(ruthenium-based materials),經常被用於作為垂直式磁記錄媒體中的中間膜,以輔助垂直式磁記錄媒體的記錄膜之磁性晶粒的結晶定向組織(crystalline orientation texture)及控制磁性晶粒的晶粒尺寸,從而提高該記錄膜之磁矯頑性(Hc)及磁晶異向性常數(magnetocrystalline anisotropy,Ku),使該記錄膜的磁交換去耦合的均一性提昇及位元錯誤率(bit error ratio,BER)降低,並使該磁記錄媒體的訊雜比(signal to noise ratio,SNR)及面記錄密度(areal recording density)提高。a ruthenium-based alloy or pure ruthenium containing at least one of cobalt, chromium, titanium, niobium, tantalum, tungsten, copper, magnesium, zirconium, manganese, lanthanum, aluminum, iron, molybdenum, and boron, and further containing oxidizing At least one of cerium (SiO 2 ), titanium oxide (TiO 2 ), cobalt monoxide (CoO), cobalt dioxide (CoO 2 ), tungsten dioxide (WO 2 ), and tantalum pentoxide (Ta 2 O 5 ) Ruthenium-based materials composed of oxides are often used as intermediate films in vertical magnetic recording media to assist in crystallographically oriented microstructure of magnetic grains of a recording film of a vertical magnetic recording medium. Orientation texture) and controlling the grain size of the magnetic crystal grains, thereby increasing the magnetic coercivity (Hc) and magnetocrystalline anisotropy (Ku) of the recording film, decoupling the magnetic exchange of the recording film The uniformity improvement and the bit error ratio (BER) are lowered, and the signal to noise ratio (SNR) and the areal recording density of the magnetic recording medium are improved.

然而,對於該記錄膜而言,藉由含有前述氧化物的釕基材料所形成的中間膜得到的結晶定向組織、磁晶異向性能與磁矯頑性的改善空間仍然不足,則無法符合目前對於高密度磁記錄媒體的要求。However, for the recording film, the space for the oriented structure, the magnetocrystalline anisotropy, and the magnetic coercivity which are obtained by the interlayer film formed of the ruthenium-based material containing the foregoing oxide are still insufficient, and thus it is not in conformity with the current Requirements for high density magnetic recording media.

有鑒於上述現有技術之缺點,本發明之目的在於有效輔助記錄膜的結晶定向組織,從而提升記錄膜的磁晶異向性能與磁矯頑性,並提高磁記錄媒體的訊雜比及面記錄密度,進而符合高密度磁記錄媒體之需求。In view of the above disadvantages of the prior art, the object of the present invention is to effectively assist the crystal orientation structure of the recording film, thereby improving the magnetic crystal anisotropy performance and magnetic coercivity of the recording film, and improving the signal-to-noise ratio and surface recording of the magnetic recording medium. Density, which in turn meets the needs of high density magnetic recording media.

為了達到前述發明目的,本發明所採取之一技術手段係提供一種釕基靶材,其中包含:一基相,其中包含有釕;以及一非晶形相,其中包含有一第一氧化物,該第一氧化物係選自由MgB4 O7 、Mg2 B2 O5 、Mg3 B2 O6 及其組合所構成之群組。In order to achieve the foregoing object, one of the technical means adopted by the present invention is to provide a ruthenium-based target comprising: a base phase containing ruthenium; and an amorphous phase containing a first oxide, the first The monooxide is selected from the group consisting of MgB 4 O 7 , Mg 2 B 2 O 5 , Mg 3 B 2 O 6 , and combinations thereof.

所述釕基靶材於高溫真空熱壓製程後,由MgB4 O7 、Mg2 B2 O5 、Mg3 B2 O6 或其組合所構成的非晶形相係均勻分布於基相中且細小,並具有良好的高溫穩定性,能預防濺鍍時電弧現象的產生,並提升濺鍍的穩定性及產品的良率。After the ruthenium-based target is subjected to a high-temperature vacuum heat-pressing process, an amorphous phase composed of MgB 4 O 7 , Mg 2 B 2 O 5 , Mg 3 B 2 O 6 or a combination thereof is uniformly distributed in the base phase and It is small and has good high temperature stability. It can prevent the occurrence of arcing during sputtering and improve the stability of sputtering and the yield of products.

較佳的是,所述釕基靶材之第一氧化物之含量佔整體釕基靶材之0.1莫耳百分比(mole percentage,mol.%)至9莫耳百分比。較佳的是,所述釕基靶材之第一氧化物之含量佔整體釕基靶材之1莫耳百分比至8莫耳百分比。更佳的是,所述釕基靶材之第一氧化物之含量佔整體釕基靶材之3莫耳百分比至6莫耳百分比。Preferably, the first oxide of the ruthenium-based target is present in an amount of from 0.1 mole percent to 9 mole percent of the overall ruthenium base target. Preferably, the first oxide of the ruthenium-based target is present in an amount from 1 mole percent to 8 mole percent of the overall ruthenium base target. More preferably, the first oxide of the ruthenium-based target is present in an amount from 3 moles to 6 mole percent of the overall ruthenium-based target.

較佳的是,所述釕基靶材之基相包含至少一選自於由鈷、鉻、鈦、鉭、矽、鎢、銅、鎂、鋯、錳、釔、鋁、鐵、鉬及硼所構成之群組中之元素。更佳的是,所述釕基靶材之基相包含鈷或鉻或鈦。再更佳的是,該基相包含釕鈷合金、釕鈷鉻合金或釕鉻合金或釕鈦合金。Preferably, the base phase of the ruthenium-based target comprises at least one selected from the group consisting of cobalt, chromium, titanium, niobium, tantalum, tungsten, copper, magnesium, zirconium, manganese, lanthanum, aluminum, iron, molybdenum and boron. The elements in the group formed. More preferably, the base phase of the ruthenium based target comprises cobalt or chromium or titanium. More preferably, the base phase comprises a samarium cobalt alloy, a samarium cobalt chrome alloy or a ruthenium chrome alloy or a niobium titanium alloy.

較佳的是,所述釕基靶材之基相中所含之元素的含量和佔整體釕基靶材之10莫耳百分比至70莫耳百分比。Preferably, the content of the elements contained in the base phase of the ruthenium-based target is from 10 mole percent to 70 mole percent of the total ruthenium base target.

較佳的是,所述釕基靶材進一步包含有一第二氧化物,該第二氧化物係包含至少一選自於由矽、鈦、鉻、鎢、鋁、鎵、鎂、鉬、錳、釔、鋯、鐵、鋅及鉭所構成之群組中之元素。Preferably, the ruthenium-based target further comprises a second oxide, the second oxide comprising at least one selected from the group consisting of niobium, titanium, chromium, tungsten, aluminum, gallium, magnesium, molybdenum, manganese, An element of a group consisting of cerium, zirconium, iron, zinc, and cerium.

較佳的是,所述釕基靶材之第二氧化物占整體釕基靶材之1.5莫耳百分比至24莫耳百分比。較佳的是,所述釕基靶材之第二氧化物占整體釕基靶材之8莫耳百分比至24莫耳百分比。Preferably, the second oxide of the ruthenium based target comprises from 1.5 mole percent to 24 mole percent of the overall ruthenium based target. Preferably, the second oxide of the ruthenium based target comprises from 8 mole percent to 24 mole percent of the overall ruthenium based target.

同樣為了達到前述之發明目的,本發明所採取之另一技術手段係提供一種用於磁記錄媒體的中間膜,其中包含:一基相,其中包含有釕;以及一非晶形相,其中包含有一第一氧化物,該第一氧化物係選自由MgB4 O7 、Mg2 B2 O5 、Mg3 B2 O6 及其組合所構成之群組。Also in order to achieve the foregoing object, another technical means adopted by the present invention is to provide an intermediate film for a magnetic recording medium comprising: a base phase containing germanium; and an amorphous phase including one The first oxide is selected from the group consisting of MgB 4 O 7 , Mg 2 B 2 O 5 , Mg 3 B 2 O 6 , and combinations thereof.

