201000651 九、發明說明： 【發明所屬之技術領域】 本發明係有關於一種免材之 4古、土 裡％玎之表w方法，詳言之，係關於 -種含貴金屬之金屬基陶練合㈣之製造方法。 【先前技術】201000651 IX. Description of the invention: [Technical field to which the invention pertains] The present invention relates to a method for exempting materials from the ancient and the earth, and in particular, relating to the metal-based ceramics containing precious metals. (4) Manufacturing methods. [Prior Art]
硬碟為現代用來儲存大量資料的主要裝置，而資料主要 是存放在硬碟碟片上之磁性薄膜記錄層，該磁性薄膜記錄 層主要成分是具有料Pt)貴金屬之姑（c。)基合金材料。習 知該磁性薄膜記錄層係利用一㈣用之乾材，以滅鑛 (Sputtering)製程方式披覆於硬碟碟片上。 在習知技術中，鈷鉻鉑-二氧化矽（C〇CrPt_Si〇2)薄膜是 目前高容量硬碟之磁記錄薄膜主要之材料。其中，由於内 含肌陶冑，因此需採㈣末冶金製程來製備c。⑽_si〇2 乾材’亦’選用Co粉、Cr粉、pt粉與si〇2粉充分混合， 或選用CoCrFt預合金粉與叫粉充分混合之後，再利用熱 壓製程或熱均壓製程將靶材成型及緻密化。 習知之粉體混合方式分為乾式混粉及濕式混粉兩種，二 者主要之差異在於是否選擇於溶液中進行混粉，但無論採 用何種混粉方式，都無法克服金屬粉體與陶«體比重差 異甚大而無法均勻混合的問題。 另外，在濕式混粉製程中，c〇粉、Cr粉、pt粉及Si〇2粉 係於-混合球體㈣行混粉，以形成混合聚體。因此，濕 式混粉製程完成後，將該混合㈣自該混合球體内取出 時，會有部分該混合漿體殘留黏滯於該混合球體内。其 131536.doc 201000651 中，由於該c〇CrPt-Sl〇2*材中之咐金屬的含量高達百分 之三十重量百分比（30 Wt%)以上，故濕式混粉製程將會造 成大量之Pt貴金屬的浪費，因而增加靶材之製造成本 & 因此，有必要提供一創新且富有進步性之含貴金屬之金 屬基陶曼複合把材之製造方法，以解決上述問題。 【發明内容】 本發明提供-種含貴金屬《金屬基陶曼複合無材之製造 方法’該製造方法包括：⑷提供磁性金屬粉體及陶瓷粉 體，該等粉體之·純度係大於99_9%;⑻將㈣:是粉體及該 磁性金屬粉體於一溶劑中進行濕式混粉，以形成漿體，其 中該陶瓷粉體披覆於該磁性金屬粉體之表面；（c)乾燥該漿 體，以形成陶金複合粉體；（d)將該陶金複合粉體與貴金屬 粉體進行乾式混粉，該貴金屬粉體之純度係大於99 9%; 及（e)成型及緻密化混合後之該陶金複合粉體及該貴金屬粉 體，以形成該含貴金屬之金屬基陶瓷複合靶材。 本發明之製造方法係先利用濕式混粉製程，將該陶瓷粉 體均勻地被覆於該磁性金屬粉體之表面，並經由乾燥製程 後，取得該陶金複合粉體，再利用乾式混粉製程將該貴金 屬粉體與該陶金粉體均勻混合’最後利用成型及緻密化製 程將該陶金複合粉體製成緻密之靶材。本發明之製造方法 可均勻地混合該磁性金屬粉體、該陶瓷粉體及該貴金屬粉 體，並且可減少靶材製作過程中該貴金屬粉體的浪費，故 可改善靶材之品質及降低靶材之製造成本。 【實施方式】 I31536.doc 201000651 圖1顯示本發明含貴金屬之金屬基陶瓷複合靶材之製造 法之机程圖，圖2顯示本發明含貴金屬之金屬基陶瓷複 :口乾材之局部放大示意圖。其中，該含貴金屬之金屬基陶 瓷複:靶材之製造方法，係可應用於磁記錄產業、光電產 業或半導體產業之溥膜滅鍍製程。配合參考圖1及圖2，首 先參考步驟S11，提供磁性金屬粉體11及陶瓷粉體12， b等粕體Π、12之純度較佳係大於99.9%。在本實施例 f 中°亥磁性金屬粉體11及該陶瓷粉體12之純度係大於 99.95%。其中，該磁性金屬粉體u可絲或钻鉻合金。 在本實施例中，該陶瓷粉體12係選用二氧化矽（Si〇2)或 一軋化鈦（Ti〇2)。其中，該陶瓷粉體12之粒徑較佳為〇.07 至1 .〇微米（μιη)。 參考步驟S12，將該陶瓷粉體12及該磁性金屬粉體丨丨於 一溶劑（例如：水或酒精）中進行濕式混粉，以形成漿體， 其中該陶瓷粉體12披覆於該磁性金屬粉體丨丨之表面。在步 ( 驟S12中，6亥磁性金屬粉體11之表面及該陶瓷粉體12之表 面帶有不同電性之電荷，使該陶瓷粉體12坡覆於該磁性金 屬粉體11之該表面，以提升混合之均句度。較佳地，該濕 式混粉之混合時間為6至24小時。 要注意的是，根據不同之混合材質及混合條件，在步驟 S12中，可另包括一調整ρΗ值步驟，加入一酸或鹼溶液以 調整該漿體之pH值，以使該磁性金屬粉體^之表面及該陶 竞粉體12之表面帶有不同電性之電荷。 參考步驟S13，乾燥該漿體，以形成陶金複合粉體。在 131536.doc 201000651 本實施例中’係以真空乾燥方法乾燥該漿體，其中，真空 乾燥之溫度係為，真空乾燥時間係為2至6小 時’真空乾燥之真空度小於760托（t〇rr)。 參考步驟S14’將該陶金複合粉體與貴金屬粉體13進行 乾式混粉’該貴金屬粉體丨3之純度係大於99·9% ^在本實 施例中，該貴金屬粉體13係選用鉑（Pt)，且其純度係大於 99.95% ’並且，該乾式混粉之混合時間較佳為4至8小時。 參考步驟S15，成型及緻密化混合後之該陶金複合粉體 及該貴金屬粉體13’以形成本發明含貴金屬之金屬基陶瓷 複〇乾材1。在本實施例中，係以熱壓（h〇t pressing)製程 或熱均壓（hot isostatic pressing)製程進行該成型及緻密化 步驟，其中’成型及緻密化之溫度係為8〇(rc至12〇〇t， 成型及緻密化之時間係為1至4小時。 較佳地’該陶瓷粉體12之重量百分比係為5%至12%，該 貝金屬粉體13之重量百分比係為2〇%至5〇%，其餘之重量 百分比係為該磁性金屬粉體11含量。在本實施例中該磁 性金屬粉體11係為鈷鉻合金，其中該陶瓷粉體12之重量百 分比為5%至12%，該貴金屬粉體13之重量百分比為2〇%至 50%，該鈷鉻合金之鉻之重量百分比係為4%至16%，其餘 之重量百分比為該始鉻合金之钻之重量百分比。 茲以下列實例予以詳細說明本發明，唯並不意謂本發明 僅侷限於此等實例所揭示之内容。 實例1 : 本實例係以銘鉻鉑-二氧化矽（C〇CrPt_si〇2)合金濺鍍靶 131536.doc 201000651 材的製作為例。首先’提供純度高達99.95%以上且具有磁 哇之鈷（C〇)粉’以及提供純度亦高達99.95%以上之鉻（Cr) 粕鉑（Pt)粉、二氧化矽（Si〇2)粉（粒徑0.25 μιη)。