TW200928007A - System and method for manufacturing high specific surface area copper material - Google Patents

System and method for manufacturing high specific surface area copper material Download PDF

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Publication number
TW200928007A
TW200928007A TW96150716A TW96150716A TW200928007A TW 200928007 A TW200928007 A TW 200928007A TW 96150716 A TW96150716 A TW 96150716A TW 96150716 A TW96150716 A TW 96150716A TW 200928007 A TW200928007 A TW 200928007A
Authority
TW
Taiwan
Prior art keywords
copper
water
cooling
drainage device
surface area
Prior art date
Application number
TW96150716A
Other languages
Chinese (zh)
Inventor
Su-Hon Lin
Chou-Sin Chen
Yung-San Chang
Ming-Cheng Ho
Jui-Chang Chou
Junn-Nan Wang
Original Assignee
Chang Chun Petrochemical Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Chang Chun Petrochemical Co Ltd filed Critical Chang Chun Petrochemical Co Ltd
Priority to TW96150716A priority Critical patent/TW200928007A/en
Priority to JP2008179635A priority patent/JP2009160654A/en
Priority to KR20080130311A priority patent/KR20090072973A/en
Priority to MYPI20085176 priority patent/MY143327A/en
Publication of TW200928007A publication Critical patent/TW200928007A/en

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0824—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
    • B22F2009/0828—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid with water
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0848—Melting process before atomisation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/086—Cooling after atomisation
    • B22F2009/0872—Cooling after atomisation by water
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/10—Copper
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Landscapes

  • Manufacture And Refinement Of Metals (AREA)
  • Electroplating Methods And Accessories (AREA)

Abstract

This invention provides a system and a method for manufacturing a high specific surface area copper material. The system comprises a heating device used for heating and melting a solid copper material to form a liquid copper, a drainage device used for receiving the liquid copper formed by the heating device and enabling the liquid copper to drain through a hole at bottom by gravity, and a cooling device used for cooling and solidifying the liquid copper drained from the hole of the drainage device bottom to form the high specific surface area copper material. The method includes heating a solid copper material to be liquid copper, draining liquid copper through the hole of the drainage device bottom by gravity, cooling and solidifying liquid copper drained from the hole of the drainage device bottom to form the high specific surface area copper material. The high specific surface area copper material produced by the system and method has excellent dissolution rate in a copper sulfate solution, is suitable for being copper ion supplier during copper electroplating process, and improves copper electroplating efficiency of whole electroplating system.

Description

200928007 九、發明說明： 【發明所屬之技術領域】 本發明係有關於-種製作鋼材之系統與方法 -有關於製作高表面積銅材之系統與方法。 特引疋 —【先前技術】 銅電鍍主要係藉由電化學作用使電解液中的 j原成金屬銅同時鍍覆於陰極基材表面上，反應式如下所 ❿陽極：H2O i/2〇2 + 2H+ +2e— 陰極：CuS〇4 + 2e- > Cu + S〇42- 為了確保銅金屬之鍍覆品質，必需使電解液中的鋼離 子維持一穩定濃度。通常，業界係利用強酸溶解鋼金屬之 方式，導入純氧或空氣供給氧氣，使銅金屬氧化為鋼離 子’以維持電解液中之銅離子濃度，如下式所示：200928007 IX. INSTRUCTIONS: TECHNICAL FIELD OF THE INVENTION The present invention relates to systems and methods for making steel materials - systems and methods for making high surface area copper. Specially cited - [Prior Art] Copper electroplating is mainly carried out by electrochemical action of the original copper in the electrolyte into the surface of the cathode substrate. The reaction is as follows: H2O i/2〇2 + 2H+ +2e—Cathode: CuS〇4 + 2e- > Cu + S〇42- In order to ensure the plating quality of copper metal, it is necessary to maintain a stable concentration of steel ions in the electrolyte. Usually, the industry uses a strong acid to dissolve steel metal, introducing pure oxygen or air to supply oxygen, and oxidizing copper metal to steel ions' to maintain the copper ion concentration in the electrolyte, as shown in the following equation:

