TW212242B - Method of manufacture magnetic recording media - Google Patents
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- TW212242B TW212242B TW82100981A TW82100981A TW212242B TW 212242 B TW212242 B TW 212242B TW 82100981 A TW82100981 A TW 82100981A TW 82100981 A TW82100981 A TW 82100981A TW 212242 B TW212242 B TW 212242B
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AG l\C 經濟部-1.準局貝工消份合作社印製 五、發明説明(1 ) 本案係一種磁性記錄媒體之製造方法,M使能形成一 高記錄密度的鈷/錳/撖氧化物的磁記錄薄膜。 目前硬碟普遍為採用水平記錄(Longitudinal' recording) 技術 的薄膜 磁碟片 (Thin film disk) , 磁記 錄媒體的磁化方向圼水平排列,磁頭在薄膜表面上滑行, 透過線圈感應磁矩或通過窜流產生磁場改變磁矩磁化方向 進行資料的讀寫,這種裝設方法稱之為播捷式硬碟櫬( Winchester disk drive) 的硬碟,是目前商品化硬碟的 主流。 目前文獻上所能找到的用於磁記錄薄膜應用研究的材 料,範圍涵蓋了水平式記錄、垂直記錄、以及磁光記錄三 大領域,而猫鍍金鼷膜在三種技術領域內均堪稱最大宗。 單就水平式磁記錄材料而言,一般之製造方法請參閲第一 圖,其中濺鍍金臑膜中的 CoCrH(M = Ni, Pt, Ta)是目前 最被廣泛使用的材料系統,雖其之抗磁力髙達約1500 Oe ,飽和磁化量(Saturation magnetization) Ms 亦高達 約 600 〜1200 emu / ca^ ,角形比(Squareness ratio) S 也有約 0.8 K上,厚度為約 5〇nm,讓其他的材料相形失 色,然金屬磁記錄薄膜仍有缺點,包括: 1)除了 CoPt合金系本身有夠強的膜面結晶異向性 外,均需借助 Cr當做底層來幫肋磁性層之結晶方向性成 長,藉Μ提升薄膜的磁結晶異方性(magnetocrystalline a η i s 〇 t r 〇 p y )與抗磁力。而根據目前的研究指出,這類薄 膜的磁性和晶粒大小均深受 Cr層厚度的影響,尤其當 Cr (請先閲讀背面之注意事項再堝寫木頁) -llv uc 1’· t- K·· 裝. 線. 本紙5艮尺度遑用中國國家標準(CNS) T4規格(210X297公龙)AG l \ C Ministry of Economics-1. Printed by the Quasi-Bureau Pongong Consumer Cooperative V. Description of the invention (1) This case is a manufacturing method of magnetic recording media. M enables the formation of a high recording density of cobalt / manganese / tungsten oxide Magnetic recording film. At present, hard disks are generally thin film disks that use Longitudinal 'recording technology. The magnetization directions of magnetic recording media are arranged horizontally. The magnetic head slides on the surface of the film, and the magnetic moment is induced through the coil or through the channel. The magnetic field generated by the flow changes the direction of magnetic moment magnetization to read and write data. This installation method is called the Winchester disk drive hard drive, which is currently the mainstream of commercial hard drives. The materials available in the literature for the application research of magnetic recording thin films cover the three major fields of horizontal recording, vertical recording, and magneto-optical recording. Cat gold-plated film is the largest in the three technical fields. . As far as horizontal magnetic recording materials are concerned, the general manufacturing method is shown in the first figure. Among them, CoCrH (M = Ni, Pt, Ta) in the sputtered gold film is currently the most widely used material system, although its The coercive force is up to about 1500 Oe, the saturation magnetization (Saturation magnetization) Ms is also up to about 600 ~ 1200 emu / ca ^, the squareness ratio (Squareness ratio) S is also about 0.8 K, the thickness is about 50 nm, let other The phase of the material is discolored, but the metal magnetic recording film still has shortcomings, including: 1) In addition to the CoPt alloy itself has a strong film crystal anisotropy, Cr needs to be used as the bottom layer to help the crystal orientation of the rib magnetic layer Growth, use M to enhance the magnetic crystalline anisotropy (magnetocrystalline a η is 〇tr 〇py) and diamagnetic force of the film. According to the current research, the magnetic and grain size of these films are deeply affected by the thickness of the Cr layer, especially when Cr (please read the precautions on the back before writing the wooden page) -llv uc 1 '· t- K ·· Packing. Thread. The original size of this paper is 5 Gen. It uses the Chinese National Standard (CNS) T4 specification (210X297 male dragon)
Λ (ί UG 層厚度較 2 ) 法鍍著一 過 3 00 t: 厚膜,勢 3 ) 在薄膜表 4 ) Κ上,而 至於 資成本低 性略差, 鍍金屬薄 21224^ 五、發明説明(2 薄時,對磁薄膜之磁性質影響程度 金靥薄膜硬度不足,因此基板上必 層 ΝίΡ來強化表面。若後續製程 ,將會導致非晶質的N i Ρ结晶化 必使磁性薄膜的雜訊升高,不利於 金臑薄膜碟片易遵腐蝕,為增畏使 面加鍍一層非晶質碳膜充做保護層 鈷基合金金臑薄膜的鈷含量均在重 鈷膈戰略物資,價格高昂使製膜成 無電鍍瞑 CoP與 CoNiP ,雖然製 ,但受陁於膜的磁性質不佳,加上 難以升級成為高記錄密度碟片選用 膜目前僅應用於磁帶製作,在硬碟 更巨。 須先以無窜鍍 中基板溫度超 且形成软磁性 資料謓寫。 用壽命,必補 〇 量百分比 60X 本偏高。 程簡單而且投 均匀性及附著 的材料。而蒸 領域尚未成热 請 先 閱 讀 背 而 之 注 意 事 項 再 堝 寫 木 頁 金 述 上 善 改 可 圖 二 第 閱 參 請 法下 方如 造因 製其 之 , 案點 本缺 由之 膜 屬Λ (ί UG layer thickness is less than 2) method plating over 3 00 t: thick film, potential 3) on the film table 4) Κ, and the capital cost is slightly worse, the metal plating is thin 21224 ^ V. Description of the invention (2 When thin, the impact of the magnetic properties of the magnetic film is insufficient. The hardness of the gold film is insufficient, so the substrate must be coated with NIP to strengthen the surface. If the subsequent process will result in the crystallization of amorphous N i P The increase in noise is not conducive to the easy compliance of the Jinmao thin film disc. To increase the fear, the surface is coated with an amorphous carbon film as a protective layer. The cobalt content of the cobalt-based alloy Jinmao thin film is in the heavy cobalt diaphragm strategic material. The high price makes the film into electroless electroplating CoP and CoNiP. Although it is made, it is affected by the poor magnetic properties of the film, and it is difficult to upgrade to a high recording density disc. The film is currently only used for tape production. It must be written with the substrate temperature in the non-channeling plating and forming soft magnetic data. The service life is 60%, which is high. The process is simple and the material is uniform and attached. The steam field has not yet become hot. Please read first Pay attention to the matter and write a gold page on the wood page. The description can be improved. Figure 2. The second reading method is as follows:
