201219104 六、發明說明： 【發明所屬之技術領域】 施該方法 -本發明係有關於一種氧族元素蒸汽冷凝及經冷凝氧族 元素再循環進人汽化元件之方法’及提供_裝置係用以實 【先前技術】 本發明之氧族元素係為元素週期表之第六主族元素 (除了氧以外)。*此，利用物理氣相沉積法(pvD)將氧族元 素部份地沉積於待塗佈物上。舉例而言，藉由物理氣相沉 積法(PVD)在基板上塗佈氧族元素。上述方法之實例已於專 利號W〇2_/034131 A2中揭露，具體而言，利用物理氣相 >儿積法(PVD)將氧族元素沉積於基板，其為製造化合物半導 體層之部分製程》 在此類物理氣相沉積法（PVD)中，通常藉由載送氣體將 氧族元素蒸汽提供至㈣佈物（如，基板），岐基板表面上 况積部分的氧族元素，並藉由如吸取方式將其他未沉積的 氧族元素蒸汽抽離。因此，關於再利用含有未沉積的氧族 凡素蒸汽之氧族元素，以進_步再進行塗佈，係具有其必 要性》其中’此未參與沉積的氧族元素蒸汽通常混合著載 送氣體及/或其他氣體或H故本發明針對此問題提供一 解決方法。 【發明内容】 201219104 上述問題可利用一方法得以解決’該方法係且有申請 專利範圍第丨項所請之特徵。 八 本發明亦提供一裝置，可利用該裝置實施解決上述問 題之方法。 上述問題可利用一裝置得以解決，該裝置係具有申請 專利範圍第5項所請之特徵。 較佳的改良係為其他申請專利範圍附屬項之標的。 本發明之方法包括：提供氧族元素蒸汽進入冷凝器， 在冷凝器中，至少部份的氧族元素蒸汽可冷凝成液態氧族 兀素’並且該液態氧族元素可經由一形成部份回流管路之 隔氣阱，再循環至汽化元件中。在此隔氣阱中亦設有一液 態氧族元素段’藉由該液態氧族元素段使存在於冷凝器及 汽化元件間之壓差達成平衡。 通常在汽化元件中的壓力較高於冷凝器中的壓力，儘 管具有此壓差，該液態氧族元素段可使液態氧族元素自冷 凝器再循環至汽化元件中，單藉由重力作用即可實現此再 循環反應。再者’就經濟效益上而言，液態氧族元素段亦 防止氧族元素蒸汽自汽化元件經過回流管路進入冷凝管 中。 本發明中’液態氧族元素段係為液態氧族元素之一凝 聚量’其延伸至回流管路的整個橫截面（至少局部地）。例 如’當回流管路橫截面由於如由嵌入物、固態氧族元素成 分、或任何其他物質使局部變得狹窄，此時即視剩餘的橫 戴面開口為回流管路的橫截面。 5 201219104 回火二族7L素蒸汽藉由通過裝設於冷凝器内的油 = 火’即可在冷凝器中達成氧族元素蒸汽之冷 提二:元族"°素蒸汽’送氣體混合物的方式，可 : 素蒸>'至冷凝器中，其中，以氮氣作為載送氣 'J用混α氣體流將氧族元素蒸汽供給至 :r:广形成-氧族元素蒸汽·載送氣體混=!氣 供給至冷凝器中。可=====素蒸汽 動，具體而言，該吸取裝置可為—通風器。讀的流 =在冷凝器中未達成冷凝之氧族元素蒸汽，較佳 地’將其供給至-過㈣，利用該過㈣將氧 與氣體混合物中的其他氣體成分(如，載送氣體)分離 氣體成分可作為殘餘氣體或廢氣發散至環境t，或者，、从 有必要，可進一步進行純化步驟。 右 虹吸管（siphon)，常在英語系國家中被稱作為隔 ㈣），原、則上可為任何形式之隔㈣，舉例而言，瓦 隔氣拼、「P型隔氣解」、或「s型隔氣牌」，較佳為一： 有至少一個U形管節(如?型隔氣阱、或S型隔氣阱)之隔氣 阱，然而，此管節之橫截面形狀不受到限制。 、 較佳地，以砸蒸汽或硫蒸氣作為氧族元素蒸汽。經過 冷凝反應後，視不同情況以得到液態硒或液態硫。 201219104 較佳地，冷凝器主要的溫度（如上述油回火板之溫度） 係維持在220。(：至300〇C之間，尤其是較佳為27〇cc>上述溫 度值特別是證實於硒蒸汽之冷凝反應中。 又較佳地，藉由液態氧族元素段至少部份固化，而形 成存封隔氣啡之固態氧族元素止子。上述情況可發生於冷 凝反應的最後，使得此回流管路持續地密封。長時間的加 熱使液態氧族元素段保持在液體狀態之步驟可被省略，當 此冷凝反應再次啟動時，不會有氧族元素蒸氣自汽化元件 經過回流管路進入冷凝器内之風險。 相反地，可藉由本發明之密封隔氣阱之固態氧族元素 止子的至少一部份熔化，形成液態氧族元素段。在冷凝反 應啟動時，可確定的是液態氧族元素可流經隔氣阱，因此 液態氧族元素可再循環至汽化元件。 較佳地，本發明所使用之回流管路，係由下行管路、 隔氣^及連接管路所形成。其巾，該下行管路連接冷凝 器與隔氣阱，該連接管路連接隔氣阱及汽化元件。主要分 布在回流管路的三個區域之溫度可各別地控制，尤其是， 可獨立地調節各自的溫度。 。藉由各別獨立地控制及/或調節上述回流管路中不同 區域中液態氧族元素的溫度，使各自的區域中液態氧族元 素的流動特性可獨立地控制及/或調節。本發明之下行管路 並非必為單調的下降形式，然而’較佳為-個下降方：或 個直立路線方向的下行管路。 201219104 透過實驗證實，較佳的實驗條件係為維持下行管路的 溫度主要分布於220。(：至27MC之間；維持隔氣啡的溫度主 要分布於190。(：及270。0：之間；以及維持連接管路的溫度主 要分布於240。0及500。(：之間，較佳為大約27〇〇c。尤其是， 當使用硒蒸汽作為氧族元素蒸汽時，經證實，由於在下行 管路的砸由半流體（semi_liquid)轉變成薄液$ (thin-liquid)’因此在連接管路的硒為薄液體，且藉主要分 布在隔氣阱之溫度可控制或調節經過隔氣阱之液態硒流。77 -本發明中’藉由-溶化閥可控制經過隔㈣之液^氧 族元素流。藉由連接-個控制電路，亦可用以調節經過隔 氣拼之液態氧族元素流。溶化閥係為一裝置，其可透過溶 化或固化存在於隔氣_物體之方式改變經過隔氣啡之流 動’在固化的狀態t，至少部份的上述物體減少隔氣牌管 路之橫截面。藉由改變液態氧族元素的黏度亦可影響流動 的改變。關㈣化閥的實例將更詳盡地敘述於本發明之設 備中。 本發明的方法之一較佳實施例中，透過調節主要分布 於隔氣阱之溫度及隔氣阱自身的溫度，以開啟及關閉經過 隔氣牌的液態氧族元素流，以此方式不是使在隔氣解中的 氧族素固化不再流動，就是使氧族元素流可通過該隔氣 當透過隔氣牌開啟此氧族元素流，接著可藉由控制或 調沛主要刀佈於下行管路的溫度，以控制或調節經過隔氣 阱的液態氧族元素流的速率。 201219104 本發明用於實施冷凝方法之設備 一連接於該冷凝5!且用於匕括一冷凝Is，及 流管路，“！ί 氧族元素移離冷凝器之回 =1中’此含有-隔氣啡之回流管路可使液峨氧族 疋素至>、流經一些時間。藉由 、 I#卜，你s , 罝第一加熱裝置於隔氣 部分隔氣牌可各別地加熱。「可各別地加 二係=此隔氣_其料同的加熱裝置分開，各別地 加熱。第一加熱元件係為熔化閥的一部分。 :上述所言，此隔氣拼原則上可為任何形式之隔氣 阱二舉例而言’如瓶式隔氣阱、「P型隔氣阱」、或「s型 隔氣阱」’較㈣一具有至少一個〜___、 或s型隔㈣）之隔㈣’然而’此管節之橫截面形狀不受 到限制。 第加熱裝置較佳為設置於隔氣拼的水平載段上。當 隔氣牌具有一 u形管節，其第一加熱褒置更佳地設置於u 形管節的彎曲處，其係由於在此處易形成一液態氧族元素 段；接著可藉由第一加熱裝置影響液態氧族元素段之凝聚 的溫度及狀態。 又較佳地’第一加熱裝置係為一熔化閥的一部分，其 中，熔化閥具有一沿著第一加熱裝置設置的冷卻裝置◊如 上述之熔化閥可用來控制或調節經過隔氣阱的液態氧族元 素流。 較佳地，該冷卻裝置具有一含有一孔腔之中空柱，其 中，該孔腔置於一中空柱護套内，且孔腔適用於沖流冷卻 介質。其冷卻裝置亦具有一開放進入孔腔之進口，其適用 9 201219104 於將冷卻介質導入孔腔；以及，一導出孔腔之出口，其適 用於將冷卻介質導出孔腔。 較佳地，中空柱環繞於部分截段的隔氣阱。獨立地， 該熔化閥較佳地設置於隔氣阱的水平截段上。當隔氣阱具 有一u形管節，其熔化閥更佳地設置於u形管節的彎曲處， 其係由於在此處易形成一液態氧族元素段；接著可藉由熔 化閥控制或調節液態氧族元素段之凝聚的溫度及狀態，進 而可控制或調節經過隔氣阱的液態氧族元素流。 實際上’第一加熱裝置具有至少一個第一型加熱元 件，其於沿著中空柱之縱向延伸位置上設置。 較佳地，第-加熱裝置包含至少兩個第一型加熱元 件，其设置於沿著中空柱之縱向延伸位置上。此中介柱μ 置於至少兩個第一型加熱元件之間，尤其是，可藉：改： 熔化閥之熱輸出及轉換速率。 又較佳地，該第一型加熱 減少熱放射至非預期的方向上 至回流管路的環境中。並且， 少溶化閥自由接觸的加熱區域 接觸的區域耗損的風險β 元件設有一絕熱層，其用以 。其主要目的為防止熱放射 該絕熱層在加熱過程中可減 ，因而降低此熔化閥所自由 較佳地，該第-加熱裝置包含至少一個第二型加 件，其設置於中空柱的外部表面區域。此第㈣ 可使因冷卻介質的沖流而冷卻之中空枉更快地加叙:·牛 炫化間的開關時間縮短。第4加熱元件尤_ = 201219104 有單元面積之熱輸出大於第一型加熱元件之加熱元件。因 此，可更進一步縮短開關時間。 又較佳地’以一外殼包覆此設置於中空柱外部表面區 至少一個第二型加熱元件，此外殼可用於防止在加熱過程 中接觸到第二型加熱元件或中空柱，該外殼可為如對應於 實際型態之外罩（cage)。 本發明裝置之另一具體實施例，該熔化閥包含至少一 個溫度感測器’其較佳地設置於中空柱的内部表面區。尤 其較佳地至J —個溫度感測器可包括例如一熱電偶，此 熱電偶與-控制或調節裝置連接，且控制或調節裝置可依 序地連接到至少部份加熱元件，使該些加熱元件可基於該 溫度感測器的讀數受到控制或調節。 ,該回流管路較佳為由下行管路、隔氣阱、及連接管路 所形成#中，該下行管路連接冷凝器至隔器解’該連接 管路連接隔氣牌及汽化元件。該下行管路上設有一第二加 熱裝置，藉由第二加熱裝置，使下行管路之至少特定部份 :可：：地加熱。再者，該連接管路上設有一第三加熱裝 置’藉由第三加熱裝詈，你、由& # 使連接管路之至少特定部份上可 /刀別地加熱，由此，此法Λ 士抽 机s路之上述不同區域可分別地 加熱。