TW201343945A - Fe-Co-Ta-Zr-based alloy sputtering target and method for producing the same - Google Patents
Fe-Co-Ta-Zr-based alloy sputtering target and method for producing the same Download PDFInfo
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本發明係關於一種鐵鈷鉭鋯基合金濺鍍靶材及其製作方法，尤指一種用以形成磁記錄媒體之軟磁層的鐵鈷鉭鋯基合金濺鍍靶材及其製作方法。The invention relates to an iron cobalt cerium-zirconium-based alloy sputtering target material and a preparation method thereof, in particular to an iron cobalt cerium-zirconium-based alloy sputtering target material for forming a soft magnetic layer of a magnetic recording medium and a manufacturing method thereof.
隨著科技日益進步，系統自動儲存資料與大量備份重要檔案的使用需求，使得人們對於磁記錄媒體(magnetic recording media)的依賴越來越高。傳統上，硬碟是以水平式磁記錄媒體為主，然而水平式磁記錄媒體在提升磁記錄密度之技術已面臨物理上的極限，因此轉而發展出另一種垂直式磁記錄媒體的疊層結構。With the advancement of technology, the system automatically stores data and the need to back up important files, making people rely more and more on magnetic recording media. Traditionally, hard disks have been dominated by horizontal magnetic recording media. However, horizontal magnetic recording media have faced physical limitations in the technique of increasing magnetic recording density, and thus a stack of another vertical magnetic recording medium has been developed. structure.
垂直式磁記錄媒體之結構包含基板、附著層、軟磁層(soft magnetic layer)、晶種層、中間層、記錄層、覆蓋層以及潤滑層。其中，軟磁層的引入可以提升寫入的效率、降低去磁場的強度並且提升記錄層的熱穩定性。為了得到優良的軟磁特性，一般係採用矯頑磁力低於20 Oe的非晶態軟磁合金作為軟磁層的材料。常見的非晶態軟磁合金，例如：鐵鈷硼基合金(Fe-Co-B based alloy)、鈷鋯鈮基合金(Co-Zr-Nb based alloy)或鈷鐵鋯基合金(Co-Fe-Zr-based alloy)等，其中又以鈷鐵鉭鋯基合金(Co-Fe-Ta-Zr-based alloy)特別受到重視。The structure of the vertical magnetic recording medium includes a substrate, an adhesion layer, a soft magnetic layer, a seed layer, an intermediate layer, a recording layer, a cover layer, and a lubricating layer. Among them, the introduction of the soft magnetic layer can improve the efficiency of writing, reduce the strength of the demagnetizing field, and improve the thermal stability of the recording layer. In order to obtain excellent soft magnetic properties, an amorphous soft magnetic alloy having a coercive force of less than 20 Oe is generally used as a material of the soft magnetic layer. Common amorphous soft magnetic alloys, such as: Fe-Co-B based alloy, Co-Zr-Nb based alloy or cobalt-iron-zirconium-based alloy (Co-Fe- Zr-based alloys, etc., among which Co-Fe-Ta-Zr-based alloys are particularly valued.
磁控濺鍍技術(magnetron sputtering technique)係藉由磁場使電子以螺旋的方式前進，其能增加電子與氣體分子碰撞的機會，提高分子的電離度，進而使濺鍍靶材的濺鍍效率提高，成為目前用以沉積高性能磁性薄膜的主要方法。由於磁控濺鍍技術可於較低的氣壓下進行，因而能夠確保磁性薄膜的濺鍍品質；又，由於磁場會使電子偏離基板，使基板能夠處於較低的溫度，因而能夠有利於將磁性薄膜濺鍍在較不耐高溫的基板上，進而提升磁控濺鍍技術的應用價值。The magnetron sputtering technique advances electrons in a spiral manner by a magnetic field, which increases the chance of electrons colliding with gas molecules, increases the ionization degree of the molecules, and improves the sputtering efficiency of the sputtering target. It has become the main method currently used to deposit high-performance magnetic films. Since the magnetron sputtering technology can be performed at a lower pressure, the sputtering quality of the magnetic film can be ensured; and since the magnetic field causes the electrons to deviate from the substrate, the substrate can be at a lower temperature, thereby facilitating the magnetic properties. The film is sputtered on a substrate that is less resistant to high temperatures, thereby increasing the application value of magnetron sputtering technology.
然而，由於包含非晶態軟磁合金成份的濺鍍靶材於外加磁場下會產生磁遮罩效應(magnetic shielding effect)，阻擋設置於濺鍍靶材下方的磁鐵的磁力線穿透，而不利於進行正常的濺鍍製程；又，聚集的磁力線會侵蝕濺鍍靶材的表面並且形成凹槽，反而會降低濺鍍靶材的利用率。所述之效應係受到靶材的磁通量所影響，因此，提高靶材的磁通量是其中一種解決上述問題的方法。However, since the sputtering target containing the amorphous soft magnetic alloy component generates a magnetic shielding effect under an applied magnetic field, the magnetic flux of the magnet disposed under the sputtering target is blocked, which is unfavorable. The normal sputtering process; in turn, the concentrated magnetic lines of force will erode the surface of the sputter target and form a groove, which in turn will reduce the utilization of the sputter target. The effect is affected by the magnetic flux of the target, and therefore, increasing the magnetic flux of the target is one of the solutions to the above problems.
磁通量(Pass Through Flux,PTF)定義為被傳輸磁場與外加磁場的比率，其測量的方式可參考ASTM Standard F 1761“圓形磁性濺鍍靶磁通量的標準試驗方法”，100%的PTF是非磁性材料的指標，而在磁性材料中PTF和最大導磁率存在反比的關聯性。Pass Through Flux (PTF) is defined as the ratio of the transmitted magnetic field to the applied magnetic field. For the measurement method, refer to ASTM Standard F 1761 “Standard Test Method for Magnetic Flux of Circular Magnetic Sputter Target”. 100% PTF is a non-magnetic material. The index, while in magnetic materials, there is an inverse correlation between PTF and maximum permeability.