Cu + H2SO4 + I/2O2 CuS〇4 + H2O ❹ 因此，快速且有效地使銅金屬溶解成銅離子，即成為 穩定供應電解液中銅離子的重要因素。 銅金屬的種類與形狀與溶解速率有極高的關聯性。一 般而言，使用整塊銅板金屬進行強酸溶解之銅金屬氧化反 應’提供電解銅箔之銅離子來源時，由於銅板金屬原料與 強酸溶液間之接觸面積有限，故溶解效率不佳。一般業界 常使用直徑10mm以下之裸銅線作為電解液中鋼離子來 源。裸銅線為電線電纜產品之主要原料，以銅錠、電解銅 板或純銅、熔鑄並經伸拉製成8· Omm或2· 6mm等各種線徑《> 110284 200928007 中華民國專利第438909號揭示銅線的傳統製造方法，係 涉及於一分離之設備熔融、鑄造與熱軋以生產直徑 7.94mm之銅棒，此銅棒再經冷拉及定期退火操作過程轉 -換成銅線，該方法消耗極多能量且需要廣大勞力與資本， -且中華民國專利第242654號中亦提到熔化塑製與熱捲作 業將增加產品受到額外氧化與材料潛在污染之機率。 雖然在相同重量下銅線較銅板具有更高反應表面 積，更適合作為電鑛液令銅離子來源，但是使用銅線較使 〇用鋼板需要付出更高原料成本1此，亦有提出利用網板 擴張機拉伸具有切痕之銅板形成銅擴張網板，再將該擴張 網板用於強酸溶解之鋼金屬氧化反應，提供電解鑛銅之銅 離子來源，藉以提高銅金屬溶解效率之方法。然而，該方 法所使用之銅板有來源限制，無法利用回收固體銅料製作 電錢用而表面積銅材。 因此，目前仍需要一種以低成本製作能夠快速且有效 ❹溶解於強酸溶液形成銅離子之電鍍用高表面積銅材製法。 【發明内容】 本發明主要目的係提供一種以低成本製作高表面積 銅材之系統與方法。 ，本發1月之另一目的係在於提供一種利用回收固體銅 料製作成高表面積銅材之系統與方法。 ，發明之再一目的係在於提供一種製作易溶於電解 液之高表面積銅材之系統與方法。 本發明之又-目的係在於提供—種製作㈣為電鍛 110284 6 200928007 銅系統銅離子來源之高表面積銅材之彡統與方法。 _為達上述及其他目的，本發明提供一種製作高表面積 銅材之系統，包含用以加熱熔融固體銅料形成液態銅水之 .加熱裝置，用以接收該加熱裝置所形成之液態銅水，使銅 水肖b夠藉由重力通過設於底部之開孔而流出之排流裝 置，以及用以冷卻固化自該排流裝置底部開孔流出之液態 銅水形成高表面積銅材之冷卻裝置。 本發明又提供一種製作高表面積銅材之方法’包括： ©加熱固體銅料形成液態銅水；藉由重力使銅水通過排流裝 置底部之開孔；以及冷卻固化自該排流裝置底部開孔流出 之液態銅水’形成高表面積銅材。 本發明之系統與方法所製作之高表面積銅材在硫酸 銅液中具有優異的溶解率，適合應用於銅電鍍製程，作為 銅離子供應源，可改善整體電鍍系統之鍍銅效率。 【實施方式】 ❹ 第1圖係顯示本發明製作高表面積銅材之系統方塊 圖。本發明之糸統包括：加熱裝置1 1 〇 ’係用以加熱固體 銅料形成液態銅水；排流裝置120，係用以接收該加熱裝 置110所形成之液態銅水，使銅水能夠藉由重力通過設於 該排流裝置底部之開孔而流出該排流裝置120 ;以及冷卻 震置130 ’係用以冷卻固化自該排流裝置120底部開孔流 出之液態銅水，形成高表面積銅材。 本發明系統所使用之固體銅料的實例包括，但非限於 鋼塊、鋼錠、電解銅板、銅片、銅線、其他廢棄銅材或其 110284 7 200928007 犯合物’例如無任何夾雜成分之一級廢銅箔；夾雜成分不 超過3/°之二級廢銅落；以及夾雜有黏合劑之三級廢銅 /备該等固體鋼料經加熱熔融後，可去除大部分油分與有 機雜質，形成液態銅水。該液態銅水注入排流裝置後，藉 由重力作用自排流裝置底部開孔流出，垂直向下流入設於 排μ裝置下方之冷卻裝置，在冷卻裝置中固化形成假比重 1.6至4.0 ’較佳18至3 5，更佳丨.8至2.6之高表面 積銅材，例如絲狀、線狀、粒狀、片狀或不規則狀之銅材， ❹較佳者為類似茶葉形狀之片狀銅材。 第2圖係顯示本發明系統之第一具體實例。於該具體 貝例中本發明之系統係使用掛禍210作為加熱裝置，用 以加熱固體銅料至熔融狀態，形成至少約1180至1300 °C，較佳約1200至1250t:之液態銅水，當銅水溫度低於 1^50°C時，銅水表面會發生凝固結膜的現象而不易倒出或 谷易塞住模具開孔。使用桶狀模具22〇作為排流裝置，接 ❹收掛竭21G中的液態銅水。如第2a @所示，該桶狀模具 220底部開設有複數個開孔222，使桶狀模具220中的液 態銅水可藉由重力作用通過底部開孔222，流出該桶狀模 具220。一般而言，該桶狀模具22〇底部開孔之孔徑係介 於Φ2.5至Φ20 mm之範圍内，較佳係介於㈣至㈣龍 之範圍内，更佳係介於Φ4Φ1〇 mm之範圍内。若開孔 孔控太小容易發生阻塞的情形，使得桶狀模具22〇内的銅 水無法順利藉由重力作用通過開孔而流出，若開孔孔經太 大則不利於形成高表面積銅材，一般而言，當孔徑低於3 110284 8 200928007 咖較容易發生阻塞的情形。調整該桶狀模具22〇底部開 孔間距與開孔數量亦有助於減少洗注槽開孔阻塞之情 形。例如，該桶狀模具220底部之開孔間距可介於1〇 ^ .50難之範圍，較佳係介於15至4〇随範圍，更佳係 於20至30 mm之範圍。 再者，維持桶狀模具高溫，例如使用電熱保溫維持 _C ’有助於改善塞料之情形。另—方面，在桶狀模具 内部喷塗高溫被覆劑，提高離形效果，亦有助於防止黏料。 如第2圖所示，於此具體實例令，係使用冷卻水池 230作為冷卻裝置，該冷卻水池23()係設置於該桶狀模呈 220下方。桶狀模具220中的銅水藉由重力作用通過底部 開孔流出後，直線地向下流入水深約2〇〇至15〇〇咖之冷 部水池230，經冷卻固化形成絲狀、線狀、粒狀、片狀或 不規則狀銅材。冷卻水池之水溫通常係介於1〇至託它， 較佳係介於28至35艺，更佳係29至33t之範圍内。 〇 於此具體實例中’本發明系統的冷卻水池之水面與該 排流裝置底部具有高度差h。通常，該高度差h係介於500 至4500 mm之範圍，較佳係介於1000至4000 mm之範圍， 更^係介於2000至3500 mm之範圍。一般而言，維持適 當高度差，例如1000 mm以上之高度差，可以避免銅水流 入冷卻水池230時發生氣爆的情形；另一方面，若高度差 過大，則會傾向於形成假比重過高之細砂粒狀銅材。如第 2b圖所不，本發明系統中之冷卻水池23〇底部可進—步 設有注水孔232向上打水，增加池内冷卻水的波動性，有 g 110284 200928007 助於形成高表面積銅材。 第3圖係顯示本發明系統之第二具體實例。同第一具 體實例，本具體實例之系統係使用坩堝310加熱固體銅料 .至熔融狀態，形成液態銅水。利用底部開設有複數個開孔 之桶狀模具320接收坩堝310中的液態銅水，使桶狀模具 320中的液態銅水藉由重力作用通過底部開孔，流出該桶 狀模具320，直線地向下流入置於該桶狀模具320下方之 冷卻水池330。 〇 於本具體實例中，該桶狀模具320底部與冷卻水池 330之水面間具有一高度差，在桶狀模具320底部與冷卻 水池3 3 0水面間，更進一步設置有風管3 4 0，以垂直銅水 流出該桶狀模具320的方向送出冷風，使桶狀模具320 底部所流出之銅水先經冷風初步降溫後，再流入冷卻水池 330，固化形成高表面積銅材。 如第3圖所示，在桶狀模具320底部與冷卻水池330 η水面間之風管340，可進一步包括多個出風口 340a、 ❹ 340b、340c，以垂直銅水流出該桶狀模具320的方向分別 送出60至100°C之熱風、20至30°C之常溫風、及15至 20°C之冷風，使桶狀模具320底部所流出之銅水經逐步降 溫後，再流入冷卻水池3 3 0，固化形成高表面積銅材。 第4圖係顯示本發明系統之第三具體實例。同第一具 體實例，本具體實例之系統係使用坩堝410加熱固體銅料 至熔融狀態，形成液態銅水。利用底部開設有複數個開孔 之桶狀模具420接收坩堝410中的液態銅水，使桶狀模具 10 110284 200928007 420中的液態銅水藉由重力作用通過底部開孔，流出該桶 狀杈具420，直線地向下流入置於該桶狀模具42〇下方之 冷卻水池430。 於本具體實例中，該捅狀模具420底部與冷卻水池 • 430之水面間具有一高度差，且設置有一系列噴嘴， 以垂直銅水流出該桶狀模具42〇的方向連續地噴出經霧 化之水氣’使桶狀模具42〇底部所流出之銅水先經霧化水 氣初步降溫後，再流入冷卻水池43〇，固化形成高表面積 〇銅材。 第5圖係顯示本發明系統之第四具體實例。本具體實 例之系統係使用坩堝51 〇加熱固體銅料至熔融狀態，形成 液態銅水。使用底部開設有複數個開孔522之滑道模具 520作為排流裝置，並以水平夾角小於9〇度之傾斜度架 設於冷卻水池530之水面上。當坩堝51〇中的液態銅水注 入該傾斜模具520 ’銅水會順著傾斜模具52〇向下流的同 〇時，藉由重力作用通過該傾斜模具52〇底部之開孔1122°， 流入下方的冷卻水池，如圖中箭號所示，固化形成高表面 積銅材。 本發明亦提供一種製作高表面積銅材之方法。如第6 圖所示，本發明之方法包括：加熱步驟S6l〇，加熱固體 銅料形成液態銅水；排流步驟S620，使鋼水藉由重力 用通過排流裝置底部開孔；以及冷卻步驟S63〇，^ ,作 化自該排流裝置底部開孔流出液態銅水形士 ^ 7 P固 成兩表面積銅 材。於一具體實例中，係將固體銅料置於堆禍中進行加熱 110284 11 200928007 t 步驟，使固體銅料’熔融形成液態銅水，視需要靜置1至4 为鉍再將坩堝中的銅水倒入底部設有複數個開孔之排流 裝置，或直接將坩堝中的銅水倒入該排流裝置。接者，使 -該排流裝置中的銅水藉由重力作用通過底部開孔而流 -出，直線地向下流入置於該排流裝置下方的冷卻裝置再 經冷卻裝置中的冷卻水固化形成絲狀、線狀、粒狀、片狀 或不規則狀的高表面積銅材。另一方面，該排流裝置底部 開孔流出之液態銅水可先經冷風初步降溫後再流入冷卻 〇水池及/或先經霧化水氣初步降溫後再流入冷卻水池，固 化形成高表面積銅材。 以下將藉由具體實例進一步說明本發明之特點與功 效，但並非將本發明侷限於此。 實施例 實施例1 將6.5公斤重之銅塊置於坩堝中加熱至熔融狀態，形 成約1200°C之液態銅水。將銅水倒入底部設有6個〇5 開孔之桶狀模具中，使銅水藉由重力作用通過桶狀模具底 部之開孔，流出該桶狀模具。桶狀模具下方設有冷卻水 池，水深1300 mm，水溫28· rc，底部設有注水孔向上打 水’水面與桶狀模具底部距離2600 mm。流出桶狀模具之 銅水藉由重力作用直線地向下流入冷卻水池，經冷卻固化 形成6. 3公斤，假比重約2. 5之銅材樣品。 110284 12 200928007 , 實施例2 - 5 根據表1所列，重複實施例丨之步驟，將所製得之鋼 材樣品假比重記錄於表i。 6-19 例i ^表1所列，改變桶狀模具底部開孔數，重複實施 ^驟，將所製得之銅材樣品假比重記錄於表1。 