如以上所述，本發明狀201219104 VI. Description of the Invention: [Technical Field of the Invention] The present invention relates to a method for vapor condensation of oxygen species and recycling of vaporized oxygen elements into a vaporization element. [Prior Art] The oxygen element of the present invention is the sixth main group element of the periodic table (except oxygen). *This, the oxygen element is partially deposited on the object to be coated by physical vapor deposition (pvD). For example, an oxygen group element is coated on a substrate by physical vapor deposition (PVD). An example of the above method is disclosed in the patent number W〇2_/034131 A2, specifically, a physical grouping method (PVD) is used to deposit an oxygen group element on a substrate, which is a part of a process for manufacturing a compound semiconductor layer. In such physical vapor deposition (PVD), the oxygen element vapor is usually supplied to the (four) cloth (for example, the substrate) by the carrier gas, and the oxygen element of the conditional portion on the surface of the substrate is borrowed and borrowed. The other undeposited oxygen element vapors are evacuated by, for example, suction. Therefore, it is necessary to re-use the oxygen-containing element containing undeposited oxygen-containing voxel vapor to carry out the coating in the next step. "The oxygen element vapor which is not involved in the deposition is usually mixed and carried. Gas and/or other gases or H The present invention provides a solution to this problem. SUMMARY OF THE INVENTION 201219104 The above problem can be solved by a method which is characterized by the requirements of the scope of the patent application. The present invention also provides a device by which a method for solving the above problems can be implemented. The above problems can be solved by means of a device having the features requested in item 5 of the scope of the patent application. The preferred improvements are those of the other patent application scopes. The method of the present invention comprises: providing oxygen group element vapor into the condenser, wherein at least a portion of the oxygen elemental vapor can be condensed into a liquid oxygen groupin' and the liquid oxygen group element can be reflowed through a portion The gas trap of the pipeline is recycled to the vaporization element. A liquid oxygen species segment is also provided in the gas trap. The liquid oxygen species segment balances the pressure difference existing between the condenser and the vaporization element. Usually the pressure in the vaporization element is higher than the pressure in the condenser, and despite this pressure difference, the liquid oxygen group element can recycle the liquid oxygen group element from the condenser to the vaporization element, by gravity alone This recycling reaction can be achieved. Furthermore, in terms of economic efficiency, the liquid oxygen group element also prevents the oxygen element vapor from entering the condenser through the return line from the vaporization element. In the present invention, the 'liquid oxygen group element segment is the amount of condensation of one of the liquid oxygen group elements' which extends to the entire cross section of the return line (at least partially). For example, when the cross-section of the return line is locally narrowed by, for example, an insert, a solid oxygen element component, or any other substance, the remaining cross-sectional opening is considered to be the cross-section of the return line. 5 201219104 The tempered two-family 7L gas vapor can be cooled in the condenser by the oil installed in the condenser = fire's: the elemental " The method can be as follows: a liquid steaming > 'to the condenser, wherein nitrogen gas is used as the carrier gas 'J to supply the oxygen element vapor to the mixed alpha gas stream to: r: broadly forming - oxygen group vapor · carrier gas The mixed gas is supplied to the condenser. The pressure can be =====, specifically, the suction device can be a ventilator. Read stream = oxygen elemental vapor that is not condensed in the condenser, preferably 'supplied to - (4), using the other gas components in the mixture of oxygen and gas (eg, carrier gas) The separated gas component may be emitted as a residual gas or exhaust gas