TW200400921A

TW200400921A - Apparatus for the generation of fluorine gas

Info

Publication number: TW200400921A
Application number: TW092118556A
Authority: TW
Inventors: Sonobe Jun; Ino Minoru; Fukuoka Muneyuki; Kimura Takako
Original assignee: Air Liquide
Priority date: 2002-07-11
Filing date: 2003-07-08
Publication date: 2004-01-16
Also published as: TWI293342B; KR20050017115A; CN1668779A; WO2004007802A3; WO2004007802A2; KR101065906B1; JP3905433B2; JP2004043885A

Abstract

To provide an apparatus for the generation of fluorine gas that is capable of very safe and highly reliable operation even during long-term operations. An apparatus 30 for the generation of fluorine gas is provided with an electrolytic cell 32 that generates, in a first gas phase region on the anode side, produce gas whose main component is fluorine gas and at the same time generation, in a second gas phase region on the cathode side, by-product gas whose main component is hydrogen gas. A first and second pressure gauges 46 and 48 are provided in order to measure the pressure in the first and second gas phase regions. A first and second conduits 52 and 72 are provided in order to withdraw the product gas and by-product gas. A first and second flow rate control valves are disposed in the first and second conduits 52 and 72. The apertures of the first and second flow rate control valves are adjusted based on the measurement results from the first and second pressure gauges 46 and 48 so as to maintain the pressures in the first and second gas phase regions at first and second set values that are substantially equal.

Description

200400921 玖、發明說明：【發明所屬之技術領域】本發明關於-種產生氟氣之裝置（下文中以氟氣產生器稱之）。更特別的是’本發明關於一種氟氣產生器（ fluorine gas generator)，該i氣產生器被配置在二至種半導體製程线的氣體供給系統中。本文中所述之半導體製程論及數道被實現來製造在基板上料㈣元件以及 /或半導體元件之連結結構（例如是：内連結與電極）的製程，其涉及在目標基板（target substrate)(例如是 •半導體晶圓或是LCD基板）上進行半導體層、介電層與導電層的特定圖案之成形的製程。在半導體元件的製造期間’數道半導體製程，例如是 4膜成形、蝕刻以及擴散等製程被實現到該目標基板（例如是：半導體晶圓或是LCD基板）上。在許多種的應用中，例如是：矽薄膜、氧化矽薄膜的蝕刻，被用來實現這些處理之該半導體製程系統運用氟基氣體（fluorine-type gas )作為製程氣體，並且該半導體製程系統被用來清潔製程反應室（process c⑽partment)的内部。氟氣已經引起注目而被接受為一種新的蝕刻氣體以及清潔氣體，但是因為它的安全性與可靠度並未被完全滿足，以致於通常不在半導體元件製造的實際位置處產生。【先前技術】電解電池基（elec1;rolytic cell_based)裝置已知在 ^uuH-uuyzi 乳體生產廄處被用來生產氟氣。例如，產生器被揭示在曰本開 _的氟氣 (灣請，卿/_ ==號Hei9侧3 一種從頂部延伸進入到 ' 所揭不的裝置中，該電解電池的内部分严志— 裒置^作用為將陰極隔室。兩個不同高度的端部至繞的至之内。這兩個探針作為 ^ 卞作為液面位準計（surface level gauge)用以起動該陽極盥 Vel200400921 (1) Description of the invention: [Technical field to which the invention belongs] The present invention relates to a device for generating fluorine gas (hereinafter referred to as a fluorine gas generator). More specifically, the present invention relates to a fluorine gas generator, which is configured in a gas supply system for two or more semiconductor process lines. The semiconductor process described in this article addresses the process by which several processes are implemented to fabricate material structures on semiconductor substrates and / or semiconductor structures (eg, internal interconnections and electrodes), which involves the process of forming a target substrate. (For example, a semiconductor wafer or an LCD substrate) a process of forming a specific pattern of a semiconductor layer, a dielectric layer, and a conductive layer. During the manufacturing of semiconductor elements, several semiconductor processes, such as 4 film forming, etching, and diffusion processes, are implemented on the target substrate (for example, a semiconductor wafer or an LCD substrate). In many applications, such as: etching of silicon films and silicon oxide films, the semiconductor process system used to achieve these processes uses a fluorine-type gas as the process gas, and the semiconductor process system is Used to clean the inside of the process c⑽partment. Fluorine gas has attracted attention and has been accepted as a new etching gas and cleaning gas, but because its safety and reliability have not been fully satisfied, it is usually not generated at the actual location of semiconductor device manufacturing. [Prior art] An electrolytic cell-based (elec1; rolytic cell-based) device is known to be used to produce fluorine gas at the ^ uuH-uuyzi milk production site. For example, the generator was revealed in the Japanese version of the fluorine gas (wan please, Qing / _ == No. Hei9 side 3 a device extending from the top into the uncovered device, the inner part of the electrolytic battery Yan Zhi — The ^ set serves to hold the cathode compartment. Two ends of different heights are within the winding range. These two probes are used as ^ 卞 as a surface level gauge to activate the anode toilet Vel.

的控制。因此，此一 f置的電流供給之0N/〇FF 裒置彳3者偵測該熔融鹽類的液面位準的方式來控制氟氣的產生。另種氟氣產生器的先前技藝被概略地說明於圖3中。此-裂置具有一種用於控制來自該電解電池之氣氣的供給之改良式結構。在此種特別的裝置中，在一個電解電池 112,的該陽極114側所產生的i氣被持續地進給通過一個導管120接著進入到—個中級的容器116’並且被短暫地健存於其中。當該容器116到達某—特定的壓力時，一個配置在一個壓縮機118與該容器ιι6之間的切換閥（ switching valve) 122被暫時地打開，並且某一特定量的氟氣被吸入到该壓縮機i 18之内。該切換閥丄2 2被重複地才木作以將4第二緩衝槽丨2 4的壓力提昇到達一個特定值。【發明内容】在本發明研究發展期間，當在圖3中所說明的該氟氣產生益被長時間地操作時，本案發明人發現有下述數種安全，與可靠度之問題發生。對於上述問題仏的銳’點末看，是相當困難將該氟氣產使用在一種自動化的生產手咣中，Υί ^ 或體元件的系統中。中例如，使用在製造半導發明：考量到先前技藝的上述問題之後發展出本發明。本二個目的是提供—#氟氣產生器，該作期門太Γ 操作，即使是在長時間的摔本發明的一個特別的目的是提供一種裝置，該裝。：於:iV:::mand)，^ ^, 〃竹引戒罝結合或組裝在一起，例如，_ 個半導體製程***。，，卽睥^ 伴P左斜/私干守（on-demand)，，意指該氣體可以狀： “份的控制情況下被供給，來響應該主製程裝置的要求之時序（timing)。以本發明的第一能揭白虹士 & 心樣匕括有：一種用於產生氟氣之裝置，该裝置被特徵化地提供有： 1control. Therefore, the 0N / 0FF setting of the current supply means 3 detects the liquid level of the molten salt to control the generation of fluorine gas. The prior art of another fluorine gas generator is schematically illustrated in FIG. 3. This split has an improved structure for controlling the supply of gas from the electrolytic cell. In this particular device, the i gas produced on the anode 114 side of an electrolytic cell 112, is continuously fed through a conduit 120 and then into an intermediate container 116 'and is temporarily stored in among them. When the container 116 reaches a certain pressure, a switching valve 122 disposed between a compressor 118 and the container 6 is temporarily opened, and a certain amount of fluorine gas is sucked into the Within compressor i 18. The switching valve 丄 2 2 is repeatedly operated to raise the pressure of the 4 second buffer tank 丨 2 4 to a specific value. [Summary of the Invention] During the research and development of the present invention, when the fluorine gas generating benefit illustrated in FIG. 3 was operated for a long time, the inventors of the present case found that the following types of safety and reliability problems occurred. At the end of the above point, it is quite difficult to use the fluorine gas production in an automated production system, or a system of solid components. For example, the invention is used in the manufacture of a semiconducting invention: the above problems have been developed in consideration of the previous art. The two objectives are to provide a ## fluorine generator, which is operated during a long time, even if it is dropped for a long time. A special object of the present invention is to provide a device which ：于: iV ::: mand), ^ ^, 〃竹引罝 or 罝 are combined or assembled together, for example, _ semiconductor process systems. , 卽睥 ^ with P left oblique / on-demand, which means that the gas can be: "Serving under control of the supply, in response to the timing of the request of the main process device. In the first aspect of the present invention, Hong Hong Shi & Heart-shaped dagger includes: a device for generating fluorine gas, the device is characteristically provided with: 1

—個電解雷孙，#恭A 以電解電池在一個電解浴（人rolyt 1C bath)中實現氟化氫的電解’該電解浴包括 :有氟化氫的溶融鹽類’並且藉以在該陽極侧的一個第— 氧相區域處產生翁能志从！ ϋ ”心產4 ’该氣體產物的主成份是氟氣， j同Τ門在陰極側上之_個第二氣相區域中產生氣體副產物，該氣體副產物的主成份為氫氣；個I始材料導官，該起始材料導管將起始的氣化氫供給到該溶融鹽類·， 10 —個第一導管，該第一相區域處抽回； —個第二導管，該第二氣相區域處抽回；一個第一壓力計，該第氣相區域的壓力；一個第二壓力計，該第氣相區域的壓力；導管將S亥氣體產物從該第一氣導管將該氣體副產物從該第二壓力計持續地量測在該第一壓力计持續地量測在該第二一個第一流率控制閥，今 ^ φ ^ Μ第一"丨L率控制閥被配置在該第一導管内；仕袭一個第二流率控制閥，妗链__ Μ第一、"IL率控制閥被配第二導管内； -個第㈣構件’該第—控制構件依據來自該第一壓力計的量測結果來調整該第—流率控制閥的隙缝，用以將該第-氣相區域的壓力維持在一個第一設定值；以及— An electrolytic thunder grandson, #Christian A. Electrolysis of hydrogen fluoride in an electrolytic bath (human rolyt 1C bath) with an electrolytic cell 'The electrolytic bath includes: molten salts with hydrogen fluoride' and a first on the anode side— Weng Nengzhi Cong is generated in the oxygen phase area!心 "Heart production 4 'The main component of this gas product is fluorine gas, j and T gate produce gas by-products in the second gas phase region on the cathode side, and the main component of this gas by-product is hydrogen; I A starting material guide, the starting material conduit supplying the starting hydrogenated gas to the molten salt, 10-a first conduit, withdrawn at the first phase region;-a second conduit, the second Withdraw at the gas phase region; a first pressure gauge, the pressure in the second gas phase region; a second pressure gauge, the pressure in the second gas phase region; By-products are continuously measured from the second pressure gauge. The first pressure gauge is continuously measured at the second first flow rate control valve. Today, the first rate control valve is configured. In the first conduit; A second flow rate control valve is officially launched, and the first and second IL rate control valves are equipped in the second conduit; a third component, the first control component is based on The measurement result from the first pressure gauge is used to adjust the gap of the first flow rate control valve for The second - vapor pressure is maintained at a first region of the set value;