現有技術用以製作軟磁性濺鍍靶材的方法包括粉末冶金法或熔煉鑄造法。其中，使用粉末冶金法製作軟磁性濺鍍靶材具有製程複雜度高與成份均勻性不易控制等缺點；而使用熔煉鑄造法雖然沒有前述問題，又對靶材的尺寸和形狀較無限制，但對於製作某些特定成份比例的鐵鈷鉭鋯基合金濺鍍靶材(Co-Fe-Ta-Zr-based alloy sputtering target)而言，例如：Fe-30Co-8Ta-5Zr濺鍍靶材，使用熔煉鑄造法卻無法製作出高磁通量的鐵鈷鉭鋯基合金濺鍍靶材，反而影響鐵鈷鉭鋯基合金濺鍍靶材進行磁控濺鍍製程的利用率與濺鍍效能。Prior art methods for making soft magnetic sputtering targets include powder metallurgy or smelting casting. Among them, the use of powder metallurgy method to produce soft magnetic sputtering target has the disadvantages of high process complexity and unsuitable control of composition uniformity; while the use of smelting casting method has no problem, but the size and shape of the target are not limited, but For the production of Co-Fe-Ta-Zr-based alloy sputtering target, for example, Fe-30Co-8Ta-5Zr sputtering target, use The smelting and casting method can not produce high-flux iron-cobalt-zirconium-based alloy sputtering targets, but it affects the utilization rate and sputtering efficiency of the iron-cobalt-zirconium-based alloy sputtering target for magnetron sputtering process.
日本公開案第JP2010-059540A號揭示一種利用粉末冶金法製作鐵鈷基合金濺鍍靶材的方法，其係將以鈷為主體的合金相粉末與以鐵為主體的合金相粉末混合，經過燒結後製得鐵鈷基合金濺鍍靶材。然而，混合兩種預合金粉末製作鐵鈷基合金濺鍍靶材容易因為兩種預合金粉末間比重或流動性等差異而導致粉末無法均勻的混合，使得鐵鈷基合金濺鍍靶材具有製程複雜度高且成份不均勻等缺點。Japanese Laid-Open Publication No. JP2010-059540A discloses a method for producing an iron-cobalt-based alloy sputtering target by powder metallurgy, which is a method in which a cobalt-based alloy phase powder is mixed with an iron-based alloy phase powder and sintered. After the iron-cobalt-based alloy sputtering target is produced. However, mixing the two pre-alloyed powders to make the iron-cobalt-based alloy sputtering target is easy to uniformly mix the powder due to the difference in specific gravity or fluidity between the two pre-alloyed powders, so that the iron-cobalt-based alloy sputtering target has a manufacturing process. Shortcomings such as high complexity and uneven composition.
有鑑於現有技術中使用粉末冶金法製作鐵鈷鉭鋯基合金濺鍍靶材具有製程複雜度高與成份均勻性不易控制等缺點，使用熔煉鑄造法又無法獲得所需之磁通量等問題；本發明之主要目的在於提供一種製程簡單的製作方法，其能製備出成份均勻且具備高磁通量特性的軟磁層用之鐵鈷鉭鋯基合金濺鍍靶材。In view of the disadvantages of using the powder metallurgy method for the preparation of the iron-cobalt-zirconium-based alloy sputtering target in the prior art, the process complexity is high and the composition uniformity is difficult to control, and the magnetic flux and the like are not obtained by the smelting casting method; The main purpose of the invention is to provide a simple manufacturing process for preparing an iron-cobalt-zirconium-zirconium-based alloy sputtering target for a soft magnetic layer having uniform composition and high magnetic flux characteristics.
為達成上述目的，本發明係提供一種鐵鈷鉭鋯基合金濺鍍靶材(Fe-Co-Ta-Zr-based alloy sputtering target)之製作方法，其包含下列步驟：(A)將一含有鐵、鈷、鉭及鋯之原料以熔煉鑄造法形成一單一預合金；(B)以氣體霧化法處理該單一預合金，令其形成一含有鐵鈷鉭鋯之單一預合金粉末；(C)預成型該含有鐵鈷鉭鋯之單一預合金粉末，以形成一初胚；以及(D)以800℃至950℃以下之溫度固化成型該初胚，以製得該鐵鈷鉭鋯基合金濺鍍靶材。In order to achieve the above object, the present invention provides a method for producing a Fe-Co-Ta-Zr-based alloy sputtering target, which comprises the following steps: (A) containing iron The raw materials of cobalt, lanthanum and zirconium are formed into a single prealloy by smelting casting method; (B) the single prealloy is treated by gas atomization to form a single prealloyed powder containing iron cobalt cerium zirconium; (C) Pre-forming the single prealloyed powder containing iron cobalt cerium zirconium to form an initial embryo; and (D) solidifying the blasting preform at a temperature of 800 ° C to 950 ° C or lower to obtain the iron cobalt cerium zirconium based alloy splash Plating target.
於本發明所述之製作方法中，含有鐵、鈷、鉭及鋯之原料可由鐵金屬、鈷金屬、鉭金屬及鋯金屬所組成；或者，該含有鐵、鈷、鉭及鋯之原料可選自於述任意兩種以上金屬之合金之組合所組成，例如：鐵鈷合金與鉭鋯合金之組合、鐵鉭合金與鈷鋯合金之組合、鐵鋯合金與鈷鉭合金之組合等，但並非僅限於此。In the preparation method of the present invention, the raw material containing iron, cobalt, lanthanum and zirconium may be composed of iron metal, cobalt metal, base metal and zirconium metal; or the raw material containing iron, cobalt, lanthanum and zirconium may be selected. It is composed of a combination of alloys of any two or more metals, for example, a combination of an iron-cobalt alloy and a cerium-zirconium alloy, a combination of a strontium-iron alloy and a cobalt-zirconium alloy, a combination of an iron-zirconium alloy and a cobalt-rhodium alloy, but not Limited to this.
較佳的，前述各種含有鐵、鈷、鉭及鋯之原料皆可經由熔煉鑄造法形成一單一預合金，以供後續利用粉末冶金法製作鐵鈷鉭鋯基合金濺鍍靶材。Preferably, the foregoing various materials containing iron, cobalt, cerium and zirconium can form a single prealloy by smelting casting method for subsequent preparation of the iron cobalt cerium-zirconium-based alloy sputtering target by powder metallurgy.
較佳的，所述之鐵鈷鉭鋯基合金濺鍍靶材係由該含有鐵鈷鉭鋯之單一預合金粉末所組成，因而能夠使濺鍍靶材的成份較為均勻。Preferably, the iron-cobalt-zirconium-zirconium-based alloy sputtering target is composed of the single prealloyed powder containing iron, cobalt, and zirconium, thereby making the composition of the sputtering target relatively uniform.