其中’ 鈷的含量為百分之四十六重量百分比(46舞鉻的含量 為5 Wt%的，鉑的含量為42 wt%，二氧化矽的含量為7The hard disk is a modern main device for storing a large amount of data, and the data is mainly a magnetic film recording layer stored on a hard disk. The magnetic film recording layer is mainly composed of a material Pt). alloy. It is known that the magnetic film recording layer is coated on a hard disk by a sputtering process using a dry material for one (four). In the prior art, a cobalt chromium-ruthenium dioxide (C〇CrPt_Si〇2) film is the main material of a magnetic recording film of a high-capacity hard disk. Among them, due to the inclusion of muscle pottery, it is necessary to adopt the (4) final metallurgical process to prepare c. (10)_si〇2 Dry material 'also' uses Co powder, Cr powder, pt powder and si〇2 powder to mix well, or CoCrFt prealloyed powder is mixed with the powder, then use hot pressing process or hot equalizing process to target Material forming and densification. The conventional powder mixing method is divided into dry mixed powder and wet mixed powder. The main difference between the two is whether or not the powder is mixed in the solution, but the metal powder cannot be overcome regardless of the mixed powder method. The problem that the body weight of the pottery is very different and cannot be evenly mixed. Further, in the wet mixing process, c powder, Cr powder, pt powder and Si〇2 powder are mixed in a mixed sphere (four) to form a mixed polymer. Therefore, after the wet mixing process is completed, when the mixing (4) is taken out from the mixing sphere, a part of the mixed slurry remains in the mixing sphere. In 131536.doc 201000651, since the content of base metal in the c〇CrPt-Sl〇2* material is as high as 30% by weight (30 Wt%) or more, the wet mixing process will cause a large amount of The waste of Pt precious metals, thus increasing the manufacturing cost of the target & therefore, it is necessary to provide an innovative and progressive method of manufacturing a precious metal-containing Tauman composite composite material to solve the above problems. SUMMARY OF THE INVENTION The present invention provides a method for producing a metal-containing Taoman composite material without a precious metal. The manufacturing method includes: (4) providing a magnetic metal powder and a ceramic powder, wherein the purity of the powder is greater than 99_9% (8) (4): the powder and the magnetic metal powder are wet-mixed in a solvent to form a slurry, wherein the ceramic powder is coated on the surface of the magnetic metal powder; (c) drying a slurry to form a ceramic gold composite powder; (d) dry mixing the ceramic gold composite powder with the precious metal powder, the purity of the precious metal powder being greater than 99 9%; and (e) forming and densification The ceramic gold composite powder and the precious metal powder are mixed to form the metal-based ceramic composite target containing the noble metal. In the manufacturing method of the present invention, the ceramic powder is uniformly coated on the surface of the magnetic metal powder by a wet mixing process, and after the drying process, the ceramic gold composite powder is obtained, and then the dry mixed powder is used. The process uniformly mixes the precious metal powder with the pottery gold powder. Finally, the pottery gold composite powder is made into a dense target by a molding and densification process. The manufacturing method of the present invention can uniformly mix the magnetic metal powder, the ceramic powder and the precious metal powder, and can reduce waste of the precious metal powder in the target manufacturing process, thereby improving