1320805 九、發明說明： 【發明所屬之技術領域】 本發明係一種濺鍍靶材、其表面處理方法及其製成之 薄膜’尤其是一種以去除表面之陶瓷相碎屑的表面處理方 法處理過的濺鍍靶材及其所濺鍍而成的薄膜。 【先前技術】 身又製作垂直磁性紀錄（perpendicuiar recording’ PMR)薄膜的靶材係含有絕緣之氧化物陶瓷相 (〇X1de ceramic phase)，因此該靶材在濺鍍過程中可能 產生區域性電弧（arc)放電，而導致陶瓷相顆粒濺散至基 材（如碟片）表面，由於濺鍍於基材表面的鍍膜僅有數奈米 的厚度，因此若濺散至基材表面的陶曼相顆粒具有大於鍍 臈厚度的粒徑，則該基材表面就會有突起的情形，故該基 材後續還需經過整平步驟以將突起之陶究相顆粒清除，但 在此同時’ 4基材表面會留下坑洞狀的缺陷（㈣如），因 而降低基材品質，由上W去 酿丨 了头 顆粒濺散的情形越少，則基 材品質就可以提升’但顆粒濺散的程度取決於垂直紀錄乾 材，因此顆粒賤散的程度就成為衡量垂直紀錄㈣品質的 重要關鍵。 該=錄乾材會在滅鑛過程中有陶究相顆 情形，係因為-般乾材（如c〇_Cr_pt_ 性的合金相以及具脆性的陶究相，因此在該乾材二展 刀具或磨輪會將該陶竟相擊碎，該被擊碎的陶-(一會鎮入合金相裡’成為錢鍵過程中陶究相顆粒的 1320805 • 主要來源。 有鑑於此，許多人針對靶材做了不同的表面處理，例 .如美國發明專利第5464520號之專利案中提到的表面處理 方式係包括離子研磨（i〇n miller)、電解拋光（electr〇_ P〇】ishing)、化學敍刻（chemical etching)、研磨（iapping) 及化學研磨（chemical pol ishing)，然而，此專利主要目 的係在於除去靶材表面的變形層（deformed layer)，因此 在說明書中並無提及去除鑲埋之陶瓷相碎屑。 • 而在美國發明專利第6024852號之專利案中針對靶材 之表面進行鏡面處理（mirr〇r treatment)，使其表面粗糙 度（Ra)小於〇. 01 # m，以減少濺鍍過程中顆粒的濺散，然 而，此專利案的標的物係不會產生陶瓷相碎屑的鈦金屬或 鈦合金靶材，因此仍然無法解決其他材質之靶材產生陶瓷 相碎屑的問題》 至於美國發明專利第6030514號之專利案中提及對靶 材進行表面處理，其係包括離子研磨（i〇n mi丨ler)、電解 ♦拋光（electro-polishing)、化學蝕刻（chemical etching)、化學研磨（chemical p〇Ushing)、雷射或電子 束剝離（laser or electron beam ablation)及機械或化 學機械研磨（mechanical or chemo-mechanical ' polishing)，該表面處理完成後再將該靶材表面用金屬包 . 覆（metal encl〇sure)的方式予以保護，以減少濺鍍時預 燒（burn-in)所需的時間’然而，該專利案所提及的處理 過程繁複，而且需要額外的金屬包覆靶材，因而提高靶材 1320805 成本，故不符合經濟效益。 ,而美國發明專利第61 153315號之專利案係對靶材進 :精密加工以降低變形層之厚度，而後再利用化學腐蝕法 完全去除變形層，&而’此處理過程繁複，而且並無針對 鑲埋之陶瓷相碎屑進行處理。1320805 IX. Description of the Invention: [Technical Field] The present invention relates to a sputtering target, a surface treatment method thereof and a film produced thereof, in particular, a surface treatment method for removing ceramic phase debris from a surface The sputter target and its sputtered film. [Prior Art] A target that produces a perpendicular magnetic recording (PMR) film contains an insulating ceramic phase (,X1de ceramic phase), so that the target may generate a regional arc during sputtering ( Arc) discharge, which causes the ceramic phase particles to splash onto the surface of the substrate (such as a disc). Since the coating on the surface of the substrate is only a few nanometers thick, if the ceramic particles are splashed to the surface of the substrate, If the particle diameter is larger than the thickness of the rhodium plated, the surface of the substrate may have protrusions, so the substrate needs to be subjected to a leveling step to remove the particles of the protrusions, but at the same time '4 substrate The surface will leave a pit-like defect ((4)), thus reducing the quality of the substrate. The less the spattering of the head particles by the W, the better the quality of the substrate can be improved. Depending on the vertical record of dry materials, the degree of particle scatter is an important factor in measuring the quality of the vertical record (4). The = dry material will have a ceramics in the process of demineralization, because the dry material (such as c〇_Cr_pt_ alloy phase and brittle ceramic phase, so the dry material two tools Or the grinding wheel will crush the pottery, the crushed pottery - (in the case of the town into the alloy phase - becomes the 1320805 of the ceramic particles in the process of the money key. • The main source. In view of this, many people target The surface treatment methods mentioned in the patent application No. 5444520 of the invention include ion milling (i〇n miller), electrolytic polishing (electr〇_P〇]ishing), Chemical etching, imaging, and chemical polishing. However, the main purpose of this patent is to remove the deformed layer on the surface of the target, so there is no mention in the specification. Inlaid ceramic phase crumbs. • In the U.S. Patent No. 6024852, the surface of the target is mirror treated to have a surface roughness (Ra) less than 〇. 01 # m To reduce the sputtering process Spattering of