較佳的，含有鐵鈷鉭鋯之單一預合金粉末之連續基底相係為鐵鈷合金相(Fe-Co alloy phase)。據此，於外加磁場下，具有軟磁特性的鐵、鈷成份較容易被翻轉至外加磁場方向，因而能夠使本發明鐵鈷鉭鋯基合金濺鍍靶材能夠具備較高的PTF值。Preferably, the continuous base phase of the single prealloyed powder containing iron cobalt cerium zirconium is an Fe-Co alloy phase. Accordingly, under the applied magnetic field, the iron and cobalt components having soft magnetic properties are easily reversed to the direction of the applied magnetic field, so that the iron-cobalt-zirconium-based alloy sputtering target of the present invention can have a high PTF value.
較佳的，所述之步驟(D)係包括以300 bar至650 bar之壓力下固化成型該初胚，更佳係於300 bar至650 bar之壓力下固化成型該初胚，以利於製作具備高磁通量特性的鐵鈷鉭鋯基合金濺鍍靶材。較佳的，所述之步驟(D)係包括以熱壓法、封罐法、熱等均壓法、或燒結法固化成型該初胚。Preferably, the step (D) comprises curing the preform by a pressure of 300 bar to 650 bar, more preferably curing the preform at a pressure of 300 bar to 650 bar, to facilitate the production. High-flux properties of iron-cobalt-niobium-zirconium-based alloy sputtering targets. Preferably, the step (D) comprises curing the preform by a hot pressing method, a sealing method, a heat equalizing method, or a sintering method.
此外，本發明亦提供一種鐵鈷鉭鋯基合金濺鍍靶材，其係由一含有鐵鈷鉭鋯之單一預合金粉末所組成，且該含有鐵鈷鉭鋯之單一預合金粉末之基底相係為鐵鈷合金相，其中鐵與鈷之含量係分別佔整體鐵鈷鉭鋯基合金濺鍍靶材之5原子百分比(atomic percentage,at%)以上，且鐵與鈷之含量和係佔整體鐵鈷鉭鋯基合金濺鍍靶材之75 at%至87 at%。In addition, the present invention also provides an iron cobalt-cerium-zirconium-based alloy sputtering target which is composed of a single prealloyed powder containing iron, cobalt, zirconium and zirconium, and the base phase of the single prealloyed powder containing iron, cobalt, zirconium and zirconium. It is an iron-cobalt alloy phase in which the content of iron and cobalt accounts for 5 atomic percent (at%) or more of the total iron-cobalt-zirconium-based alloy sputtering target, respectively, and the content of iron and cobalt and the total amount of cobalt 75 at% to 87 at% of the iron, cobalt, zirconium-based alloy sputtering target.
較佳的，所述之鐵鈷鉭鋯基合金濺鍍靶材可由前述之製作方法所製得。Preferably, the iron-cobalt-zirconium-zirconium-based alloy sputtering target can be obtained by the above-mentioned manufacturing method.
較佳的，於本發明之鐵鈷鉭鋯基濺鍍靶材中，鉭與鋯之含量和可佔整體鐵鈷鉭鋯基合金濺鍍靶材之13 at%至25 at%。Preferably, in the iron-cobalt-zirconium-based sputtering target of the present invention, the content of lanthanum and zirconium may be from 13 at% to 25 at% of the total iron-cobalt-zirconium-based alloy sputtering target.
較佳的，於本發明之鐵鈷鉭鋯基濺鍍靶材中，可進一步包括有至少一添加金屬，其中該至少一添加金屬係選於由下列所組成之群組：硼、鋁及鉻。Preferably, in the iron cobalt cerium-zirconium-based sputtering target of the present invention, at least one added metal may be further included, wherein the at least one added metal is selected from the group consisting of boron, aluminum and chromium. .
較佳的，於本發明之鐵鈷鉭鋯基濺鍍靶材中，鉭、鋯及至少一添加金屬之含量和可佔整體鐵鈷鉭鋯基合金濺鍍靶材之5 at%至20 at%。當本發明之鐵鈷鉭鋯基濺鍍靶材更包括前述之添加金屬時，其鉭與鋯之含量和較佳係佔整體鐵鈷鉭鋯基合金濺鍍靶材之8 at%以上，較佳係介於8 at%至20at%之間；且所述之至少一添加金屬之含量和係佔整體鐵鈷鉭鋯基合金濺鍍靶材之5 at%至17 at%之間。Preferably, in the iron-cobalt-zirconium-based sputtering target of the present invention, the content of cerium, zirconium and at least one added metal may be 5 at% to 20 at the total target of the iron-cobalt-zirconium-based alloy sputtering target. %. When the iron-cobalt-zirconium-zirconium-based sputtering target of the present invention further comprises the aforementioned additive metal, the content of lanthanum and zirconium is preferably more than 8 at% of the total iron-cobalt-zirconium-based alloy sputtering target. Preferably, the amount of the at least one added metal is between 5 at% and 17 at% of the total iron-cobalt-zirconium-based alloy sputtering target.
較佳的，本發明之鐵鈷鉭鋯基合金濺鍍靶材之厚度小於或等於12毫米(mm)時，且其具有大於或等於20%之磁通量，更佳係具有20%至25%之磁通量，再更佳係具有約30%至35%之磁通量。Preferably, the thickness of the iron cobalt cerium-zirconium-based alloy sputtering target of the present invention is less than or equal to 12 millimeters (mm), and it has a magnetic flux greater than or equal to 20%, more preferably 20% to 25%. More preferably, the magnetic flux has a magnetic flux of about 30% to 35%.
綜上所述，本發明將各個軟磁性成份控制於適當的範圍，並使用含有鐵鈷鉭鋯之單一預合金粉末作為製作軟磁層用之鐵鈷鉭鋯基合金濺鍍靶材的原料，藉此簡化鐵鈷鉭鋯基合金濺鍍靶材的製程複雜度，同時形成成份較為均勻的鐵鈷鉭鋯基合金濺鍍靶材。In summary, the present invention controls each soft magnetic component to an appropriate range, and uses a single prealloyed powder containing iron cobalt cerium zirconium as a raw material for the iron cobalt cerium zirconium based alloy sputtering target for soft magnetic layer. The simplification of the process complexity of the iron-cobalt-zirconium-zirconium alloy sputtering target and the formation of a relatively uniform composition of the iron-cobalt-zirconium-based alloy sputtering target.
