KR20090014798A - Infrared ray spectroscopy analyzer for in-situ diagnostics of the process - Google Patents

Abstract

An infrared spectrometer capable of performing real-time process diagnosis is provided to perform spectrum analysis in a vacuum state using infrared rays to correctly measure beam intensity to thereby improve measurement sensitivity. An infrared spectrometer capable of real-time process diagnosis includes an incident window(11), a receiving part(12), a projecting window(13), a reactor(10), a detector(20), and an analyzer(30). A beam is inputted to the incident window. The receiving part receives the incident beam. The projecting window projects a beam obtained when the incident beam is refracted and scattered according to reaction by-product or reactant. The reactor includes a reflecting mirror(14) and has a vacuum state. The reflecting mirror reflects the beam inputted to the incident window such that the beam reciprocates in the receiving part at least once and is projected through the projecting window. The detector detects the beam projected from the reactor. The analyzer performs quantitative and qualitative analysis of a sample by using the intensity of the detected beam.

Description

Infrared Ray Spectroscopy Analyzer for In-situ Diagnostics of the Process

The present invention relates to an infrared spectrometer capable of real-time process diagnostics, and more particularly, to quantitatively and qualitatively analyze a reaction byproduct or a reactant by measuring a beam emitted from the reaction by-product or reactant in a vacuum state. The present invention relates to an infrared spectrometer capable of real-time process diagnosis.

Every atom or molecule is constantly moving in space and contains the corresponding energy. These energies, related to the motion of atoms or molecules, are quantized, so they can always exist in a particular energy state. Atoms or molecules that are moving in a particular energy state can absorb energy from the outside and rise to a higher energy state. When energy is expressed as a wave, E = hv. Where h is the Plank constant and v is the frequency. Therefore, the energy ΔE = h (V 2 -V 1) = h · Δv required to be excited to a higher energy state. Since h is a constant, the energy needed to lift an atom or molecule is a function of frequency only, and the spectrum that appears when an atom or molecule absorbs some energy is a function of frequency. The energy state of an atom or molecule depends on the type of motion and, as a result, the amount of energy it can absorb. Among them, there are vibrations, rotations, and translational movements of the molecules corresponding to the energy of the infrared region. Particularly related to infrared spectroscopy are transitions due to vibrations and rotational movements. In general, the energy required for vibration has a larger value than the energy required for rotation. The motion corresponding to the mid-infrared region, which is most commonly used among the infrared regions, is mainly a vibration movement. Therefore, infrared spectroscopy is a device analysis method that can obtain information about the vibration-rotational motion of molecules by using light sources that can emit light in the infrared region, to check the structure of the molecules and perform quantitative analysis.

Conventional infrared spectroscopic analyzers quantitatively and qualitatively analyze the reaction by-products or reactants by scanning the beam by scanning the beam to the reaction by-products or reactants received at atmospheric pressure.

As such, the conventional infrared spectrometer is spectroscopically analyzed under atmospheric pressure, so it is difficult to accurately spectroscopicly analyze the reaction byproduct or the reactant, and the reaction byproduct or the reactant is absorbed by the incident window where the beam is incident, the exit window where the beam is emitted, and the reflection mirror. There was a problem that the deposition is not properly delivered beam.

When the reaction by-products or reactants are adsorbed and deposited on the entrance window, the exit window, and the reflection mirror, the maintenance is performed by disassembling and cleaning them. This maintenance cycle is short, which makes it difficult to diagnose in real time.

The present invention has been made to solve the above problems, and an object of the present invention is to provide an infrared spectrometer capable of real-time process diagnosis by performing a spectroscopic analysis in a vacuum state. You can also tell the equipment check interval (PM cycle) by monitoring the gas coming out of the reactor during process shutdown.

In addition, another object of the present invention is infrared spectroscopy capable of real-time process diagnostics to enable accurate spectroscopic analysis by preventing contamination by reaction by-products or reactants adsorbed and deposited on the entrance window and exit window, reflection mirror, crystal, etc. To provide an analyzer.

It is still another object of the present invention to provide an infrared spectrometer capable of real-time process diagnosis to extend the maintenance cycle by reducing the pollution degree by adsorption and deposition.