I A 之 理 處 極 陽 受 不 卻 切 密 係 闉 成 組 與 性 : 磁響 膜影 薄層 }底The reason of I A is that the extreme sun is not affected but the closeness is tight. The group and sex: the thin film of the magnetic resonance film
—1 A 度 硬 面 表 化 強 肋 幫 層 底 經濟部中央櫺準局工消赀合作社 質 物 瓷 ; 陶 高之 升鈍 訊搔 雜性 號活 訊學 OJ使化 ,致乃 不锇 有,化 雖相氧 }性} 2 磁 3 為 li A 但 問 蝕 腐 有 沒 廉 低 較 本 成 此 因 少 最 羼 金 資 含 層 , 護份 保成 鍍要 另主 爾為 無赖 故 Μ 在 4 存 題 本紙張尺度逍用中國國家標準(CNS)T4規格(210X297公;«:) A6 B6 五、發明説明(3 ) 而本案之主要目的為降低成本,因Μ鐵為主要成份。 本案之次一目的為達成較佳之訊號雜訊比。 本案之另一目的為達成較佳之抗蝕性。 本案之再一目的為賴由添加鈷錳等元素,配合適當熱 處理條件,可使其抗磁力高過 1000 Oe 。 本案係一種磁性記錄媒體之製造方法,包括:提供一 基板;提供一 Μ錳與辨製成之靶材,在其上方貼有鈷和娥 之小Η , Κ供調節其成份比例;以及令靶材在控製條件下 ,在基板上形成一磁性記錄媒體薄膜。而該上述之基板可 為矽晶片、玻璃片、以及金饜Η,而為增強其表面硬度, 則可於基板上加鍍一層 A b 0$膜,而此磁性記錄媒體係Μ 直流電漿法或以射頻電漿法所製成。而靶材係以純度約為 99.7之錳和戡製成,在其上並貼有純度約 99.9的鈷和锇 小片,Μ調節磁性記錄媒體薄膜之成份比例。而此磁性記 錄媒體薄膜之成份係Κ陽離子重量百分比之 Co鈷約 0〜 20¾ 、Μη 錳約 0〜18.53ί 、K 及 Fe 锇約 61.5 〜99. 5¾ 所形成,而此薄膜之較佳比例為 Co鈷約 6〜12¾、Μη錳 約 0.1〜6¾。此形成之磁性記錄媒體薄膜需具’ F e (諳先閲讀背面之注意事項再填寫本頁) .¾. 經 濟 部 中 央 標 準 局 印 製 2 ui 相或及 Fe3〇+相,故上述之磁性記錄媒體薄膜需經第一道 熱處理程序,即在約 200〜350TC (較佳為 300〜3401) ,Η氣氛下恆溫約 0 . 1〜2小時(較诖為 0 . 5〜1小時) ,將 〇(-「&0彡相堪原成 Fe30+相.此後再經第二道熱斑 理程序,即升溫至約 300〜400Ό ( 較佳為 340〜380C) ,大氣下恆溫約 0 . 1〜4小時(較佳為 0 . 5〜2小時)。 •綠· 甲 4 (210X297公嬗) 2122μ:^ A6 B6 五、發明説明(4 ) 如欲使磁性記錄媒體薄膜之抗磁力約至 3 00 0 Oe 以上則 需經第三道熱處理程序,即在於約 3 0 0〜3 8 0 較佳約 為 340〜380¾ ),空氣爐内退火約 0.1〜4小時(較佳 為約 2〜8小時)。經上之製造方法及熱處理程序下所得 到磁性記錄媒體薄膜之厚度約為 30〜500 nm ,其磁性值 之抗磁力約為 900〜4000 0e (較佳為 1200〜2000 0e), 飽和磁化量約為 44〜310 emu/on3 (較佳約為 200 emu/ ci/m上),角形比約 0.47〜0.90(較佳約為 0.7 Μ上) 。為俾免磁頭磨損,可於此磁性記錄媒體薄膜上加一潤滑 (請先閑讀背面之注意事項再填寫本页) 層 佳 較 獲 而 例 驗 實 及 Μ 例 圖 示 所 明 說 之 下 藉 得 案 本 解 了 構 結 之構 膜结 屬之 金膜 之鐵 般化 一 氧 前.案 目本 係係 圖圖 一二 第第 7 7 中中中 案案案 本本本 係係係 圖圖圖 三四五 第第第 ej -之 之 膜 f 薄 薄Γ f 3 3 ο ο ft ·* 形形 圖圖 射射 嬈繞 y y a a r 之 後 火 退 膜 a 繞 形 圖 射 異 1 月 C • 1 新 d η 曰 技ΓΡ 科pe 於ί 由錄 記 直 垂 ε a — m 出< 推錄 一 記 逐光 術磁 技和 碟} 磁 S 膜in 13 薄 的 新 Γ ο C e Γ 點夕 優之 的擊 量衝 容的 錄術 記技 大新 其了 ,除 洶 , 洶術 勢技 來錄 記 g F n d 水 Γ 8 Ο 碑 i * « 統 傳 脅 威 1 S 嚴 e η—1 A degree of hard surface surface strong ribbed layer bottom Ministry of Economics Central Bureau of Industry and Engineering Cooperative Society quality ceramics; Tao Gaozhi's blunt information and dominance of the number of active information learning OJ, but not the lack of Although the phase oxygen is 2), the magnetic 3 is li A, but the cost of corrosion is lower than the original cost. Because there is less money in the gold layer, the protection of the coating must be maintained. The paper size of the title book uses the Chinese National Standard (CNS) T4 specification (210X297; «:) A6 B6 V. Description of the invention (3) The main purpose of this case is to reduce costs because iron is the main component. The second purpose of this case is to achieve a better signal-to-noise ratio. Another purpose of this case is to achieve better corrosion resistance. The other purpose of this case is to add elements such as cobalt and manganese, together with appropriate heat treatment conditions, to make its coercive force higher than 1000 Oe. This case is a method of manufacturing a magnetic recording medium, which includes: providing a substrate; providing a target made of Mn and discriminated, with small Η, Κ of cobalt and e on top of it for adjusting the composition ratio; and making the target Under controlled conditions, a magnetic recording medium film is formed on the substrate. The above substrate can be a silicon wafer, a glass sheet, and gold noodles. To enhance the surface hardness, a layer of Ab 0 $ film can be plated on the substrate, and the magnetic recording medium is a DC plasma method or Made by radio frequency plasma method. The target material is made of manganese and zirconia with a purity of about 99.7, and small pieces of cobalt and osmium with a purity of about 99.9 are pasted on it. M adjusts the composition ratio of the thin film of the magnetic recording medium. The composition of the magnetic recording medium film is K cobalt weight percent Co cobalt about 0 ~ 20¾, Mn Mn about 0 ~ 18.53ί, K and Fe osmium about 61.5 ~ 99. 5¾ formed, and the preferred ratio of this film is Co cobalt is about 6 ~ 12¾, Mn manganese is about 0.1 ~ 6¾. The magnetic recording media film formed must have 'F e (know the precautions on the back and then fill in this page). ¾. The Central Standards Bureau of the Ministry of Economic Affairs prints the 2 ui phase or Fe3〇 + phase, so the above magnetic recording The media film needs to undergo the first heat treatment process, that is, about 200 ~ 350TC (preferably 300 ~ 3401), constant temperature under H atmosphere for about 0.1 ~ 2 hours (compared to 0.5 ~ 1 hour). (-"&Amp; 0 彡 phase can be made into Fe30 + phase. After that, the second hot spotting process is performed, that is, the temperature is raised to about 300 ~ 400Ό (preferably 340 ~ 380C), and the constant temperature under the atmosphere is about 0.1 ~ 4. Hours (preferably 0.5 ~ 2 hours). • Green · A 4 (210X297 public transmutation) 2122μ: ^ A6 B6 5. Description of the invention (4) If you want to make the magnetic recording medium film diamagnetic force is about 3 0 0 0 Above Oe, a third heat treatment process is required, that is, about 3 0 0 ~ 3 8 0 (preferably about 340 ~ 380¾), and annealing in an air furnace for about 0.1 ~ 4 hours (preferably about 2 ~ 8 hours). The thickness of the magnetic recording medium film obtained under the above manufacturing method and heat treatment process is about 30 ~ 500 nm, and its magnetic value is diamagnetic About 900 ~ 4000 0e (preferably 1200 ~ 2000 