TW318151B - The method and apparatus for cleaning particles on silicon wafer using super- or sub-critical fluid - Google Patents

Abstract

A method for cleaning particles on silicon wafer surface by using super- or sub-critical fluid. It is the super- or sub-critical fluid with adorning agent by using static and dynamic ways to clean particles on silicon wafer surface. In which, the adorning agent is the mixing liquid composed by water, EDTA, H2O2, KHO, NH4CL, HNO3, Hydrochloric acid and mixing liquid of HNO3 and H3PO, and the pressure of super- or sub-critical fluid is less than 5000psi.

Description

Α7 Β7 318151 V. Description of the invention (i) The present invention relates to a method and device for washing silicon wafers using supercritical or subcritical fluids (for example: carbon dioxide or water), in particular to using supercritical or subcritical fluids (For example: carbon dioxide or water) A waste liquid-free and highly efficient method and device for cleaning contaminant impurities on the surface of silicon wafers to meet the needs of semiconductor and integrated circuit manufacturing plants. The traditional method used for washing the surface contaminants of silicon wafers is the wet cleaning method. The method is to use various acid and alkali solutions and deionized water to treat silicon crystals under different mixing ratios. The wet cleaning method is more dangerous to personnel and there will be waste liquid. Therefore, the dry cleaning method is gradually replacing the current use in the semiconductor and integrated circuit industry. Wet washing method. The dry washing methods that have been developed include low-energy ion splashing, low temperature plasma, peroxidation treatment, steam phase washing and supercritical or subcritical fluid washing methods, in addition to simplifying the current semiconductor washing steps, It can also avoid the disadvantages of waste liquid generation and personnel hazards of the wet washing method, which can increase productivity and reduce production costs. Supercritical fluids (such as carbon dioxide or water) are fluids formed by carbon dioxide or water above their specific critical temperature and critical pressure. Subcritical fluids (such as carbon dioxide or water) are fluids formed by carbon dioxide or water at temperatures above their specific critical temperature but below critical pressure. The method of using supercritical or subcritical fluid to wash the silicon crystal pattern is to use supercritical or subcritical fluid to have liquid-like high solubility and gas-like diffusion coefficient and viscosity, so it can quickly penetrate into the cracks of the human wafer Boundary layer (bmmday h! Yer l'ilms), removes the impure organic or inorganic contamination in the wafer, and the supercritical fluid and the secondary fluid are converted during the conversion, because ------ 1-si « C Please read the precautions on the back before filling out this page) Printed and burned by the Employees Consumer Cooperative of the Central Standard Falcon Bureau of the Ministry of Economic Affairs

Biani CNS) Λ4 Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs 318 ί 51 5. Description of the invention (2) High pressure changes to low pressure, so the fluid will expand and the flow rate will increase rapidly, then it can be dissolved into it A large amount of contaminants are carried away from the silicon wafer, so the impurities on the silicon wafer can be removed. The supercritical or subcritical fluid washing method of the invention has the characteristics of wet washing method, the liquid penetrates into the cracks of the silicon wafer to dissolve and take away impurities, and after adding a small amount of polar modifier, it can also have the washing The function of washing inorganic and organic impurities also has the advantages of the simple dry washing method and the high compatibility of online use. In addition, this method requires less fluid volume, fast washing, and does not pollute the environment. It is believed that it will be the main method of silicon wafer washing in the future. Based on safety and environmental considerations, carbon dioxide or water is currently the most widely used as the object of supercritical or subcritical fluids, and its characteristics are described as follows: (1) Carbon dioxide chooses carbon dioxide as a supercritical or subcritical fluid because supercritical or The second carbon dioxide fluid has very low viscosity, high diffusion coefficient and low surface tension, and is inexpensive and safe. The critical temperature Tc of carbon dioxide is 31 ° C. The critical pressure Pc is 73atm. When it approaches its critical pressure, its density will increase rapidly. For example, the density of carbon dioxide under general pressure is 0.002g / cm3, while the supercritical carbon dioxide fluid The density is 0.4 ~ 0.9g / cm3, and the solubility and density (called solvent strength) at this time are comparable to commonly used organic solvents. At the same temperature, different solvent pressures can be changed to obtain different solvent strengths. The conversion between columnar supercritical and subcritical carbon dioxide fluids can increase soil cleaning efficiency. However, due to the supercritical or subcritical gasification of carbon dioxide fluid, the ring is very late: the solubility of the dye is poor, so it is often (please read the precautions on the back before filling this page)

