559566 A7 B7 五、發明説明（1 ) 發明領域 (請先閱讀背面之注意事項再填寫本頁) 本發明大致有關飽和液純化法。更明確地，本發明有 關在汽化過程中使用微波能量純化飽和液以產生超高純度 氣體之方法。 發明背景 半導體製造設備使用之加工用氣通常透過圓筒供給。 爲了滿足這些氣體之高流速產品與超高純度要求之漸增需 求，氣體製造商通常使用超高純度大型汽化傳輸系統以處 理極性液化壓縮氣。一般說來，該在地（on-site )系統利用 微波能量來源而增加並控制水性極性液（如氨）之蒸發率 。該在地系統可提供純化、更短的響應時間，及在非常高 流速（對半導體產業大體量超過1 0 0 0升/分鐘）下準 確的可控制蒸發。爲維持極性液化混合物之蒸發，必須加 入能量於此系統中取代由客戶使用端得到之氣流熱氣。若 不如此做，氣體中之溫度降低且極性液之蒸發率減至汽-液灘最後接近冷卻而使所有蒸汽流動停止。 經濟部智恶財產局8工消費合作社印製 . 若液化氣需要另外純化，汽化器系統可減少傳輸至汽 相之雜質量，因而加入純化步驟。該雜質會因液體蒸發自 汽相中排除並保留在液灘中，其包括第I族、第I I族及 第I I I族金屬，和這些元素的氧化物、碳酸鹽、氫化物 和鹵化物。這些雜質源自一些包括閥驅動之摩擦、液體容 器之熱膨脹和收縮、裝塡時之器皿容器開口伸張或膨脹壓 ......等等。水氣是#質之另一來源。根據汽-液平衡平衡 本紙張尺度適用中國"^家標準（CNS ) A4規格（210X 297公釐） T '~" 559566 A7 B7 五、發明説明（2) (請先閲讀背面之注意事項再填寫本頁} 資料，液相水氣濃度約爲汽相濃度的2 - 3倍。仔細處理 液相變成汽相之蒸發可減少數量等級之水氣與其他非揮發 性殘留物（non-volatile residues, NVR )。 傳輸純化氣之一般實例是通過汽化器方法，其使用電 阻加熱。自儲存槽抽出蒸汽並以內部加熱器或外部傳動加 熱器（external band heater)之熱源加熱以提供超過周圍可 得熱能之熱能。該蒸汽隨即與非低溫液化壓縮氣通過熱交 •換器而進一步促成儲存槽中之蒸發。傳導與對流由線路來 源（其增加系統之響應時間）傳送熱度至整體液體。使用 沈浸型加熱器或殻狀與管狀熱交換器可釋出微粒並充當雜 質沸騰（如水氣）核晶過程來源，因爲該核晶過程來源大 致比整體液體熱。攪動促進沸騰成梯度且核晶過程部位於 是產生。攪動亦增進非揮發性殘留物移動，增加轉成汽相 之可能性。 美國專利號碼第4，6 7 1 ，9 5 2號揭示由不純之 液態二氧化硫產生二氧化硫氣體之加工法與裝置。該加工 法使用不純之液態二氧化硫並以9 1 5、2 4 5 0、 經濟部智慈財產局8工消资合作社印製 5 8 5 0，或1 8 0 0 0 Μ Η z之頻率接受微波能源持續 足以產生二氧化硫氣體之時間，若有的話，收集該氣體並 去除所得之不純液態二氧化硫。該二氧化硫之蒸發壓在 70°F爲34 · 4p s i g且二氧化硫之純度達到 9 8.9 9 %。 美國專利號碼第4，2 8 5，7 7 4號揭示自啤酒連 續產生濃縮醇之裝置。將數個濃縮機室與數個廢物利用室 -5 - 本紙張尺度適用中國國家標準（CNS ) A4規格（210X 297公釐） 559566 A7 __B7__ 五、發明説明（3) (salvage cells )相連並排成一列。透過供給導管供應啤酒 (請先閱讀背面之注意事項再填寫本頁) .至第一個上游濃縮機室。然後啤酒流過對應啤酒體積相鄰 室中之通道達到相鄰上游室之預定水準。位於每室中之微 波點火球（ignition bulb )加熱啤酒並沸騰或蒸發醇含量。 該氣體醇透過每一濃縮機室至次一個相鄰上游室之液體通 道連續起泡直到氣體醇達到第一濃縮機室（其中氣體醇濃 縮且冷凝於管柱中成爲約含9 5 %醇和約5 %水之液態溶 液）。由稀釋液獲得醇，回收廢物利用室中大致上用過之 啤酒並返回供應導管而再循環。 美國專利號碼第5，8 8 2，4 1 6號揭示以汽化型 式傳送液體試劑至化學蒸汽沈澱反應器之液體傳輸系統。 * 該反應器對該液體傳輸系統呈蒸汽收集模式。該液體傳輸 系統包括以縱軸決定及以密封牆界定之長型汽化流體流動 通道。流體流動通道中包括汽化加熱元件，其與縱軸形成 橫向而加熱液體至汽化。然後該汽化液傳輸至化學蒸汽沈 澱反應器。 經濟部智慈財產局員工消費合作社印紫 美國專利號碼第5，8 4 6，3 8 6號揭示自液體氨 貯存槽抽取氨蒸汽之在地汽化器。該氨汽化器通過微波過 濾之過濾器，並隨後用高P Η純水洗淨。商業級氨轉變成 完全高純度之氨而不需傳統之管柱蒸餾。存放氨於液態貯 存槽。外部沈浸加熱來源在做爲單一階段蒸餾之液態氨供 給貯存槽中自蒸汽中抽取蒸汽，在液相之後留下一些固體 雜質和高沸騰雜質。透過微濾器抽取貯存槽通道蒸汽空間 之氨蒸汽。壓力調節器控制已過濾蒸汽之流動並引導至滌 -6 - 本纸張尺度適用中國國家標準（CNS ) Α4規格（2ΙΟΧ297公釐） 559566 A7 B7 五、發明説明（4) (請先閱讀背面之注意事項再填寫本頁) 氣管柱/循環幫浦組合體且隨後到任一個蒸餾管柱、淨化 使用液體產物點或使用氣體點線路轉換之去離子水溶解單 元。貯存槽之蒸汽頂部空間控制著流速。微波能量快速取 代能量損耗至所提之微波系統。在微波汽化器/蒸發器系 統中使用循環幫浦，其可能是金屬雜質的來源。 美國專利號碼第5，5 2 3，6 5 2號揭示在介電電 漿室、一對汽化器、一個微波調頻和傳輸配件及磁場產生 配件中使用微波能量。該室界定一內部範圍，其中按既定 線路發送源頭氣體並使之離子化形成電漿。微波調頻和傳 輸配件以T E Μ方式供給微波能量至該室。 無任何前述技藝被視爲教導或建議利用微波能量控制 在飽和液沸點以下的蒸發而產生超高純度氣體。 本發明簡述 經濟部智慈財產局員工消費合作社印製 本發明之觀點有關分離極性液之方法，包含（a )引 入有效之微波能量至比液體表面低至多約3 0 m m深度之 液體中；（b )控制引入液體中之微波能量以保持溫度低 於該液體之沸點；（c )在微波能量存在時蒸發該液體並 .維持溫度低於該液體之沸點以形成純化汽體及（d)獲得 蒸發之純化汽體。 本發明之另一觀點有關分離極性液之方法，包含引入 有效之微波能量至比液體表面低至多約3 0 m m深度液體 中以達到液體之沸點；控制微波能量接近該液體之沸點； 在微波能量存在時蒸發該液體並維持溫度低於該液體之沸 本紙張尺度適用中國國家標準（CMS ) A4規格U10X297公釐） 559566 A7 B7 五、發明説明（5 ) 點以形成純化汽體並獲得蒸發之純化汽體。 藉控制該液體之蒸氣壓，使引入之微波能量比該液體 .沸點溫度約高至多5 °C。 所得純化液體之純度爲低於1 P p m之雜質。 圖式簡單說明 由下列較佳具體例及附帶圖式之說明，熟知此技藝之 人士可想到其他目標、特性及優點。 圖1顯示蒸發器1中之不同溫度區域。 圖1 a描述波紋或擾動效應。 圖2例示極性液體穿透深度處溫度T p D與汽相流速之 ^關係，以及溫度與氣相雜質水準之關係。 圖3顯示依本發明預定條件，氨之液-汽平衡。 圖4提出本發明貯存、汽化、控制與輸送方法之槪要 圖。 圖5爲氨之汽-液平衡曲線。 圖6爲通量對流速之函數曲線圖。通量爲單位受熱面 積之輸入瓦特數。 圖7顯示雜質隨時間減少之函數。此圖建議了在約1 小時後，雜質量穩定而達一底部平坦値。 符號說明 圖1至3中： 本紙張尺度適用中國國家標準（CNS ) A4規格（210X29?公釐） (請先閲讀背面之注意事項再填寫本頁) 訂 經濟部智慈財產局員工消費合作社印製 -8- 559566 A7 B7 五、發明説明（6) 經濟部智慧財產局員工消費合作社印製 1 蒸 發 器 2 整 體 液體 3 穿 透 深度 4 穿 透 深度 頂 度 5 穿 透 深度 底 部 6 頂 部 控制 區 域 7 波 導 9 白 由 面表 面 1 0 純 化 氨氣 1 2 石 英 窗 P D 預 定 壓力 R D 波 紋 /擾 動 高度 T 3 室 溫 丁 Μ 1 N 最低 溫 度 丁 A 攪 動 點 T B 沸 點 T C 可 接 受過 熱 T D 預 定 溫度 F D 預 定 流動 圖4中 ·· 1 圓 桶 2 進 料 流 3 E S 〇板 4 液 流 (請先閱讀背面之注意事項再填寫本頁) 本紙張尺度適用中國國家標準（CNS ) A4規格（210X 297公釐） -9- 559566 經濟部智1財產局員工消費合作社印繁 kl B7五、發明説明（7) 5 液流 6 閥 7 線路 1 0蒸發器 1 1線路 1 2水準或重力傳輸器 1 3水準控制器 1 4線路 15閥 2 0氮氣槽 2 1線路 2 2淸潔氣體控制板 2 3淸潔線路 3 0磁電管 3 1波導 3 2安全對接環 4 0線路 4 2流出孔 . 4 3流動傳輸器 4 5流動控制器 4 7流動限制控制閥 4 8產物流 5 1線路 5 2溫度傳輸器 (請先閲讀背面之注意事項再填寫本頁) 本紙張尺度適用中國國家標準（CNS ) A4規格（2I0X297公釐） -10- 559566 A7 B7 五、發明説明（8) 5 3溫度控制器 5 6線路 (請先閲讀背面之注意事項再填寫本頁) * 5 7壓力傳輸 5 8壓力控制器 6 0低位準選取 6 1線路 7 0線路 7 1閥 7 2液流 7 3廢液筒 8 1 ^ 8 2 ' 8 3 ' 8 4 壓力與溫度控制器 本發明詳細說明 經濟部智慧財產局員工消費合作社印製 本發明使用不純極性液（即：氨）並添加熱氣於其中 以蒸發該極性液而在汽相中獲得更高純度。如此確保熱氣 之添加緩慢完成。利用微波輻射能維持該極性液灘之溫度 在該壓力之該極性液之沸點以下。極性液之沸騰或攪動不 常發生。然而，較佳施加充足之微波能量以達到該極性液 之沸點溫度，並隨後調整該微波能量低於該極性液之沸點 溫度’但仍足以使微波能量蒸發該極性液。據稱此種純化 極性液而保持其純度之微波能量使用有二項原因。第一、 •使攪動（若沸騰保持在最低限度將於系統中發生）減到最 低令雜質保留在不發生蒸發之液灘底部。第二、水汽、有 機油，及非揮發性殘留物較佳保留在該極性液之液相中。 本紙張尺度適用中國國家標準（CNS ) A4規格（210乂297公釐） -11 - 559566 A7 B7 五、發明説明（9) (請先閱讀背面之注意事項再填寫本頁) 本發明藉保持溫度低於該極性液之沸點而防止該系統之蒸 發。如此確保蒸汽中徹底的汽相變換（U.ansfil )，其中水 氣、有機油及非揮發性殘留物保留在液相中而未轉變成汽 相。若容許極性液以較長的時間沸騰，某些蒸汽、有機油 及非揮發性殘留物藉攪動可轉變成（在廣泛的濃度中）汽 相。最後，本發明可產生P P m不純水準之氨蒸汽。 微波能量取代蒸發中消耗的能量，同時在容器中維持 汽液平衡。當容器中之液體蒸發且汽體流動增加，該蒸氣 壓下降。同時，因爲該液體蒸發與容器中之液體蒸發，溫 度下降且液體變涼。壓力下降亦防止點沸騰。該微波能量 維持適當的壓力及溫度平衡，因而保持該系統之蒸發率及 會b量。 其一操作方法是以批次模式進行此法。該極性液容許 減少至某種水準，且隨後關閉微波，並接著再裝滿容器中 .之極性液。另一操作方法是在施加微波能量時連續添加極 性液。 經濟部智慈財產局S工消費合作社印製 當於蒸汽塡充之頂部抽去蒸發之極性液時，可能發生 點沸騰。如此壓力降低。同時，當於蒸汽塡充之頂部抽去 極性液時，該液滴溫度導致液體變涼。該變涼液體會在減 低之壓力下點沸騰。該微波能量取代該系統之熱氣及壓力 損耗而重建汽-液/壓力溫度平衡。容器之平衡係在低於 (但非常接近）該壓力下之沸點。藉重建此平衡，本發明 以防止極性液之點沸騰而作用。 利用微波能量做爲熱氣來源之優點包括：（1 )避免 -12- 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） 559566 A7 B7 五、發明説明（id (請先閱讀背面之注意事項再填寫本頁) 液灘中氨蒸發對蒸發能量更替中快速熱氣之迅速響應；（ 2 )無微粒污物；（3 )有效的能源利用。微波能量來源 對加熱極性物質是非常有效的，該極性物質中正負電荷中 心等距分離，雖然分子上之淨電荷爲零。因此，在極性物 質中如水或氨中，此電荷分離使分子與能量結合，而導致 加熱。 當傳送微波能量至液體保存槽中，依電容率、滲透性 及操作之微波方式，擴散該液體至某種深度以加熱體積層 。當表面隨蒸發而縮減，更深層被加熱。由於加熱元素爲 該液體本身，當電源關閉，加熱立即停止，導致“迅速響 應”。 透過波導及石英窗傳送微波能量。其中有少量或沒有 污物，因爲不以接觸任何核晶過程而沸騰其他雜質來源傳 3會巨〇 經濟部智態財產局員工消費合作社印製 體積加熱產生高效能，因爲它不依賴傳導與對流變成 大範圍。進一步，因爲滲透深度預計約接近3 0 m m，更 佳約爲1 6 m m至2 0 m m，加熱氣體積隨蒸發到達貯存 . 槽上段。 爲了滿足安全成本有效大量來源及傳送系統之需要， 本發明提供傳送極高純度極性或非極性加工氣之方法和裝 置。該傳送系統係能夠維持高流速之蒸發系統。該蒸發系 統包括大量的極性或非極性飽和液化學產物，其中該化學 製品至少具有一汽相及一液柑。 痕量水氣一氨系統之汽-液平衡資料將產生。大部份 本紙張尺度適用中國國家標準（CNS) A4規格（2】OX 297公釐） 559566 A7 B7 五、發明説明（11) (請先閱讀背面之注意事項再填寫本頁) 水氣保留在液相中。該水氣在液相之濃度約爲在汽相之濃 ’度的2 - 3等級。觀察到痕量油及其他非揮發性殘留物（ N V R )介於二相之間的類似分佈。依據所用Smolen刊物 之汽-液平衡資料，藉把氨自液相蒸發或蒸餾成汽相使該 汽相水氣減少，有時稱爲“汽相轉變（transfill) ” 。 完全的汽相轉變可減少水氣含量二級，即：自1 〇 〇 p p m減低至小於1 p p m。此純化僅在以慢到足以防止 液態氨快速沸騰的轉變流速進行而達成。若發生沸騰，則 無法純化’因爲液相中全部的水氣將輕易蒸發成汽相。然 而，低流動氣相轉變容許系統維持合適的汽-液平衡水氣 分配並產生二級的水氣濃度降低。同時在汽相中油及 N V R濃度中發生類似之降低。 經濟部智慈財產局員工消費合作社印製 爲維持低蒸發率，必須於此系統中添加能量而取代蒸 發所需之熱氣。若不如此，該系統溫度降低，蒸發率降低 ，且氨開始沸騰。結果，將喪失水氣、油及非揮發性殘留 物（N V R )所有的純化優點。利用具有攪動內部或外部 加熱器之標準汽化器法傾向藉產生梯度和核晶過程點促進 沸騰。攪動亦增加非揮發性殘留物（N V R )的移動性， 因而增加成爲汽相的通路機會。 本發明利用微波加熱來修正維持蒸發法所需之可控制 . 能量的數量。 本發明實例中，自蒸發器頂部抽取蒸發產物，該蒸汽 具有比壓縮液相更低之雜質濃度。該微波能量導致液體蒸 發。