1373387 18812pifl 修正日期101年6月13曰 爲第94143995號中文說明書無劃線修正本 六、發明說明： 【發明所屬之技術領域】 本發明係關於一種用以製造使用於濺鍍用靶材等高 融點金屬類燒結體之高融點金屬類粉末的製造方法以及乾 材的製造方法。 【先前技術】 如今，於液晶顯示器（Liquid Crystal Display，以下 稱為LCD)等平面顯示裝置之薄膜電極以及薄膜佈線等 中，使用電阻較小之鉬(Mo)等高融點金屬膜，作為用以形 成該金屬薄膜之材料，廣泛用於濺鍍用把材。而且，近年 來，伴隨平面顯示裝置市場之急劇擴大，含有M〇之高融 點金屬之需要亦日益激增，用以製造靶材之燒結用原料粉 末供給日漸不足。 於上述狀況下，如今研究有再利用廢舊靶材之方法。 例如，k議有如下方法：將廢舊乾材溶化於溶液中並使之 化學性分離而再生為金屬粉末之化學性濕式分離方法，或 藉由電子束溶解而進行精煉製作高純度化之鑄錠之方法， 然而化學性方法存在有成本較高之問題，又，於藉由電子 束熔煉而製作溶解鑄錠之方法中，存在有由於鑄錠較難進 行加工而難以應用於產業上之問題。此外，亦提議有將廢 舊靶材粉碎，並使所獲得之粉末通過熱電漿，使之球狀化 以及南純度化製成微粉末之粉末原料之製作方法(例如，參 照曰本專利特開2001 —342506號公報）。 [發明所欲解決之問題] 1373387 lg812pifl 修正日期101年6月13日 ，爲第941侧5號中文說明書無 上述日本專利特開2°G1-3425。6號公報，認為可藉 由將經過機械性粉碎之純度較低的粉末導人至熱電漿中， 而實現高融點金屬或責金屬粉末之球狀化、低氧化以及高 純度化4一其中存在有由於是使用熱電敷裝置，故而於製 造來自廢舊耙材之粉末時，會導致絲變高之問題。 【發明内容】 本發明之目的在於提供一種可無需利用藉由化學方 法^熱電聚進行溶融精煉之所謂高成本方法，而易於自廢 舊尚融點金屬_材，低成本且穩定地製造高融點金屬類 粉末之方法。 本發明者們對自廢舊高融點金屬類靶材製造高融點 金屬類粉末之方法進行各種研究之結果發現，通過切割而 將廢舊乾材製成切削屑，藉此將微裂縫導入切削屑内部由 此提高粉碎性，並且組合將於切割或粉碎時所導入之氧等 雜質除去之熱處理，藉此可製造含有與廢舊高融點金屬類 靶材同等位準純度之高融點金屬類粉末，故而實現本發明。 即’本發明提供一種高融點金屬類粉末的製造方法， 其將廢舊高融點金屬類靶材，進行切割處理而製成切削 屑’並於對切削屑實施粉碎處理而製成微粉末後，進而於 還原性氣體環境中實施熱處理。 又，本發明提供一種高融點金屬類粉末之製造方法， 其將廢舊高融點金屬類靶材’進行切割處理而製成切削 屑，並於還原性氣體環境中對該切削屑實施熱處理後，進 而實施粉碎處理而製成微粉末。 5 I8812pifl 爲第_95號中文說明書無劃線修正本 修正日期⑼年6月13日 又，本發明之高融點金屬類粉末的製造方法，較好 是上述切割處理是使用切割機。 的 又，本發明之高融點金屬類粉末的製造方法，較好 是上述切削屑之粉碎處理是衝擊粉碎處理。 、 又，本發明之高融點金屬類粉末的製造方法，較好 是上述在還原性氣體環境中實施之熱處理是在含氫的 環境下進行的。 〃 又，本發明之高融點金屬類粉末的製造方法，較好的 是上述在還原性氣體環境中實施之熱處理是在小於等於 100 Pa之減壓氣體環境下進行的。 ' 又，本發明之高融點金屬類粉末的製造方法，較好的 是藉由上述粉碎處理而製成之微粉末的平均粒徑是介於 至 1000 μιη 之間。 、 又，本發明之高融點金屬類粉末的製造方法，較好的 是高融點金屬為純銷(Mo)。 又，本發明提供一種靶材的製造方法，其將以上述製 邊方法而獲得之高融點金屬類粉末，進行燒結。 可藉由本發明，而易於自廢舊高融點金屬類靶材，低 成本且穩定地製造高融點金屬類粉末，故可低成本且穩定 地製造高融點金屬類靶材，因而於產業上具有較高之利用 價值。 為讓本發明之上述和其他目的、特徵和優點能更明顯 易懂，下文特舉較佳實施例，並配合所附圖式，作詳細說 明如下。 1373387 18812pifl 修正日期101年6月13日 爲第94143995號中文說明書無劃線修正本 【實施方式】 本發明最重要之特徵在於發現有如下方面：將廢舊高 融點金屬類耙材之塊體切割為固定形狀，並製作使金屬組 織内部產生微裂縫之切削屑，藉此可易於藉由粉碎而使之 微粉末化。 一般而言，於高融點金屬類靶材之製造中，由於溶解 溫度較高，故而難以使用溶解鑄造法來進行製造，而是利 用將原料粉末加以燒結而製成塊體之粉末燒結法來進行製 造。因此，為再生廢舊靶材，而必須對可成為燒結用原料 之粉末進行加工。 根據本發明者們之研究，發現有若自作為於室溫下幾 乎無延展性之組成類之高融點金屬類材料，藉由切割處理 而強制性賦予其機械性應力並製作切削屑，則可將微裂縫 局部性導入切削屑。自該情形可推測出，於室溫下缺乏延 展性之組成類中，藉由切割而短時間強制性賦予應力，故 而超出其本來之延展性’因此將產生局雜微裂縫。而且， 因導入^切削屑之局部性微裂縫的存在，而可易於自難以 粉碎之尚密度高融點金屬類塊體獲得微粉末。 又，至於在室溫下幾乎毫無延展性之高融點金屬類之 代表例，尤其可列舉，鉻(Cr)、鉬(M〇)、鶴(w)之金屬組成 以及於Cr、Mo、W中且於小於等於5〇%範圍中包含有合 金兀素之成分組成。therm〇_lester之延展性測試中，例如 Mo直至15 G C附近為止並未顯示出延展性，進而融點更高 之W若未達到M〇以上之高溫亦未顯示出延展性等，故可 7 1373387 I8812pifl 修正曰期101年6月13曰 爲第94143995號中文說明書無劃線修正本 認為該等組成幾乎毫無延展性，而，考慮到易於產生由 切割而導入微裂縫，故而該等成分組成可較好適合於使用 本發明之製造方法製作粉末。 以下，就本發明之向融點金屬類粉末的製造方法按 照順序加以說明。 於本發明中’首先，對廢舊高融點金屬類輕材進行切 割處理而製作切則。藉由切割處理製作切綱之原因在 於，如上所述，可將微裂縫導入切削屑由此提高粉碎性。 本發明者們，於分析藉由切割而製作之切削屑與切削 屬中微裂縫之產生的相關關係後，發現若使切削屑厚度超 過2 mm左右則於切削屑之兩端存在有微裂縫，但是㈣ 存在並未貫通其;m自中㈣縫出現關形成—體化之 傾向，故而難以進行其後之粉碎。進而，於藉由切割 進行切割時，由於__力變缝輯於設備方面亦較 又，若使切顧之厚度未滿3G_則可充分將微 裂缝導入至_射，但有時可㈣現製作切則之效率 較低’而且成為⑽導致粉碎性下降。因此，較好 慮到切則之粉碎性，而使切削屑之厚度為3〇卿至2 _ 左右。 又，於進行切割時，可使用藉由車床，鑽孔器 ί等之切削而可獲取切則者。較好的是，藉由切割^ 传切削屑’並且藉由廢舊高融點金屬類崎之組成，而、= 當設定所使用之設備物#j之條件H於 ^ 器、切割射最好較切戰。其原因在於，、若藉由3 188l2pifl 修正日期101年6月13日 爲第94143995號中文說明書無劃線修正本 機’則-般而言可將作為平板狀且形錄大之被切削物之 廢舊乾材加以固定且可以較高生產效率實施切削。 其次，將所獲得之切削屑進行粉碎處理而製成微粉 末。於切削屑内部可藉由切割處理而局部性導入微裂縫， 故而較直接使塊體成為微粉末，更$於實施微粉末化。 至於切削屑之粉碎方法，並未做特別限定，可利用球 磨機’振動磨碎機，顎式粉碎機，衝擊式粉碎機，錘磨機， 衝擊式粉碎機等，但較好的是可使所獲得之微粉末的平均 粒徑為20至1000 μιη之方法。 再，，於粉碎處理中，必須極力避免雜質之混入同時 慮批量生產性。於以因球磨機，振動磨碎機等所產生之 ^擦力為絲力讀碎處理之方法，存在有超微細粉末變 付較多’粒度難以控制，而且微粉末易於氧化之傾向。又， 亦存在如下傾向，由於使用罐裝故而不利於批量生產，進 :由於污染將導致雜質增多。又，存在如下傾向，以滾筒 粉碎機等之1縮力’剪力為主應力⑽碎處理方法，或組 合^擦力之粉碎處理方法，转在有因與粉碎工具接觸 而此入有雜質絲度難以控φ卜因此，最可行的是，藉由 ^可更好抑制與粉碎工具或内殼之接觸之錘磨機或 粉碎機等的衝擊力融應力的衝擊粉碎而實施粉碎 又’使㈣賴或衝擊式粉碎機，由於 =粉碎原料之切則故於批量生產之效果方面來看車1= 進而’於還原性氣體環境巾對切朗或微粉末實施熱 1373387 2 〇 遛‘3_中文說明書無劃賺正本 修正_〇1年6月13日 處理。該熱處理於進行切割處理或粉碎處理中，對於將所 導入之氧降低至與廢舊高融點金屬類靶材同等位準 為止十分必要。 ^ 再者’較可行的是降低該氧之熱處理，根據切削屬或 微粉末之成分組成而設定適當條件。例如，較可行的是合 成分組成為Mo或W等之情形時，設為導入有作為還】二 介具有優良效果之氫的還原性氣體環境。又，於鈮(Nb)、' 欽(Ti)等具有吸附氫之傾向故設為導入有氫之氣體環境較 為不可行之MoTi合金或MoNb合金等情形時，較好的是 於小於等於100 Pa之減壓氣體環境下藉由還原作用而降低 氧之方法。雖然亦取決附著於切削屑或微粉末表面之氧含 量，但確保一般性迴轉式幫浦之吸引力者即可有效將氧除 去。 、 又，至於還原性氣體環境下進行熱處理之溫度條件， 雖因切削屑或微粉末之成分組成存在有若干差異，但較可 行的是大概設為500至1500°C。其原因在於，若為50(rc： 以下則降低氧之效果極小，而另一方面，若超過則 經過粉碎之高融點金屬類粉末彼此之接觸部分將開始擴散 結合，故而難以進行再次粉碎。又，更好的溫度條件是6〇〇 至1300°c，尤其好的是800至1200。(：。 又，於還原性氣體環境中對微粉末實施熱處理之情形 時，根據溫度條件，有時微粉末彼此會輕微結合，故而可 於實施熱處理後將出現結合之微粉末解體而製成微粉末， 或亦可進而以低於解體前之熱處理溫度之溫度對該微粉末 10 1373387 mi2pifl 修正曰期101年6月13日 爲第94143995號中文說明書無 實施熱處理而降低氧。 β又’於根據本發明所製作之高融點金屬類粉末用作加 歷燒結用之原料粉末之情形時，考慮到對加塵容器之填充 性或生產效率’則較可行的是平均粒徑為20至1〇〇〇 μηι。 因在於’若使粒徑為平均粒徑不足20 μηι則有時難以 &向對力器之填充密度’故而難以有效實施粉碎處理 直至上述平均粒徑下降至2〇μιη為止。又，其原因在於， 於含有平均粒徑超過_μιη之粗祕末之情形時，由於 粉末間之顯現象叫致無法提高填充密度。 "又於切割廢售向融點金屬類乾材時，為除去附著於 刀削屑之碳、t、氫等雜質，而較可行的是附加清洗切削 屑之工序。 ▲至於該清洗工序，可利用贼以上之熱水、丙_、乙 ，等但考慮到*全性與進—步促進除去上述雜質，較可 打的是於實施溫水清洗後，使用驗紅#用之水溶性清潔 劑及純水加以漂淨之方法。 再者，於進行切割時，有時考慮到作紐效率而使用 切=油，但於該情形時為除去切削油，較可行的是使用烴 青洗切削屬。至於烴系溶劑’考慮到環境方面或火 =暴X之風險，較好的是使用石堰系或環烧系「第3石油 類」。 右盘^根據本發明而獲得之高融點金屬類粉末，由於具 金屬嶋同等位準之純度，故而藉由將 齡末燒結Μ於獲得純度較高之妹，故而 188l2pifl 修正日期101年6月13日 爲第94143995號中文說明書無劃線修正本 製造方法較為合適。 [實施例1] 以下就本發明之實施例加以說明。 一面塗布切削油一面藉由使用有超硬WC製晶片之切 割機，對廢舊Mo靶材實施切割處理，獲取厚度約5〇 μιη 之切削屑。於圖1中模式性表示有該Μ〇切削屑之外觀之 圖，於圖2中表示有光學顯微鏡所觀察之微組織寫真之 圖。自圖2可獲悉，沿者經過切割之Μ〇切削屑之粒界存 有微裂縫。 其後，藉由離心分離機而除去附著於所獲取之M〇切 削屑之切削油，並使之浸潰於烴系溶劑中，同時使用搖動 或，聲，將其清洗並使之乾燥。再者，於藉由油分濃度計 測里附著於該Mo切削屑之油分後，發現清洗乾燥後之油 分為小於等於1 mg/50g。 使用超硬WC規格之衝擊式粉碎機對清洗乾燥後之 Mo切削屑實施衝擊粉碎之粉碎處理，藉此獲得M〇微粉 末使用雷射繞射式粒度分佈測量裝置(Malvern公司製造 之master sizer 2000)對所獲得之M〇微粉末測量粒度分佈 後，結果其平均粒徑(1>5())為198 s繼而，於使爐内氫氣壓力為0.115 MPa之還原性氣體 %境下對該末’實施丨綱。c且保持2小時之熱處 理並且進行除去粉碎處理時所導入之氧等雜質之處理。 …丄又於表1中表不分析測量廢舊Mo把材，附著有切 ’之切割處理後之Mo切㈣，清洗乾燥後之M〇切削 丄川387 18812pifi 修正曰期丨〇丨年6月13曰 爲第94143995號中文說明書無劃線修正本 屑’粉碎處理後之Mo微粉末以及熱處理後之Mo微 t自雜質之結果。再者，各自之雜質係藉由Fe:原^ 、C .燃燒-紅外線吸收法，〇 :惰性氣體溶解_紅外 f收法，N以及Η :惰性氣體溶解_熱傳導法而進行分=1373387 18812pifl Amendment date June 13th, 2011 is the 94143995 Chinese manual without a slash correction. 6. Description of the Invention: The present invention relates to a method for manufacturing a target for sputtering. A method for producing a high melting point metal powder of a molten metal sintered body and a method for producing a dry material. [Prior Art] A thin-melt metal film such as molybdenum (Mo) having a small electric resistance is used as a thin film electrode and a thin film wiring of a flat display device such as a liquid crystal display (hereinafter referred to as LCD). The material for forming the metal thin film is widely used for a sputtering material. Moreover, in recent years, with the rapid expansion of the market for flat display devices, the demand for high melting point metals containing M〇 has been increasing, and the supply of raw materials for sintering for producing targets has become insufficient. Under the above circumstances, research has now been conducted on ways to reuse used targets. For example, there is a method in which a chemical wet separation method in which a waste dry material is dissolved in a solution and chemically separated to be regenerated into a metal powder, or refined by electron beam dissolution to produce a high-purity casting Ingot method, however, the chemical method has a problem of high cost, and in the method of producing a dissolved ingot by electron beam melting, there is a problem that it is difficult to apply it to the industry because the ingot is difficult to process. . In addition, a method for producing a powder material in which a waste target is pulverized and the obtained powder is passed through a hot plasma to be spheroidized and purified to a fine powder