藉由由MgB4 O7 、Mg2 B2 O5 、Mg3 B2 O6 或其組合所構成的非晶形相,所述中間膜的釕的基相之晶粒性能適當地被包覆,令所述中間膜能提供更為優越的結晶定向效果給形成於所述中間膜上的記錄膜,使得該記錄膜結晶定向組織、磁晶異向性能與磁矯頑性良好,並能優化由該中間膜及記錄膜所製得的磁記錄媒體的訊雜比及面記錄密度。By the amorphous phase composed of MgB 4 O 7 , Mg 2 B 2 O 5 , Mg 3 B 2 O 6 or a combination thereof, the grain properties of the ruthenium base phase of the intermediate film are appropriately coated, The intermediate film can provide a superior crystal orientation effect to the recording film formed on the intermediate film, so that the recording film crystal orientation structure, magnetic crystal anisotropy performance and magnetic coercivity are good, and can be optimized by The signal-to-noise ratio and the surface recording density of the magnetic recording medium produced by the interlayer film and the recording film.

較佳的是,所述中間膜的第一氧化物之含量佔整體釕基靶材之0.1莫耳百分比(mole percentage,mol.%)至9莫耳百分比。較佳的是,所述釕基靶材之第一氧化物之含量佔整體釕基靶材之1莫耳百分比至8莫耳。更佳的是,所述中間膜的第一氧化物之含量佔整體中間膜的之3莫耳百分比至6莫耳百分比。藉此,所述中間膜的非晶項能具有更優良的高潤濕性,使中間膜能具有較佳結晶定向組織,以更為有效地輔助垂直式磁記錄媒體的記錄膜之磁性晶粒的結晶定向組織,並提升記錄膜的磁晶異向性能與磁矯頑性,提高磁記錄媒體的訊雜比及面記錄密度。Preferably, the content of the first oxide of the intermediate film is from 0.1 mole percent (mol. percentage) to 9 mole percent of the overall ruthenium base target. Preferably, the first oxide of the ruthenium-based target is present in an amount from 1 mole to 8 moles of the total ruthenium-based target. More preferably, the content of the first oxide of the intermediate film is from 3 mole percent to 6 mole percent of the overall interlayer film. Thereby, the amorphous item of the intermediate film can have more excellent high wettability, so that the intermediate film can have a better crystal orientation structure to more effectively assist the magnetic grain of the recording film of the vertical magnetic recording medium. The crystal orientation structure improves the magnetic crystal anisotropy performance and magnetic coercivity of the recording film, and improves the signal-to-noise ratio and surface recording density of the magnetic recording medium.

較佳的是,所述釕基靶材之基相包含至少一選自於由鈷、鉻、鈦、鉭、矽、鎢、銅、鎂、鋯、錳、釔、鋁、鐵、鉬及硼所構成之群組中之元素。更佳的是,所述中間膜的基相包含鈷或鉻或鈦。更佳的是,該基相包含釕鈷合金、釕鈷鉻合金或釕鉻合金或釕鈦合金。Preferably, the base phase of the ruthenium-based target comprises at least one selected from the group consisting of cobalt, chromium, titanium, niobium, tantalum, tungsten, copper, magnesium, zirconium, manganese, lanthanum, aluminum, iron, molybdenum and boron. The elements in the group formed. More preferably, the base phase of the interlayer film comprises cobalt or chromium or titanium. More preferably, the base phase comprises a samarium cobalt alloy, a samarium cobalt chromium alloy or a niobium chromium alloy or a niobium titanium alloy.

較佳的是,所述釕基靶材之基相中所含之元素的含量和佔整體釕基靶材之10莫耳百分比至70莫耳百分比。Preferably, the content of the elements contained in the base phase of the ruthenium-based target is from 10 mole percent to 70 mole percent of the total ruthenium base target.

較佳的是,所述中間膜進一步包含有一第二氧化物,該第二氧化物係包含至少一選自於由矽、鈦、鉻、鎢、鋁、鎵、鎂、鉬、錳、釔、鋯、鐵、鋅及鉭所構成之群組中之元素。藉由該第二氧化物之添加,係能提供記錄膜所需的晶粒結晶定向組織。Preferably, the intermediate film further comprises a second oxide, the second oxide comprising at least one selected from the group consisting of niobium, titanium, chromium, tungsten, aluminum, gallium, magnesium, molybdenum, manganese, niobium, An element of a group consisting of zirconium, iron, zinc, and antimony. By the addition of the second oxide, it is possible to provide a crystal grain oriented structure required for the recording film.

較佳的是,所述中間膜的第二氧化物占整體釕基靶材之1.5莫耳百分比至24莫耳百分比。更佳的是,所述中間膜的第二氧化物占整體釕基靶材之8莫耳百分比至24莫耳百分比。Preferably, the second oxide of the interlayer film comprises from 1.5 mole percent to 24 mole percent of the overall ruthenium based target. More preferably, the second oxide of the interlayer film comprises from 8 mole percent to 24 mole percent of the overall ruthenium based target.

較佳的是,所述中間膜係由所述釕基靶材經由濺鍍製程所製成。可選用之濺鍍製程例如:磁控濺鍍製程、電子電漿製程、離子束濺鍍製程,但並非僅限於此。Preferably, the intermediate film is made of the ruthenium-based target through a sputtering process. Optional sputtering processes such as, but not limited to, magnetron sputtering processes, electronic plasma processes, and ion beam sputtering processes.

據此,所述中間膜於濺鍍成形時係具有高度的濺鍍穩定性及良率,且其係具有MgB4 O7 、Mg2 B2 O5 、Mg3 B2 O6 或其組合所構成的非晶形相,則能提供更為優越的結晶定向效果給形成於所述中間膜上的記錄膜,提升該記錄膜結晶定向組織、磁晶異向性能與磁矯頑性,使得由該中間膜及記錄膜所製得的磁記錄媒體係能具有符合高密度磁記錄媒體之要求的訊雜比及面記錄密度。Accordingly, the interlayer film has high sputter stability and yield during sputtering, and has MgB 4 O 7 , Mg 2 B 2 O 5 , Mg 3 B 2 O 6 or a combination thereof. The amorphous phase formed can provide a more superior crystal orientation effect to the recording film formed on the intermediate film, and enhance the crystal orientation structure, magnetocrystalline anisotropy performance and magnetic coercivity of the recording film, so that The magnetic recording medium produced by the interlayer film and the recording film can have a signal-to-noise ratio and a surface recording density which meet the requirements of a high-density magnetic recording medium.

以下,將藉由下列具體實施例詳細說明本發明的實施方式,所屬技術領域具有通常知識者可經由本說明書之內容輕易地了解本發明所能達成之優點與功效,並且於不悖離本發明之精神下進行各種修飾與變更,以施行或應用本發明之內容。In the following, embodiments of the present invention will be described in detail by the following specific embodiments, and those skilled in the art can readily understand the advantages and functions of the present invention, and without departing from the invention. Various modifications and changes are made in the spirit of the invention to practice or apply the invention.

實施例Example 11 to 66 :釕基靶材之製備及分析: Preparation and analysis of ruthenium-based targets

實施例1至6的釕基靶材之製備如下所述: 將一金屬粉末與一第一氧化物混合及球磨後得到一混合粉末。然後,令該混合粉末於650°C之溫度及760巴(bar)之壓力下進行氫氣還原2小時得到一還原粉末。接著,令該還原粉末於經高速研磨機研磨2小時至4小時後,均勻填充於一石墨模具中並施予一來自於一油壓機且為300磅/平方英寸(psi)的壓力,以形成一初胚。再將該初胚與該石墨模具一同放入一熱壓爐中,以1000°C至1200°C之燒結溫度及422巴(bar)之燒結壓力持續燒結3小時,得到各實施例的釕基靶材。The preparation of the ruthenium-based targets of Examples 1 to 6 was as follows: A metal powder was mixed with a first oxide and ball-milled to obtain a mixed powder. Then, the mixed powder was subjected to hydrogen reduction at a temperature of 650 ° C and a pressure of 760 bar for 2 hours to obtain a reduced powder. Next, the reduced powder is ground in a high speed grinder for 2 hours to 4 hours, uniformly filled in a graphite mold and applied to a hydraulic press at a pressure of 300 psi to form a Early embryo. The priming embryo was placed in a hot press furnace together with the graphite mold, and sintered at a sintering temperature of 1000 ° C to 1200 ° C and a sintering pressure of 422 bar for 3 hours to obtain a sulfhydryl group of each example. Target.