此外，本發明利用粉末冶金法能夠製得一種由含有鐵鈷鉭鋯之單一預合金粉末組成的鐵鈷鉭鋯基合金濺鍍靶材，且含有鐵鈷鉭鋯之單一預合金粉末的基底相為鐵鈷合金相，其能使鐵鈷鉭鋯基合金濺鍍靶材具備高磁通量的特性，進而提升其濺鍍品質與利用率。In addition, the present invention utilizes a powder metallurgy method to produce an iron-cobalt-zirconium-based alloy sputtering target composed of a single prealloyed powder containing iron, cobalt, and zirconium, and a base phase of a single prealloyed powder containing iron, cobalt, and zirconium. It is an iron-cobalt alloy phase, which enables the iron-cobalt-zirconium-based alloy sputtering target to have high magnetic flux characteristics, thereby improving its sputtering quality and utilization.
以下，將藉由具體實施例說明本發明之實施方式，熟習此技藝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, the embodiments of the present invention will be described by way of specific examples, and those skilled in the art can readily understand the advantages and functions of the present invention, and can carry out various kinds without departing from the spirit of the present invention. Modifications and variations are made to implement or apply the subject matter of the invention.
實施例1Example 1
將18609公克的鈷金屬塊、15675公克的鐵金屬塊、12697公克的鉭金屬塊以及3200公克的鋯金屬塊進行熔煉鑄造，以形成鈷鐵鉭鋯之單一預合金。A 18609 gram cobalt metal block, a 15675 gram iron metal block, a 12697 gram base metal block, and a 3200 gram zirconium metal block were smelted to form a single prealloy of cobalt iron lanthanum zirconium.
接著，取約50公斤的單一預合金，利用氣霧化噴粉機台(gas atomization equipment)，以1650℃的霧化溫度下進行霧化噴粉，以形成含有鐵鈷鉭鋯之單一預合金粉末。於此，所形成之含有鐵鈷鉭鋯之單一預合金粉末的粒徑大約55至250微米(μm)。Next, about 50 kg of a single prealloy was taken, and atomized dusting was carried out at a atomization temperature of 1650 ° C using a gas atomization equipment to form a single prealloy containing iron, cobalt, zirconium and zirconium. powder. Here, the formed single prealloyed powder containing iron cobalt cerium zirconium has a particle diameter of about 55 to 250 micrometers (μm).
之後，取680公克之含有鈷鐵鉭鋯之單一預合金粉末，以滾動混粉機均勻混合約20分鐘後，將均勻混合的粉末均勻填充於石墨模具，並以壓力約為500磅/平方英寸的油壓機進行預成型步驟，以形成一初胚。Thereafter, 680 g of a single prealloyed powder containing cobalt, iron, zirconium and zirconium was uniformly mixed by a rolling mixer for about 20 minutes, and the uniformly mixed powder was uniformly filled in a graphite mold at a pressure of about 500 psi. The hydraulic press performs a preforming step to form an initial embryo.
然後，將初胚與石墨模具一同置入熱壓爐中進行燒結，以熱壓溫度約為850℃及壓力約為500 bar持續熱壓60分鐘後，製得直徑約96毫米(mm)且厚度約8 mm之鐵鈷鉭鋯基合金濺鍍靶材。於此，所形成之鐵鈷鉭鋯基合金濺鍍靶材係為45Co-40Fe-10Ta-5Zr濺鍍靶材。Then, the initial embryo and the graphite mold are placed in a hot press furnace for sintering, and the hot pressing temperature is about 850 ° C and the pressure is about 500 bar for 60 minutes, and the diameter is about 96 mm (mm) and the thickness is obtained. Approximately 8 mm of iron, cobalt, zirconium-based alloy sputtering target. Here, the formed iron cobalt cerium-zirconium-based alloy sputtering target is a 45Co-40Fe-10Ta-5Zr sputtering target.
以ASTM Standard F1761標準試驗方法測量濺鍍靶材的磁通量，證實利用本發明之製作方法確實可以使厚度約8 mm之鐵鈷鉭鋯基合金濺鍍靶材具有高達35%之磁通量。The magnetic flux of the sputter target was measured by the ASTM Standard F1761 standard test method, and it was confirmed that the iron-cobalt-zirconium-based alloy sputtering target having a thickness of about 8 mm can be made to have a magnetic flux of up to 35% by the manufacturing method of the present invention.
以掃描式電子顯微鏡(型號為Hitachi N-3400 SEM)觀察本發明鐵鈷鉭鋯基合金濺鍍靶材之金相微結構。如圖1及圖2所示，黑色相係為本發明鐵鈷鉭鋯基合金濺鍍靶材之連續基底相。The metallographic microstructure of the iron-cobalt-zirconium-based alloy sputtering target of the present invention was observed by a scanning electron microscope (model Hitachi N-3400 SEM). As shown in FIGS. 1 and 2, the black phase is a continuous base phase of the iron-cobalt-zirconium-based alloy sputtering target of the present invention.
以能量散射光譜儀(型號為HORIBA 7021-H EDS)分析鐵鈷鉭鋯基合金濺鍍靶材中各金相的元素成份，本發明鐵鈷鉭鋯基合金濺鍍靶材係由鐵鈷鉭鋯之單一預合金粉末所組成，且黑色相係為鐵鈷合金相，其結果係如下表1所示。The elemental composition of each metal phase in the iron-cobalt-zirconium-based alloy sputtering target was analyzed by an energy scattering spectrometer (model HORIBA 7021-H EDS). The iron-cobalt-zirconium-based alloy sputtering target of the present invention is composed of iron, cobalt, zirconium and zirconium. It consists of a single prealloyed powder, and the black phase is an iron-cobalt alloy phase. The results are shown in Table 1 below.
表1：實施例1中黑色相與白色相中各成份之含量。Table 1: The content of each component in the black phase and the white phase in Example 1.