the quality of the target and reducing the target. Manufacturing cost of materials. Embodiments I31536.doc 201000651 FIG. 1 is a machine view showing a manufacturing method of a metal-based ceramic composite target containing noble metal according to the present invention, and FIG. 2 is a partially enlarged schematic view showing a metal-based ceramic composite: dry material of the noble metal according to the present invention. . Among them, the method for producing a metal-based ceramic composite containing a noble metal can be applied to a ruthenium film extruding process in the magnetic recording industry, the photovoltaic industry or the semiconductor industry. Referring to FIG. 1 and FIG. 2, first, referring to step S11, magnetic metal powder 11 and ceramic powder 12 are provided, and the purity of b, etc., is preferably greater than 99.9%. In the present embodiment f, the purity of the magnetic metal powder 11 and the ceramic powder 12 is greater than 99.95%. Among them, the magnetic metal powder u can be a wire or a chrome alloy. In the present embodiment, the ceramic powder body 12 is made of cerium oxide (Si 〇 2) or a titanium nitride (Ti 〇 2). The particle size of the ceramic powder 12 is preferably 〇.07 to 1. 〇micron (μιη). Referring to step S12, the ceramic powder 12 and the magnetic metal powder are wet-mixed in a solvent (for example, water or alcohol) to form a slurry, wherein the ceramic powder 12 is coated on the slurry. The surface of the magnetic metal powder crucible. In step S12, the surface of the 6-well magnetic metal powder 11 and the surface of the ceramic powder 12 have different electrical charges, so that the ceramic powder 12 is coated on the surface of the magnetic metal powder 11. Preferably, the mixing time of the wet mixed powder is 6 to 24 hours. It is noted that, according to different mixed materials and mixing conditions, in step S12, another The step of adjusting the pH value is performed by adding an acid or alkali solution to adjust the pH of the slurry so that the surface of the magnetic metal powder and the surface of the ceramic powder 12 have different electrical charges. Drying the slurry to form a ceramic gold composite powder. In the present embodiment, in the present embodiment, the slurry is dried by a vacuum drying method, wherein the vacuum drying temperature is 2, and the vacuum drying time is 2 to The vacuum degree of vacuum drying for 6 hours is less than 760 Torr (t〇rr). The mixed powder of the pottery gold composite powder and the noble metal powder 13 is dry-mixed with reference to step S14'. The purity of the noble metal powder 丨3 is greater than 99· 9% ^ In the present embodiment, the precious metal powder 13 Platinum (Pt) is used, and the purity thereof is greater than 99.95% 'and the mixing time of the dry mixed powder is preferably 4 to 8 hours. Referring to step S15, the ceramic gold composite powder after molding and densification mixing and The precious metal powder 13' is formed to form the metal-based ceramic retanning material 1 containing the noble metal of the present invention. In the present embodiment, the hot isostatic pressing process or the hot isostatic pressing process is performed. The forming and densification step, wherein the temperature for forming and