Ο 列 13-14 〇Cu + H2SO4 + I/2O2 CuS〇4 + H2O ❹ Therefore, the rapid and effective dissolution of copper metal into copper ions is an important factor for stably supplying copper ions in the electrolyte. The type and shape of copper metal has a very high correlation with the dissolution rate. In general, when a copper ion source for electrolytic acid dissolution is used to provide a copper ion source for electrolytic copper foil, the dissolution efficiency is not good because the contact area between the copper metal material and the strong acid solution is limited. In the industry, bare copper wires with a diameter of 10 mm or less are often used as the source of steel ions in the electrolyte. The bare copper wire is the main raw material of wire and cable products. It is made of copper ingot, electrolytic copper plate or pure copper, cast and stretched to make various wire diameters such as 8·Omm or 2·6mm. > 110284 200928007 China Patent No. 438909 The traditional manufacturing method of copper wire involves melting, casting and hot rolling of a separate device to produce a copper rod having a diameter of 7.94 mm, which is then converted into a copper wire by a cold drawing and periodic annealing operation. It consumes a lot of energy and requires a lot of labor and capital. - And Republic of China Patent No. 242654 also mentions that melt molding and hot coiling operations will increase the chances of products being subject to additional oxidation and potential contamination of materials. Although the copper wire has a higher reaction surface area than the copper plate under the same weight, it is more suitable as a source of copper ions for electric ore. However, the use of copper wire requires higher raw material cost than the use of the steel plate. The expander stretches the copper plate with the cut to form a copper expanded mesh plate, and then uses the expanded mesh plate for the oxidation reaction of the molten metal of the strong acid to provide a source of copper ions of the electrolytic copper, thereby improving the dissolution efficiency of the copper metal. However, the copper plate used in this method has a source limitation, and it is not possible to use the recovered solid copper material to make electricity for the surface and copper. Therefore, there is still a need for a process for producing a high surface area copper material for electroplating which can be quickly and efficiently dissolved in a strong acid solution to form copper ions at a low cost. SUMMARY OF THE INVENTION A primary object of the present invention is to provide a system and method for producing a high surface area copper material at low cost. Another object of the present invention in January is to provide a system and method for producing high surface area copper using recycled solid copper. A further object of the invention is to provide a system and method for making a high surface area copper material that is readily soluble in an electrolyte. Still another object of the present invention is to provide a system and method for producing a high surface area copper material from a copper ion source of copper system 110284 6 200928007. For the above and other objects, the present invention provides a system for producing a high surface area copper material, comprising: a heating device for heating molten solid copper material to form liquid copper water for receiving liquid copper water formed by the heating device, A cooling device for allowing copper water to flow out through gravity through a hole provided in the bottom, and a cooling device for cooling the liquid copper water which is solidified from the bottom opening of the drainage device to form a high surface area copper material. The invention further provides a method for producing a high surface area copper material comprising: heating a solid copper material to form liquid copper water; passing copper water through the opening of the bottom of the drainage device by gravity; and cooling solidifying from the bottom of the drainage device. The liquid copper water flowing out of the hole 'forms a high surface area copper. The high surface area copper material produced by the system and method of the present invention has excellent dissolution rate in copper sulphate solution and is suitable for use in a copper electroplating process. As a copper ion supply source, the copper plating efficiency of the overall electroplating system can be improved. [Embodiment] Fig. 1 is a block diagram showing the system for producing a high surface area copper material according to the present invention. The system of the present invention comprises: a heating device 1 1 〇' for heating solid copper material to form liquid copper water; and a drainage device 120 for receiving liquid copper water formed by the heating device 110, so that the copper water can be borrowed The drainage device 120 is flowed out by gravity through an opening provided at the bottom of the drainage device; and the cooling vibration 130' is used to cool the liquid copper water which solidifies and flows out from the bottom opening of the drainage device 120 to form a high surface area. Copper. Examples of solid copper materials used in the system of the present invention include, but are not limited to, steel blocks, steel ingots, electrolytic copper plates, copper sheets, copper wires, other waste copper materials or their 110284 7 200928007 com-compounds, for example, without any inclusions. Scrap copper foil; two-stage scrap copper with no inclusion component of more than 3/°; and three-stage scrap copper mixed with binder/heated and melted to remove most of the oil and organic impurities Liquid copper water. After the liquid copper water is injected into the drainage device, it flows out from the bottom opening of the drainage device by gravity, and flows