綜合掃描式電子顯微鏡與能量散射光譜儀之分析結果證實，本實施例之鐵鈷鉭鋯基合金濺鍍靶材係由含有鐵鈷鉭鋯之單一預合金粉末所組成，且該含有鐵鈷鉭鋯之單一預合金粉末的基底相係為鐵鈷合金相。The analysis results of the integrated scanning electron microscope and the energy scattering spectrometer confirmed that the iron-cobalt-zirconium-based alloy sputtering target of the present embodiment is composed of a single prealloyed powder containing iron, cobalt, zirconium and zirconium, and the iron-cobalt-cerium-containing zirconium is contained. The base phase of the single prealloyed powder is an iron cobalt alloy phase.
實施例2Example 2
將18609公克的鈷金屬塊、15675公克的鐵金屬塊、12697公克的鉭金屬塊以及3200公克的鋯金屬塊進行熔煉鑄造，以形成鈷鐵鉭鋯之單一預合金。A 18609 gram cobalt metal block, a 15675 gram iron metal block, a 12697 gram base metal block, and a 3200 gram zirconium metal block were smelted to form a single prealloy of cobalt iron lanthanum zirconium.
接著，取約50公斤的單一預合金，利用氣霧化噴粉機台(gas atomization equipment)，以1650℃的霧化溫度下進行霧化噴粉，以形成含有鐵鈷鉭鋯之單一預合金粉末。於此，所形成之含有鐵鈷鉭鋯之單一預合金粉末的粒徑大約55至250微米。Next, about 50 kg of a single prealloy was taken, and atomized dusting was carried out at a atomization temperature of 1650 ° C using a gas atomization equipment to form a single prealloy containing iron, cobalt, zirconium and zirconium. powder. Here, the formed single prealloyed powder containing iron cobalt cerium zirconium has a particle diameter of about 55 to 250 μm.
之後，取680公克之含有鈷鐵鉭鋯之單一預合金粉末，以滾動混粉機均勻混合約20分鐘後，將均勻混合的粉末均勻填充於石墨模具，並以壓力約為500磅/平方英寸的油壓機進行預成型步驟，以形成一初胚。Thereafter, 680 g of a single prealloyed powder containing cobalt, iron, zirconium and zirconium was uniformly mixed by a rolling mixer for about 20 minutes, and the uniformly mixed powder was uniformly filled in a graphite mold at a pressure of about 500 psi. The hydraulic press performs a preforming step to form an initial embryo.
然後，將初胚與石墨模具一同置入熱壓爐中進行燒結，以熱壓溫度約為950℃及壓力約為500 bar持續熱壓60分鐘後，製得直徑約96 mm且厚度約8 mm之鐵鈷鉭鋯基合金濺鍍靶材。於此，所形成之鐵鈷鉭鋯基合金濺鍍靶材係為45Co-40Fe-10Ta-5Zr濺鍍靶材。Then, the blasting is placed in a hot press furnace together with a graphite mold for sintering, and after a hot pressing temperature of about 950 ° C and a pressure of about 500 bar for 60 minutes, a diameter of about 96 mm and a thickness of about 8 mm are obtained. The iron, cobalt, zirconium-based alloy sputtering target. Here, the formed iron cobalt cerium-zirconium-based alloy sputtering target is a 45Co-40Fe-10Ta-5Zr sputtering target.
以ASTM Standard F1761標準試驗方法測量濺鍍靶材的磁通量，證實利用本發明之製作方法確實可以使厚度約8 mm之鐵鈷鉭鋯基合金濺鍍靶材具有高達30%之磁通量。The magnetic flux of the sputter target was measured by the ASTM Standard F1761 standard test method, and it was confirmed that the iron-cobalt-zirconium-based alloy sputtering target having a thickness of about 8 mm can be made to have a magnetic flux of up to 30% by the manufacturing method of the present invention.
以掃描式電子顯微鏡(型號為Hitachi N-3400 SEM)觀察本發明鐵鈷鉭鋯基合金濺鍍靶材之金相微結構。如圖3及圖4所示，黑色相係為本發明鐵鈷鉭鋯基合金濺鍍靶材之連續基底相。The metallographic microstructure of the iron-cobalt-zirconium-based alloy sputtering target of the present invention was observed by a scanning electron microscope (model Hitachi N-3400 SEM). As shown in FIGS. 3 and 4, the black phase is a continuous base phase of the iron-cobalt-zirconium-based alloy sputtering target of the present invention.
以能量散射光譜儀(型號為HORIBA 7021-H EDS)分析鐵鈷鉭鋯基合金濺鍍靶材中各金相的元素成份，本發明鐵鈷鉭鋯基合金濺鍍靶材係由鐵鈷鉭鋯之單一預合金粉末所組成，且黑色相係為鐵鈷合金相，其結果係如下表2所示。The elemental composition of each metal phase in the iron-cobalt-zirconium-based alloy sputtering target was analyzed by an energy scattering spectrometer (model HORIBA 7021-H EDS). The iron-cobalt-zirconium-based alloy sputtering target of the present invention is composed of iron, cobalt, zirconium and zirconium. It consists of a single prealloyed powder, and the black phase is an iron-cobalt alloy phase. The results are shown in Table 2 below.
表2：實施例2中黑色相與白色相中各成份之含量。Table 2: The content of each component in the black phase and the white phase in Example 2.
綜合掃描式電子顯微鏡與能量散射光譜儀之分析結果證實，本實施例之鐵鈷鉭鋯基合金濺鍍靶材係由含有鐵鈷鉭鋯之單一預合金粉末所組成，且該含有鐵鈷鉭鋯之單一預合金粉末的基底相係為鐵鈷合金相。The analysis results of the integrated scanning electron microscope and the energy scattering spectrometer confirmed that the iron-cobalt-zirconium-based alloy sputtering target of the present embodiment is composed of a single prealloyed powder containing iron, cobalt, zirconium and zirconium, and the iron-cobalt-cerium-containing zirconium is contained. The base phase of the single prealloyed powder is an iron cobalt alloy phase.
比較例1Comparative example 1
將18609公克的鈷金屬塊、15675公克的鐵金屬塊、12697公克的鉭金屬塊以及3200公克的鋯金屬塊投入坩堝進行熔煉鑄造，以形成一鑄錠。A 18609 gram cobalt metal block, a 15675 gram iron metal block, a 12697 gram base metal block, and a 3200 gram zirconium metal block were placed in a crucible for casting to form an ingot.