to the environment t, or, if necessary, may be further subjected to a purification step. The siphon is often referred to as the partition (4) in the English-speaking countries. The original can be any form (4). For example, the tile is separated, the "P-type gas solution", or " S-type gas barrier", preferably one: a gas trap having at least one U-shaped pipe joint (such as a gas trap or an S-type gas trap), however, the cross-sectional shape of the pipe joint is not affected limit. Preferably, helium vapor or sulfur vapor is used as the oxygen element vapor. After the condensation reaction, depending on the situation, liquid selenium or liquid sulfur is obtained. 201219104 Preferably, the main temperature of the condenser (such as the temperature of the oil tempering plate described above) is maintained at 220. (: between 300 〇C, especially preferably 27 〇 cc) The above temperature values are particularly confirmed in the condensation reaction of selenium vapor. Further preferably, the liquid oxygen group element is at least partially cured, and Forming a solid oxygen group stop of the ventricle. The above situation may occur at the end of the condensation reaction, so that the return line is continuously sealed. The long-time heating keeps the liquid oxygen group element in a liquid state. Omitted, when this condensation reaction is started again, there is no risk of oxygen group vapor entering the condenser from the vaporization element through the return line. Conversely, the solid oxygen element of the sealed gas trap of the present invention can be used. At least a portion of the child is melted to form a liquid oxygen group element. Upon initiation of the condensation reaction, it is determined that the liquid oxygen species can flow through the gas trap, so that the liquid oxygen species can be recycled to the vaporization element. The return pipeline used in the present invention is formed by a descending pipeline, a gas barrier, and a connecting pipeline. The descending pipeline connects the condenser and the gas trap, and the connecting pipeline is connected to the gas trap. And vaporization elements. The temperatures mainly distributed in the three regions of the return line can be individually controlled, in particular, the respective temperatures can be independently adjusted. By individually controlling and/or regulating the above-mentioned return line The temperature of the liquid oxygen group elements in different regions allows the flow characteristics of the liquid oxygen group elements in the respective regions to be independently controlled and/or regulated. The pipeline under the present invention is not necessarily in a monotonously decreasing form, however, - a descending side: or a downward line in the direction of an upright route. 201219104 It has been confirmed by experiments that the preferred experimental conditions are to maintain the temperature of the downstream pipeline mainly distributed at 220. (: to 27MC; maintain the gas barrier The temperature is mainly distributed between 190. (: and 270. 0: between; and the temperature at which the connecting pipe is maintained is mainly distributed between 240. 0 and 500. (: between, preferably about 27 〇〇 c. Especially, when When selenium vapor is used as the oxygen element vapor, it has been confirmed that selenium in the connecting pipe is a thin liquid because the helium in the down pipe is converted from a semi-liquid to a thin liquid (thin-liquid) main The temperature of the gas trap can control or regulate the liquid selenium flow through the gas trap. 77 - In the present invention, the liquid oxygen group element passing through the partition (four) can be controlled by the -dissolving valve. The circuit can also be used to regulate the flow of the liquid oxygen element element through the gas barrier. The melting valve is a device that can be dissolved or solidified in the form of a gas barrier to the object. t, at least some of the above objects reduce the cross section of the gas barrier tube. The change in flow can also be affected by changing the viscosity of the liquid oxygen species. Examples of the (four) valve will be described in more detail in the apparatus of the present invention. In a preferred embodiment of the method of the present invention, the liquid oxygen species flow passing through the gas barrier is opened and closed by adjusting the temperature mainly distributed in the gas trap and the temperature of the gas trap itself. It is not that the oxygenation of the oxygen species in the gas barrier is no longer flowing, that is, the oxygen element flow can pass through the gas barrier to open the oxygen element flow through the gas barrier, and then the main knife cloth can be controlled or adjusted. Down the pipeline Degree, to control or regulate the rate of liquid through the barrier gas trap chalcogen stream. 