實施例1至6的金屬粉末之組份、第一氧化物的組份、金屬粉末與第一氧化物之莫耳比、還原粉末之研磨時間、初胚的燒結溫度及初胚的燒結時間示於表1中。The components of the metal powder of Examples 1 to 6, the composition of the first oxide, the molar ratio of the metal powder to the first oxide, the grinding time of the reduced powder, the sintering temperature of the blast, and the sintering time of the blast In Table 1.

實施例2至5與實施例1及6之釕基靶材之製備不同處如下所述: 於實施例2至5中,該金屬粉末與該第一氧化物係進一步與一第二氧化物混合;接著,實施例2至5係令混合後的金屬粉末、第一氧化物與第二氧化物經球磨後得到實施例2至5之混合粉末。The preparation of the ruthenium-based targets of Examples 2 to 5 and Examples 1 and 6 is different as follows: In Examples 2 to 5, the metal powder and the first oxide system are further mixed with a second oxide. Next, Examples 2 to 5 obtained the mixed metal powder, the first oxide and the second oxide by ball milling to obtain the mixed powder of Examples 2 to 5.

實施例2至5之第二氧化物的組份及金屬粉末、第一氧化物與第二氧化物之莫耳比示於表2中。The components of the second oxide of Examples 2 to 5 and the metal powder, the molar ratio of the first oxide to the second oxide are shown in Table 2.

以感應耦合電漿光譜儀(inductively coupled plasma spectrometer (ICP),廠牌:Perkin Elmer,型號:5300DV)分析實施例1至6的之釕基靶材之成份,分析結果示於表3中。The components of the ruthenium-based targets of Examples 1 to 6 were analyzed by an inductively coupled plasma spectrometer (ICP), brand: Perkin Elmer, model: 5300 DV, and the results of the analysis are shown in Table 3.

參閱圖1至6所示為利用掃描式電子顯微鏡(scanning electronic microscopy,SEM,廠牌:Hitachi,型號:3400N,加速電壓:15千伏特,工作距離:3釐米)分析實施例1至6之釕基靶材所得到的金相圖。由圖1至6可觀察到各實施例之釕基靶材中主要含有一淺色相與一深色相,並請參閱表4所示,經由能量分散元素分析光譜儀(Energy Dispersive Spectrometer,EDS)結果證實,各實施例之淺色相係由各實施例之金屬粉末所構成的含有釕的基相;實施例1及6之深色相係分別由實施例1及6之第一氧化物所構成的第一氧化物相;實施例2至5之深色相係個別由實施例2至5之第一氧化物所構成的第一氧化物相與第二氧化物所構成的第二氧化物相所組成。Referring to Figures 1 to 6, the analysis of Examples 1 to 6 was carried out using a scanning electron microscopy (SEM, brand: Hitachi, model: 3400N, accelerating voltage: 15 kV, working distance: 3 cm). A metallographic diagram obtained from a base target. It can be observed from FIGS. 1 to 6 that the ruthenium-based target of each embodiment mainly contains a light-colored phase and a dark-colored phase, and is shown in Table 4, and an Energy Dispersive Spectrometer (EDS) result is obtained. It was confirmed that the pale phase of each example was a base containing ruthenium composed of the metal powder of each example; the dark phase of Examples 1 and 6 was composed of the first oxides of Examples 1 and 6, respectively. The first oxide phase; the dark phase of Examples 2 to 5 is a second oxide phase composed of the first oxide phase and the second oxide composed of the first oxides of Examples 2 to 5 composition.

請參閱圖1至6所示,各實施例之含有釕的基相中並未發現有鎂原子或硼原子固溶的現象。且如表4中所示,透過EDS分析,於含有釕的基相(淺色相)並未檢測到鎂原子或硼原子,證實各實施例之釕基靶材係含有具備良好高溫穩定性的第一氧化物相,且該第一氧化物相並不會與所述含有釕的基相產生固溶的現象。再者,從圖1至6可觀察到各實施例之深色相具有分佈均勻於淺色相中且細小之特點,故有助於各實施例之釕基靶材於濺鍍時避免產生電弧現象,進而提高濺鍍的穩定性及其所濺鍍而成之中間膜的良率。Referring to Figs. 1 to 6, the phenomenon in which the magnesium atom or the boron atom was solid-solved was not observed in the ruthenium-containing base phase of each of the examples. As shown in Table 4, by the EDS analysis, no magnesium atom or boron atom was detected in the base phase (light phase) containing ruthenium, and it was confirmed that the ruthenium-based target of each example contained a good high-temperature stability. A mono-oxide phase, and the first oxide phase does not cause solid solution with the ruthenium-containing base phase. Furthermore, it can be observed from FIGS. 1 to 6 that the dark phase of each embodiment has a uniform distribution in the light phase and is fine, so that the ruthenium-based target of each embodiment can be prevented from arcing during sputtering. In turn, the stability of the sputtering and the yield of the sputtered interlayer film are improved.

以X光繞射儀[X-ray diffractometer (XRD),廠牌:Rigaku,型號:Ultima IV,採用Cu的Kα射線掃描條件為每分鐘6度的速度由2θ=20度掃描至2θ=80度]量測實施例1及4至6之釕基靶材的X光繞射光譜,並將各實施例之X光繞射光譜與國際粉末繞射委員會(joint committee of powder diffraction standard,JCPDS)的繞射資料檔(powder diffraction file,PDF)進行比對,實施例1及4至6之X光繞射光譜與比對結果如圖7至12所示。X-ray diffractometer (XRD), label: Rigaku, model: Ultima IV, scanning with Kα ray of Cu at a speed of 6 degrees per minute from 2θ=20 degrees to 2θ=80 degrees The X-ray diffraction spectra of the ruthenium-based targets of Examples 1 and 4 to 6 were measured, and the X-ray diffraction spectra of the respective examples were compared with the joint committee of powder diffraction standard (JCPDS). The diffraction diffracted data (PDF) was compared. The X-ray diffraction spectra and alignment results of Examples 1 and 4 to 6 are shown in FIGS. 7 to 12.

