201035328 六、發明說明： 【發明所屬之技術領域】 本發明係關於焊料資源回收之發明，特別是關於再利 用焊料糊時，焊料粉末和添加物的分離之發明。 【先前技術】 u 近年來隨著電子零件之微細化、高密度化，使得可以 簡便且高精確度方式安裝之焊料糊，在電子機器組裝過程 中被廣泛認知爲不可或缺之技術。 0 焊料糊係熔融焊料錠塊，利用所謂噴霧法、離心分離 法之方法，作成粒徑範圍爲數〜數十μηι程度之粉體且分級 後，混合由松脂成分、觸變劑、溶劑等所構成之焊劑，製 作而成。 但是，因爲焊劑之反應性高，即使做成焊料糊後，與 焊料粉末之間仍繼續反應，因此特性劣化。亦即，焊料糊 存在有較短的一定期間之儲藏壽命（Shelf life)。 因此，爲了延長其壽命，揭示有將焊料粉末和焊劑與 〇 氮氣等非活性氣體一起密封保存之技術（參照專利文獻1)。 且，將糊中的焊料粉末表面腐蝕作爲焊料糊特性劣化 之原因，而揭示有在焊料粉末表面使用腐蝕抑制劑之發明 (參照專利文獻2)。 但是，焊料糊長期地變化，未停止特性劣化的情形， 針對上述之先行發明，未用盡的的剩餘焊料糊，結局是作 爲廢棄物被排出。 關於焊料回收及再利用之發明，也揭示於專利文獻3， 201035328 其係揭不使從基板機械性地剝離'回收後的焊料，再熔融 且再生之方法。 上述被廢棄之焊料糊係與使從印刷基板機械性地剝離 之焊料不同’以有機物爲始含有各種物質。因此，被廢棄 之焊接的焊料糊係藉由燃燒處理的方式，分解去除有機物 成分’然後以通常的焊料之再利用方法再熔融、再利用。 [先行技術文獻] [專利文獻] 〇 [專利文獻1]日本特開平8- 1 3 22 76號公報 [專利文獻2]日本特開平8-215884號公報 [專利文獻3]日本特開2000-307239號公報 【發明內容】 [發明所欲解決之課題] 但是’如上述’燃燒處理後再熔融、且回到焊料錠塊 後再利用的方法中，爲了再生成焊料糊，必須再度投入大 量的能量進行粉體化。再者，隨著有機物分解，也大量地 ^ 釋出一氧化碳氣體或有害氣體。亦即，藉由以往已知之方 法再利用被被廢棄之焊料糊時，會有大量的能量之再投 資’或直接排出所謂的二氧化碳、有毒氣體之環境汚染物 質之課題。 [解決課題之手段] 本發明係鑑於上述課題而被想到者，其係藉由有機溶 劑洗淨焊料糊’使焊料粉和有機成分分離後再利用者。 具體而言’本發明係提供一種廢焊料糊之成分分離方 201035328 法，其具有：分類步驟，係將焊料糊回收分類；混合步驟， 係將前述被分類後的焊料糊和溶劑混合而獲得混合液；分 離步驟，係自前述混合液分離成焊料粉末、不溶性物質、 溶解性物質和前述溶劑；及乾燥步驟，係使前述焊料粉末 乾燥。. 且，本發明係提供一種廢焊料糊之再生方法，其係將 '焊劑混合分散於前述焊料粉末之焊劑分散步驟。 [發明之功效] Ο 本發明中，由於提供以藉由有機溶劑之洗淨爲基本的 成分之分離處理，因此具有可以簡便且低能量、低成本從 廢棄焊料糊分離合金粒子、松脂成分或焊劑成分等之效 果。特別是本發明中’有所謂熔融及再粉體化所要的能量 之消除、或抑制有害氣體或温室效應氣體之釋出的效果。 【實施方式】 本發明中可成分分離或再生之廢焊料糊，係數〜數十微 米大小的焊料粉末分散於焊劑中而成者。廢焊料糊因爲是 〇 可利用之物廢棄，所以將其回收並集中。 本發明基本上是藉由洗淨廢焊料糊的方式，分離焊料 粉末和焊劑’且再利用該焊料粉末。因而，同時處理多數 之糊時’必須事先區分所含有的焊料粉末之成分別。焊料 粉末之熔點係根據組成而異’因此若將不同組成之焊料粉 末放在一起，再生之焊接焊料糊的熔點將不同。 具體而言，現在作爲無鉛焊料所利用者’係以Sn爲基 本，由Ag、Cu、Bi、Zn等元素作成的2元系、3元系、4元 201035328 系爲主。且，有時也會在該等中加入微量添加元素。 本發明中再利用之廢焊料糊，係將至少主成分之元素 和含量都一致之焊料糊彼此一起處理較佳。將微量添加元 素亦一致之廢焊料糊一起處理更佳。 因而’本發明之分類步驟，亦可包含將回收來的廢焊 料糊進行組成分析之步驟。組成分析亦可直接將廢焊料糊 進行X射線質量分析。糊中所含的焊劑成分係較輕的元素， 在質量分析之結果中，與焊料粉末之峰値有明顯的差異。 焊料粉末的大小較佳亦爲同時地處理收集到的糊彼此 爲佳。焊料粉末的大小幅度爲數〜數十微米之大小。然後， 其大小之差異即是使其熔融時的熱量之差異，因此根據用 途集中大小爲適當。 焊料粉末之大小亦可利用實體顯微鏡等，直接觀察並 予以分類。因而，分類步驟亦可包含測量焊料粉之大小的 步驟。此外，集中焊料粉末之大小的分級步驟若是後來進 行，則在分類步驟時亦可不進行精確度較高的大小分類。 焊劑成分亦爲彼此成分相同的廢焊料糊彼此一起處理 較佳。因而，分類步驟中亦可包含區分焊劑的分子量之步 驟。針對於此，可適當地利用氣相層析儀。分類步驟中無 法詳盡至焊劑中的組成亦無妨。 接著，本發明之混合步驟中，將回收所收集之廢焊料 糊和溶劑混合。廢焊料糊大多含有多數之有機物和鹵素， 可使用將該等個別地溶解之溶劑。具體而言，對於松脂成 分，萜烯系溶劑較能溶解。 201035328 且，混合步驟之目的在於分離有機物成分和焊料粉 末，因此只要從焊料粉末表面洗掉有機物成分即可，有機 物成分亦可不溶解在溶劑中。就此意義而言，混合步驟也 可說是進行洗淨。因而，本發明之混合步驟中可利用之溶 劑爲大多數之有機溶劑皆可利用。 例如可舉出苯、甲苯、己烷、環己烷、二乙基醚、三 氯甲烷、乙酸乙酯、乙酸甲酯、二氯甲烷、四氯乙烷、石 油醚、稀釋劑、汽油、輕油、四氫呋喃、丙酮、乙腈、二 〇 甲基甲醯胺、二甲亞颯、甲醇、乙醇、丙醇、乙酸、甲酸、 油酸、硬脂酸、異丙醇、己基乙二醇、二乙二醇單己醚、 2-乙基己基乙二醇、2-乙基己基二乙二醇單、苯基乙二醇、 苯基二乙二醇、苄基乙二醇、苄基二乙二醇、甲基丙二醇、 甲基二丙二醇、甲基丙基三乙二醇、丙基丙二醇、丙基二 丙二醇、丁基丙二醇、丁基二丙二醇、苯基丙二醇、二甲 基乙二醇、二甲基二乙二醇 '二甲基三乙二醇、二乙基二 乙二醇、二丁基二乙二醇、二甲基二丙二醇、葱品醇等。 〇 ^ 混合之方法係將廢焊料糊投入溶劑中較佳。若一面攪 拌一面投入更佳。此時的攪拌係以橡膠片等素材較軟的攪 拌片進行攪拌較佳。因爲硬的金屬片會粉碎焊料粉末。 焊料粉末係因其製法而獲得球體狀，藉由其直徑均 等，可利用預定温度均等地熔融作爲糊。攪拌時因爲焊料 粉末粉碎而使粉末形狀變成不定形，是再利用時無法獲得 均等之熔融特性或印刷轉印量的原因。 且，亦可將超音波加在混合溶液中進行攪拌。相較於 201035328 物理式攪拌，可更有效地洗掉附著於表面之有機物成分。 接著，本發明之分離步驟中，將上述混合液分離爲焊 料粉末、不溶性物質、溶解性物質及溶劑。具體而言，靜 置混合液使焊料粉末沈澱。然後，分離沈澱後的焊料粉末 和上層澄清液成分。上層澄清液成分係不溶性物質浮在溶 解性物質溶解的溶劑中之狀態者。 上層澄清液成分可藉由進行過濾、離心分離或沈澱分 離的方式，分離爲不溶性物質和溶解性物質溶解的溶劑。 且’溶解性成分和溶劑可藉由蒸餾的方式分離。分離後的 溶劑可利用作爲再度混合步驟之溶劑。 混合步驟和分離步驟可連續進行多數次。在焊料粉末 的合金粒子表面吸附著焊劑成分，也有洗淨1次無法洗掉之 情形。在附著於焊料粉末表面的有機物，附著有活性劑之 一種的鹵化物、有機酸、胺等，也是可充分想到的。因爲 該等活性劑之反應性豐富，而有再利用焊料粉末時添加的 樹脂成分、或焊料粉末表面本身劣化之虞，也是可充分想 到的。 具體而言，做成焊料糊時，會產生儲存壽命顯著降低 的問題。因而，必須充分洗淨焊料粉末表面。 另一方面’分離後的焊料粉末係藉由乾燥步驟被乾 燥。乾燥係於室温或低於熔點温度的温度中進行較佳。若 疋較溶點局’則微小粉末會再熔融成爲錠塊。且，若是高 於使用的溶劑之沸點的温度，則可容易地使焊料粉末乾 燥。藉由如以上之步驟’可依成分分離廢焊接焊料糊。 201035328 使用乾燥後的焊料粉末再製造焊料糊時，亦可再度進 行分級。本發明可一次處理焊料之組成或大小集中的廢焊 料糊，但也有一起處理不同製造廠商的糊之情形。由於根 據製造廠商分級之等級也有不同的情形，因此從糊中分離 焊料粉末時，進行再度分級之步驟較佳。 在焊料粉末加入另外調製的焊劑，進行混煉分散，可 再度獲得焊料糊。接著利用具體之實施例進行說明。 [實施例1] 使用有機溶劑（甲苯）處理1 〇g之廢焊料糊。以下表示順 序。此外，其中的處理全部在室温（2 5 °c程度）進行。 (1) 從容器取出l〇g之廢焊接焊料。 (2) 添加10ml之甲苯。 (3) 藉由超音波或物理式分散（攪拌等）使其充分分散。 (4) 靜置至合金粒子成分沈澱。 (5) 去除上層澄清液。 (6) 試行3次（2)〜（5)。 試行後回收的合金粒子部（焊料粉末）乾燥並進行分 析。各階段回收的溶液（或分散液）進行過濾，區分爲濾液 和過濾材。濾液係藉由蒸餾操作而區分爲有機溶劑和溶解 性物質。 藉由上述操作，將廢焊料糊區分爲以下。 (a) 合金粒子部 (b) 不溶性物質（相當於過濾材） (c) 溶解性物質（藉由蒸餾回收之可溶於有機溶劑之成分） 201035328 (d)有機溶劑（此處爲甲苯） 從作爲原料使用的廢焊料糊（1〇g) ’回收到8.5〜9.2g之 合金粒子。此値和焊料糊之添加合金粒子量一致’因此可 視爲大致100%之合金粒子被回收所得者。此外’回收量之 變動係來自於廢焊料糊中的不均等性者’並非操作過程之 損失。且，除了蒸發到大氣中，（d)有機溶劑之回收率也大 致爲1 〇 〇 %。 第1圖係於藉由有機溶劑之第1次〜第3次洗淨操作之各 階段所回收的金屬粒子之掃描型電子顯微鏡（SEM ’倍率： 500倍、5000倍及15000倍）。此外，洗淨操作之1次係進行1 次上述混合步驟和分離步驟之意。照片中的白色箭號係依 照倍率，各爲 60μιη、6μιη、2μιη。 洗淨第1次之操作所回收的粒子表面係斑駁模樣’增加 倍率後，呈現粒子間被接著之狀態。隨著洗淨操作之重複 次數增加，粒子表面的斑駁模樣和粒子間之接著狀態減 少，雖然有若干殘留，但藉由3次之洗淨操作’粒子表面被 清淨化。 第2圖係於藉由有機溶劑之第1次〜第3次洗淨操作之各 階段所回收的金屬粒子之紅外分光測量（FT-IR)結果。横軸 爲波長之逆數，縱軸表示強度（任意單位）。圖中之洗淨操 作第1次係表示「洗淨1次」等。洗淨操作第1次之測量光譜 中，在1 0 0 0〜1 8 0 0 cm -1及2 8 0 0〜3 0 0 0 cm “觀測到明瞭的峰値 (以箭號表式），因此判斷大量殘存有機物。隨著洗淨操作 次數增加，該等有機物之峰値減少，因此判斷已藉由洗淨 -10- 201035328 操作充分去除有機物。 第3圖係顯示藉由有機溶劑之洗淨操作第1次（上段） 及洗淨操作第3次（下段）的SEM/EDX之元素分佈圖。分析 元素爲碳（C)、氧（0)、錫（Sn)、銀（Ag)及銅（Cu)。此外，試 料粒子係接合在碳帶（Carbon tape)進行測量。亦即，粒子 表面上碳較少時，可優先檢測出來自基材之碳帶的信號。 洗淨第1次及第3次，氧、錫、銀、銅皆以和SEM像觀測 到的粒子形狀同樣地觀測到金屬元素及氧。 Ο 關於碳，洗淨操作第3次之觀測中，碳僅存在黑圓圈10 的部分。這正表示來自粒子的下地之碳帶的反應，大致未 能觀測到來自粒子表面的反應。另一方面，清淨操作第1 次之觀測中，可觀測到碳一樣地散佈在粒子表面。亦即， 碳係根據洗淨次數而有不同的分布狀態，相對於1次之洗淨 中存在粒子表面上，在進行3次之洗淨操作後，粒子表面上 的碳量銳減。 由以上結果，了解第1圖所觀測到的粒子表面上的斑駁 〇 模樣和粒子間之接著，係1次之洗淨中未能去除的有機物， 藉由重複洗淨操作即可去除該等。 第4圖係顯示未使用的原料粉體（a)及藉由有機溶劑之 3次之洗淨操作所回收的粉體（b)之SEM的表面觀察結果。倍 率各爲3500倍和15000倍。圖中的白色箭號係3500倍爲 8·57μιη、15000 倍爲 2·0μιη。 從圖中了解到各表面狀態非常地近似，任一金屬粉表 面皆平滑。通常，考慮到金屬粒子表面係被氧化物層覆蓋， 201035328 即認爲粒子表面之平滑化係氧化被膜之溶解去除所得者° 因此，接著利用XPS測量粒子表面到粒子内部之深度影像。 