極性液之微波加熱係基於正負電荷在空間中不會結合 本紙張尺度適用中國國家標準（CNS )八4規格（210X297公釐） ~ -- 559566 A7 _B7 五、發明説明（d (請先閱讀背面之注意事項再填寫本頁) 的前提。因此，分子具有使自身朝向對應電場的傾向。然 而，電磁波譜微波範圍中之電場以遠超過分子移動之速率 振盪。如此造成內部阻抗力，其與電場交互作用並產生熱 氣。有關此黏加熱類型之精準微波頻率不重要。然而，重 要的是藉電磁波之電場產生正好足夠之內部磨擦力以增加 飽和液蒸氣壓而至維持客戶所需的流速。 現在轉至圖1，其顯示本發明之一般操作。不純之氨 液進料被餵入蒸發器（未顯示）。微波能量源經由波導7 供應動力至蒸發器系統。此微動力加熱之穿透深度3 (自 氨液頂部算起）可達3 Omm。在此穿透深度之下爲整體 液體2，爲較未受熱。較未受熱指該整體液體爲室溫或高 於室溫，且顯著低於液體沸點T B。在穿透深度中有一溫度 梯度，上部流體之溫度較底部5爲高。所用加熱流體之微 波能量由蒸發器容器之頂部控制區域6引入。 經濟部智慈財產局員工消費合作社印製 當微波加熱穿透深度3之氨液，該氨開始蒸發。純化 氨氣1 0則自蒸發器系統排出。因爲汽相排出則氨液的蒸 汽壓開始降低，同樣地穿透深度3之液溫亦降低。爲了避 免點沸騰，加入微波動力以確保穿透深度之液溫不會降至 液體可於減壓沸騰之溫度。圖3上之3 /點顯示當壓力降 太快時，氨可能的狀態。此時，氨在攪動區線的太下方， 所以雜質將可進入氣體產物中。 蒸汽之壓力溫度平衡應維持使系統於沸點附近之溫度 操作。易言之，動力應維持使系統在汽-液平衡線附近操 作。見圖3。此操作型態確保夠高之流速，且不損及純度 -15- 本紙張尺度適用中國國家標準（CNS ) A4規格（210X 297公釐） 559566 A7 _____B7 _ 五、發明説明（θ 〇 (請先閱讀背面之注意事項再填寫本頁) 本發明首要目標爲高產物流速與高純度。已知若過熱 (高於T B )操作蒸發器系統將給出大的流量生產率，但雜 質水準亦提高。若可接受此雜質增加，則可嘗試於T B以上 溫度操作來達到高流量生產率。本案非顯而易知之處在於 在接近T B時操作。本發明中，穿透深度之氨液的過熱維持 於低於約3 0 °F的溫度，較好低於約2 0 °F，最好低於約 1 0 °F。 • 圖2例示流速與雜質隨操作溫度變化之函數，當溫度 升高時，流速與雜質水準均提高。於丁 π i η處，汽相系統 之雜質很低，但相對的流速太低而無法達到本發明目標， 即，汽相產物之高流速。 經濟部智慧財產局員工消費合作社印製 當操作溫度升高時，流速開始接近可接受之預定範圍 。高於Td (穿透深度處流體之預定溫度）時，雜質水準可 能升高。如圖2所建議’ T D爲較佳操作溫度。於T A處’ 流速便夠高。雖然此溫度時之雜質較低溫時爲高’仍可符 合本案目標。高於T c時’雜質水準變差，且無法被半導體 產業所接受。 * 總而言之，圖2例示流速與雜質水準間之適切交換。 於T D處，系統提供半導體產業可接受之流速與雜質水準。 爲了維持所求蒸發流速’須將動力加至系統中以補充 蒸發所需之熱。若非如此’系統溫度將降低、蒸發速度將 降低，使得所求蒸發流速無法達到。若仍以高的速率排出 蒸汽，壓力將降低而液體將開始沸騰。結果’水氣、油與 本紙張尺度顧中酬家M規格（210X 297公釐）口6- 一 559566 經濟部智毡財產局員工消費合作社印製 A7 B7 五、發明説明（ N V R等所有純化優點都將失去。 • 使用內部或外部加熱器及攪動之標準蒸發器傾向於產 生梯度與成核位置而促進沸騰。攪動亦會提高N V R之移 動，所以使其進入蒸汽相之機率提高了。 本發明以控制動力用微波加熱來維持蒸發過程。有效 量之微波動力被加入液體中，使穿透深度處之液體溫度基 本上維持在所預定壓力之氨的沸騰溫度。 圖3例示蒸發器系統之操作條件。該系統被預定成在 預定壓力與溫度參數（各爲Pd與Td)內操作。應注意到 T D接近沸騰溫度T B，T B係對應於飽和壓力P D。現在討 論操作條件的一個循環。在循環開始時，系統約在室溫（ * τ 3 )及常壓（Patm )，即如圖3之點1。當加入微波動力 時，穿透深度被加熱了。穿透深度係真正被微波能量加熱 之液體頂層（可深達3 0 m m )。另外，當加入微波動力 時，穿透深度之溫度與壓力升高。如此便可達到預定溫度 Td與壓力PD，即如圖3之點3。當達到預定之壓力與溫 度時，液體蒸發速率開始提高。在穿透深度之底部，溫度 略低於T D。此處的溫度對應於圖1之T 2。蒸汽於自由面 (freeboard)處離開液體，所謂的自由面指蒸汽與液體間之界 面。在較高之蒸汽需求率下，蒸汽以較快速率流出系統， 導致系統之蒸汽壓力降低。大量的蒸汽壓力降低導致液體 於預定溫度T D之過度擾動。爲了避免此一結果’提商微波 動力，使液溫高於T D，導致流體如預期地增加蒸發。 提高蒸汽流速且不提高微波動力的另一結果爲穿透深 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -17- ^^裝 訂 AW (請先閱讀背面之注意事項再填寫本頁) 559566 A7 B7 五、發明説明（id (請先閲讀背面之注意事項再填寫本頁) 度之同步溫度降低。當液體變成蒸汽，留下的液體爲低於 丁。之過冷，造成流速之降低，即圖3之點4。爲了避免溫 度與壓力低於最低之P l與T l，就增加微波動力，使液體 溫度與蒸汽壓力升至T D與P D，如圖3之點3。微波動力 •能夠回復穿透深度之溫度。結果蒸汽壓-溫度平衡得以回 復而循環重新開始。總之，本發明將壓力與溫度維持在汽 -液平衡曲線之下，並嘗試維持壓力與溫度低於R D約 1 · 0 〃之攪動曲線。 圖4例示本發明整個微波蒸發器流程圖。圓桶1經由 線路7將不純氨進料供應至蒸發器1 〇。首先，進料流2 經過E S〇板（緊急關掉板）3，得出液流4，若閥1 5 打開，其繼續成爲液流5而經過閥6，然後以液流7進入 蒸發器1 0。圓桶進料至蒸發器1 〇達一設定水準。 線路1 1傳輸氨特定水準之水準或重力傳輸器1 2。 '此資料被送至水準控制器1 3，其經由線路1 4控制閥 1 5而調節氨進料流。若槽中氨水準太低，閥會打開而令 氨液進料塡滿槽。若有足夠氨，則閥會關閉。 經濟部智慈財產咼S工消費合作社印繁 若系統須要淸洗，氮氣槽2 0經由線路2 1饋料至淸 潔氣體控制板2 2，然後氮氣就經由淸潔線路2 3被饋至 E S 0板3。以氮氣與惰性物淸洗可以確保蒸發器系統乾 燥。 一旦蒸發器已適宜地塡滿，打開磁電管3 〇而供給微 波動力。當需要氨產物流時，則打開微波動力之供應與磁 電管3 0。該微波單元能夠供應高瓦特數，且由反動壓力 i紙張尺度適用中國國家標準（CNS ) A4規格( 210X 297公釐） ~ 559566 A7 B7 五、發明説明（1硿 (請先閱讀背面之注意事項再填寫本頁) 控制器5 8與反動溫度控制器5 3之綜合經由線路6 1控 制其循環。該壓力與溫度控制器位於氨槽內部，即8 1、 8 2、8 3與8 4所示。微波動力供應與磁電管係於 2·45GHz或任何微波範圍內適宜區域下操作。 由磁電管3 0產生之單模態微波，由波導3 1下傳， 經由特殊預定之安全對接環3 2引入蒸發器中。 經濟部智慧財產局員工消費合作社印紫 來自微波之入射波接近汽-液界面平面，導致液體介 質中之傳送波與汽相介質之反射波。氨爲介電質，所以穿 透之電場與磁場深度將受限。在上述操作下，穿透深度爲 自由面下約1 6 m m至約2 0 m m (自由面溫度爲約 2 0 t )。在加熱時，自由面下氨之約1 6 m m至約2 0 m m層將蒸發。產物蒸氣由流出孔4 2與流動限制控制閥 4 7 (由反動流動控制器4 5控制）排出。本發明以最高 2 5 0 0氣體c c/m i η的速率提供產物流至客戶電池 端。平均動力輸入爲2 0 0至4 5 0 0瓦特/平方英呎。 在氨的例子中，所用微波能量通量爲約0 · 3至約1 0瓦 特/平方英吋，較好爲約0 . 3至約2 0瓦特/平方英吋 ，更好爲約0 · 3至約3 0瓦特/平方英吋。此可藉由維 •持液汽相間之熱平衡而達成。ρ I D (常比積體衍生）控 制環路控制微波動力，可以迅速回應需求而維持穩定蒸汽 壓力（因產物高流速而損失），即，藉由補充熱給系統。 氣態氨由氨槽流出。線路4 0流經流出孔4 2，其流 經流動限制控制閥而生產超高純度氣態氨產物流4 8。於 此同時，流動傳輸器4 3測量流過流出孔之液流。傳輸器 -19- 本紙張尺度適用中國國家標準（CNS ) Α4規格（210X 297公釐） 559566 A7 經濟部智慈財產局員工消費合作社印製 五、發明説明（θ 會通知液流水準給流動控制器。流動傳輸器之資料傳至流 動控制器4 5，其指示流動限制控制閥之開閉。 有關溫度與壓力之資料係於氨槽之頂部讀取。溫度資 料經由線路5 1傳輸至溫度傳輸器。同時，壓力資料經由 線路5 6傳輸至壓力傳輸器。雖然圖示爲外部，該溫度與 壓力傳輸器實際上係位於系統內部，在自由面之上。溫度 與壓力傳輸器將資料轉換成可被溫度控制器5 3與壓力控 制器5 8判讀之訊號。溫度與壓力控制器5 3與5 8將其 資料送至低位準選取6 0，其經由線路6 1指示磁電管需 要多少微波動力以回復平衡。隨著提高之產物流，蒸汽壓 Ρν降低，引起微波動力提高。故當穿透深度溫度tpd增 加’微波動力將降低，進而降低蒸汽壓力，而動力之控制 循環則繼續。 壓力控制器，溫度控制器與低位準選取包括一通用控 制器。低位準選取6 0決定磁電管3 0應爲開或關。低位 準選取6 0藉由選取溫度與壓力間之最低相對値而運作。 舉例而言，若壓力水準較溫度水準低，則低位準選取6 0 將「低選」壓力水準而丟棄溫度輸入（只要溫度不是太高 )。低位準選取6 0將認爲壓力正降低，故經由線路6 1 ，磁電管會被告知要打開。當壓力爲低選的訊號，但尙未 低於預定之參數，線路6 1會指示磁電管仍爲關閉。上段 說明亦適用於當溫度爲低選之訊號。 當因爲蒸發而使槽中液體量降低，整體液體中的雜質 會增加。當雜質水準太高時，將廢液移出槽中。經由線路 (請先閲讀背面之注意事項再填寫本頁) --φ 裝· .項再填寫木 •1Τ Φ 本紙張尺度適用中國國家標準（CNS ) Α4規格（210X297公釐） -20- 559566 A7 • _B7____ 五、發明説明（id 7 0與閥7 1排出氨，形成液流7 2，貯存於廢液桶7 3 〇 (請先閱讀背面之注意事項再填寫本頁) 本發明可利用任何極性飽和液而操作，然而，有關本 發明之目的，特別是相關飽和液可包括，但不受限於N Η 3 、HF、SiHCl3、SiH2Cl2、C4H8、C3F8 、Η B r 、C 5 F 8、C 1 F 3、T E〇S和類似物。該裝 置選用之頻率爲915、2450、5850及 1 8000MHz。藉此方法達成1至2500升/分鐘 或更高之高流速，且水氣和N V R水準小於約1 p p m。 保留在液灘中之污物可藉連續塡充而持續丟棄或定期丟棄 。該系統性能藉整合幾何形和以特別預定形狀置於液體體 積周圍之多個磁電管而最佳化。如此可減少微波干擾型態 數，其造成聚焦點和加熱不均。 顯示於一個或更多之圖式的本發明特性僅供參考，因 爲各項特性可依本發明與其他特性結合。其他具體例爲熟 知此技藝之人士認可且意欲爲申請專利範圍所包括。 經濟部智慈財產局員工消費合作社印製 -21 - 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐）559566 A7 B7 V. Description of the invention (1) Field of invention (Please read the precautions on the back before filling out this page) The present invention relates generally to a saturated liquid purification method. More specifically, the present invention relates to a method for purifying a saturated liquid using microwave energy in a vaporization process to produce an ultra-high purity gas. BACKGROUND OF THE INVENTION Process gases used in semiconductor manufacturing equipment are usually supplied through cylinders. To meet the increasing demand for high-flow products and ultra-high purity requirements for these gases, gas manufacturers often use ultra-high-purity large-scale vaporization transfer systems to process polar liquefied compressed gas. Generally speaking, the on-site system uses a microwave energy source to increase and control the evaporation rate of an aqueous polar liquid (such as ammonia). This local system can provide purification, shorter response time, and accurate controllable evaporation at very high flow rates (larger than 1000 l / min for the semiconductor industry). In order to maintain the evaporation of the polar liquefied mixture, energy must be added to this system to replace the hot air flow from the customer's end of use. If this is not done, the temperature in the gas will decrease and the evaporation rate of the polar liquid will decrease to the point at which the vapor-liquid beach finally approaches cooling, stopping all vapor flow. Printed