之後，以熱等均壓法消除鑄錠內部的縮孔，再以線割/車床作業獲得直徑約96 mm且厚度約8 mm之鐵鈷鉭鋯基合金濺鍍靶材。於此，所形成之鐵鈷鉭鋯基合金濺鍍靶材係為45Co-40Fe-10Ta-5Zr濺鍍靶材。Thereafter, the shrinkage cavities inside the ingot were removed by a heat equalization method, and an iron-cobalt-zirconium-based alloy sputtering target having a diameter of about 96 mm and a thickness of about 8 mm was obtained by a wire cutting/turning operation. Here, the formed iron cobalt cerium-zirconium-based alloy sputtering target is a 45Co-40Fe-10Ta-5Zr sputtering target.
以ASTM Standard F1761標準試驗方法測量鐵鈷鉭鋯基合金濺鍍靶材的磁通量，其厚度約8 mm之鐵鈷鉭鋯基合金濺鍍靶材的磁通量僅為28%。The magnetic flux of the iron-cobalt-zirconium-based alloy sputtering target was measured by the ASTM Standard F1761 standard test method, and the magnetic flux of the iron-cobalt-zirconium-based alloy sputtering target having a thickness of about 8 mm was only 28%.
以掃描式電子顯微鏡觀察本比較例之鐵鈷鉭鋯基合金濺鍍靶材之金相微結構。如圖5所示，黑色相係為本比較例之鐵鈷鉭鋯基合金濺鍍靶材的連續基底相。The metallographic microstructure of the iron-cobalt-zirconium-based alloy sputtering target of this comparative example was observed by a scanning electron microscope. As shown in FIG. 5, the black phase is a continuous base phase of the iron-cobalt-zirconium-based alloy sputtering target of the comparative example.
以能量散射光譜儀分析濺鍍靶材中各金相的元素成份，本比較例之鐵鈷鉭鋯基合金濺鍍靶材中黑色相係為鐵鈷合金相，其結果係如下表3所示。The elemental composition of each metal phase in the sputtering target was analyzed by an energy scattering spectrometer. The black phase of the iron-cobalt-zirconium-based alloy sputtering target of this comparative example was an iron-cobalt alloy phase, and the results are shown in Table 3 below.
表3：比較例1中黑色相與白色相中各成份之含量。Table 3: Content of each component in the black phase and the white phase in Comparative Example 1.
如圖5所示，使用熔煉鑄造法所製得之鐵鈷鉭鋯基合金濺鍍靶材的黑色相分佈情形與使用粉末冶金法所製得之鐵鈷鉭鋯基合金濺鍍靶材的黑色相分佈情形並不相同(請參閱圖1至圖4)，其會影響鐵鈷鉭鋯基合金濺鍍靶材中磁性成份翻轉的能力，而降低鐵鈷鉭鋯基合金濺鍍靶材的磁通量。As shown in Fig. 5, the black phase distribution of the iron-cobalt-zirconium-based alloy sputtering target prepared by the smelting casting method and the black of the iron-cobalt-zirconium-based alloy sputtering target obtained by the powder metallurgy method are shown. The phase distribution is not the same (see Figure 1 to Figure 4), which affects the ability of the magnetic component to be reversed in the iron-cobalt-zirconium-based alloy sputtering target, and reduces the magnetic flux of the iron-cobalt-zirconium-based alloy sputtering target. .
因此，對相同厚度的鐵鈷鉭鋯基合金濺鍍靶材而言，使用熔煉鑄造法所製得的鐵鈷鉭鋯基合金濺鍍靶材的磁通量較低，並不利於提升濺鍍品質與濺鍍靶材之利用率。Therefore, for the same thickness of the iron-cobalt-zirconium-based alloy sputtering target, the iron-cobalt-zirconium-based alloy sputtering target obtained by the smelting casting method has a low magnetic flux, which is not favorable for improving the sputtering quality and the sputtering quality. Sputter target utilization.
比較例2Comparative example 2
將34467公克的鈷金屬塊、12464公克的鉭金屬塊以及3141公克的鋯金屬塊進行熔煉鑄造，以形成一Co-10Ta-5Zr之預合金。另外，取33850公克的鐵金屬塊、12903公克的鉭金屬塊及3252公克的鋯金屬塊進行熔煉鑄造，以形成Fe-10Ta-5Zr之預合金。A 34467 gram cobalt metal block, a 12464 gram base metal block, and a 3141 gram zirconium metal block were smelted and cast to form a Co-10Ta-5Zr prealloy. In addition, 33,850 grams of iron metal blocks, 12,903 grams of base metal blocks, and 3,252 grams of zirconium metal blocks were smelted and cast to form a pre-alloy of Fe-10Ta-5Zr.
之後，取5公斤的Co-10Ta-5Zr預合金及5公斤的Fe-10Ta-5Zr預合金，分別利用氣霧化噴粉機台，以1650℃的霧化溫度下進行霧化噴粉，形成鈷鉭鋯預合金粉末及鐵鉭鋯預合金粉末。於此，所形成之鈷鉭鋯預合金粉末的粒徑大約55至250微米，且所形成之鐵鉭鋯預合金粉末的粒徑大約55至250微米。After that, 5 kg of Co-10Ta-5Zr prealloy and 5 kg of Fe-10Ta-5Zr prealloy were taken, and the atomized powder was sprayed at an atomization temperature of 1650 ° C to form an atomized powder. Cobalt cerium zirconium prealloyed powder and iron cerium zirconium prealloyed powder. Here, the formed cobalt-cerium-zirconium prealloyed powder has a particle diameter of about 55 to 250 μm, and the formed iron-cerium-zirconium prealloyed powder has a particle diameter of about 55 to 250 μm.
之後，取366公克之鈷鉭鋯預合金粉末與314公克之鐵鉭鋯預合金粉末，以滾動混粉機混合約20分鐘後，將均勻混合的粉末均勻填充於石墨模具，並以壓力約為500磅/平方英寸的油壓機進行預成型步驟，以形成一初胚。Thereafter, 366 g of cobalt-cerium-zirconium prealloyed powder and 314 g of iron-cerium-zirconium prealloyed powder were mixed and mixed by a rolling mixer for about 20 minutes, and the uniformly mixed powder was uniformly filled in the graphite mold, and the pressure was about A 500 psi hydraulic press performs a preforming step to form an initial embryo.