vertically downward into the cooling device disposed under the discharge device, and solidifies in the cooling device to form a pseudo specific gravity of 1.6 to 4.0'. Preferably, the surface area of the copper material is from 18 to 35, more preferably from 8 to 2.6, such as a filament, a wire, a granule, a sheet or an irregular copper material, preferably a tea-like sheet. Copper. Figure 2 shows a first specific example of the system of the present invention. In the specific example, the system of the present invention uses the smashing 210 as a heating device for heating the solid copper material to a molten state to form a liquid copper water of at least about 1180 to 1300 ° C, preferably about 1200 to 1250 t: When the temperature of the copper water is lower than 1^50 ° C, the surface of the copper water will solidify and consolidate, which is not easy to be poured out or the valley is easy to plug the mold opening. Using a barrel mold 22 as a drainage device, the liquid copper water in the 21G was exhausted. As shown in Fig. 2a @, the bottom of the barrel mold 220 is provided with a plurality of openings 222, so that the liquid copper water in the barrel mold 220 can flow out of the barrel mold 220 by gravity through the bottom opening 222. Generally, the aperture of the bottom opening of the barrel mold 22 is in the range of Φ2.5 to Φ20 mm, preferably within the range of (4) to (4) dragon, and more preferably between Φ4Φ1〇mm. Within the scope. If the hole control is too small, it is easy to block, so that the copper water in the barrel mold 22 cannot flow smoothly through the opening through gravity. If the hole is too large, it is not suitable for forming high surface area copper. In general, when the aperture is lower than 3 110284 8 200928007, the coffee is more prone to blockage. Adjusting the opening pitch and the number of openings in the bottom of the barrel mold 22 also helps to reduce the blockage of the opening of the washing tank. For example, the opening pitch of the bottom of the barrel mold 220 may be in the range of 1 〇 ^ .50, preferably in the range of 15 to 4 inches, more preferably in the range of 20 to 30 mm. Furthermore, maintaining the barrel mold at a high temperature, for example, using electrothermal insulation to maintain _C' helps to improve the condition of the plug. On the other hand, spraying a high-temperature coating agent inside the barrel mold improves the release effect and helps prevent sticking. As shown in Fig. 2, in this specific example, a cooling water tank 230 is used as a cooling device, and the cooling water tank 23 () is disposed below the barrel mold 220. The copper water in the barrel mold 220 flows out through the bottom opening by gravity, and flows straight down into the cold water pool 230 having a water depth of about 2 〇〇 to 15 ,, and is cooled and solidified to form a filament, a line, Granular, flaked or irregular copper. The water temperature of the cooling pool is usually between 1 and Torr, preferably between 28 and 35, more preferably between 29 and 33 Torr. 〇 In this specific example, the water surface of the cooling pool of the system of the present invention has a height difference h from the bottom of the drainage device. Typically, the height difference h is in the range of 500 to 4500 mm, preferably in the range of 1000 to 4000 mm, and more preferably in the range of 2000 to 3500 mm. In general, maintaining a proper height difference, for example, a height difference of 1000 mm or more, can avoid a gas explosion when copper water flows into the cooling pool 230; on the other hand, if the height difference is too large, the pseudo-specific gravity is too high. Fine sand granular copper. As shown in Fig. 2b, the bottom of the cooling water tank 23 in the system of the present invention can be further provided with a water injection hole 232 for watering upward to increase the fluctuation of the cooling water in the pool, and g 110284 200928007 helps to form a high surface area copper material. Figure 3 is a diagram showing a second specific example of the system of the present invention. As with the first specific example, the system of this embodiment uses 坩埚310 to heat the solid copper material to a molten state to form liquid copper water. The liquid copper water in the crucible 310 is received by the barrel mold 320 having a plurality of openings at the bottom, so that the liquid copper water in the barrel mold 320 passes through the bottom opening by gravity, and flows out of the barrel mold 320, linearly The cooling pool 330 placed below the barrel mold 320 flows downward. In this embodiment, there is a height difference between the bottom of the barrel mold 320 and the water surface of the cooling pool 330. Further, a duct 3404 is disposed between the bottom of the barrel mold 320 and the water surface of the cooling pool 330. The cold water is sent out in the direction in which the vertical copper water flows out of the barrel mold 320, so that the copper water flowing out from the bottom of the barrel mold 320 is initially cooled by the cold air, and then flows into the cooling water tank 330 to be solidified to form a high surface area copper material. As shown in FIG. 3, the