densification is 8 〇 (rc to 12 〇〇t, and the molding and densification time is 1 to 4 hours. Preferably, the weight of the ceramic powder 12 is The percentage is 5% to 12%, and the weight percentage of the shell metal powder 13 is 2% to 5%, and the remaining weight percentage is the content of the magnetic metal powder 11. In the present embodiment, the magnetic metal The powder 11 is a cobalt chromium alloy, wherein the weight percentage of the ceramic powder 12 is 5% to 12%, and the weight percentage of the precious metal powder 13 is 2% to 50%, and the weight percentage of the chromium of the cobalt chromium alloy It is 4% to 16%, and the remaining weight percentage is the diamond of the starting chrome alloy. The present invention will be described in detail by the following examples, which are not intended to be construed as limited only by the examples. Example 1: This example is chrome-platinum-cerium oxide (C〇CrPt_si〇2) Alloy sputter target 131536.doc 201000651 The production of the material is taken as an example. Firstly, 'provide a cobalt (C〇) powder with a purity of up to 99.95% and with magnetic wow, and provide chromium (Cr) ruthenium platinum with a purity of up to 99.95% or more. (Pt) powder, cerium oxide (Si〇2) powder (particle size 0.25 μιη). Wherein the content of cobalt is 46% by weight (46% of the chromium content is 5 Wt%, the content of platinum is 42% by weight, and the content of cerium oxide is 7
Wt/〇接著，將Co粉、Cr粉及Si〇2粉體放入pH值為7之去 離水中進仃濕式混粉i 8小時。接著，將c〇Cr_si〇2漿體放 入一真空烘箱中，在真空度為76 t〇rr中進行真空乾燥步 驟，其中，乾燥溫度係為12〇它，乾燥時間為4小時，即可 將Si〇2粉體均勻地被覆在c〇粉及Cr粉的表面上。最後，取 乾燥後之CoCr-Si〇2粉體，與Pt粉體以不加溶劑之乾式混 粉方式充分混合4小時之後，將混合均勻的粉體放入—石 墨模具中，以熱壓方式，在n〇(rc、持溫15小時之條件 下，將混合粉體壓成靶材形狀並將靶材緻密化之後，即製 得问純度、組織細緻、成分均勻之c〇CrPt_Si〇2靶材。 實例2 : 本實例係以鈷鉻鉑-二氧化鈦（c〇CrPt_Ti〇2)合金濺鍍靶 材的製作為例。首先，提供純度高達99.95%以上具有磁性 之鈷（C〇)粉，以及提供純度亦高達99.95%以上之鉻（Cr) 卷、鉑（Pt)粉、以及二氧化鈦（Ti〇2)粉（粒徑〇 〇7 。其 中，鈷的含量為48 wt%，鉻的含量為13 wt%，鉑的含量為 3 1 Wt% ’二氧化鈦的含量為8 wt%。接著，將c〇粉、Cr粉 與Ti〇2粉體放入去離水中，且以氨水調整溶液之pH值為$ 之後，進行濕式混粉12小時。接著，將CoCr-Ti〇2漿體放 131536.doc •10- 201000651 入真空烘粕中，在真空度為76 torr中進行真空乾燥步 驟，其中，乾燥溫度係為1601，乾燥時間為2小時，即可 將Τι〇2粉體均勻地被覆在c〇粉及cr粉的表面上。最後，取 乾燥後的CoCr-Ti〇2粉體，與Pt粉體以不加溶劑之乾式混 粉方式充分混合6小時之後，將混合均勻的粉體以不鏽鋼 封罐（canning)之後，以熱均壓方式在8〇〇<t、持溫4小時的 條件下，將粉體壓成靶材形狀並將靶材緻密化之後，即可 製得尚純度、組織細緻、成分均勻之c〇CrPt_Ti〇2靶材。 本發明之製造方法係先利用濕式混粉製程，將該陶瓷粉 體均勻地被覆於該磁性金屬粉體之表面，並經由乾燥製程 後，取得該陶金複合粉體，再利用乾式混粉製程將該貴金 屬粉體與該陶金粉體均勻混合，最後利用成型及緻密化製 程將該陶金複合粉體製成緻密之靶材。本發明之製造方法 可均句地混合該磁性金屬粉體、該陶瓷粉體及該貴金屬粉 體，並且可減少靶材製作過程中該貴金屬粉體的浪費，故 可改善靶材之品質及降低靶材之製造成本。 上述實施例僅為說明本發明之原理及其功效，並非限制 本發明。因此習於此技術之人士對上述實施例進行修改及 變化仍不脫本發明之精神。本發明之權利範圍應如後述之 申請專利範圍所列。 【圖式簡單說明】 圖1顯示本發明含貴金屬之金屬基陶瓷複合靶材之製造 方法之流程圖；及 圖2顯示本發明含貴金屬之金屬基陶瓷複合靶材之局部 131536.doc 201000651 放大示意圖。 【主要元件符號說明】 I 本發明含貴金屬之金屬基陶瓷複合靶材 II 磁性金屬粉體 12 陶瓷粉體 13 貴金屬粉體 131536.doc -12-Wt/〇 Next, the Co powder, the Cr powder and the Si〇2 powder were placed in a pH value of 7 to be immersed in the water for 8 hours. Next, the c〇Cr_si〇2 slurry is placed in a vacuum oven, and a vacuum drying step is performed in a vacuum degree of 76 t〇rr, wherein the drying temperature is 12 Torr, and the drying time is 4 hours. The Si〇2 powder was uniformly coated on the surfaces of the c powder and the Cr powder. Finally, the dried CoCr-Si〇2 powder is mixed with the Pt powder in a dry mixing manner without solvent addition for 4 hours, and then the uniformly mixed powder is