201219104 The apparatus for carrying out the condensation method of the present invention is connected to the condensation 5! and is used to include a condensation Is, and a flow line, "!ί Oxygen element moves away from the condenser back=1" This contains - The gas-repellent reflux line can make the liquid 峨 疋 至 至 & 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 Heating. "You can add two systems separately = this gas barrier _ the same heating device is separated and heated separately. The first heating element is part of the melting valve.: As mentioned above, this gas barrier is in principle For example, the trap type gas trap, the "P-type gas trap", or the "s-type gas trap" may have at least one ~___, or s-type partition. (4)) (4) 'However' the cross-sectional shape of this pipe joint is not limited. Preferably, the first heating device is disposed on the horizontal load of the gas barrier. When the gas barrier card has a U-shaped pipe joint, the first heating device is preferably disposed at the bend of the U-shaped pipe joint because it is easy to form a liquid oxygen group element portion here; A heating device affects the temperature and state of condensation of the liquid oxygen species. Still preferably, the first heating device is part of a melting valve, wherein the melting valve has a cooling device disposed along the first heating device. For example, the melting valve can be used to control or regulate the liquid passing through the gas trap. Oxygen element flow. Preferably, the cooling device has a hollow column containing a cavity, wherein the cavity is placed in a hollow column jacket and the cavity is adapted to flow through the cooling medium. The cooling device also has an inlet for opening into the bore, which is adapted to introduce a cooling medium into the bore; and an outlet for the outlet, which is adapted to direct the cooling medium out of the bore. Preferably, the hollow column surrounds a partial section of the gas trap. Independently, the melting valve is preferably disposed on a horizontal section of the gas trap. When the gas trap has a U-shaped pipe joint, the melting valve is preferably disposed at the bend of the U-shaped pipe joint because it is easy to form a liquid oxygen group element portion; then it can be controlled by a melting valve or The temperature and state of condensation of the liquid oxygen species are adjusted to control or regulate the flow of liquid oxygen species through the gas trap. In fact, the first heating means has at least one first type of heating element disposed in a longitudinally extending position along the hollow column. Preferably, the first heating means comprises at least two first type heating elements disposed in a longitudinally extending position along the hollow column. The intermediate column μ is placed between at least two first-type heating elements, in particular, by: the heat output and the slew rate of the melting valve. Still preferably, the first type of heating reduces heat radiation to an unintended direction into the environment of the return line. Moreover, the area where the heating zone where the dissolution valve is freely contacted is at risk of being worn out. The beta element is provided with a heat insulating layer for use. The main purpose of the heat-preventing layer is to prevent the heat-insulating layer from being reduced during the heating process, thereby reducing the freedom of the melting valve. Preferably, the first heating device comprises at least one second-type additive member disposed on the outer surface of the hollow column. region. This (4) allows the