第5圖係未使用的原料粉體（a)及藉由有機溶劑之3次 之洗淨操作所回收的粉體（b)之XPS的Sn(3d軌道）之分析結 果。粒子表面進行Ar氣體之5秒~3 5秒之濺鎪蝕刻，進行深 度方向之分析。横軸爲結合能量（eV)，縱軸爲每1秒的計算 數（kcps)。 從未使用原料粒子（a)最表面的影像（圖中Osec)’在 〇 486-487eV(l)僅觀測到錫氧化物之峰値，錫金屬（48 5eV前 後）之峰値（2)係於檢測界限以下。然後，隨著蝕刻時間增 加，錫氧化物之峰値（1)減少，藉由3 5秒之蝕刻成爲大致只 有錫金屬之峰値（2)。 另一方面，藉由3次之洗淨操作所回收的粉體之情形 (b)，係從最表面的影像亦觀測到錫金屬（4)，僅進行5秒之 蝕刻，成爲大致只有錫金屬之峰値（4)。由於以相同蝕刻條 件進行，因此了解回收的金屬粉之氧化物層厚度比未使用 〇 粉體薄》 第6圖係使用未使用的原料粉體（a)及藉由有機溶劑之 3次之洗淨操作所回收的粉體（b)，作成焊料糊，且回流後 之焊接基板的光學顯微鏡像之1 5 0倍像。且，使用之焊劑 含量爲12%。此外，原料粉體及回收之粉體皆爲Sn-Ag-Cu 之組成。 任一情形皆未觀測到焊料球等工業上使用過程中的障 礙。此外，觀測到回收之焊料粉體對基板之潤濕性較高。 -12- 201035328 亦即，了解藉由本處理法所再生之粉體，可直接資源回收。 [實施例2] 使用有機溶劑（甲苯）處理log之廢焊料糊。以下表示順 序。此外，以下（3)〜（5)的處理全部在70°C。 (1) 從容器取出10g之廢焊接焊料。 (2) 添加10ml之甲苯。 (3) 藉由超音波或物理式分散（攪拌等）使其充分分散。 (4) 靜置至合金粒子成分沈澱。 〇 ' (5)去除上層澄清液。 (6)試行3次（2)〜（5)。 試行後回收的合金粒子部乾燥並進行分析。將各階段 回收的溶液（或分散液）進行過濾，區分爲濾液和過濾材。 濾液係藉由蒸餾操作而區分爲有機溶劑和溶解性物質。 藉由上述操作，將廢焊料糊區分爲以下。 (a) 合金粒子部 (b) 不溶性物質（相當於過濾材） ^ (〇溶解性物質（藉由蒸餾回收之可溶於有機溶劑之成分） (d)有機溶劑（此處爲甲苯） 從作爲原料使用的廢焊料糊（l〇g)，回收到8.5〜9.2g之 合金粒子。此値和焊接焊料之添加合金粒子量一·致’因此 可視爲大致100%之合金粒子被回收所得者。此外，回收量 之變動係來自於廢焊料糊中的不均等性者，並非操作過程 之損失。且，除了蒸發到大氣中，（d)有機溶劑之回收率也 大致爲100%。 -13- 201035328 第7圖係於藉由有機溶劑之70 °C之第1次〜第3次洗淨之 各階段所回收的金屬粒子之掃描型電子顯微鏡像（SEM，倍 率：5 00倍、5 0 00倍及1 5 000倍）。此外，洗淨操作之1次係 進行1次上述混合步驟和分離步驟之意。照片中的白色箭號 係依照倍率，各爲60μιη、6μιη、2μιη。 得知與室温處理的情形同樣地，洗淨操作第1次之操作 所回收的粒子表面形成斑駁模樣，增加倍率後，呈現粒子 間被接著之狀態。隨著洗淨操作之增加，粒子表面的斑駁 〇 模樣和粒子間之接著狀態減少，雖然有若干殘留，但藉由3 次之洗淨操作，粒子表面被清淨化。但是，雖然有若干， 但觀測到有機物之殘留量較室温處理爲多之傾向。 [實施例3] 本實施例中’針對再生之焊料糊的儲藏性（儲存壽命） 進行說明。所用之焊料粉係於實施例1中洗淨操作1次、2 次、3次者，使以下組成之焊劑對焊料粉末爲丨〇重量份、混 煉而得之焊料糊。此外，作爲比較例，亦準備有利用從未 Ο 使用的錠塊製作而得之焊料粉末之焊料糊。 焊劑組成係丙烯酸改質松香爲50重量份、二乙二醇單 己醚爲3 6重量份、硬化篦麻油爲1 〇重量份、鹵系活性劑爲3 重量份、戊二酸爲1重量份。 且，作爲溶劑可使用者爲己二醇、丁基乙二醇、二乙 二醇單己醚、葱品醇等通常之焊劑所使用者。溶劑係於 20〜80重量％、較佳爲30~60重量％之範圍內使用於焊劑中。 關於儲藏性，在製作糊之後直接放入容量500cc之塑膠 -14- 201035328 容器，於35 °C之環境下放置。此外，製作多數瓶之各個糊， 一旦開封後之糊，即針對其後之儲藏性進行觀察。亦即， 儲藏性就是觀察封入容器且經過預定時間後首次被開封之 糊。 儲藏性之評價係以測量開封後的容器内之糊的黏度之 方式予以評價。黏度係以JISZ3 2 84附屬書6之螺旋式黏度計 (10旋轉）測量出。結果顯示於表1。 【表1】 洗淨1次 洗淨2次 洗淨3次 現行粉末 製造時黏度 136Pa«s 170 Pa*s 201 Pa#s 200 Pa.s 焊劑含量 16% 14% 12% 12% 翌曰黏度 (35°C之環境） 170 Pa#s 240 Pa#s 201 Paes 200 Pa*s 洗淨1次的情形，係洗淨後之液體混濁，即使乾燥也不 形成粉末狀態，而是形成塊狀（糊凝固之狀態）。使用它製 造焊料糊時，較使用未使用之焊料粉末而成之糊黏度還要 〇 更低。且，即使與新的焊劑成分混煉，焊料糊中仍殘存塊 狀物。 使用未使用之焊料粉末而成的焊料糊，在剛製造後顯 示大約200Pa · S程度之黏度。該黏度降低則對印刷性造成 影響而不佳。且，儘管全部的焊劑含量以12%調整，使用 洗淨1次和2次之焊料粉末者仍較使用未使用之焊料粉末者 之黏度低。 且，製造後測量各焊劑含量時，使用洗淨1次和2次之 -15- 201035328 焊料粉末者，被檢測出較調製時添加之焊劑量（12%)更 多。認爲其係因焊料粉末表面殘留有焊劑量’所以含量增 加、黏度降低。且’放置在35°c之環境後’使用洗淨1次、 2次之焊料粉末者’在第1日產生黏度上升。根據以上情形’ 使用洗淨次數1次、2次之焊料粉末者’無法達到目的之黏 度設定，且儲藏性差。 洗淨2次的情形，較洗淨1次之洗淨液顏色呈現接近透 明之白濁色。乾燥後，大致形成粉末狀態’但部分存在有 〇 塊狀物。使用它製造焊料糊時’黏度若干低於使用未使用 之焊料粉末而成的糊。且’焊料糊中部分存在有塊狀。然 後，終究在製造1日後黏度上升。因而，儲藏性差。 洗淨3次的情形，洗淨液完全形成透明，乾燥後完全呈. 現粉末狀態。使用它製造焊料糊時，可獲得和使用未使用 之焊料粉末時相同的黏度。且，儲藏性亦與由未使用之焊 料粉末製作的糊相同之性能。 未能完全去除焊劑時，即使乾燥也不形成粉末狀態， 〇 而是形成塊狀（糊凝固之狀態）。因此，認爲即使以相同之 焊劑含量製造，實際上焊劑含量會變多、黏度會降低。亦 即，未能完全洗淨焊料粉末表面時，焊劑含量會因洗淨情 況產生變化，黏度根據每批次呈現不穩定。 且，存在有塊狀物時，印刷時之轉印率不穩定，成爲 不良品之原因。其係因近年來發展零件微細間距化，因此 被印刷之圖案也被微細間距化，若存在有這種塊狀物，則 印刷時的轉印率不穩定將招致品質不良之結果。 -16 - 201035328 且，未能完全去除焊劑時，目的以外的焊劑成分將混 入，無法發揮本來的性能，對儲藏性等造成不良影響。因 此，最低必須3次以上（視情況至液體呈透明爲止之）洗淨。 洗淨程度會有根據廢焊料糊之糊量而異之情形。於該 情形下，可將洗淨所用的溶劑之透過率作爲指標。具體而 言係比較光對作爲基準之無色透明液體的透過率和洗淨液 之光的透過率。此外，作爲基準之液體爲純水即可。 其係將作爲基準之液體以及洗淨液放置於僅離開預定 〇 距離長所設置之光源和受光體之間之受光部的光強度比作 比較者。洗淨液中所含的雜質愈少，相對於作爲基準之液 體的透過率愈接近1。相對於作爲基準之液體而言，本發明 顯示至少80%以上、較佳爲90%以上之透過率爲佳。 表2係顯示洗淨後的溶液之透過率的測量結果。測量係 於具有5 cm之間隔的平行玻璃平面之容器加入洗淨後的溶 液，將白色LED光從一方之玻璃平面垂直地照射，在另一 方之玻璃平面放置受光元件，測量出透過光的強度作爲受 ^ 光元件之輸出電壓。然後，將純水時的透過率設爲1 0 0 %時 之値。 【表2】 洗淨1次 洗淨2次 洗淨3次 純水(基準） 透過率 50% 70% 100% 100% 根據以上結果，藉由本處理法，廢焊料糊中的金屬粒 子表面係藉由有機溶劑之洗淨而被清淨化，其回收率爲大 致1 0 0 %，可直接作爲資源回收粉體再利用。再者，相較於 -17- 201035328 剛從錠塊製作後的焊料粉末，由於表面氧化物層薄，因此 可說是較以往富於反應性之粒子。且，回收之有機物質亦 因對使用之有機溶劑的溶解度差而被分離，可以再利用。 洗淨所用的有機溶劑亦於除去蒸發部分後，可1〇〇%資源回 收。 [産業上的利用性] 本發明可適合利用於焊料糊資源回收。 【圖式簡單說明】 0 第1圖係於藉由有機溶劑之第1次〜第3次洗淨之各階 段所回收的金屬粒子之掃描型電子顯微鏡（SEM,倍率：500 倍、5 000倍及1 5 000倍）。 第2圖係於藉由有機溶劑之第1次〜第3次洗淨之各階 段所回收的金屬粒子之紅外分光測量（FT-IR)結果。 第3圖係顯示藉由有機溶劑之洗淨第1次（上段）及洗 淨第3次（下段）的SEM/EDX之元素分佈圖的照片。 第4圖係顯示未使用的原料粉體（a)及藉由有機溶劑之 ^ 3次之洗淨操作所回收的粉體（b)之SEM的表面觀察結果的 照片。 第5圖係未使用的原料粉體（a)及藉由有機溶劑之3次 之洗淨操作所回收的粉體（b)之XPS的Sn(3d軌道）之分析 結果之影像。 第6圖係使用未使用的原料粉體（a)及藉由有機溶劑之 3次之洗淨操作所回收的粉體（b)，作成焊料糊，且回流後 之焊接基板的光學顯微鏡像之照片。 -18- 201035328 第7圖係於藉由70 °C之有 淨之各階段所回收的金屬粒 (SEM > 倍率：500 倍、5000 倍 【主要元件符號說明】 Μ 。 機溶劑之第1次〜第3次洗 子之掃描型電子顯微鏡像 及 1 5 0 0 0 倍）。201035328 VI. Description of the Invention: [Technical Field] The present invention relates to the invention of the recovery of solder resources, and more particularly to the invention of separation of solder powder and additives when the solder paste is reused. [Prior Art] In recent years, with the miniaturization and high density of electronic components, solder pastes that can be mounted in a simple and highly accurate manner have been widely recognized as indispensable technologies in the assembly process of electronic devices. 