Wooden paper wound κ 度 通; π 屮 闲 W i ', 〆 Printed by the Central Bureau of Economic Affairs Employee Consumers ’Cooperative-318151 _B7_ V. Description of the invention (3) Some polar modifiers (such as hydrogen peroxide and water, etc.) will be added ), These modifiers not only increase the polarity of supercritical or subcritical carbon dioxide fluids, but also oxygen (the surface of silicon wafers, and can dissolve organic contaminants, so add polar modifiers in supercritical or subcritical carbon dioxide fluids) It is a good way to enhance the solvent strength to improve the washing efficiency. (2) Since supercritical or subcritical carbon dioxide fluids in water do not have polarity, even if polar modifiers can be added to increase its polarity, the increased polarity has a certain limit Therefore, it is impossible to effectively wash highly polar substances, so it is of great help to develop supercritical or subcritical fluids with large polarity changes (that is, from polar fluids to nonpolar fluids), while supercritical or subcritical An example is water fluid. The critical temperature of water is 374 X: and the critical pressure is 227 atm. Supercritical or subcritical water fluid can be changed by temperature and pressure Adjust its dielectric constant. The larger the dielectric constant, the greater the polarity. The smaller the dielectric constant, the lower the polarity. The dielectric constant of water at normal temperature and pressure is 80, and with the temperature and pressure When it is increased, the dielectric constant will gradually decrease. For example, at 250 and 50 bar, the dielectric constant of water is 27, and the dielectric constant of supercritical water fluid is 1 ~ 10. Therefore, supercritical water fluid can be used Non-polar to polar contaminants can be washed 'and general supercritical fluids cannot wash such a wide range of contaminants'. Because the critical temperature and critical pressure of supercritical water fluids are quite high, high-heat steam will It is difficult to disassemble and unload the washing device. Therefore, it is necessary to design a high-temperature steam discharge pipeline. In addition, there must be no gas in the supercritical or subcritical water fluid to prevent the pipeline of the device from being corroded. In the water (please read the notes on the back before filling this page)

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The Printing Disaster of the Employee Consumer Cooperative of the Central Bureau of Samples of the Ministry of Economic Affairs 318151 " V. Description of Invention (4) Oxygen blowing. The object of the present invention is to provide a method and device for cleaning contaminants on the surface of a silicon wafer using supercritical or subcritical fluids. The present invention is characterized by adding a suitable modifier to a supercritical or subcritical fluid to enhance the solubility of the fluid to polar contaminants and enhance the fluid's detergency. Another feature of the present invention is that a washing tank is designed in the washing device, so that several complete silicon wafers can be put in to improve the washing efficiency. The method of the present invention can change the dissolution strength of supercritical or subcritical fluids by the change of pressure, thereby affecting the solubility of pollutants in the fluid to improve the washing efficiency; the increase in temperature, especially when the temperature is above 100 ° C Contaminants with strong silicon wafer bonding will have the effect of thermal desorption and can also improve the washing efficiency: the washing time is also a factor that affects the washing efficiency. If a quantitative supercritical is passed into the washing tank Or sub-critical fluid washing, which means static washing, after more than a certain time, the contaminants that have been washed out may return to the silicon wafer. Finally, the contaminants will be supercritical or subcritical Balance between fluid and silicon wafer: If the supercritical or subcritical fluid is continuously flowed through the washing tank, which means dynamic washing, the contaminants that have been washed out will not return to the silicon wafer. However, dynamic washing may not be able to wash the contaminants hidden in the fine cracks of the silicon crystal pattern, and may use excessive amounts of supercritical or subcritical fluids. Therefore, the present invention adopts a combination of static and dynamic washing methods to simultaneously Make two parties Advantages "· In the following, the following embodiments will be used together with a table diagram to explain the invention in more detail: · 1 if '： ί · ^ I (NS i,; (please read the precautions on the back and then fill in this page )