請參閱圖7至12所示,實施例1-5的釕基靶材的X光繞射光譜的特徵峰並未與Mg2 B2 O5 晶體的X光繞射光譜(編號86-0531)的特徵峰相匹配,且實施例6的釕基靶材的X光繞射光譜的特徵峰並未與MgB4 O7 晶體的X光繞射光譜(編號31-0787)的特徵峰相匹配。而實施例1及6的釕基靶材的X光繞射光譜的特徵峰係與釕晶體之X光繞射光譜(編號70-0274)的特徵峰相匹配,實施例2至5的釕基靶材的X光繞射光譜的一部分特徵峰與釕晶體的X光繞射光譜(編號70-0274)的特徵峰、鉻晶體的X光繞射光譜(編號88-2323)的特徵峰及鈷晶體的X光繞射光譜(編號15-0806)的特徵峰相匹配。並且,依據圖1至6及前述EDS分析結果:實施例1至6之釕基靶材包含有由釕或釕、鈷與鉻所構成的基相及Mg2 B2 O5 或MgB4 O7 所構成的第一氧化物相。且由此可知,於燒結後實施例1至6的釕基靶材中的Mg2 B2 O5 或MgB4 O7 的晶體結構為非晶,亦即,於燒結後實施例1至6的釕基靶材之第一氧化物相為非晶相。因此,實施例1至6的釕基靶材包含有由釕或釕、鈷與鉻所構成的基相及由Mg2 B2 O5 或MgB4 O7 所構成的非晶相。7 to 12, the characteristic peaks of the X-ray diffraction spectrum of the ruthenium-based target of Examples 1-5 are not the X-ray diffraction spectrum of the Mg 2 B 2 O 5 crystal (No. 86-0531). The characteristic peaks were matched, and the characteristic peak of the X-ray diffraction spectrum of the ruthenium-based target of Example 6 did not match the characteristic peak of the X-ray diffraction spectrum (No. 31-0787) of the MgB 4 O 7 crystal. The characteristic peaks of the X-ray diffraction spectrum of the ruthenium-based targets of Examples 1 and 6 matched the characteristic peaks of the X-ray diffraction spectrum (No. 70-0274) of the ruthenium crystal, and the ruthenium groups of Examples 2 to 5 The characteristic peak of a part of the characteristic peak of the X-ray diffraction spectrum of the target and the X-ray diffraction spectrum of the ytterbium crystal (No. 70-0274), the characteristic peak of the X-ray diffraction spectrum of the chromium crystal (No. 88-2323), and cobalt The characteristic peaks of the X-ray diffraction spectrum (No. 15-0806) of the crystal match. Further, according to the results of FIGS. 1 to 6 and the aforementioned EDS analysis, the ruthenium base materials of Examples 1 to 6 comprise a base phase composed of ruthenium or osmium, cobalt and chromium, and Mg 2 B 2 O 5 or MgB 4 O 7 . The first oxide phase is formed. It can be seen from this that the crystal structure of Mg 2 B 2 O 5 or MgB 4 O 7 in the ruthenium-based targets of Examples 1 to 6 after sintering is amorphous, that is, after sintering, Examples 1 to 6 The first oxide phase of the ruthenium based target is an amorphous phase. Therefore, the ruthenium-based targets of Examples 1 to 6 contain a base phase composed of ruthenium or osmium, cobalt and chromium, and an amorphous phase composed of Mg 2 B 2 O 5 or MgB 4 O 7 .

比較例Comparative example 11 :現有釕基靶材與實施例: Existing bismuth-based targets and examples 11 and 66 之釕基靶材之比較Comparison of bismuth-based targets

本比較例中係以一現有釕基靶材與實施例1及6之釕基靶材進行比較,本比較例之現有釕基靶材係由釕與三氧化二硼(B2 O3 )以92.50:7.50之莫耳比例所製成。In this comparative example, a conventional ruthenium-based target was compared with the ruthenium-based targets of Examples 1 and 6. The conventional ruthenium-based target of the comparative example was made of ruthenium and boron trioxide (B 2 O 3 ). 92.50: 7.50 molar ratio made.

圖13至15所示依序為實施例1之釕基靶材、實施例6之釕基靶材及本比較例之現有釕基靶材個別經濺鍍製成的中間膜之穿透式電子顯微鏡(TEM)圖。其中,本比較例之現有釕基靶材個別經濺鍍製成的中間膜包含有一由釕所構成的基相10以及一由三氧化二硼所構成的三氧化二硼相11。13 to 15 are the through-type electrons of the interlayer film of the ruthenium-based target of Example 1, the ruthenium-based target of Example 6, and the conventional ruthenium-based target of the comparative example which were individually sputter-sputtered. Microscope (TEM) image. The intermediate film formed by sputtering of the conventional ruthenium-based target of the comparative example comprises a base phase 10 composed of ruthenium and a boron trioxide phase 11 composed of boron trioxide.

由圖13至15可見,相較於本比較例之現有釕基靶材個別經濺鍍製成的中間膜之基相10的各晶粒100內的晶格排列而言,實施例1及6之釕基靶材所製得的中間膜的基相20、30的各晶粒200、300內的晶格排列較為有序,故實施例1及6之釕基靶材所製得的中間膜的基相20、300的結晶性顯然較本比較例之現有釕基靶材個別經濺鍍製成的中間膜之基相10為佳。As can be seen from Figs. 13 to 15, Examples 1 and 6 are compared with the lattice arrangement in the respective crystal grains 100 of the base phase 10 of the interlayer film which is separately sputter-plated by the prior art bismuth-based target of the comparative example. The lattice arrangement in the crystal grains 200, 300 of the base phases 20, 30 of the intermediate film obtained by the ruthenium-based target is relatively order, so the intermediate film prepared by the ruthenium-based targets of Examples 1 and 6 The crystallinity of the base phase 20, 300 is obviously better than the base phase 10 of the intermediate film which is separately sputtered from the prior art ruthenium base of the comparative example.

如圖13及14所示,由Mg2 B2 O5 或MgB4 O7 所構成的非晶相21、31位於基相20、30的兩相鄰晶粒200、300之間,即位於兩相鄰晶粒200、300的晶界上,並由各晶粒200、300的晶界係相當明顯可知非晶相21、31係完全包覆基相20、30的各晶粒200、300,可證實透過由Mg2 B2 O5 或MgB4 O7 所構成的非晶相21、31,係能令實施例1及6之釕基靶材所製得的中間膜的基相20、30的晶粒200、300係彼此獨立地分佈於中間膜內。如圖15所示,反觀本比較例之現有釕基靶材製成的中間膜,其三氧化二硼相11雖為非晶相,但由於三氧化二硼相11之濕潤性過佳,使得本比較例之現有釕基靶材製成的中間膜相較於實施例1及6之釕基靶材所製得的中間膜而言,除了基相10之晶粒分佈較為不均以外,基相10之平均晶粒尺寸之標準差也較大。As shown in FIGS. 13 and 14, the amorphous phases 21, 31 composed of Mg 2 B 2 O 5 or MgB 4 O 7 are located between two adjacent crystal grains 200, 300 of the base phases 20, 30, that is, at two The grain boundaries of the adjacent crystal grains 200 and 300 and the grain boundary of each of the crystal grains 200 and 300 are relatively obvious. It is understood that the amorphous phases 21 and 31 completely cover the respective crystal grains 200 and 300 of the base phases 20 and 30, It can be confirmed that the amorphous phase 21, 31 composed of Mg 2 B 2 O 5 or MgB 4 O 7 is the base phase 20, 30 of the intermediate film which can be obtained by the ruthenium-based targets of Examples 1 and 6. The crystal grains 200, 300 are distributed independently of each other in the intermediate film. As shown in FIG. 15, in contrast to the intermediate film made of the conventional ruthenium-based target of the comparative example, although the boron trioxide phase 11 is an amorphous phase, the wettability of the boron trioxide phase 11 is excellent. The intermediate film made of the conventional ruthenium-based target of the comparative example is more uneven than the intermediate film obtained by the ruthenium-based target of Examples 1 and 6, except that the grain distribution of the base phase 10 is relatively uneven. The standard deviation of the average grain size of phase 10 is also large.