particles, however, the subject matter of this patent does not produce titanium or titanium alloy targets with ceramic phase debris, so it still cannot solve the problem of ceramic phase debris generated by targets of other materials. Patent No. 6030514 refers to the surface treatment of a target, which includes ion milling, electro-polishing, chemical etching, chemical polishing ( Chemical p〇Ushing), laser or electron beam ablation and mechanical or chemo-mechanical ' polishing. After the surface treatment is completed, the target surface is covered with metal. The metal encl〇sure is protected to reduce the time required for burn-in during sputtering. However, the process mentioned in this patent is complicated and requires additional metal coated targets. The material, thus increasing the cost of the target 1320805, is not economical. The patent of the US Patent No. 61 153315 relates to the target: precision machining to reduce deformation The thickness and then completely removed by chemical etching deformable layer, & the 'process of this complex, and not processed for burying clastic ceramic insert.
於美國發明專利第62841 !!號之專利案中，該案發明 人針對靶材表面進行處理’以完全除去加工應變層，並經 過長時間的化予腐使靶材表面的粗糙度(邮，似 roughness)介於靶材之平均晶粒的〇1%〜1〇%之間然而該 專利與前-個專利案一#，其處理過程繁複，而且並無針 對鑲埋之陶竞相碎屑進行處理。 另外，有人針對具備不同脆性相之賤鑛乾材表面進行 ，理’以減少其表面缺陷，其方法係利用切削加工進行一 次加工，將該賤鑛乾材切削―至1〇_，接著利用.剛 之粗磨粒砂紙或磨石研磨進行精加工，藉由精加：L除去以 不：延性之物質所在之處為起點而形成的缺陷，如龜裂、 脫洛所致之凹陷等’以使㈣表面呈現平滑狀1而此處 理過程並無針對鑲埋之陶究相碎屬進理 究相判並非以其不且延性物質所在鑲埋之陶 卜八、r玍物質所在之處為起點，因此精 加工並不能去除陶瓷相碎屑。 綜上所述，這些專利案中所提及的乾材表面處理方式 過程繁複’而且並無針對鑲埋之陶究碎屑進行處理，因此， 如何在簡單的表面處理過程中將鑲埋之陶究碎屑去除以提 尚賤鍍輕材及薄膜品質，係目„界研究的課題。 本發明濺鍍靶材之表面處理 表面以研磨器具由粗到細進行多道研磨其係於濺鍍靶材的 本發明之賤餘材係將該φ 粗到細進行多道研磨，俾使 1益/、由 0.07//m。 人面的粗糙度（Ra)小於 公具係可為砂紙、砂布、砂輪、研磨機^ 上述之夕道研磨的實施例係期砂紙進行以下步驟： 1·以120號(一平方英时有12〇顆砂療，以下 的砂紙於濺鍍靶材表面研磨2_5分鐘. 2.續以400號砂紙於濺鍍靶材表面研磨 3·再以1 000號砂紙於濺鍍靶材表面研磨 4.將乾材表面以清水沖洗； 2 - 5分鐘； 2-5分鐘 5·:以高壓空氣(3〜10kg/cin2)將靶材表面吹乾，即 可完成無陶瓷相碎屑之高品質靶材。 上述以砂紙進行研磨的實施例，在步冑丨與步驟2之 間尚可包含以240號的砂紙於濺鍍靶材表面研磨2_5分 鐘，並在步驟2與步驟3之間將濺鍍靶材表面以_號砂 紙研磨2 - 5分鐘。 請參看第一圖所示，其係利用掃描式電子顯微鏡 (scanning electronic micr〇sc〇py，SEM)觀察以磨床或 車床加工完成後的靶材表面金相圖，此時之表面粗糙度（Ra) 一般大於3#m，由於經過研磨加工後的表面具有塑性變形 層存在’其會將陶瓷相碎屑遮蓋，故會有陶瓷相碎屑完全 鑲埋於靶材内，此陶瓷相碎屑無法用化學腐蝕法（如以稀 1320805 釋的氫氟酸（di lute HF)為溶劑）完全去除，而圖中的黑色 暗點以能量散射光譜儀（Energy Dispersive Spectrograph， EDS)檢驗後證實是陶瓷相的成分。 請參看第二圖所示，其係將靶材依序藉由12〇、24〇、 40 0、800及1〇〇〇號的砂紙各研磨2至5分鐘，復以超音 波震盪器藉由清水洗滌，並以高壓空氣吹乾後，最後，以 SEM檢驗其表面所得到的結果，發現該靶材表面的金相已 經改變，且靶材上的陶瓷相碎屑已徹底被去除，此時之表 面粗糙度（Ra)—般小於0. 〇7// m。 藉由研磨器具在減鍍乾材的表面進行粗研磨至細研磨 ^精研磨）之夕道研磨，且該研磨器具的磨粒粒徑（如砂紙 系號數越小越粗）及研磨次數係依陶瓷相碎屑鑲嵌於濺鍍 靶材表面的深度與尺寸而改變，因此可將鑲嵌於靶材表面 處的陶究相碎屑徹底清除，以達到本發明的目的。 【圖式簡單說明】 第—圖係以掃描式電子顯微鏡觀察經過磨床或車床加 工後的濺鍍靶材表面金相圖。 第一圖係以掃描式電子顯微鏡觀察將第一圖之濺鍍靶 材表面經過本發明之方法處理後的表面金相圖。 【主要元件符號說明】 無 10In the patent of US Patent No. 62841!!, the inventor of the case processed the surface of the target to completely remove the strained layer of the process, and after a long period of time, the surface of the target was roughened (post, Roughness) Between 1% and 1% of the average grain size of the target. However, the patent and the previous patent case # are complicated in processing and are not used for the embedded ceramics. deal with. In addition, some people have carried out the surface of the dry ore material with different brittle phases, so as to reduce the surface defects. The method is to use the cutting process for one-time processing, and the dry material of the antimony ore is cut to -1〇, and then utilized. Just coarse-grain sandpaper or grindstone grinding for finishing, by adding: L removes defects such as cracks, delamination caused by cracking, etc. (4) The surface is smooth and 1 and the process is not related to the inlaid ceramics. The reason is not based on the location of the inlaid Tao Bu Ba and r玍 substances in which the ductile material is located. Therefore, finishing does not remove ceramic phase debris. In summary, the dry surface treatment methods mentioned