The Ministry of Economic Affairs, Central Standard Falcon Bureau Employee and Consumer Cooperative Indy Van A7 318151 B7 V. Description of the invention (5) Brief description of the drawings: Figure 1 shows the device for washing silicon wafers using supercritical or subcritical water fluid Schematic diagram: FIG. 2 is a schematic diagram of the device for washing silicon wafers using supercritical or subcritical carbon dioxide fluid according to the present invention: FIG. 3 (a) is a diagram of the present invention which can carry a plurality of complete silicon wafers Sample holder: Figure 3 (b) shows a schematic diagram of a laundering tank that can carry a plurality of complete silicon wafers according to the present invention; Figure 4 shows a schematic view of the laundering tank used in Embodiment 1 of the present invention Figures, Figures 5 to 7 show the results of the first embodiment of the invention to add various modifiers to the supercritical carbon dioxide fluid washing results; Figure 8 (a) shows the second embodiment of the present invention, has received Scanning electron microscope observation of aluminum contaminated silicon wafers. Figure 8 (b) shows the second embodiment of the present invention. The sand wafers after being washed with pure supercritical carbon dioxide fluid under the scanning electron microscope Observation diagram: Figure 9 (a) shows the actual In the second example, the observation diagram of the silicon wafer contaminated with aluminum under the scanning electron microscope: Figure 9 (b) shows the example 2 of the present invention. The silicon wafer after the critical carbon dioxide fluid is washed in the scanning type: j: the observation country of the microscope K: The circle 10 (a) shows the third embodiment of the present invention. The silicon wafer is used more (please read the back side first Matters needing attention and then fill out this page) ------------- Order --- i. Recognize K degrees as appropriate '!, Min Biao Biao Ping (r,' s 318151 Central Standard of the Ministry of Economic Affairs Printed by Jubei Consumer Cooperative Society ^ V. Description of the invention (6) Examination of the low-pressure supercritical carbon dioxide fluid under the scanning electron microscope before washing: Figure 10 (b) shows the third embodiment of the invention, silicon The wafer is washed with a lower pressure supercritical carbon dioxide fluid and then observed under a scanning electron microscope: Figure 11 (a) shows the third embodiment of the present invention, the silicon wafer uses higher pressure supercritical carbon dioxide The observation diagram under the scanning electron microscope before the fluid is washed; and Figure 11 (b) shows the third embodiment of the present invention. The circle is observed under a scanning electron microscope after being washed with supercritical carbon dioxide fluid at a higher pressure: Figure 12 shows the observation diagram of the original silicon wafer under the atomic force microscope in the fourth embodiment of the present invention; Figure Π Shown is the inspection diagram under atomic force microscope of the original silicon wafer treated with hydrofluoric acid aqueous solution in the fourth embodiment of the present invention; Figure I4 shows the original silicon wafer treated with hydrofluoric acid in the fourth embodiment of the present invention The observation diagram under the atomic force microscope after the aqueous solution treatment; Figure 15 shows the observation diagram of the silicon wafer contaminated with aluminum under the atomic force microscope in the fourth embodiment of the present invention: Figure 16 shows the embodiment of the present invention Fourth, after adding 〇.im. (Water supercritical carbon dioxide fluid washed after observation under an atomic force microscope; FIG. 17 shows the fourth embodiment of the present invention, after adding 〇.im (water super Critical: Zi 1 seven-carbon fluid: successively; l [(observation under sub-force microscope -------- ^ 9 · ^ ----- ^ — 11 ^ ----- w (please Read the precautions on the back before filling out this page) The size of this paper is suitable for Chuanzhong (戤 Min 孓. Dagger (OS))) Employee consumption cooperation of the Central Government of the Ministry of Economy Du Yin ¾ A7 318151 B7 — V. Description of the invention (7) Figure ° As shown in Figure 1, in the present invention, supercritical or subcritical dioxygen (carbon carbon fluid is used to wash silicon) In the wafer device, a stainless steel tube 2 is inserted into a cylinder containing liquid carbon dioxide 1, and the liquid carbon dioxide is drawn out through a filter 4, and the liquid carbon dioxide is sent to the liquid pump 5 through the stainless steel tube 3 to receive pressurization, and then enter A supply box 6 is heated to achieve supercritical or subcritical. Then, the supercritical or subcritical carbon dioxide fluid that has been supercritical or subcritical will be made of stainless steel or polyetherether copper lining stainless steel material (Polyether ether ketone) made of multiple high-pressure laundering tank 7 complete silicon wafers for laundering, the supercritical or subcritical carbon dioxide fluid after laundering will be made by polyether ether ketone The corrosion-resistant and oxidation-resistant pipeline 8 enters the restrictor 9 for pressure relief, and then passes through the capillary 10 to be transferred into the collection bottle 11 and is collected in the collection solvent 12. As shown in FIG. 2, in the device for washing silicon wafers using supercritical or subcritical water fluid in the present invention, a stainless steel tube 2 is inserted into a container containing liquid high-purity water 1, and the liquid high-purity water is drawn through The stainless steel pipe 2 and the pump valve 3 enter the liquid pump 4 for pressurization. The liquid pump 4 is driven by an air compressor 5. The pressurized fluid is sent to the pre-cooked oven 10 via the three-way valve 6 and Preheat to 10 (TC, then transfer to the high temperature oven H through the switching valve 9 and use the preheating coil 13 to heat to the set temperature to make the water flow supercritical or sub-beep, the function of the switching valve 9 In order to control the switching between static and Xian state washing, the critical or subcritical water fluid will be connected to the standard \ Made by: Nomura: Gangmura quality or polyether K ® lined with stainless steel (please read the notes on the back first (Fill in this page again)