•^個第二控制構件，該笫-伙制接姓分A 卑—控制構件依據來自該第二塵力計的量測結果來調整該第二流率控制閥的隙縫，用以將該第二氣相區域的壓力維持在一個第二設定值’其中，該第二設定值大致寻於該第一設定值。本發明的第二態樣包括有：該第一態樣的裝置，其特徵在於該第一設定值與該第二設定值為76〇__82〇托耳（ Torr) 0 本發明的第三態樣包括有：根據該第—與該第二態樣的裝置’其特徵在於額外地提供有一個第一抽吸裝置，咳 200400921 第-抽吸裝置被配置在該第一導管内，該第一導管位於該第-流率控制閥的下游處，並且該第一抽吸裝置能夠抽吸該第一導管。本發明的第四態樣包括有：根據該第三態樣的裝置，其特徵在於該第二導管被配置於第二流率控制閥的下游處，以將該第二流率控制閥連接到一個第二抽吸裝置，該第二抽吸裝置能夠抽吸該第二導管。本發明的第五態樣包括有：根據該第-到第四態樣的任何一個的装置，其中，該裝置特徵在於也被提供有： · 一個切換閥，該切換閥被配置在該起始材料導管内；们電仙' 1 5器（current integrator )，該電流整 a器查〇於4電解電池的陽極側上的電極以及該電解電池的陰極側上的電極之間被供給的電流；以及個控制構件，該控制構件依據該電流整合器所產生的量測結果來操作該切換閥’用以控制進入到該溶融鹽類之内的氟化氫之供給。本發明的第六態樣包括有：根據該第五態樣的裝置，籲其特徵在於被進給通過該起始材料導管之氣化氯為—種氣设明的第七態樣包括冑：根據該第六態樣的裝置，其特徵在於配置該起始材料導管，用以將氣化氫氣體供給到該電解電池之陰極側上的溶融鹽類之内，以及—個可以 :鼠氣，應到該起始材料導f之内的導管被連接到該起始 ’枓導官’其位於前述的切換閥之下游處，並且該氟化氫• ^ second control member, the unit-name system is followed by A, and the control member adjusts the gap of the second flow rate control valve according to the measurement result from the second dust meter to use the first The pressure in the second gas phase region is maintained at a second set value, where the second set value is approximately the first set value. A second aspect of the present invention includes: the device of the first aspect, characterized in that the first set value and the second set value are 76〇__82〇 Torr 0 The third aspect of the present invention Samples include: according to the first and second aspects of the device 'characterized in that a first suction device is additionally provided, and the 400400921 second suction device is arranged in the first catheter, the first A conduit is located downstream of the first flow rate control valve, and the first suction device is capable of suctioning the first conduit. A fourth aspect of the present invention includes: the device according to the third aspect, wherein the second conduit is disposed downstream of the second flow rate control valve to connect the second flow rate control valve to A second suction device capable of suctioning the second catheter. A fifth aspect of the present invention includes: the device according to any one of the first to fourth aspects, wherein the device is also characterized by being provided with: a switching valve configured at the start In the material conduit; they are electric current (current integrator), which checks the current supplied between the electrode on the anode side of the 4 electrolytic cell and the electrode on the cathode side of the electrolytic cell; And a control component, which controls the switching valve 'according to the measurement result generated by the current integrator to control the supply of hydrogen fluoride into the molten salt. A sixth aspect of the present invention includes the device according to the fifth aspect, which is characterized in that the vaporized chlorine fed through the starting material conduit is-a seventh aspect of the specified gas species including: The device according to the sixth aspect is characterized in that the starting material conduit is configured to supply hydrogenated gas into molten salts on the cathode side of the electrolytic cell, and one can: rat gas, A conduit that should be within the starting material guide f is connected to the starting 'steering officer' which is located downstream of the aforementioned switching valve, and the hydrogen fluoride

12 200400921 與該氮氣混合而一起被供給到該熔融鹽類之内。本發明的第八態樣包括有：一種氣氣產生器，其被特徵化地提供有：一個電解電池’該電解電池在一個電解浴（ electrolytic bath)中實現氟化氫的電解，該電解浴包括含有氟化氫的熔融鹽類，並且藉以在該陽極側的一個第一氣相區域處產生氣態產物，該氣體產物的主於同一時間’在陰極側上之-個第二氣相區域中;=體副產物，該氣體副產物的主成份為氫氣；鲁 -個起始材料導管，該起始材料導管將起始的氟化氫供給到該炫融鹽類；個第一導官，該第一導管將該氣體產物從該第一氣相區域處抽回；一個第二導管’該第二導管將該氣體副產物從該第二氣相區域處抽回；一個切換閥，該切換閥被配置在該起始材料導管之内 β 個電流整合器，該電流整合器整合於該電解電池的陽極側上的電極以及該電解電池的陰極側上的電極之間被供給的電流；以及個&制構件，該控制構件依據該電流整合器所產生的量測結果來摔作兮术作5玄切換閥’用以控制進入到該熔融鹽類之内的氟化氫之供給。 | 本^月的第九態樣包括有：根據該第八態樣的裝置， 13 200400921 其特徵在於被進給it過該起始材料導管之說化氣為—種氣體。 ” 本發明的第十態樣包括有：根據該第九態樣的裝置，其特徵在於配置該起始材料導管，用以將氟化氨氣體供认到該電解電池之陰極側上的熔融鹽類之内，以及一個可= 將氮氣供應到該起始材料導管之内的導管被連接到該起= 材料導管，其位於前述的切換闕的下游處，並且該氣化氣與該氮氣混合而一起被供給到該熔融鹽類之内。！此外’此-發明的若干實施例探討本發明的許多實施方式，並且此-發明之不同的實施例可以由所揭示的構成元件之複數種合適的組合來衍生出。例如，當本發明的— 個實施例已經從揭示的整組構成元件中省略某些構成元件而衍生出日寺，這些個被省略的元件可以透過習知技蓺來適當地實現於能實際運作的被衍生出之發明實施例。【實施方式】在發展本發明期間，本案發明人研究說明於圖3中之先前技藝的氟氣產生器有關的安全性與可靠度。本案發明人由於此一研究的結果而獲致下列的知識。〜在圖3所說明的裝置之操作中，該切換闕122於該容器1 1 6達到壓力上限的他· .、9 -ΙΓ、+ α ㈣狀/兄下被打開’並且達到麼力下限的狀況下被關閉。上述情況造成在該氟氣導管12〇中極大的壓力變化產生。由這些極大壓力變化& g丨# 刀支化所弓I起的該熔融鹽類之霧氣在入口處到該氣氣導管120處累積，該炫融鹽類 34 200400921 之務氧is·成遠氟氣導管12 0被堵塞。此外，由於該切換閥 122頻繁的打開與關閉，該切換閥122的承座（seat )是相當容易被固化的溶融鹽類顆粒的機械性作用（ mechanical action)與該氟氣的化學性作用（chemical action)而損壞。對於另一個與說明於圖3中之裝置有關的問題，須注心在陰極側上所產生的虱氣通過該排氣系統（ system)的導管121，並且在稀釋過後從該系統處由一個最小值到一個通常控制的數值之方式被釋放。可以被預期籲到的疋在该排放系統（discharge system )中的壓力將是以工廠環境為函數的方式改變。例如，當該排氣系統具有一個高的抽吸容量時’在該陰極側上之壓力將自發地變成一個負壓並且在該陰極側上與其連結的該熔融鹽類之液面將上升。該液面在此一種情況下歷經一個主要的變化，其12 200400921 is mixed with the nitrogen gas and supplied into the molten salt together. An eighth aspect of the present invention includes: a gas generator, which is characterized by being provided with: an electrolytic cell, the electrolytic cell realizes the electrolysis of hydrogen fluoride in an electrolytic bath, the electrolytic bath includes Molten salts of hydrogen fluoride and thereby produce gaseous products at a first gas phase region on the anode side, the main of the gas products being at the same time 'in a second gas phase region on the cathode side; = bulk side The main component of the gas by-product is hydrogen; a starting material conduit that supplies the starting hydrogen fluoride to the dazzling molten salts; a first guide, the first conduit A gas product is withdrawn from the first gas phase region; a second conduit 'the second conduit withdraws gas byproducts from the second gas phase region; a switching valve, the switching valve is arranged at the starting Β current integrators within the starting material conduit, the current integrators integrating current supplied between an electrode on the anode side of the electrolytic cell and an electrode on the cathode side of the electrolytic cell; and &Amp; braking member, the control member based on the measurement result of the current generated by the integrator to fall for surgery as Xi Xuan switching valve 5 'for controlling the feed of hydrogen fluoride into the molten salt within it. The ninth aspect of this month includes the device according to the eighth aspect, 13 200400921, which is characterized in that the gas that is fed through the starting material conduit is a kind of gas. A tenth aspect of the present invention includes the device according to the ninth aspect, characterized in that the starting material conduit is configured to supply ammonia fluoride gas to the molten salt on the cathode side of the electrolytic cell. Inside, and a pipe that can supply nitrogen into the starting material pipe is connected to the starting material pipe, which is located downstream of the aforementioned switching ridge, and the gasification gas is mixed with the nitrogen together Are supplied into the molten salt. In addition, 'this-invention's several embodiments explore many embodiments of this invention, and this-invention's different embodiments can be composed of a plurality of suitable combinations of the disclosed constituent elements For example, when an embodiment of the present invention has omitted some constituent elements from the entire set of constituent elements disclosed to derive the temple, these omitted elements can be appropriately implemented through conventional techniques. An embodiment of the invention that can be practically derived. [Embodiment] During the development of the present invention, the inventor of the present case studied the fluorine gas generator of the prior art illustrated in FIG. 3 Related to safety and reliability. As a result of this research, the inventor of this case obtained the following knowledge. ~ In the operation of the device illustrated in FIG. 3, the switch 阙 122 was reached at the pressure limit of the container 1 1 6 ·., 9 -ΙΓ, + α ㈣ shape / brother is opened 'and closed under the condition that the lower limit of force is reached. The above situation results in a large pressure change in the fluorine gas conduit 120. These extreme pressure changes & g 丨 # The mist of the molten salt from the bow of the knife branch accumulates at the entrance to the gas duct 120, the dazzling molten salt 34 200400921 is the oxygen is a remote fluorine gas duct 12 0 In addition, due to the frequent opening and closing of the switching valve 122, the seat of the switching valve 122 is a mechanical action of the molten salt particles that is relatively easily solidified and the chemical action of the fluorine gas. Damage caused by chemical action. For another problem related to the device illustrated in FIG. 3, care must be taken that the lice generated on the cathode side pass through the duct 121 of the exhaust system, and After dilution The system is released from a minimum to a commonly controlled value. It can be expected that the pressure in the discharge system will change as a function of the factory environment. For example, when the When the exhaust system has a high suction capacity, the pressure on the cathode side will spontaneously become a negative pressure and the liquid level of the molten salt connected to it on the cathode side will rise. The liquid level is here One case undergoes a major change, which