in the south is also proposed (for example, refer to Japanese Patent Laid-Open No. 2001). -342506). [Problems to be solved by the invention] 1373387 lg812pifl The date of revision is June 13, 101, and the Chinese manual of No. 5 of the 941th side is not disclosed in Japanese Patent Laid-Open No. 21-3G1-3425. No. 6, which is believed to be The pulverized powder with low purity is introduced into the hot plasma, and the spheroidization, low oxidation and high purity of the high melting point metal or the metal powder are realized. When a powder from a waste coffin is produced, it causes a problem that the filament becomes high. SUMMARY OF THE INVENTION An object of the present invention is to provide a so-called high-cost method capable of performing melt-refining refining by chemical method, and it is easy to manufacture a high-melting point at a low cost and stably from a waste metal. A method of metal powder. The present inventors have conducted various studies on a method for producing a high-melting-point metal powder from a waste high-melting-point metal target, and found that the waste dry material is made into chips by cutting, thereby introducing micro cracks into the chips. The interior thereof thereby improves the pulverizability, and combines the heat treatment for removing impurities such as oxygen introduced during cutting or pulverization, thereby producing a high melting point metal powder containing the same level of purity as the waste metal of the high melting point metal target. Therefore, the present invention has been achieved. That is, the present invention provides a method for producing a high-melting-point metal powder, which comprises cutting a waste high-melting-point metal target to form a chip, and pulverizing the chip to form a fine powder. Further, heat treatment is performed in a reducing gas atmosphere. Moreover, the present invention provides a method for producing a high-melting-point metal powder, which comprises cutting a waste high-melting-point metal target to form chips, and heat-treating the chips in a reducing gas atmosphere. Further, a pulverization treatment is carried out to prepare a fine powder. 5 I8812pifl is the _95 Chinese manual without a sizing correction. The date of the correction is June 13 (9). In addition, in the method for producing the high melting point metal powder of the present invention, it is preferred that the cutting process be a cutting machine. Further, in the method for producing a high melting point metal powder of the present invention, it is preferred that the pulverization treatment of the chips is an impact pulverization treatment. Further, in the method for producing a high melting point metal powder of the present invention, it is preferred that the heat treatment performed in the reducing gas atmosphere is carried out in an atmosphere containing hydrogen. Further, in the method for producing a high melting point metal powder of the present invention, it is preferred that the heat treatment performed in the reducing gas atmosphere is carried out under a reduced pressure atmosphere of 100 Pa or less. Further, in the method for producing a high melting point metal powder of the present invention, it is preferred that the fine powder obtained by the above pulverization treatment has an average particle diameter of between 1000 μm and n. Further, in the method for producing a high melting point metal powder of the present invention, it is preferred that the high melting point metal is a pure pin (Mo). Moreover, the present invention provides a method for producing a target material, which