進一步分別於本比較例之現有釕基靶材製成的中間膜及實施例1及6之釕基靶材所製得的中間膜上以於50標準毫升/分鐘(sccm)之氣體流量(使用氬氣)、20毫托(mTorr)之氣壓及200瓦(W)之濺鍍功率之條件下濺鍍成形一由同一鈷鉑合金靶材(CoPtX,X=Cr、B、Mo、Ti、Si、Ta、Ru)所構成的記錄膜,並以TEM分析之。請參閱圖16至18所示,相較於形成於本比較例之現有釕基靶材製成的中間膜上的記錄膜之晶粒分佈而言,形成於實施例1及6之釕基靶材所製得的中間膜上的記錄膜之晶粒分佈顯然較為均勻;如表5所示,實施例1及6之釕基靶材所製得的中間膜上的記錄膜之晶粒尺寸之標準差分別為0.69奈米及1.05奈米,顯然低於形成於本比較例之現有釕基靶材製成的中間膜上的記錄膜之2.90奈米。Further, a gas flow rate of 50 standard milliliters per minute (sccm) was used on the intermediate film made of the conventional ruthenium-based target of the comparative example and the ruthenium-based target of Examples 1 and 6 (using Sputtering a target of the same cobalt-platinum alloy target (CoPtX, X=Cr, B, Mo, Ti, Si under argon), 20 mTorr (mTorr) gas pressure and 200 W (W) sputtering power The recording film composed of Ta, Ru) was analyzed by TEM. Referring to FIGS. 16 to 18, the ruthenium-based targets formed in Examples 1 and 6 are compared with the grain distribution of the recording film formed on the interlayer film made of the conventional ruthenium-based target of the comparative example. The grain distribution of the recording film on the interlayer film prepared by the material is obviously uniform; as shown in Table 5, the grain size of the recording film on the interlayer film obtained by the ruthenium-based targets of Examples 1 and 6 The standard deviations were 0.69 nm and 1.05 nm, respectively, which were apparently lower than the 2.90 nm of the recording film formed on the interlayer film made of the conventional ruthenium-based target of this comparative example.

基於形成於本比較例之現有釕基靶材製成的中間膜與實施例1及6之釕基靶材所製得的中間膜上的記錄膜係以由同一鈷鉻鉑合金靶材經相同的濺鍍製程所構成,故由圖16至18及表5之結果可證實,相較本比較例之現有釕基靶材製成的中間膜而言,包含由釕所構成的基相及由Mg2 B2 O5 或MgB4 O7 所構成的非晶相之實施例1或6之釕基靶材製成的中間膜,係能提供更為優良的結晶定向效果給記錄膜,則能有效提升記錄膜之結晶定向組織、磁晶異向性能與磁矯頑性,從而提高磁記錄媒體的訊雜比及面記錄密度,進而達到高密度磁記錄媒體之要求。The recording film on the interlayer film prepared based on the intermediate film formed of the conventional ruthenium base material of the comparative example and the ruthenium base target of Examples 1 and 6 is the same as the same cobalt chrome platinum alloy target According to the results of the sputtering process, it can be confirmed from the results of FIGS. 16 to 18 and Table 5 that the intermediate film made of the conventional ruthenium-based target of the comparative example contains the base phase composed of ruthenium and An intermediate film made of the ruthenium-based target of Example 1 or 6 in an amorphous phase composed of Mg 2 B 2 O 5 or MgB 4 O 7 can provide a more excellent crystal orientation effect to the recording film, and The crystal orientation structure, the magnetocrystalline anisotropy performance and the magnetic coercivity of the recording film are effectively improved, thereby improving the signal-to-noise ratio and the surface recording density of the magnetic recording medium, thereby achieving the requirement of a high-density magnetic recording medium.

比較例Comparative example 22 :現有釕基靶材與實施例: Existing bismuth-based targets and examples 11 and 66 之釕基靶材之比較Comparison of bismuth-based targets

本比較例中係以一現有釕基靶材與實施例1及6之釕基靶材進行比較,本比較例之現有釕基靶材係由釕與五氧化二鉭(Ta2 O5 )以95.00:5.00之莫耳比例所製成。In the comparative example, a conventional ruthenium-based target was compared with the ruthenium-based targets of Examples 1 and 6. The conventional ruthenium-based target of the comparative example was made of ruthenium and tantalum pentoxide (Ta 2 O 5 ). Made with a molar ratio of 95.00:5.00.

圖19所示本比較例之現有釕基靶材經濺鍍製成的中間膜之穿透式電子顯微鏡(TEM)圖。其中,本比較例之現有釕基靶材個別經濺鍍製成的中間膜包含有一由釕所構成的基相40以及一由五氧化二鉭所構成的五氧化二鉭相41。Fig. 19 is a transmission electron microscope (TEM) image of an intermediate film formed by sputtering of the conventional ruthenium-based target of this comparative example. The intermediate film formed by sputtering of the prior art ruthenium-based target of the comparative example comprises a base phase 40 composed of tantalum and a tantalum pentoxide phase 41 composed of tantalum pentoxide.

由圖13、14及19可見,相較於本比較例之現有釕基靶材個別經濺鍍製成的中間膜之基相40的各晶粒400內的晶格排列而言,實施例1及6之釕基靶材所製得的中間膜的基相20、30的各晶粒200、300內的晶格排列較為有序,故實施例1及6之釕基靶材所製得的中間膜的基相20、30的結晶性顯然較本比較例之現有釕基靶材個別經濺鍍製成的中間膜之基相40為佳。As can be seen from Figures 13, 14 and 19, Example 1 is compared to the lattice arrangement in the respective crystal grains 400 of the base phase 40 of the intermediate film which is separately sputtered by the prior art bismuth-based target of the comparative example. And the lattice arrangement in the crystal grains 200 and 300 of the base phases 20 and 30 of the interlayer film prepared by the ruthenium-based target of 6 is relatively order, so that the ruthenium-based targets of Examples 1 and 6 are obtained. The crystallinity of the base phases 20, 30 of the interlayer film is preferably better than the base phase 40 of the interlayer film which is separately sputtered from the prior art ruthenium base of the comparative example.

如圖19所示,本比較例之現有釕基靶材製成的中間膜,其五氧化二鉭相41位於其基相40的兩相鄰晶粒400之間,即位於兩相鄰晶粒400的晶界上。如圖13、14及19所示,本比較例之現有釕基靶材製成的中間膜與實施例1及6之釕基靶材所製得的中間膜相比後,可見本比較例之現有釕基靶材製成的中間膜除了基相40之晶粒分佈較為不均以外,基相40之平均晶粒尺寸之標準差也較大。As shown in FIG. 19, the intermediate film made of the conventional ruthenium-based target of the comparative example has a ruthenium pentoxide phase 41 between two adjacent crystal grains 400 of the base phase 40, that is, located in two adjacent crystal grains. On the grain boundary of 400. As shown in FIGS. 13 , 14 and 19 , the intermediate film made of the conventional ruthenium-based target of the comparative example is compared with the intermediate film prepared by the ruthenium-based target of Examples 1 and 6, and the comparative example can be seen. The intermediate film made of the conventional ruthenium-based target has a larger standard deviation of the average grain size of the base phase 40 except that the grain distribution of the base phase 40 is relatively uneven.

於本比較例之現有釕基靶材製成的中間膜濺鍍成形一由鈷鉻鉑合金靶材所構成的記錄膜,並以TEM分析之;其中,形成本比較例之現有釕基靶材製成的中間膜上的記錄膜所使用的鈷鉻鉑合金靶材及製程參數係相同於形成於比較例1之現有釕基靶材製成的中間膜上的記錄膜,亦相同於形成於實施例1及6之釕基靶材所製得的中間膜上的記錄膜。A recording film composed of a cobalt-chromium-platinum alloy target was sputter-sputtered by an intermediate film made of the conventional ruthenium-based target of the comparative example, and analyzed by TEM; wherein the existing ruthenium-based target of the comparative example was formed. The cobalt chrome-platinum alloy target used in the recording film on the prepared intermediate film and the process parameters were the same as those of the recording film formed on the intermediate film made of the conventional ruthenium-based target of Comparative Example 1, and were also formed in the same manner. The recording film on the interlayer film prepared by the ruthenium base materials of Examples 1 and 6.

請參閱圖16、17及20所示,相較於形成於本比較例之現有釕基靶材製成的中間膜上的記錄膜而言,形成於實施例1及6之釕基靶材所製得的中間膜上的記錄膜之晶粒分佈顯然較為均勻;如表5所示,實施例1及6之釕基靶材所製得的中間膜上的記錄膜之晶粒尺寸之標準差分別為0.69奈米及1.05奈米,顯然低於形成於本比較例之現有釕基靶材製成的中間膜上的記錄膜之1.33奈米。Referring to FIGS. 16, 17, and 20, the ruthenium-based target materials formed in Examples 1 and 6 are formed in comparison with the recording film formed on the interlayer film made of the conventional ruthenium-based target of the comparative example. The grain distribution of the recording film on the obtained intermediate film was apparently uniform; as shown in Table 5, the standard deviation of the grain size of the recording film on the interlayer film obtained by the ruthenium-based targets of Examples 1 and 6 It was 0.69 nm and 1.05 nm, which was apparently lower than 1.33 nm of the recording film formed on the interlayer film made of the conventional ruthenium base target of this comparative example.