0e), the saturation magnetization is about 44 ~ 310 emu / on3 (preferably about 200 emu / ci / m), the angle ratio is about 0.47 ~ 0.90 (preferably About 0.7 μM.) In order to avoid magnetic head wear, you can add a lubricating film to this magnetic recording medium (please read the precautions on the back side before filling out this page). Explained clearly that the borrowed textbook solved the structure of the structure of the structure of the gold film before the iron-like oxygenation. The text of the case is shown in Figure 1 2 in the 7th and 7th cases of the middle case. Department of system diagrams Figures three four fiveth ej-the film f thin thin Γ f 3 3 ο ο ft · * shape chart after shooting around yyaar after fire retreating film a shape chart shooting strange January C • 1 new d η said technology ΓΡ branch pe Yuί from the record vertical ε a — m out < push a record of the optical technique and disc} magnetic S film in 13 thin new Γ ο C e Γ point Xi Youzhi's recording skills for hitting Rong Rong are very new. In addition to the fierce, fierce tactical skills to record g F nd 水 Γ 8 Ο monument i * «Unified threat 1 S Yan e η
C 經濟部中央標準局印製 向 不 得 不 碟 ec 碩 統 傳 J 小 、 短 r 薄 輕 。 Γ 進 趨挺 日度 品密 產錄 技記 科高 ,更 甲 4 (210X297 公沒) 21224^ A6 _B6 五、發明説明(5 )C. Printed by the Central Bureau of Standards of the Ministry of Economics. It is widely known that ec masters are small, short, thin and light. Γ advances and tends to be daily, close and confidential, technical records, high, and higher A 4 (210X297 public) 21224 ^ A6 _B6 V. Description of the invention (5)
要作為水平式髙記錄密度的磁記錄薄膜,必須符合下 列幾項條件:磁記錄材料要有高抗磁力(coercivity) He ,至少應高於 1000 Oe;殘餘磁化量(residual magnetization) Mr 要夠高;磁薄膜之膜厚愈薄,使薄膜磁區 相互間之去磁反應(demagnetization interaction) 降 低;Μ及高的訊號雜訊比(signal to noise ratio) SNRTo be a horizontal recording density magnetic recording film, the following conditions must be met: the magnetic recording material must have a high coercivity He, at least higher than 1000 Oe; the residual magnetization (residual magnetization) Mr should be high enough ; The thinner the thickness of the magnetic thin film, the lower the demagnetization interaction between the magnetic regions of the thin film (demagnetization interaction); Μ and high signal to noise ratio (signal to noise ratio) SNR
O 自從 IBM在 1990年發表記錄密度達 l(ib/in2 之磁 記錄技術 Μ 來(T. Yogi et al, IEEE Trans. Magn., MAG-26, (1990), 2271),人們發現磁記錄的記錄極限堪 有很大的空間,一般預測,到西元 2010年抵達 10Gb/in 是可能的(E. S. Murdock, IEEE Trans. Magn., MAG-28, (1992), 3078),彼時所需的記錄媒體有五種設計,最低 的抗磁力铺求是約 2500 0e,最高者需達約 4500 0e,前 者之 Mr5須達約 1.0 menu /cm2 ,後者只須約 0.35memu /cmz ,由此技術發展的趨勢評估,在可見的未來,高 He 薄膜(He > 2000 0e)實有迫切的爾要,本案之另一目的 即在於開發這類薄膜,Μ因應記錄密度大幅提昇之需。 經濟部中央標準局印製 (請先閲讀背面之注意事項再填寫本頁) 為對氧化戡薄膜能進一步了解,故先從文獻著手,依 據文獻(E. T. Wuori and D.E, Speliotis, Plating ίη the Electronic Industry , 3rd symposium, (1971), 315)指出,M蒸鍍法鍍著金靥撖薄膜,先於約 450〜500 t:氧化成 a-FqOj ,再於約 400¾,通 h及 C0的氣 氛下可通原成 Fe彡0+ 。另一文獻(R. L. Comstock and 甲 4 (210X297 父簷) 經濟部中央榣準局ΚΧ工消费合作社印製 21224^ Λ6 __no_ 五、發明説明(6 ) E. B . Moore, IBM J. Res. Dev. 18, ( 1 9 7 4 ) , 5 5 ) 指 出M旋轉鍍著法 Fe(H〇9)3 · 9ΗΑ0之水溶液嗔塗到約 300 〜3 5 0 TC 的基板上即可得到 α - F ^ 03薄膜,再經堪原與 氧化熱處理可分別獲得 Fe3〇+和 7 -F^ 03薄膜。 早期的研究皆偏重在相的合成方面,並未添加任何添 加物,因此抗磁力不高,只有 200 0e左右。但自1977 年起,開始有人取法針狀 7 - F & 03 磁粉添加 C 〇而提高 He的結果,轉用於薄膜方面。文獻(M. Satuo et al, IEEE Trans. Hagn.. MAG - 1 3, (1977), 1400)提出 M 蒸 鍍法製作C 〇χ F e0+薄膜。他們先將F e鍍在玻璃基板 上,約於 400 1C氧化成a-Fe2〇3,接著再鍍著一層 Co 於真空中退火,使 C 〇擴敗到 a - F e2 03内並形成 C ox Fe3_x. 0+ ,所得之薄膜抗磁力大幅提升至700 0e。 基於抗磁力的顯著提升,許多研究人員相繼投入此一 領域。文獻(S. Hattori et al, IEEE Trans. Hagn., HAG-15, (1979), 1549)首先提出以反應性濺渡法可成功 製備添加Co, Ti的氧化鐵磁性薄膜。先於通 Ar-(U之氣 氛下鍍著 oc -Fe2 03,再於 氣氛下通原成 Fe3 0_ ,可 再氧化成 7 - F 4 0彡。所得的薄膜抗磁力約為 7 0 0 0 e ,角 形比約為 0.8 ,記錄密度約為 1100 bits/mm2。這套方法 為目前工業上生產氧化戡系硬碟磁片最普遍的製程。 隔年,依文獻(S · Hattori et a 1 , IEEE Trans. Magn. , MAG- 1 5, ( 1 98 0 ) , 1 1 1 4 ) 指出同一批人將製程稍 加改良,省略一步,直接Μ反應性濺鍍法合成 Fe3 0+ (請先閲讀背而之注意事項再项寫木頁) 裝- 訂_ 線· 本紙張尺度逍用中Η國家樣準(CNS)肀4規格(210x297公龙)O Since IBM published a magnetic recording technology with a recording density of 1 (ib / in2) in 1990 (T. Yogi et al, IEEE Trans. Magn., MAG-26, (1990), 2271), people found that There is a lot of room for the record limit. It is generally predicted that it will be possible to reach 10Gb / in by 2010 (ES Murdock, IEEE Trans. Magn., MAG-28, (1992), 3078), the record required at that time The media has five designs, the lowest diamagnetic force is about 2,500 0e, the highest one needs to be about 4,500 0e, the former Mr5 must reach about 1.0 menu / cm2, the latter only needs to be about 0.35memu / cmz, resulting from the development of technology Trend assessment shows that in the foreseeable future, high-He films (He > 2000 0e) are urgently needed. Another purpose of this case is to develop such films. M responds to the need for a significant increase in recording density. Central Standard of the Ministry of Economy Printed by the Bureau (please read the precautions on the back and then fill out this page) In order to understand the oxide film further, so start with the literature, based on the literature (ET Wuori and DE, Speliotis, Plating ίη the Electronic Industry, 3rd symposium, (1971), 315) pointed out that The gold-thin film, first about 450 ~ 500 t: oxidized to a-FqOj, then about 400¾, can be converted into Fe 彡 0+ under the atmosphere of h and C0. Another document (RL Comstock and A4 ( 210X297 father eaves) Printed by the Ministry of Economic Affairs, Central Bureau of Industry and Commerce KKX Consumer Consultation Co., Ltd. 21224 ^ Λ6 __no_ V. Description of Invention (6) E. B. Moore, IBM J. Res. Dev. 18, (1 9 7 4), 5 