TW200401883A - A method and apparatus for monitoring liquid levels within a vessel - Google Patents

Abstract

A method and apparatus for monitoring liquid levels within a vessel, particularly the level of an organometallic compound within a bubbler. A metallic probe is hermetically sealed within a mounting that is sealed within a mounting that is sealed within the port of the vessel. The part of the probe that is sealed within the mounting is made of a nickel alloy and encased in a glass material by a metal to glass matched seal. The method comprising the steps of inserting at least one metallic probe into a vessel to act as a first electrode, hermetically sealing the probe within the vessel, providing a further electrode to form a capacitor, applying an electric current to the capacitor and monitoring the capacitance thereof.

Description

200401883

V. Description of the invention (1) [Technical field to which the invention belongs] The present invention relates to a device and method for monitoring the liquid level in a container, and particularly to a water level probe for monitoring a chemically reactive liquid in the container, such as an organometallic compound. ; Insert at least one probe into the container to serve as the first electrode, and seal the probe in the container, and set a second electrode as a capacitor, and then supply a capacitor current to monitor its capacitance. [Previous technology] In the electronics and optoelectronic industries, _ · 一, u μ π is difficult; metal chemical vaporization method produces a layer of metal thin film on its solid bottom layer, usually the metal precursor is transferred to the bottom layer through the container and contains metal The bubbler of the precursor material has an inlet tube, an immersion tube, and an outlet tube carrier gas, such as hydrogen helium. Nitrogen is introduced into the bubbler through the inlet tube, and then transported to the bottom of the bubbler through the immersion tube. Before the carrier gas escapes the bubbler through the outlet pipe, it can obtain = some of the vapors of the metal precursors, and this precursor vapors will be transferred to a reactor, the precursors will be decomposed to produce on the solid bottom layer; House. In addition, the content of the precursor material in the bubbler will not be corroded with the use of the device. The probe of Γ cannot be used, because the organometallic compound: the point measurement method can be used to measure the drive system. The upper and lower positions are measured, and then the precursors in the container are measured for rupture and gas'; bf: 'It is a glass tube, and the glass tube may look at the water level indication; the container' bubbler can also be used without precision The calculation of time; when the energy is reduced or according to special circumstances, the bubble can be replaced, but this will cause the

200401883 V. Description of the invention (2) There may still be a bubbler in the container. Obviously, the container contains high strength and toughness. In this case, the reaction is' so that the gas can not be damaged. The person is susceptible to air. People are aiming at the above invention. . [Summary of the invention] The liquid in the measuring container of the present invention is used to overcome or I The water level of the chemical compound in the measuring container of the present invention is as described above. When the material of the hundredth to the tenth of the present invention can be used, the method of replacing the vehicle and the bridge is too early. The method is to set an accurate probe to monitor the machine metal < Water level; however, the probe must be set and U 4, and the organometallic compounds that are in contact with each other must be compatible. The needles must not affect the chemicals contained in the bubbler. π "W purity metal precipitate, in addition, the probe is also hermetically sealed, because the material contained in the bubbler and the pressure must be maintained; therefore, the lack of 'intensive research, design, and The main purpose of the present invention is to provide a device that can continuously monitor the water level of the body, especially an organometallic compound, which reduces the disadvantages of conventional conventional equipment. Another object is to provide a method that can continuously learn the water level of liquids, which is an organic gold; to overcome or at least reduce the shortcomings of conventional methods. The first object of the present invention is to provide a device, a body water level, which includes at least one device enclosed in a trough to serve as a first electrode, and another-: forming an electric valley, and then setting an electronic control device With k and a monitoring device to monitor capacitors, the second goal is to provide a way to monitor the capacity:

Page 7 20041883 V. Description of the invention (3) if cube 2; the steps are: seed at least one probe into the first electrode of the container field, seal the probe in the container, and use the & electrode as a capacitor , Then supply capacitor current and monitor its power. It is important to note that the two separate electrodes are provided in order to change the capacitance of the capacitor formed in its dielectric. In this case, the amount of water in the container varies between the needles, so the liquid in the container can be monitored. The filling container is a metal container, such as stainless steel, and = and Γ two electricity: the two parallel probes are sealed in the device; long rod or plate probe is better.疋 Hollow or solid’is made of stainless steel. The probe of the present invention is particularly suitable for monitoring the water level of the organometallic compound. The probe is best combined with the opening at the top of the container. = An inlet tube and an outlet tube are provided. „:% Is taken with a glass seal in — 田 ～ 产 上 f in the opening of the joint, more preferably, the opening of the prober is: ίϊί :, and the fixed seat or cover is set in the container. J ^ Plug-in BNC plug. 、 The probe is made of rubber. At least a part of the extension from the mouth to the bottom can be coated with a coating such as Teflon. Covered and sealed The probe in the broken glass material is preferably at least _ part containing page 8, 20041883. V. Description of the invention (4) 70% of the nickel alloy, and the precipitate of the alloy is added with aluminum and / or Titanium can be hardened afterwards. Suitable alloys of this type include those sold on the market under the trade name Inconel χ_75〇, Inconel 60 0 or FeNiCo. Among them, Nichrome χ_75〇 is the best, sealed The glass of some probes is preferably collarate silicate glass, which is more suitable for Needle with seal 0 The glass material is then sealed in a fixing seat, and the fixing seat preferably contains a nickel alloy, such as nickel-chromium alloy χ_7 5 0, and the fixing seat is preferably provided with a gasket surface seal in combination with its joint surface and inner surface Accessories, such as a "profile of a ruler" to facilitate the assembly of electrical connectors and the seal between glass and metal. The gasket is preferably a gasket that can be deformed when tightened to facilitate the fixed seal between metal and electrical connector. It is best to be covered with a layer of insulating material, such as polyetheretherketone (PEEK). Traditional devices refer to AC or DC power to the probe, and a monitor, such as a capacitance calculator, is used to measure the change in capacitance. It is also best to have a recorder to record the change in capacitance. The recorder can include A display, such as a liquid crystal display, preferably enables the capacitor to be continuously monitored and provides continuous readings with the liquid level. Dare

~ Second ~ 'The blood state device is equipped with a system calibration device to match the special liquid capacity in the special ^ 彳 ^ device. For example, there is no liquid bone in the container, and the capacitance recorded on the recorder can be set to "0 ", And the container $ =, set it to" 100 ", preferably, the monitoring device can be calibrated] In addition to the characteristics of the liquid contained in the container, in addition, the monitoring provides the rate of liquid discharge or addition. Right ^

Page 9 20041883 V. Description of the invention (5) The bubbler in the embodiment of the present invention, the bubbler includes an inlet tube, a metal probe in the valleyr, and an electronic control. Device for measuring the capacitance of a capacitor. [Embodiment] In order to fully understand the present invention, the description is as follows: As shown in the first and second figures, the device can continuously monitor the water level of gaseous substances. The bubbler 2 is provided with a device containing an organic metal compound and a sealed device. A metal container, the metal container is a two-leaf immersion tube, and another is sealed in the container and a probe to form a capacitor, which supplies a capacitor current, and a monitor is a preferred embodiment and illustrates the present invention in conjunction with the drawings. The organometallic compound tube 4 in the container of the water level monitor bubbler 2 of the first embodiment _ enters the immersion tube 6 and an outlet, and the inlet tube 4 and the immersion tube 6 communicate with each other, and a metal bubbler 2 extends through it The center and the entire length of 'the upper end of the probe 10-in the glass layer 12' and sealed at the top of the container to maintain the pressure in the bubbler 2 'and isolate the contents from the outside air and immerse in the bubble W The bottom end of the probe 10 containing the precursor is coated with a non-chemical and heat resistant material such as polytetrafluoroethylene (PTFE) or other synthetic rubber materials, the top of the probe 10 and an electronic control device 14 Connection, the electronics Communication system 14 is provided with a power source and a monitoring device, which monitoring device shown ^ bubbler the liquid level of 2 readings. ^ As mentioned above, the probe 10 can be sealed in the bubbler 2. For a better understanding of the present invention and a clearer indication of how to implement it, please refer to the following examples. The first example is a survey of This invention—implementing a consumer 'and