Infrared spectrometer capable of real-time process diagnosis of the present invention for achieving the above object is a real-time process of the incident window 11, the beam is incident, the beam incident to the incident window 11 is incident and the reaction by-product or reactant Receiving unit 12 temporarily accommodated for diagnosis, the exit window 13, where the beam incident in the receiving unit 12 is refracted and scattered by the reaction by-product or reactant is emitted, and the receiving unit (12) a reflection mirror 14 mounted inside and reflecting the beam incident to the entrance window 11 so as to reciprocate the inside of the receiving portion 12 at least once and exiting to the exit window 13; A reactor 10 in which the inner vacuum is added; A detector (20) for detecting the refraction and scattering of the beam emitted from the reactor (10); An analyzer 30 analyzing the qualitative and quantitative analysis of the sample using the detected beam intensity; Characterized in that comprises a.

In addition, the receiving portion 12 of the reactor 10 is characterized in that formed in a zigzag flow path.

In addition, the reactor 10 is characterized in that the pressure regulator 15 for adjusting the pressure in the reactor is further provided.

In addition, reaction by-products or reactants are adsorbed and deposited on the incident window 11, the exit window 13, or the reflection mirror 14 by the entrance window 11, the exit window 13, or the reflection mirror 14. It is characterized in that the air curtain 16 for injecting nitrogen gas (inert gas) is further provided to prevent it.

In addition, the reactor 10 is characterized in that the temperature can be adjusted.

In addition, the reactor 10 is further provided with an inlet 17 for injecting a gas or liquid to clean the sample adsorbed and deposited in the entrance window 11, the exit window 13 and the reflection mirror (14). It is characterized by.

In addition, an infrared spectrometer capable of real-time process diagnosis according to another embodiment of the present invention includes an incident window 111 into which a beam is incident and a beam incident into the incident window 111 is incident and a real time process diagnosis of a reaction byproduct or reactant is performed. Receiving portion 112 temporarily accommodated to be possible, and the fixed beam in the receiving portion 112, the incident beam is refracted and scattered by the reaction by-product or reactant incident and at least once inside A crystal 114 for reciprocating emission, a plasma electrode 115 spaced around the crystal 114 and providing continuous radiation in the far infrared region, and an emission for emitting a beam emitted from the crystal 114 A reactor 110 including a window 116, the interior of which is vacuumed; A detector (120) for detecting the refraction and scattering of the beam emitted from the reactor (110); An analyzer 130 for analyzing the qualitative and quantitative analysis of the sample using the detected beam intensity; Characterized in that comprises a.

In addition, the reactor 110 is characterized in that the pressure regulator 117 for adjusting the pressure in the reactor is further provided.

In addition, the cleaning port 118 for injecting nitrogen gas to the crystal 114 and the plasma electrode 115 to prevent the reaction by-products or reactants are adsorbed and deposited is further provided.

In addition, the fixing part 113 is characterized in that the temperature can be adjusted to adjust the temperature of the crystal (114).

In addition, the reactor 110 is an injection hole for injecting a gas or liquid between the crystal 114 and the plasma electrode 115 to clean the sample adsorbed and deposited on the crystal 114 and the plasma electrode 115 119 is further characterized in that it is provided.

In the present invention, since the spectroscopic analysis is performed in a vacuum state using infrared rays, it is easy to analyze the reaction by-products or the components of the reactants by accurately measuring the beam intensity due to the refraction and scattering of the beam, compared to the conventional spectroscopic analysis under normal pressure. There is this. In addition, it is possible to improve the measurement sensitivity by using the multi-pass, and to prevent contamination by the reaction by-products or reactants adsorbed and deposited on the entrance window and exit window, reflection mirror, crystal, etc. The maintenance cycle can be extended by reducing the number of cycles, which allows real-time process diagnosis.

Hereinafter, an infrared spectrometer capable of real-time process diagnosis of the present invention will be described in detail with reference to the accompanying drawings.

1 is a view showing the structure of an infrared spectrometer capable of real-time process diagnosis according to the present invention.

As shown, an infrared spectrometer capable of real-time process diagnosis according to the present invention includes an entrance window 11, a receiving portion 12, an exit window 13, and a reflection mirror 14, and the inside of the apparatus is in a vacuum state. Reactor 10; A detector (20) for detecting the refraction and scattering of the beam emitted from the reactor (10); An analyzer 30 analyzing the qualitative and quantitative analysis of the sample using the detected beam intensity; It is made, including.

The reactor 10 is provided with an entrance window 11, a receiving portion 12, an exit window 13, and a reflection mirror 14, and the inside of the reactor 10 is in a vacuum state. The reactor 10 is a beam is injected into the reaction by-products or reactants injected by the reaction by-products or reactants. In addition, the reactor 10 is further provided with a pressure regulator 15 for adjusting the pressure in the reactor 10 is possible to measure in the optimum pressure range.

The incident window 11 is mounted to the reactor 10 and the beam is incident.