5) Point out that the M spin coating method of Fe (H〇9) 3 · 9ΗΑ0 aqueous solution can be applied to the substrate of about 300 ~ 3 5 0 TC to obtain α-F ^ 03 thin film, which can be subjected to the original heat treatment with oxidation The Fe3〇 + and 7-F ^ 03 films were obtained separately. Early studies focused on the synthesis of phases without adding any additives, so the diamagnetic force is not high, only about 200 0e. But since 1977, some people Take the needle-like 7-F & 03 magnetic powder and add C 〇 to improve the result of He, and transfer it to the thin film. Literature (M. Satuo et al, IEEE Trans. Hagn .. MAG-1 3, (1977), 1400) The M vapor deposition method is proposed to produce C 〇χ F e0 + thin film. They first plated Fe on a glass substrate and oxidized it to a-Fe2〇3 at about 400 1C, then plated a layer of Co and annealed in vacuum to expand C 〇 to a-F e2 03 and form Cox Fe3_x. 0+, the diamagnetic force of the resulting film is greatly increased to 700 0e. Based on the significant improvement of diamagnetic force, many researchers have successively invested in this field. The literature (S. Hattori et al, IEEE Trans. Hagn., HAG-15, (1979), 1549) first proposed that the reactive sputtering method can be successfully used to prepare iron oxide magnetic films with Co and Ti added. It is plated with oc -Fe2 03 under the atmosphere of Ar- (U, and then formed into Fe3 0_ under the atmosphere, which can then be oxidized to 7-F 4 0. The resulting magnetic resistance of the thin film is about 7 0 0 0 e , The aspect ratio is about 0.8, and the recording density is about 1100 bits / mm2. This method is the most common process for the industrial production of oxide-based hard disks. In the next year, according to the literature (S · Hattori et a 1, IEEE Trans . Magn., MAG- 1 5, (1 98 0), 1 1 1 4) pointed out that the same batch of people improved the process slightly, omitting one step, and synthesized Fe3 0+ by direct M reactive sputtering method (please read the back first Matters needing attention to write a wooden page) Binding-Binding _ Line · This paper standard is used in Chinese National Standards (CNS) 4 specifications (210x297 male dragon)
212^ Λ G It G212 ^ Λ G It G
經濟部中央榣準局只工消t合作社印M 五、發明説明(7 ) 再氧化而得 7-Fe203。 雖然角形比 S提高至約 0.85, 但抗磁力卻稍有降低,只有約 600 0e。 因此後灌的研究 者較少採用此製程,多半採用他們於 1979年發表的實驗 流程。 到 1984年,前述研究群中的 0 Ishii和 I. Hata-keyama 於文獻(J. AppI. Phys. 55, (1984), 2269)中 提出採用反應性濺鍍法在氧化戡磁性薄膜内添加餓(Os) 獲致重大突破。他們發現添加 Os有下列諸項好處:大幅 提高抗磁力到約 1 9 2 0 0 e ,只添加 C 〇無法達到;能有效 抑制後讀熱處理造成的晶粒成長,進而提高薄膜的SNR 值,和Μ往添加 Cu有相同的作用;經過磁場下(7 KOe) 退火,抗磁力可提升至約 2100 0e;提高抗磁角形比( Coercive Squareness, S*)約至 0.95,比以往添加 Ti 更有效。而這個材料最大的缺點就是 0s太貴了,亦因此 锇氧磁性薄膜尚存研究的空間。 前述之文獻多Μ真空鍍膜方式製備锇氧磁性薄膜,設 備費用較昂貴。另一可行但設備簡易的製法為嗔霧裂解鍍 著法。依據文獻(M. Langlet et al, IEEE Trans. Magn., MAG-22, (1986), 151)指出噴霧裂解法亦可製備 高抗磁力的戡氧磁性薄膜。將鐡乙豳丙酮(iron acety-lacetonate)溶於正丁酵(butanol)内,利用超音波震 通器將溶液箱化,並M Ar-Og之混合氣體將霧化的液滴吹 送到約 420〜550t!的玻璃基板表面沈積成 7-Feii03 -Fe 0+薄膜。經過適當的熱處理所得之膜,其抗磁力最大 (請先閱讀背面之注意事項再艰离本頁) 裝· 訂- -線- 本紙張尺度遑用中國Η家標準(CNS)肀4規格(210X2町公*) 經濟部中央榣準局β工消t合作社印製The Central Bureau of Economics of the Ministry of Economic Affairs only prints M of the cooperative and the cooperative. V. Description of invention (7) 7-Fe203 is obtained by reoxidation. Although the angular ratio S is increased to about 0.85, the coercive force is slightly reduced, only about 600 0e. Therefore, post-irrigation researchers rarely adopt this process, and most of them adopt the experimental procedure published in 1979. By 1984, 0 Ishii and I. Hata-keyama in the aforementioned research group proposed in the literature (J. AppI. Phys. 55, (1984), 2269) that reactive sputtering method was used to add (Os) made a major breakthrough. They found that the addition of Os has the following benefits: greatly improve the coercive force to about 1 9 2 0 0 e, can not be achieved only by adding C 〇; can effectively suppress the grain growth caused by post-reading heat treatment, and thereby improve the SNR value of the film, and Adding Cu to Μ has the same effect; after annealing under a magnetic field (7 KOe), the coercive force can be increased to about 2100 0e; and the Coercive Squareness (S *) is increased to about 0.95, which is more effective than adding Ti in the past. The biggest disadvantage of this material is that 0s is too expensive, so there is still room for research on osmium oxide magnetic films. The aforementioned document uses a multi-M vacuum coating method to prepare osmium-oxygen magnetic thin film, and the equipment cost is relatively expensive. Another feasible method with simple equipment is the fogging cracking plating method. According to the literature (M. Langlet et al, IEEE Trans. Magn., MAG-22, (1986), 151), it is pointed out that the spray cracking method can also prepare high magnetic resistive oxygen magnetic films. Dissolve iron acety-lacetonate in butanol, use ultrasonic vibrator to tank the solution, and the mixed gas of M Ar-Og blows the atomized droplets to about 420 ~ 550t! The surface of the glass substrate is deposited into 7-Feii03-Fe 0+ film. The film obtained after proper heat treatment has the highest diamagnetism (please read the notes on the back before leaving this page). Binding · Binding-This paper uses the Chinese Standard (CNS) 4 specifications (210X2) Machiko *) Printed by the Central Bureau of Economic Affairs of the Ministry of Economic Affairs, printed by β Gongxiaot Cooperative