200401883 V. Description of the invention (6) Measuring the level of trimethylgallium (TMG) in the bubbler 2. The second example is to investigate the use of the same device to measure the level of trimethylaluminum (TMA) in the bubbler 2. An example is investigating the use of a device to measure the level of trimethyl aluminum (TMA) in bubbler 2. The fourth example is investigating the use of a device to measure the level of trimethylgallium (TMG) in bubbler 2. And refer to the attached drawings, where: [Example 1]

A study was performed to prove the ability of the container water level monitoring device in the first embodiment of the present invention to be able to continuously monitor the water level of trimethylgallium (TMG) in the bubbler 2, and the probe 10 described above was sealed in In bubbler 2, when there is no liquid in bubbler 2, the monitor is reset to zero, then dimethylgallium (approximately 180 g = 157 ml) is injected into bubbler 2, and the reading is set to the lowest point, then The material in the bubbler 2 is discharged from the bubbler 2 through the immersion foot and flows into another container. At this time, the water level indicated by Te ietren (iTM continues to be recorded. From this record, it can be known that when the material in the bubbler 2 is During discharge, the reading will drop from 100% to 0%. As shown in the third figure, the slope of the slope in the graph depends on the rate of material discharge. Once all the material in bubbler 2 is discharged, the More material was injected into the bubbler 2 to inspect the monitoring device, and the reading rose from 0% to 100%. [Example 2] A study was performed to prove that the container water level monitoring device in the first embodiment of the present invention can Continuous monitoring of trimethylaluminum (TMA in bubbler 2) ) Of the water level, as described in Example 1, when there is no liquid in the bubbler 2, the monitor connected to the probe 10 is reset to zero, and then three bubbles are injected into the bubbler 2.

200401883 V. Description of the invention (7) ----- Base aluminum (approximately 120 g = 160 ml), and # — After that, the material of the bubbler 2 * flows into the other container through the immersion, responsibility, and two points. Smooth trendTM:;: "The J bubbler 2 came from this record. It can be known from this record that when the bubbler 2 is recorded, it depends on the rate of material discharge. The steepness of the slope in the graph is the fifth and sixth in the figure. Description of the present invention bubbler 2 t probe 10, the probe]. Including one or two inserted and its tail section 22 is sealed in a fixed seat 30 f · 'ice 0,

(Inconel x-7 ^ 〇V iron alloy X-750 has characteristics similar to nickel-chromium-iron alloy 600 precipitates will harden after adding Shao and titanium; sealed in glass material 34. In! Chrome-iron alloy 60 0 has high Heat resistance and high corrosion resistance. This nickel-containing gold can resist the corrosion resistance of many organic and inorganic compounds. This avoids ions stress corrosion cracking of gerbils. Chromium can resist sulfurization and can resist oxidation or corrosion at high temperatures. Solution, and the corrosion of surface purity water, nickel-chromium alloy χ_75〇 has very good resistance to oxygen and southern tensile strength, and it has latent fracture when it is high at 1 300 ° F (700 ° C) > JDL Characteristics. The tail section 22 of the probe 10 made of Inconel X-750 is glass-to-metal: the mating section of mutual cooperation must rely on an oxide layer to seal the metal to glass, so glass with the same thermal expansion coefficient must be used. Tritium and metal can make glassy

200401883 V. Description of the invention (8) The glass is subjected to the minimum stress during the fusion process. The tantalum soft mother-in-law, Na ^ 7 ferroalloy or iron-nickel-cobalt alloy is best fused with borosilicate glass to seal each other. The probe 10 has a glass-to-metal seal. The tail section 22 is sealed in the fixed seat 30, and the seat 32 of the fixed seat 30 is also made of nickel-chromium alloy χ-750. The SwagelokR VCR profile combined with the semi-English 忖 face and the inner rim is suitable for assembling BNC joints and glass-to-metal seals. The VCR is a type of integrity and seals to the purity of the metal gasket surface. The gasket will be convex by the fitting. The cross section is deformed by compression, and the metal and metal seals are firm. The insulating edge 36 of BNC polyether ether ketone (PEEK) and the electrode connection member 38 are arranged at the top of the tail section 22 of the probe 10 together. [Example 3] Research to prove the ability of the water surface monitoring device in the second embodiment of the present invention to be able to continuously monitor the water level of trimethylaluminum (TMA) in the bubbler 2. The results are shown in FIG. When the bubbler 2 is filled with trimethylaluminum, the calibration stage is 100%. When the bubbler 2 is empty, the calibration stage is 0%. It should be noted that the liquid in the bubbler 2 is filled and extracted. Positive pressure must be used to quickly change the water level. [Example 4] Another study was performed to prove the ability of the water level monitoring device in the second embodiment of the present invention to continuously monitor the trisium gallium (TMG) in the bubbler 2. The process is the same as that described in Example 3, but its The number of calibration levels is decreased from 100% of the reading instead of 0% as described in Example 3. The result is shown in Figure 8.口 The results obtained from Examples 3 and 4 show that in the second embodiment of the present invention