by the Industrial and Commercial Property Cooperative of the Ministry of Economic Affairs and Consumer Cooperative. If the liquefied gas needs additional purification, the vaporizer system can reduce the amount of impurities transferred to the vapor phase, so a purification step is added. This impurity is removed from the vapor phase by liquid evaporation and remains in the liquid beach. It includes Group I, Group I I, and Group I I I metals, and oxides, carbonates, hydrides, and halides of these elements. These impurities originate from a number of factors including valve-driven friction, thermal expansion and contraction of liquid containers, expansion or expansion pressure of container openings during installation, and so on. Water vapor is another source of #quality. According to the vapor-liquid equilibrium balance, this paper applies China's standard (CNS) A4 (210X 297 mm) T '~ " 559566 A7 B7 V. Description of the invention (2) (Please read the notes on the back first Fill out the information on this page}, the liquid phase water vapor concentration is about 2-3 times the vapor phase concentration. Careful treatment of the liquid phase to vapor phase evaporation can reduce the amount of water vapor and other non-volatile residues (non-volatile residues, NVR). A general example of the transfer of purified gas is through a vaporizer method, which uses resistance heating. Steam is extracted from a storage tank and heated by a heat source such as an internal heater or external band heater to provide more than the surrounding available The thermal energy of heat. The steam and the non-low temperature liquefied compressed gas then pass through a heat exchanger to further evaporate the storage tank. Conduction and convection transfer heat from the line source (which increases the response time of the system) to the overall liquid. Use immersion Heater or shell and tube heat exchanger can release particles and serve as the source of nuclear boiling process of impurities boiling (such as water and gas), because the source of nuclear process is large It is hotter than the whole liquid. Stirring promotes boiling to a gradient and the core crystal process is located. Stirring also promotes the movement of non-volatile residues, increasing the possibility of transition to the vapor phase. US Patent Nos. 4, 6 7 1, 9 5 No. 2 discloses a processing method and a device for generating sulfur dioxide gas from impure liquid sulfur dioxide. The processing method uses impure liquid sulfur dioxide and is printed with 9 1 5, 2, 4 50, 8 Chihsin Property Bureau, Ministry of Economic Affairs, 8 Industrial Cooperatives, and 5 The frequency of 8 5 0, or 1 8 0 0 Μ Η z receives microwave energy for a time sufficient to generate sulfur dioxide gas, if any, collect the gas and remove the impure liquid sulfur dioxide obtained. The evaporation pressure of the sulfur dioxide is 70 ° F is 34 · 4p sig and the purity of sulfur dioxide reaches 9 8.9 9%. US Patent No. 4, 2 8 5, 7 7 4 discloses a device for continuously producing concentrated alcohol from beer. Several concentration chambers and several wastes Utilization room-5-This paper size applies the Chinese National Standard (CNS) A4 specification (210X 297 mm) 559566 A7 __B7__ 5. Description of the invention (3) (salvage cells) are connected and arranged in a row. Through The supply duct supplies beer (please read the notes on the back before filling this page). Go to the first upstream concentrator room. Then the beer flows through the passage in the adjacent room corresponding to the beer volume to the predetermined level of the adjacent upstream room. A microwave ignition bulb (ignition bulb) in each chamber heats the beer and boils or evaporates the alcohol content. The gaseous alcohol continuously foams through the liquid passage from each concentrator chamber to the next adjacent upstream chamber until the gaseous alcohol reaches the first concentrator. Chamber (where the gaseous alcohol is concentrated and condensed in the column to a liquid solution containing approximately 95% alcohol and approximately 5% water). Alcohol is obtained from the diluent, and the roughly used beer in the waste utilization room is recovered and returned to the supply duct for recycling. U.S. Patent No. 5,8 8 2, 4 1 6 discloses a liquid transfer system for transferring liquid reagents to a chemical vapor deposition reactor in a vaporized manner. * The reactor is in a vapor collection mode for this liquid transfer system. The liquid transfer system includes a long vaporized fluid flow path defined by a longitudinal axis and defined by a sealing wall. The fluid flow path includes a vaporization heating element that forms a lateral direction with the longitudinal axis to heat the liquid to vaporize. The vaporized liquid is then transferred to a chemical vapor deposition reactor. Employees' Cooperatives of the Intellectual Property Office of the Ministry of Economic Affairs of the United States of America, US Patent No. 5, 8 4 6, 3 8 6 discloses a local vaporizer that extracts ammonia vapor from a liquid ammonia storage tank. The ammonia vaporizer was passed through a microwave-filtered filter and then washed with high-P Η pure water. Commercial grade ammonia is converted to completely high purity ammonia without the need for traditional column distillation. Store ammonia in a liquid storage tank. The external immersion heating source supplies liquid ammonia as a single-stage distillation to the storage tank to extract steam from the steam, leaving some solid impurities and high boiling impurities behind the liquid phase. The ammonia vapor in the steam space of the storage tank passage was extracted through the microfilter. The pressure regulator controls the flow of filtered steam and guides it to polyester-6-This paper size applies to China National Standard (CNS) A4 (2ΙΟ × 297 mm) 559566 A7 B7 V. Description of the invention (4) (Please read the back Please fill in this page again for the matters needing attention) Air column / circulation pump combination and then to any distillation column, purify the deionized water dissolving unit using liquid product point or gas point line conversion. The head space of the steam in the storage tank controls the flow rate. The microwave energy quickly replaces the energy loss to the