duct 340 between the bottom of the barrel mold 320 and the water surface of the cooling pool 330 may further include a plurality of air outlets 340a, 340b, 340c for flowing the vertical copper water out of the barrel mold 320. The direction sends 60 to 100 ° C hot air, 20 to 30 ° C normal temperature wind, and 15 to 20 ° C cold air, so that the copper water flowing out from the bottom of the barrel mold 320 is gradually cooled, and then flows into the cooling pool 3 30, cured to form a high surface area copper. Figure 4 is a diagram showing a third embodiment of the system of the present invention. As with the first specific example, the system of this embodiment uses 坩埚410 to heat the solid copper material to a molten state to form liquid copper water. The liquid copper water in the crucible 410 is received by a barrel mold 420 having a plurality of openings at the bottom, so that the liquid copper water in the barrel mold 10 110284 200928007 420 flows through the bottom opening by gravity, and flows out of the barrel cookware. 420, flowing straight down into the cooling pool 430 placed under the barrel mold 42. In this embodiment, the bottom of the mold 420 has a height difference from the water surface of the cooling pool 430, and a series of nozzles are arranged to continuously spray the atomized copper water out of the barrel mold 42〇. The water gas 'the copper water flowing out from the bottom of the barrel mold 42 is first cooled by the atomized water gas, and then flows into the cooling water tank 43 〇 to solidify to form a high surface area bismuth copper material. Fig. 5 is a view showing a fourth specific example of the system of the present invention. The system of this specific example uses 坩埚51 〇 to heat the solid copper material to a molten state to form liquid copper water. A slide mold 520 having a plurality of openings 522 at the bottom is used as a draining device, and is disposed on the water surface of the cooling water tank 530 with an inclination of a horizontal angle of less than 9 degrees. When the liquid copper water in the crucible 51〇 is injected into the inclined mold 520 'the copper water will flow down the inclined mold 52〇, the gravity passes through the opening of the inclined mold 52〇 at the bottom of the opening 1122°, flowing into the lower side. The cooling pool, as indicated by the arrows in the figure, solidifies to form a high surface area copper. The invention also provides a method of making a high surface area copper material. As shown in FIG. 6, the method of the present invention comprises: heating step S6l, heating solid copper material to form liquid copper water; discharging step S620, allowing molten steel to pass through the bottom opening of the drainage device by gravity; and cooling step S63〇, ^ , from the bottom opening of the drainage device, the liquid copper water shape is formed into a two-surface copper material. In a specific example, the solid copper material is placed in a stack to heat the 110284 11 200928007 t step, so that the solid copper material is 'melted to form liquid copper water, and if necessary, it is allowed to stand for 1 to 4, and then the copper in the crucible. The water is poured into the bottom and a plurality of draining devices are arranged, or the copper water in the crucible is directly poured into the draining device. Receiving, the copper water in the drainage device flows out through the bottom opening by gravity, flows straight down into the cooling device placed under the drainage device, and is solidified by the cooling water in the cooling device. Forming a high surface area copper material in the form of filaments, wires, granules, flakes or irregularities. On the other hand, the liquid copper water flowing out from the bottom opening of the drainage device can be first cooled by the cold air and then flow into the cooling water pool and/or first cooled down by the atomized water gas before flowing into the cooling pool to form a high surface area copper. material. The features and effects of the present invention are further illustrated by the following examples, but the invention is not limited thereto. EXAMPLES Example 1 A 6.5 kg copper block was placed in a crucible and heated to a molten state to form a liquid copper water of about 1200 °C. The copper water is poured into a barrel mold having 6 〇5 openings at the bottom, so that the copper water flows out of the barrel mold by gravity through the opening of the bottom of the barrel mold. There is a cooling water tank below the barrel mold, the water depth is 1300 mm, the water temperature is 28· rc, and the bottom is provided with a water injection hole to draw water. The water surface is 2600 mm away from the bottom of the barrel mold. 5的铜材样。 The copper water sample of the 5% of the pseudo-specific gravity of about 2.5. 110284 12 200928007, Examples 2 - 5 According to Table 1, the procedure of Example 重复 was repeated, and the pseudo proportion of the obtained steel sample was recorded in Table i. 6-19 Example i ^ Table 1, change the number of openings at the bottom of the barrel mold, repeat the procedure, and record the pseudo-specific gravity of the prepared copper sample in Table 1. Ο Column 13-14 〇