基於形成於本比較例之現有釕基靶材製成的中間膜與實施例1及6之釕基靶材所製得的中間膜上的記錄膜係以由同一鈷鉻鉑合金靶材並經相同的濺鍍製程所構成,故由圖16、17及20與表5之結果可證實,相較本比較例之現有釕基靶材製成的中間膜而言,包含由釕所構成的基相及由Mg2 B2 O5 或MgB4 O7 所構成的非晶相之實施例1或6之釕基靶材製成的中間膜,係能提供更為優良的結晶定向效果給記錄膜,則能有效提升記錄膜之結晶定向組織、磁晶異向性能與磁矯頑性,從而提高磁記錄媒體的訊雜比及面記錄密度,進而達到高密度磁記錄媒體之要求。The recording film on the interlayer film prepared based on the intermediate film formed of the conventional ruthenium base material of the comparative example and the ruthenium base target of Examples 1 and 6 is made of the same cobalt chrome platinum alloy target. The same sputtering process is used, and it can be confirmed from the results of Figs. 16, 17, and 20 and Table 5 that the intermediate film made of the conventional ruthenium-based target of the comparative example contains a base composed of ruthenium. An intermediate film made of the ruthenium-based target of Example 1 or 6 which is composed of an amorphous phase composed of Mg 2 B 2 O 5 or MgB 4 O 7 can provide a more excellent crystal orientation effect to the recording film. , the crystal orientation structure, the magnetocrystalline anisotropy performance and the magnetic coercivity of the recording film can be effectively improved, thereby improving the signal-to-noise ratio and the surface recording density of the magnetic recording medium, thereby achieving the requirements of the high-density magnetic recording medium.

比較例Comparative example 33 :現有釕基靶材與實施例: Existing bismuth-based targets and examples 11 and 66 之釕基靶材之比較Comparison of bismuth-based targets

本比較例中係以一現有釕基靶材與實施例1及6之釕基靶材進行比較,本比較例之現有釕基靶材係由釕、鈷、鉻與二氧化鈦(TiO2 )以25.00:61.00:6.00:8.00之莫耳比例所製成。In this comparative example, a conventional ruthenium-based target was compared with the ruthenium-based targets of Examples 1 and 6. The conventional ruthenium-based target of the comparative example was made of ruthenium, cobalt, chromium and titanium dioxide (TiO 2 ) at 25.00. : 61.00: 6.00: 8.00 molar ratio made.

圖21所示本比較例之現有釕基靶材經濺鍍製成的中間膜之穿透式電子顯微鏡(TEM)圖。其中,本比較例之現有釕基靶材個別經濺鍍製成的中間膜包含有一由釕、鈷及鉻所構成的基相50與一由二氧化鈦所構成的二氧化鈦相51。Fig. 21 is a transmission electron microscope (TEM) image of an intermediate film of the conventional ruthenium-based target of this comparative example which was sputter-plated. The intermediate film formed by sputtering of the prior art ruthenium-based target of the comparative example comprises a base phase 50 composed of ruthenium, cobalt and chromium and a titania phase 51 composed of titanium dioxide.

由圖13、14及21可見,相較於本比較例之現有釕基靶材個別經濺鍍製成的中間膜之基相50的各晶粒500內的晶格排列而言,實施例1及6之釕基靶材所製得的中間膜的基相20、30的各晶粒200、300內的晶格排列較為有序,故實施例1及6之釕基靶材所製得的中間膜的基相20、30的結晶性顯然較本比較例之現有釕基靶材個別經濺鍍製成的中間膜之基相50為佳。 如圖19所示,本比較例之現有釕基靶材製成的中間膜,其二氧化鈦相51位於其基相50的兩相鄰晶粒500之間,即位於兩相鄰晶粒500的晶界上。請參閱圖13、14及21所示,本比較例之現有釕基靶材製成的中間膜與實施例1及6之釕基靶材所製得的中間膜相比後,可見本比較例之現有釕基靶材製成的中間膜除了基相50之晶粒分佈較為不均以外,基相50之平均晶粒尺寸之標準差也較大。As can be seen from Figures 13, 14 and 21, Example 1 is compared to the lattice arrangement in the respective crystal grains 500 of the base phase 50 of the intermediate film which is separately sputtered by the prior art bismuth-based target of the comparative example. And the lattice arrangement in the crystal grains 200 and 300 of the base phases 20 and 30 of the interlayer film prepared by the ruthenium-based target of 6 is relatively order, so that the ruthenium-based targets of Examples 1 and 6 are obtained. The crystallinity of the base phases 20, 30 of the interlayer film is obviously better than the base phase 50 of the interlayer film formed by sputtering of the conventional ruthenium-based target of the comparative example. As shown in FIG. 19, in the intermediate film made of the conventional ruthenium-based target of the comparative example, the titania phase 51 is located between two adjacent crystal grains 500 of the base phase 50, that is, the crystals located in the two adjacent crystal grains 500. In the world. Referring to FIGS. 13 , 14 and 21 , the comparative example is obtained by comparing the intermediate film made of the conventional ruthenium-based target of the comparative example with the intermediate film prepared by the ruthenium-based target of Examples 1 and 6. The intermediate film made of the conventional ruthenium-based target has a larger standard deviation of the average grain size of the base phase 50 except that the grain distribution of the base phase 50 is relatively uneven.

於本比較例之現有釕基靶材製成的中間膜濺鍍成形一由鈷鉻鉑合金靶材所構成的記錄膜,並以TEM分析之;其中,形成本比較例之現有釕基靶材製成的中間膜上的記錄膜所使用的鈷鉻鉑合金靶材及製程參數係相同於形成於比較例1之現有釕基靶材製成的中間膜上的記錄膜,亦相同於形成於實施例1及6之釕基靶材所製得的中間膜上的記錄膜。A recording film composed of a cobalt-chromium-platinum alloy target was sputter-sputtered by an intermediate film made of the conventional ruthenium-based target of the comparative example, and analyzed by TEM; wherein the existing ruthenium-based target of the comparative example was formed. The cobalt chrome-platinum alloy target used in the recording film on the prepared intermediate film and the process parameters were the same as those of the recording film formed on the intermediate film made of the conventional ruthenium-based target of Comparative Example 1, and were also formed in the same manner. The recording film on the interlayer film prepared by the ruthenium base materials of Examples 1 and 6.

請參閱圖16、17及22所示,相較於形成於本比較例之現有釕基靶材製成的中間膜上的記錄膜而言,形成於實施例1及6之釕基靶材所製得的中間膜上的記錄膜之晶粒分佈顯然較為均勻;如表5所示,實施例1及6之釕基靶材所製得的中間膜上的記錄膜之晶粒尺寸之標準差分別為0.69奈米及1.05奈米,顯然低於形成於本比較例之現有釕基靶材製成的中間膜上的記錄膜之2.52奈米。Referring to FIGS. 16, 17, and 22, the ruthenium-based target materials formed in Examples 1 and 6 are formed in comparison with the recording film formed on the interlayer film made of the conventional ruthenium-based target of the comparative example. The grain distribution of the recording film on the obtained intermediate film was apparently uniform; as shown in Table 5, the standard deviation of the grain size of the recording film on the interlayer film obtained by the ruthenium-based targets of Examples 1 and 6 It was 0.69 nm and 1.05 nm, which was apparently lower than 2.52 nm of the recording film formed on the interlayer film made of the conventional ruthenium base target of this comparative example.