placed in a graphite mold by hot pressing. After n 〇 (rc, holding temperature for 15 hours, the mixed powder is pressed into the shape of the target and the target is densified, then the c〇CrPt_Si〇2 target with purity, fine structure and uniform composition is obtained. Example 2: This example is based on the preparation of a cobalt-chromium-platinum-titanium dioxide (c〇CrPt_Ti〇2) alloy sputtering target. First, a cobalt (C〇) powder having a purity of up to 99.95% or more is provided. Providing chromium (Cr) rolls, platinum (Pt) powders, and titanium dioxide (Ti〇2) powders having a purity of up to 99.95% or more (particle size 〇〇7, wherein the cobalt content is 48 wt%, and the chromium content is 13 Wt%, the content of platinum is 3 1 Wt% 'the content of titanium dioxide is 8 wt%. Then, the powder of c〇 powder, Cr powder and Ti〇2 is placed in the deionized water, and the pH of the solution is adjusted with ammonia water. After that, wet mixing is carried out for 12 hours. Then, the CoCr-Ti〇2 slurry is placed in a vacuum of 131536.doc •10- 201000651 In the drying process, a vacuum drying step is performed in a vacuum degree of 76 torr, wherein the drying temperature is 1601 and the drying time is 2 hours, and the Τι〇2 powder can be uniformly coated on the surface of the c powder and the cr powder. Finally, the dried CoCr-Ti〇2 powder is taken and thoroughly mixed with the Pt powder in a dry mixing manner without solvent, and after the mixed powder is canned with stainless steel, Under the condition of 8 〇〇<t and holding temperature for 4 hours, the powder is pressed into the shape of the target and the target is densified, then the purity, fine structure and uniform composition can be obtained. c〇CrPt_Ti〇2 target. The manufacturing method of the present invention firstly uses the wet mixing process to uniformly coat the ceramic powder on the surface of the magnetic metal powder, and after the drying process, the ceramic gold composite is obtained. The powder is uniformly mixed with the pottery powder by a dry mixing process, and finally the pottery gold composite powder is made into a dense target by a molding and densification process. The manufacturing method of the present invention can be Mixing the magnetic metal powder uniformly The ceramic powder and the precious metal powder can reduce the waste of the precious metal powder in the target manufacturing process, thereby improving the quality of the target and reducing the manufacturing cost of the target. The above embodiments are merely illustrative of the principle of the present invention. The present invention is not limited to the scope of the invention, and the scope of the invention should be as defined in the appended claims. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a flow chart showing a method for producing a metal-based ceramic composite target containing noble metal according to the present invention; and Fig. 2 is a schematic enlarged view showing a portion of a metal-based ceramic composite target containing precious metal of the present invention, 131536.doc 201000651. [Description of main component symbols] I Metal composite ceramic composite target containing precious metal II Magnetic metal powder 12 Ceramic powder 13 Precious metal powder 131536.doc -12-