A G W C 五、發明説明(8 ) 約為 800 Oe,Ms 值約為 400 emu /on3。若添加 10 wtS! Co可提高抗磁力約至 1000 〇e M上,Ms值約為 350 emu / cm ^ 。 本案基於反應性濺鍍法可製作厚度較薄且附著性較佳 的薄膜,並發規調整鈷(錳)離子/鐵離子之重董百分比 ,配合熱處理條件,可製得高抗磁力之鈷(錳)氣化餓磁 性薄膜,有效克腋前述文獻中添加鈷、鈦、銅離子抗磁力 低於 1000 0e之缺點,同時避免使用價格昂貴的餓元素 亦能製得抗磁力高達約 4000 0e之此磁性薄膜,實乃一 富經濟效益,且又可得優良磁性薄膜的方法。 由於適當的添加如鈷,錳等元素控制抗磁力,作為高 記錄密度磁性薄膜之用途,琨將本案之製程詳述如下:提 供一基板,基板可為矽晶片,玻璃片或金屬片,本例之基 板採用 η型〔S i 0 X / S ί ( 1 0 0 )〕 晶片與康寧公司出品的 7059玻璃基板,二者皆具有光學鈒平坦度,試片先Μ鑽 石刀切割成 0 . 5 X 0 . 5 i η2 ,再加Μ清洗,清洗的步驟為 將基板浸於丙酮中,Μ超音波振通 5分鐘,消除表面油脂 ,再浸於去離子水中,Μ超音波振通 5分鐘,消除表面之 有櫬溶劑,然後取出Κ氮氣槍吹乾;提供一靶材,由本案 採用直流(dc)或射頻(rf)磁控濺射方式鍍膜,為使磁 鐵之磁場能有效輔助濺鍍過程,故靶材應盡量為非導磁性 ,使磁場的磁力線得以穿透,達到磁控的效果,然而本案 中選用組成的 Fe與 Co皆為高導磁率之材料,故合金靶 材之製作方式較為特殊,將純度大於約 99.7的霣解撖與 本紙5艮尺度逍用中B國家標準(CNS)肀4規格(210x297公;¢) (請先閲讀背面之注意事項再项寫木頁) 裝· 線. 21224^A G W C Fifth, the invention description (8) is about 800 Oe, and the Ms value is about 400 emu / on3. If adding 10 wtS! Co can increase the coercive force to about 1000 〇e M, Ms value is about 350 emu / cm ^. This case is based on the reactive sputtering method to produce a thinner film with better adhesion, concurrently adjust the weight percentage of cobalt (manganese) ions / iron ions, and with heat treatment conditions, high coercive cobalt (manganese ) Gasification magnetic film, effectively overcome the shortcomings of adding cobalt, titanium and copper ions in the aforementioned literature. The magnetic resistance is less than 1000 0e, while avoiding the use of expensive hungry elements can also produce a magnetic resistance of up to about 4000 0e. Thin film is a method with rich economic benefits and excellent magnetic thin film. Due to the appropriate addition of elements such as cobalt and manganese to control the coercive force, as a high recording density magnetic film, Kun detailed the process of this case as follows: provide a substrate, the substrate can be a silicon wafer, glass or metal sheet, this example The substrate adopts the η type [S i 0 X / S ί (1 0 0)] chip and the 7059 glass substrate produced by Corning, both of which have optical flatness. The test piece is first cut with a diamond knife to 0.5 X 0.5 i η2, then add M cleaning, the cleaning step is to immerse the substrate in acetone, M ultrasonic wave vibration for 5 minutes to eliminate surface grease, and then immerse in deionized water, M ultrasonic wave vibration for 5 minutes, eliminate There is a solvent on the surface, and then take out the K nitrogen gun to blow dry; provide a target material, which is coated by direct current (dc) or radio frequency (rf) magnetron sputtering method, so that the magnetic field of the magnet can effectively assist the sputtering process, Therefore, the target material should be as non-magnetic as possible, so that the magnetic field lines of the magnetic field can penetrate to achieve the effect of magnetron control. However, the selected Fe and Co in this case are materials with high magnetic permeability, so the manufacturing method of the alloy target is more special , The purity is large At about 99.7 years old, and the paper is used in the 5 gen standard for the use of the B National Standard (CNS) 4 specifications (210x297 g; ¢) (please read the precautions on the back and then write the wooden page). Installation and line. 21224 ^
Λ G ___lj_6_ 五、發明説明(9 ) (請先閲讀背面之注意事項#堝寫本頁) 電解錳在電動天平上稱取,而每次稱合金的總重為 150克 ,戡錳重量比為 3:1,根據相圖所示,這個組成在室溫下 為 7 -Fe非磁性相,可避開靶材#磁問題,將稱好的料倒 入氧化鋁坩鍋内,在大氣下Μ高遇波熔煉後鍰冷之,熔好 的靶材Κ車床車削成直徑 1英吋的圓棒,再Κ水冷式切割 櫬裁切成厚 2.5mm之圓片,經 ICP分析所得圓片組成之 重量百分比為 Fe: Mn = 77:23, 與原始配比相去不遠,至 於成份之調整則是在圓片上貼附純度約 99.9的锇和錳的 薄片(p e 1 1 e t) Μ行調節磁性記錄媒體薄膜之成份比例; 在控製條件下,在基板上形成一磁性記錄媒體薄膜,本案 所用的真空濺鍍設備,與一般商用傳統濺鍍系統無異,排 氣系統在理想狀態下終極ffi力可達 2 X 1 0< T 〇「r ,抽真空 前,先將靶材嵌於濺射槍底,基板亦置於基座盤上適當位 置,接著進行腔體粗抽,抽到 5 X 1 0< T 〇 r r ,此時打開基 座下之石英燈進行加熱,真空達 lX10_;lT〇rr後,關閉粗 抽閥,開始细抽進行高真空排氣,真空度達 lxl Torr 經濟部中央標準局貝工汸伢合作社印製 後可進行濺鍍製程。濺鍍前先行預濺鍍(pre-sputtering ),Μ期將靶材表面完全清除乾淨,暴露出新鲜的表面可 供進行鍍膜,預濺鍍條件因系統而異,就本系铳而言係通 入 15 mT〇「r的 Ar,設定直流電源供應器輸出功率為 30 瓦,進行 10分鐘,此時電流值已趨近定值,濺鍍速率保 持恆定,可打開基板上方之遮板 (shutter)進行薄膜鍍 著,濺鍍方式可採用直流(dc)或射頻(rf)濺鍍,熟悉 本項技藝人士皆知濺鍍條件依所使用系統不同而有很大差 本紙張尺度逍用中國國家標準(CNS) f 4規格(210X297公;¢) 21224^Λ G ___lj_6_ V. Description of the invention (9) (Please read the notes on the back #Cube to write this page) The electrolytic manganese is weighed on the electric balance, and the total weight of the alloy is 150 grams each time, and the weight ratio of manganese is 3: 1, according to the phase diagram, this composition is a 7-Fe non-magnetic phase at room temperature, which can avoid the target #magnetic problem, pour the weighed material into the alumina crucible, under the atmosphere M Gao Yubo smelted it after melting. The melted target material was turned by a lathe into a round bar with a diameter of 1 inch. The water-cooled cutting was then cut into 2.5mm thick wafers. The weight percentage of the wafers obtained by ICP analysis It is Fe: Mn = 77:23, which is not far from the original ratio. As for the adjustment of the composition, a thin film of osmium and manganese with a purity of about 99.9 (pe 1 1 et) is adjusted on the wafer. The proportion of ingredients; under control conditions, a magnetic recording medium film is formed on the substrate. The vacuum sputtering equipment used in this case is no different from the general commercial traditional sputtering system. The exhaust system can achieve an ultimate ffi force of 2 in an ideal state. X 1 0 < T 〇 "r, before evacuating, first insert the target material into the sputtering gun At the bottom, the substrate is also placed in an appropriate position on the pedestal tray, and then the cavity is roughly pumped to 5 X 1 0 <T 〇rr, at this time the quartz lamp under the pedestal is turned on for heating, and the vacuum reaches lX10_; lT〇rr