導致該熔融鹽類被抽入該氫氣導管121内，並且因此阻塞該導管121。 A 一旦該熔融鹽類在該等導管12〇與121内已經被固化籲後钐止該及置並且執行維護操作變得需要，其亦造成該衣置所連接之整個系統的停工。除此之外，該氟氣導管 12 〇 ” 4氫氣導管i 21兩者之一的阻礙亦導致該電解電、，也 112之内的平衡壓力之干擾。在該電解電池I〗？之内的平衡壓力之主要干擾的發生會導致在該電解電池112之内的氟孔與氫氣之間的接觸，其會有產生***的危險。，本發明具有一種依據上述知識之結構。此一發明的若 15 200400921 干實施例被說明於下文中及本文中所附的圖式。在下文的說明中，這些具有近乎相同的結構與功能之構成元件被指定-個相同的符號，而且其說明解釋將僅在需要時才被重複。圖1包含一個概略圖式，其說明一種半導體製程*** ，該半導體製程系統併人-個氟氣產生器，該氟氣產生琴為本發明的一個實施例。此一半導體製程系統包含有一個半導體製程裝置10，該半導體製程裝置10在一個例如This causes the molten salt to be drawn into the hydrogen conduit 121, and thus blocks the conduit 121. A Once the molten salt has been solidified in the conduits 120 and 121, stopping the placement and performing maintenance operations becomes necessary, which also causes a shutdown of the entire system to which the garment is connected. In addition, the obstruction of one of the fluorine gas conduit 12 0 ″ 4 and the hydrogen conduit i 21 also causes the interference of the equilibrium pressure within the electrolytic cell, and also within 112. Within the electrolytic cell I? The occurrence of the main disturbance of the equilibrium pressure will cause the contact between the fluorine holes and the hydrogen in the electrolytic cell 112, which will cause the risk of explosion. The present invention has a structure based on the above knowledge. 15 200400921 Dry embodiments are described below and in the drawings attached hereto. In the following description, these constituent elements having almost the same structure and function are designated with the same symbol, and the description and explanation thereof will only be It is repeated only when needed. Figure 1 contains a schematic diagram illustrating a semiconductor process system that incorporates a fluorine gas generator, which is an embodiment of the present invention. This one The semiconductor process system includes a semiconductor process device 10, which

士半導體晶圓或是LCD基板之目標基板上執行—種例如是薄膜成型、蝕刻、或擴散之製程。該半導體製程裝置10被提供有一個製程反應室Μ，該製減應室12握住該目標基板，並且該半導體製㈣其：被實施。配置在該製程反應室12之内的是一個裝爲平臺14 (支撐構件），該裝設平臺14功用有如一個下力電極與個用於裝設該目標基板的平臺兩者。一個上方電極16亦被配置在該製程反應室12之内，該製程反應室rIt is performed on a target substrate of a semiconductor wafer or an LCD substrate—a process such as thin film forming, etching, or diffusion. The semiconductor process apparatus 10 is provided with a process reaction chamber M, the process chamber 12 holds the target substrate, and the semiconductor process is performed. Arranged within the process reaction chamber 12 is a mounting platform 14 (supporting member), which functions as a downward electrode and a platform for mounting the target substrate. An upper electrode 16 is also disposed in the process reaction chamber 12, and the process reaction chamber r

㈣該震設平4 14°RF (高頻hlgh freqUency)電力可以伙個RF電源15橫跨該兩電極14與16的方式被施加，用^在邊製程反應室12之内形成一· RF場其目的為將該製=體轉換成電漿一種排氣系統18被連接到該製程反應至12之下方區域’以達成排空該製程反應室的内部並且於其中建立真空之目的。一個氣體供給系、统20被連接到該製程反雍$彳9 + l + ^ t 體之目的。-之上方區域’以達成供給該製程氣 16 200400921 圖2包含一個概略圖示，其表示該半導體製程裝置 1 ox的修正過之實例，該半導體製程裝置】〇χ可以被用來與說明於圖1中之該氣體供給系統20相結合。此一半導體製程裝置ιοχ被提供有一個製程反應室12，該製程反應室 12握持住該目標基板，而且該半導體製程於其中被實施。一個裝設平臺14 (支撐構件）被配置在該製程反應室12 之内’以達成裝設該目標基板之目的。一個排氣系統i 8 被連接到該製程反應室12之上方區域，以達成排空該製程反應室的内部並且於其中建立真空之目的。一個遠端電鲁漿室13被連接到該製程反應室12之上方區域，以達成形成電漿之目的。該遠端電漿室13之周邊被盤繞有一個線圈天線17。來自該RF電源15到該線圈天線丨7的RF電力的應用導致在該遠端電漿室13中形成感應場，以達成將及製程氣體轉換成電製之目的。一個氣體供應系統2 〇被連接到該遠端電聚室1 3之上方區域，以供應該製程氣體。包含有本發明實施例之該氟氣產生器也可以與不利用籲電漿例如來將清冻氣體供應到一個熱的CVD設備之半導體製程設備一起使用。再次參照圖1，一個流量管理區段22被配置在該氣體供應系統20之内；此一流量管理區段22可以將任何指定的氣體（例如是.用於完成一道半導體製程的製程氣體或者是用於清潔該製程反應室12之内部）在一個特定的速度下供應到s亥装私反應室12之内，並且也能夠選擇性的 17 200400921 刀換。一個氣體儲存區段24被連接到該流量管理區段& 邊氣體儲存區段24包含有··複數個氣體源並儲存數種活I1生以及/或惰性氣體。同樣被連接到該流量管理區段U 的疋一個氣體產生區段26，該氣體產生區段26藉著一個反應程序來產生氟氣類之製程氣體。 —個包括有本發明的一個實施例之氟氣產生器3〇係以種可分離的方式連接到該流量管理區段22與該氣體產生區段26。更特別的是，此一氟氣產生器3〇不是直接震 The seismic level 4 14 ° RF (high-frequency hlgh freqUency) power can be applied with an RF power source 15 across the two electrodes 14 and 16 to form an RF field within the side-process reaction chamber 12 The purpose is to convert the system into a plasma. An exhaust system 18 is connected to the area below the process reaction 12 to achieve the purpose of emptying the interior of the process reaction chamber and establishing a vacuum therein. A gas supply system, system 20, is connected to the process for the purpose of $ 彳 9 + l + ^ t system. -The upper area 'to achieve the supply of the process gas 16 200400921 Figure 2 contains a schematic diagram showing a modified example of the semiconductor process device 1 ox, the semiconductor process device] 0χ can be used as illustrated in the figure The gas supply system 20 in 1 is combined. This semiconductor process device is provided with a process reaction chamber 12, the process reaction chamber 12 holds the target substrate, and the semiconductor process is performed therein. An installation platform 14 (supporting member) is disposed within the process reaction chamber 12 'to achieve the purpose of installing the target substrate. An exhaust system i 8 is connected to the area above the process reaction chamber 12 to achieve the purpose of evacuating the inside of the process reaction chamber and establishing a vacuum therein. A remote plasma chamber 13 is connected to the area above the process reaction chamber 12 to achieve the purpose of forming a plasma. A coil antenna 17 is coiled around the distal plasma chamber 13. The application of RF power from the RF power source 15 to the coil antenna 17 results in the formation of an induction field in the remote plasma chamber 13 to achieve the purpose of converting the process gas into electricity. A gas supply system 20 is connected to the area above the remote galvanic chamber 13 to supply the process gas. The fluorine gas generator including the embodiment of the present invention can also be used with a semiconductor process equipment that does not use a plasma, for example, to supply a freezing gas to a hot CVD equipment. Referring again to FIG. 1, a flow management section 22 is configured within the gas supply system 20; the flow management section 22 may use any specified gas (for example, a process gas used to complete a semiconductor process or a Used to clean the inside of the reaction chamber 12 of the process) is supplied into the private reaction chamber 12 at a specific speed, and can also be selectively changed. A gas storage section 24 is connected to the flow management section & the side gas storage section 24 contains a plurality of gas sources and stores several kinds of live and / or inert gases. Also connected to the flow management section U is a gas generating section 26 which generates a process gas such as fluorine gas through a reaction procedure. A fluorine gas generator 30 including an embodiment of the present invention is connected to the flow management section 22 and the gas generating section 26 in a separable manner. More specifically, this fluorine gas generator 30 is not directly

將该亂氣供給到該流量管理區段22，就是被用來將該起始的氟氣供應到該氣體產生區段26 (切換閥未被顯示）。該氣體產生區段26藉由將該起始的氟氣與其它的鹵素氣體 (例如疋.氯）反應而可以產生，例如是：—種鹵素與鹵素間之氟化合物氣體。 δ亥氟氣產生器30包含有：一個氣密式電解電池32， •^氣氆式包解電池32容納一種電解浴，該電解浴包括：含有氟化氫之熔融鹽類。該熔融鹽類包括有：氟化鉀（Supplying the turbulent gas to the flow management section 22 is used to supply the initial fluorine gas to the gas generating section 26 (the switching valve is not shown). The gas generating section 26 can be generated by reacting the starting fluorine gas with other halogen gas (e.g., 疋. Chlorine), for example: a fluorine compound gas between halogen and halogen. The delta helium gas generator 30 includes: a gas-tight electrolytic cell 32, and a gas-encapsulated battery 32 containing an electrolytic bath, the electrolytic bath including: molten salts containing hydrogen fluoride. The molten salts include: potassium fluoride (