comprises sintering a high-melting point metal powder obtained by the above-described side edge method. According to the present invention, it is easy to manufacture a high-melting point metal powder at a low cost and stably from a waste metal element of a high melting point, so that a high melting point metal target can be manufactured at a low cost and stably, and thus industrially. Has a higher use value. The above and other objects, features and advantages of the present invention will become more <RTIgt; 1373387 18812pifl Correction date June 13, 101 is the Chinese manual of No. 94143995. There is no slash correction. [Embodiment] The most important feature of the present invention is that the following aspects are found: cutting the block of waste high melting metal casket In order to fix the shape and to produce chips which cause micro-cracks inside the metal structure, it is possible to easily pulverize by pulverization. In general, in the production of a high melting point metal target, since the dissolution temperature is high, it is difficult to manufacture by a dissolution casting method, but a powder sintering method in which a raw material powder is sintered to form a bulk. Made for manufacturing. Therefore, in order to regenerate the used target, it is necessary to process the powder which can be used as a raw material for sintering. According to the study by the present inventors, it has been found that if a high-melting-point metal material which is a composition having almost no ductility at room temperature is forcibly imparted with mechanical stress by cutting treatment, and then chips are produced, Locality of microcracks can be introduced into the chips. From this point, it can be inferred that in the composition which lacks ductility at room temperature, the stress is forcibly imparted by cutting for a short time, and thus the original ductility is exceeded, and thus a micro-crack is generated. Further, due to the presence of local micro-cracks introduced into the cutting chips, it is possible to easily obtain fine powder from a high-density melting point metal block which is difficult to pulverize. Further, as a representative example of the high melting point metal having almost no ductility at room temperature, in particular, the metal composition of chromium (Cr), molybdenum (M〇), and crane (w) and Cr, Mo, The composition of the alloy alizarin is contained in W and in the range of 5% or less. In the ductility test of therm〇_lester, for example, Mo did not show ductility until it was near 15 GC, and the melting point was higher. If it did not reach the high temperature of M〇 or more, it did not show ductility, etc. 1373387 I8812pifl Corrected the period of June, 2013, the 13th issue of the Chinese manual No. 94143995. There is no slash correction. It is considered that these compositions are almost non-extensible, and it is considered that it is easy to produce micro-cracks introduced by cutting. It is preferably suitable for producing a powder using the production method of the present invention. Hereinafter, the method for producing the melting point metal powder of the present invention will be described in order. In the present invention, first, the cut and processed high-melting point metal light materials are cut and manufactured. The reason why the cutting is produced by the cutting process is that, as described above, the microcracks can be introduced into the chips to thereby improve the pulverizability. The present inventors analyzed the correlation between the chips produced by cutting and the occurrence of microcracks in the