After that, close the rough pumping valve and start fine pumping for high vacuum exhaust. The vacuum degree is lxl Torr. The Ministry of Economic Affairs Central Standards Bureau Beigongyi Cooperative Society can print the sputtering process after printing. Pre-sputtering (pre-sputtering) is performed before sputtering. sputtering), the target surface is completely cleaned in the M phase, and the fresh surface is exposed for coating. The pre-sputtering conditions vary depending on the system. For this system, 15 mT〇r Ar is set, set The output power of the DC power supply is 30 watts for 10 minutes. At this time, the current value has approached the fixed value, and the sputtering rate is kept constant. The shutter above the substrate can be opened for thin film plating. The sputtering method can be used Direct current (dc) or radio frequency (rf) sputtering. Those skilled in the art know that the sputtering conditions are very different depending on the system used. The paper size is free to use the Chinese National Standard (CNS) f 4 specifications (210X297); ¢ ) 21224 ^
Λ C Η C 經濟部中央標準局员工消费合作社印t 五、發明説明(10) 異,故本案對濺鍍條件除在所舉實例中說明外並不特別限 制,熟習濺鍍技術人士只要根據本發明閭述之成份及熱處 理條件,即可令其鍍得薄膜具本案所舉之性質,而此磁性 記錄媒體薄膜之成份係K陽離子重量百分比之 Co鈷約 0 〜20%、Μη錳約 0〜18,5!ϋ Μ及 Fe锇約 61.5〜99.5!1;所 形成,而此薄膜之較佳比例為 Co鈷約 6〜12X、 Μη錳約 0.1〜6%。此形成之磁性記錄媒體薄膜需具 7-Fea2 03 相 或及卩%0+相,故上述之磁性記錄媒體薄膜需經第一道熱 處理程序,即在約 2 0 0〜3501 (較佳約為3 0 0〜34 Ot:), 之氣氛下恆溫約 0 · 1〜2小時(較佳為 0 . 5〜1小時), 將a-Fh〇3相堪原成 Fe3〇4相,此後再經第二道熱旃理 程序,即再升溫至約 300〜400C (較佳約為 340〜38〇·〇 ),大氣下恆溫約 0 . 1〜4小時(較佳約為0 . 5〜2小時)。 如欲使磁性記錄媒體薄膜之抗磁力约至 300 0 0 e Μ上則 需經第三道熱處理程序,即在約 300〜380TC (較佳約為 340〜380¾),空氣爐内退火約 0.1〜4小時(較佳為 2 〜8小時)。經上之製造方法及熱處理程序下所得的磁性 記錄媒體薄膜之厚度約為 30〜500 nra ,其磁性值之抗磁 力約為 900〜4000 0e (較佳約為 1200〜2000 0e), 飽 和磁化量約為 44〜310 emu/on5 (較佳約為 200 eBu / cm3 Μ上)角形比約為 0.47〜0.90(較佳約為 0.7以上)。 為俾免磁頭磨損可於此磁性記錄媒體薄膜上加一潤滑層。 由上述製程所得之薄膜,M X-ray 繞射分析可證明 為純粹 相與7-Fe20j相之薄膜,本案的製程利用 (請先閲讀背面之i.t意事項#堺寫木頁) 裝· 訂_ 線· 本紙張尺度边用中《 B家標準(CNS) T4規格(210X29741) 212細Λ C Η C The Ministry of Economic Affairs, Central Standards Bureau, Employee Consumer Cooperatives printed t V. The description of the invention (10) is different, so the sputtering conditions in this case are not particularly limited except those described in the examples given. The composition and heat treatment conditions of the invention can make the plated film have the properties mentioned in this case, and the composition of the magnetic recording medium film is K cobalt weight percent Co cobalt about 0 ~ 20%, Mn manganese about 0 ~ 18,5! Ϋ Μ and Fe osmium about 61.5 ~ 99.5! 1; formed, and the preferred ratio of this film is Co cobalt about 6 ~ 12X, Mn about 0.1 ~ 6%. The formed magnetic recording medium film needs to have a 7-Fea2 03 phase or a 0% phase, so the above magnetic recording medium film needs to undergo the first heat treatment process, that is, about 200 to 3501 (preferably about 3 0 0 ~ 34 Ot :), the constant temperature under the atmosphere is about 0. 1 ~ 2 hours (preferably 0.5 ~ 1 hour), the a-Fh〇3 phase can be transformed into Fe3〇4 phase, and then after The second thermal management procedure, that is, to raise the temperature to about 300 ~ 400C (preferably about 340 ~ 38〇 · 〇), the temperature under the atmosphere is about 0.1 ~ 4 hours (preferably about 0.5 ~ 2 hours ). If you want to make the magnetic resistance of the magnetic recording medium film to about 300 0 0 0 e Μ need to go through the third heat treatment process, that is about 300 ~ 380TC (preferably about 340 ~ 380¾), annealing in the air furnace about 0.1 ~ 4 hours (preferably 2-8 hours). The thickness of the magnetic recording medium film obtained under the above manufacturing method and heat treatment process is about 30 ~ 500 nra, the magnetic value of the coercive force is about 900 ~ 4000 0e (preferably about 1200 ~ 2000 0e), the saturation magnetization Approximately 44 ~ 310 emu / on5 (preferably about 200 eBu / cm3 Μ) corner ratio is about 0.47 ~ 0.90 (preferably about 0.7 or more). To avoid wear of the magnetic head, a lubricant layer can be added on the magnetic recording medium film. The X-ray diffraction analysis of the film obtained by the above process can be proved to be a film of pure phase and 7-Fe20j phase, and the process of this case is used (please read the it on the back of it # 堺 写 木 页) Installation · Order_ Line · This paper is used in "B home standard (CNS) T4 specification (210X29741) 212 fine
Λ G jj_G_ 五、發明説明(11) (請先閲讀背而之注意事項再艰寫本頁) 不同的合金添加組成,配合熱處理條件來控製抗磁力的高 低,而K濺鍍法製得之薄膜,其附著性與膜面平整度極佳 ,具鏡面反射之程度,加上氧化辙系薄膜本身具有高訊號 雜訊比,故本案非常適合高密度磁記錄薄膜之用。 為求對此磁性記錄媒體更#一步的了解,玆先舉一例 加Μ說明: 靶之金屬重量比為 Fe: Co: Μη = 96.4: 2.4: 1.2, 基板為 η型〔Si〇x/Si(100)〕晶片,Κ直流濺鍍法鍍 膜,濺鍍條件為靶材至基板距離為 5 cm ,基板溫度保持 約 100Ό, 基板旋轉轉速為 20 RPM,濺鍍分壓比控制為 Ar: = 1:1 ,而總壓為 30 mTorr ,輸入功率定在 30 瓦,工作電流為 70 ibA ,初鍍膜進行約 300〜340 C 堪 原熱處理 1小時,爐冷後所得之膜其抗磁力約為 2250 0e ,飽和磁化量約為 100 emu/απ5 ,角形比約為 0.7 。如 將前堪原熱處理後之膜再於約 3 5 0〜400 1〕氣化 2小時. 埔冷後所得之膜其抗磁力約為 1300 0e,飽和磁化量約為 55 emu/απ’ ,角形比約為 0.75。 當然熟習於本技藝之人士,得就前述例子為如下諸般 變化: 經濟部中央標準局员工消费合作社印製 1 )如上述之例僅將基板更改為康寧 7 0 5 9玻璃,而 其他條件不變,將初鍍膜在約 300〜340C 下堪原熱處理 1小時,則爐冷後所得之瞑其抗磁力為 2450 0e,飽和磁 化最約為 1 0 5 e m u / on3 ,角形比約為 0 . 6 8。