1與氟化氯（HF)之混合物（KF/2HF)，或者是氟化氫與彿萊明鹽類（Fremy，s salt)。該氣密式電解電池32藉由 —個隔離薄片（partiti〇n sheet) 35而被分隔成一個陽極室34與一個陰極室36，該隔離薄片35從頂部延伸進入該熔融鹽類。一個碳質電極（陽極）42被浸入於在該陽極至34中之熔融鹽類内，而同時，一個鎳質電極（陰極）軻被浸入於在該陰極室36中之熔融鹽類内。被附著於該氣密式電解電池32為一個電流源38與一個電流整合器4〇， 18 其中，該電流源38 w ,、； + Λ ^干在該陽極42與該陰極44之間佴庫電流，而该電流整合器4。整合被供給的電流。仏應於該電解過程期間，該氣力，廳⑽而被加熱到並保持：8= 二=破附解浴中的氟化氫之電解導致在墙：9〇C之間。在该電 “…士％極室34的氣相區域中 ▲ 物，該氣體產物的主成份為氟氣（F2)，而在忒陰極室36的氣相區域中產生生乳體副產物，該氣體副產的主成份為氳氣。氟化氫依據於該熔融鹽類之中的氟化氮氣體的蒸氣壓之供獻而被混合（例如是：5%)在該氣體產物與該氣體副產物兩者中。—個第—壓力規Μ被配置在該陽極室34上，而一個第二a力規Μ被配置在該陰極室36上，用以連續地量測該等個別氣相區域的壓力。一個第一導管52被連接到該陽極室34，用以抽回氣體產物，並且將該氣體產物傳輸到該流量管理區段22與該氣體供應系.統20之氣體產生區段26。從上游處依續被配置在該第-導管52》：-個第—流率控制閥“、一個吸收E 56 ' -個迷你緩衝槽（minibuffer tank ) 58、一個壓縮機（抽吸裝置）62、以及一個主緩衝槽64。被產生在該該陽極室34中的氣體產物由該壓縮機（抽吸裝置）62 透過該第一導管52的抽吸強力地從該陽極室34處被抽出，並且被儲存在該主缓衝槽64内。在圖】中的元件符號 66代表一個管線過濾器。如上所〉主意到的，氟化氫將在數種百分比（例如是： 5 % )被混合在該氣體產物中。當該氣體產物通過該吸收 29 200400921 民56時，該氟化氣被降本 m 以踢此^^ 因此，該吸收£ 56應該容納以及收方式〉及取氣/μ _ 匕虱的吸收劑容量。依據處理與壓力損 …：下，该吸收劑應該包括有：被充填在該吸收£ 56 里的小弹丸。該吸收劑可以包含收能力如溫度函數般p、、s电^ 疋，、迎，皿度改變之吸收劑，例如是，氟化鋼（NaF )。一個溫声烟，去里度5周即式套（加熱器）57被配置在該吸的周圍之上，用以調節該吸收E 56的溫度。在該主缓衝槽64内的壓力由一個被配置在該主緩衝上的壓力規65持續地量測。此-量測結果被傳遞到 δ玄控制構件3 9，贫i^也丨4JL /0» n r、控制構件39被連接到該電流源38。依據所傳輸的量測結果’該控制構件39藉由切換該電流源 38的開與關來控制供給到該氣密式電解電池&的電流。因此，當在該主緩衝槽64内之壓力已下降到某一壓力時 m源38被開啟’並且開始產生氟氣。當在該主煖衝槽64内之壓力已經增加到某一壓力時，該電流源⑽被關閉’並且停止產生氟氣。此使電解被停止而不用設定在省陽極至34與該陰極室36之間該氣密式電解電池犯之内的熔融鹽類之液面差。在該主緩衝槽64内之壓力被設定到，例如，從大氣壓力到較大氣壓力大〇. 18 Mpa。 —個第二導管72被連接到該陰極室36以將該氣體副產物抽出。此一第二導管7 2以可脫離的方式被連接到，】疋座半導體製造工廉的該排氣系統（抽吸裝置） 78之—導管。一個第二流率控制閥74以及—個解毒器（ detoXlfier) 76被配置在該第二導管72中。於該陰極室％ 20 200400921 產生的該氣體副產物被強力地從該陰極官 - 广/ 至36中精由該排氧糸統78的該第二導管72，並被移動通過該解毒器π且祐:傳輸到該排氣系統78中。如上述所注意到的，於電解的過程期間，該陽極室料與該陰極室36之間的壓力平衡無論如何會被擾動，因為這彳2結果使得該氣密式電解電池32中的液面水位之改變很容易發生。-般而言，在-氣體切換式操作（咖_ switching operati〇n)(例如是：該氣密式電解電池犯氣的清除，或者是在起始氟化氫的供給結束之後的氮塌乱清除過程）之後，在該氣密式電解電池32中的液面水位也容易立即的改變。這些液面的變化會對該氟氣產生器的安全性與可靠度產生不利的影響。 ° 然而，在圖1中所說明之該氟氣產生器的情況中，該陽極室34中的該氣相區域的壓力由一個第一壓力規連續地量測’而該陰極t 36巾的該氣相區域的壓力由一個第一壓力規48連續地量測。這些量測的結杲被傳輪到第一控制構件55與第二控制構件75，該第一控制構件Η與籲該第二控制構件乃被個別地連接到該第一流率控制閥54 與該第二流率控制閥74。依據所傳輸的量測結果，該第— 控制構件55與該第二控制構件75調整該第一流率控制閥 54與5玄第二流率控制閥74的孔徑，用以將該陽極室34中的該氣相區域的壓力與該陰極室36中的該氣相區域的壓力個別地維持在第一與第二設定值，該等設定值彼此大致相等。 21 400921 為在。亥陽極室34與該陰極室36中的壓力之每一個被持、貝地與獨立地量測與控制，在該陽極室料與該陰極室36中的熔融鹽類之液面的均勻狀態被維持。換言之， …構防止5亥電解電池3 2在下列變化中之不利的影響 •產生鼠氣的狀態、該第一導管52與該第二導管Μ内之主兄°玄1縮機62與半導體製造廠之排氣系統78的運轉 :况以及其它的情況。此一情況使其可以避免對昂貴的電極產生損害，例如陽極效應，並且可以安全地且不會在電解中犬然中止的情況下實施此一程序。此外，不需要常吊:隹修’因為熔融鹽類在連接到該第-導f 52與該第二導g 72的入口處由於固化所引起的阻塞不會發生。對於该陽極室34中之氣相區域的第一設定值盘該^ 極室36巾之氣相區域的第二設定值係較佳地域力相 82"町並且更佳為屬力達到77〇 T〇rr。為了穩定在該陽極室34與該陰極室36中的壓力，該第—流率控制… β玄弟二流率控制閥74_孔徑必需以-種高速響應的方式被持續地調整。此-種考量使得利用—㈣於該第一流率控制間54與該第二流率控制間74的壓電間（ρ )較佳。 +、再度參照圖卜—個起始材料導管82被配置在該電解電池32的陰極室36中，以將氟化氫氣體（可消耗的起始材料）供給到該熔融鹽類中.品頬中，此—起始材料導管82被配置來沉浸到該熔融鹽類之内。一個氣化氯Μ以及一個礼氣源94以可脫離的方式透過該等導而被連接:】 22 °亥起始材料導管82。中，用於切：：96被配置在用於該氮氣源' 94的該導管93 換間==於Γ啟與關閉狀態之間的導管93。該切在” Λ 3°的操作期間-直開啟，而氮氣 Μ的炫融鹽類之内。直被供給到該電解電池的範圍內，廿流率被設定在〇.2到騎min 為1到5〇 L/'且較佳為2到I〇 L/min的範圍，該氟化氫則融鹽該氟化氫幾乎完全不溶解於該炼排出内’並且通過在該陰極側的上之該溶融鹽類且被 -:切換間86被配置在用於該氟化氫源Μ的該導管切換\二=齡料開啟與關閉狀態之間的導管.該與關連接到該切換閥86之控制構件87來控制開啟 ^才°冑解過程期間’被供給該陽極42與該陰極44 間的電流由該電流整合器4Q戶斤整合，且此—數值輪到該控制構件8 7。钬媸、士 A ± 傳測的數值，該二知作*亥切換閥8 6，用以調節供、=該溶融鹽類之内的氣化氣氣體（在氮氣中混合的氟化風）。用於該控制構件87的設定數值被建立，例如，將在該炼融鹽類之内的氟化氫之濃度維持在娜到41%的範圍。依據下述理論，供給到該電解電池32之I化氫氣體的：給由供給的電流之整合而受到控制。因此，根據法拉也疋律纟甩解所產生的氟氣的總量係直接正比於電力的 23 200400921 200400921 疋律不言電解的條件（溫度、濃度1 with a mixture of chlorine fluoride (HF) (KF / 2HF), or hydrogen fluoride and Fleming salts (Fremy, s salt). The airtight electrolytic cell 32 is divided into an anode chamber 34 and a cathode chamber 36 by a partition sheet 35, and the partition sheet 35 extends from the top into the molten salt. A carbonaceous electrode (anode) 42 is immersed in the molten salt in the anodes to 34, and at the same time, a nickel-based electrode (cathode) 轲 is immersed in the molten salt in the cathode chamber 36. Attached to the air-tight electrolytic cell 32 is a current source 38 and a current integrator 40, 18, among which the current source 38 w,,; + Λ ^ is stored between the anode 42 and the cathode 44 Current while the current integrator 4. Integrate the supplied current. During the electrolysis process, the gas is heated and maintained: 8 = 2 = electrolysis of hydrogen fluoride in the decomposition bath results in a wall: 90 ° C. In the gas phase region of the electric pole chamber 34, the main component of the gas product is fluorine gas (F2), and in the gas phase region of the tritium cathode chamber 36, a by-product of raw milk is generated, and the gas The main component of the by-product is radon. Hydrogen fluoride is mixed (for example: 5%) between the gas product and the gas by-product based on the vapor pressure contribution of the nitrogen fluoride gas in the molten salt. A first pressure gauge M is disposed on the anode chamber 34, and a second pressure gauge M is disposed on the cathode chamber 36 to continuously measure the pressure of the individual gas phase regions. A first conduit 52 is connected to the anode chamber 34 for retrieving gas products and transmitting the gas products to the flow management section 22 and the gas generation section 26 of the gas supply system 20. From upstream It is successively arranged in the "-duct 52": a "flow-rate control valve", an absorption E 56 '-a minibuffer tank 58, a compressor (suction device) 62, and One main buffer slot 64. The gas product generated in the anode chamber 34 is strongly extracted from the anode chamber 34 by the suction of the compressor (suction device) 62 through the first duct 52, and is stored in the main buffer Slot 64. The symbol 66 in the figure represents a line filter. As mentioned above, the idea is that hydrogen fluoride will be mixed in the gas product at several percentages (for example: 5%). When the gas product passes through the absorption 29 200400921 min 56, the fluorinated gas is reduced in cost to kick this ^^ Therefore, the absorption £ 56 should be accommodated and collected> and the gas absorption / μ _ absorbent capacity of the dagger . According to treatment and pressure loss ...: The absorbent should include: small pellets filled in the absorbent £ 56. The absorbent may include an absorbent having a yield capacity p, s, 电, 、, 电,, and 电 as the temperature function changes, for example, fluorinated steel (NaF). A warm-sounding smoke, which is 5 weeks in length, is provided with a sleeve (heater) 57 on the periphery of the suction to adjust the temperature of the absorption E56. The pressure in the main buffer groove 64 is continuously measured by a pressure gauge 65 arranged on the main buffer. The measurement result is transmitted to the delta control member 39, and the control member 39 is connected to the current source 38. According to the transmitted measurement result ', the control member 39 controls the current supplied to the air-tight electrolytic cell & by switching the current source 38 on and off. Therefore, when the pressure in the main buffer tank 64 has dropped to a certain pressure, the m source 38 is turned on 'and begins to generate fluorine gas. When the pressure in the main warming bath 64 has increased to a certain pressure, the current source ⑽ is turned off 'and the generation of fluorine gas is stopped. This causes the electrolysis to be stopped without the liquid level difference of the molten salt set in the airtight electrolytic cell between the anode anode 34 and the cathode chamber 36. 18 Mpa。 The pressure in the main buffer tank 64 is set to, for example, larger from atmospheric pressure to a larger air pressure of 0.18 Mpa. A second conduit 72 is connected to the cathode chamber 36 to extract the gas by-products. This second duct 72 is detachably connected to the exhaust system (suction device) 78 of the semiconductor manufacturing industry, the duct. A second flow rate control valve 74 and a detoxlfer 76 are disposed in the second conduit 72. The gas by-product produced in the cathode chamber% 20 200400921 is forcibly refined from the cathode tube-36/36 to the second conduit 72 of the oxygen depletion system 78 and moved through the detoxifier π and You: Transfer to the exhaust system 78. As noted above, during the process of electrolysis, the pressure balance between the anode chamber material and the cathode chamber 36 will be disturbed anyway, because this 彳 2 results in the liquid level in the air-tight electrolytic cell 32 Changes in water levels can easily occur. -In general, in-gas switching operation (such as: gas removal of the gas-tight electrolytic cell, or the nitrogen collapse removal process after the end of the supply of hydrogen fluoride) After that, the liquid surface water level in the air-tight electrolytic cell 32 is also easily changed immediately. These changes in liquid level can adversely affect the safety and reliability of the fluorine gas generator. ° However, in the case of the fluorine gas generator illustrated in FIG. 1, the pressure of the gas phase region in the anode chamber 34 is continuously measured by a first pressure gauge, and the cathode t 36 towel of the The pressure in the gas phase region is continuously measured by a first pressure gauge 48. These measured results are transferred to the first control member 55 and the second control member 75, and the first control member and the second control member are individually connected to the first flow rate control valve 54 and the第二流率控制阀 74。 The second flow rate control valve 74. According to the transmitted measurement results, the first control member 55 and the second control member 75 adjust the apertures of the first flow rate control valve 54 and the second flow rate control valve 74, and are used for The pressure in the gas phase region and the pressure in the gas phase region in the cathode chamber 36 are individually maintained at first and second set values, and the set values are substantially equal to each other. 21 400921 is in. Each of the pressure in the anode chamber 34 and the cathode chamber 36 is held, measured and controlled independently, and the uniform state of the liquid level of the molten salt in the anode chamber material and the cathode chamber 36 is controlled. maintain. In other words,… constructs the 5 Hai electrolytic battery 3 2 from adverse effects in the following changes: • The state of rat gas, the main brothers in the first duct 52 and the second duct M, and the semiconductor manufacturing 62 and semiconductor manufacturing. The operation of the plant's exhaust system 78: condition and other conditions. This situation makes it possible to avoid damage to expensive electrodes, such as the anodic effect, and to carry out this procedure safely and without interruption during electrolysis. In addition, there is no need to hang: repairing because the molten salt does not cause blockage due to solidification at the entrances connected to the first-conductor f 52 and the second-conductor g 72. For the first setting value of the gas phase region in the anode chamber 34, the second setting value of the gas phase region in the electrode chamber 36 is preferably the regional force phase 82 " and more preferably the force reaches 77 ° T. 〇rr. In order to stabilize the pressure in the anode chamber 34 and the cathode chamber 36, the first flow rate control ... The β-secondary flow rate control valve 74_aperture must be continuously adjusted in a high-speed response manner. This consideration makes it better to use the piezoelectric space (ρ) between the first flow rate control room 54 and the second flow rate control room 74. +, Referring again to FIG. A starting material conduit 82 is arranged in the cathode chamber 36 of the electrolytic cell 32 to supply hydrogen fluoride gas (consumable starting material) to the molten salt. This—the starting material conduit 82 is configured to be immersed into the molten salt. A vaporized chlorine M and a courtesy gas source 94 are connected in a detachable manner through these channels:] 22 ° starting material conduit 82. In, cut :: 96 is arranged in the conduit 93 for the nitrogen source '94. Interchange == the conduit 93 between Γ opened and closed. The cutting is performed during the operation of "Λ 3 °-straight open, and the nitrogen M is melted into the salt. It is supplied to the range of the electrolytic cell, and the flow rate is set to 0.2 to 1 min. To 50L / 'and preferably 2 to 10L / min, the hydrogen fluoride is molten salt, the hydrogen fluoride is almost completely insoluble in the refining discharge', and the molten salt is passed on the cathode side And the switch-over room 86 is configured for the switchover of the conduit for the hydrogen fluoride source M. The conduit between the open and closed states of the aged material. The connection is controlled by a control member 87 connected to the switch valve 86 to open. During the disintegration process, the current supplied between the anode 42 and the cathode 44 is integrated by the current integrator 4Q, and this—the value turns to the control member 87. 钬媸, ± A ± pass test The value of the two is known as the * Hai switch valve 86, which is used to adjust the gas supply gas (fluorinated wind mixed in nitrogen) within the molten salt. It is used for the setting of the control member 87. The value is established, for example, to maintain the concentration of hydrogen fluoride in the smelting salts in the range of Na to 41%. According to the following theory, the supply of hydrogen hydride gas to the electrolytic cell 32 is controlled by the integration of the supplied current. Therefore, according to Faraday's law, the total amount of fluorine gas generated is directly proportional to the deflection. 23 200400921 200400921 The conditions of electrolysis (temperature, concentration)