0 A solder paste-based molten solder ingot is prepared by a method such as a so-called spray method or a centrifugal separation method, and a powder having a particle size ranging from several to several tens of μm is classified, and then mixed with a rosin component, a thixotropic agent, a solvent, or the like. Made of flux, made. However, since the flux has high reactivity, even after the solder paste is formed, the reaction continues with the solder powder, so that the characteristics are deteriorated. That is, the solder paste has a short shelf life (Shelf life). Therefore, in order to prolong the life thereof, a technique of sealing and storing solder powder and flux together with an inert gas such as helium nitrogen gas has been disclosed (see Patent Document 1). Further, the surface corrosion of the solder powder in the paste is a cause of deterioration of the characteristics of the solder paste, and an invention in which a corrosion inhibitor is used on the surface of the solder powder has been disclosed (see Patent Document 2). However, in the case where the solder paste is changed for a long period of time and the characteristic deterioration is not stopped, the remaining solder paste which has not been used up in the above-described first invention is discharged as waste. The invention for the recovery and reuse of the solder is also disclosed in Patent Document 3, 201035328, which discloses a method of mechanically peeling off the recovered solder from the substrate, remelting and regenerating. The discarded solder paste is different from the solder which is mechanically peeled off from the printed substrate. The organic material contains various substances. Therefore, the solder paste to be discarded is decomposed and removed by the combustion treatment, and then remelted and reused by a usual solder re-use method. [PRIOR ART DOCUMENT] [Patent Document 1] Japanese Laid-Open Patent Publication No. Hei No. Hei 8-215884 (Patent Document 3) JP-A-2000-307239 [Brief Description of the Invention] [Problem to be Solved by the Invention] However, in the method of remelting after the combustion treatment and returning to the solder ingot as described above, in order to regenerate the solder paste, a large amount of energy must be reinvested. Powdering. Furthermore, as the organic matter decomposes, carbon monoxide gas or harmful gas is also released in a large amount. That is, when the discarded solder paste is reused by a conventionally known method, there is a large amount of energy re-investment or direct discharge of so-called environmental pollutants of carbon dioxide and toxic gases. [Means for Solving the Problem] The present invention has been conceived in view of the above problems, and the solder powder is washed by an organic solvent to separate the solder powder from the organic component and reused. Specifically, the present invention provides a component separation method of a waste solder paste 201035328, which has a classification step of classifying a solder paste, and a mixing step of mixing the above-mentioned classified solder paste and a solvent to obtain a mixture. a liquid separation step of separating the mixture into a solder powder, an insoluble material, a soluble substance, and the solvent; and a drying step of drying the solder powder. Further, the present invention provides a method of regenerating a waste solder paste by mixing and dispersing a flux in a flux dispersing step of the solder powder. [Effects of the Invention] In the present invention, since the separation treatment is based on the cleaning of the organic solvent, the alloy particles, the rosin component or the flux can be separated from the waste solder paste in a simple, low-energy, low-cost manner. The effect of ingredients, etc. In particular, in the present invention, there is an effect of eliminating the energy required for melting and re-pulping, or suppressing the release of harmful gases or greenhouse gases. [Embodiment] In the present invention, a waste solder paste which can be separated or regenerated by a component is obtained by dispersing a solder powder having a coefficient of several tens of micrometers in a flux. The waste solder paste is discarded because it is available, so it is collected and concentrated. The present invention basically separates the solder powder and the solder by the method of washing the waste solder paste and reuses the solder powder. Therefore, when a plurality of pastes are simultaneously processed, it is necessary to distinguish the solder powders contained in advance separately. The melting point of the solder powder varies depending on the composition. Therefore, if solder powders of different compositions are put together, the melting point of the regenerated solder paste will be different. Specifically, the user who is currently used as a lead-free solder is based on Sn, and a ternary system, a ternary system, and a 4-membered 201035328 which are mainly composed of elements such as Ag, Cu, Bi, and Zn are mainly used. Moreover, a trace amount of an additive element may be added to these. The waste solder paste to be reused in the present invention is preferably treated with at least a solder paste in which the elements and contents of the main component are the same. It is better to treat the waste solder paste which is also consistent with the trace amount of added elements. Thus, the classification step of the present invention may further comprise the step of performing compositional analysis of the recovered waste solder paste. The composition analysis can also directly perform the X-ray quality analysis of the waste solder paste. The flux component contained in the paste is a lighter element, and in