hollow enthalpy cooled by the rushing of the cooling medium to be added more quickly: • The switching time between the cows is shortened. The fourth heating element is especially _ = 201219104 The heating output with the unit area is larger than the heating element of the first type heating element. Therefore, the switching time can be further shortened. Further preferably, the outer surface of the hollow column is covered with at least one second type heating element, and the outer casing can be used to prevent contact with the second type heating element or the hollow column during heating, the outer casing can be For example, it corresponds to the actual type of cage. In another embodiment of the apparatus of the present invention, the melting valve includes at least one temperature sensor 'which is preferably disposed in an interior surface region of the hollow column. Particularly preferably, the J temperature sensor may comprise, for example, a thermocouple connected to the control or regulating device, and the control or regulating device may be sequentially connected to at least a portion of the heating element to make the The heating element can be controlled or adjusted based on the reading of the temperature sensor. Preferably, the return line is formed by a down line, a gas trap, and a connecting line. The down line connects the condenser to the separator. The connecting line connects the gas barrier and the vaporization element. The descending pipeline is provided with a second heating device, and at least a specific portion of the descending pipeline can be heated by the second heating device. Furthermore, the connecting pipe is provided with a third heating device 'by the third heating device, and you can heat at least a certain portion of the connecting pipe by the &#, thereby, the method The different areas of the above-mentioned pumping machine can be separately heated. As described above, the present invention
,缺 ^ 發月之下仃官路並非必為單調的下 降形式，然而，較佳為—個A 方向的下行管路。個為下降方H個為直立路線 201219104 較佳地，該下行管路設計為一下向流管（d〇wnpipe)，該 連f S路設S十為一連接管（c〇nnecting pipe)，其中該下向 流管及該連接管的橫截面形狀不受到限制。 冷凝器可經由一過濾管路與一過濾器連接，過濾器可 於一含有氧族元素蒸氣之氣體混合物中將氧族元素蒸汽過 滤出來。 未達成冷凝的氧族元素蒸汽可藉由此過濾器過濾出 來’使得僅冑少量或甚至無氧族元素蒸汽進入大氣中。 一較佳地，冷凝器經由回流管路與一汽化元件連接，液 態氧族元素可因此回到該汽化元件中，並再重複利用。汽 化兀件可例包括一腔體之石墨塊形&，而纟冷凝過程 中炫化的氧族元素置於該腔體中。 一通風器可用於提供氧族元素蒸汽進入冷凝器内，該 通風器可用於產生一氣流導入該冷凝器中。舉例而言，可 藉由通風器將一氧族元素蒸汽_載送氣體混合物流導入冷 凝器中。 【實施方式】 圖1及圖2說明本發明的方法及設備之第一具體實施 例。在此具體實施例中，本發明之設備具有一冷凝器9及一 連接於s亥冷凝器9之回流管路丨7，回流管路丨7可將液態氧族 兀素自冷凝器9移離。此具體實施例中，确蒸汽氮氣混合物 36係作為氧族元素蒸汽而提供至冷凝器9中。在此，氮氣係 作為砸蒸汽之載送氣體。 201219104 碼蒸Ά氮氣混合物36之场蒸汽，係由一汽化元件1產 生’其中’液態砸2置於汽化元件1内。於過壓下，氮氣經 由一氮氣進氣口 3導入至汽化元件丨中，並由液態硒2上方通 過。此氮氣作為載送氣體並在此吸收硒蒸汽。如圖所示， 此形成的砸蒸汽氮氣混合物3 6接著經過一供應線5進入一 塗佈頭4。於一塗佈頭4的塗佈區ό中，一部分含在硒蒸汽氮 氣混合物36内的硒蒸汽沉積於一基板7上。為了達成均勻地 塗佈，此基板7可較佳地以一個穩定速度引導經過塗佈頭4 下方。然而，大部分的硒蒸汽仍然存在於硒蒸汽氮氣混合 物36内，並經過一進給線8進入冷凝器9(如圖丨所示 如圖1中所示之態樣的變化可為，汽化元件丨及塗佈頭4 可以單一元件形式作成。舉例來說，一勻相石墨塊可同時 配置有汽化元件及塗佈頭。此塗佈頭本身進一步詳細地描 述於德國的專利申請號102009009022中。 在本具體實施例中，硒蒸汽氮氣混合物36藉由一通風 器14進入冷凝器9中，其中，該通風器14可用以形成一硒蒸 汽氮氣混合物氣體流《因此，通風器丨4於進給線8内產生一 負壓。油回火板1 〇維持在約270〇c之溫度，並設置於冷凝器 中。硒蒸汽氮氣混合物36中至少大部分硒蒸汽會在該些油 回火板上冷凝並收集於一漏斗丨丨，接著經過一回流管路 17(如圖！所*的虛線）回到汽化元件卜未達成冷凝的砸蒸汽 與載送氣體氮氣一同經過一過濾管路π導入一過濾器12， 由過濾器12將氮氣分離出來，剩餘的氮氣和其他進一步的 (3 201219104 氣體組成物經一吸引管路15及一排氣管路16進入大氣中， 或提供至一進一步的廢氣處理設施。 圖2之部分放大圖說明回流管路17的細節。如圖2所 示’回流管路17包含一隔氣阱35,該隔氣阱35在此例中設 計為一 S型隔氣拼。圖2亦表示回流管路17係由一下行管 路、隔氣阱35本身、以及一連接管路所形成，其中，該下 行管路連接冷凝器9至隔氣阱35，下行管路在此例設計為一 下向流管18;連接管路設計為一連接管2〇。 隔氣阱35含有一 U形管節19，藉由一存在於u形管節19 中之液態硒段21平衡冷凝管9與汽化元件1之間的壓差。此 壓差的平衡如圖2所示’液態硒段21於U形管節19内之左邊 咼度高於右邊高度。因此’在汽化元件1如預期地分布著一 較高於冷凝器9的壓力。若經冷凝後，此時液態硒從冷凝器 進入回流管路17,液態硒段21兩邊的高度上升至右邊的液 態砸可越過隔氣阱35’液態硒接著會進入連接管2〇，再到 達汽化元件1。 在圖2中’一熔化閥24設置於U形管節19的彎曲處。藉 由改變此區域硒的溫度，使得此熔化閥24可控制經過隔氣 拼35砸的流動《若液態硒冷卻下來，其黏性增加使得流動 降低，相反地，藉由加熱可使此流動增加。在一極端的情 況中’藉著讓U形管節19内的任何硒固化或熔化，以此方式 使經過隔氣阱35的流動可完全地中止或啟動。因此藉由溶 化閥24使經過回流管路17中硒的流動可開啟或關閉。以下 根據詳細的圖3做更詳盡地解釋。 201219104 圖3表示一固態硒止子22設置於U形管節19内，可藉由 形成此固態硒止子22,以關閉回流管路17(例如，在冷凝程 序結束後或關於製程的中斷）。圖3說明此裝置再重新操作 後的情況。在冷凝管9中，砸蒸汽已被冷凝下來，使得液態 硒存在於下向流管18内。在U形管節19中，藉由熔化閥24 使固態硒止子22接著熔化，至少直到可形成液態硒段21且 液態硒23可通過U形管節19的程度。此熔化閥24代表一第一 加熱裝置，藉此第一加熱裝置使隔氣阱35可分別地加熱。 如圖3所示，下向流管18上設有一第二加熱裝置39,以 及連接管20設有一第三加熱裝置4〇。利用此方式的設計使 下向流管18和連接管20亦可分別地加熱。因此，下向流管 18或連接管20中液態砸流動的特性，特別是流動速度，可 各別獨立地控制。為了更清楚表示，此第二加熱裝置及第 三加熱裝置未表示在圖2中。 圖4係為透過圖2及圖3之溶化閥之剖面示意圖，由此可 知’熔化閥24包括一含有一護套31的中空柱28。置於護套 31之孔腔37可用於沖流一冷卻介質。