然後，將初胚與石墨模具一同置入熱壓爐中進行燒結，以熱壓溫度約為1100℃及壓力約為500 bar持續熱壓90分鐘後，製得直徑約96 mm且厚度約8 mm之鐵鈷鉭鋯基合金濺鍍靶材。Then, the blasting is placed in a hot press furnace together with a graphite mold for sintering, and after a hot pressing temperature of about 1100 ° C and a pressure of about 500 bar for 90 minutes, a diameter of about 96 mm and a thickness of about 8 mm are obtained. The iron, cobalt, zirconium-based alloy sputtering target.
以ASTM Standard F1761標準試驗方法測量濺鍍靶材的磁通量，其厚度約8 mm之鐵鈷鉭鋯基合金濺鍍靶材的磁通量約為33%。The magnetic flux of the sputter target was measured by the ASTM Standard F1761 standard test method, and the magnetic flux of the iron-cobalt-zirconium-based alloy sputtering target having a thickness of about 8 mm was about 33%.
請參閱圖6及表4所示，以掃描式電子顯微鏡觀察並以能量散射光譜儀分析分析鐵鈷鉭鋯基合金濺鍍靶材，本發明鐵鈷鉭鋯基合金濺鍍靶材包含兩種分別以Co-10Ta-5Zr及Fe-10Ta-5Zr預合金粉末為主的金相。Referring to FIG. 6 and Table 4, the iron-cobalt-zirconium-based alloy sputtering target is observed by a scanning electron microscope and analyzed by an energy scattering spectrometer. The iron-cobalt-zirconium-based alloy sputtering target of the present invention comprises two kinds of respectively. The metallographic phase is mainly composed of Co-10Ta-5Zr and Fe-10Ta-5Zr prealloyed powder.
表4：比較例2中黑色相與白色相中各成份之含量。Table 4: Content of each component in the black phase and the white phase in Comparative Example 2.
如表4之EDS分析結果證實，兩種預合金粉末已相互擴散並且分別分佈於不同的金相中，導致濺鍍靶材中形成有許多內部孔洞，而使濺鍍靶材的密度下降。As shown in the EDS analysis of Table 4, the two prealloyed powders have been mutually diffused and distributed in different metal phases, resulting in the formation of many internal voids in the sputter target, which reduces the density of the sputter target.
比較例3Comparative example 3
將18609公克的鈷金屬塊、15675公克的鐵金屬塊、12697公克的鉭金屬塊以及3200公克的鋯金屬塊進行熔煉鑄造，以形成鈷鐵鉭鋯之單一預合金。A 18609 gram cobalt metal block, a 15675 gram iron metal block, a 12697 gram base metal block, and a 3200 gram zirconium metal block were smelted to form a single prealloy of cobalt iron lanthanum zirconium.
接著，取約50公斤的單一預合金，利用氣霧化噴粉機台，以1650℃的霧化溫度下進行霧化噴粉，以形成含有鐵鈷鉭鋯之單一預合金粉末。於此，所形成之含有鐵鈷鉭鋯之單一預合金粉末的粒徑大約55至250微米。Next, about 50 kg of a single prealloy was taken, and atomized dusting was carried out at an atomization temperature of 1650 ° C by means of a gas atomizing dusting machine to form a single prealloyed powder containing iron, cobalt, zirconium and zirconium. Here, the formed single prealloyed powder containing iron cobalt cerium zirconium has a particle diameter of about 55 to 250 μm.
之後，取680公克之含有鈷鐵鉭鋯之單一預合金粉末，以滾動混粉機均勻混合約20分鐘後，將均勻混合的粉末均勻填充於石墨模具，並以壓力約為500磅/平方英寸的油壓機進行預成型步驟，以形成一初胚。Thereafter, 680 g of a single prealloyed powder containing cobalt, iron, zirconium and zirconium was uniformly mixed by a rolling mixer for about 20 minutes, and the uniformly mixed powder was uniformly filled in a graphite mold at a pressure of about 500 psi. The hydraulic press performs a preforming step to form an initial embryo.
然後，將初胚與石墨模具一同置入熱壓爐中進行燒結，以熱壓溫度約為1100℃及壓力約為500 bar持續熱壓90分鐘後，製得直徑約96 mm且厚度約8 mm之鐵鈷鉭鋯基合金濺鍍靶材。於此，所形成之鐵鈷鉭鋯基合金濺鍍靶材係為40Fe-45Co-10Ta-5Zr濺鍍靶材。Then, the blasting is placed in a hot press furnace together with a graphite mold for sintering, and after a hot pressing temperature of about 1100 ° C and a pressure of about 500 bar for 90 minutes, a diameter of about 96 mm and a thickness of about 8 mm are obtained. The iron, cobalt, zirconium-based alloy sputtering target. Here, the formed iron cobalt cerium-zirconium-based alloy sputtering target is a 40Fe-45Co-10Ta-5Zr sputtering target.
以ASTM Standard F1761標準試驗方法測量濺鍍靶材的磁通量，所製成之厚度約8 mm的鐵鈷鉭鋯基合金濺鍍靶材僅具有15%之磁通量，並不利於進行濺鍍製程。The magnetic flux of the sputter target was measured by the ASTM Standard F1761 standard test method. The iron-cobalt-zirconium-based alloy sputter target having a thickness of about 8 mm has only 15% of the magnetic flux and is not favorable for the sputtering process.
以掃描式電子顯微鏡觀察本比較例之鐵鈷鉭鋯基合金濺鍍靶材的金相微結構。如圖7及圖8所示，白色相係為本比較例之鐵鈷鉭鋯基合金濺鍍靶材的連續基底相。The metallographic microstructure of the iron-cobalt-zirconium-based alloy sputtering target of this comparative example was observed by a scanning electron microscope. As shown in FIGS. 7 and 8, the white phase is a continuous base phase of the iron-cobalt-zirconium-based alloy sputtering target of the comparative example.
以能量散射光譜儀分析濺鍍靶材中各金相的元素成份，其結果係如下表5所示。圖中所示之白色連續相係為鐵鈷鉭鋯基底相，而非鐵鈷基底相，所述之鐵鈷鉭鋯基底相係導致鐵鈷鉭鋯基合金濺鍍靶材的磁通量下降的原因。The elemental composition of each metal phase in the sputtering target was analyzed by an energy scattering spectrometer, and the results are shown in Table 5 below. The white continuous phase shown in the figure is an iron cobalt cerium zirconium base phase instead of an iron-cobalt base phase, which causes the magnetic flux of the iron cobalt cerium-zirconium alloy sputtering target to decrease. .
