TWI752655B - Fe-pt based sputtering target and method of preparing the same - Google Patents

Fe-pt based sputtering target and method of preparing the same Download PDF

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TWI752655B
TWI752655B TW109133429A TW109133429A TWI752655B TW I752655 B TWI752655 B TW I752655B TW 109133429 A TW109133429 A TW 109133429A TW 109133429 A TW109133429 A TW 109133429A TW I752655 B TWI752655 B TW I752655B
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platinum
iron
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less
based target
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TW202212581A (en
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羅鴻文
陳又菱
蔡登安
鄭惠文
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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 Fe-Pt based sputtering target and a method of preparing the same. The Fe-Pt based sputtering target includes iron, platinum, and boron nitride. Based on the total amount of the Fe-Pt based sputtering target, the amount of the boron nitride is more than 0 at% and less than or equal to 50 at%. In addition, a metallography of the Fe-Pt based sputtering target comprises black phases. The black phases have an average size less than 3 μm, and the black phases have a dispersion uniformity less than 5 × 10 -4. By controlling the content of the boron nitride of the Fe-Pt based sputtering target and limiting the average size and the dispersion uniformity of the black phases in the metallography of the Fe-Pt based sputtering target, the Fe-Pt based sputtering target can elevate bending strength of the Fe-Pt based sputtering target, reduce the occurrence of abnormal discharges during sputtering, and mitigate the problem of particulate contamination of a magnetic recording layer formed by the Fe-Pt based sputtering target. Therefore, the quality and yield of the magnetic recording layer formed by the Fe-Pt based sputtering target can be improved.

Description

鐵鉑基靶材及其製法Iron-platinum-based target and method for making the same

本創作係關於一種鐵鉑基靶材及其製法,尤指一種應用於磁記錄媒體之鐵鉑基靶材及其製法。 This work is about an iron-platinum-based target and its manufacturing method, especially an iron-platinum-based target used in magnetic recording media and its manufacturing method.

磁記錄是指利用磁性材料的磁滯特性將資訊儲存於記錄媒體。根據磁頭磁化的方向,現有技術之磁記錄媒體可區分為水平式磁記錄媒體(longitudinal magnetic recording,LMR)及垂直式磁記錄媒體(perpendicular magnetic recording,PMR)。作為資訊儲存的記憶媒體,高熱穩定性是首要需求。不僅如此,隨著人們對於磁記錄媒體之資訊儲存容量的需求愈來愈高,如何提升磁記錄媒體之記錄密度已然成為相關領域關注的研究重點。然而,在水平式磁記錄媒體之磁記錄密度現今已逼近物理極限的困境下,能延緩超順磁極限、達到更高記錄密度的垂直式磁記錄媒體,成為解決問題的技術方向。 Magnetic recording refers to the use of the hysteresis properties of magnetic materials to store information on a recording medium. According to the magnetization direction of the magnetic head, magnetic recording media in the prior art can be classified into horizontal magnetic recording media (longitudinal magnetic recording, LMR) and perpendicular magnetic recording media (perpendicular magnetic recording, PMR). As a memory medium for information storage, high thermal stability is the primary requirement. Not only that, with the increasing demand for the information storage capacity of magnetic recording media, how to improve the recording density of magnetic recording media has become a research focus in related fields. However, under the predicament that the magnetic recording density of the horizontal magnetic recording medium is now approaching the physical limit, a perpendicular magnetic recording medium that can delay the superparamagnetic limit and achieve a higher recording density has become a technical direction to solve the problem.

一般而言,垂直式磁記錄媒體的層狀結構由下至上包含有基板、附著層、軟磁層(soft underlayer)、晶種層(seed layer)、中間層(intermediate layer)、磁記錄層(magnetic recording layer)、覆蓋層以及潤滑層,其中,磁記錄層通常選用鈷鉻鉑基合金系統作為主要成分。然而,隨著垂直式磁記錄媒體的技術趨於成熟,鈷鉻鉑基合金系統之磁記錄層亦逐漸接近磁記錄密度極限,為了再進一步提高垂直式磁記錄媒體的記錄密度,業界遂發展出選用鐵鉑基合金系統製作熱輔助磁記錄媒體(heat-assisted magnetic recording medium,HAMR medium)之磁記錄層,其在寫入磁場的同時以熱能的方式作用於記錄位的磁性顆粒上,藉由將該磁性顆粒的溫度提高至居里點(Curie temperature)之上,使得該磁性顆粒的磁力頑性暫時被降低,又由於鐵鉑基合金的磁性顆粒尺寸可較鈷鉻鉑基合金的磁性顆粒尺寸縮小,進而可提高磁記錄媒體的記錄密度。不過,由於熱輔助磁記錄的技術會在相同的區域重複聚焦加熱,作為磁記錄層之磁性複合材料因而需具有高熱穩定性,故於鐵鉑基合金系統中會額外添加具有高熱穩定性的氮化硼(boron nitride,BN),藉此在鐵鉑基合金的晶粒之間形成阻隔及減少磁耦合效應。 Generally speaking, the layered structure of a perpendicular magnetic recording medium includes a substrate, an adhesive layer, a soft underlayer, a seed layer, an intermediate layer, and a magnetic recording layer from bottom to top. recording layer), a cover layer and a lubricating layer, wherein the magnetic recording layer is usually a cobalt-chromium-platinum-based alloy system as the main component. However, as the technology of perpendicular magnetic recording media tends to mature, the magnetic recording layer of the cobalt-chromium-platinum-based alloy system is gradually approaching the limit of magnetic recording density. In order to further improve the recording density of perpendicular magnetic recording media, the industry has developed a The use of iron-platinum alloy system to make heat-assisted magnetic recording medium (HAMR) The magnetic recording layer of the medium) acts on the magnetic particles of the recording bit in the form of thermal energy while writing the magnetic field, and by raising the temperature of the magnetic particles to above the Curie temperature, the magnetic The magnetic coercivity of the particles is temporarily reduced, and the magnetic particle size of the iron-platinum-based alloy can be reduced compared with that of the cobalt-chromium-platinum-based alloy, thereby increasing the recording density of the magnetic recording medium. However, since the technology of thermally assisted magnetic recording will repeatedly focus heating in the same area, the magnetic composite material used as the magnetic recording layer needs to have high thermal stability, so nitrogen with high thermal stability will be added to the iron-platinum-based alloy system. Boron nitride (BN) is used to form a barrier between the grains of the iron-platinum-based alloy and reduce the magnetic coupling effect.

然而,由於氮化硼的粒徑小且具有容易產生團聚、不易分散等特性,因此,若直接將氮化硼添加於鐵鉑基合金系統中製成靶材,則會於所述靶材金相圖中明顯觀察到團聚的氮化硼,導致所述靶材的抗折強度(bending strength)不佳,並且容易於後續應用的濺鍍過程中形成異常放電以及產生大量微粒掉落至濺鍍形成的磁記錄層,進而影響到磁記錄層之膜層的品質與良率。 However, due to the small particle size of boron nitride and the characteristics of easy to agglomerate and difficult to disperse, if boron nitride is directly added to the iron-platinum-based alloy system to make a target, it will be in the target gold. The agglomerated boron nitride is clearly observed in the phase diagram, resulting in poor bending strength of the target, and is prone to abnormal discharge and a large number of particles falling to the sputtering process in the subsequent application of the sputtering process. The formed magnetic recording layer further affects the film quality and yield of the magnetic recording layer.

有鑒於現有技術所面臨的缺陷,本創作之目的在於提升靶材的抗折強度,並同時於後續應用的濺鍍過程中降低異常放電的發生頻率,以及減輕微粒掉落的問題,進而提升濺鍍形成的磁記錄層之品質與良率。 In view of the defects faced by the prior art, the purpose of this creation is to improve the flexural strength of the target material, and at the same time reduce the frequency of abnormal discharge in the subsequent sputtering process, and reduce the problem of particle falling, thereby improving the sputtering process. The quality and yield of the magnetic recording layer formed by plating.

為達成前述目的,本創作提供一種鐵鉑基靶材,其包含鐵(Fe)、鉑(Pt)以及氮化硼(BN);其中,以該鐵鉑基靶材整體之原子總數為基準,氮化硼的含量係大於0原子百分比(atomic percentage,at%)且小於或等於50at%;該鐵鉑基靶材的金相包含複數黑色相,該等黑色相的平均尺寸小於3微米(μm),且該等黑色相於金相中的分散均勻度小於5×10-4,其中該分散均勻度係透過以下算式計算而得:(金相中的黑色相之總面積/金相之整體面積)/金相中的黑色相之總個數。 In order to achieve the aforementioned object, the present invention provides an iron-platinum-based target material, which comprises iron (Fe), platinum (Pt) and boron nitride (BN); wherein, based on the total number of atoms of the iron-platinum-based target material as a whole, The content of boron nitride is greater than 0 atomic percentage (atomic percentage, at%) and less than or equal to 50 at%; the metallographic phase of the iron-platinum-based target includes a plurality of black phases, and the average size of these black phases is less than 3 microns (μm ), and the dispersion uniformity of these black phases in the metallographic phase is less than 5×10 -4 , wherein the dispersion uniformity is calculated by the following formula: (the total area of the black phase in the metallographic phase/the overall area of the metallographic phase)/in the metallographic phase The total number of black phases.

依據本創作,藉由控制鐵鉑基靶材中的氮化硼含量、黑色相之平均尺寸範圍和黑色相之分散均勻度範圍,能夠使鐵鉑基靶材的相組成分佈呈現良好的均勻性,進而有效提升鐵鉑基靶材的抗折強度,並同時確保於後續應用的濺鍍過程中能降低異常放電的發生頻率,以及減輕微粒掉落的問題。 According to this creation, by controlling the boron nitride content in the iron-platinum-based target, the average size range of the black phase, and the dispersion uniformity range of the black phase, the phase composition distribution of the iron-platinum-based target can be well uniform. , thereby effectively improving the flexural strength of the iron-platinum-based target, and at the same time ensuring that the frequency of abnormal discharge can be reduced in the subsequent sputtering process, and the problem of particle falling can be alleviated.

依據本創作,各黑色相的尺寸係指金相中各黑色相通過中心點之最大長度;而取前述多組數據之平均值,即為所述之黑色相的平均尺寸。 According to this creation, the size of each black phase refers to the maximum length of each black phase passing through the center point in the metallographic phase; and the average value of the aforementioned multiple sets of data is the average size of the black phase.

依據本創作,所述黑色相的分散均勻度係代表在金相中,平均而言,單一個黑色相佔靶材總面積的比例。舉例來說,若在金相中的黑色相之總面積以及金相之整體面積不變的情況下,當黑色相之總個數愈多,即代表每一個黑色相在金相中所佔有的面積比例愈小,因此表示每一個黑色相愈能均勻散佈於金相中,簡言之,所述黑色相的分散均勻度的數值愈小,代表金相中的黑色相分佈愈均勻。 According to the present invention, the dispersion uniformity of the black phase represents in the metallographic phase, on average, the proportion of a single black phase to the total area of the target. For example, if the total area of the black phase in the metallographic phase and the overall area of the metallographic phase remain unchanged, when the total number of black phases is greater, it means that each black phase occupies a smaller area ratio in the metallographic phase. , so it means that each black phase can be evenly dispersed in the metallographic phase. In short, the smaller the value of the dispersion uniformity of the black phase, the more uniform the black phase distribution in the metallographic phase.

依據本創作,所述氮化硼可為六方氮化硼(h-BN)、立方氮化硼(c-BN)、密排六方氮化硼(w-BN)或其組合,但不限於此。 According to the present invention, the boron nitride can be hexagonal boron nitride (h-BN), cubic boron nitride (c-BN), hexagonal close-packed boron nitride (w-BN) or a combination thereof, but not limited thereto .

較佳的,以該鐵鉑基靶材整體之原子總數為基準,氮化硼的含量係大於或等於3at%且小於或等於30at%。更佳的,以該鐵鉑基靶材整體之原子總數為基準,氮化硼的含量係大於或等於5at%且小於或等於25at%。藉由進一步控制氮化硼的含量於特定範圍中,可使得以該鐵鉑基靶材進行濺鍍所形成的膜層具有較佳的磁性性質。 Preferably, the content of boron nitride is greater than or equal to 3 at % and less than or equal to 30 at % based on the total number of atoms of the entire iron-platinum-based target. More preferably, the content of boron nitride is greater than or equal to 5 at % and less than or equal to 25 at % based on the total number of atoms of the whole iron-platinum-based target. By further controlling the content of boron nitride within a specific range, the film layer formed by sputtering the iron-platinum-based target can have better magnetic properties.