基於形成於本比較例之現有釕基靶材製成的中間膜與實施例1及6之釕基靶材所製得的中間膜上的記錄膜係以由同一鈷鉻鉑合金靶材並經相同的濺鍍製程所構成,故由圖16、17及22至及表5之結果可證實,相較本比較例之現有釕基靶材製成的中間膜而言,包含由釕所構成的基相及由Mg2 B2 O5 或MgB4 O7 所構成的非晶相之實施例1或6之釕基靶材製成的中間膜,係能提供更為優良的結晶定向效果給記錄膜,則能有效提升記錄膜之結晶定向組織、磁晶異向性能與磁矯頑性,從而提高磁記錄媒體的訊雜比及面記錄密度,進而達到高密度磁記錄媒體之要求。The recording film on the interlayer film prepared based on the intermediate film formed of the conventional ruthenium base material of the comparative example and the ruthenium base target of Examples 1 and 6 is made of the same cobalt chrome platinum alloy target. The same sputtering process is used, and it can be confirmed from the results of FIGS. 16, 17, and 22 to and Table 5 that the intermediate film made of the conventional ruthenium-based target of the comparative example includes the ruthenium. An intermediate film made of the base phase and the ruthenium target of Example 1 or 6 composed of an amorphous phase composed of Mg 2 B 2 O 5 or MgB 4 O 7 can provide a more excellent crystal orientation effect for recording The film can effectively improve the crystal orientation structure, magnetic crystal anisotropy performance and magnetic coercivity of the recording film, thereby improving the signal-to-noise ratio and the surface recording density of the magnetic recording medium, thereby achieving the requirements of a high-density magnetic recording medium.

綜上所述,經由實驗結果證實,實施例1至6之釕基靶材於高溫真空熱壓製程後,由MgB4 O7 或Mg2 B2 O5 所構成的非晶形相係分佈均勻於基相中且細小,係能預防濺鍍時電弧現象的產生,並提升濺鍍的穩定性及產品的良率。且由實施例1至6之釕基靶材製成之用於磁記錄媒體之中間膜,亦會形成由MgB4 O7 或Mg2 B2 O5 所構成的非晶形相包覆含有釕的基相之晶粒,係能提供更為優越的結晶定向效果給形成於中間膜上的記錄膜,使得記錄膜具有良好的結晶定向組織、磁晶異向性能與磁矯頑性,進而提高磁記錄媒體的訊雜比及面記錄密度,因而符合高密度磁記錄媒體之要求。In summary, it was confirmed by experimental results that the amorphous phase system composed of MgB 4 O 7 or Mg 2 B 2 O 5 was uniformly distributed after the high temperature vacuum heat-pressing process of the ruthenium-based targets of Examples 1 to 6 The small and medium-sized phase prevents arcing during sputtering and improves the stability of the sputtering and the yield of the product. Further, the intermediate film for the magnetic recording medium made of the ruthenium-based target of Examples 1 to 6 is also formed of an amorphous phase consisting of MgB 4 O 7 or Mg 2 B 2 O 5 and containing ruthenium. The crystal grains of the base phase can provide a superior crystal orientation effect to the recording film formed on the intermediate film, so that the recording film has a good crystal orientation structure, magnetic crystal anisotropy performance and magnetic coercivity, thereby improving magnetic The recording medium has a signal-to-noise ratio and a surface recording density, and thus meets the requirements of a high-density magnetic recording medium.

表1 各實施例金屬粉末之組份、第一氧化物之組份、金屬粉末及第一氧化物之莫耳數比及製程參數 Table 1 The composition of the metal powder of each example, the composition of the first oxide, the molar ratio of the metal powder and the first oxide, and the process parameters

表2 實施例2至5之金屬粉末、第一氧化物與第二氧化物之組份及莫耳比 Table 2 Metal powders of Examples 2 to 5, components of the first oxide and the second oxide, and molar ratio

表3 各實施例之感應耦合電漿光譜儀成份分析 Table 3 Inductively coupled plasma spectrometer composition analysis of each example

表4 各實施例之能量分散元素分析光譜儀分析結果 Table 4 Energy dispersive element analysis spectrometer analysis results of each example

表5 形成於實施例1、6與比較例1至3之靶材所製成的中間膜上的記錄膜之平均晶粒尺寸及其標準差 Table 5 Average grain size and standard deviation of the recording film formed on the interlayer film of the targets of Examples 1, 6 and Comparative Examples 1 to 3

10、20、30、40、50‧‧‧基相
100、200、300、400、500‧‧‧晶粒
11‧‧‧三氧化二硼相
21、31‧‧‧非晶相
41‧‧‧五氧化二鉭相
51‧‧‧二氧化鈦相
10, 20, 30, 40, 50‧ ‧ base phase
100, 200, 300, 400, 500‧‧‧ grains
11‧‧‧Diboron phase
21, 31‧‧‧Amorphous phase
41‧‧‧ bismuth pentoxide
51‧‧‧ Titanium dioxide phase

圖1為利用掃描式電子顯微鏡分析實施例1之釕基靶材所得到的金相圖; 圖2為利用掃描式電子顯微鏡分析實施例2之釕基靶材所得到的金相圖; 圖3為利用掃描式電子顯微鏡分析實施例3之釕基靶材所得到的金相圖; 圖4為利用掃描式電子顯微鏡分析實施例4之釕基靶材所得到的金相圖; 圖5為利用掃描式電子顯微鏡分析實施例5之釕基靶材所得到的金相圖; 圖6為利用掃描式電子顯微鏡分析實施例6之釕基靶材所得到的金相圖; 圖7為實施例1之釕基靶材之X光繞射光譜圖; 圖8為實施例2之釕基靶材之X光繞射光譜圖; 圖9為實施例3之釕基靶材之X光繞射光譜圖; 圖10為實施例4之釕基靶材之X光繞射光譜圖; 圖11為實施例5之釕基靶材之X光繞射光譜圖; 圖12為實施例6之釕基靶材之X光繞射光譜圖; 圖13為實施例1之釕基靶材經濺鍍得到的中間膜之穿透式電子顯微鏡影像圖; 圖14為實施例6之釕基靶材經濺鍍得到的中間膜之穿透式電子顯微鏡影像圖; 圖15為比較例1之現有釕基靶材(釕:三氧化二硼為92.50莫耳:7.50莫耳)經濺鍍得到的中間膜之穿透式電子顯微鏡影像圖; 圖16為形成於實施例1之釕基靶材經濺鍍得到的中間膜上的記錄膜之穿透式電子顯微鏡影像圖; 圖17為形成於實施例6之釕基靶材經濺鍍得到的中間膜上的記錄膜之穿透式電子顯微鏡影像圖; 圖18為形成於比較例1之現有釕基靶材經濺鍍得到的中間膜上的記錄膜之穿透式電子顯微鏡影像圖; 圖19為比較例2之現有釕基靶材(釕:五氧化二鉭為95.00莫耳:5.00莫耳)經濺鍍得到的中間膜之穿透式電子顯微鏡影像圖; 圖20為形成於比較例2之現有釕基靶材經濺鍍得到的中間膜上的記錄膜之穿透式電子顯微鏡影像圖; 圖21為比較例3之現有釕基靶材(釕:鈷:鉻:二氧化鈦為25.00莫耳:61.00莫耳:6.00莫耳:8.00莫耳)經濺鍍得到的中間膜之穿透式電子顯微鏡影像圖; 圖22為形成於比較例3之現有釕基靶材經濺鍍得到的中間膜上的記錄膜之穿透式電子顯微鏡影像圖。1 is a metallographic diagram obtained by analyzing a ruthenium-based target of Example 1 by a scanning electron microscope; FIG. 2 is a metallographic diagram obtained by analyzing a ruthenium-based target of Example 2 by a scanning electron microscope; The metallographic pattern obtained by analyzing the ruthenium-based target of Example 3 by a scanning electron microscope; FIG. 4 is a metallographic diagram obtained by analyzing the ruthenium-based target of Example 4 by a scanning electron microscope; The metallographic pattern obtained by analyzing the ruthenium-based target of Example 5 by a scanning electron microscope; FIG. 6 is a metallographic diagram obtained by analyzing the ruthenium-based target of Example 6 by a scanning electron microscope; X-ray diffraction spectrum of the ruthenium-based target; FIG. 8 is an X-ray diffraction spectrum of the ruthenium-based target of Example 2; FIG. 9 is an X-ray diffraction spectrum of the ruthenium-based target of Example 3. Figure 10 is an X-ray diffraction spectrum of the ruthenium-based target of Example 4; Figure 11 is an X-ray diffraction spectrum of the ruthenium-based target of Example 5; Figure 12 is a ruthenium-based target of Example 6. X-ray diffraction spectrum; Figure 13 is a transmission electron microscope image of the interlayer film obtained by sputtering of the ruthenium-based target of Example 1. Figure 14 is a transmission electron microscope image of the interlayer film obtained by sputtering of the ruthenium-based target of Example 6; Figure 15 is a conventional ruthenium-based target of Comparative Example 1 (钌: boron trioxide is 92.50) Mohr: 7.50 mole) Transmissive electron microscope image of the interlayer film obtained by sputtering; FIG. 16 is a penetration of the recording film formed on the interlayer film obtained by sputtering of the ruthenium-based target of Example 1. FIG. 17 is a transmission electron microscope image of a recording film formed on the interlayer film obtained by sputtering on the ruthenium-based target of Example 6; FIG. 18 is an existing 形成 formed in Comparative Example 1. A transmissive electron microscope image of a recording film on an intermediate film obtained by sputtering on a base target; FIG. 19 is a conventional ruthenium-based target of Comparative Example 2 (钌: bismuth pentoxide is 95.00 mol: 5.00 mol a transmission electron microscope image of the intermediate film obtained by sputtering; FIG. 20 is a transmission electron microscope image of the recording film formed on the interlayer film obtained by sputtering of the conventional ruthenium-based target of Comparative Example 2. 21 is a conventional ruthenium-based target of Comparative Example 3 (钌:cobalt:chromium:titanium dioxide) 25.00 Moule: 61.00 Mo Er: 6.00 Mo Er: 8.00 Mohr) Transmissive electron microscope image of the intermediate film obtained by sputtering; FIG. 22 shows that the conventional ruthenium base formed in Comparative Example 3 was sputtered. A transmission electron microscope image of the recording film on the intermediate film.