110284 13 200928007 ‘ 實施例13 (Lot 69) 將6 · 5公斤重之銅塊置於掛堝中加熱至熔融狀態，形 成約1200 C之液態銅水❶將銅水倒入底部設有13個①5 -開孔之桶狀模具中，使銅水藉由重力作用通過桶狀模具底 -部之開孔，流出該桶狀模具。桶狀模具下方設有冷卻水 池，水深1300 mm，水溫31。(：，底部設有注水孔向上打水， 水面與桶狀模具底部距離37〇〇 mm，水氣喷嘴設於桶狀模 具下方距模具底部500 mm位置。流出桶狀模具之銅水藉 Ο由重力作用直線地向下，經霧化水氣初步冷卻後流入冷卻 水池，經冷卻固化形成6.3公斤，假比重約3.0之銅材樣 品。 實施例14 (Lot 71) 將6. 5公斤重之銅塊置於坩堝中加熱至熔融狀態，形 成約1200°C之液態銅水。將銅水倒入底部設有13個（1>5 ❹開孔之桶狀模具中，使銅水藉由重力作用通過桶狀模具底 邻之開孔，流出該桶狀模具。桶狀模具下方設有冷卻水 池，水深1300 mm’水溫3rc，底部設有注水孔向上打水， 水面與桶狀模具底部距離700賴。流出桶狀模具之銅水 藉由重力作用直線地向下流入冷卻水池，經冷卻固化形成 6公斤，假比重約3· 5之銅材樣品。 測試例1 分別取60公斤假比重約2·3之銅材樣品i與2.6咖 110284 14 200928007 之銅線（假比重〇 ，番你‘ .1Qn . .)置於硫敲銅電解液液中（硫酸濃度 =30克/升）’進行溶解測試，歷時％小時。測試完畢， 銅線與鋼材樣品i，以去離子水清洗，放入供 相乾燥去除水分，秤重，計管 * 0 卞外/合解速率，並將結果記錄於 衣6 0 _測試例2 分別取3 0公斤逢 1 p ❹之鋼線(假比重3 5 ) .之銅材樣品2與“m 為nn & 、·）置於攸酸鋼電解液液中（硫酸濃度 畢，取出幻铃’進行溶解測試，歷時19. 5小時。測試完 畢取出剩餘的銅線與銅㈣品2> 錄於表2。 重计异洛解逮率，並將結果記110284 13 200928007 ' Example 13 (Lot 69) The 6.5 kg copper block was placed in a hanging crucible and heated to a molten state to form a liquid copper leeches of about 1200 C. The copper water was poured into the bottom and 13 were placed. - In the barrel mold of the opening, the copper water flows out of the barrel mold by gravity through the opening of the bottom portion of the barrel mold. Below the barrel mold is a cooling water tank with a water depth of 1300 mm and a water temperature of 31. (: There is a water injection hole at the bottom to draw water upwards, the water surface is at a distance of 37〇〇mm from the bottom of the barrel mold, and the water gas nozzle is located 500 mm below the bottom of the mold under the barrel mold. The copper water flowing out of the barrel mold is used by The weight of the copper is 6. 5 kg of copper. The copper is sampled (Lot 71). The copper is 6.5 kg. The block is placed in a crucible and heated to a molten state to form a liquid copper water of about 1200 ° C. The copper water is poured into the bottom and 13 (1 > 5 ❹ open hole barrel molds are used to make the copper water by gravity The barrel mold is flowed out through the opening of the bottom of the barrel mold. A cooling pool is arranged under the barrel mold, the water depth is 1300 mm' water temperature 3rc, and the bottom is provided with a water injection hole to draw water upward, and the water surface is at a distance of 700 from the bottom of the barrel mold. The copper water flowing out of the barrel mold flows straight down into the cooling pool by gravity, and is solidified by cooling to form 6 kg of copper material with a pseudo-specific gravity of about 3.5. Test Example 1 Take a pseudo-specific gravity of about 60 kg. ·3 copper samples i and 2.6 coffee 110284 14 200928007 Copper wire (false proportion 〇, Fan you '.1Qn . . .) placed in sulfur-thawed copper electrolyte solution (sulfuric acid concentration = 30 g / liter) 'dissolution test, lasted for an hour. Test completed, copper wire and Steel sample i, washed with deionized water, placed in phase for drying to remove moisture, weighed, counted * 0 卞 outside / recombination rate, and the results were recorded in clothing 60 0 test case 2 respectively take 30 kg 1 p ❹ steel wire (false specific gravity 3 5 ). The copper sample 2 and "m is nn &, ·) are placed in the bismuth acid electrolyte solution (the sulfuric acid concentration is completed, the magic bell is taken out) for the dissolution test. It lasted for 19.5 hours. After the test, the remaining copper wire and copper (four) product 2 were taken out. Recorded in Table 2. The rate of the drug was counted and the result was recorded.