表5：比較例3中黑色相與白色相中各成份之含量。Table 5: Content of each component in the black phase and the white phase in Comparative Example 3.
經由上述兩種實施例與比較例3之結果證實，固化成型的溫度較佳係介於800℃至950℃，以形成具備高磁通量特性的鐵鈷鉭鋯基合金濺鍍靶材。It was confirmed by the results of the above two examples and Comparative Example 3 that the temperature of the solidification molding was preferably from 800 ° C to 950 ° C to form an iron cobalt cerium-zirconium-based alloy sputtering target having high magnetic flux characteristics.
比較實施例1與比較例1至比較例3的實驗結果證實，本發明以含有鈷鐵鉭鋯之單一預合金粉末作為原料，可於800至950℃之燒結溫度下進行固化成型，藉以有效控制所形成的鐵鈷鉭鋯基合金濺鍍靶材之金相微結構，形成以連續的鐵鈷合金相為主的基底相。此外，相較於比較例1至比較例3所述之製作方法，本發明利用單一預合金粉末進行粉末冶金法，可簡化製作特定成份比例之鐵鈷鉭鋯基合金濺鍍靶材所需之步驟，成功製造出磁通率高達30%以上的軟磁層用之鐵鈷鉭鋯基合金濺鍍靶材。The experimental results of Comparative Example 1 and Comparative Example 1 to Comparative Example 3 confirmed that the present invention uses a single prealloyed powder containing cobalt iron cerium zirconium as a raw material, and can be solidified at a sintering temperature of 800 to 950 ° C, thereby effectively controlling The metal microstructure of the formed iron cobalt cerium-zirconium-based alloy sputtering target forms a base phase mainly composed of a continuous iron-cobalt alloy phase. In addition, compared with the production methods described in Comparative Example 1 to Comparative Example 3, the present invention utilizes a single prealloyed powder for powder metallurgy, which simplifies the preparation of a specific composition ratio of iron, cobalt, zirconium-based alloy sputtering target. In the step, an iron-cobalt-niobium-zirconium-based alloy sputtering target for a soft magnetic layer having a magnetic flux of more than 30% was successfully produced.
上述實施例僅係為了方便說明而舉例而已，本發明所主張之權利範圍自應以申請專利範圍所述為準，而非僅限於上述實施例。The above-mentioned embodiments are merely examples for convenience of description, and the scope of the claims is intended to be limited to the above embodiments.
圖1係為本發明實施例1之鐵鈷鉭鋯基合金濺鍍靶材的金相微結構影像圖。BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a view showing a metallographic microstructure of an iron-cobalt-zirconium-based alloy sputtering target according to Embodiment 1 of the present invention.
圖2係為本發明實施例1之鐵鈷鉭鋯基合金濺鍍靶材的金相微結構影像圖。2 is a view showing a metallographic microstructure of an iron-cobalt-zirconium-based alloy sputtering target according to Embodiment 1 of the present invention.
圖3係為本發明實施例2之鐵鈷鉭鋯基合金濺鍍靶材的金相微結構影像圖。3 is a metallographic microstructure image of an iron-cobalt-zirconium-based alloy sputtering target according to Embodiment 2 of the present invention.
圖4係為本發明實施例2之鐵鈷鉭鋯基合金濺鍍靶材的金相微結構影像圖。4 is a view showing a metallographic microstructure of an iron-cobalt-zirconium-based alloy sputtering target according to Embodiment 2 of the present invention.
圖5係為比較例1之鐵鈷鉭鋯基合金濺鍍靶材的金相微結構影像圖。Fig. 5 is a metallographic microstructure image of the iron-cobalt-zirconium-based alloy sputtering target of Comparative Example 1.
圖6係為比較例2之鐵鈷鉭鋯基合金濺鍍靶材的金相微結構影像圖。Fig. 6 is a metallographic microstructure image of the iron-cobalt-zirconium-based alloy sputtering target of Comparative Example 2.
圖7係為比較例3之鐵鈷鉭鋯基合金濺鍍靶材的金相微結構影像圖。Fig. 7 is a metallographic microstructure image of the iron-cobalt-zirconium-based alloy sputtering target of Comparative Example 3.
圖8係為比較例3之鐵鈷鉭鋯基合金濺鍍靶材的金相微結構影像圖。Fig. 8 is a metallographic microstructure image of the iron-cobalt-zirconium-based alloy sputtering target of Comparative Example 3.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111424245A (en) * | 2020-04-24 | 2020-07-17 | 先导薄膜材料（广东）有限公司 | Preparation method of cobalt-tantalum-zirconium target material |
| CN111957982A (en) * | 2020-08-31 | 2020-11-20 | 宁波江丰电子材料股份有限公司 | Preparation method of iron-cobalt-tantalum alloy powder, iron-cobalt-tantalum alloy powder and application |
| CN112059195A (en) * | 2020-08-31 | 2020-12-11 | 宁波江丰电子材料股份有限公司 | Preparation method of iron-tantalum alloy powder, iron-tantalum alloy powder and application |
| TWI716166B (en) * | 2019-10-28 | 2021-01-11 | 光洋應用材料科技股份有限公司 | Fe-co-based alloy target and method for producing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI716166B (en) * | 2019-10-28 | 2021-01-11 | 光洋應用材料科技股份有限公司 | Fe-co-based alloy target and method for producing the same |
| CN111424245A (en) * | 2020-04-24 | 2020-07-17 | 先导薄膜材料（广东）有限公司 | Preparation method of cobalt-tantalum-zirconium target material |
| CN111957982A (en) * | 2020-08-31 | 2020-11-20 | 宁波江丰电子材料股份有限公司 | Preparation method of iron-cobalt-tantalum alloy powder, iron-cobalt-tantalum alloy powder and application |
| CN112059195A (en) * | 2020-08-31 | 2020-12-11 | 宁波江丰电子材料股份有限公司 | Preparation method of iron-tantalum alloy powder, iron-tantalum alloy powder and application |
| CN112059195B (en) * | 2020-08-31 | 2023-08-15 | 宁波江丰电子材料股份有限公司 | Preparation method of ferrotantalum alloy powder, ferrotantalum alloy powder and application |
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