the result of the mass analysis, there is a significant difference from the peak of the solder powder. It is preferable that the size of the solder powder is also such that the collected pastes are treated at the same time. The size of the solder powder is in the range of several to several tens of micrometers. Then, the difference in size is the difference in the amount of heat when it is melted, and therefore it is appropriate depending on the size of the use. The size of the solder powder can also be directly observed and classified using a stereo microscope or the like. Thus, the sorting step can also include the step of measuring the size of the solder powder. Further, if the grading step of concentrating the size of the solder powder is performed later, the classification of the size with higher accuracy may not be performed at the classification step. It is preferable that the flux composition is also treated with waste solder pastes having the same composition as each other. Thus, the step of classifying may also include the step of distinguishing the molecular weight of the flux. For this, a gas chromatograph can be suitably used. It is also possible that the classification step cannot be detailed to the composition of the flux. Next, in the mixing step of the present invention, the collected waste solder paste and the solvent are recovered and mixed. Most of the waste solder paste contains a large amount of organic matter and halogen, and these solvents which are individually dissolved can be used. Specifically, the terpene-based solvent is more soluble in the rosin component. 201035328 Moreover, the purpose of the mixing step is to separate the organic component and the solder powder. Therefore, the organic component may not be dissolved in the solvent as long as the organic component is washed away from the surface of the solder powder. In this sense, the mixing step can also be said to be washed. Thus, the solvent which can be utilized in the mixing step of the present invention is available to most organic solvents. Examples thereof include benzene, toluene, hexane, cyclohexane, diethyl ether, chloroform, ethyl acetate, methyl acetate, dichloromethane, tetrachloroethane, petroleum ether, diluent, gasoline, and light. Oil, tetrahydrofuran, acetone, acetonitrile, dimethyl methionine, dimethyl hydrazine, methanol, ethanol, propanol, acetic acid, formic acid, oleic acid, stearic acid, isopropanol, hexyl glycol, diethyl Glycol monohexyl ether, 2-ethylhexyl glycol, 2-ethylhexyl diethylene glycol mono, phenylethylene glycol, phenyl diethylene glycol, benzyl glycol, benzyl diethylene Alcohol, methyl propylene glycol, methyl dipropylene glycol, methyl propyl triethylene glycol, propyl propylene glycol, propyl dipropylene glycol, butyl propylene glycol, butyl dipropylene glycol, phenyl propylene glycol, dimethyl glycol, two Methyl diethylene glycol 'dimethyl triethylene glycol, diethyl diethylene glycol, dibutyl diethylene glycol, dimethyl dipropylene glycol, onion alcohol, and the like. 〇 ^ The method of mixing is preferably to put the waste solder paste into a solvent. It is better if you stir on one side. The agitation at this time is preferably carried out by stirring a soft agitating piece such as a rubber sheet. Because the hard metal sheet will smash the solder powder. The solder powder is obtained in a spherical shape by the production method, and by equalizing its diameter, it can be uniformly melted as a paste by a predetermined temperature. When the powder is pulverized during stirring, the shape of the powder becomes amorphous, which is why the same melt characteristics or printing transfer amount cannot be obtained at the time of reuse. Further, ultrasonic waves may be added to the mixed solution for stirring. Compared to the 201035328 physical agitation, the organic components attached to the surface can be washed more effectively. Next, in the separation step of the present invention, the mixed liquid is separated into a solder powder, an insoluble matter, a soluble substance, and a solvent. Specifically, the mixture is allowed to stand to precipitate the solder powder. Then, the precipitated solder powder and the supernatant liquid component are separated. The upper clear liquid component is in a state in which the insoluble matter floats in the solvent in which the soluble substance is dissolved. The upper clear liquid component can be separated into a solvent in which the insoluble matter and the soluble substance are dissolved by filtration, centrifugation or precipitation separation. And the 'soluble component and solvent can be separated by distillation. The separated solvent can be used as a solvent for the remixing step. The mixing step and the separating step can be carried out continuously for a plurality of times. The flux component is adsorbed on the surface of the alloy particles of the solder powder, and it may be washed once and cannot be washed off. It is also conceivable that a halide, an organic acid, an amine or the like which adheres to an organic substance adhering to the surface of the solder powder to the active material. Since the reactivity of the active agents is