cutting genus, and found that if the thickness of the chips exceeds about 2 mm, microcracks are present at both ends of the chips. However, (4) there is no penetration; m has a tendency to form and form from the middle (four) seam, so it is difficult to carry out the subsequent smashing. Furthermore, when cutting by dicing, the __ force change stitching is also more complicated in terms of equipment, and if the thickness of the cut is less than 3G_, the micro crack can be sufficiently introduced into the _ shot, but sometimes (4) The efficiency of making cuts is now lower, and it becomes (10) that the pulverization is degraded. Therefore, it is preferable to consider the pulverizability of the cutting, and the thickness of the cutting chips is about 3 〇 to 2 _. Further, when cutting is performed, it is possible to obtain a cutter by cutting by a lathe, a drill, or the like. Preferably, by cutting the cutting chips' and by using the composition of the scrap metal of the high melting point, and = setting the condition of the equipment #j used in the apparatus, the cutting shot is preferably better. Fight. The reason is that if the 3D 188l2pifl correction date is June 13, the Japanese manual No. 94143995 is not slashed to correct the machine', then it can be used as a flat shape and a large-sized object to be cut. Waste dry materials are fixed and cutting can be performed with higher productivity. Next, the obtained chips were pulverized to prepare fine powder. The microcracks can be locally introduced into the inside of the chips by the dicing process, so that the blocks are made into a fine powder more directly, and the powder is more powdered. The pulverization method of the chips is not particularly limited, and a ball mill 'vibration mill, a jaw mill, an impact mill, a hammer mill, an impact mill, etc. can be used, but it is preferable to use The obtained fine powder has a mean particle diameter of from 20 to 1000 μm. Further, in the pulverization treatment, it is necessary to avoid the incorporation of impurities as much as possible while considering mass productivity. In the method of rubbing force generated by a ball mill, a vibratory grinder or the like as a wire force pulverizing treatment, there is a tendency that the ultrafine powder is more fulfiled, the particle size is difficult to control, and the fine powder tends to be oxidized. Further, there is also a tendency that the use of cans is not advantageous for mass production, and contamination is increased due to contamination. In addition, there is a tendency to use a 1st force 'shear force of a drum mill or the like as a main stress (10) crushing method, or a combination of a rubbing force and a rubbing method, and the like may be caused by contact with the crushing tool. It is difficult to control the degree φ. Therefore, it is most feasible to carry out the pulverization by the impact pulverization of the impact force of the hammer mill or the pulverizer which can better suppress the contact with the pulverizing tool or the inner casing. Lai or impact pulverizer, because of the cutting of the pulverized raw material, the effect of mass production is on the vehicle 1 = and then 'reducing the gas to the cut or fine powder in the reducing gas environment towel 1373387 2 〇遛'3_中文The manual has no plan to earn the original amendment _ 6 1 June 13th. This heat treatment is necessary for the cutting treatment or the pulverization treatment to reduce the introduced oxygen to the same level as the waste high melting point metal target. ^ Further, it is more feasible to reduce the heat treatment of the