Inline concentration meter and concentration detection method

Abstract

An inline concentration meter includes a light source unit emitting mixed light containing at least two wavelengths with a phase difference, a detecting unit including a light incident part for entering the mixed light emitted from the light source unit into a fluid passage of a detector body and at least two light detection parts receiving the mixed light passed through the fluid passage, a computing processor unit conducting frequency analyzes of detection signals of the mixed light output from the respective light detection parts and computing variations of intensities of the detection signals corresponding to absorbances in at least two frequency ranges to compute a concentration of fluid in the fluid passage based on the variations of the intensities of the detection signals, and a recording/displaying unit recording and displaying a value of the fluid concentration computed at the computing processor unit.

Claims

1. An inline concentration meter, comprising: a light source unit for emitting mixed light having at least two wavelengths with a phase difference; a detecting unit including a light incident part for entering the mixed light emitted from the light source unit into a fluid passage of a detector body and at least first and second light detection parts for receiving the mixed light emitted into the fluid passage, wherein a first light path through the fluid passage is defined between the light source and the first light detection part, and a second light path through the fluid passage, longer than the first light path, is defined between the light source and the second light detection part; wherein the second light path includes a first portion including the first light path and a second portion defined through the fluid passage between the first light detection part and the second light detection part; a computing processor unit for conducting frequency analyses of detection signals of the mixed light output from the respective light detection parts and computing variations of intensities of the detection signals corresponding to absorbances in at least two frequency ranges to compute a concentration of fluid in the fluid passage based on the variations of the intensities of detection signals in the at least two frequency ranges; wherein, from results of the frequency analyses through FFT (fast Fourier transformation) and/or the computed results of the variations of the light intensities corresponding to the absorbances in the respective frequency ranges, respective light absorption matrixes are obtained in the computing processor unit, and then the concentration of the raw material gas is continuously computed in real time based on the light absorption matrixes by using an algorithm for computing the raw material gas concentration; and a recording/displaying unit for recording and displaying a value of the fluid concentration computed at the computing processor unit; wherein, the light source unit emits ultraviolet light in a wavelength region of 200 nm to 400 nm; and wherein part of the mixed light is entered into the first light detection part through a light transmitting window of the first light detection part and part of the mixed light reflected on the light transmitting window is entered into the second light detection part.

2. The inline concentration meter according to claim 1, wherein the light source unit emits mixed light containing three wavelengths.

3. The inline concentration meter according to claim 2, wherein the one light incident part is arranged on one side of the detector body and three light detection parts are arranged on another side opposing to the one side.

4. The inline concentration meter according to claim 1, wherein the light source unit has an LED or laser diode as a light source.

5. The inline concentration meter according to claim 1, wherein the computing processor unit conducts the frequency analyses through Fourier transformation or wavelet transformation.

6. The inline concentration meter according to claim 1, wherein the computing processor unit computes a concentration of organic metal raw material gas included in the mixed gas flowing in the fluid passage.

7. The inline concentration meter according to claim 1, wherein the detecting unit comprises one light incident part and the first and second light detection parts.

8. The inline concentration meter according to claim 7, wherein the one light incident part is arranged on one side of the detector body and the first and second light detection parts are arranged on another side opposing to the one side.

9. The inline concentration meter according to claim 7, wherein the one light incident part and the second light detection part are arranged on one side of the detector body and the first light detection part is arranged on another side opposing to the one side.

10. The inline concentration meter according to claim 1, wherein the light source unit emits mixed ultraviolet light of three ultraviolet lights with different wavelengths.

11. The inline concentration meter according to claim 1, wherein the computing processor unit respectively conducts frequency analysis of detection signals of mixed light containing three wavelengths through Fourier transformation.

12. The inline concentration meter according to claim 1, wherein the light source unit emits mixed light that a beam combiner provides by combining ultraviolet lights with different wavelengths.