rich, it is also conceivable that the resin component added when the solder powder is reused or the surface of the solder powder itself is deteriorated. Specifically, when a solder paste is formed, there is a problem that the storage life is remarkably lowered. Therefore, the surface of the solder powder must be sufficiently washed. On the other hand, the separated solder powder is dried by a drying step. Drying is preferably carried out at a temperature of room temperature or below the melting point. If the 疋 is more concentrated, the tiny powder will remelt into the ingot. Further, if the temperature is higher than the boiling point of the solvent to be used, the solder powder can be easily dried. The solder solder paste can be separated by composition according to the above steps. 201035328 When re-manufacturing solder paste using dried solder powder, it can be graded again. The present invention can treat the waste solder paste with a concentrated composition or size of the solder at a time, but it also has a case where the paste of different manufacturers is handled together. Since the grades according to the manufacturer are also different, it is preferable to perform the step of re-grading when separating the solder powder from the paste. A solder paste is added to the solder powder to carry out kneading and dispersing, and the solder paste can be obtained again. Description will be made using specific embodiments. [Example 1] A waste solder paste of 1 〇g was treated with an organic solvent (toluene). The following shows the order. Further, all of the treatments were carried out at room temperature (about 25 ° C). (1) Remove l〇g of scrap solder from the container. (2) Add 10 ml of toluene. (3) It is sufficiently dispersed by ultrasonic or physical dispersion (stirring, etc.). (4) Allow to stand until the alloy particles are precipitated. (5) Remove the upper clear solution. (6) Trial 3 times (2) ~ (5). The alloy particle portion (solder powder) recovered after the trial was dried and analyzed. The solution (or dispersion) recovered in each stage is filtered and classified into a filtrate and a filter. The filtrate is classified into an organic solvent and a soluble substance by a distillation operation. By the above operation, the waste solder paste is classified into the following. (a) Alloy particle part (b) Insoluble matter (corresponding to filter material) (c) Solubility substance (component soluble in organic solvent by distillation) 201035328 (d) Organic solvent (here, toluene) The waste solder paste (1 〇 g) used as a raw material 'recovered 8.5 to 9.2 g of alloy particles. This is the same as the amount of the alloy particles added to the solder paste. Therefore, it can be considered that approximately 100% of the alloy particles are recovered. In addition, the change in the amount of recovery is due to the inequality in the waste solder paste, which is not a loss of operation. Moreover, in addition to evaporation to the atmosphere, (d) the recovery rate of the organic solvent is also approximately 1 〇 〇 %. Fig. 1 is a scanning electron microscope (SEM apos; magnification: 500 times, 5000 times, and 15000 times) of metal particles recovered by each stage of the first to third cleaning operations of the organic solvent. Further, the washing operation was performed once for the above mixing step and separation step. The white arrows in the photographs are in accordance with the magnifications, each being 60 μm, 6 μm, and 2 μm. The surface of the particles recovered by the first operation is washed, and the magnification is increased, and then the state between the particles is followed. As the number of repetitions of the washing operation increases, the mottled pattern on the surface of the particles and the subsequent state between the particles are reduced, and although there are some residues, the surface of the particles is cleaned by the washing operation three times. Fig. 2 is a result of infrared spectroscopic measurement (FT-IR) of metal particles recovered at each stage of the first to third washing operations of the organic solvent. The horizontal axis represents the inverse of the wavelength, and the vertical axis represents the intensity (arbitrary unit). The first washing operation in the figure indicates "washing once" and the like. In the first measurement spectrum of the cleaning operation, at 1 0 0 0 to 1 0 0 0 cm -1 and 2 8 0 0 to 3 0 0 0 cm "A clear peak was observed (in the form of an arrow), Therefore, a large amount of residual organic matter is judged. As the number of washing operations increases, the peak of the organic matter decreases, so that it is judged that the organic matter has been sufficiently removed by the washing operation of -10-201035328. Fig. 3 shows the washing by the organic solvent. Elemental map of SEM/EDX for the first (upper) and third (lower) cleaning operations. The analysis elements are carbon (C), oxygen (0), tin (Sn), silver (Ag), and copper. (Cu) Further, the sample particles are bonded to a carbon ribbon for measurement, that is, when the carbon content on the surface of the particles is small, the signal from the carbon ribbon of the substrate