JfG 緦重類）。佑Η 乂 u …入’電極的種 ,二則的效率關係式，使用方程4(1)… t的貫施例之電解電Α 3 。响。 /生王B7軋矾戍子可以被決定 z = 6.8X , (1) 其中， z =氣氣產生流率（cc/min)。 x -電量（此—情況下的電解電流值（幻）。在該熔融鹽類之内的起始氟化氫之濃卢，#|| e B 4 g 乳< /辰度例如是達到餐 γ。纟’起始氟化氫的供給在該炼融鹽類之内的說化氫之濃度從其起始6“1%濃度下降之後並且到達— 下限（例如39%)之前被較發生。當該氟化氫的濃度ς 到最低濃度下限以下時’該炫融鹽類之溶點的增加在最糟的知況下會導致該熔融鹽類的固化，並使其不可能實施電解。當該I化氫的濃度超過起始濃度時，其在該炫融鹽Ζ 令產生的氟化氫之高蒸汽麼亦將提高混合於該氟氣中的氟化氫之濃I。上述情況在該吸㈣56 4產生一個高負栽修在該吸附劑（例如是：氟化自（NaF))上，該吸附劑以可吸附的方式補獲該氟化氯。因此將該說化氯的濃度維持在上述範圍内，例如是：39%到41%，是必需的。方程式（2 )顯不氟氣生產與氟化氫消耗之間的關係。此處，產生！莫爾的氟氣需要有2莫爾的I化氫。 (2Z + 0.05Z + 0.05Z) t/1000 = T ( 2) 其中，JfG (important class). ΗΗ 乂 u… the type of the electrode, the efficiency equation of the two, using the electrolytic electrode A 3 of the embodiment of Equation 4 (1) ... t. ring . / Shengwang B7 Alum dumplings can be determined z = 6.8X, (1) where z = gas flow rate (cc / min). x-the amount of electricity (in this case-the value of the electrolytic current (magic). In the molten salt, the concentration of the initial hydrogen fluoride, # || e B 4 g milk < The supply of starting hydrogen fluoride is said to occur after the concentration of hydrogen fluoride within the smelting salts is reduced from its initial 6 "1% concentration and before reaching the lower limit (eg 39%). When the hydrogen fluoride's When the concentration is below the lower limit of the minimum concentration, the increase of the melting point of the dazzling molten salt will lead to the solidification of the molten salt and make it impossible to perform electrolysis under the worst known conditions. When the initial concentration is exceeded, the high vapor content of the hydrogen fluoride produced by the molten salt Z will also increase the concentration of hydrogen fluoride I mixed in the fluorine gas. The above situation produces a high load in the suction 56 4 The adsorbent (for example: fluorinated from (NaF)), the adsorbent replenishes the chlorine fluoride. Therefore, the concentration of the chlorine chloride is maintained within the above range, for example: 39% It is necessary to reach 41%. Equation (2) shows the relationship between the production of fluorine gas and the consumption of hydrogen fluoride. Here, Moore's fluorine gas needs 2 Moore's hydrogen hydride. (2Z + 0.05Z + 0.05Z) t / 1000 = T (2) where,

24 200400921 氫流率（cc/mi m 1莫爾的氣氣所需要的氣化被裝載於莫爾的氟氣中之氟化氫流莫爾的氫氣中之氟化氫流第一項 0.052：率(cc/min)。第二項〇.〇5“被裝載於率(cc/min) ° t =生產時間（min)。 T =氟化氫消耗量（L )。方程式（3 )依播古妒斗伙據方矛主式（1 )將方24 200400921 Hydrogen flow rate (cc / mi m 1 Moore gas required to vaporize the hydrogen fluoride flow contained in Moore's fluorine gas The hydrogen fluoride flow in Moore's hydrogen gas The first term 0.052: rate (cc / min). The second term 0.05 is the loading rate (cc / min) ° t = production time (min). T = hydrogen fluoride consumption (L). Equation (3) Spear Master (1) General