oxygen, and set appropriate conditions depending on the composition of the cutting genus or the fine powder. For example, in the case where the composition of the components is Mo or W, it is more preferable to introduce a reducing gas atmosphere which is a hydrogen having excellent effects. In addition, when Nb or 'Ti' has a tendency to adsorb hydrogen, it is preferably a MoTi alloy or a MoNb alloy which is not feasible in a gas atmosphere in which hydrogen is introduced, and is preferably 100 Pa or less. A method of reducing oxygen by reduction under a reduced pressure gas atmosphere. Although it depends on the oxygen content attached to the surface of the chips or fine powder, it ensures that the attractiveness of the general rotary pump can effectively remove oxygen. Further, as for the temperature conditions for heat treatment in a reducing gas atmosphere, although there are some differences in the composition of the chips or the fine powder, it is more preferable to set it to 500 to 1500 °C. The reason for this is that if 50 (rc: hereinafter, the effect of reducing oxygen is extremely small, on the other hand, if it exceeds, the portion where the pulverized high-melting-point metal powder contacts each other will start to diffuse and bond, and thus it is difficult to re-pulverize. Further, a better temperature condition is 6 Torr to 1300 ° C, particularly preferably 800 to 1200. (: Further, when the fine powder is subjected to heat treatment in a reducing gas atmosphere, depending on temperature conditions, sometimes The fine powders are slightly combined with each other, so that the combined micro-powder may be disintegrated to form a fine powder after the heat treatment, or the micro-powder 10 1373387 mi2pifl may be corrected at a temperature lower than the heat treatment temperature before the disintegration. On June 13, 101, the Chinese specification No. 94143995 was used to reduce oxygen without performing heat treatment. β and 'in the case where the high melting point metal powder produced according to the present invention is used as a raw material powder for calendaring, considering For the filling or production efficiency of the dust container, it is more feasible that the average particle size is 20 to 1 〇〇〇μηι. Because 'if the particle size is less than 20 μηη It is sometimes difficult to & the packing density of the force device. Therefore, it is difficult to effectively perform the pulverization treatment until the average particle diameter falls to 2 〇 μηη. Further, the reason is that the coarse particle containing the average particle diameter exceeds _μιη In the case of the phenomenon, the filling density cannot be increased due to the phenomenon between the powders. " In the case of cutting the scrap metal to dry metal, in order to remove impurities such as carbon, t, hydrogen and the like attached to the blade shavings, It is feasible to add the process of cleaning the chips. ▲ As for the cleaning process, hot water, C-, B, etc. of the thief can be used, but the above-mentioned impurities are promoted in consideration of the fullness and the advancement. After the warm water washing, the method of rinsing with the water-soluble detergent and pure water used in the test red # is used. Further, when cutting, the cut=oil is sometimes used in consideration of the efficiency of the yarn, but In the case of removing the cutting oil, it is more feasible to use the hydrocarbon-washing genus. As for the hydrocarbon-based solvent, it is preferable to use the sarcophagus or the ring-burning system in consideration of the environmental risk or the risk