較佳的,以該鐵鉑基靶材整體之原子總數為基準,鉑的含量係大於或等於10at%且小於或等於45at%。 Preferably, the content of platinum is greater than or equal to 10 at% and less than or equal to 45 at% based on the total number of atoms of the entire iron-platinum-based target.

較佳的,以該鐵鉑基靶材整體之原子總數為基準,鐵的含量係大於或等於5at%且小於或等於84at%。 Preferably, the iron content is greater than or equal to 5 at% and less than or equal to 84 at% based on the total number of atoms of the entire iron-platinum-based target.

在一些實施例中,該鐵鉑基靶材更包含第一成分,該第一成分係選自由氧化物(oxide)、碳化物(carbide)、氮化物(nitride)及其組合所組成之群組;其中,以該鐵鉑基靶材整體之原子總數為基準,該第一成分的含量係大於0at%且小於或等於50at%,且氮化硼與該第一成分的含量總和係大於或等於6at%且小於或等於50at%。較佳的,以該鐵鉑基靶材整體之原子總數為基準,該第一成分的含量係大於或等於5at%且小於或等於35at%,且氮化硼與該第一成分的含量總和係大於或等於6at%且小於或等於50at%。 In some embodiments, the iron-platinum-based target further includes a first component selected from the group consisting of oxides, carbides, nitrides, and combinations thereof ; Wherein, based on the total number of atoms of the iron-platinum-based target as a whole, the content of the first component is greater than 0at% and less than or equal to 50at%, and the sum of the content of boron nitride and the first component is greater than or equal to 6at% and less than or equal to 50at%. Preferably, based on the total number of atoms of the iron-platinum-based target as a whole, the content of the first component is greater than or equal to 5 at% and less than or equal to 35 at%, and the sum of the content of boron nitride and the first component is Greater than or equal to 6at% and less than or equal to 50at%.

在一些實施例中,該鐵鉑基靶材更包含碳(C),以該鐵鉑基靶材整體之原子總數為基準,碳的含量係大於或等於2at%且小於或等於40at%。 In some embodiments, the iron-platinum-based target further comprises carbon (C). Based on the total number of atoms in the iron-platinum-based target, the carbon content is greater than or equal to 2 at % and less than or equal to 40 at %.

在一些實施例中,鐵鉑基靶材之金相中的黑色相成分包含氮化硼;在另一些實施例中,鐵鉑基靶材之金相中的黑色相成分包含氮化硼與第一成分;在另一些實施例中,鐵鉑基靶材之金相中的黑色相成分包含氮化硼與碳;在另一些實施例中,鐵鉑基靶材之金相中的黑色相成分包含氮化硼、第一成分與碳。 In some embodiments, the black phase component in the metallographic phase of the iron-platinum-based target comprises boron nitride; in other embodiments, the black-phase component in the metallographic phase of the iron-platinum-based target comprises boron nitride and the first component; in In other embodiments, the black phase components in the metallographic phase of the iron-platinum-based target include boron nitride and carbon; in other embodiments, the black-phase components in the metallographic phase of the iron-platinum-based target include boron nitride, the first component with carbon.

較佳的,該氧化物可為二氧化矽(SiO2)、二氧化鈦(TiO2)、三氧化二鉻(Cr2O3)、五氧化二鉭(Ta2O5)、氧化鈷(CoO)、三氧化二錳(Mn2O3)、三氧化二硼(B2O3)、二氧化鉿(HfO2)、氧化鎂(MgO)、三氧化二鋁(Al2O3)、二氧化鋯(ZrO2)、五氧化二鈮(Nb2O5)、五氧化二釩(V2O5)、三氧化鎢(WO3)、三氧化二鐵(Fe2O3)、氧化鋅(ZnO)或其組合,但不限於此。 Preferably, the oxide can be silicon dioxide (SiO 2 ), titanium dioxide (TiO 2 ), chromium trioxide (Cr 2 O 3 ), tantalum pentoxide (Ta 2 O 5 ), cobalt oxide (CoO) , manganese trioxide (Mn 2 O 3 ), boron trioxide (B 2 O 3 ), hafnium dioxide (HfO 2 ), magnesium oxide (MgO), aluminum oxide (Al 2 O 3 ), dioxide Zirconium (ZrO 2 ), Niobium Pentoxide (Nb 2 O 5 ), Vanadium Pentoxide (V 2 O 5 ), Tungsten Trioxide (WO 3 ), Iron Trioxide (Fe 2 O 3 ), Zinc Oxide ( ZnO) or a combination thereof, but not limited thereto.

較佳的,該氮化物可為氮化鋁(AlN)、氮化鈦(TiN)、氮化鉻(CrN)、氮化鋯(ZrN)、氮化鉭(TaN)、氮化鉿(HfN)、氮化矽(Si3N4)、氮化碳鈦(TiCN)、氮化鎢(WN)或其組合,但不限於此。應理解的是,本說明書中所指之氮化物不包含鐵鉑基靶材中的必要成分一氮化硼,亦即,前述「氮化硼與該第一成分的含量總和係大於或等於6at%且小於或等於50at%」係指第一成分(例如 前述列舉的氮化鋁)與氮化硼的含量總和係大於或等於6at%且小於或等於50at%。 Preferably, the nitride can be aluminum nitride (AlN), titanium nitride (TiN), chromium nitride (CrN), zirconium nitride (ZrN), tantalum nitride (TaN), hafnium nitride (HfN) , silicon nitride (Si 3 N 4 ), titanium carbon nitride (TiCN), tungsten nitride (WN) or a combination thereof, but not limited thereto. It should be understood that the nitrides referred to in this specification do not include boron nitride, an essential component in the iron-platinum-based target, that is, the above-mentioned "the sum of the content of boron nitride and the first component is greater than or equal to 6at. % and less than or equal to 50 at%” means that the total content of the first component (for example, the aforementioned aluminum nitride) and boron nitride is greater than or equal to 6 at% and less than or equal to 50 at%.

較佳的,該碳化物可為碳化矽(SiC)、碳化硼(B4C)、碳化鈦(TiC)、碳化鎢(WC)、碳化鉭(TaC)、碳化鉿(HfC)、碳化鋯(ZrC)、碳化釩(VC)、碳化鈮(NbC)、碳化鉻(Cr3C2)或其組合,但不限於此。 Preferably, the carbide can be silicon carbide (SiC), boron carbide (B 4 C), titanium carbide (TiC), tungsten carbide (WC), tantalum carbide (TaC), hafnium carbide (HfC), zirconium carbide ( ZrC), vanadium carbide (VC), niobium carbide (NbC), chromium carbide (Cr 3 C 2 ), or a combination thereof, but not limited thereto.

在另一些實施例中,該鐵鉑基靶材更包含第二成分,該第二成分係選自由銀(Ag)、金(Au)、鍺(Ge)、銅(Cu)、鎳(Ni)、鈷(Co)、鋁(Al)、鎂(Mg)、錳(Mn)、矽(Si)、鍶(Sr)及其組合所組成之群組;其中,以該鐵鉑基靶材整體之原子總數為基準,該第二成分的含量係大於或等於2at%且小於或等於40at%。較佳的,該第二成分的含量係大於或等於2at%且小於或等於20at%;更佳的,該第二成分的含量係大於或等於2at%且小於或等於10at%。透過於鐵鉑基靶材中添加前述第二成分,有助於進一步提升鐵鉑基靶材的緻密程度。 In other embodiments, the iron-platinum-based target further comprises a second component selected from silver (Ag), gold (Au), germanium (Ge), copper (Cu), nickel (Ni) , Cobalt (Co), Aluminum (Al), Magnesium (Mg), Manganese (Mn), Silicon (Si), Strontium (Sr) and a group consisting of combinations thereof; wherein, the iron-platinum-based target as a whole Based on the total number of atoms, the content of the second component is greater than or equal to 2 at % and less than or equal to 40 at %. Preferably, the content of the second component is greater than or equal to 2 at% and less than or equal to 20 at%; more preferably, the content of the second component is greater than or equal to 2 at% and less than or equal to 10 at%. By adding the aforementioned second component to the iron-platinum-based target, the density of the iron-platinum-based target can be further improved.

在另一些實施例中,該鐵鉑基靶材更包含該第二成分以及碳;其中,以該鐵鉑基靶材整體之原子總數為基準,該第二成分的含量係大於或等於2at%且小於或等於40at%,碳的含量係大於或等於2at%且小於或等於10at%。 In other embodiments, the iron-platinum-based target further comprises the second component and carbon; wherein, based on the total number of atoms of the iron-platinum-based target as a whole, the content of the second component is greater than or equal to 2 at% and less than or equal to 40 at %, and the carbon content is greater than or equal to 2 at % and less than or equal to 10 at %.

在另一些實施例中,該鐵鉑基靶材更包含該第一成分以及該第二成分;其中,以該鐵鉑基靶材整體之原子總數為基準,該第一成分的含量係大於0at%且小於或等於50at%,且該第一成分與氮化硼的含量總和係大於或等於6at%且小於或等於50at%,該第二成分的含量係大於或等於2at%且小於或等於40at%。 In other embodiments, the iron-platinum-based target further comprises the first component and the second component; wherein, based on the total number of atoms of the iron-platinum-based target as a whole, the content of the first component is greater than 0 at % and less than or equal to 50at%, and the total content of the first component and boron nitride is greater than or equal to 6at% and less than or equal to 50at%, the content of the second component is greater than or equal to 2at% and less than or equal to 40at% %.

在另一些實施例中,該鐵鉑基靶材更包含該第一成分、該第二成分以及碳;其中,以該鐵鉑基靶材整體之原子總數為基準,該第一成分的含量係大於0at%且小於或等於50at%,且該第一成分與氮化硼的含量總和係大於 或等於6at%且小於或等於50at%,該第二成分的含量係大於或等於2at%且小於或等於40at%,碳的含量係大於或等於2at%且小於或等於10at%。 In other embodiments, the iron-platinum-based target further comprises the first component, the second component and carbon; wherein, based on the total number of atoms of the iron-platinum-based target as a whole, the content of the first component is More than 0at% and less than or equal to 50at%, and the total content of the first component and boron nitride is greater than or equal to 6 at % and less than or equal to 50 at %, the content of the second component is greater than or equal to 2 at % and less than or equal to 40 at %, and the content of carbon is greater than or equal to 2 at % and less than or equal to 10 at %.