以6.8X代換所獲得。矛式（2)中的Z 0.01428X X t = τ ^ (3) 其中， x =電量（A)。 1生產時間（min )。 T 一氟化氫消耗量（L )。可〉肖耗的氟化惫的暑;^ 3丨λ 鹽類之内0& , 電解電池32的熔融化氣：：開始電解之前在該溶融鹽類之内的敦化虱所給定之濃度為41% 的鼠介备从曰在該電解電池32中惫電、、也/、中c為熔融鹽類的總量。當該電解池32被使用在氟化氫濃度於39% :分，。之間的範圍睹 μ熔融鹽類中的氟化氫之濃产、關係於方"肖耗量之間的轾式（4 )中被給定。然後，可消耗最大耗之乱化虱的里由方程式（5 )中被給定。 =0.39 (0-41C-HFc) / (C-HFc) =0.39 ( 〇 25 200400921Get it at 6.8X. Z 0.01428X X t in the spear formula (2) = τ ^ (3) where x = electric quantity (A). 1 production time (min). T hydrogen fluoride consumption (L). May> Xiao consumption of fluorinated exhausted summer; ^ 3 丨 λ within the salt 0 &, the melting gas of the electrolytic cell 32: The concentration given by the Dunhua louse in the molten salt before starting electrolysis is 41 The percentage of rats that are exhausted in the electrolytic cell 32 is that c is the total amount of molten salts. When the electrolytic cell 32 is used at a hydrogen fluoride concentration of 39%: min. The range between these is given by the concentration of hydrogen fluoride in μ molten salts, which is given by formula (4), which is related to the consumption of Xiao. Then, the maximum consumable lice that can be consumed is given by equation (5). = 0.39 (0-41C-HFc) / (C-HFc) = 0.39 (〇 25 200400921

HFc = 0.033C 其中在方程式（4)與方程式（5) _ C =該熔融鹽類的重量。 HFc =氟化氫的消耗量。 (3)中的T以〇 (6) (7)HFc = 0.033C where Eq. (4) and Eq. (5) _C = the weight of the molten salt. HFc = consumption of hydrogen fluoride. T in (3) is 0 (6) (7)

方程式（6 )與方程式（7 )由方程式在方程式（5)巾的HFc取代的方式所獲得 °·〇1428Χ X t = 0.033C X X t = 2.3C 其中在方程式（6)與方程式（？）中， x =電量（A)。 t =生產時間（min)。 C =該熔融鹽類的重量。因此對於齓化虱/辰度於3 9 %與41 %的範圍内情況下，該電量X與氟化氫生產時間t之間的關係可以被決定，假如起始被引入該電解電池32内的熔融鹽類（KF/2HF) 之重量C為已知的情況時。在目前的情況中，氟化氫氣體的進給時機（低於濃度範圍的下限）可以藉由沿著時間軸的電罝之積分所給得到的數值而被確定，並且結果電量X 不需要被固定。本文上述的此一發明的實施例之益處現在將被考量。曰本開平（Laid Open )專利申請（pct )號Hei 9_ 505853 (下文以853公開號表示）揭示一種氟電池，該氣電池包含有：一個控制感測器裝置與一個電流供給裝置，該控制感測器裝置偵測在該電解電池中的電解液位平’而 26 200400921 °亥電抓供給裝置響應來自該控制感測器裝置的訊號，來啟動或知止電流的供給以響應此一訊號。在此—種情況中，氟氣產生一直持續直到液面位準下降到達一個預設的位置 ’在該預設的位置處則發出一個訊號。因為響應此一訊號 ’該電解控制裝置停止電流供應到該電池，電解被停止並且電解液液面位準的下降也同樣停止。Equation (6) and equation (7) are obtained by replacing the equation with the HFC of equation (5). ° · 1428 × X t = 0.033CXX t = 2.3C where in equation (6) and equation (?), x = power (A). t = production time (min). C = weight of the molten salt. Therefore, for the case of pupae lice / cages in the range of 39% and 41%, the relationship between the amount of electricity X and the production time t of hydrogen fluoride can be determined. If the molten salt is initially introduced into the electrolytic cell 32 When the weight C of the class (KF / 2HF) is known. In the present case, the timing of feeding the hydrogen fluoride gas (below the lower limit of the concentration range) can be determined by the value given by the integration of the electric energy along the time axis, and as a result, the electric quantity X need not be fixed. The benefits of the embodiments of this invention described above will now be considered. Laid Open patent application (pct) No. Hei 9_505853 (hereinafter referred to as 853 publication number) discloses a fluorine battery, the gas battery includes: a control sensor device and a current supply device, the control sensor The detector device detects the level of the electrolyte in the electrolytic cell, and in response to the signal from the control sensor device, the power supply device responds to this signal by responding to the signal from the control sensor device. In this case, the generation of fluorine gas is continued until the liquid level drops to a preset position, and a signal is issued at the preset position. Because in response to this signal, the electrolysis control device stops supplying current to the battery, the electrolysis is stopped and the lowering of the electrolyte level also stops.

綜上所述揭示於此一說明書中的技術謹慎地運用液面的改及，來實施電流〇N/〇FF的控制，並且不用考量抑制此一變化。然而，液面位準的變化在該電解作用中必需被減少’用於持續地產生氟氣並同時維持一種穩定的狀態。該853專利亦清楚地看出在電解電池中的陽極室是作為:個氣儲槽（fluorine reserv〇ir)的功能。然而，由於付合需求的氟氣生產之困難度，該等用於在一個可實施的位準之半導體製程的氟氣產生器需要一部壓縮機與某一尺寸的容器。揭示於該專利討論中的技術不能夠容忍此種外在環境之改變。因此，對應於該853專利之被提供商用的氟氣產生系鲁統被提供有一種轟鳴式的壓縮機（bell〇ws_type compressor)與容量數升的容器。此一種系統將就氣透過一個0N/0FF切換閥的動作間歇地儲存在其缓衝槽之中。此種方法的使用使該未被中斷的氟氣之生產能夠不會中斷氟氣的生產。然而，當氣體能夠被穩定的在該此—情況中產生時，實際的經驗仍然顯示：於此一種所討論的長期生產情況期間，發生下述問題。 27 200400921 由該氟氣所承載的該無雜質的熔融鹽類之霧氣渗透入該導管或是在該壓縮機與該電解電池之間的容器。因為注種霧氣具有溶點大約80t:左右，其在該導管之間顯現出— 種固恶。當此種霧氣累積時，其將引起如下的問題：（1 )該導管的阻塞’以及⑴對該_FF閥的閥座造成j 壞。、該先前的問題導致電解動作立即的中止，並且需要。 -種操作讀去該鹽類阻塞該導f。因為易反應的二氣也將出現在該導管中，此種移除動作是相當危險而且需要極大的勇氣。後面的問題再度需要當在閥體處的浅漏時停止電解動作。此外’該⑽聊之頻繁的重複動作引起過早地磨損。此外’因為該討論中的控制方法不能避免在該陽極室中的液面位準某一程度的變化，介於該液體與該電極表面之間的接觸面積也持續地經歷變化。於電解期間在目前效率下所導致的變化使要維持氟氣生產量的穩定十分困難。於此處出現的另一個問題為：該陽極效應可能需要更換該電極（典型上，碳被用於該陽極）。當如揭示於該專利中的氟氣產量之控制藉由0N/0FF切換一個電源供應器以各應e亥控制感應益（c〇ntr〇i sens〇r )的方式實施時，在被容納之圍繞的環境（在此討論的情況中為連接到—個壓縮機）中也不會改變。並且，最後的方析中，於該電解電池處使用一個壓縮機以伺服半導體製程之情況下是需要的。另一方面，氟氣生產不受到來自該電解電池的下游側之In summary, the technology disclosed in this specification carefully uses the modification of the liquid level to implement the control of the current ON / OFF, and does not need to consider suppressing this change. However, changes in the level of the liquid must be reduced in this electrolysis' to continuously generate fluorine gas while maintaining a stable state. The 853 patent also clearly sees that the anode compartment in an electrolytic cell functions as a gas reservoir. However, due to the difficulty of meeting the demand for fluorine gas production, such fluorine gas generators for semiconductor processes at a practical level require a compressor and a container of a certain size. The technology disclosed in this patent discussion cannot tolerate such changes in the external environment. Therefore, the supplied fluorine gas generating system corresponding to the 853 patent is provided with a bellows type compressor and a container with a capacity of several liters. This system intermittently stores gas in its buffer tank through the action of a 0N / 0FF switching valve. The use of this method enables the production of the uninterrupted fluorine gas without interrupting the production of fluorine gas. However, when gas can be stably generated in this case, practical experience still shows that during the long-term production situation in question, the following problems occur. 27 200400921 The mist of the impurity-free molten salt carried by the fluorine gas penetrates into the duct or the container between the compressor and the electrolytic cell. Because the injection mist has a melting point of about 80t :, it appears between the ducts-a kind of solid evil. When this kind of mist accumulates, it will cause the following problems: (1) Blockage of the duct 'and ⑴ cause damage to the valve seat of the _FF valve. This previous problem caused an immediate suspension of the electrolysis action and was needed. -An operation reads that the salt blocks the lead f. Because reactive gas will also be present in the catheter, this removal action is quite dangerous and requires great courage. The latter problem needs to stop the electrolysis action when there is a shallow leak in the valve body. In addition, the frequent repetitive actions of the chatter caused premature wear. In addition, 'because the control method under discussion cannot avoid a certain degree of change in the level of the liquid level in the anode chamber, the contact area between the liquid and the electrode surface also continuously undergoes changes. The change in current efficiency during the electrolysis period makes it difficult to maintain a stable production of fluorine gas. Another problem that arises here is that the anode effect may require the electrode to be replaced (typically, carbon is used for the anode). When the control of the fluorine gas production as disclosed in the patent is implemented by switching a power supply to 0N / 0FF in a way that each responds to control the gain (c0ntr〇i sens〇r), it is contained in The surrounding environment (connected to a compressor in the case discussed here) will also not change. And, in the final analysis, it is necessary to use a compressor at the electrolytic cell to servo the semiconductor process. On the other hand, fluorine gas production is not affected by the downstream side of the electrolytic cell.