of the fire X. Oil class. Right disk ^ according to The high-melting-point metal powder obtained by the invention has the purity of the same level as the metal ruthenium, so that by sintering the old age to obtain a sister with higher purity, the 188l2pifl correction date is June 13th, the first 94143995. The Chinese manual is not suitable for the correction of the manufacturing method. [Embodiment 1] Hereinafter, an embodiment of the present invention will be described. A waste Mo target is applied to a cutting machine by using a cutting machine having a superhard WC wafer. The material was subjected to a dicing process to obtain chips having a thickness of about 5 μm. Fig. 1 schematically shows the appearance of the swarf chips, and Fig. 2 shows a micro-tissue picture observed by an optical microscope. It can be seen from Fig. 2 that there are micro-cracks in the grain boundary of the cutting chips after cutting. Thereafter, the cutting oil adhering to the obtained M dicing chips is removed by a centrifugal separator and immersed in a hydrocarbon solvent while being washed and dried by shaking or sound. Further, after the oil component attached to the Mo cuttings was measured by the oil concentration, it was found that the oil after washing and drying was 1 mg/50 g or less. A super-hard WC-type impact pulverizer is used to perform pulverization treatment on the cleaned and dried Mo chips, thereby obtaining a laser diffraction type particle size distribution measuring device (Malvern's master sizer 2000) for M 〇 micro powder. After measuring the particle size distribution of the obtained M 〇 micropowder, the average particle diameter (1 > 5 ()) was 198 s, and then the reducing gas was made to have a hydrogen pressure of 0.115 MPa in the furnace. 'Implementation. c. The treatment was carried out for 2 hours while the impurities such as oxygen introduced during the pulverization treatment were removed. ... 丄 丄 于 表 表 表 表 表 表 表 表 表 表 表 表 表 表 表 表 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四 四曰 is the Chinese manual No. 94143995 without the slash correction of the results of the Mo fine powder after the pulverization treatment and the Mo micro-t self-contamination after the heat treatment. Furthermore, the respective impurities are obtained by Fe: original, C. combustion-infrared absorption method, 〇: inert gas dissolution_infrared f method, N and Η: inert gas dissolution_heat conduction method.
▼去〇 ’只J▼去〇 ‘J only
[表1] -------- 雜質（質量ppm) — C 〇 Fe ^-----_ 2 一廢舊Mo乾材 17 360 70 切割處理後之Mo切削屑 1110 670 78 —----- 150 ^_ 6 ^. 5 洗淨乾燥後之Mo切削屑 14 460 76 粉碎處理後之Mo微粉末 12 592 82 熱處理後之Mo微粉末 3 34 75 ^--—. 1 自表1可知，熱處理後之Mo微粉末，含有與廢舊 Mo靶材同等以下位準之雜質，尤其是可大幅降低氧含量。 又，根據本發明，由於較之廢舊靶材可大幅度降低氧 含量，故而作為氧含量之降低較為有限之用以藉由粉末燒 結法而製造靶材之原料粉末尤其合適。 [實施例2] 於使爐内氫氣壓力為0.115 MPa之還原性氣體環境 下，對以與實施例1相同之方法而獲得之清洗乾燥後之 13 18812pifl 爲第94143995號中文說明書無劃線修正本 修正日期101年6月13日[Table 1] -------- Impurity (ppm by mass) — C 〇Fe ^-----_ 2 A waste Mo dry material 17 360 70 Mo chip cutting after cutting 1110 670 78 —-- --- 150 ^_ 6 ^. 5 Washing and drying Mo chips 14 460 76 Mo fine powder after pulverization treatment 12 592 82 Mo fine powder after heat treatment 3 34 75 ^---. 1 As shown in Table 1 The Mo fine powder after the heat treatment contains impurities equivalent to the following levels of the waste Mo target, and in particular, the oxygen content can be greatly reduced. Further, according to the present invention, since the oxygen content can be greatly reduced as compared with the waste target, it is particularly suitable as a raw material powder for producing a target by a powder sintering method as a reduction in oxygen content. [Example 2] In the reducing gas atmosphere in which the hydrogen pressure in the furnace was 0.115 MPa, the 13 18812 pifl obtained after the washing and drying in the same manner as in Example 1 was No. 94143995. Revised date June 13, 101