在此，任何冷卻介質 皆可使用，例如’一氣態膠体（aerosol)、水、油或氮氣。進 口 29可用於將冷卻介質導入孔腔28中。溶化閥24亦具有一 出口30，藉此出口30可用於將冷卻介質導出孔腔28外。中 空柱設置於U形管節19的一部位25。藉由冷卻介質的沖流經 過孔腔37，使部位25及其中的硒可因此冷卻》 熔化閥24亦包括第一型加熱元件26a、26b，其設置於 沿著中空柱28之縱向延伸位置上，此中空柱28係設置於該 15 201219104 些第-型加熱元件26a、2讣之間一第二型加孰元件”， 其設置於中空柱28之外部表面區域仏上，且Μ大於第一 型加熱元件26a、26b之單元面積熱輸出。因此，因冷卻介 質先冷卻下來的護套31，可相對較快速地加熱。第一型加 熱元件26a、26b及第二型加熱元件32, 一同形成第一加埶 裝置26a、26b、32 ’使具有第—加熱裝置w、说、32的 隔氣阱3 5可因此分別地加熱。 第二型加熱元件26a、26b±提供一絕熱層27，其用以 減少非預期熱放射至環境中，同時，可作為防止接觸的保 護。以-外殼33包覆第二型加熱元件32和中空㈣，作為 防止任何與第二加熱元件32〇空柱㈣意地接觸之防 護。此外殼33作用於防止與第二型加熱元件32、絕熱層U、 及中空柱28無意地接觸之防護。 一溫度感測器34,其設置於中空柱28之内部表面區域 31b上’可包括例如一熱電偶。如同第一型加熱元件^、 26b與第二型加熱元件32，以及在進⑼與出㈣的間似 閥42-樣’溫度感測器34連接於—控制或調節裝㈣(如圖 3所不)。因此，第一型加熱元件26a、26b與第二型加熱元件 32’以及在進口 29與出口 3〇的閥43與閥42可基於該溫度感 測器的讀數受到控制及/或調節。 【圖式簡單說明】 圖1係為本發明的方法與設備之—具體實施例的概念圖。 圖2係為圖1設備之詳細示意圖。 201219104 圖3係為圖2於密閉情況下之回流管路之詳細放大圖 圖4係為透過圖2及圖3之熔化閥之剖面示意圖。 【主要元件符號說明】 1 汽化元件 2 液態硒 3 氮氣進氣口 4 塗佈頭 5 供應線 6 塗佈區 7 基板 8 進給線 9 冷凝器 1〇 油回火板 11 漏斗 12 過濾器 13 過濾管路 14 通風器 15 吸引管路 16 排氣管路 17 回流管路 18 下向流管 19 U形管節 20 連接管 21 液態硒管 22 固態砸止子 23 液態晒 24 熔化閥 25 U形管節的一部位 26a第一型加熱元件 26b第一型加熱元件 27 絕熱層 28 中空柱 29 進口 30 出〇 31 中空柱護套 31a中空柱外部表面區 31b中空柱内部表面區 32第二型加熱元件 33 外殼 34 溫度感測器 35 隔氣阱 36砸蒸汽氮氣混合物 37 孔腔 38 控制/調節裝置 39 第二加熱裝置 201219104 40 第三加熱裝置 43 進口閥 42 出口閥 i 8, lack of ^ under the moon, the official road is not necessarily a monotonous descending form, however, it is better to be a descending line in the A direction. H is an upright route 201219104. Preferably, the down pipe is designed as a downward flow pipe (d〇wnpipe), and the connection f S road is set to S is a connection pipe (c〇nnecting pipe), wherein The cross-sectional shape of the downflow tube and the connecting tube is not limited. The condenser can be connected to a filter via a filter line which filters the oxygen element vapor in a gas mixture containing oxygen element vapor. Oxygen vapor which has not reached condensation can be filtered by this filter to cause only a small amount or even an oxygen-free elemental vapor to enter the atmosphere. Preferably, the condenser is connected to a vaporization element via a return line, whereby the liquid oxygen species can be returned to the vaporization element and reused. The vaporization element can be exemplified by a graphite block of a cavity and an oxygen element which is condensed during the condensation process is placed in the cavity. A ventilator can be used to provide oxygen elemental vapor into the condenser, which can be used to generate a gas stream into the condenser. For example, a stream of oxygen-carrier gas mixture can be introduced into the condenser by a ventilator. [Embodiment] Figs. 1 and 2 illustrate a first embodiment of the method and apparatus of the present invention. In this embodiment, the apparatus of the present invention has a condenser 9 and a return line 丨7 connected to the sigma condenser 9, and the return line 丨7 can remove the liquid oxygen steroid from the condenser 9. . In this embodiment, the vapor nitrogen mixture 36 is supplied to the condenser 9 as oxygen group vapor. Here, nitrogen gas is used as a carrier gas for helium vapor. The field steam of the 201219104 code steamed nitrogen gas mixture 36 is produced by a vaporization element 1 and the liquid liquid 2 is placed in the vaporization element 1. Under an overpressure, nitrogen is introduced into the vaporization element crucible through a nitrogen gas inlet 3 and passed over the liquid selenium 2 . This nitrogen acts as a carrier gas and absorbs the selenium vapor there. As shown, the resulting helium vapor nitrogen mixture 36 then passes through a supply line 5 into a coating head 4. A part of the selenium vapor contained in the selenium vapor nitrogen gas mixture 36 is deposited on a substrate 7 in the coating zone of the coating head 4. In order to achieve uniform coating, the substrate 7 can preferably be guided under the coating head 4 at a steady speed. However, most of the selenium vapor is still present in the selenium vapor nitrogen mixture 36 and enters the condenser 9 via a feed line 8 (as shown in Figure 1, the change in the aspect shown in Figure 1 may be, the vaporization element The crucible and coating head 4 can be formed as a single component. For example, a homogeneous phase graphite block can be provided with both a vaporization