如將此堪原 熱處理後之膜再於約 350〜400t:氧化 2小時,爐冷後所 本紙張尺度边用中國國家楳準(CNS)甲4規格(210X297公*) 五、發明説明(12)Λ G jj_G_ V. Description of the invention (11) (Please read the precautions before writing this page) Different alloys are added to the composition, combined with heat treatment conditions to control the level of diamagnetic force, and the film prepared by the K sputtering method, Its adhesion and film flatness are excellent, with the degree of specular reflection, and the oxide film has a high signal-to-noise ratio, so this case is very suitable for high-density magnetic recording films. In order to understand the magnetic recording media more step by step, here is an example to add M description: the metal weight ratio of the target is Fe: Co: Mn = 96.4: 2.4: 1.2, the substrate is η type [Si〇x / Si ( 100)] Wafer, K DC sputtering method coating, sputtering conditions are 5 cm between the target and the substrate, the substrate temperature is maintained at about 100Ό, the substrate rotation speed is 20 RPM, and the sputtering partial pressure ratio is controlled to Ar: = 1: 1, and the total pressure is 30 mTorr, the input power is set at 30 watts, the operating current is 70 ibA, the initial coating is subjected to a heat treatment of about 300 ~ 340 C for 1 hour, and the anti-magnetic force of the film obtained after furnace cooling is about 2250 0e, The saturation magnetization is about 100 emu / απ5 and the angular ratio is about 0.7. For example, the film after heat treatment before Qiankan was vaporized at about 3 5 0 ~ 400 1] for 2 hours. The anti-magnetic force of the film after Po cooling is about 1300 0e, the saturation magnetization is about 55 emu / απ ', angular The ratio is about 0.75. Of course, those who are familiar with this skill must make the following changes to the aforementioned example: Printed by the Employees ’Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 1) As in the above example, only the substrate is changed to Corning 7 0 5 9 glass, and other conditions remain unchanged. , The primary coating is heat-treated at about 300 ~ 340C for 1 hour, then the diamagnetism obtained after furnace cooling is 2,450 0e, the saturation magnetization is about 1 0 5 emu / on3, and the angular ratio is about 0.68 . For example, the film after heat treatment at about 350 ~ 400t: oxidized for 2 hours, after the furnace is cooled, the paper scale is used in China National Standard (CNS) A 4 specifications (210X297 g *) V. Description of the invention (12 )
AG H G 經濟部中央標準局员工消t合作社印製 得之膜其抗磁力約為 900 Oe,飽和磁化量約為 45 emu/ cm^ ,角形比為 0.90。 2) 如上述之例,僅將靶之金屬重董百分比更改為|?e :Co: Μη =89.3: 10.5: 0.2,其他條件不變,初鍍膜仍K 約 3 ϋ 0〜3 4 0 t 堪原熱處理 1小時,爐冷後所得之薄膜其 抗磁力約為 1 1 7 0 0 e ,飽和磁化虽約為 2 6 0 e m u / ,角 形比約 0.56。請參間第三圖,該圖為此膜之 X-ray繞射 圖形,分析後可確證為F e3 0+相。再將此遢原熱處理後之 膜,再於約 360〜400C氧化 2小時,爐冷後所得之膜其 之抗磁力約為 3000 0e,飽和磁化畺約為 310 emu /cm3 , 角形比約為 0.61。請參閲第四圖,該圖為此膜之 X-ray 繞射圖形,分析後可確證為 γ-FeiOj,如此膜再經約 340〜360¾ 8小時退火熱處理,晡冷後所得之薄膜其抗 磁力約為 3 8 0 0 0 e,飽和磁化量約為 2 6 0 emu/,角形 比約為 0 . 6 3 ,請參閲第五圖,該圖為此膜之X - r a y繞射 圖形,分析後可確證仍為 7-Fe;l03相。 3) 如上述之例,靶之金屬重量百分比為 Fe: Co: Μη = 89.3: 10.5: 0.2,基板為康寧 7 0 5 9玻璃,初鍍膜 Μ約 300〜340t:堪原熱處理 1小時,爐冷後所得之膜其 抗磁力約為 1020 0e,飽和磁化量約為 270 emu /on3 ,角 形比約為 0 . 6 2 。如將此埵原後之初鍍膜,再經約 3 6 0〜 380¾ 氧化 2小時,爐冷後所得之膜其抗磁力約筠 2700 0e,飽和磁化量約為 2 9 0 emu/cnr 角形比為 0.90,如 此膜再經約 340〜36〇·Ιΰ退火熱處理約 8小時,則《冷後 本紙張尺度边用中國國家櫺準(CNS)甲4規格(210X297公;«:) (請先閲讀背而之注意事項再堝寫本頁) 裝· 線< ,1224AG H G The film printed by the Cooperative Society of the Central Standards Bureau of the Ministry of Economy has a diamagnetic force of about 900 Oe, a saturation magnetization of about 45 emu / cm ^, and an angular ratio of 0.90. 2) As in the above example, only the percentage of heavy metal in the target is changed to |? E: Co: Μη = 89.3: 10.5: 0.2, other conditions remain unchanged, the initial coating is still K about 3 ϋ 0 ~ 3 4 0 t After the original heat treatment for 1 hour, the diamagnetism force of the film obtained after furnace cooling is about 1 1 700 e, although the saturation magnetization is about 2 60 emu / and the angular ratio is about 0.56. Please refer to the third figure, which is the X-ray diffraction pattern of this film, which can be confirmed as F e3 0+ phase after analysis. The heat-treated film is then oxidized at about 360 ~ 400C for 2 hours. After the furnace is cooled, the anti-magnetic force of the film is about 3,000 0e, the saturation magnetization is about 310 emu / cm3, and the angular ratio is about 0.61 . Please refer to the fourth figure, which is the X-ray diffraction pattern of this film, which can be confirmed as γ-FeiOj after analysis, so that the film is subjected to annealing treatment for about 340 ~ 360¾ 8 hours, and the resistance of the film obtained after cooling The magnetic force is about 3 800 0 0 e, the saturation magnetization is about 2 6 0 emu /, and the angular ratio is about 0.63. Please refer to the fifth figure, which is the X-ray diffraction pattern of this film. After analysis, it can be confirmed that it is still 7-Fe; phase l03. 3) As in the above example, the weight percentage of the target metal is Fe: Co: Mn = 89.3: 10.5: 0.2, the substrate is Corning 7 0 5 9 glass, the initial coating film M is about 300 ~ 340t: the original heat treatment is 1 hour, the furnace is cooled The resulting film has a coercive force of about 1020 0e, a saturation magnetization of about 270 emu / on3, and an angular ratio of about 0.62. For example, after the initial coating of the original film, and then oxidized for about 3 6 0 ~ 380¾ for 2 hours, the film obtained after furnace cooling has a magnetic resistance of about 2700 0e and a saturation magnetization of about 2 9 0 emu / cnr. 0.90, so the film is then annealed for about 340 ~ 36〇 · Ιΰ for about 8 hours, then "after cooling, the paper size is used in China National Standards (CNS) A 4 specifications (210X297;« :) And the precautions will be written on this page) Installation · Line <, 1224