200401883 V. Description of the invention (9) The bubbler 2 provided with the probe 10 can continuously monitor the water level in the bubbler 2 'When the bubbler 2 is: ¾ liquid and drained liquid, it can be shown by the production of the graph Get fast response time. "Also, = provide _ kinds of measuring probes are suitable for monitoring the water level of the liquid contained in the bubbler 2, and the bubbler 2 has strong toughness, and the organometallic compounds are compatible. Therefore, the present '3 bubbler 2 The organic moon is enough to continuously monitor when the material in the bubbler 2 has been used up and needs to be added by the purchaser. The sealer is then sealed in the bubbler 2 ", Mark 2: 4: Probe, combined in-make the bubbler 2 It is easy to suffer, the pressure of A is held on the second side, and the content of the second ring is isolated from the outside air. ™ 9 φ Mountain Moon Dagger temperature does not affect the measurement of the water level and the use of air bubbles Γ; the content 1 is coated with synthetic rubber of the probe 10 does not have a value of 10 tb. Therefore, the purity of the precursor can be maintained. The invention's probe 10 is different than traditional glass probes. When you know that the needle is worried about moving or handling, you should also explore: ::: 重 # 'Especially the nature of the content in the bubble container σ To break 4 otherwise it will be because the gas = sealed in the fixed seat 3 ::; =, =; indicator =, the front driver two r see τ :, put into the organic: it belongs to this and can be shock-resistant when it is lost, even if only one million Eight f: 乂 ", will not pollute the next, it will not be polluted, it is made of the high purity of the knife and has a high integrity test. The second vibration = 10 must be able to reach the water level of the metal precursor of the stainless copper machine = In the bubble state 2), there is a continuous display of kernels.

Page 14 20041883 V. Description of the invention (ί), easy to operate, and reliable and accurate. In addition, the capacitor is set as a fixed seat 30 or a cover seat 30 and an electrical connection device is provided for the probe 10 . In summary, the embodiments of the present invention have indeed achieved the effects, and have not seen the application requirements of the invention patent disclosed by those who have the same characteristics. The probe 10 currently does not have a part of the whole, and it is fixed. This structure is also the first to achieve the expected purpose. Therefore, the present invention can be applied, and I would like to ask for a review of the 200401883. Description] The first figure is a front view of an embodiment of a container water level monitoring device provided with a probe according to the present invention. The second figure shows a cross-sectional view of the probe in the first figure. ^ The third figure is a graph showing the variation of the tritium gallium water level with the measurement time in the bubbler of the container water level monitoring device of the present invention. The fourth figure is a graph showing the variation of the water level of Mikasa Kisho in the bubbler of the container water level monitoring device of the present invention with the measurement time. The fifth figure shows a longitudinal sectional view of a probe in a second embodiment of the present invention. The sixth figure shows a cross-sectional view of the probe in the fifth figure. The seventh figure shows the curve of the water level of trimethyl I in the container water level monitoring device of the present invention as measured with the time measured by the probes shown in the fifth and sixth figures. The eighth figure is a graph of the trisalium gallium water level in the container of the container water level monitoring device according to the present invention as measured with time, as measured by the probes shown in the fifth and sixth figures. [Illustration of figure number] 10 probe 12 glass layer 14 electronic control device 2 bubbler 20 non-steel long tube 22 tail section 30 fixed seat 32 seat body 34 glass material 36 insulation edge 38 electrode connector 4 into V tube 6 dip Rupture tube 8 out D tube