element and a coating head. This coating head itself is described in further detail in German Patent Application No. 102009009022. In the present embodiment, the selenium vapor nitrogen mixture 36 enters the condenser 9 via a ventilator 14, wherein the ventilator 14 can be used to form a selenium vapor nitrogen mixture gas stream. Thus, the ventilator 丨4 is fed. A negative pressure is generated in line 8. The oil tempering plate 1 is maintained at a temperature of about 270 〇c and is disposed in the condenser. At least a majority of the selenium vapor in the selenium vapor nitrogen mixture 36 will be on the oil tempering plates. Condensed and collected in a funnel, and then returned to the vaporization element through a return line 17 (as shown by the dashed line in Figure *). The vapor that has not reached condensation is introduced into the filter line π together with the carrier gas nitrogen. filter The separator 12 is separated from the nitrogen by the filter 12, and the remaining nitrogen and other further (3 201219104 gas composition enters the atmosphere via a suction line 15 and an exhaust line 16 or is supplied to a further exhaust gas treatment. Figure 2 is a partial enlarged view illustrating the details of the return line 17. As shown in Figure 2, the return line 17 includes a gas trap 35, which in this example is designed as an S-type gas barrier. Fig. 2 also shows that the return line 17 is formed by a lower line, a gas trap 35 itself, and a connecting line, wherein the down line connects the condenser 9 to the gas trap 35, and the down line is here. The example is designed as a downward flow tube 18; the connecting line is designed as a connecting tube 2 〇. The gas trap 35 contains a U-shaped tube section 19, and the condensing tube is balanced by a liquid selenium section 21 present in the u-shaped tube section 19. The pressure difference between 9 and the vaporization element 1. The balance of this pressure difference is as shown in Fig. 2. The left side of the liquid selenium section 21 in the U-shaped tube section 19 is higher than the right side height. Therefore, 'in the vaporization element 1 is as expected. The ground is distributed with a higher pressure than the condenser 9. If it is condensed, the liquid selenium is condensed at this time. Entering the return line 17, the height of the liquid selenium section 21 rises to the right, and the liquid helium can pass over the gas trap 35'. The liquid selenium then enters the connecting tube 2〇 and reaches the vaporizing element 1. In Fig. 2, a melting valve 24 is disposed at the bend of the U-shaped tube section 19. By changing the temperature of the selenium in this area, the melting valve 24 can control the flow through the gas barrier 35. If the liquid selenium is cooled down, the viscosity increases and the flow is lowered. Conversely, this flow can be increased by heating. In an extreme case 'by allowing any selenium in the U-shaped tube section 19 to solidify or melt, in this way the flow through the gas trap 35 can be completely Suspend or start. Therefore, the flow of selenium through the return line 17 can be opened or closed by the melting valve 24. The following is explained in more detail based on the detailed Figure 3. 201219104 Figure 3 shows a solid selenium stopper 22 disposed within the U-shaped tube section 19 by which the solid selenium stopper 22 is formed to close the return line 17 (e.g., after the end of the condensation process or with respect to process interruption) . Figure 3 illustrates the situation after the device is re-operated. In the condenser 9, the helium vapor has been condensed so that liquid selenium is present in the downflow tube 18. In the U-shaped tube section 19, the solid selenium stopper 22 is subsequently melted by the melting valve 24, at least until the liquid selenium section 21 can be formed and the liquid selenium 23 can pass through the U-shaped tube section 19. This melting valve 24 represents a first heating means whereby the first heating means allows the gas traps 35 to be separately heated. As shown in Fig. 3, a second heating means 39 is provided on the downflow tube 18, and a third heating means 4 is provided in the connecting tube 20. With this design, the downflow