於本發明的第一實施態樣中,該鐵鉑基靶材包含鐵、鉑以及氮化硼;於此實施態樣中,氮化硼的含量係大於或等於0.1at%且小於或等於50at%。於本發明的第二實施態樣中,該鐵鉑基靶材包含鐵、鉑、氮化硼以及碳;於此實施態樣中,氮化硼的含量係大於或等於1at%且小於或等於30at%,碳的含量係大於或等於1at%且小於或等於40at%,更具體而言,碳的含量係大於或等於2at%且小於或等於40at%。於本發明的第三實施態樣中,該鐵鉑基靶材包含鐵、鉑、氮化硼以及該第一成分;於此實施態樣中,氮化硼的含量係大於或等於1at%且小於或等於50at%,該第一成分的含量係大於或等於4at%且小於或等於30at%。於本發明的第四實施態樣中,該鐵鉑基靶材包含鐵、鉑、氮化硼以及該第二成分;於此實施態樣中,氮化硼的含量係大於或等於10at%且小於或等於50at%,該第二成分的含量係大於或等於1at%且小於或等於20at%,更具體而言,該第二成分的含量係大於或等於2at%且小於或等於20at%。於本發明的第五實施態樣中,該鐵鉑基靶材包含鐵、鉑、氮化硼、該第一成分以及該第二成分;於此實施態樣中,氮化硼的含量係大於或等於2at%且小於或等於30at%,該第一成分的含量係大於或等於5at%且小於或等於30at%,該第二成分的含量係大於或等於5at%且小於或等於50at%,更具體而言,該第二成分的含量係大於或等於5at%且小於或等於40at%。於本發明的第六實施態樣中,該鐵鉑基靶材包含鐵、鉑、氮化硼、該第一成分以及碳;於此實施態樣中,氮化硼的含量係大於或等於1at%且小於或等於20at%,該第一成分的含量係大於或等於10at%且小於或等於50at%,碳的含量係大於或等於2at%且小於或等於20at%。於本發明的第七實施態樣中,該鐵鉑基靶材包含鐵、鉑、氮化硼、該第二成分以及碳;於此實施態樣中,氮化硼的含量係大於或等 於1at%且小於或等於30at%,該第二成分的含量係大於或等於1at%且小於或等於20at%,更具體而言,該第二成分的含量係大於或等於2at%且小於或等於20at%,碳的含量係大於或等於5at%且小於或等於40at%。於本發明的第八實施態樣中,該鐵鉑基靶材包含鐵、鉑、氮化硼、該第一成分、該第二成分以及碳;於此實施態樣中,氮化硼的含量係大於或等於1at%且小於或等於30at%,該第一成分的含量係大於或等於5at%且小於或等於50at%,更具體而言,該第一成分的含量係大於或等於5at%且小於或等於40at%,該第二成分的含量係大於或等於2at%且小於或等於20at%,碳的含量係大於或等於2at%且小於或等於15at%。於前述第一、第三、第四、第五實施態樣中,該鐵鉑基靶材可選擇性地不包含碳。 In the first embodiment of the present invention, the iron-platinum-based target material includes iron, platinum and boron nitride; in this embodiment, the content of boron nitride is greater than or equal to 0.1at% and less than or equal to 50at %. In the second embodiment of the present invention, the iron-platinum-based target material includes iron, platinum, boron nitride and carbon; in this embodiment, the content of boron nitride is greater than or equal to 1 at% and less than or equal to 30 at%, the carbon content is greater than or equal to 1 at% and less than or equal to 40 at%, more specifically, the content of carbon is greater than or equal to 2 at% and less than or equal to 40 at%. In a third embodiment of the present invention, the iron-platinum-based target material includes iron, platinum, boron nitride and the first component; in this embodiment, the content of boron nitride is greater than or equal to 1 at% and Less than or equal to 50 at%, the content of the first component is greater than or equal to 4 at% and less than or equal to 30 at%. In the fourth embodiment of the present invention, the iron-platinum-based target material includes iron, platinum, boron nitride and the second component; in this embodiment, the content of boron nitride is greater than or equal to 10 at% and Less than or equal to 50 at %, the content of the second component is greater than or equal to 1 at % and less than or equal to 20 at %, more specifically, the content of the second component is greater than or equal to 2 at % and less than or equal to 20 at %. In a fifth embodiment of the present invention, the iron-platinum-based target comprises iron, platinum, boron nitride, the first component and the second component; in this embodiment, the content of boron nitride is greater than or equal to 2at% and less than or equal to 30at%, the content of the first component is greater than or equal to 5at% and less than or equal to 30at%, the content of the second component is greater than or equal to 5at% and less than or equal to 50at%, more Specifically, the content of the second component is greater than or equal to 5 at % and less than or equal to 40 at %. In the sixth embodiment of the present invention, the iron-platinum-based target material includes iron, platinum, boron nitride, the first component and carbon; in this embodiment, the content of boron nitride is greater than or equal to 1at % and less than or equal to 20 at%, the content of the first component is greater than or equal to 10 at% and less than or equal to 50 at%, and the content of carbon is greater than or equal to 2 at% and less than or equal to 20 at%. In a seventh embodiment of the present invention, the iron-platinum-based target material includes iron, platinum, boron nitride, the second component and carbon; in this embodiment, the content of boron nitride is greater than or equal to At 1 at% and less than or equal to 30 at%, the content of the second component is greater than or equal to 1 at% and less than or equal to 20 at%, more specifically, the content of the second component is greater than or equal to 2 at% and less than or equal to 20at%, the carbon content is greater than or equal to 5at% and less than or equal to 40at%. In an eighth embodiment of the present invention, the iron-platinum-based target material comprises iron, platinum, boron nitride, the first component, the second component and carbon; in this embodiment, the content of boron nitride is greater than or equal to 1at% and less than or equal to 30at%, the content of the first component is greater than or equal to 5at% and less than or equal to 50at%, more specifically, the content of the first component is greater than or equal to 5at% and Less than or equal to 40 at%, the content of the second component is greater than or equal to 2 at% and less than or equal to 20 at%, and the content of carbon is greater than or equal to 2 at% and less than or equal to 15 at%. In the aforementioned first, third, fourth, and fifth embodiments, the iron-platinum-based target may optionally not contain carbon.

較佳的,該鐵鉑基靶材所具有的抗折強度係大於或等於700百萬帕(MPa)。更佳的,該鐵鉑基靶材所具有的抗折強度係大於或等於700MPa且小於或等於1600MPa。 Preferably, the flexural strength of the iron-platinum-based target is greater than or equal to 700 megapascals (MPa). More preferably, the flexural strength of the iron platinum-based target material is greater than or equal to 700 MPa and less than or equal to 1600 MPa.

此外,本創作另提供一種鐵鉑基靶材之製法,其包含以下步驟:步驟(a):混合鐵原料、鉑原料以及氮化硼原料,以得到一原料混合物,其中,該氮化硼原料的平均粒徑係小於5微米;步驟(b):將該原料混合物進行研磨4小時至12小時,隨後以800目數(mesh)至1200目數的篩網過篩,接著取篩上物並重複前述研磨與過篩的步驟,以獲得一鐵鉑基混合原料;以及步驟(c):燒結該鐵鉑基混合原料,以獲得該鐵鉑基靶材;其中,以該鐵鉑基混合原料整體之原子總數為基準,氮化硼原料的添加量係大於0at%且小於或等於50at%;該鐵鉑基靶材的金相包含複數黑色相,該等黑色相的平均尺寸小於3微米,且該等黑色相的分散均勻度小於5×10-4,其中該分散均勻度係透過以下算式計算而得:(金相中的黑色相之總面積/金相之整體面積)/金相中的黑色相之總個數。 In addition, the present invention further provides a method for producing an iron-platinum-based target, which includes the following steps: step (a): mixing iron raw materials, platinum raw materials and boron nitride raw materials to obtain a raw material mixture, wherein the boron nitride raw materials The average particle size is less than 5 microns; step (b): the raw material mixture is ground for 4 hours to 12 hours, then sieved with a sieve of 800 mesh to 1200 mesh, and then the material on the sieve is taken and filtered. Repeat the above-mentioned steps of grinding and sieving to obtain an iron-platinum-based mixed raw material; and step (c): sintering the iron-platinum-based mixed raw material to obtain the iron-platinum-based target; wherein, the iron-platinum-based mixed raw material is Based on the total number of atoms in the whole, the addition amount of boron nitride raw materials is greater than 0at% and less than or equal to 50at%; the metallographic phase of the iron-platinum-based target contains a plurality of black phases, and the average size of these black phases is less than 3 microns, And the dispersion uniformity of these black phases is less than 5×10 -4 , wherein the dispersion uniformity is calculated by the following formula: (the total area of the black phase in the metallographic phase/the overall area of the metallographic phase)/the amount of the black phase in the metallographic phase. The total number of.

藉由控制鐵鉑基混合原料中氮化硼原料的平均粒徑大小以及含量範圍,並同時透過過篩之技術手段,可使得後續形成鐵鉑基靶材時獲得具有特定平均尺寸範圍以及特定分散均勻度範圍的黑色相,進而使所製得鐵鉑基靶材具有較佳的抗折強度,且同時能於後續濺鍍過程中降低異常放電發生頻率以及減輕微粒掉落的問題。 By controlling the average particle size and content range of the boron nitride raw material in the iron-platinum-based mixed raw material, and at the same time through the technical means of sieving, the iron-platinum-based target can be formed with a specific average size range and specific dispersion. The black phase in the uniformity range enables the prepared iron-platinum-based target to have better flexural strength, and at the same time, it can reduce the frequency of abnormal discharge and the problem of particle falling in the subsequent sputtering process.

依據本創作,在步驟(a)中的混合步驟可選用任何能夠均勻混合原料的方式,例如該混合步驟可為將原料置入混粉機中以達到均勻混合原料之目的,但不限於此。 According to the present invention, the mixing step in step (a) can be any method that can uniformly mix the raw materials, for example, the mixing step can be by placing the raw materials in a mixer to achieve the purpose of uniformly mixing the raw materials, but not limited to this.

依據本創作,於步驟(a)中的混合步驟完成後,可再接續進行一還原步驟,該還原步驟可為任何能夠使已發生氧化之原料還原的手段。舉例而言,該還原步驟可為氫氣還原法、真空還原法、碳還原法或鋅還原法,但不限於此。較佳的,該還原步驟為氫氣還原法。 According to the present invention, after the mixing step in step (a) is completed, a reduction step can be followed, and the reduction step can be any means capable of reducing the oxidized raw material. For example, the reduction step may be a hydrogen reduction method, a vacuum reduction method, a carbon reduction method or a zinc reduction method, but is not limited thereto. Preferably, the reduction step is a hydrogen reduction method.

依據本創作,於步驟(b)獲得該鐵鉑基混合原料後,可另接續進行一預壓步驟,該預壓步驟可為任何能夠將該鐵鉑基混合原料壓製成為具有固定形狀的手段。舉例而言,該預壓步驟可為將該鐵鉑基混合原料置入油壓機中並以約為250磅力每平方英吋(pound per square inch,psi)至350psi之壓力進行預壓,但不限於此。 According to the present invention, after the iron-platinum-based mixed raw material is obtained in step (b), a pre-pressing step may be performed successively, and the pre-pressing step may be any means capable of pressing the iron-platinum-based mixed raw material into a fixed shape. For example, the pre-pressing step can be performed by placing the iron-platinum-based mixed raw material in an oil press and pre-pressing at a pressure of about 250 pounds per square inch (psi) to 350 psi, but not limited to this.

較佳的,以該鐵鉑基混合原料整體之原子總數為基準,鉑原料的添加量係大於或等於10at%且小於或等於45at%。 Preferably, based on the total number of atoms of the whole iron-platinum-based mixed raw material, the addition amount of the platinum raw material is greater than or equal to 10 at% and less than or equal to 45 at%.

較佳的,以該鐵鉑基混合原料整體之原子總數為基準,氮化硼原料的添加量係大於或等於3at%且小於或等於30at%。更佳的,以該鐵鉑基靶材整體之原子總數為基準,氮化硼的含量係大於或等於5at%且小於或等於25at%。 Preferably, based on the total number of atoms of the whole iron-platinum-based mixed raw material, the addition amount of the boron nitride raw material is greater than or equal to 3 at% and less than or equal to 30 at%. More preferably, the content of boron nitride is greater than or equal to 5 at % and less than or equal to 25 at % based on the total number of atoms of the whole iron-platinum-based target.

較佳的,以該鐵鉑基混合原料整體之原子總數為基準,鐵原料的添加量係大於或等於5at%且小於或等於84at%。 Preferably, based on the total number of atoms of the whole iron-platinum-based mixed raw material, the addition amount of the iron raw material is greater than or equal to 5 at% and less than or equal to 84 at%.

較佳的,在步驟(b)中,該重複前述研磨與過篩的步驟係重複至少三次以上,以獲得該鐵鉑基混合原料。具體而言,該重複步驟係指該原料混合物經過研磨、過篩的步驟後,取篩上物再次以相同的條件進行研磨以及過篩。 Preferably, in step (b), the above-mentioned steps of grinding and sieving are repeated at least three times to obtain the iron-platinum-based mixed raw material. Specifically, the repeated steps refer to the steps of grinding and sieving the raw material mixture, and then taking the material on the sieve for grinding and sieving again under the same conditions.