表2 測試例1 測試前重量 溶解測試時間 (小時） 溶解速率 ί公斤^時、 銅材樣品1 2· 6 mm銅綠 ---- 4 羨品2 VI^J L· 8譲銅線 60 — 60 — 30 30 94 ------- 94 ------ —------ 19.5 19. 5 16 --- 34 ------—. ------ 17 29 0.47 - 0. 28 ------— 0. 67 0. 05 〇 根據表2結果顯示，本發明劁 有較佳的溶Mm 兩表面積銅材具 解率’適合應用於銅電鍍製程作為鋼離子供應 110284 15 200928007 . 源，改善整體電鍍系統之鍍銅效率。 【圖式簡單說明】 第1圖係本發明製作高表面積銅材系統之方塊圖； 第2圖係說明本發明系統之第一具體實例； . 第2a圖係說明本發明第一具體實例之桶狀模具； 第2b圖係說明本發明第一具體實例之冷卻水池； 第3圖係說明本發明系統之第二具體實例； 第4圖係說明本發明系統之第三具體實例； ❹ 第5圖係說明本發明系統之第四具體實例；以及 第6圖係本發明製作高表面積銅材方法之流程圖。 【主要元件符號說明】 110 加熱裝置 120 排流裝置 130 冷卻裝置 210、310、410、510 坩堝 220、320、420、520 模具 222 、 522 開孔 230、330、430、530 冷卻水池 232 注水孔 340 風管 340a、340b、340c 出風口 440 噴嘴 16 110284Table 2 Test Example 1 Pre-test weight dissolution test time (hours) Dissolution rate ί kg ^, copper sample 1 2 · 6 mm patina ---- 4 ^ 2 VI ^ JL · 8 譲 copper wire 60 — 60 — 30 30 94 ------- 94 ------------------ 19.5 19. 5 16 --- 34 -------. ------ 17 29 0.47 - 0. 28 ------- 0. 67 0. 05 〇 According to the results in Table 2, the present invention has a better solution of molten Mm two-surface copper material, which is suitable for use in copper electroplating processes as steel ions. Supply 110284 15 200928007 . Source, improve the copper plating efficiency of the overall plating system. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a block diagram of a high surface area copper system of the present invention; Fig. 2 is a first specific example of the system of the present invention; Fig. 2a is a view showing a barrel of the first embodiment of the present invention 2b is a cooling water tank according to a first embodiment of the present invention; FIG. 3 is a second concrete example of the system of the present invention; and FIG. 4 is a third concrete example of the system of the present invention; A fourth embodiment of the system of the present invention is illustrated; and Figure 6 is a flow chart of a method of making a high surface area copper material of the present invention. [Main component symbol description] 110 Heating device 120 Drain device 130 Cooling device 210, 310, 410, 510 坩埚 220, 320, 420, 520 Mold 222, 522 Opening 230, 330, 430, 530 Cooling pool 232 Water injection hole 340 Duct 340a, 340b, 340c air outlet 440 nozzle 16 110284