28 200400921 衫響疋必要的。端視在該8 5 3直制士隹茨專利中之控制方法的展望並不適合用於半導體製程的祠服，並因此是不實際的。本發明上述之實施例的一個重要的特點為其並不受到在5亥如置電池（P Q S t - C e 1〗、4红rf» h 、PQSt Gell) W中的改變之影響，並且能。持續地並穩定地產生氟氣。此—氟氣供給剌於半導體製程的伺1，亦即，必要假設是使用及裝置（例如是_個壓縮機）。 ,連接到該壓縮機下游處的緩衝槽之㈣規被連接到該電流源。當該壓力下陪_到！—叙& + —、卜降到*數值時，該電源被開啟並且氟氣被產生。當該壓力上井釗I ^ . 、 i刀上开到某一數值時，該電源被關閉 0此·一方法的使用使得傳丨卜雷 i 文付1〒止冤解動作而不用如該853專利中之不同液面位準的精心製作成為可能。該853專利教示：為了安全之故，較佳為在陰極側出口處的壓力一直處於大氣壓力（或者是出口處的壓力稍大於大氣壓力）之情況下來操作。然而，在—實際的半導體工場中維持上述情況幾乎不可能，由於發生在該陰極侧的導管中極大的壓力變化。此外’物專利僅聚焦在該陽極室中的崖力變化，並且將其建立在該前提之上，該前提為：在該陰極室中的壓力一直是大氣壓力。由依據本發明的上述實施例之獨立的流率控制器所維持的壓力使在該電解電池的兩個電極室中之壓力—直被維持衡定 '然而’實際上，該液面位準無法由該壓力決定，並且針對此-理由，為了增進安全性之故，一個液面位準感測器以一種較佳的形式被置入在該陽極與陰極側之中， 29 200400921 並且較仏為在該陰極側。尸該起始的無水的氟化氫（AHF)係通常為氣體，並且由氣泡方式被供給到該電解電池的熔融鹽類（刚之内。請顯示一種非常快速的吸收到類之内的速率，因此，當該AHF以一種低流率的方式被供給時，該陰極室可以立即地呈現出負壓狀態。當上述情況發生時，該熔融鹽類在該AHF進給導管内上升，並且在最糟的情況時將結束固化且使持續供給成為可能。因此，該 AHF進給流率係相當地快速，但是對可以實際使用的該謝 | 進給流率有限制。因此，在本發明上述的實施例中，在提升整體流率為目的之AHF進給期間與該AHF進給期間之間隔期間，該 AHF被混合到氮氣中。目μ氣幾乎是完全不可溶於熔融鹽類中’其通過在該陰極側上的熔融鹽類並且被排出。進入到s亥陰極室之氮氣流率一直被維持，不管電解動作是否實際在進行中。上述情況導致於電解期間在該陰極側所產生的氫氣的稀釋，並且使維持遠離***界限的情況成為可鲁能’即使當氟氣由於在液面變化的突然與不可預期的改變下被導入該陰極側時。該氮氣流率以該電解電池之尺寸大小為基礎的情況下被最佳化地調節。該敦氣產生器3〇以可分離的方式被併入在上述所描述的實施例之半導體製程系統中，但是該氟氣產生器30也可以被永久地被裝置^ 此一系統中。此外’被配置在該半導體製造工廠中的若干兀件可以被使用來將其中數種元件分配給該氧氣產生器 30 200400921 ，例如：該壓縮機62、該主緩衝槽64、該解毒器76等等。該氟氣可以交替地被供給到該流量管理區段22或該氣體產生區段26，抑或是可以與其它種製程氣體分離之方式被直接供給到該製程反應室12。該氣體產生區段2 6也可以被構型以產生其它的氟系統製程氣體，而不是鹵素與幽素間的氟化合物。28 200400921 T-shirts are loud and necessary. The outlook of the control method in the 8 5 3 direct-control patent is not suitable for use in semiconductor service, and is therefore impractical. An important feature of the above-mentioned embodiment of the present invention is that it is not affected by the changes in the battery 50 (P Q S t-C e 1), 4 red rf »h, PQSt Gell, and can be. Continuously and steadily produces fluorine gas. This—fluorine gas supply is used in semiconductor manufacturing processes, that is, it is necessary to assume the use and equipment (for example, a compressor). A gauge connected to a buffer tank downstream of the compressor is connected to the current source. When the pressure accompanies _ to! —S & + — When the value is reduced to *, the power is turned on and fluorine gas is generated. When the pressure on the blade I ^., I is turned on to a certain value, the power supply is turned off. The use of this method makes the transmission of Brei i 1 to stop the action of injustice without using the 853 patent. The elaboration of different liquid levels becomes possible. The 853 patent teaches that for safety reasons, it is preferred to operate with the pressure at the cathode side outlet always at atmospheric pressure (or the pressure at the outlet is slightly greater than atmospheric pressure). However, it is almost impossible to maintain the above situation in an actual semiconductor factory due to the extreme pressure change occurring in the cathode-side duct. In addition, the patent only focuses on the change of cliff force in the anode chamber, and establishes it on the premise that the pressure in the cathode chamber is always atmospheric pressure. The pressure maintained by the independent flow rate controller according to the above-mentioned embodiment of the present invention allows the pressure in the two electrode chambers of the electrolytic cell to be maintained constant. However, in fact, the liquid level It is determined by this pressure, and for this reason, for the sake of improving safety, a liquid level sensor is placed in the anode and cathode sides in a better form, 29 200400921 and more On the cathode side. The starting anhydrous hydrogen fluoride (AHF) is usually a gas, and is supplied to the molten salt of the electrolytic cell by a bubble method (inside. Please show a very fast rate of absorption into the category, so When the AHF is supplied in a low flow rate manner, the cathode chamber can immediately assume a negative pressure state. When the above situation occurs, the molten salt rises in the AHF feed conduit, and at the worst In this case, the curing will be completed and continuous supply will be possible. Therefore, the AHF feed flow rate is quite fast, but there is a limit to the actual feed rate. Therefore, in the above-mentioned implementation of the present invention, In the example, during the interval between the AHF feed period and the AHF feed period for the purpose of increasing the overall flow rate, the AHF is mixed into nitrogen. The mesh μ gas is almost completely insoluble in molten salts. The molten salt on the cathode side is discharged. The nitrogen flow rate into the cathode chamber is always maintained, regardless of whether or not the electrolysis operation is actually in progress. The dilution of the hydrogen gas generated on the pole side makes it possible to maintain the situation away from the explosion limit, even when fluorine gas is introduced into the cathode side due to sudden and unexpected changes in liquid level. The nitrogen flow rate is The size of the electrolytic cell is optimally adjusted based on the size. The gas generator 30 is detachably incorporated in the semiconductor process system of the embodiment described above, but the fluorine gas The generator 30 can also be permanently installed in this system. In addition, several components configured in the semiconductor manufacturing plant can be used to assign several of these components to the oxygen generator 30 200400921, for example: The compressor 62, the main buffer tank 64, the detoxifier 76, etc. The fluorine gas can be alternately supplied to the flow management section 22 or the gas generating section 26, or can be separated from other process gases The method is directly supplied to the process reaction chamber 12. The gas generating section 26 can also be configured to generate other fluorine system process gases, instead of between halogen and peptone. Fluorocarbon.

然而’於本發明内之概念之技術範疇内的數種修正改變可以由此一領域中熟此技藝之人士所想出，應被瞭解到的是：這些修正與改變也落入本發明的範躊内。如上述所描述的，本發明提供一種氟氣產生器，該氟氣產生器能夠非常安全並高可㈣㈣，即便是於長_ 【圖式簡單說明】 (一）圖式部分明一個半導體製程系 —個實施例之一個氟圖1為一個概略圖式，其描述說However, 'there are several correction changes within the technical scope of the concept in the present invention that can be conceived by those skilled in the art in this field, and it should be understood that these corrections and changes also fall into the scope of the present invention踌内. As described above, the present invention provides a fluorine gas generator, which can be very safe and highly reliable, even if it is long _ [Simplified description of the drawing] (a) The part of the drawing shows a semiconductor process system One of the embodiments of FIG. 1 is a schematic diagram, which describes

統，該半導體製程系統併入本發明的氣產生器。 v 1叫m令固珥，其描述嘮M / 統之一個修St I ^ 次月一個半導體製 l改貫例，该修改實例結進給系統來—起使用。。兒明於圖丨中之圖3為一個概略圖式，1 氣產生器。說明-個先前技藝 31 200400921 (二）元件代表符號 10X半導體製程裝置 10半導體製程裝置 12製程反應室 1 3遠端電漿室 14電極（裝設平臺（支撐構件）） 1 5 RF電源 1 6電極 17線圈天線 18排氣系統 2 0氣體供應糸統 22流量管理區段 24氣體儲存區段 26氣體產生區段 30氟氣產生器 3 2電解電池 33加熱器 3 4陽極室 3 5隔離薄片 36陰極室 3 8電流源 39控制構件 40電流整合器 4 2陽極 32 200400921 44陰極 46第一壓力規 48第二壓力規 52第一導管 54第一流率控制閥 55第一控制構件 5 6吸收匣 57溫度調節式套（加熱器） 58迷你緩衝槽 62壓縮機（抽吸裝置） 64主缓衝槽 65壓力規 6 6管線過濾器 72第二導管 74第二流率控制閥 75第二控制構件 76解毒器 7 8排氣系統 82起始材料導管 83導管 84氟化氫源 8 6切換閥 87控制構件 93導管 33 200400921 94氮氣源 96切換間 11 2電解電池 114陽極 11 6中級的容器 11 8壓縮機 120導管 121氫氣導管 122切換閥 124第二缓衝槽System, the semiconductor process system is incorporated into the gas generator of the present invention. v 1 is called m Linggu, which describes 唠 M / system of a repair St I ^ a semiconductor system next month l a modified example, this modified example is used in the feed system. . Children are shown in Figure 丨 Figure 3 is a schematic diagram, 1 gas generator. Explanation-a previous technique 31 200400921 (II) Symbols for component 10X semiconductor process device 10 semiconductor process device 12 process reaction chamber 1 3 remote plasma chamber 14 electrodes (installation platform (supporting member)) 1 5 RF power supply 1 6 electrodes 17 coil antenna 18 exhaust system 2 0 gas supply system 22 flow management section 24 gas storage section 26 gas generation section 30 fluorine gas generator 3 2 electrolytic cell 33 heater 3 4 anode chamber 3 5 isolation sheet 36 cathode Chamber 3 8 current source 39 control member 40 current integrator 4 2 anode 32 200400921 44 cathode 46 first pressure gauge 48 second pressure gauge 52 first conduit 54 first flow rate control valve 55 first control member 5 6 absorption box 57 temperature Adjustable sleeve (heater) 58 Mini buffer tank 62 Compressor (suction device) 64 Main buffer tank 65 Pressure gauge 6 6 Line filter 72 Second conduit 74 Second flow rate control valve 75 Second control member 76 Detoxification 7 8 exhaust system 82 starting material conduit 83 conduit 84 hydrogen fluoride source 8 6 switching valve 87 control member 93 conduit 33 200400921 94 nitrogen source 96 switching room 11 2 electrolytic battery 114 anode 11 6 intermediate container 11 8 compression Hydrogen conduit 120 conduit 121 valve 122 to switch the second buffer tank 124