Claims (11)

一種釕基靶材,其中包含: 一基相,其中包含有釕;以及 一非晶形相,其中包含有一第一氧化物,該第一氧化物係選自由MgB4 O7 、Mg2 B2 O5 、Mg3 B2 O6 及其組合所構成之群組。A ruthenium-based target comprising: a base phase comprising ruthenium; and an amorphous phase comprising a first oxide selected from the group consisting of MgB 4 O 7 and Mg 2 B 2 O 5 , a group of Mg 3 B 2 O 6 and combinations thereof. 如請求項1所述之釕基靶材,其中該第一氧化物之含量係佔整體釕基靶材之0.1莫耳百分比至9莫耳百分比。The ruthenium-based target of claim 1, wherein the first oxide is present in an amount from 0.1 mole percent to 9 mole percent of the overall ruthenium base target. 如請求項1或2所述之釕基靶材,其中該基相進一步包含至少一選自於由鈷、鉻、鈦、鉭、矽、鎢、銅、鎂、鋯、錳、釔、鋁、鐵、鉬及硼所構成之群組中之元素。The ruthenium-based target according to claim 1 or 2, wherein the base phase further comprises at least one selected from the group consisting of cobalt, chromium, titanium, niobium, tantalum, tungsten, copper, magnesium, zirconium, manganese, lanthanum, aluminum, An element in a group of iron, molybdenum and boron. 如請求項1或2所述之釕基靶材,其中包含有一第二氧化物,該第二氧化物係包含至少一選自於由矽、鈦、鉻、鎢、鋁、鎵、鎂、鉬、錳、釔、鋯、鐵、鋅及鉭所構成之群組中之元素。The ruthenium-based target according to claim 1 or 2, comprising a second oxide comprising at least one selected from the group consisting of ruthenium, titanium, chromium, tungsten, aluminum, gallium, magnesium, and molybdenum An element of a group consisting of manganese, cerium, zirconium, iron, zinc and cerium. 如請求項4所述之釕基靶材,其中該第二氧化物佔整體釕基靶材之1.5莫耳百分比至24莫耳百分比。The ruthenium-based target of claim 4, wherein the second oxide comprises from 1.5 mole percent to 24 mole percent of the overall ruthenium base target. 一種用於磁記錄媒體的中間膜,其中包含: 一基相,其中包含有釕;以及 一非晶形相,其中包含有一第一氧化物,該第一氧化物係選自由MgB4 O7 、Mg2 B2 O5 、Mg3 B2 O6 及其組合所構成之群組。An interlayer film for a magnetic recording medium, comprising: a base phase containing ruthenium; and an amorphous phase comprising a first oxide selected from the group consisting of MgB 4 O 7 , Mg A group consisting of 2 B 2 O 5 , Mg 3 B 2 O 6 and combinations thereof. 如請求項6所述之用於磁記錄媒體的中間膜,其係由如請求項1至5項中任一項所述之釕基靶材所製成。The intermediate film for a magnetic recording medium according to claim 6, which is made of the ruthenium-based target according to any one of claims 1 to 5. 如請求項6或7所述之用於磁記錄媒體的中間膜,其中該第一氧化物之含量係佔整體用於磁記錄媒體的中間膜之0.1莫耳百分比至9莫耳百分比。The intermediate film for a magnetic recording medium according to claim 6 or 7, wherein the content of the first oxide is from 0.1 mol% to 9 mol% of the intermediate film for the magnetic recording medium as a whole. 如請求項6或7所述之用於磁記錄媒體的中間膜,其中該基相包含至少一選自於由鈷、鉻、鈦、鉭、矽、鎢、銅、鎂、鋯、錳、釔、鋁、鐵、鉬及硼所構成之群組中之元素。The intermediate film for a magnetic recording medium according to claim 6 or 7, wherein the base phase comprises at least one selected from the group consisting of cobalt, chromium, titanium, lanthanum, cerium, tungsten, copper, magnesium, zirconium, manganese, lanthanum An element of a group consisting of aluminum, iron, molybdenum and boron. 如請求項6或7所述之用於磁記錄媒體的中間膜,其中進一步包含有一有別於第一氧化物之第二氧化物,該第二氧化物係包含至少一選自於由矽、鈦、鉻、鎢、鋁、鎵、鎂、鉬、錳、釔、鋯、鐵、鋅及鉭所構成之群組中之元素。The interlayer film for a magnetic recording medium according to claim 6 or 7, further comprising a second oxide different from the first oxide, the second oxide system comprising at least one selected from the group consisting of An element of a group consisting of titanium, chromium, tungsten, aluminum, gallium, magnesium, molybdenum, manganese, cerium, zirconium, iron, zinc, and cerium. 如請求項10所述之用於磁記錄媒體的中間膜,其中該第二氧化物佔整體用於磁記錄媒體的中間膜之1.5莫耳百分比至24莫耳百分比。The intermediate film for a magnetic recording medium according to claim 10, wherein the second oxide accounts for 1.5 mol% to 24 mol% of the intermediate film for the magnetic recording medium as a whole.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112739846A (en) * 2018-09-25 2021-04-30 Jx金属株式会社 Sputtering target and powder for producing sputtering target

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112739846A (en) * 2018-09-25 2021-04-30 Jx金属株式会社 Sputtering target and powder for producing sputtering target
TWI727334B (en) * 2018-09-25 2021-05-11 日商Jx金屬股份有限公司 Sputtering target and powder used for manufacturing sputtering target

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