在一些實施例中,該鐵鉑基混合原料更包含第一成分,該第一成分係選自由氧化物原料、碳化物原料、氮化物原料及其組合所組成之群組;其中,以該鐵鉑基混合原料整體之原子總數為基準,該第一成分的含量係大於0at%且小於或等於50at%,且該第一成分與氮化硼原料的添加量總和係大於或等於6at%且小於或等於50at%。較佳的,以該鐵鉑基混合原料整體之原子總數為基準,該第一成分的含量係大於或等於5at%且小於或等於35at%,且該第一成分與氮化硼原料的添加量總和係大於或等於6at%且小於或等於50at%。 In some embodiments, the iron-platinum-based mixed raw material further comprises a first component, and the first component is selected from the group consisting of oxide raw materials, carbide raw materials, nitride raw materials and combinations thereof; wherein, the iron is used as the raw material. Based on the total number of atoms of the whole platinum-based mixed raw material, the content of the first component is greater than 0at% and less than or equal to 50at%, and the total amount of the first component and the boron nitride raw material added is greater than or equal to 6at% and less than or equal to 50at%. Preferably, based on the total number of atoms of the whole iron-platinum-based mixed raw material, the content of the first component is greater than or equal to 5at% and less than or equal to 35at%, and the addition amount of the first component and the boron nitride raw material The sum is greater than or equal to 6 at% and less than or equal to 50 at%.

在一些實施例中,該鐵鉑基混合原料更包含碳原料,以該鐵鉑基混合原料整體之原子總數為基準,碳原料的添加量係大於或等於2at%且小於或等於40at%。 In some embodiments, the iron-platinum-based mixed raw material further comprises carbon raw material, and the amount of carbon raw material added is greater than or equal to 2 at% and less than or equal to 40 at% based on the total number of atoms of the entire iron-platinum-based mixed raw material.

在另一些實施例中,該鐵鉑基混合原料更包含第二成分,該第二成分係選自由銀原料、金原料、鍺原料、銅原料、鎳原料、鈷原料、鋁原料、鎂原料、錳原料、矽原料、鍶原料及其組合所組成之群組;其中,以該鐵鉑基混合原料整體之原子總數為基準,該第二成分的添加量係大於或等於2at%且小於或等於40at%。 In other embodiments, the iron-platinum-based mixed raw material further comprises a second component, and the second component is selected from silver raw materials, gold raw materials, germanium raw materials, copper raw materials, nickel raw materials, cobalt raw materials, aluminum raw materials, magnesium raw materials, A group consisting of manganese raw materials, silicon raw materials, strontium raw materials and their combinations; wherein, based on the total number of atoms of the entire iron-platinum-based mixed raw material, the addition amount of the second component is greater than or equal to 2at% and less than or equal to 40at%.

較佳的,在步驟(c)中,燒結溫度為600℃至1200℃,燒結壓力為350巴(bar)至1800bar。於其中一實施態樣,在步驟(c)中,燒結時間可為5分 鐘至4小時。更佳的,在步驟(c)中,燒結溫度為700℃至1100℃,燒結壓力為380bar至1750bar。於其中一實施態樣,在步驟(c)中,燒結時間可為3小時。 Preferably, in step (c), the sintering temperature is 600°C to 1200°C, and the sintering pressure is 350 bar to 1800 bar. In one embodiment, in step (c), the sintering time may be 5 minutes clock to 4 hours. More preferably, in step (c), the sintering temperature is 700°C to 1100°C, and the sintering pressure is 380 bar to 1750 bar. In one embodiment, in step (c), the sintering time may be 3 hours.

依據本創作,所述燒結步驟可為熱壓成型法(hot pressing,HP)、熱均壓成型法(hot isostatic pressing,HIP)或放電等離子體燒結法(spark plasma sintering,SPS)。舉例而言,當燒結步驟採用HP時,其燒結溫度可為800℃至1100℃,燒結壓力可為350bar至400bar,燒結時間可為2小時至4小時,但不限於此;當燒結步驟採用HIP時,其燒結溫度可為800℃至1100℃,燒結壓力可為1700bar至1800bar,燒結時間可為2小時至4小時,但不限於此;當燒結步驟採用SPS時,其燒結溫度可為700℃至1100℃,燒結壓力可為450bar至550bar,燒結時間可為5分鐘至1小時,但不限於此。 According to the present invention, the sintering step may be hot pressing (HP), hot isostatic pressing (HIP) or spark plasma sintering (SPS). For example, when HP is used in the sintering step, the sintering temperature can be 800°C to 1100°C, the sintering pressure can be 350bar to 400bar, and the sintering time can be 2 hours to 4 hours, but not limited thereto; when the sintering step adopts HIP , the sintering temperature can be 800℃ to 1100℃, the sintering pressure can be 1700bar to 1800bar, and the sintering time can be 2 hours to 4 hours, but not limited thereto; when the sintering step adopts SPS, the sintering temperature can be 700℃ To 1100° C., the sintering pressure may be 450 bar to 550 bar, and the sintering time may be 5 minutes to 1 hour, but not limited thereto.

圖1係實施例5之鐵鉑基靶材以掃描式電子顯微鏡放大2000倍之金相圖;圖2係比較例3之鐵鉑基靶材以掃描式電子顯微鏡放大2000倍之金相圖;圖3係實施例22之鐵鉑基靶材以掃描式電子顯微鏡放大2000倍之金相圖;圖4係比較例17之鐵鉑基靶材以掃描式電子顯微鏡放大2000倍之金相圖。 Figure 1 is a metallographic diagram of the iron-platinum-based target of Example 5 magnified by a scanning electron microscope 2000 times; Figure 2 is a metallographic diagram of the iron-platinum-based target of Comparative Example 3 magnified 2000 times by a scanning electron microscope; Figure 3 is a metallographic image of the iron-platinum-based target of Example 22 magnified 2000 times by a scanning electron microscope; Figure 4 is a metallographic image of the iron-platinum-based target of Comparative Example 17 magnified 2000 times by a scanning electron microscope.

為驗證氮化硼的含量、金相中黑色相的平均尺寸以及金相中黑色相的分散均勻度對鐵鉑基靶材的影響,以下列舉數種鐵鉑基靶材作為例示,詳細說明本創作的實施方式,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創作所能達成之優點與功效,並且於不悖離本創作之精神下進行各種修飾與變更,以施行或應用本創作之內容。 In order to verify the influence of the content of boron nitride, the average size of the black phase in the metallographic phase, and the dispersion uniformity of the black phase in the metallographic phase on the iron-platinum-based target, several iron-platinum-based targets are listed below as examples, and the embodiments of this invention are described in detail. , those with ordinary knowledge in the technical field can easily understand the advantages and effects of this creation through the content of this specification, and make various modifications and changes without departing from the spirit of this creation, in order to implement or apply this creation. content.

實施例1至5:鐵鉑基靶材Examples 1 to 5: Iron-platinum-based targets

依據下表1所列之鐵鉑基靶材的組成,秤取適量平均粒徑小於100微米之鐵粉末、平均粒徑小於20微米之鉑粉末以及平均粒徑小於5微米之氮化硼粉末置於混粉機中混合,隨後將混合後的粉末以氫氣還原法進行還原,接著將還原後的混合粉末置入高速研磨機中進行研磨4至12小時,隨後以800目數至1200目數的篩網過篩,並取篩上物重複三次前述研磨與過篩的流程,以獲得該鐵鉑基混合粉末。 According to the composition of the iron-platinum-based target listed in Table 1 below, weigh an appropriate amount of iron powder with an average particle size of less than 100 microns, platinum powder with an average particle size of less than 20 microns and boron nitride powder with an average particle size of less than 5 microns. Mix in a powder mixer, and then reduce the mixed powder by hydrogen reduction method, then put the reduced mixed powder into a high-speed mill for grinding for 4 to 12 hours, and then use 800 to 1200 mesh. The sieve is sieved, and the above-mentioned material on the sieve is taken and repeated three times to obtain the iron-platinum-based mixed powder.

接著,將該鐵鉑基混合粉末置入油壓機中並以約為300psi之壓力進行預壓,隨後依據下表1所列之燒結製程以及燒結溫度進行燒結,以獲得實施例1至5之鐵鉑基靶材,其中,若燒結步驟採用HP,其燒結壓力約為380bar、燒結時間為3小時;若燒結步驟採用SPS,其燒結壓力約為500bar、燒結時間為10分鐘。 Next, the iron-platinum-based mixed powder was placed in a hydraulic press and pre-pressed at a pressure of about 300 psi, and then sintered according to the sintering process and sintering temperature listed in Table 1 below, to obtain the iron-platinum of Examples 1 to 5 For the base target, if HP is used in the sintering step, the sintering pressure is about 380 bar and the sintering time is 3 hours; if the sintering step is SPS, the sintering pressure is about 500 bar and the sintering time is 10 minutes.

於下表1中,實施例1至5之鐵鉑基靶材的組成可由aFe-bPt-cBN之通式所示;其中,a代表鐵相對於鐵鉑基靶材之原子總數的含量比例,b代表鉑相對於鐵鉑基靶材之原子總數的含量比例,c代表氮化硼相對於鐵鉑基靶材之原子總數的含量比例。 In Table 1 below, the composition of the iron-platinum-based targets of Examples 1 to 5 can be represented by the general formula of aFe-bPt-cBN; wherein, a represents the content ratio of iron relative to the total number of atoms of the iron-platinum-based target material, b represents the content ratio of platinum to the total number of atoms of the iron-platinum-based target, and c represents the content ratio of boron nitride to the total number of atoms of the iron-platinum-based target.

實施例6至7:鐵鉑基靶材(含有碳)Examples 6 to 7: Iron-platinum-based targets (containing carbon)

實施例6至7與實施例1至5的製作流程相似,即秤取適量的不同成分粉末經過混合、還原、研磨過篩、預壓以及燒結等步驟後,獲得實施例6至7之鐵鉑基靶材。實施例6至7所採用的燒結製程以及燒結溫度列於下表1中,其中,若燒結步驟採用HP,其燒結壓力約為380bar、燒結時間為3小時;若燒結步驟採用SPS,其燒結壓力約為500bar、燒結時間為10分鐘。 The production processes of Examples 6 to 7 are similar to those of Examples 1 to 5, that is, after weighing an appropriate amount of powders of different components and going through the steps of mixing, reducing, grinding and sieving, pre-pressing and sintering, the iron platinum of Examples 6 to 7 is obtained. base target. The sintering process and sintering temperature used in Examples 6 to 7 are listed in Table 1 below. If the sintering step adopts HP, the sintering pressure is about 380 bar and the sintering time is 3 hours; if the sintering step adopts SPS, the sintering pressure About 500 bar, the sintering time is 10 minutes.

實施例6至7與實施例1至5的不同之處在於依據下表1所列之鐵鉑基靶材的組成,秤取適量平均粒徑小於100微米之鐵粉末、平均粒徑小於20微 米之鉑粉末、平均粒徑小於5微米之氮化硼粉末以及平均粒徑小於10微米之碳粉末置於混粉機中混合。 The difference between Examples 6 to 7 and Examples 1 to 5 is that according to the composition of the iron-platinum-based target listed in Table 1 below, an appropriate amount of iron powder with an average particle size of less than 100 microns and an average particle size of less than 20 microns are weighed. The platinum powder of rice, the boron nitride powder with an average particle size of less than 5 microns, and the carbon powder with an average particle size of less than 10 microns are mixed in a mixer.

於下表1中,實施例6至7之鐵鉑基靶材的組成可由aFe-bPt-cBN-d1C之通式所示;其中,a、b以及c如前述分別代表鐵、鉑以及氮化硼相對於鐵鉑基靶材之原子總數的含量比例,d1則代表碳相對於鐵鉑基靶材之原子總數的含量比例。 In Table 1 below, the composition of the iron-platinum-based targets of Examples 6 to 7 can be represented by the general formula of aFe-bPt-cBN-d1C; wherein a, b and c respectively represent iron, platinum and nitride as previously described The content ratio of boron to the total number of atoms of the iron-platinum-based target, and d1 represents the content ratio of carbon to the total number of atoms of the iron-platinum-based target.

實施例8至13:鐵鉑基靶材(含有第一成分)Examples 8 to 13: Iron-platinum-based targets (containing the first component)

實施例8至13與實施例1至5的製作流程相似,即秤取適量的不同成分粉末經過混合、還原、研磨過篩、預壓以及燒結等步驟後,獲得實施例8至13之鐵鉑基靶材。實施例8至13所採用的燒結製程以及燒結溫度列於下表1中,其中,若燒結步驟採用HP,其燒結壓力約為380bar、燒結時間為3小時;若燒結步驟採用SPS,其燒結壓力約為500bar、燒結時間為10分鐘;若燒結步驟採用HIP,其燒結壓力約為1750bar、燒結時間為3小時。 Examples 8 to 13 are similar to the production processes of Examples 1 to 5, that is, weigh an appropriate amount of powders of different components and go through the steps of mixing, reducing, grinding and sieving, pre-pressing and sintering to obtain the iron platinum of Examples 8 to 13. base target. The sintering process and sintering temperature used in Examples 8 to 13 are listed in Table 1 below. If the sintering step adopts HP, the sintering pressure is about 380 bar and the sintering time is 3 hours; if the sintering step adopts SPS, the sintering pressure The sintering time is about 500 bar and the sintering time is 10 minutes; if the sintering step adopts HIP, the sintering pressure is about 1750 bar and the sintering time is 3 hours.