can be preferentially detected. In the third time, oxygen, tin, silver, and copper all observed metal elements and oxygen in the same manner as the particle shape observed by the SEM image. Ο About carbon, in the third observation of the cleaning operation, carbon only has a black circle 10 The part that represents the reaction of the carbon band from the lower ground of the particle, and the reflection from the surface of the particle is hardly observed. On the other hand, in the first observation of the clean operation, it is observed that carbon is scattered on the surface of the particles. That is, the carbon system has different distribution states depending on the number of times of washing, and is compared with the one-time washing. On the surface of the particles, after three washing operations, the amount of carbon on the surface of the particles is sharply reduced. From the above results, it is understood that the mottled ruthenium pattern on the surface of the particles observed in Fig. 1 and the subsequent between the particles are The organic matter that has not been removed in the first wash can be removed by repeating the washing operation. Fig. 4 shows the unused raw material powder (a) and the three-time washing operation by the organic solvent. The surface observation result of the SEM of the recovered powder (b) was 3500 times and 15000 times each. The white arrow number in the figure was 3,500 times of 8.57 μm, and 15,000 times was 2·0 μιη. The surface state of each metal is very similar, and the surface of any metal powder is smooth. Generally, considering that the surface of the metal particle is covered by the oxide layer, 201035328 considers that the smoothing of the surface of the particle is dissolved by the oxide film. Therefore, Using XPS The depth image of the particle surface to the inside of the particle. Fig. 5 is the raw material powder (a) and the powder recovered by the three-time washing operation of the organic solvent (b) of the XPS Sn (3d orbital) As a result of the analysis, the surface of the particle was subjected to a sputtering process for 5 seconds to 35 seconds of Ar gas, and the depth direction was analyzed. The horizontal axis is the binding energy (eV), and the vertical axis is the number of calculations per second (kcps). The image of the outermost surface of the raw material particle (a) (Osec in the figure) is only observed at 〇486-487eV(l), and the peak of tin oxide (before and after 48 5eV) is tied to Below the detection limit. Then, as the etching time increases, the peak 値(1) of the tin oxide decreases, and the etch of 35 seconds becomes a peak of only tin metal (2). On the other hand, in the case of the powder recovered by the three-time washing operation (b), the tin metal (4) was observed from the image on the outermost surface, and only 5 seconds of etching was performed to become substantially only tin metal. Peak 値 (4). Since it is carried out under the same etching conditions, it is understood that the thickness of the oxide layer of the recovered metal powder is thinner than that of the unused bismuth powder. Fig. 6 uses unused raw material powder (a) and three times of washing with an organic solvent. The powder (b) recovered by the net operation was used as a solder paste, and the image of the optical microscope of the soldered substrate after the reflow was 150 times. Also, the flux content used was 12%. Further, the raw material powder and the recovered powder are all composed of Sn-Ag-Cu. In any case, no obstacles in industrial use such as solder balls were observed. Further, it was observed that the recovered solder powder had a high wettability to the substrate. -12- 201035328 That is, the powder recovered by this treatment method can be directly recovered from resources. [Example 2] A log waste solder paste was treated with an organic solvent (toluene). The following shows the order. Further, the following treatments (3) to (5) were all at 70 °C. (1) Remove 10 g of scrap solder from the container. (2) Add 10 ml of toluene. (3) It is sufficiently dispersed by ultrasonic or physical dispersion (stirring, etc.). (4) Allow to stand until the alloy particles are precipitated. 〇 ' (5) Remove the upper clear solution. (6) Trial 3 times (2) ~ (5). The alloy particle portion recovered after the trial was dried and analyzed. The solution (or dispersion) recovered in each stage is filtered and classified into a filtrate and a filter. The filtrate is classified into an organic solvent and a soluble substance by a distillation operation. By the above operation, the waste solder paste is classified into the following. (a) Alloy particle part (b) Insoluble matter (corresponding to filter material) ^ (〇Soluble substance (component soluble in organic solvent by distillation) (d) Organic solvent (here, toluene) The waste solder paste (10 g) used in the raw material was recovered to 8.5 to 9.2 g of the alloy particles. The amount of the alloy particles added to the solder and the solder was one of the results, so that it was considered that approximately 100% of the alloy particles were recovered. In addition, the change in the amount of recovery comes from the inhomogeneity in the waste solder paste, and is not a loss of operation. Moreover, in addition to evaporation to the atmosphere, (d) the recovery rate of the organic solvent is also approximately 100%. 