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Claims (1)

200401883 VI. Scope of patent application 1 · A probe, an electrode and a device for the capacitor of the device. 2 · Rushen device, of which 3. Rushen device, 4 · Rushen device, which is sealed in the container 5. Rushen device, of which 6. Rushen device, of which 7 · Rushen device, which seat or cover Middle 8 · Rushen device, of which 9. Rushen device, which is made of rubber. In the monitoring container, the probe is the scope of the patent of the first electrode application capacitor. The scope of the patent of the container itself is the scope of the patent, which is one of the probes. Patent scope, glass material please patent scope 'Probe range is patented, patent scope' Probe is dense. Patent range, 'fixed seat clear patent scope', Probe self-tight liquid level device is mainly provided with at least a seal at The container serves as the first electrode, and is separately opened to form a capacitor; further, an electronically controlled current and a monitoring device to monitor the capacitance of the liquid level in the container described in item 1 is a metal container serving as the second electrode. The liquid level in the monitoring container described in item 1 or 2 is made of stainless steel. The end of the liquid water level in the monitoring container described in item 1 is sealed in a glass material, and the liquid water level in the monitoring container described in item 4 is borosilicate glass. The liquid level in the monitoring container described in item 4 is sealed in the opening at the top of the container. The liquid water level in the monitoring container described in item 4 is sealed in a fixed position inserted in the container opening. The electrical connector for the probe is provided in the liquid water level in the monitoring container described in item 7. The extension of the liquid level in the monitoring container described in item 1 below the seal is coated with a layer of synthetic 200401883 VI. Scope of patent application _10. The device for monitoring the liquid level in a container as described in item 4 or 9 of the scope of patent application, its towel, a probe sealed in glass, and: nickel alloy. π slave state 11 · The device for monitoring the liquid level in a container as described in item 10 of the scope of patent application, wherein the alloy is a nickel-chromium alloy or an iron-nickel-cobalt alloy. 12. The device for monitoring liquids in a container as described in item 10 of the scope of the patent application, wherein the alloy contains Shao and / or titanium. Taxi 13. The device for monitoring the liquid level in a container as described in item 11 of the scope of patent application, wherein the alloy is nickel-chromium alloy X-750. Taxi 1 4 · Monitor the liquid level in the container as described in item 7 of the scope of patent application, wherein the fixed seat is made of nickel alloy. Taxi 1 5 · Monitor the liquid level in the container as described in item 14 of the scope of the patent application, where the alloy is Nichrome X-750. State 16 · The device for monitoring the liquid level in a container as described in item 1 of the scope of patent application, wherein a monitor is added to monitor the change in capacitance. State 17 • The clothing for monitoring the liquid level in the container as described in item 1 of the scope of the patent application, wherein a recorder is added to record the change in capacitance. State 1 8 · As described in item 1 of the scope of the patent application, the monitor of the liquid level in the container is provided with a display for displaying the liquid level in the container. Taxi 1 9 · As described in item 1 of the scope of the patent application, the device for monitoring the water level in the container is provided with a calibrator for calibrating the monitoring device, so that the special capacitance can meet the special capacity of the liquid in the container. 20 · The device for monitoring the water level in a container as described in item 1 of the scope of the patent application is used to monitor the water pumping of organometallic compounds. Page 18 200401883 VI. Scope of patent application 2 1. The device for monitoring the liquid level in a container as described in item 1 of the scope of patent application, wherein the container is a bubbler. 22. The device for monitoring the liquid level in a container according to item 21 of the scope of the patent application, wherein the bubbler contains an organometallic compound, the bubbler is provided with a sealed metal container, the metal container is provided with an inlet tube, An outlet tube, an immersion tube, and a probe are sealed in the container. The container and the probe constitute a capacitor, an electronic control device is provided to supply the capacitor current, and a monitor is used to measure the capacitance of the capacitor. 23. A method for monitoring the level of liquid in a container, the method includes the steps of inserting at least one probe into the container as a first electrode, sealing the probe in the container, and setting a second electrode as a capacitor , Then supply capacitor current and monitor its capacitance. Page 19