mentioned microwave system. A circulating pump is used in a microwave vaporizer / evaporator system, which may be a source of metal impurities. U.S. Patent No. 5,5 2 3,6 5 2 discloses the use of microwave energy in a dielectric plasma chamber, a pair of vaporizers, a microwave frequency modulation and transmission accessory, and a magnetic field generation accessory. The chamber defines an internal area in which the source gas is sent and ionized to form a plasma in accordance with a predetermined circuit. The microwave frequency modulation and transmission accessory supplies microwave energy to the chamber in a TEM manner. None of the aforementioned techniques are considered to teach or suggest the use of microwave energy to control evaporation below the boiling point of a saturated liquid to produce ultra-high purity gases. The present invention briefly describes the method of separating the polar liquid by the consumer cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs, which includes (a) introducing effective microwave energy into the liquid at a depth of up to about 30 mm lower than the liquid surface; (B) controlling the microwave energy introduced into the liquid to keep the temperature below the boiling point of the liquid; (c) evaporating the liquid in the presence of microwave energy and maintaining the temperature below the boiling point of the liquid to form purified vapors and (d) Evaporated purified vapor was obtained. Another aspect of the present invention relates to a method for separating a polar liquid, including introducing effective microwave energy into a liquid at a depth of up to about 30 mm lower than the liquid surface to reach the boiling point of the liquid; controlling the microwave energy to approach the boiling point of the liquid; Evaporate the liquid when it exists and keep the temperature lower than the boiling point of the liquid. The paper size applies the Chinese National Standard (CMS) A4 specification U10X297 mm. 559566 A7 B7 V. Description of the invention (5) point to form purified vapor and get evaporated. Purified gas. By controlling the vapor pressure of the liquid, the introduced microwave energy is about 5 ° C higher than the boiling temperature of the liquid. The purity of the obtained purified liquid was less than 1 P p m of impurities. Brief description of the drawings From the following preferred specific examples and accompanying drawings, those skilled in the art can think of other goals, characteristics and advantages. FIG. 1 shows different temperature regions in the evaporator 1. Figure 1a describes the ripple or disturbance effect. Figure 2 illustrates the relationship between the temperature T p D and the vapor phase flow velocity at the depth of penetration of a polar liquid, and the relationship between temperature and the impurity level of the gas phase. Figure 3 shows the liquid-vapor equilibrium of ammonia in accordance with the predetermined conditions of the present invention. Figure 4 presents a summary of the method of storage, vaporization, control and transportation of the present invention. Figure 5 is the vapor-liquid equilibrium curve of ammonia. Figure 6 is a graph of flux versus flow rate. The flux is the input watts per unit heating area. Figure 7 shows the decrease in impurities as a function of time. This figure suggests that after about 1 hour, the impurity is stable and reaches a flat bottom. Explanation of symbols in Figures 1 to 3: This paper size applies to the Chinese National Standard (CNS) A4 specification (210X29? Mm) (Please read the precautions on the back before filling out this page) Ordered by the Intellectual Property Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs -8- 559566 A7 B7 V. Description of the invention (6) Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economy 1 Evaporator 2 Whole liquid 3 Penetration depth 4 Penetration depth top 5 Penetration depth bottom 6 Top control area 7 Waveguide 9 White surface 1 1 Purified ammonia gas 1 2 Quartz window PD Predetermined pressure RD Ripple / disturbance height T 3 Room temperature D M 1 N Minimum temperature D A Stir point TB Boiling point TC Acceptable overheating TD Predetermined temperature FD Predetermined flow diagram 4 medium ... 1 drum 2 feed flow 3 ES 〇 plate 4 liquid flow (please read the precautions on the back before filling this page) This paper size applies the Chinese National Standard (CNS) A4 size (210X 297 mm)- 9- 559566 Employees' Cooperatives, Intellectual Property Cooperatives, Intellectual Property Office, Intellectual Property Department, Intellectual Property, Kl B7 V. Description of the invention (7) 5 Liquid flow 6 Valve 7 Line 1 0 Evaporator 1 1 Line 1 2 Level or gravity transmitter 1 3 Level controller 1 4 Line 15 valve 2 0 Nitrogen tank 2 1 Line 2 2 Clean gas Control board 2 3 clean line 3 0 magnetron 3 1 waveguide 3 2 safety docking ring 4 0 line 4 2 outflow hole. 4 3 flow transmitter 4 5 flow controller 4 7 flow restriction control valve 4 8 product flow 5 1 line 5 2 Temperature transmitter (please read the precautions on the back before filling this page) This paper size applies to Chinese National Standard (CNS) A4 specification (2I0X297 mm) -10- 559566 A7 B7 V. Description of invention (8) 5 3 Temperature controller 5 6 lines (please read the precautions on the back before filling this page) * 5 7 pressure transmission 5 8 pressure controller 6 0 low level selection 6 1 line 7 0 line 7 1 valve 7 2 liquid flow 7 3 waste Liquid cylinder 8 1 ^ 8 2 '8 3' 8 4 Pressure and temperature controller Detailed description of the present invention Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs The present invention uses an impure polar liquid (ie, ammonia) and adds hot gas to it to evaporate This polar liquid gives higher purity in the vapor phase. This ensures that the hot gas addition is completed slowly. Using microwave radiation can maintain the temperature of the polar liquid beach below the boiling point of the polar liquid at the pressure. Boiling or agitation of polar liquids is rare. However, it is preferable to apply sufficient microwave energy to reach the boiling point temperature of the polar liquid, and then adjust the microwave energy to be lower than the boiling point temperature of the polar liquid 'but still be sufficient to allow