201035328 Fig. 7 is a scanning electron microscope image of a metal particle recovered by each stage of the first to third cleaning of the organic solvent at 70 ° C (SEM, magnification: 500 times, 500 00 In addition, the washing operation is performed once for the above mixing step and separation step. The white arrows in the photograph are 60 μm, 6 μm, and 2 μm each according to the magnification. In the case of room temperature treatment, the washing operation is the same. The surface of the particles recovered by the operation of the first operation forms a mottled pattern, and after increasing the magnification, the state between the particles is followed. As the washing operation increases, the mottled appearance of the surface of the particle and the subsequent state between the particles are reduced, although there are several Residual, but the surface of the particles was cleaned by three washing operations. However, although there were some, it was observed that the residual amount of organic matter was much higher than that at room temperature. [Embodiment 3] The storage property (storage life) of the regenerated solder paste will be described. The solder powder used in the first embodiment is washed once, twice, or three times in the first embodiment, and the flux of the following composition is used as the weight of the solder powder. In addition, as a comparative example, a solder paste of a solder powder obtained by using an ingot which has never been used is also prepared. The flux composition is 50 parts by weight of acrylic modified rosin, and two The diol monohexyl ether is 36 parts by weight, the hardened castor oil is 1 part by weight, the halogenated active agent is 3 parts by weight, and the glutaric acid is 1 part by weight. Further, as a solvent, the user can be hexanediol. A user of a usual flux such as glycol, diethylene glycol monohexyl ether or onion alcohol. The solvent is used in the flux in the range of 20 to 80% by weight, preferably 30 to 60% by weight. Storage, after the paste is prepared, directly put into a plastic container of 500cc capacity - 14-201035328, and place it at 35 ° C. In addition, make each paste of most bottles, once the paste is opened, it is stored for the subsequent storage. The storage property is the observation that the paste is sealed for the first time after being sealed for a predetermined period of time. The evaluation of the storage property is evaluated by measuring the viscosity of the paste in the container after the opening. The viscosity is JISZ3 2 84 The spiral viscometer (10 rotation) of Attachment 6 was measured. The results are shown in Table 1. [Table 1] Washing once, washing twice, washing 3 times, current powder production, viscosity 136Pa«s 170 Pa*s 201 Pa#s 200 Pa.s flux content 16% 14% 12% 12% 翌曰 viscosity ( 170°C environment) 170 Pa#s 240 Pa#s 201 Paes 200 Pa*s When washing once, the liquid after washing is turbid, even if it is dry, it does not form a powder, but forms a block (paste) The state of solidification). When it is used to make a solder paste, the paste viscosity is lower than that of the unused solder powder. Moreover, even if it is kneaded with a new flux component, a block remains in the solder paste. A solder paste using unused solder powder exhibits a viscosity of about 200 Pa·s immediately after fabrication. This decrease in viscosity does not affect printability. Further, although the total flux content was adjusted by 12%, the use of the solder powder for one or two times of cleaning was lower than that of the unused solder powder. Further, when the content of each flux was measured after the production, the solder powder of -15-201035328 which was washed once and twice was detected to be more than the amount of solder added (12%) at the time of preparation. It is considered that the amount of solder is left on the surface of the solder powder, so the content is increased and the viscosity is lowered. In the case where the product was placed in an environment of 35 ° C and the solder powder was washed once or twice, the viscosity increased on the first day. According to the above situation, the use of the solder powder once and twice the number of times of soldering is not able to achieve the desired viscosity setting, and the storage property is poor. In the case of washing twice, the color of the washing liquid which is washed one time is close to the transparent white turbid color. After drying, it is roughly in a powder state 'but a part of the lumps are present. When it is used to manufacture a solder paste, the viscosity is somewhat lower than that of using an unused solder powder. And there is a block in the portion of the solder paste. Then, after all, the viscosity increased after one day of manufacture. Therefore, the storage property is poor. In the case of washing 3 times, the washing liquid is completely transparent, and after drying, it is completely in a powder state. When it is used to