Λ fi W C 五、發明説明(;L3) 所得之薄膜其抗磁力約為4000 Oe,飽和磁化量約為255 e m u / ,角形比約為 0 . 8 3。 為求對此磁性記錄媒體更明確的了解,玆再舉一例加 Μ說明: 靶之金靨重最百分比為 Fe: Co: Μη = 79.5: 10.5: 10.0,基板為 η型〔Si0x/Si(100)〕晶片,Μ射頻猫 鍍法鍍膜,濺鍍條件為靶材至基板距離約為5 C m ,基板 溫度保持約 100Ό, 基板旋轉轉速為 20 RPM,濺鍍分壓 比控制為 Ar: 0之=1:1 ,而總壓為 30 mTorr ,輸入功 率定在50瓦,工作電流為70 mA ,初鍍膜進行約300〜 340¾堪原熱處理1小時,逋冷後所得之膜其抗磁力約為 1200 0e,飽和磁化量約為 200 emu /cm3 , 角形比約為 0. 45 υ如將此經堪原熱處理後之膜,再經約 360〜38010氧 化 2小時,熵冷後所得之膜其抗磁力約為 27 0 0 0 e ,飽 和磁化量約為1 2 8 e m u / 〇/ ,角形比約為0 . 4 5。 當然上述之例亦可有如下諸般變化: 經濟部中央檁準局貝工消伢合作社印製 (請先閲讀背面之注意亊項再堺寫本頁) 丁 1) 如上述之例僅將基板更改為康寧 7059玻璃,其 他條件不變,將此初鍍之膜以約 300〜3401 堪原熱處理 1小時,爐冷後所得之膜其抗磁力約為 1050 0e,飽和磁 化量約為 205 emu /cm3 ,角形比約為 0.47。如將此經堪 原熱處理後之膜,再經約 360〜400T0氧化 2小時,爐冷 後所得之膜其抗磁力約為 2520 0e,飽和磁化量約為115 emu/ αη^ ,角形比為 0.48。 2) 如上述之例將靶之金屬重量百分比更改為Fe:Co: 本紙張尺度逍用中國Η家樣準(CNS)甲4規格(210X297公;a:) Λ ο Π c 2l224i〇 五、發明説明(1勺 Μη = 71.0: 10.5: 18.5, 其他條件不變,將所得初鍍膜 Κ約 300〜340 ¾ 堪原熱處理 1小時,爐冷後所得之膜其 抗磁力約為 1400 0e,飽和磁化虽約為 150 erau /cm3 ,角 形比約 0 . 4 3。如將此經堪原熱處理後之膜,再經約3 6 0〜 4 0 0 1C氧化約 2小時,爐冷後所得之膜其抗磁力約為 2 6 5 0 0 e ,飽和磁化量約為 1 5 0 e m u / cm3 ,角形比約為 〇 . 3 0。 3)如上述之例,將靶材之金屬重量百分比更改為Fe :Co: Μη = 71.0: 10.5: 18.5,而基板亦改為康寧 7 059 玻璃,其他條件不變,將此所得初鍍之膜以約 300〜340 "C 遨原熱處理1小時,燫冷後所得之膜其抗磁力約為 1350 0e,飽和磁化量約為165emu/cm3 ,角形比約為 0.41 。如將此經缠原熱處理後之膜,再經約3 6 0〜4 0 0 t:氧化 2小時,爐冷後所得之膜其抗磁力約為 2200 0e,飽和磁 化量約為 145 emu/απ3 .角形比為 0 . 3 3。 由上之說明以及圖示,熟習於本技藝人士深知本發明 能達到前揭之目的,然皆不脫如附申請專利範圍所欲保護 者。 :再場寫木頁) 經濟部中央斗局EX工消费合作社印製 本紙張尺度边用中S Η家樣準(CNS) TM規格(210X297公;¢)Λ fi W C 5. Description of the invention (; L3) The resulting film has a coercive force of approximately 4000 Oe, a saturation magnetization of approximately 255 e m u /, and an angular ratio of approximately 0.83. In order to get a clearer understanding of this magnetic recording medium, here is another example to add M description: The target percentage of gold weight is Fe: Co: Mn = 79.5: 10.5: 10.0, the substrate is η type [Si0x / Si (100 )〕 Wafer, M RF cat plating method, sputtering conditions are: target to substrate distance is about 5 C m, substrate temperature is maintained about 100Ό, substrate rotation speed is 20 RPM, sputtering partial pressure ratio is controlled to Ar: 0 = 1: 1, and the total pressure is 30 mTorr, the input power is set at 50 watts, the working current is 70 mA, the initial coating is subjected to a heat treatment of about 300 ~ 340¾ for 1 hour, and the anti-magnetic force of the resulting film after cooling is about 1200 0e, the saturation magnetization is about 200 emu / cm3, and the aspect ratio is about 0.45. If the film after heat treatment is subjected to the original heat treatment, it is then oxidized for about 360 ~ 38010 for 2 hours. It is about 27,000 e, the saturation magnetization is about 1 2 8 emu / 〇 /, and the angle ratio is about 0.45. Of course, the above example can also be changed as follows: Printed by the Ministry of Economic Affairs Central Purification Bureau Beigong Consumer Cooperative (please read the notes on the back before writing this page) D1) As in the above example, only the substrate is changed For Corning 7059 glass, the other conditions remain unchanged. The initial film is heat-treated at about 300 ~ 3401 for 1 hour. After the furnace is cooled, the anti-magnetic force of the film obtained is about 1050 0e, and the saturation magnetization is about 205 emu / cm3. , The aspect ratio is about 0.47. For example, the film after heat treatment can be oxidized for about 360 ~ 400T0 for 2 hours. After the furnace is cooled, the magnetic resistance of the film is about 2520 0e, the saturation magnetization is about 115 emu / αη ^, and the angle ratio is 0.48. . 2) Change the metal weight percentage of the target to Fe: Co as described in the above example: This paper scale is easy to use Chinese Η home sample standard (CNS) A 4 specifications (210X297 g; a :) Λ ο Π c 2l224i〇 V. Invention Description (1 spoon Mn = 71.0: 10.5: 18.5, other conditions remain unchanged, the obtained initial coating K is about 300 ~ 340 ¾ can be heat-treated for 1 hour, the diamagnetic resistance of the film obtained after furnace cooling is about 1400 0e, although the saturation magnetization Approximately 150 erau / cm3, the angle ratio is about 0.4 3. If this film is heat-treated, it will be oxidized by about 3 6 0 ~ 4 0 0 1C for about 2 hours. The magnetic force is about 2 6 5 0 0 e, the saturation magnetization is about 1 5 0 emu / cm3, the angular ratio is about 0.3 0. 3) As in the above example, change the metal weight percentage of the target to Fe: Co : Μη = 71.0: 10.5: 18.5, and the substrate is also changed to Corning 7 059 glass, other conditions remain unchanged, the obtained preliminary film is heat-treated at about 300 ~ 340 " C Ahara for 1 hour, and then obtained after cooling The diamagnetic force of the film is about 1350 0e, the saturation magnetization is about 165emu / cm3, and the angular ratio is about 0.41. If the film after the heat treatment of the original wrap is subjected to about 3 6 0 ~ 4 0 0 t: oxidation for 2 hours, the film obtained after furnace cooling has a diamagnetic resistance of about 2200 0e and a saturation magnetization of about 145 emu / απ3 .Angle ratio is 0.33. From the above description and illustrations, those skilled in the art know that the present invention can achieve the purpose of pre-disclosure, but none of them are as protected as the scope of the patent application. : Write a wooden page again) Printed by the Ministry of Economic Affairs, Central Bureau of Industry and Technology, EX Industrial and Consumer Cooperatives. This paper is used in the middle of the standard (CNS) TM specifications (210X297; ¢)
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