the microwave energy to evaporate the polar liquid. The use of microwave energy for purifying polar liquids while maintaining their purity is said to be for two reasons. First, • Minimize agitation (which will occur in the system if boiling is kept to a minimum) so that impurities remain at the bottom of the liquid beach where evaporation does not occur. Second, water vapor, organic oil, and non-volatile residues are preferably retained in the liquid phase of the polar liquid. This paper size is applicable to Chinese National Standard (CNS) A4 specification (210 乂 297 mm) -11-559566 A7 B7 V. Description of the invention (9) (Please read the precautions on the back before filling this page) The invention keeps the temperature by Below the boiling point of the polar liquid prevents evaporation of the system. This ensures a complete vapor phase transformation (U.ansfil) in the steam, in which water, organic oil and non-volatile residues remain in the liquid phase without being transformed into a vapor phase. If polar liquids are allowed to boil for a longer period of time, certain vapors, organic oils, and non-volatile residues can be transformed (in a wide range of concentrations) into the vapor phase by agitation. Finally, the invention can produce ammonia vapor at impure levels of P P m. Microwave energy replaces the energy consumed in evaporation while maintaining vapor-liquid equilibrium in the container. As the liquid in the container evaporates and the vapor flow increases, the vapor pressure decreases. At the same time, as the liquid evaporates and the liquid in the container evaporates, the temperature drops and the liquid becomes cold. The pressure drop also prevents point boiling. The microwave energy maintains a proper pressure and temperature balance, thus maintaining the evaporation rate and the amount of the system. One method of operation is to perform this method in batch mode. The polar liquid is allowed to decrease to a certain level, and the microwave is then turned off, and then the polar liquid in the container is refilled. Another method of operation is to continuously add polar fluid while applying microwave energy. Printed by the Industrial and Commercial Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs When the evaporated polar liquid is drawn on the top of the steam charge, a point boiling may occur. This reduces the pressure. At the same time, when the polar liquid is removed from the top of the steam charge, the liquid droplet temperature causes the liquid to cool. The cooling liquid will boil at a reduced pressure. The microwave energy replaces the system's hot gas and pressure losses and rebuilds the vapor-liquid / pressure temperature equilibrium. The equilibrium of the vessel is the boiling point below (but very close to) this pressure. By rebuilding this equilibrium, the present invention works by preventing the boiling of the polar liquid. The advantages of using microwave energy as a source of hot gas include: (1) Avoid -12- This paper size applies Chinese National Standard (CNS) A4 specifications (210X297 mm) 559566 A7 B7 V. Description of the invention (id (please read the first Please fill in this page again.) Ammonia evaporation in the liquid beach responds quickly to rapid hot gas in evaporation energy replacement; (2) no particulate pollution; (3) efficient energy use. Microwave energy source is very effective for heating polar substances The positive and negative charge centers in the polar substance are separated at equal distances, although the net charge on the molecule is zero. Therefore, in a polar substance such as water or ammonia, this charge separation binds the molecule with energy and causes heating. When transmitting microwave energy to In the liquid storage tank, the liquid layer is diffused to a certain depth to heat the volume layer according to the permittivity, permeability and operating microwave method. When the surface shrinks with evaporation, the deeper layer is heated. Because the heating element is the liquid itself, when The power is turned off and the heating stops immediately, resulting in a "quick response." Microwave energy is transmitted through the waveguide and quartz window. There is little or no Because it does not boil any other source of impurities by contact with any nuclear crystal process, it is said that the volumetric heating produced by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs will produce high-efficiency because it does not rely on conduction and convection to become a large area. Further, Because the penetration depth is expected to be approximately 30 mm, more preferably approximately 16 mm to 20 mm, the volume of heated gas reaches the storage with evaporation. The upper part of the tank. In order to meet the needs of a large number of sources and delivery systems that are safe and cost effective, the present invention provides delivery Method and device for extremely high-purity polar or non-polar processing gas. The transfer system is an evaporation system capable of maintaining a high flow rate. The evaporation system includes a large number of polar or non-polar saturated liquid chemical products, wherein the chemical product has at least one vapor phase and One liquid tangerine. The vapor-liquid equilibrium data of the trace water vapor-ammonia system will be generated. Most of the paper sizes are in accordance with the Chinese National Standard (CNS) A4 specification (2) OX 297 mm. 559566 A7 B7 V. Description of the invention (11) (Please read the notes on the back before filling out this page) Water and gas remain in the liquid phase. The concentration of this water and gas in the liquid phase is about 2 to 3 levels of phase concentration. Similar distributions of trace oils and other non-volatile residues (NVR) between the two phases were observed. Based on the vapor-liquid equilibrium data of the Smolen publication used, ammonia Evaporation or distillation from the liquid phase to the vapor phase reduces the water vapor in the vapor phase, sometimes referred to as a "transfill." A complete vapor phase transition can reduce the water and gas content by two levels, from 100 ppm Reduced to less than 1 ppm. This purification is achieved only at a transition flow rate that is slow enough to prevent the rapid boiling of liquid