tube 18 and the connecting tube 20 can also be separately heated. Therefore, the characteristics of the liquid helium flow in the downflow pipe 18 or the connecting pipe 20, particularly the flow velocity, can be independently controlled. For the sake of clarity, the second heating means and the third heating means are not shown in Fig. 2. Fig. 4 is a schematic cross-sectional view through the melting valve of Figs. 2 and 3, whereby it is known that the melting valve 24 includes a hollow post 28 containing a sheath 31. A bore 37 placed in the jacket 31 can be used to flush a cooling medium. Here, any cooling medium can be used, such as 'a gaseous aerosol, water, oil or nitrogen. The inlet 29 can be used to introduce a cooling medium into the bore 28. The meltdown valve 24 also has an outlet 30 whereby the outlet 30 can be used to direct the cooling medium out of the bore 28. The hollow column is disposed at a portion 25 of the U-shaped tube section 19. The portion 25 and the selenium therein can be cooled by the flow of the cooling medium through the cavity 37. The melting valve 24 also includes first type heating elements 26a, 26b disposed in a longitudinally extending position along the hollow column 28. The hollow column 28 is disposed between the 15th and 19th type heating elements 26a, 2A, and a second type of twisting element, which is disposed on the outer surface area of the hollow column 28, and is larger than the first The unit area of the heating elements 26a, 26b is thermally outputted. Therefore, the jacket 31 cooled by the cooling medium can be heated relatively quickly. The first type heating elements 26a, 26b and the second type heating element 32 are formed together. The first twisting device 26a, 26b, 32' allows the gas traps 35 having the first heating means w, say 32 to be heated separately. The second type heating elements 26a, 26b ± provide a heat insulating layer 27 Used to reduce unintended thermal radiation into the environment, and at the same time, to protect against contact. The second type heating element 32 and the hollow (four) are covered by the outer casing 33 as a means to prevent any hollowing element (second) from the second heating element 32. Protection against contact. This enclosure 33 acts to prevent inadvertent contact with the second type heating element 32, the heat insulating layer U, and the hollow post 28. A temperature sensor 34, which is disposed on the inner surface area 31b of the hollow post 28, may include, for example, a Thermocouples, like the first type of heating elements ^, 26b and the second type of heating elements 32, and between the inlets (9) and (4), the valve 42-like temperature sensor 34 is connected to - control or adjustment (4) (such as 3, therefore, the first type of heating elements 26a, 26b and the second type of heating element 32' and the valves 43 and 42 at the inlet 29 and the outlet 3 can be controlled based on the reading of the temperature sensor and BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a conceptual diagram of a specific embodiment of the method and apparatus of the present invention. Fig. 2 is a detailed schematic diagram of the apparatus of Fig. 1. 201219104 Fig. 3 is a closed condition of Fig. 2 FIG. 4 is a schematic cross-sectional view of the melting valve through FIG. 2 and FIG. 3. [Main component symbol description] 1 vaporization component 2 liquid selenium 3 nitrogen gas inlet 4 coating head 5 supply line 6 Coating area 7 Substrate 8 Feed line 9 Condenser 1 〇 oil Tempering plate 11 Funnel 12 Filter 13 Filtration line 14 Ventilation 15 Suction line 16 Exhaust line 17 Return line 18 Down flow tube 19 U-shaped tube section 20 Connection tube 21 Liquid selenium tube 22 Solid 砸 砸23 Liquid drying 24 Melting valve 25 One part of U-shaped pipe joint 26a First type heating element 26b First type heating element 27 Insulation layer 28 Hollow column 29 Inlet 30 Outlet 31 Hollow column sheath 31a Hollow column outer surface area 31b hollow Column inner surface area 32 second type heating element 33 outer casing 34 temperature sensor 35 gas trap 36 砸 steam nitrogen mixture 37 cavity 38 control / regulating device 39 second heating device 201219104 40 third heating device 43 inlet valve 42 outlet Valve i 8