The accommodating part 12 is temporarily accommodated to enable real-time process diagnosis of the reaction byproduct or the reactant, and the beam incident on the incident window 11 is incident. In this case, the incident beam causes refraction and scattering with the reaction byproduct or the reactant. By measuring the intensity of the refracted and scattered beam in this way it is possible to analyze the quality and quantification of the sample. The accommodating part 12 temporarily receives the exhaust gas discharged from the exhaust port and the like and discharges it after spectroscopic analysis, thereby real-time process diagnosis is possible. In addition, the receiving part 12 may be inserted directly into the exhaust port to enable real-time process diagnosis as shown in FIG. 1, and by collecting a small port at the exhaust port and collecting and sampling reaction by-products or reactants collected therefrom. Process diagnostics can also be enabled in real time.

The receiving part 12 is formed in a zigzag flow path as shown in FIG. 2 so that the incident beam is reflected by the reflecting mirror 14 to have a zigzag path so that the path of the beam is increased to increase the detection distance of the beam. Can be increased.

The exit window 13 is emitted after the beam incident in the receiving part 12 passes through the reaction byproduct or the reactant.

The reflection mirror 14 is mounted inside the accommodation part 12 inside the entrance window 11 and the exit window 13, and a beam incident through the entrance window 11 is at least inside the accommodation part 12. Reflects to be reciprocated more than once to serve to exit to the exit window (13). When the incident beam is reciprocated inside the receiving part 12, the effect of increasing the detection distance of the beam may be brought to improve the measurement sensitivity.

The detector 20 detects the refraction and scattering of the beam emitted from the reactor 10. The detector 20 is known and uses an IR detector such as MCT.

The analyzer 30 analyzes the qualitative and quantitative analysis of the sample using the intensity of the beam detected by the detector 20.

3 is a view showing the structure of an infrared spectrometer capable of real-time process diagnosis of another form according to the present invention.

As shown, another type of infrared spectrometer capable of real-time process diagnosis of the present invention includes an incident window 111, a receiving part 112 temporarily receiving a reaction by-product or a reactant, and an inside of the receiving part 112. A crystal 114 fixed by the fixing part 113 to allow the incident beam to reciprocate at least once inside, a plasma electrode 115 spaced apart from the crystal 114, and an emission window ( Reactor 110 comprising 116; A detector (120) for detecting the refraction and scattering of the beam emitted from the reactor (110); An analyzer 130 for analyzing the qualitative and quantitative analysis of the sample using the detected beam intensity; It is made, including.

The reactor 110 includes an incident window 111, a receiving portion 112, an emission window 116, a crystal 114, and a plasma electrode 115, and the inside of the reactor 110 is in a vacuum state. The reactor 110 has a beam incident on the reaction byproduct or the reactant into which the reaction byproduct or the reactant is input, and the incident beam reacts with the reaction byproduct or the reactant to cause refraction and scattering to be emitted. In addition, the reactor 110 is further provided with a pressure regulator 117 for adjusting the pressure in the reactor 110, similar to the infrared spectroscopic analyzer capable of real-time process diagnosis of the present invention described above to measure in the optimum pressure range It becomes possible.

The incident window 111 and the exit window 116 are the same as the infrared spectrometer capable of real-time process diagnosis of the present invention described above.

The receiving unit 112 temporarily receives a beam incident to the incident window 111 to allow real-time process diagnosis of a reaction byproduct or a reactant.

The crystal 114 is fixed by the fixing part 113 in the accommodating part 112, and the incident beam is refracted and scattered by the reaction byproduct or the reactant to enter the reciprocating inside and at least once or more. Do it. The beam incident by the crystal 114 can be measured by reciprocating the inside. In addition, the fixing part 113 is preferably capable of temperature control to adjust the temperature of the crystal 114.

The plasma electrode 115 is provided spaced around the crystal 114, and serves to facilitate cleaning of the crystal 114 or decomposition of reaction by-products or reactants or foreign substances adsorbed and deposited on the crystal 114. do.

Cleaning port 118 for injecting the same nitrogen gas as the infrared spectrometer capable of real-time process diagnosis of the present invention described above to prevent the adsorption by-products or reactants are adsorbed and deposited on the crystal 114 and the plasma electrode 115 It is preferable that it is further provided.

In addition, the reactor 110 is an injection hole for injecting a gas or liquid between the crystal 114 and the plasma electrode 115 to clean the sample adsorbed and deposited on the crystal 114 and the plasma electrode 115 It is preferable that 119 is further provided.

The detector 120 and the analyzer 130 are the same as the infrared spectrometer capable of real-time process diagnosis of the present invention described above.