ammonia. If boiling occurs, purification cannot be performed because all water vapor in the liquid phase will easily evaporate into the vapor phase. The low-flow gas phase transition allows the system to maintain a proper vapor-liquid equilibrium water-vapor distribution and produce a secondary water-vapor concentration reduction. At the same time, similar reductions in oil and NVR concentrations in the vapor phase occurred. Printed by the Consumer Cooperatives of the Intellectual Property Office of the Ministry of Economic Affairs To maintain a low evaporation rate, energy must be added to this system to replace the heat needed for evaporation. Otherwise, the temperature of the system decreases, the evaporation rate decreases, and ammonia begins to boil. As a result, all the purification advantages of water vapor, oil, and non-volatile residues (NVR) will be lost. The use of standard vaporizer methods with agitated internal or external heaters tends to promote boiling by generating gradients and nuclei process points. Agitation also increases the mobility of non-volatile residues (NVR), thus increasing the opportunity to become a vapor phase. The invention uses microwave heating to modify the amount of controllable energy required to maintain the evaporation method. In the example of the present invention, the vaporized product is extracted from the top of the evaporator, and the vapor has a lower impurity concentration than the compressed liquid phase. This microwave energy causes the liquid to evaporate. The microwave heating of polar liquid is based on the positive and negative charges in space. It will not be combined with the paper size. Applicable to the Chinese National Standard (CNS) 8-4 (210X297 mm) ~-559566 A7 _B7 V. Description of the invention (d (Please read the back first) Precautions before filling this page). Therefore, molecules have a tendency to orient themselves towards the corresponding electric field. However, the electric field in the microwave range of the electromagnetic spectrum oscillates at a rate far exceeding the molecular movement. This creates an internal impedance force that interacts with the electric field It acts and generates heat. The precise microwave frequency of this sticky heating type is not important. However, what is important is that the electric field of the electromagnetic wave generates just enough internal friction to increase the saturated liquid vapor pressure to maintain the flow rate required by the customer. Now turn Turning to Figure 1, it shows the general operation of the present invention. Impure ammonia liquid feed is fed into an evaporator (not shown). A microwave energy source is supplied to the evaporator system via a waveguide 7. The penetration depth of this micro-power heating is 3 (From the top of the ammonia solution) up to 3 Omm. Below this penetration depth is the whole liquid 2, which is less heated. Less heated The overall liquid is at or above room temperature, and is significantly lower than the liquid boiling point TB. There is a temperature gradient in the penetration depth, and the temperature of the upper fluid is higher than that of the bottom 5. The microwave energy of the heating fluid is used by the evaporator container. The top control area 6 is introduced. It is printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs when the microwave heat penetrates the ammonia liquid of depth 3, and the ammonia begins to evaporate. Purified ammonia gas 10 is discharged from the evaporator system. The vapor pressure of the ammonia liquid begins to decrease, and the temperature of the liquid at the penetration depth 3 also decreases. In order to avoid point boiling, microwave power is added to ensure that the temperature of the liquid at the penetration depth does not drop to the temperature at which the liquid can boil at reduced pressure. The 3 / point on 3 shows the possible state of ammonia when the pressure drop is too fast. At this time, ammonia is too below the line of the agitation zone, so impurities can enter the gas product. The pressure and temperature balance of the steam should be maintained so that the system Operate at a temperature near the boiling point. In other words, the power should be maintained so that the system operates near the vapor-liquid equilibrium line. See Figure 3. This type of operation ensures a sufficiently high flow rate without compromising purity -15- Paper size applies Chinese National Standard (CNS) A4 specification (210X 297 mm) 559566 A7 _____B7 _ V. Description of the invention (θ 〇 (Please read the notes on the back before filling this page) The primary goal of the present invention is high product flow rate and High purity. It is known that operating the evaporator system overheated (above TB) will give a large flow rate productivity, but the level of impurities will also increase. If this increase in impurities is acceptable, you can try to operate at temperatures above TB to achieve high flow rate productivity The non-obvious thing in this case is that it operates near TB. In the present invention, the superheat of the ammonia liquid at the penetration depth is maintained at a temperature below about 30 ° F, preferably below about 20 ° F, and most It is well below about 10 ° F. • Figure 2 illustrates the function of flow rate and impurities as a function of operating temperature. As the temperature increases, both the flow rate and impurity level increase. At π π i η, the impurities in the vapor phase system are very low, but the relative flow rate is too low to achieve the object of the present invention, that is, the high flow rate of the vapor phase product. Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs When the operating temperature increases, the flow rate starts to approach an acceptable predetermined range. Above Td (the predetermined temperature of the fluid at the penetration depth), the level of impurities may increase. As suggested in Figure 2, 'TD is the preferred operating temperature. At TA, the flow velocity is high enough. Although the impurity at this temperature is higher at lower temperature, it can still meet the objective of this case. Above T c, the level of the impurities becomes worse and cannot be accepted by the semiconductor industry. * In summary, Figure 2 illustrates the proper exchange between flow rate and impurity level. At T D, the system provides flow rates and impurity levels acceptable to the semiconductor industry. In order to maintain the desired evaporation flow rate ', power must be added to the system to supplement the heat required for evaporation. If this is not the case, the system temperature will decrease and the evaporation rate will decrease, so that the required evaporation flow rate cannot be achieved. If steam is still discharged at a high rate, the pressure will decrease and the liquid will begin to boil. Result 'Water, gas, oil and paper size Gu Zhongyunjia M specification (210X 297 mm) Mouth 6-559559 Printed by the Intellectual Property Bureau of the Ministry of Economy Staff Consumer Cooperatives A7 B7 V. Description of the invention (NVR and other purification advantages Both will be lost. • Standard evaporators using internal or external heaters and agitation tend to produce gradients and nucleation sites to promote boiling. Stirring will also increase the movement of the NVR, so its chance of entering the vapor phase is increased. The invention Microwave heating is used to control the power to maintain the evaporation process. An effective amount of microwave power is added to the liquid so that the temperature of the liquid at the penetration depth is substantially maintained at the boiling temperature of ammonia at a predetermined pressure. Figure 3 illustrates the operation of an evaporator system Conditions. The system is scheduled to operate within predetermined pressure and temperature parameters (each Pd and Td). It should be noted that TD is close to the boiling temperature TB, and TB corresponds to the saturated pressure PD. Now a cycle of operating conditions is discussed. In the cycle At the beginning, the system is at room temperature (* τ 3) and normal pressure (Patm), which is shown in point 1 of Figure 3. When microwave power is added, the penetration depth is increased The penetration depth is the top layer of the liquid (which can be as deep as 30 mm) which is really heated by microwave energy. In addition, when microwave power is added, the temperature and pressure of the penetration depth increase. In this way, the predetermined temperature Td and pressure can be achieved. PD, as shown in point 3 of Figure 3. When the predetermined pressure and temperature are reached, the liquid evaporation rate starts to increase. At the bottom of the penetration depth, the temperature is slightly lower than TD. The temperature here corresponds to T 2 in Figure 1. Steam leaves the liquid at the freeboard. The so-called free surface refers to the interface between steam and liquid. At higher steam demand rates, steam flows out of the system at a faster rate, resulting in a decrease in the system's steam pressure. A large amount of steam The pressure drop causes excessive disturbance of the liquid at the predetermined temperature TD. To avoid this result, 'providing microwave power, making the liquid temperature higher than TD, causing the fluid to increase evaporation as expected. Another result of increasing the steam flow rate without increasing the microwave power In order to penetrate deep paper, the Chinese National Standard (CNS) A4 specification (210X297 mm) is applicable. -17- ^^ Binding AW (Please read the precautions on the back before filling this page) 55 9566 A7 B7 V. Description of the invention (id (please read the precautions on the back before filling this page), the temperature will decrease. When the liquid turns into steam, the remaining liquid will be lower than D. It will be too cold, resulting in a decrease in flow rate. That is, point 4 in Fig. 3. In order to avoid the temperature and pressure lower than the lowest P l and T l, increase the microwave power to increase the liquid temperature and vapor pressure to TD and PD, as shown in point 3 in Figure 3. Microwave power • The temperature can be restored to the penetration depth. As a result, the vapor pressure-temperature balance is restored and the cycle restarts. In short, the present invention maintains the pressure and temperature below the vapor-liquid equilibrium curve and tries to maintain the pressure and temperature below about RD about 1 · 0 agitation curve. FIG. 4 illustrates a flowchart of the entire microwave evaporator of the present invention. The drum 1 supplies impure ammonia feed to the evaporator 10 via line 7. First, the feed stream 2 passes through the ES plate (emergency shutdown plate) 3 to obtain the liquid stream 4. If the valve 1 5 is opened, it continues to become the liquid stream 5 and passes through the valve 6 and then enters the evaporator 1 with the liquid stream 7 0. The drum is fed to the evaporator 10 to a set level. Line 1 1 transmits a level of ammonia specific level or gravity transmitter 1 2. 'This information is sent to the level controller 13 which regulates the ammonia feed stream via line 14 control valve 15. If the ammonia level in the tank is too low, the valve will open and the ammonia feed will fill the tank. If there is sufficient ammonia, the valve will close. The Ministry of Economic Affairs, Intellectual Property, Industrial and Consumer Cooperatives, India Fanfan If the system needs to be cleaned, the nitrogen tank 20 is fed to the Jiejie gas control board 2 2 through the line 21, and then the nitrogen is fed to the ES through the Jiejie line 2 3 0 板 3。 