實施例8至13與實施例1至5的不同之處在於依據下表1所列之鐵鉑基靶材的組成,秤取適量平均粒徑小於100微米之鐵粉末、平均粒徑小於20微米之鉑粉末、平均粒徑小於5微米之氮化硼粉末以及平均粒徑小於10微米之第一成分置於混粉機中混合。於此,該第一成分可為碳化硼粉末、二氧化矽粉末、氮化鋁粉末、二氧化鈦粉末、碳化鉭粉末、五氧化二鉭粉末、氮化鈦粉末、碳化鉻粉末或其組合。 The difference between Examples 8 to 13 and Examples 1 to 5 is that according to the composition of the iron-platinum-based target listed in Table 1 below, an appropriate amount of iron powder with an average particle size of less than 100 microns and an average particle size of less than 20 microns are weighed. The platinum powder, the boron nitride powder with an average particle size of less than 5 microns, and the first component with an average particle size of less than 10 microns are placed in a mixer to mix. Here, the first component may be boron carbide powder, silicon dioxide powder, aluminum nitride powder, titanium dioxide powder, tantalum carbide powder, tantalum pentoxide powder, titanium nitride powder, chromium carbide powder, or a combination thereof.

於下表1中,實施例8至13之鐵鉑基靶材的組成可由aFe-bPt-cBN-d2B4C-d3SiO2-d4AlN-d5TiO2-d6TaC-d7Ta2O5-d8TiN-d9Cr3C2之通式所示;其中,a、b以及c如前述分別代表鐵、鉑以及氮化硼相對於鐵鉑基靶材之原子總數的含量比例,d2、d3、d4、d5、d6、d7、d8、d9則分別代表碳化硼、二氧化 矽、氮化鋁、二氧化鈦、碳化鉭、五氧化二鉭、氮化鈦以及碳化鉻相對於鐵鉑基靶材之原子總數的含量比例。 In Table 1 below, the compositions of the iron-platinum-based targets of Examples 8 to 13 may be aFe-bPt-cBN-d2B 4 C-d3SiO 2 -d4AlN-d5TiO 2 -d6TaC-d7Ta 2 O 5 -d8TiN-d9Cr 3 C 2 is shown in the general formula; wherein, a, b and c respectively represent the content ratio of iron, platinum and boron nitride relative to the total number of atoms of the iron-platinum-based target, d2, d3, d4, d5, d6, d7 , d8, and d9 respectively represent the content ratio of boron carbide, silicon dioxide, aluminum nitride, titanium dioxide, tantalum carbide, tantalum pentoxide, titanium nitride and chromium carbide relative to the total number of atoms in the iron-platinum-based target.

於本說明書中,所述「氮化硼與該第一成分的含量總和」係指c、d2、d3、d4、d5、d6、d7、d8、d9之總和。 In this specification, the "total content of boron nitride and the first component" refers to the sum of c, d2, d3, d4, d5, d6, d7, d8, and d9.

實施例14:鐵鉑基靶材(含有第二成分)Example 14: Iron-platinum-based target (containing the second component)

實施例14與實施例1至5的製作流程相似,即秤取適量的不同成分粉末經過混合、還原、研磨過篩、預壓以及燒結等步驟後,獲得實施例14之鐵鉑基靶材。實施例14所採用的燒結製程以及燒結溫度列於下表1中,其中,實施例14的燒結步驟採用HP,其燒結壓力約為380bar、燒結時間為3小時。 The production process of Example 14 is similar to that of Examples 1 to 5, that is, an appropriate amount of powders of different components are weighed and subjected to the steps of mixing, reduction, grinding and sieving, pre-pressing and sintering to obtain the iron-platinum-based target of Example 14. The sintering process and sintering temperature used in Example 14 are listed in Table 1 below, wherein the sintering step in Example 14 adopts HP, the sintering pressure is about 380 bar, and the sintering time is 3 hours.

實施例14與實施例1至5的不同之處在於依據下表1所列之鐵鉑基靶材的組成,秤取適量平均粒徑小於100微米之鐵粉末、平均粒徑小於20微米之鉑粉末、平均粒徑小於5微米之氮化硼粉末以及平均粒徑小於20微米之第二成分置於混粉機中混合。於此,該第二成分為銀粉末。 The difference between Example 14 and Examples 1 to 5 is that according to the composition of the iron-platinum-based target listed in Table 1 below, an appropriate amount of iron powder with an average particle size of less than 100 microns and platinum with an average particle size of less than 20 microns are weighed. The powder, the boron nitride powder with an average particle size of less than 5 microns and the second component with an average particle size of less than 20 microns are mixed in a mixer. Here, the second component is silver powder.

於下表1中,實施例14之鐵鉑基靶材的組成可由aFe-bPt-cBN-e1Ag之通式所示;其中,a、b以及c如前述分別代表鐵、鉑以及氮化硼相對於鐵鉑基靶材之原子總數的含量比例,e1則代表銀相對於鐵鉑基靶材之原子總數的含量比例。 In Table 1 below, the composition of the iron-platinum-based target material of Example 14 can be represented by the general formula of aFe-bPt-cBN-e1Ag; wherein a, b and c respectively represent iron, platinum and boron nitride as mentioned above. Regarding the content ratio of the total number of atoms of the iron-platinum-based target, e1 represents the content ratio of silver to the total number of atoms of the iron-platinum-based target.

實施例15至25:鐵鉑基靶材(含有第一成分及第二成分)Examples 15 to 25: Iron-platinum-based targets (containing the first and second components)

實施例15至25與實施例1至5的製作流程相似,即秤取適量的不同成分粉末經過混合、還原、研磨過篩、預壓以及燒結等步驟後,獲得實施例15至25之鐵鉑基靶材。實施例15至25所採用的燒結製程以及燒結溫度列於下表1中,其中,若燒結步驟採用HP,其燒結壓力約為380bar、燒結時間為3小時;若燒結步驟採用SPS,其燒結壓力約為500bar、燒結時間為10分鐘;若燒結步驟採用HIP,其燒結壓力約為1750bar、燒結時間為3小時。 Examples 15 to 25 are similar to the production processes of Examples 1 to 5, that is, after weighing an appropriate amount of powders of different components and going through the steps of mixing, reducing, grinding and sieving, pre-pressing and sintering, the iron platinum of Examples 15 to 25 is obtained. base target. The sintering process and sintering temperature used in Examples 15 to 25 are listed in Table 1 below. If the sintering step adopts HP, the sintering pressure is about 380 bar and the sintering time is 3 hours; if the sintering step adopts SPS, the sintering pressure The sintering time is about 500 bar and the sintering time is 10 minutes; if the sintering step adopts HIP, the sintering pressure is about 1750 bar and the sintering time is 3 hours.

實施例15至25與實施例1至5的不同之處在於依據下表1所列之鐵鉑基靶材的組成,秤取適量平均粒徑小於100微米之鐵粉末、平均粒徑小於20微米之鉑粉末、平均粒徑小於5微米之氮化硼粉末、平均粒徑小於20微米之第一成分以及平均粒徑小於20微米之第二成分置於混粉機中混合。於此,該第一成分可為碳化矽粉末、三氧化二鉻粉末、氧化鈷粉末、氮化鋁粉末、氧化鎂粉末、三氧化二錳粉末、二氧化矽粉末、二氧化鈦粉末、三氧化二鋁粉末、氮化鈦粉末、三氧化二硼粉末、二氧化鉿粉末或其組合;該第二成分可為銀粉末、銅粉末、鎂粉末、錳粉末、鈷粉末、鍺粉末、鋁粉末、鎳粉末、矽粉末、鍶粉末、金粉末或其組合。 The difference between Examples 15 to 25 and Examples 1 to 5 is that according to the composition of the iron-platinum-based target listed in Table 1 below, an appropriate amount of iron powder with an average particle size of less than 100 microns and an average particle size of less than 20 microns are weighed. The platinum powder, the boron nitride powder with an average particle size of less than 5 microns, the first component with an average particle size of less than 20 microns, and the second component with an average particle size of less than 20 microns are mixed in a mixer. Here, the first component can be silicon carbide powder, chromium oxide powder, cobalt oxide powder, aluminum nitride powder, magnesium oxide powder, manganese oxide powder, silicon dioxide powder, titanium dioxide powder, aluminum oxide powder powder, titanium nitride powder, boron trioxide powder, hafnium dioxide powder or a combination thereof; the second component can be silver powder, copper powder, magnesium powder, manganese powder, cobalt powder, germanium powder, aluminum powder, nickel powder , silicon powder, strontium powder, gold powder, or a combination thereof.

此外,依據下表1所列實施例15、16、20以及23之鐵鉑基靶材的組成,可於前述製程中秤取適量平均粒徑小於20微米之碳粉末與前述粉末一起置於混粉機中混合。 In addition, according to the composition of the iron-platinum-based targets of Examples 15, 16, 20 and 23 listed in Table 1 below, an appropriate amount of carbon powder with an average particle size of less than 20 microns can be weighed and placed together with the aforementioned powder in the aforementioned process. Mix in a mixer.

於下表1中,實施例15至25之鐵鉑基靶材的組成可由aFe-bPt-cBN-d1C-d3SiO2-d4AlN-d5TiO2-d8TiN-d10SiC-d11Cr2O3-d12CoO-d13MgO-d14Mn2O3-d15Al2O3-d16B2O3-d17HfO2-e1Ag-e2Cu-e3Mg-e4Mn-e5Co-e6Ge-e7Al-e8Ni-e9Si-e10Sr-e11Au之通式所示;其中,a、b以及c如前述分別代表鐵、鉑以及氮化硼相對於鐵鉑基靶材之原子總數的含量比例,d1、d3、d4、d5、d8、d10、d11、d12、d13、d14、d15、d16、d17則分別代表碳、二氧化矽、氮化鋁、二氧化鈦、氮化鈦、碳化矽、三氧化二鉻、氧化鈷、氧化鎂、三氧化二錳、三氧化二鋁、三氧化二硼以及二氧化鉿相對於鐵鉑基靶材之原子總數的含量比例,e1、e2、e3、e4、e5、e6、e7、e8、e9、e10、e11則分別代表銀、銅、鎂、錳、鈷、鍺、鋁、鎳、矽、鍶以及金相對於鐵鉑基靶材之原子總數的含量比例。 In Table 1, the embodiment of the iron 15 to 25 may be composed of a platinum-based target aFe-bPt-cBN-d1C- d3SiO 2 -d4AlN-d5TiO 2 -d8TiN-d10SiC-d11Cr 2 O 3 -d12CoO-d13MgO-d14Mn Example 2 O 3 -d15Al 2 O 3 -d16B 2 O 3 -d17HfO 2 -e1Ag-e2Cu-e3Mg-e4Mn-e5Co-e6Ge-e7Al-e8Ni-e9Si-e10Sr-e11Au is shown in the general formula; among them, a, b and c represents the content ratio of iron, platinum and boron nitride to the total number of atoms in the iron-platinum-based target as mentioned above, d1, d3, d4, d5, d8, d10, d11, d12, d13, d14, d15, d16, d17 represents carbon, silicon dioxide, aluminum nitride, titanium dioxide, titanium nitride, silicon carbide, chromium oxide, cobalt oxide, magnesium oxide, manganese oxide, aluminum oxide, boron oxide and The content ratio of hafnium oxide to the total number of atoms in the iron-platinum-based target, e1, e2, e3, e4, e5, e6, e7, e8, e9, e10, e11 represent silver, copper, magnesium, manganese, cobalt, The content ratio of germanium, aluminum, nickel, silicon, strontium and gold relative to the total number of atoms in the iron-platinum-based target.

於本說明書中,所述「第二成分的含量」係指e1、e2、e3、e4、e5、e6、e7、e8、e9、e10以及e11之總和。 In this specification, the "content of the second component" refers to the sum of e1, e2, e3, e4, e5, e6, e7, e8, e9, e10, and e11.