manufacture a solder paste, the same viscosity as when using an unused solder powder can be obtained. Moreover, the storage property is also the same as that of the paste made of the unused solder powder. When the flux is not completely removed, even if it is dried, no powder is formed, and 〇 is formed into a block shape (a state in which the paste is solidified). Therefore, it is considered that even if the same flux content is used, the flux content is actually increased and the viscosity is lowered. That is, when the surface of the solder powder is not completely washed, the flux content changes due to the washing condition, and the viscosity is unstable depending on each batch. Further, when a block is present, the transfer rate at the time of printing is unstable, which is a cause of defective products. Since the number of parts is finely pitched in recent years, the pattern to be printed is also finely pitched. If such a block is present, the transfer rate at the time of printing is unstable, resulting in poor quality. -16 - 201035328 In addition, when the flux is not completely removed, the flux components other than the target are mixed, and the original performance cannot be exhibited, which adversely affects the storage property. Therefore, it must be washed at least 3 times (depending on the liquid to be transparent). The degree of washing will vary depending on the amount of paste of the waste solder paste. In this case, the transmittance of the solvent used for the washing can be used as an index. Specifically, the transmittance of light as a reference colorless transparent liquid and the transmittance of light of the cleaning liquid are compared. Further, the liquid as a reference may be pure water. This is a comparison of the light intensity ratio of the reference liquid and the cleaning liquid placed on the light receiving portion between the light source and the light receiving body which are disposed only apart from the predetermined length. The less impurities contained in the cleaning liquid, the closer the transmittance to the liquid as a reference is. The present invention exhibits a transmittance of at least 80% or more, preferably 90% or more, relative to the liquid as a reference. Table 2 shows the measurement results of the transmittance of the washed solution. The measurement system is added to the cleaned solution in a container having a parallel glass plane with a spacing of 5 cm, and the white LED light is vertically irradiated from one of the glass planes, and the light-receiving element is placed on the other glass plane to measure the intensity of the transmitted light. As the output voltage of the light-receiving element. Then, when the transmittance in pure water is set to 100%. [Table 2] Washing once, washing twice, washing 3 times of pure water (reference) Transmittance 50% 70% 100% 100% According to the above results, the surface of the metal particles in the waste solder paste is borrowed by this treatment method. It is cleaned by washing with an organic solvent, and its recovery rate is approximately 100%, which can be directly reused as a resource recovery powder. Furthermore, compared with -17-201035328, the solder powder immediately after the ingot production is thinner than the surface oxide layer, so it can be said to be more reactive particles. Moreover, the recovered organic matter is also separated due to the poor solubility of the organic solvent used, and can be reused. The organic solvent used for the washing can also be recovered by 1% of the resources after the evaporation portion is removed. [Industrial Applicability] The present invention can be suitably used for the recovery of solder paste resources. [Simple description of the drawing] 0 Fig. 1 is a scanning electron microscope (SEM, magnification: 500 times, 5,000 times) of metal particles recovered by each stage of the first to third washing of the organic solvent. And 15,000 times). Fig. 2 is a result of infrared spectroscopic measurement (FT-IR) of metal particles recovered by each stage of the first to third washing of the organic solvent. Fig. 3 is a photograph showing an elemental distribution of SEM/EDX of the first (upper stage) and third (lower stage) washing by an organic solvent. Fig. 4 is a photograph showing the surface observation results of the SEM of the unused raw material powder (a) and the powder (b) recovered by the washing operation of the organic solvent. Fig. 5 is an image of the analysis result of the Sn (3d orbital) of the XPS of the powder (b) recovered by the unused raw material powder (a) and the three-time washing operation of the organic solvent. Fig. 6 is a view showing an optical microscope image of a solder substrate after the reflow, using the unused raw material powder (a) and the powder (b) recovered by the three-time washing operation of the organic solvent. photo. -18- 201035328 Figure 7 is a metal particle recovered by each stage at 70 °C (SEM > magnification: 500 times, 5000 times [main symbol description] 。. The first time of machine solvent ~ Scanning electron microscope image of the 3rd wash and 1 500 times).
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