0 plate 3. Rinse with nitrogen and inerts to ensure that the evaporator system is dry. Once the evaporator has been properly filled, the magnetron 30 is turned on to supply the microwave power. When an ammonia product stream is required, the microwave power supply and the magnetron 30 are turned on. This microwave unit can supply high wattage, and the reaction pressure i paper size applies Chinese National Standard (CNS) A4 specifications (210X 297 mm) ~ 559566 A7 B7 V. Description of the invention (1 硿 (Please read the precautions on the back first) (Fill in this page again) The combination of the controller 5 8 and the reaction temperature controller 5 3 controls its cycle via line 61. The pressure and temperature controller is located inside the ammonia tank, namely 8 1, 8, 2, 8 3, and 8 4 The microwave power supply and the magnetron are operated at 2.45GHz or any suitable range in the microwave range. The single-mode microwave generated by the magnetron 30 is transmitted by the waveguide 31 and passed through a special predetermined security docking ring 3 2 Introduced into the evaporator. The employee cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs ’s consumer cooperative. The incident wave from the microwave is close to the plane of the vapor-liquid interface, which causes the transmission wave in the liquid medium and the reflected wave in the vapor phase medium. The penetration depth of the electric and magnetic fields will be limited. Under the above operation, the penetration depth is about 16 mm to about 20 mm below the free surface (free surface temperature is about 20 t). When heating, the free surface is below the free surface. About 16 mm to about The 20 mm layer will evaporate. The product vapor is discharged from the outflow hole 42 and the flow restriction control valve 4 7 (controlled by the reaction flow controller 45). The present invention provides production at a rate of up to 2 500 gas cc / mi η Logistics to customer battery side. The average power input is from 200 to 4 500 watts per square foot. In the ammonia example, the microwave energy flux used is from about 0.3 to about 10 watts per square inch. It is preferably about 0.3 to about 20 watts per square inch, and more preferably about 0.3 to about 30 watts per square inch. This can be achieved by thermal equilibrium between the liquid-holding vapor phase.ρ The ID (constant product-derived) control loop controls the microwave power, which can quickly respond to demand and maintain a stable vapor pressure (loss due to high product flow rate), that is, by supplemental heat to the system. Gaseous ammonia flows out of the ammonia tank. Circuit 40 passes through the outflow hole 42, which passes through the flow restriction control valve to produce an ultra-high purity gaseous ammonia product stream 48. At the same time, the flow transmitter 43 measures the flow of liquid through the outflow hole. Transporter-19 -This paper size applies to China National Standard (CNS) Α4 size (210X 297mm) 559566 A7 Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs. 5. Description of the invention (θ will notify the flow controller to the flow controller. The information of the flow transmitter is transmitted to the flow controller 45, which instructs the opening and closing of the flow restriction control valve. The temperature and pressure data is read on the top of the ammonia tank. The temperature data is transmitted to the temperature transmitter via line 51. At the same time, the pressure data is transmitted to the pressure transmitter via line 56. Although the illustration is external, the temperature and pressure The pressure transmitter is actually located inside the system, above the free surface. The temperature and pressure transmitter converts the data into signals that can be interpreted by the temperature controller 5 3 and the pressure controller 58. The temperature and pressure controllers 5 3 and 5 8 send their data to the low level and select 60, which instructs how much microwave power the magnetron needs to restore balance through line 61. With increasing product flow, the vapor pressure ρv decreases, causing an increase in microwave power. Therefore, when the penetration depth temperature tpd is increased, the microwave power will decrease, thereby reducing the steam pressure, and the power control cycle will continue. The pressure controller, temperature controller and low level selection include a universal controller. Selecting a low level of 60 determines whether the magnetron 30 should be on or off. The low level selection 60 operates by selecting the lowest relative pressure between temperature and pressure. For example, if the pressure level is lower than the temperature level, selecting a low level of 60 will “low select” the pressure level and discard the temperature input (as long as the temperature is not too high). Selecting a low level of 60 will consider the pressure to be decreasing, so via line 6 1 the magnetron will be told to turn on. When the pressure is a low-selected signal, but is not lower than the predetermined parameter, line 61 will indicate that the magnetron is still closed. The above description is also applicable to the signal when the temperature is low. When the amount of liquid in the tank is reduced due to evaporation, impurities in the overall liquid will increase. When the level of impurities is too high, remove the waste liquid out of the tank. Via the line (please read the precautions on the back before filling this page)-φ installed.. Then fill in the wood • 1T Φ This paper size applies to China National Standard (CNS) Α4 specification (210X297 mm) -20- 559566 A7 • _B7____ 5. Description of the invention (id 70 and valve 7 1 discharge ammonia to form a liquid stream 7 2 and store it in a waste tank 7 3 〇 (Please read the precautions on the back before filling this page) This invention can use any polarity Saturated liquid operation, however, for the purposes of the present invention, in particular, the related saturated liquid may include, but is not limited to, NΗ3, HF, SiHCl3, SiH2Cl2, C4H8, C3F8, ΗBr, C5F8, C 1 F 3, TE0S and the like. The frequency of this device is 915, 2450, 5850 and 1 8000MHz. This method can achieve high flow rate of 1 to 2500 l / min or higher, and the water vapor and NVR levels are less than About 1 ppm. The dirt remaining in the liquid beach can be continuously discarded or continuously discarded by continuous charging. The system performance is optimized by integrating the geometry and multiple magnetrons placed around the volume of the liquid in a specially predetermined shape. .This can reduce the number of microwave interference patterns, which cause Uneven focus and heating. The characteristics of the invention shown in one or more drawings are for reference only, as the characteristics can be combined with other characteristics according to the invention. Other specific examples are recognized by those skilled in the art and intended to be applied The scope of patent is included. Printed by the Consumer Cooperatives of the Intellectual Property Office of the Ministry of Economic Affairs-21-This paper size applies to China National Standard (CNS) A4 (210X297 mm)