Claims (1)

200928007 . 十、申請專利範圍·· 1. 一種製作高表面積銅材之系統，包括： 加熱裝置’係用以加熱固體銅料形成液態銅水； - 排流裝置’係用以接收該加熱裝置所形成之液態 銅水，使銅水能夠藉由重力通過設於排流裝置底部之 開孔而流出該排流裝置；以及 冷卻裝置’係用以冷卻固化自該排流裝置底部開 孔流出之液態銅水’形成高表面積銅材。 ❹2.如申請專利範圍第1項之系統，其中，該固體銅料係 選自銅塊、銅錠、電解銅板、銅片、銅線、廢棄銅材 及其混合物。 3. 如申請專利範圍第1項之系統，其中，該排流裝置底 部開孔之孔徑係介於Φ2. 5至20 mm之範圍内。 4. 如申請專利範圍第1項之系統，其中，該冷卻裝置係 冷卻水池。 ❹5.如申請專利範圍第4項之系統，其中，該冷卻水池係 設置於該排流裝置下方。 6. 如申請專利範圍第5項之系統，其中，該冷卻水池之 水面與該排流裝置底部距離5〇〇至4500 mm。 7. 如申請專利範圍第5項之系統，其中，該冷卻水池之 水深係200至1500 mm。 8. 如申請專利範圍第5項之系統，其中，該冷卻水池底 部係設有注水孔向上打水。 9·如申請專利範圍第5項之系統，其中，該冷卻裝置復 17 110284 200928007 . 包括設置於該冷卻水池與該排流裝置間的風管。 10.如申請專利範圍第5項之系、統，其中，該冷卻 包括設置於該冷卻水池與該排流裝置間的噴嘴。、又 -11. 一種製作高表面積銅材之方法，包括： ' 加熱固體銅料形成液態銅水； 使銅水藉由重力作用通過排流裝置底部之開 孑L ;以及200928007 . X. Patent Application Scope 1. A system for making high surface area copper, comprising: heating device 'for heating solid copper material to form liquid copper water; - draining device' for receiving the heating device Forming liquid copper water so that the copper water can flow out of the drainage device by gravity through an opening provided at the bottom of the drainage device; and the cooling device is configured to cool and solidify the liquid liquid flowing out from the bottom opening of the drainage device Copper water 'forms high surface area copper. The system of claim 1, wherein the solid copper material is selected from the group consisting of copper blocks, copper ingots, electrolytic copper plates, copper sheets, copper wires, waste copper materials, and mixtures thereof. 3. The range of the aperture of the bottom opening of the venting device is in the range of Φ2.5 to 20 mm, as in the system of claim 1. 4. The system of claim 1, wherein the cooling device is a cooling pool. ❹ 5. The system of claim 4, wherein the cooling water tank is disposed below the drainage device. 6. The system of claim 5, wherein the water surface of the cooling pool is 5 to 4500 mm from the bottom of the drainage device. 7. The system of claim 5, wherein the cooling pool has a water depth of 200 to 1500 mm. 8. The system of claim 5, wherein the bottom of the cooling pool is provided with a water injection hole to draw water upward. 9. The system of claim 5, wherein the cooling device further comprises a duct disposed between the cooling pool and the draining device. 10. The system of claim 5, wherein the cooling comprises a nozzle disposed between the cooling pool and the drainage device. -11. A method of making a high surface area copper material, comprising: 'heating the solid copper material to form liquid copper water; and causing the copper water to pass through the bottom of the drainage device by gravity; 冷卻固化自該排流裝置底部開孔流出之液態鋼 水’形成高表面積銅材。 12.如申請專利範圍第n項之方法，其中，該固體鋼料 係選自銅塊、銅錠、電解銅板、銅板、銅線、廢棄鋼 材或其混合物。 13·如申請專利範圍第n項之方法，其中，該排流裝置 底部開孔之孔徑係介於φ 2. 5至20 mm之範圍内。 14.如申請專利範圍第Π之方法，其中，該排流裝置底 〇 開孔流出之液態銅水係於冷卻水池中固化形成高 表面積銅材。 15. 如申請專利範圍第14項之方法，其中，該冷卻水池 係設置於該排流裝置下方。 16. 如申請專利範圍第15項之方法，其中，該冷卻水池 之水面與該排流裝置底部距離5〇〇至4500 ππη。 17. 如申請專利範圍第15項之方法，其中，該冷卻水池 之水深係200至1500 18 ·如申叫專利範圍第15項之方法，其中’該冷卻水池 18 Π0284 200928007 . 底部係設有注水孔向上打水。 19.如申請專利範圍第丨5項之方法，其中，該排流裝置 底部開孔流出之液態銅水係先經冷風初步降溫後再 ' 流入冷卻水池中固化形成高表面積銅材。 -20.如申請專利範圍第！ 5項之方法’其中’該排流裝置 底部開孔流出之液態銅水係先經霧化水氣初步降溫 後再流入冷卻水池中固化形成高表面積鋼材。 〇Cooling and solidifying the liquid steel water flowing out from the bottom opening of the drainage device forms a high surface area copper material. 12. The method of claim n, wherein the solid steel material is selected from the group consisting of copper blocks, copper ingots, electrolytic copper plates, copper plates, copper wires, waste steel materials, or mixtures thereof. 13. The method of claim n, wherein the aperture of the bottom opening of the drainage device is in the range of φ 2.5 to 20 mm. 14. The method of claim </ RTI> wherein the liquid copper water flowing out of the bottom of the drainage device is solidified in a cooling water bath to form a high surface area copper material. 15. The method of claim 14, wherein the cooling water tank is disposed below the drainage device. 16. The method of claim 15, wherein the water surface of the cooling pool is 5 to 4500 ππη from the bottom of the drainage device. 17. The method of claim 15, wherein the cooling pool has a water depth of 200 to 1500 18. The method of claim 15 is wherein the cooling pool is 18 Π 0284 200928007. The hole is pumped up. 19. The method of claim 5, wherein the liquid copper water flowing out from the bottom opening of the drainage device is first cooled by the cold air and then poured into the cooling pool to form a high surface area copper material. -20. If you apply for a patent scope! The method of item 5 wherein the liquid copper water flowing out from the bottom opening of the drainage device is first cooled by the atomized water gas and then flows into the cooling pool to form a high surface area steel. 〇 110284 19110284 19
TW96150716A 2007-12-28 2007-12-28 System and method for manufacturing high specific surface area copper material TW200928007A (en)

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TW96150716A TW200928007A (en) 2007-12-28 2007-12-28 System and method for manufacturing high specific surface area copper material
JP2008179635A JP2009160654A (en) 2007-12-28 2008-07-09 System and method for manufacturing copper material with high specific surface area
KR20080130311A KR20090072973A (en) 2007-12-28 2008-12-19 Systems and methods for producing high surface area copper materials
MYPI20085176 MY143327A (en) 2007-12-28 2008-12-19 System and method for producing copper material of high surface area

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