in these patent cases are complicated and there is no treatment for the embedded ceramic chips, so how to embed the pottery in a simple surface treatment process. Scrap removal to improve the quality of enamel plating and film quality, the subject of research. The surface treatment surface of the sputtering target of the present invention is multi-pass grinding from coarse to fine by grinding tools. The remaining material of the present invention is a plurality of grindings of the φ coarse to fine, and the yttrium is made to be 1//, and is 0.07//m. The roughness of the human surface (Ra) is smaller than that of the public system, and may be sandpaper, emery cloth, Grinding wheel, grinder ^ Example of the above-mentioned evening grinding The following steps are carried out on the sandpaper: 1. With 120 gauges (12 square inches of sand in one square inch, the following sandpaper is ground on the surface of the sputtering target for 2_5 minutes. 2. Continue grinding the surface of the sputter target with 400 grit sandpaper. 3. Grind the surface of the sputter target with 1000 grit sandpaper. 4. Rinse the surface of the dry material with water; 2 - 5 minutes; 2-5 minutes 5. : Drying the surface of the target with high-pressure air (3~10kg/cin2) to complete the non-ceramic phase debris The high-quality target. The above-mentioned embodiment of grinding with sandpaper may further include grinding the surface of the sputtering target with a No. 240 sandpaper for 2 to 5 minutes between the step and the step 2, and between the steps 2 and 3. The surface of the sputter target is ground for 2 - 5 minutes with _ sandpaper. Please refer to the first figure, which is observed by scanning electron microscopy (SEM) after grinding or lathe processing. The metallographic map of the target surface, the surface roughness (Ra) is generally greater than 3 #m, since the surface after the grinding process has a plastic deformation layer, which will cover the ceramic phase debris, so there will be a ceramic phase. The debris is completely embedded in the target, and the ceramic phase debris cannot be completely removed by chemical etching (such as di lute HF released as dilute 1320805), while the black dark spots in the figure are energy. After the Energy Dispersive Spectrograph (EDS) test, it is confirmed to be the composition of the ceramic phase. Please refer to the second figure, which is to sequentially target the target by 12〇, 24〇, 40 0, 800 and 1〇〇〇. Grinding sandpaper for 2 to 5 minutes, complex After the ultrasonic oscillator was washed with water and dried with high-pressure air, and finally, the surface of the target was examined by SEM, and the metal phase of the target was changed, and the ceramic phase on the target was detrived. Has been completely removed, at this time the surface roughness (Ra) is generally less than 0. 〇7 / / m. By grinding the surface of the dry plating dry material to coarse grinding to fine grinding ^ fine grinding) And the abrasive grain size of the grinding tool (such as the smaller the sandpaper number is, the coarser) and the number of grindings are changed according to the depth and size of the ceramic phase debris embedded in the surface of the sputtering target, so that the target can be mounted on the target The crumbs at the surface of the material are thoroughly removed to achieve the object of the present invention. [Simple description of the diagram] The first-graph is a scanning electron microscope to observe the metallographic diagram of the surface of the sputtering target after grinding or lathe processing. The first figure is a surface metallographic diagram of the surface of the sputter target of the first graph after being treated by the method of the present invention by a scanning electron microscope. [Main component symbol description] None 10