13. A concentration detection method comprising the steps of: entering mixed light of three ultraviolet lights having different wavelengths with phase differences, emitted from a light source unit from one light incident part arranged on a detector body with a fluid passage, into the fluid passage; detecting the respective three ultraviolet lights passed through the fluid passage by at least first and second light detection parts arranged on the detector body, wherein a first light path through the fluid passage is defined between the light source and the first light detection part, and a second light path through the fluid passage, longer than the first light path, is defined between the light source and the second light detection part, wherein the second light path includes a first portion including the first light path and a second portion defined through the fluid passage between the first light detection part and the second light detection part; conducting frequency analyses of detection signals of the mixed light detected by the respective light detection parts; computing variations of intensities of the detection signals detected by the light detection parts corresponding to absorbances in three frequency ranges; and computing a concentration of organic metal material gas included in mixed gas that flows through the fluid passage based on the at least six computed variations of the intensities of the detection signals in the three frequency ranges.

14. The concentration detection method according to claim 13, wherein the number of the light detection parts is three and the concentration of the organic metal material gas included in the mixed gas that flows through the fluid passage is computed based on nine computed variations of intensities corresponding to the absorbances.

15. The concentration detection method according to claim 13, wherein the mixed light entering from the light incident part is detected by the first light detection part and reflected light from the first light detection part is entered to the second light detection part.

16. The concentration detection method according to claim 13, wherein the mixed light entering from the light incident part is dispersed and entered to the first and second light detection parts.

Description

BRIEF DESCRIPTION OF DRAWINGS

(1) FIG. 1A schematic diagram showing a configuration of a raw material fluid concentration meter of an embodiment of the present invention.

(2) FIG. 2A schematic diagram of a configuration of a light source unit.

(3) FIG. 3A longitudinal partial view of a configuration of a detecting unit.

(4) FIG. 4A graph showing examples of ultraviolet light absorption (transmittance) characteristics of organic metal raw material gases.

(5) FIG. 5 (a) to (c) are explanatory diagrams of detection value processing in a computing processor unit, and (d) is an explanatory diagram of computed light absorption matrixes , , and .

(6) FIG. 6 A diagram showing an application example of the gas concentration meter of the present invention.

(7) FIG. 7 A diagram showing an application example of a conventional inline gas concentration meter.

(8) FIG. 8 A schematic diagram of a configuration of the conventional inline gas concentration meter.

(9) FIG. 9 A schematic diagram of a configuration of a conventional ultraviolet absorption type gas concentration meter.

DESCRIPTION OF EMBODIMENTS

(10) Hereinafter, embodiments of the present invention are described with reference to the drawings.

(11) FIG. 1 is a schematic diagram showing a configuration of a raw material fluid concentration meter of an embodiment of the present invention.

(12) A raw material gas concentration meter GD according to the present invention includes a light source unit 1 with an LED light source 1a, a detecting unit 2 that has a light incident part 9, a detector body 6 with a fluid passage 6a, and light detection parts 10, a computing processor unit 3 as well as a recording/displaying unit 4. Here the detecting unit 2 is formed for inline installation in a pipeline as described later.

(13) In other words, three ultraviolet lights having different wavelengths are emitted from the light source unit 1 with different phases and entered to a beam combiner 1a.sub.4 (FIG. 2). The respective ultraviolet lights entered are mixed in the beam combiner 1a.sub.4 and then the mixed light is entered to the light incident part 9 of the detecting unit 2 through an optical fiber 5.

(14) The ultraviolet light entered to the light incident part 9 of the detecting unit 2 runs through raw material gas G in the fluid passage 6a, and is detected by the light detection parts 10 provided to at least two different locations.

(15) In the embodiment, as described later based on FIGS. 2 to 5, the three ultraviolet lights having wavelengths of .sub.1, .sub.2, and .sub.3 with the phase differences are emitted from the LED light source 1a and the mixed light of the three ultraviolet lights is entered to the one light incident part 9, then the ultraviolet light radiated into the fluid gas G from the light incident part 9 is detected by the two light detection parts 10 to detect so-called absorbances of the ultraviolet light. Here, to the second light detection part, reflected light from a sapphire made light transmitting window 9a of the first light detection part is entered.