： · Ν ίί-ΐ- (C'NS) \:; i) ^ " Λ7 313151 " 1 B7 Printed by the Employees ’Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs ¾ V. Invention Instructions (8) Into the sink 12 In order to perform washing of multiple complete silicon wafers, the water after washing is controlled by the three-way valve 14 and enters the restrictor 15 for pressure relief, and then enters the collection bottle 17 through the capillary tube 16 and is collected in the collection solvent 18 in. The high-purity liquid nitrogen 8 is filtered by the filter 7 to wash the device pipeline, and the gaseous carbon dioxide 19 is used to drive the switching valve 9. In addition, the liquid carbon dioxide 20 is quickly cooled by the control of the on-off valve 21淸 洗 槽 12. After the washing operation is completed, the fluid in the washing tank 12 can be discharged via the three-way valve 14 to facilitate disassembly. Example 1 A plurality of silicon wafers of lxlcm2 were first immersed in a 1:50 solution of hydrofluoric acid for 30 seconds, then rinsed with deionized water and immersed in each metal standard solution of 100 Ppm for 2 minutes. Rinse with deionized water and blow dry with nitrogen to become a control sample. Place the control sample in the washing tank as shown in Figure 4 and place it in the device of the present invention (as shown in Figure 1), and then use supercritical carbon dioxide fluid (pressure 3000psi, temperature 80) with various modifiers added ° C., Static washing time of 10 minutes, dynamic rinsing time of 10 minutes, modifier added in an amount of 0.1 mL) for washing, and after completion, take out the more wafers to become a clean sample. The modifiers used in this example are water, hydrochloric acid + hydrogen peroxide, hydrogen peroxide, chlorine oxychloride 'nitric acid, ammonium hydroxide' nitric acid + phosphoric acid and ethylenediaminetetraacetic acid (EDTA), potassium hydroxide. Each silicon wafer uses static secondary ion mass spectrometry before and after washing (instrument model CAMECAims-4i ', primary ion source Ο, acceleration voltage 12.5KV, impact energy 1 SLV, primary current 50pA, mass resolution ~ 3 () ()) Measurement, each piece is randomly taken at three points for measurement, and divided (please read the precautions on the back before filling this page) -------------- Installed ------ ordered .----- ^ It is suitable for printing papers (CNS) · ,, Printed by the Shell Industry Consumer Cooperation of the Central Standards Bureau of the Ministry of Economic Affairs • " 1- '* ·' 'T ^. 318151 V. Description of the invention (9) Do not average the silicon element after correction, the value obtained is the relative pollution amount.

S As shown in Figures 5 to 7, it is the result of using the method of this embodiment to clean the silicon wafer by adding supercritical carbon dioxide fluid with different modifiers, as can be seen from the figure, except that the modifier is using ammonium hydroxide In addition to the poor cleaning effect, the cleaning effect of other modifiers has good performance. This is because under this cleaning condition, ammonium hydroxide will cause crystallization in the cleaning tank and remain on the silicon wafer. "On" if considering the purity and corrosiveness of the modifier, water is the best choice. Example 2 A lxlcm2 silicon wafer was subjected to the same procedure as in Example 1, except that the silicon wafer was immersed in a lOOppm aluminum metal standard solution for 1Ό minutes. And use pure supercritical carbon dioxide fluid (3000psi, temperature 80 ° C, static washing time 5 minutes, dynamic washing time 20 minutes) to… wash silicon wafers. Figure 8 (a) is an observation diagram obtained by using a scanning electron microscope to contaminate the aluminum metal impurities on the surface of the silicon wafer before washing, and Figure 8 (b) is the aluminum metal on the surface of the silicon wafer after washing Observation of the scanning electron microscope of the contamination of impurities. 'Comparison of the two figures shows that the washing efficiency of pure supercritical carbon dioxide fluid is not good, but when the added water is a modifier, it is shown in Figure 9 (a) Observation diagram obtained by using a scanning electron microscope to contaminate aluminum metal impurities on the surface of the silicon wafer before washing and Figure 9 (b) of the sand table after washing, and scanning electron microscope observation diagram of aluminum metal contamination ， It can be clearly seen from the comparison of the two pictures that it has a superior cleaning efficiency (please read the precautions on the back before filling this page)