Claims

200400921 拾、申請專利範圍： 1.一種用於產生氟氣之裳置’其特徵在於：個電解浴中之氣個電解電池’該電解電池完成在化氫的電解，該電解浴包括含有氟化氫线㈣類而在陽極側上的一個第一氣相區域處產生產物氣體心物氣體之主要成份為氟氣，並且同時在陰極側上的1 二氣相區域處產生副產物氣體，該副產物為氫氣； I成份進一個起始材料導管’該起始材料導管將起始氟化氣給到該熔融鹽類之内；導管將該產物氣體從該第—氣導管將該副產物氣體從該第二一個第一導管，該第一相區域處抽出；一個第二導管，該第— 氣相區域處抽出；一個第一壓力規，芎笛 η 4, m ^ , 成第一壓力規連續地量測在該第_ 氣相區域中之壓力；個第二壓力規，該第二壓力規連續地量測在該第二氣相區域中之壓力； ——個第一流率控制間’該第-流率控制閥被配置在該弟一導管中； -個第二流率控制閱，該第二流率控制閥被配置在該弟二導管中； "'個第一控制構件，該第-控制構件依據來自該第— 差力規所量測的結果來調節該第一流率控制閥之孔徑，用 35 200400921 x將。亥第一氣相區域中之壓力維持在一個第一設定值；以及一個第二控制構件’該第二控制構件依據來自該第二 i力規所量測的結果來調節該第二流率控制閥之孔徑，用 j將該第二氣相區域中之壓力維持在一個，該第二設定值貝裊專於該第一設定值。 2.如申凊專利範圍第丨項之用於產生氟氣的裝置，其中，该第一設定值與該第二設定值為76〇_82〇 τ〇π。胜' 3.如申請專利範圍帛1項之用於產生氟氣的裝置，其晋:在於，其亦提供有—個第—抽吸裝置，該第—抽吸裝 ’配置在該第—流率控制閥下游處的該第一導管中且抽吸該第一導管。业特二：申Ϊ專利範圍帛2項之用於產生氟氣的裝置，Α 提供有—個第—抽吸裝置，該第—抽吸f 罝被配置在續繁_ ^#· I 在 1隹3弟一導音中，該第— 制閥下旌步并n 導B °亥在6亥第一流率控閃下游處，並且可以抽吸該第一導管。 5. 如申請專利範圍第3 φ a吐用於產生氟氣的裝詈，甘中，该第二導管被配置，置其澈 '奉括用將遠弟二流率控制閥順基π 游連接到—個第阳阀順者下第二導管。 4置，該弟二抽吸裝置可以抽吸該 6. 如申請專利範圍第4項之中，今楚-，首a ;產生默1氧的裝置，甘遠第二導管被配置，用以置其游i車姐：?丨 & 弟—/;IL率控制閱順I π 子連接到一個第二抽吸裝置，誃 ^丨貝者下第二導管。 ” C 、置可以抽吸該 36 ^如中請專利範圍第1項利6項其中任—項之用於產生氟氣的裝置’其特徵在於，其亦提供有，一個切換閥，兮+TJ 4A Ba ^ μ 換閥被配置在該起始材料導管中；一個電流_人哭. _ _ 。°。，该電流整合器整合於該電解電池的 %極側上的電極以及哕 A_ ^ °x電解電池的陰極側上的電極之間被供給的電流；以及一個控制構件。制構件依據該電流整合器所產生的里測結果來操作令如姑^日日 ^ 、閥，用以控制進入到該熔融鹽類之内的氟化氫之供給。 8 ‘如申請專利笳圚筮弟7項之用於產生氟氣的裝置，其中，進，.·&通過該起始枯料刊竹等s之亂化氫為氣體。 9. 如申請專利筋園笛 ,^ 圍第8項之用於產生氟氣的裝置，其中’ δ玄起始材料導營祜 ^ , -置，用以將該氟化氫氣體進給到 S亥電解電池的陰極上的熔融鹽類之内，並且特徵在於一個可以將氮翁i#仏 ’ >Ό §χ起始材料導管内的導管被連接到該處’其在該切換關的Τ、、祕士 it έΛν 5,, ^ ^ /免，並且與氮氣混合之氟化氫被進給到该熔融鹽類之内。 10. 種用於產生氟氣之裝置，其特徵在於：電解電池，該電解電池完成在一個電解浴中之氟二H该電解浴包括含有氟化氫之炫融鹽類，並從 ^ 们苐一氣相區域處產生產物氣體，該產物：體之主要成份為氣氣，並且同時在陰極側上的一個第一氣相區域處差在Sl ^ ^ M 田物氣體’該副產物氣體之主要成份肩7氧氣； 37 200400921 -個起始材料導管，該起始材料導管將起始氣化氯進給到該熔融鹽類之内； -個第-導管，該第一導管將該產物氣體從該第一氣相區域處抽出；〃-個第二導管’該第一導管將該副產物氣體從該第二氣相區域處抽出；一個切換閥，該切換閥被配置在該起始材料導管中，· 0 一個電流整合器，該電流整合器整合於該電解電池的陽極侧上的電極以及該電解電池的陰極側上的電極之間被供給的電流；以及 -個控制構件’該控制構件依據該電流整合器所產生的$測結果來操作該bM 換闕’用以控制進入到該熔融鹽類之内的氟化氫之供給。 11·如申請專利範圍帛1G項之用於產生氟氣的裝置，其中，進給通過該起始㈣導管之氟化氫為氣體。 12.如申請專利笳圚铱圍第11項之用於產生氟氣的裝置，其中，β亥起始材料導營# @ $ S被配置’用以將該氟化氫氣體進給到該電解電池的陰極彻上的炫融鹽類之内’並且特徵在於一個可以將氮氣進給刹兮如 ^ ^ ' j s亥起始材料導管内的導管被連接到該處’其在該切換閥的下游處，並且與氮氣混合之氟化氫被進給到該熔融鹽類之内。拾壹、圖式：如次頁 38200400921 The scope of the patent application: 1. A device for generating fluorine gas, which is characterized by: gas in an electrolytic bath, and an electrolytic cell. The electrolytic cell completes the electrolysis of hydrogen, and the electrolytic bath includes a line containing hydrogen fluoride. Tritium is produced in a first gas phase region on the anode side. The main component of the core gas is fluorine gas, and at the same time a by-product gas is generated in the second gas phase region on the cathode side. The by-product is Hydrogen; I component into a starting material conduit 'The starting material conduit feeds the starting fluorinated gas into the molten salt; the conduit removes the product gas from the first-gas conduit and the byproduct gas from the first Two first conduits, withdrawn at the first phase region; one second conduit, withdrawn at the first-gas phase region; one first pressure gauge, flute η 4, m ^, continuously forming the first pressure gauge Measure the pressure in the first gas phase region; a second pressure gauge, the second pressure gauge continuously measures the pressure in the second gas phase region; a first flow rate control room -flow A control valve is arranged in the first conduit; a second flow rate control valve, the second flow rate control valve is arranged in the second conduit; " a first control member, the first control member Adjust the aperture of the first flow rate control valve according to the measurement result from the first differential gauge, using 35 200400921 x will. The pressure in the first gas phase region is maintained at a first set value; and a second control member 'the second control member adjusts the second flow rate control according to a result measured from the second force gauge. The aperture of the valve maintains the pressure in the second gas phase region at one with j, and the second set value is specialized to the first set value. 2. The device for generating fluorine gas according to item 丨 of the patent application, wherein the first set value and the second set value are 76-82-τ0π. Win '3. If the device for generating fluorine gas according to item 1 of the scope of patent application, its advantage is that it also provides a first suction device, the first suction device is arranged in the first flow In the first conduit downstream of the rate control valve and suck the first conduit. Industry special second: the scope of the patent application for 2 items of the device for generating fluorine gas, A is provided with a first suction device, the first suction f 罝 is configured in the continuation _ ^ # · I at 1 In the first pilot sound of the third brother, the first control valve and the n pilot B ° are downstream of the first flow rate control flash of the sixteenth hour, and the first catheter can be sucked. 5. As in the scope of patent application No. 3 φ a for the equipment for generating fluorine gas, Ganzhong, the second conduit is configured, and it is used to connect the distant second-rate control valve Shunji Pi to — The first male valve goes down the second catheter. 4 sets, the second suction device can suck the 6. As in the scope of the patent application No. 4, Jin Chu-, the first a; a device to generate silent oxygen, the Ganyuan second catheter is configured to set His tour car sister:? 丨 &younger-/; IL rate control read Shun I π son is connected to a second suction device, 誃 ^ 丨贝下下下管. C. The device can pump the 36 ^ as described in the patent scope of item 1 to item 6 of any of the items-the device for generating fluorine gas is characterized in that it also provides, a switching valve, Xi + TJ 4A Ba ^ μ valve is configured in the starting material conduit; a current _ crying. _ _ °. The current integrator is integrated on the electrode on the% pole side of the electrolytic cell and 哕 A_ ^ ° x The current supplied between the electrodes on the cathode side of the electrolytic cell; and a control component. The control component operates an order such as a valve and a valve according to the measured results generated by the current integrator to control access to The supply of hydrogen fluoride within the molten salt. 8 'As for the device for generating fluorine gas in the 7th patent application, in which, ..., & Randomly hydrogenated gas is a gas. 9. For example, a patent application for a device for generating fluorine gas in item 8 of the patent, where the δ starting material is used to generate the hydrogen fluoride gas. Into the molten salt on the cathode of the Shai electrolytic cell, and It is characterized in that a catheter inside the nitrogen starting material i # 仏 '> Ό §χ starting material conduit is connected to the place where it is located at the switch, 秘, 秘 5, νΛν 5 ,, ^ ^ / free, And hydrogen fluoride mixed with nitrogen is fed into the molten salt. 10. A device for generating fluorine gas, characterized by: An electrolytic cell, the electrolytic cell completes the electrolysis of fluorine in a electrolytic bath. The bath includes dazzling molten salts containing hydrogen fluoride, and generates a product gas from a gas phase region. The main component of the product: the gas is gas, and at the same time, it is in a first gas phase region on the cathode side. Sl ^ ^ M field gas' the main component of the by-product gas is 7 oxygen; 37 200400921-a starting material conduit which feeds the starting vaporized chlorine into the molten salt;- A second conduit, the first conduit extracts the product gas from the first gas phase region; 〃 a second conduit, the first conduit extracts the byproduct gas from the second gas phase region; a Switching valve, which is configured In the starting material conduit, a current integrator that integrates a current supplied between an electrode on the anode side of the electrolytic cell and an electrode on the cathode side of the electrolytic cell; and The control component 'the control component operates the bM switch according to the $ test result produced by the current integrator' is used to control the supply of hydrogen fluoride into the molten salt. 11. · If the scope of the patent application is 1G item A device for generating fluorine gas, wherein hydrogen fluoride fed through the starting tritium duct is a gas. 12. The device for generating fluorine gas according to item 11 of the patent application of osmium iridium, wherein βHai starts Material Guide Camp # @ $ S is configured 'to feed the hydrogen fluoride gas into the molten salt on the cathode of the electrolytic cell' and is characterized by a nitrogen gas feed such as ^ ^ js A conduit in the helium starting material conduit is connected there 'it is downstream of the switching valve, and hydrogen fluoride mixed with nitrogen is fed into the molten salt. Pick up, schema: as next page 38