比較例1至20:鐵鉑基靶材Comparative Examples 1 to 20: Iron-platinum-based targets

比較例1至20之製備方法與實施例大致相同,其主要不同之處在於氮化硼粉末的平均粒徑並未小於5微米以及還原後的混合粉末於高速研磨後並未再進行過篩步驟,除此之外皆依照實施例的製備流程製得比較例1至20之鐵鉑基靶材。比較例1至20之鐵鉑基靶材的組成以及各成分以原子百分比記的含量皆列於下表1中,比較例1至20之鐵鉑基靶材亦可如同前述各實施例所載之通式表示,且其中各成分的含量表示方式亦如同前述各實施例所載。 The preparation methods of Comparative Examples 1 to 20 are basically the same as those of the Examples, the main difference is that the average particle size of the boron nitride powder is not less than 5 microns and the reduced mixed powder is not subjected to a sieving step after high-speed grinding. , other than that, the iron-platinum-based targets of Comparative Examples 1 to 20 were prepared according to the preparation process of the examples. The compositions of the iron-platinum-based targets of Comparative Examples 1 to 20 and the content of each component in atomic percentage are listed in Table 1 below. The general formula is expressed, and the content of each component is expressed as described in the foregoing embodiments.

比較例21至22:鐵鉑基靶材Comparative Examples 21 to 22: Iron-platinum-based targets

先將鑽石碳粉及複數個直徑為5毫米(mm)的磨球放置於一球磨罐,進行高能球磨3小時後得一經研磨的鑽石碳粉,其平均粒徑為0.5微米,接著再將氮化硼以400目數的篩網進行過篩,隨後,依照下表1所列之組成秤取鐵原料、鉑原料、所述經研磨後的鑽石碳粉以及所述過篩後的氮化硼,並混合以得到一混合物。再將該混合物進行高能球磨3小時後獲得一鐵鉑基合金粉末,再依照下表1所列之燒結製程和燒結溫度,將所述鐵鉑基合金粉末進行燒結3小時,以獲得比較例21及22之鐵鉑基靶材。比較例21及22之鐵鉑基靶材的組成以及各成分以原子百分比記的含量皆列於下表1中,比較例21及22之鐵鉑基靶材亦可如同前述各實施例所載之通式表示,且其中各成分的含量表示方式亦如同前述各實施例所載。 First, the diamond carbon powder and a plurality of grinding balls with a diameter of 5 millimeters (mm) were placed in a ball mill, and after high-energy ball milling for 3 hours, a ground diamond carbon powder with an average particle size of 0.5 microns was obtained. Boronide is sieved with a 400-mesh sieve, and then, iron raw material, platinum raw material, the ground diamond carbon powder and the sieved boron nitride are weighed according to the composition listed in Table 1 below. , and mixed to obtain a mixture. The mixture was then subjected to high-energy ball milling for 3 hours to obtain an iron-platinum-based alloy powder, and the iron-platinum-based alloy powder was sintered for 3 hours according to the sintering process and sintering temperature listed in Table 1 to obtain Comparative Example 21 And 22 iron platinum-based targets. The compositions of the iron-platinum-based targets of Comparative Examples 21 and 22 and the content of each component in atomic percent are listed in Table 1 below. The general formula is expressed, and the content of each component is expressed as described in the foregoing embodiments.

Figure 109133429-A0305-02-0017-1
Figure 109133429-A0305-02-0017-1
Figure 109133429-A0305-02-0018-2
Figure 109133429-A0305-02-0018-2
Figure 109133429-A0305-02-0019-3
Figure 109133429-A0305-02-0019-3

分析1:鐵鉑基靶材之金相微結構Analysis 1: Metallographic microstructure of iron-platinum-based targets

分析1-1:觀察金相中黑色相的分布型態和形貌Analysis 1-1: Observe the distribution and morphology of the black phase in the metallographic phase

先將實施例1至25與比較例1至22之鐵鉑基靶材進一步進行以線割與磨床加工後,製得直徑為2英吋、厚度為3mm的圓形靶材,再分別於距離圓心為0.5半徑的靶材部位進行採樣,以線割方式取得一10mm×10mm的試片。 First, the iron-platinum-based targets of Examples 1 to 25 and Comparative Examples 1 to 22 were further processed by wire cutting and grinding to obtain circular targets with a diameter of 2 inches and a thickness of 3 mm. The center of the target is 0.5 radius for sampling, and a 10mm × 10mm test piece is obtained by wire cutting.

接著以掃描式電子顯微鏡(型號為Hitachi製造的SE-3400)以2000倍的放大倍率拍攝實施例1至25與比較例1至22之鐵鉑基靶材的試片的金相微結構。於此以實施例5、比較例3、實施例22以及比較例17之鐵鉑基靶材進行示範性說明,其拍攝結果分別如圖1至圖4所示。比較圖1與圖2以及圖3與圖4的結果可明顯觀察到,實施例5及實施例22之鐵鉑基靶材中的黑色相呈現點狀均勻分布的型態,反觀比較例3及比較例17之鐵鉑基靶材中的黑色相則呈現狹長形且較為粗大的型態,且有黑色相分布不均勻的現象。 Next, the metallographic microstructures of the test pieces of the iron-platinum-based targets of Examples 1 to 25 and Comparative Examples 1 to 22 were photographed with a scanning electron microscope (model SE-3400 manufactured by Hitachi) at a magnification of 2000 times. Herein, the iron-platinum-based targets of Example 5, Comparative Example 3, Example 22, and Comparative Example 17 are used for exemplary illustration, and the photographing results are shown in FIG. 1 to FIG. 4 , respectively. Comparing the results of Fig. 1 and Fig. 2 and Fig. 3 and Fig. 4, it can be clearly observed that the black phase in the iron-platinum-based targets of Example 5 and Example 22 presents a point-like uniform distribution pattern. The black phase in the iron-platinum-based target of Comparative Example 17 was elongated and relatively coarse, and the distribution of the black phase was uneven.

分析1-2:金相中黑色相之平均尺寸Analysis 1-2: Average size of black phase in metallography

採用影像分析軟體Image J,分別分析實施例1至25與比較例1至22之鐵鉑基靶材的試片的金相,所述金相係以與分析1相同的方式,採用掃描式電子顯微鏡以放大2000倍的倍率進行拍攝而得,其拍攝方式皆為於同一試片中以隨機方式拍攝五個不同區域,並獲得五張金相圖,再直接以所述影像分析軟體ImageJ中內建之分析平均粒徑功能「Feret’s Diameter」統計出前述五張金相圖中黑色相之尺寸,最後再以軟體計算前述五張金相圖中的黑色相之平均尺寸,以代表所述鐵鉑基靶材的黑色相之平均尺寸,並將結果記載於下表2中。 The image analysis software Image J was used to analyze the metallographic phases of the test pieces of the iron-platinum-based targets of Examples 1 to 25 and Comparative Examples 1 to 22, respectively. The microscope was photographed at a magnification of 2000 times. The photographing method was to randomly photograph five different areas in the same test piece, and obtain five metallographic images, and then directly use the built-in image analysis software ImageJ. The average particle size analysis function "Feret's Diameter" counts the size of the black phase in the five metallographic diagrams, and finally calculates the average size of the black phase in the five metallographic diagrams by software to represent the black phase of the iron-platinum-based target. average size, and the results are recorded in Table 2 below.

分析1-3:金相中黑色相之分散均勻度Analysis 1-3: Dispersion uniformity of black phase in metallography

同樣採用影像分析軟體Image J,並將分析1-2經拍攝得到之實施例1至25與比較例1至22之鐵鉑基靶材的試片的金相圖,再進一步以所述影像分析軟體內建之「Area」功能分析出金相圖的總面積、金相圖中黑色相的總面積以及黑色相的個數,接著依據本說明書所定義之分散均勻度的計算方式計算得到黑色相的分散均勻度,最後再以軟體計算前述五張金相圖中的黑色相之分散均勻度,以代表所述鐵鉑基靶材的黑色相之分散均勻度,並將結果記載於下表2中。 The image analysis software Image J was also used to analyze the metallographic diagrams of the test pieces of the iron-platinum-based targets of Examples 1 to 25 and Comparative Examples 1 to 22 obtained by analyzing 1-2, and further analyze the images with the images. The "Area" function built into the software analyzes the total area of the metallographic diagram, the total area of the black phase in the metallographic diagram and the number of black phases, and then calculates the black phase according to the calculation method of dispersion uniformity defined in this manual. Finally, the dispersion uniformity of the black phase in the aforementioned five metallographic diagrams is calculated by software to represent the dispersion uniformity of the black phase of the iron-platinum-based target, and the results are recorded in Table 2 below.

分析2:緻密程度量測與抗折強度分析Analysis 2: Density Measurement and Flexural Strength Analysis

先將實施例1至25與比較例1至22之鐵鉑基靶材進一步進行以線割與磨床加工,以製得尺寸為厚3mm、寬4mm、長25mm的試片,並透過阿基米德法方式得到實施例1至25與比較例1至22之鐵鉑基靶材的緻密程度,並將結果紀錄於下表2中。 First, the iron-platinum-based targets of Examples 1 to 25 and Comparative Examples 1 to 22 were further processed by wire cutting and grinding to obtain test pieces with a thickness of 3 mm, a width of 4 mm, and a length of 25 mm. The compactness of the iron-platinum-based targets of Examples 1 to 25 and Comparative Examples 1 to 22 was obtained by German method, and the results were recorded in Table 2 below.

接著,將實施例1至25與比較例1至22之鐵鉑基靶材的試片置於萬能試驗機上以量測三點抗折,具體步驟為將試片放置於三點抗折治具,並以跨距為20mm、加壓速度為每秒0.008mm之操作條件,量測試片彎曲至斷裂前的最大荷重,再依照以下算式進行計算:抗折強度=(3×最大荷重×跨距)/(2 ×試片寬度×試片厚度×試片厚度),以得到實施例1至25與比較例1至22之鐵鉑基靶材的抗折強度,並將結果紀錄於下表2中。 Next, place the test pieces of the iron-platinum-based targets of Examples 1 to 25 and Comparative Examples 1 to 22 on a universal testing machine to measure the three-point bending resistance. Under the operating conditions of a span of 20mm and a pressing speed of 0.008mm per second, measure the maximum load before the test piece is bent to break, and then calculate it according to the following formula: Flexural strength = (3 × maximum load × span distance)/(2 × width of the test piece × thickness of the test piece × thickness of the test piece) to obtain the flexural strength of the iron-platinum-based targets of Examples 1 to 25 and Comparative Examples 1 to 22, and the results are recorded in Table 2 below.

分析3:靶材濺鍍品質分析Analysis 3: Target sputtering quality analysis

先將實施例1至25與比較例1至22之鐵鉑基靶材進一步進行以線割與磨床加工後,製得直徑為2英吋、厚度為3mm的圓形靶材,接著將該靶材置於持續通有50sccm(Standard Cubic Centimeter per Minute)之氬氣流量、0.01托耳(torr)至0.001托耳之真空度的磁控濺鍍機台(高敦科技所組裝)中,再以200瓦(W)之功率預濺鍍(pre-sputter)該靶材600秒,以清除靶材表面的髒汙,獲得可供評估其濺鍍品質的待測靶材。 The iron-platinum-based targets of Examples 1 to 25 and Comparative Examples 1 to 22 were further processed by wire cutting and grinding to obtain circular targets with a diameter of 2 inches and a thickness of 3 mm. The material was placed in a magnetron sputtering machine (assembled by Gordon Technology) with a continuous flow of 50sccm (Standard Cubic Centimeter per Minute) and a vacuum of 0.01 torr to 0.001 Torr. The target was pre-sputtered with a power of 200 watts (W) for 600 seconds to remove contamination on the surface of the target to obtain a target to be tested for evaluating the sputtering quality.

接著,使該待測靶材置於通有50sccm之氬氣流量、0.01托耳至0.001托耳之真空度的濺鍍環境下,以50W至150W之功率持續進行濺鍍製程300秒,並監測各待測靶材在濺鍍製程中發生異常放電的次數以及微粒掉落的數量,其中,微粒掉落數量係使用KLA-Tencor Surfscan 6420偵測掉落微粒中尺寸在0.5微米以上的微粒數量,並將結果紀錄於下表2中。 Next, the target to be tested is placed in a sputtering environment with an argon flow rate of 50 sccm and a vacuum of 0.01 Torr to 0.001 Torr, and the sputtering process is continued at a power of 50W to 150W for 300 seconds, and monitoring The number of abnormal discharges and the number of particles dropped during the sputtering process of each target to be measured The results are recorded in Table 2 below.