Α7 318151 Β7 Ministry of Economic Affairs, Central Standard Falcon Bureau Beigong Consumer Cooperative Printing Disaster 5. Invention Description (1 ()) Embodiment 3 This embodiment is based on the supercritical fluid being a high-pressure fluid, which may cause image structure on the surface of the silicon wafer Damage, so the silicon wafer was subjected to the procedure as in Example 1, but not immersed in a metal standard solution, and pure supercritical carbon dioxide fluid (pressure 3000 psi, temperature 80 ° C, static washing time 5 minutes, dynamic washing) Time 20 minutes) Wash the silicon wafer. Before and after washing, the scanning electron microscope as shown in Example 2 was observed on the surface of the silicon wafer. The results are shown in Figure 10 (a) and Figure 10 (b), respectively. Repeat the previous procedure, but increase the pressure of the pure supercritical carbon dioxide fluid to 5000 psi, then the observation results of the scanning electron microscope before and after washing the wafer surface are shown in Figure 11 (a) and Figure 11 respectively (b) As shown in the figure. It can be seen from Figure 11 (a) and Figure 11 (b) that part of the structure on the surface of the silicon wafer has been destroyed after washing, and from Figure 10 (a) and 10 ( b) The figure shows that there is no such damage on the silicon wafer. This may be due to the high flow rate generated by the pure supercritical carbon dioxide fluid at a higher pressure, which forms a turbulent flow in the wash tank, resulting in uneven stress on the structure on the silicon wafer. It can be seen from the embodiment that the pressure of the supercritical fluid is not suitable to be too high 'so as not to damage the structure of the silicon wafer. Example 4 In order to understand the changes in surface topography of silicon wafers before and after washing with supercritical carbon dioxide fluid and the washing efficiency of pollutants in deep trenches, we sought a piece with both flat and deep trench structures (about 1 011 m ) The observation of the silicon wafer Lili Atomic Force Microscope as shown in Figure 12 'Hydrogen fluoride (please read the precautions on the back before filling in this page) © 装 — I 丁 n L: ii J' * mf tm · A7 B7 Economy Printed by the Central Committee of the Ministry of Internal Affairs and Social Security 3 18151 V. Description of the invention (u) After etching with an aqueous acid solution as shown in Figure 13, two different structures can be observed. The yellow area in the figure represents no pollution. The silicon surface of the object, the red area represents the silicon surface containing contaminants (aluminum metal contaminants or natural oxides or silicon dioxide). Atomic force microscope was used to observe the surface morphology of this silicon wafer before and after aluminum metal contamination and supercritical carbon dioxide fluid (washing conditions are the same as in Example 2) after adding a small amount of water as a modifier. From the series of atomic force microscope observation results in Figures 14 and 15, it is known that there is indeed aluminum metal contamination covering the surface of the silicon wafer. After washing, the image is like the flat structure part of Figure 16 and the depth of Figure 17 As shown in the structure part, most of the pollutants are washed away; it can be seen that the supercritical fluid washing method can not only wash the pollutants on the surface of the flat structure, but also penetrate the fine deep trench to wash the pollutants out. It is difficult to achieve with the traditional wet washing method. Because the surface tension of the liquid is greater than that of the supercritical fluid, it cannot effectively penetrate deep and fine trenches to wash away pollutants. Although the present invention has been disclosed above with more expensive examples, it is not intended to limit the present invention. Anyone who is familiar with this skill can make some changes and retouching without departing from the spirit and scope of the present invention, so The scope of protection of the present invention shall be subject to the scope defined in the attached patent application. (Please read the notes on the back before filling this page)

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Claims (1)