Reference numerals 40 and 140 denote focusing lenses, and 50 and 150 denote focusing lenses and flat mirrors.

1 is a view showing the structure of an infrared spectrometer capable of real-time process diagnosis according to the present invention.

2 shows another type of reactor of the present invention.

3 is a view showing the structure of an infrared spectroscopy analyzer capable of real-time process diagnosis of another form according to the present invention.

** Description of the symbols for the main parts of the drawings **

10,110 reactor 11,111 entrance window

12,112: accommodation 13,116: exit window

14: reflection mirror 15,117: pressure regulator

16: air curtain 17,119: inlet

20,120: detector 30,130: analyzer

113: fixed part 114: crystal

115: plasma electrode 118: cleaning port

Claims (12)

An incident window 11 through which the beam is incident, Receiving unit 12 is a beam incident to the incident window 11 is incident and temporarily accommodated to enable real-time process diagnosis of the reaction by-product or reactant, An emission window 13 in which the beam incident in the receiving part 12 is refracted and scattered by the reaction by-product or the reactant is emitted; A reflection mirror 14 mounted inside the accommodating part 12 and reflecting the beam incident to the incident window 11 to reciprocate the inside of the accommodating part 12 at least once so as to be emitted to the exit window 13. Reactor 10 including a vacuum inside; A detector 20 for detecting a beam emitted from the reactor 10; An analyzer 30 analyzing the qualitative and quantitative analysis of the sample using the detected beam intensity; Infrared spectrometer capable of real-time process diagnostics, characterized in that comprises a. The method of claim 1, Infrared spectrometer capable of real-time process diagnosis, characterized in that the receiving portion 12 of the reactor 10 is formed in a zigzag flow path. The method of claim 1, The reactor 10 is an infrared spectrometer capable of real-time process diagnostics, characterized in that the pressure regulator 15 for adjusting the pressure in the reactor is further provided. The method of claim 1, The incident window 11, the exit window 13, or the reflection mirror 14 may be prevented from adsorbing and depositing reaction by-products or reactants with the entrance window 11, the exit window 13, or the reflection mirror 14. Infrared spectrometer capable of real-time process diagnostics, characterized in that the air curtain 16 is further provided to inject nitrogen gas. The method of claim 1, The reactor 10 is an infrared spectrometer capable of real-time process diagnostics, characterized in that the temperature can be adjusted. The method of claim 1, The reactor 10 is further provided with an inlet 17 for injecting gas or liquid in order to clean the sample adsorbed and deposited in the incident window 11, the exit window 13 and the reflection mirror 14 Infrared spectrometer with real-time process diagnostics. An incident window 111 through which the beam is incident, Receiving unit 112 is incident to the incident beam 111 is incident to receive the reaction by-products or reactants temporarily to enable real-time process diagnosis of the reactants; The crystal 114 is fixed by the fixing part 113 in the receiving portion 112 and the incident beam is refracted and scattered by the reaction by-products or reactants to enter and reciprocate the inside at least once or more, and A plasma electrode 115 spaced apart from the crystal 114 and providing continuous radiation in a far infrared region; A reactor (110) including an emission window (116) for emitting a beam emitted from the crystal (114), the inside of which is in a vacuum state; A detector (120) for detecting the refraction and scattering of the beam emitted from the reactor (110); An analyzer 130 for analyzing the qualitative and quantitative analysis of the sample using the detected beam intensity; Infrared spectrometer capable of real-time process diagnostics, characterized in that comprises a. The method of claim 7, wherein The reactor 110 is an infrared spectrometer capable of real-time process diagnostics, characterized in that the pressure regulator 117 for adjusting the pressure in the reactor is further provided. The method of claim 7, wherein Infrared spectrometer capable of real-time process diagnosis, characterized in that the crystal 114 and the plasma electrode 115 is further provided with a cleaning port 118 for injecting an inert gas to prevent the reaction by-products or reactants are adsorbed and deposited . The method of claim 7, wherein The fixed part 113 is an infrared spectrometer capable of real-time process diagnosis, characterized in that the temperature can be adjusted to adjust the temperature of the crystal (114). The method of claim 7, wherein The reactor 110 is an inlet 119 for injecting gas or liquid between the crystal 114 and the plasma electrode 115 to clean the sample adsorbed and deposited on the crystal 114 and the plasma electrode 115. Infrared spectrometer capable of real-time process diagnosis, characterized in that the further provided. The method according to any one of claims 1 to 11, The analyzer is an infrared spectrometer, characterized in that used in the equipment cleaning cycle or maintenance cycle (PM cycle) analysis by analyzing the gas coming from the resting equipment.

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