Figure 109133429-A0305-02-0022-7
Figure 109133429-A0305-02-0022-7
Figure 109133429-A0305-02-0023-5
Figure 109133429-A0305-02-0023-5
Figure 109133429-A0305-02-0024-6
Figure 109133429-A0305-02-0024-6

實驗結果討論Discussion of experimental results

根據本創作各實施例的製作流程並配合表2的結果可知,藉由控制氮化硼粉末的含量與平均粒徑於特定範圍中,並同時透過過篩之技術手段,使所製得之鐵鉑基靶材中的氮化硼含量不超過50at%,且所述鐵鉑基靶材的金相中黑色相的平均尺寸小於3微米,以及黑色相的分散均勻度小於5×10-4,據此,實施例1至25之鐵鉑基靶材皆同時具有抗折強度大於或等於700MPa、異常放電次數低於30次以及微粒掉落數量低於50顆的功效;反觀各比較例於製程中並沒有同時控制氮化硼粉末的含量與平均粒徑,也沒有進行研磨後過篩的步驟,因此無法同時符合本創作所界定氮化硼含量、黑色相的平均尺寸以及黑色相的分散均勻度的特定範圍,不僅無法穩定地提升鐵鉑基靶材的抗折強度,更無法有效降低異常放電次數(最低仍有36次)以及微粒掉落數量(最低仍有105顆)。 According to the production process of each embodiment of the present invention and the results in Table 2, it can be seen that by controlling the content and average particle size of boron nitride powder within a specific range, and at the same time through the technical means of sieving, the prepared iron The content of boron nitride in the platinum-based target is not more than 50at%, and the average size of the black phase in the metallographic phase of the iron-platinum-based target is less than 3 microns, and the dispersion uniformity of the black phase is less than 5×10 -4 , accordingly , the iron-platinum-based targets of Examples 1 to 25 all have the effects of flexural strength greater than or equal to 700 MPa, abnormal discharge times less than 30 times and particle drop number less than 50; The content and average particle size of the boron nitride powder are not controlled at the same time, and the step of sieving after grinding is not carried out, so it cannot meet the requirements of the boron nitride content, the average size of the black phase and the dispersion uniformity of the black phase as defined in this work. In a specific range, not only can it not stably improve the flexural strength of the iron-platinum-based target, but also cannot effectively reduce the number of abnormal discharges (the minimum is still 36) and the number of particles dropped (the minimum is still 105).

再進一步參看實施例1、實施例5以及比較例1、比較例4的組別,相較於比較例1(氮化硼含量為60at%)以及比較例4(氮化硼含量為0at%),實施例1(氮化硼含量為0.1at%)以及實施例5(氮化硼含量為50at%)的氮化硼含量由於在本創作所界定的大於0at%且小於或等於50at%的特定範圍中,因此實施例1與實施例5不論在抗折強度(分別為1476MPa以及871MPa)、異常放電次數(分別為0次以及15次)或微粒掉落數量(分別為1顆以及36顆)的結果皆優於比較例1以及比較例4的結果(抗折強度分別為467MPa以及824MPa;異常放電次數分別為103次以及226次;微粒掉落數量分別為1666顆以及1394顆)。由此可知,將氮化硼的含量控制於特定範圍中確實有助於提升靶材的抗折強度、降低異常放電發生以及減少微粒掉落。 Further referring to the groups of Example 1, Example 5, Comparative Example 1, and Comparative Example 4, compared with Comparative Example 1 (with a boron nitride content of 60 at%) and Comparative Example 4 (with a boron nitride content of 0 at%) , the boron nitride content of Example 1 (with a boron nitride content of 0.1 at%) and Example 5 (with a boron nitride content of 50 at%) is due to the specific characteristics defined in this work that are greater than 0 at% and less than or equal to 50 at% Therefore, in Example 1 and Example 5, regardless of the flexural strength (1476MPa and 871MPa, respectively), the number of abnormal discharges (0 and 15, respectively) or the number of particles dropped (1 and 36, respectively) The results are better than those of Comparative Example 1 and Comparative Example 4 (flexural strength of 467 MPa and 824 MPa, respectively; number of abnormal discharges: 103 and 226; number of particles dropped: 1666 and 1394). From this, it can be seen that controlling the content of boron nitride in a specific range is indeed helpful to improve the flexural strength of the target material, reduce the occurrence of abnormal discharge, and reduce the drop of particles.

再進一步參看實施例4與比較例3的組別,雖然比較例3的組成與實施例4完全相同,即比較例3的氮化硼含量在本創作所界定的範圍中,但其所 具有的黑色相平均尺寸以及分散均勻度皆不在本創作所界定之範圍中,據此,實施例4在抗折強度(911MPa)、異常放電次數(11次)以及微粒掉落數量(20顆)的結果皆遠優於比較例3(分別為812MPa、106次以及895顆)。由此可知,除了氮化硼的含量需控制於特定範圍外,黑色相平均尺寸以及分散均勻度亦需控制於本創作所界定之特定範圍中,才能同時有效地提升靶材的抗折強度、減少異常放電與微粒掉落。 Further referring to the groups of Example 4 and Comparative Example 3, although the composition of Comparative Example 3 is exactly the same as that of Example 4, that is, the content of boron nitride in Comparative Example 3 is within the range defined by this work, but the The average size of the black phase and the uniformity of dispersion are not within the scope defined by this work. Accordingly, Example 4 has the flexural strength (911MPa), the number of abnormal discharges (11 times) and the number of particles dropped (20). The results were far better than those of Comparative Example 3 (812MPa, 106 times and 895 pieces, respectively). It can be seen that, in addition to the content of boron nitride that needs to be controlled within a specific range, the average size and dispersion uniformity of the black phase also need to be controlled within the specific range defined in this work, in order to effectively improve the flexural strength of the target at the same time, Reduce abnormal discharge and particle fall.

此外,再由實施例8至13的結果可知,於鐵鉑基靶材中另添加第一成分,並在氮化硼含量範圍、氮化硼與第一成分含量總和、黑色相平均尺寸以及黑色相分散均勻度皆於本創作所界定的特定範圍中時,亦可同時具有提升靶材的抗折強度、降低異常放電發生以及減少微粒掉落之功效。進一步參看實施例8、12以及比較例5、6的組別,雖然實施例8與比較例6的組成相同、實施例12與比較例5的組成相同,不過比較例5、6的黑色相平均尺寸以及分散均勻度均不在於本創作所界定之特定範圍中,因此仍存有嚴重的異常放電以及微粒掉落等問題。 In addition, from the results of Examples 8 to 13, it can be seen that the first component is added to the iron-platinum-based target, and the range of the content of boron nitride, the sum of the content of boron nitride and the first component, the average size of the black phase and the black When the phase dispersion uniformity is within the specific range defined in this work, it can also improve the flexural strength of the target material, reduce the occurrence of abnormal discharge and reduce the drop of particles. Further referring to the groups of Examples 8, 12 and Comparative Examples 5 and 6, although the composition of Example 8 and Comparative Example 6 is the same, and the composition of Example 12 and Comparative Example 5 is the same, the black phase of Comparative Examples 5 and 6 is average. The size and dispersion uniformity are not within the specific range defined by this creation, so there are still serious problems such as abnormal discharge and particle falling.

再參看實施例14至25的組別,該等組別另添加有第二成分,而相較於實施例1至13所列出的緻密程度結果,實施例14至25所具有的緻密程度有明顯的提升,其皆高於98%且最高可達99.97%,由此可知,於鐵鉑基靶材中另添加第二成分確實有助於進一步提升鐵鉑基靶材的緻密程度。然而,雖然比較例11至18分別依序與實施例14、15、16、17、18、20、22以及25的組成相同,但比較例11至18的黑色相平均尺寸以及分散均勻度都不在於本創作所界定之特定範圍中,故依然有嚴重的異常放電以及微粒掉落等問題。此外,再進一步參看比較例19以及20的組別,該等組別除了黑色相平均尺寸以及分散均勻度都不在於本創作所界定之特定範圍中之外,其所含有第二成分的含量也不在本創作進一步界定之2at%至40at%的特定範圍中,因此不僅具有較高的異常放電 次數(109次以及117次)與微粒掉落數量(1236顆以及1344顆),鐵鉑基靶材的緻密程度(96.13%以及95.20%)也明顯較差。 Referring again to the groups of Examples 14 to 25, which additionally have a second component added, and compared to the results of the densification levels listed in Examples 1 to 13, Examples 14 to 25 have densification levels that are The obvious improvement is higher than 98% and up to 99.97%. It can be seen that adding the second component to the iron-platinum-based target does help to further improve the density of the iron-platinum-based target. However, although Comparative Examples 11 to 18 have the same composition as Examples 14, 15, 16, 17, 18, 20, 22, and 25, respectively, the average size of the black phase and the dispersion uniformity of Comparative Examples 11 to 18 are not In the specific scope defined by this creation, there are still serious problems such as abnormal discharge and particle falling. In addition, further referring to the groups of Comparative Examples 19 and 20, except that the average size of the black phase and the uniformity of dispersion are not within the specific range defined in this creation, the content of the second component contained in these groups is also It is not in the specific range of 2at% to 40at% further defined in this creation, so it not only has a higher abnormal discharge The number of times (109 and 117) and the number of particles dropped (1236 and 1344), the density of the iron-platinum-based targets (96.13% and 95.20%) is also significantly poorer.

綜上所述,本創作藉由適當控制鐵鉑基靶材之氮化硼含量,以及控制其金相中黑色相的平均尺寸與分散均勻度,進而可同時達成提升鐵鉑基靶材的抗折強度、降低鐵鉑基靶材在濺鍍過程中發生異常放電之發生機率以及減輕微粒掉落於膜層上的問題,進而提升濺鍍形成的磁記錄層之膜層品質與良率。 To sum up, in this work, by properly controlling the boron nitride content of the iron-platinum-based target, and controlling the average size and dispersion uniformity of the black phase in the metallographic phase, the flexural strength of the iron-platinum-based target can be improved at the same time. , Reduce the probability of abnormal discharge of iron-platinum-based targets during the sputtering process and reduce the problem of particles falling on the film, thereby improving the film quality and yield of the magnetic recording layer formed by sputtering.

上述實施例僅係為說明本創作之例示,並非於任何方面限制本創作所主張之權利範圍。本創作所主張之權利範圍自應以申請專利範圍所述為準,而非僅限於上述具體實施例。 The above-mentioned embodiments are only examples to illustrate the present creation, and are not intended to limit the scope of the rights claimed by the present creation in any respect. The scope of rights claimed in this creation should be subject to the scope of the patent application, rather than being limited to the above-mentioned specific embodiments.