(16) Here, although not shown in the drawings, the entered light may be dispersed from the one light incident part 9 and the mixed light may be directly entered to the at least two or more light detection parts 10.

(17) The light detection values (light reception values) of the mixed light (synthesized light) containing the three wavelengths of .sub.1, .sub.2, and .sub.3 detected by the two light detection parts 10a and 10b are separately input to the computing processor unit 3 for frequency analyses through Fourier transformation and the like to compute intensities of the light detection values of the three frequency range components, and values corresponding to total six absorbances (two light detection partsthree frequency ranges) are found.

(18) Then eventually, a concentration of the raw material gas that passes in the fluid passage 6a is computed and displayed based on a matrix of the computed values corresponding to the six absorbances.

(19) Referring to FIG. 2, the light source unit 1 includes the multi LED light source 1a, the beam combiner 1a.sub.4, a reflect mirror 1b, and the optical fiber 5. The three types of ultraviolet lights respectively having the wavelengths of .sub.1, .sub.2, and .sub.3 are emitted from the multi LED light source 1a and the ultraviolet lights are combined by the beam combiner 1a.sub.4 into the one light to be entered to the detecting unit 2 via the reflect mirror 1b and the optical fiber 5.

(20) Here in the embodiment shown in FIG. 2, phase differences are given between the respective ultraviolet lights by differentiating light emission start times of respective LED light sources 1a.sub.1, 1a.sub.2, and 1a.sub.3, though the ultraviolet lights may be simultaneously emitted from the LED light sources 1a.sub.1, 1a.sub.2, and 1a.sub.3 with the phase differences between the respective ultraviolet lights given by a phase adjuster (not shown) that is separately provided.

(21) So-called a multi LED is used as the LED light source 1a, and specifically, a small-sized tri-color high-luminance LED in a wavelength region of 200 nm to 400 nm is used in the embodiment.

(22) Here in the implementation examples shown in FIGS. 1 and 2, the LED is used as the light source, though a so-called LD (laser diode), which is included in a group of LEDs, may, of course, be used as the light source.

(23) As shown in FIG. 3, the detecting unit 2 includes the detector body 6, the one light incident part 9, and the two light detection parts 10a and 10b.

(24) The detector body 6 is made of stainless steel and the fluid passage 6a is arranged therein. Further, an inlet block 7 as well as an outlet block 8 are airtightly fixed to each side of the detector body 6 via gasket-type seals 11 with bolts (not shown). Here, a reference sign 6b designates a leakage inspection hole, a reference sign 6c designates a fixation hole for the light incident part 9, and a reference sign 6d designates fixation holes for the light detection parts 10.

(25) The light incident part 9 is arranged on a top face of the detector body 6 and the light detection parts 10a and 10b are respectively arranged on the top face and a down face of the detector body 6 to obliquely face each other. The mixed light of the three ultraviolet lights respectively having the wavelengths of .sub.1, .sub.2, and .sub.3 with the phase differences is entered to the sapphire made light transmitting window 9a in the light incident part 9 from the light source unit 1 via the optical fiber 5.

(26) Most of the entered mixed light is entered to the fluid passage 6a through the sapphire made light transmitting window 9a, though part of the incident mixed light is reflected by the sapphire made light transmitting window 9a, and intensity of the reflected light is detected by photo diodes 12 to be used for detection of so-called fluctuations of the light source or the like.

(27) The light incident part 9 is arranged to obliquely face to the first light detection part 10a, and most of the light entered from the light incident part 9 is entered to the photo diode 12 in the first light detection part 10a through the fluid gas G in the fluid passage 6a as well as the sapphire made light transmitting window 9a of the first light detection part 10a for light intensity detection of the entered light.