Mo切削屑，實施12〇〇。〇下保持2小時之熱處理，並且實 施除去粉碎處理時所導入之氧等雜質之處理。使用超硬 WC規格之衝擊式粉碎機對該熱處理後之M〇切削屑實施 衝擊粉碎之粉碎處理Mo而獲得Mo微粉末。以與實施例1 相同之方式，使用雷射繞射式粒度分佈測量裝置(Maivern 公司製造之master sizer 2000)測量所獲得之Mo微粉末之 粒度分佈後’發現其平均粒徑（D5Q)為198 μιη。 於表2中表示，藉由與實施例1同樣之分析測量方 法’對廢舊Mo靶材，附著有切削油之切割處理後之Mo 切削屑，清洗乾燥後之Mo切削屑，還原性氣體環境下之 熱處理後之Mo切削屑以及粉碎處理後之Mo微粉末雜質 進行分析測量的結果。 [表2] 雜質（質量ppm) C 0 Fe Η 廢舊Mo靶材 17 360 70 2 切割處理後之Mo切削屑 1110 670 78 150 洗淨乾燥後之Mo切削屑 14 460 76 6 熱處理後之Mo切削屑 1 29 80 1 粉碎處理後之Mo微粉末 5 235 76 4 自表2亦可獲悉，藉由本發明之製造方法而獲得之 1373387 18812pifl 修正日期101年6月13日 爲第94143995號中文說明書無劃線修正本Mo cutting chips were carried out 12 〇〇. The heat treatment was carried out for 2 hours under the sputum, and the treatment of removing impurities such as oxygen introduced during the pulverization treatment was carried out. The Mo fine powder was obtained by subjecting the heat-treated M 〇 chips to the pulverization treatment Mo by impact pulverization using an ultra-hard WC-type impact pulverizer. In the same manner as in Example 1, the particle size distribution of the obtained Mo fine powder was measured using a laser diffraction type particle size distribution measuring device (master sizer 2000 manufactured by Maivern Co., Ltd.), and the average particle diameter (D5Q) was found to be 198. Ιιη. Table 2 shows the same measurement and measurement method as in the first embodiment. For the waste Mo target, the Mo cutting chips after the cutting treatment of the cutting oil are adhered, and the Mo cutting chips after the cleaning and drying are performed under a reducing gas atmosphere. The results of the analysis and measurement of the Mo chips after the heat treatment and the Mo fine powder impurities after the pulverization treatment. [Table 2] Impurities (ppm by mass) C 0 Fe 废 Waste Mo target 17 360 70 2 Mo chips after cutting 1110 670 78 150 Mo chips after washing and drying 14 460 76 6 Mo chips after heat treatment 1 29 80 1 Mo fine powder after pulverization treatment 5 235 76 4 It can also be learned from Table 2 that 1373387 18812pifl obtained by the manufacturing method of the present invention has a correction date of June 13, 101, which is No. 94143995. Amendment
Mo微粉末，含有與廢舊M〇 材同等位準以下之雜質 度降低氧含量。x，根據本發明可獲悉，由ί 大幅度降低氧含量，故而作為氧含量之降 尤限之用以藉由粉末燒結法而製造靶材之原料粉末 ^本發明已雜佳實施例揭露如上，然其並非用以 S本發明，任何„此技齡，在不脫縣發明之 ^乾圍内’當可作些許之更動與潤錦，因此本發明之保護 fe圍當視後附之申請專利範圍所界定 、 【圖式簡單說明】 為羊 >圖1是模式性繪示實施例i中所獲取之翻切削屑之 硯之圖。 圖2疋顯不實施例i中所獲取之鉬切削屑的光學顯微 鏡所觀察之微組織寫真之圖。 【主要元件符號說明】 M. 15Mo fine powder containing impurities below the same level as the waste M 降低 material to reduce the oxygen content. x, according to the present invention, it is known that the oxygen content is greatly reduced by ί, so that the raw material powder for producing the target by the powder sintering method is particularly limited as the oxygen content is lowered. However, it is not used in the present invention, any of the "technical ages, in the insufficiency of the invention" can be used to make some changes and moisturizing, so the protection of the present invention is attached to the application patent The scope is defined, [Simplified description of the drawings] is a sheep> Fig. 1 is a diagram schematically showing the entanglement of the cutting chips obtained in the embodiment i. Fig. 2 shows the molybdenum cutting obtained in the embodiment i Micro-tissue photograms observed by optical microscopy of the chips. [Main component symbol description] M. 15