Claims (20)

一種鐵鉑基靶材,其包含鐵、鉑以及氮化硼;其中,以該鐵鉑基靶材整體之原子總數為基準,氮化硼的含量係大於0原子百分比且小於或等於50原子百分比;該鐵鉑基靶材的金相包含複數黑色相,該等黑色相的平均尺寸小於3微米,且該等黑色相於金相中的分散均勻度小於5×10-4,其中該分散均勻度係透過以下算式計算而得:(金相中的黑色相之總面積/金相之整體面積)/金相中的黑色相之總個數。 An iron-platinum-based target, comprising iron, platinum and boron nitride; wherein, based on the total number of atoms of the iron-platinum-based target as a whole, the content of boron nitride is greater than 0 atomic percent and less than or equal to 50 atomic percent ; The metallographic phase of the iron-platinum-based target material includes a plurality of black phases, the average size of these black phases is less than 3 microns, and the dispersion uniformity of these black phases in the metallographic phase is less than 5 × 10 -4 , wherein the dispersion uniformity is It is calculated by the following formula: (total area of black phase in metallographic phase/overall area of metallographic phase)/total number of black phase in metallographic phase. 如請求項1所述之鐵鉑基靶材,其中,以該鐵鉑基靶材整體之原子總數為基準,氮化硼的含量係大於或等於3原子百分比且小於或等於30原子百分比。 The iron-platinum-based target according to claim 1, wherein, based on the total number of atoms of the whole iron-platinum-based target, the content of boron nitride is greater than or equal to 3 atomic percent and less than or equal to 30 atomic percent. 如請求項1所述之鐵鉑基靶材,其中,以該鐵鉑基靶材整體之原子總數為基準,氮化硼的含量係大於或等於5原子百分比且小於或等於25原子百分比。 The iron-platinum-based target according to claim 1, wherein, based on the total number of atoms of the whole iron-platinum-based target, the content of boron nitride is greater than or equal to 5 atomic percent and less than or equal to 25 atomic percent. 如請求項1所述之鐵鉑基靶材,其中,以該鐵鉑基靶材整體之原子總數為基準,鉑的含量係大於或等於10原子百分比且小於或等於45原子百分比。 The iron-platinum-based target according to claim 1, wherein, based on the total atomic number of the iron-platinum-based target as a whole, the content of platinum is greater than or equal to 10 atomic percent and less than or equal to 45 atomic percent. 如請求項1所述之鐵鉑基靶材,其中,該鐵鉑基靶材更包含第一成分,該第一成分係選自由氧化物、碳化物、氮化物及其組合所組成之群組;其中,以該鐵鉑基靶材整體之原子總數為基準,該第一成分的含量係大於0原子百分比且小於或等於50原子百分比,且該第一成分與氮化硼的含量總和係大於或等於6原子百分比且小於或等於50原子百分比。 The iron-platinum-based target material as claimed in claim 1, wherein the iron-platinum-based target material further comprises a first component, and the first component is selected from the group consisting of oxides, carbides, nitrides and combinations thereof ; Wherein, based on the total number of atoms of the iron-platinum-based target as a whole, the content of the first component is greater than 0 atomic percent and less than or equal to 50 atomic percent, and the total content of the first component and boron nitride is greater than or equal to 6 atomic percent and less than or equal to 50 atomic percent. 如請求項1所述之鐵鉑基靶材,其中,該鐵鉑基靶材更包含碳,以該鐵鉑基靶材整體之原子總數為基準,碳的含量係大於或等於2原子百分比且小於或等於40原子百分比。 The iron-platinum-based target material according to claim 1, wherein the iron-platinum-based target material further comprises carbon, and based on the total number of atoms of the whole iron-platinum-based target material, the carbon content is greater than or equal to 2 atomic percent and Less than or equal to 40 atomic percent. 如請求項5所述之鐵鉑基靶材,其中,該氧化物包含二氧化矽、二氧化鈦、三氧化二鉻、五氧化二鉭、氧化鈷、三氧化二錳、三氧化二硼、二氧化鉿、氧化鎂、三氧化二鋁、二氧化鋯、五氧化二鈮、五氧化二釩、三氧化鎢、三氧化二鐵、氧化鋅或其組合。 The iron-platinum-based target according to claim 5, wherein the oxide comprises silicon dioxide, titanium dioxide, chromium oxide, tantalum pentoxide, cobalt oxide, manganese oxide, boron oxide, and oxide Hafnium, magnesium oxide, aluminum oxide, zirconium dioxide, niobium pentoxide, vanadium pentoxide, tungsten trioxide, iron oxide, zinc oxide, or combinations thereof. 如請求項5所述之鐵鉑基靶材,其中,該氮化物包含氮化鋁、氮化鈦、氮化鉻、氮化鋯、氮化鉭、氮化鉿、氮化矽、氮化碳鈦、氮化鎢或其組合。 The iron-platinum-based target according to claim 5, wherein the nitride comprises aluminum nitride, titanium nitride, chromium nitride, zirconium nitride, tantalum nitride, hafnium nitride, silicon nitride, and carbon nitride Titanium, tungsten nitride, or a combination thereof. 如請求項5所述之鐵鉑基靶材,其中,該碳化物包含碳化矽、碳化硼、碳化鈦、碳化鎢、碳化鉭、碳化鉿、碳化鋯、碳化釩、碳化鈮、碳化鉻或其組合。 The iron-platinum-based target material according to claim 5, wherein the carbide comprises silicon carbide, boron carbide, titanium carbide, tungsten carbide, tantalum carbide, hafnium carbide, zirconium carbide, vanadium carbide, niobium carbide, chromium carbide or the like combination. 如請求項1所述之鐵鉑基靶材,其中,該鐵鉑基靶材更包含第二成分,該第二成分係選自由銀、金、鍺、銅、鎳、鈷、鋁、鎂、錳、矽、鍶及其組合所組成之群組;其中,以該鐵鉑基靶材整體之原子總數為基準,該第二成分的含量係大於或等於2原子百分比且小於或等於40原子百分比。 The iron-platinum-based target material according to claim 1, wherein the iron-platinum-based target material further comprises a second component selected from the group consisting of silver, gold, germanium, copper, nickel, cobalt, aluminum, magnesium, The group consisting of manganese, silicon, strontium and their combinations; wherein, based on the total number of atoms of the iron-platinum-based target as a whole, the content of the second component is greater than or equal to 2 atomic percent and less than or equal to 40 atomic percent . 如請求項10所述之鐵鉑基靶材,其中,該鐵鉑基靶材更包含碳,以該鐵鉑基靶材整體之原子總數為基準,碳的含量係大於或等於2原子百分比且小於或等於10原子百分比。 The iron-platinum-based target material as claimed in claim 10, wherein the iron-platinum-based target material further comprises carbon, and based on the total number of atoms of the whole iron-platinum-based target material, the carbon content is greater than or equal to 2 atomic percent and Less than or equal to 10 atomic percent. 如請求項5所述之鐵鉑基靶材,其中,該鐵鉑基靶材更包含第二成分,該第二成分係選自由銀、金、鍺、銅、鎳、鈷、鋁、鎂、錳、矽、鍶及其組合所組成之群組;其中,以該鐵鉑基靶材整體之原子總數為基準,該第二成分的含量係大於或等於2原子百分比且小於或等於40原子百分比。 The iron-platinum-based target material according to claim 5, wherein the iron-platinum-based target material further comprises a second component selected from the group consisting of silver, gold, germanium, copper, nickel, cobalt, aluminum, magnesium, The group consisting of manganese, silicon, strontium and their combinations; wherein, based on the total number of atoms of the iron-platinum-based target as a whole, the content of the second component is greater than or equal to 2 atomic percent and less than or equal to 40 atomic percent . 如請求項12所述之鐵鉑基靶材,其中,該鐵鉑基靶材更包含碳,以該鐵鉑基靶材整體之原子總數為基準,碳的含量係大於或等於2原子百分比且小於或等於10原子百分比。 The iron-platinum-based target material according to claim 12, wherein the iron-platinum-based target material further comprises carbon, and based on the total number of atoms of the whole iron-platinum-based target material, the carbon content is greater than or equal to 2 atomic percent and Less than or equal to 10 atomic percent. 如請求項1至13中任一項所述之鐵鉑基靶材,其中,該鐵鉑基靶材的抗折強度係大於或等於700百萬帕。 The iron-platinum-based target according to any one of claims 1 to 13, wherein the flexural strength of the iron-platinum-based target is greater than or equal to 700 megapascals. 一種鐵鉑基靶材之製法,其包含以下步驟:步驟(a):混合鐵原料、鉑原料以及氮化硼原料,以得到一原料混合物,其中,該氮化硼原料的平均粒徑係小於5微米;步驟(b):將該原料混合物進行研磨4小時至12小時,隨後以800目數至1200目數的篩網過篩,接著取篩上物並重複前述研磨與過篩的步驟,以獲得一鐵鉑基混合原料;以及步驟(c):燒結該鐵鉑基混合原料,以獲得該鐵鉑基靶材;其中,以該鐵鉑基混合原料整體之原子總數為基準,氮化硼原料的添加量係大於0原子百分比且小於或等於50原子百分比;該鐵鉑基靶材的金相包含複數黑色相,該等黑色相的平均尺寸小於3微米,且該等黑色相的分散均勻度小於5×10-4,其中該分散均勻度係透過以下算式計算而得:(金相中的黑色相之總面積/金相之整體面積)/金相中的黑色相之總個數。 A method for producing an iron-platinum-based target, comprising the following steps: step (a): mixing iron raw materials, platinum raw materials and boron nitride raw materials to obtain a raw material mixture, wherein the average particle size of the boron nitride raw materials is less than 5 microns; step (b): grinding the raw material mixture for 4 hours to 12 hours, then sieving with a sieve of 800 to 1200 meshes, then taking the sieve and repeating the above-mentioned grinding and sieving steps, to obtain an iron-platinum-based mixed raw material; and step (c): sintering the iron-platinum-based mixed raw material to obtain the iron-platinum-based target; wherein, based on the total number of atoms of the whole iron-platinum-based mixed raw material, nitriding The addition amount of boron raw material is greater than 0 atomic percent and less than or equal to 50 atomic percent; the metallographic phase of the iron-platinum-based target contains a plurality of black phases, the average size of these black phases is less than 3 microns, and the dispersion of these black phases The uniformity is less than 5×10 -4 , wherein the dispersion uniformity is calculated by the following formula: (total area of black phases in the metallographic phase/overall area of the metallographic phase)/total number of black phases in the metallographic phase. 如請求項15所述之製法,其中,以該鐵鉑基混合原料整體之原子總數為基準,鉑原料的添加量係大於或等於10原子百分比且小於或等於45原子百分比。 The production method according to claim 15, wherein, based on the total number of atoms of the entire iron-platinum-based mixed raw material, the amount of platinum raw material added is greater than or equal to 10 atomic percent and less than or equal to 45 atomic percent. 如請求項15所述之製法,其中,該鐵鉑基混合原料更包含第一成分,該第一成分係選自由氧化物原料、碳化物原料、氮化物原料及其組合所組成之群組;其中,以該鐵鉑基混合原料整體之原子總數為基準,該第一成分的添加量係大於0原子百分比且小於或等於50原子百分比,且該第一成分與氮化硼原料的添加量總和係大於或等於6原子百分比且小於或等於50原子百分比。 The production method of claim 15, wherein the iron-platinum-based mixed raw material further comprises a first component, and the first component is selected from the group consisting of oxide raw materials, carbide raw materials, nitride raw materials and combinations thereof; Wherein, based on the total number of atoms of the whole iron-platinum-based mixed raw material, the addition amount of the first component is greater than 0 atomic percent and less than or equal to 50 atomic percent, and the sum of the addition amount of the first component and the boron nitride raw material is greater than or equal to 6 atomic percent and less than or equal to 50 atomic percent. 如請求項15所述之製法,其中,該鐵鉑基混合原料更包含碳原料;其中,以該鐵鉑基混合原料整體之原子總數為基準,該碳原料的添加量係大於或等於2原子百分比且小於或等於40原子百分比。 The production method according to claim 15, wherein the iron-platinum-based mixed raw material further comprises carbon raw material; wherein, based on the total number of atoms of the iron-platinum-based mixed raw material as a whole, the addition amount of the carbon raw material is greater than or equal to 2 atoms percent and less than or equal to 40 atomic percent. 如請求項15所述之製法,其中,該鐵鉑基混合原料更包含第二成分,該第二成分係選自由銀原料、金原料、鍺原料、銅原料、鎳原料、鈷原料、鋁原料、鎂原料、錳原料、矽原料、鍶原料及其組合所組成之群組;其中,以該鐵鉑基混合原料整體之原子總數為基準,該第二成分的添加量係大於或等於2原子百分比且小於或等於40原子百分比。 The method of claim 15, wherein the iron-platinum-based mixed raw material further comprises a second component, and the second component is selected from the group consisting of silver raw materials, gold raw materials, germanium raw materials, copper raw materials, nickel raw materials, cobalt raw materials, and aluminum raw materials , a group consisting of magnesium raw materials, manganese raw materials, silicon raw materials, strontium raw materials and their combinations; wherein, based on the total number of atoms of the iron-platinum-based mixed raw materials as a whole, the addition amount of the second component is greater than or equal to 2 atoms percent and less than or equal to 40 atomic percent. 如請求項15所述之製法,其中,在該步驟(c)中,燒結溫度為600℃至1200℃,燒結壓力為350巴至1800巴。 The production method according to claim 15, wherein, in the step (c), the sintering temperature is 600°C to 1200°C, and the sintering pressure is 350 bar to 1800 bar.
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