Japan) No. 83 56 applied for the patent scope amendment too A8 B8 C8 D8 318151 Amendment date: 86/04/0? Patent application scope 1. A method for washing the surface contaminants of silicon wafers by using supercritical or subcritical fluids. A supercritical or subcritical fluid with a modifier added will be used to clean the contaminant impurities on the surface of the silicon wafer by a static method and a dynamic method; wherein the modifier is selected from the group consisting of water, ethylenediaminetetraacetic acid, hydrogen peroxide, and hydrogen A combination of potassium oxide, ammonium chloride, nitric acid, hydrochloric acid and hydrogen peroxide, and nitric acid and phosphoric acid, and the pressure of the supercritical or subcritical fluid is less than 5000 psi. 2. The method as described in item 1 of the patent application scope, wherein the supercritical or subcritical fluid is a supercritical or subcritical carbon dioxide fluid. 3. The method as described in item 1 of the patent application scope, wherein the modifier is water. 4. The method as described in item 1 of the patent application scope, in which the supercritical or subcritical fluid can enhance its solvent strength by adjusting the temperature and pressure to improve the washing efficiency. 5.-A method for cleaning contaminants on the surface of silicon wafers by using supercritical or subcritical fluids, which uses supercritical or subcritical water fluids to clean contaminants on the surface of silicon crystals by a static method and a dynamic method Impurities. 6. The method as described in item 5 of the patent application scope, in which the supercritical or subcritical water fluid can enhance its solvent strength by adjusting the temperature and pressure to improve the washing efficiency, Or a subcritical carbon dioxide fluid device for washing contaminants on the surface of silicon wafers, including a washing tank in which a plurality of complete silicon wafers can be placed. A liquid pump and an oven are provided in front of the washing tank to- Liquid carbon dioxide is pressurized and heated to a specific pressure and a specific (read the precautions on the back before filling out this page) Binder •• ί ··,---- ίνν- · ί thread --- Μ Α8 Β8 C8 D8 318151 6. The temperature in the patent application range allows the liquid carbon dioxide to be supercritical or subcritical. The supercritical or subcritical carbon dioxide fluid will then pass through the laundering tank to perform the plural pieces of complete silicon Washing of contaminants on the wafer surface. 8. The device as described in item 7 of the patent application scope, in which-a flow restrictor is provided after the wash tank to relieve pressure of the supercritical or subcritical carbon dioxide fluid after the wash, in the flow restrictor A collection bottle is provided afterwards, which contains a collection solvent to collect the supercritical or subcritical carbon dioxide fluid after pressure relief. 9. The device as described in item 8 of the patent application scope, wherein the wash tank is made of stainless steel or stainless steel lined with ether ether ketone. 10. A device for washing contaminants on the surface of silicon wafers using supercritical or subcritical water fluids, including a washing tank, in which a plurality of complete silicon wafers can be placed, and a liquid pump is installed in front of the washing tank It is used to pressurize a water fluid to a specific pressure, a preheating oven is used to preheat the water fluid, an oven then heats the water fluid to a specific temperature to make the water fluid supercritical or subcritical The supercritical or subcritical water fluid will then pass through the wash tank to wash the surface contaminants of the plurality of complete silicon crystal patterns. 11. The device as described in item 10 of the patent application, wherein a switching valve is provided in the preheating oven to switch the supercritical or subcritical water fluid through the laundering tank to perform the plural pieces The dynamic and static cleaning of contaminants on the surface of a complete sand wafer, the switching valve is driven by gaseous carbon dioxide. 12. The device as described in item 11 of the scope of patent application 'one of the current limit n / 1- n-m _ 丁 · ^ 农-. · I ----, 1τ ------. v > (please read the precautions on the back and then fill out this page) 姥 济 祁 中央 榮 局 Mu consumption Cooperative Society Print ¾-318151. MU _ 品 ._ 6. The patent application scope is installed after the wash tank to release the pressure of the supercritical or subcritical water fluid after the wash, and also in the flow restrictor Then set up a collection bottle, which contains-collect solvent to collect the supercritical or subcritical water fluid after pressure relief 1 3. The device as described in item 12 of the scope of patent application. Among them, high-purity if liquid nitrogen is used Wash residues in the pipeline of the device < M. The device as described in item 13 of the patent application scope, one of which is liquid :: Carbon oxide is used to quickly cool the wash tank. 15. The device as described in item 14 of the patent application scope, in which the washing g is made of stainless steel or stainless steel material lined with ether ether ketone, please read the precautions on the back and then fill out this page) —install- -Booking line ----