(28) Here, since the mixed light is entered to the sapphire made light transmitting window 9a in the first light detection part 10a at a certain angle of inclination, part of the mixed light is reflected here and the reflected light from the first light detection part 10a is entered to the second light detection part 10b on the top face through the fluid passage 6a.

(29) Respective light intensities of the mixed light containing the wavelengths of .sub.1, .sub.2, and .sub.3 detected by the light detection parts 10a and 10b change depending on light absorption by the raw material fluid G (process fluid) flowing in the fluid passage 6a. In other words, the respective light intensities vary by the concentration of the raw material gas G and the like.

(30) Here, the respective light intensity signals detected by the photo diodes 12 are input to the computing processor unit 3 which is described later and the concentration of the raw material gas G is automatically computed therein.

(31) The light incident part 9 and the light detection parts 10a as well as 10b have completely the same configuration, and as shown in FIG. 3, each includes a holding-fixing body 9c with a flange reception hole 9b at a center thereof, a first fixation flange 9d and a second fixation flange 9e that are arranged on an outer surface of the detector body 6, the sapphire made light transmitting panel 9a airtightly inserted and fixed between the both flanges 9d and 9e, and the photo diode 12 that is located at an upper side of the light transmitting board 9a and fixed to the first fixation flange 9d.

(32) In other words, the second fixation flange 9e and the first fixation flange 9d are airtightly integrated by pressing a protrusion of the first fixation flange 9d into a recession of the second fixation flange 9e with the sapphire made light transmitting panel 9a inserted and fixed therebetween.

(33) The second fixation flange 9e and the first fixation flange 9d integrated together are inserted to the flange reception hole 9b of the holding-fixing body 9c, and the holding-fixing body 9c is pressed and fixed to the detector body 6 via the gasket-type seal 11 with a fixing bolt (not shown) to airtightly fix the light incident part 9 and the light detection parts 10a and 10b to the detector body 6.

(34) In FIG. 3, reference signs 7b and 8b designate coupling parts, the reference sign 6b designates the leakage inspection hole, the reference sign 6c designates the fixation hole for the light incident part 9, and the reference sign 6d designate the fixation holes for the light detection parts 10a and 10b. The light incident part 9 and the light detection parts 10a as well as 10b are fixed with fixing bolts (not shown).

(35) In the embodiment shown in FIG. 3, the light incident part 9 is arranged on the top face of the detector body 6 and the light detection parts 10 are respectively arranged on the top face and the down face of the detector body 6, though the light incident part 9 and the light detection parts 10 may be arranged in a row on one same face.

(36) Additionally, in the embodiment shown in FIG. 3, the number of the light detection parts 10 is two, though the number of the light detection parts may, of course, be three or even four. However, the most proper number of the light detection parts 10 should be two to three in regards to measurement precision and a cost of the concentration meter.

(37) The light intensities detected by the respective light detection parts 10a and 10b on the top face vary by length of a light path in the fluid passage 6a, the concentration of the raw material gas G and the like, and the detected light intensity signals corresponding to the absorbances are input to the computing processor unit 3 for computing the concentration of the raw material in the raw material fluid.

(38) FIG. 4 shows examples of ultraviolet light absorption (transmittance) characteristics of organic metal raw material gases to ultraviolet light with wavelengths of 200 nm to 350 nm. In FIG. 4, a curve E.sub.1, a curve E.sub.2, and a curve E.sub.3 respectively indicate the ultraviolet light transmittance of 0.10% TMGa gas, 0.01% TMIn gas, and 0.81% TMAl gas.

(39) Here, the concentration Cd of the raw material may basically be computed by the following formula (1) based on the absorbance A obtained by the spectrophotometer.
A=log.sub.10(I.sub.0/I)=CdIFormula (1):
In the formula (1), I.sub.0 represents the intensity of the light entered from the light incident part 9, I represents the intensity of the transmitted light (intensity of the light entered to the photo diode 12 of the light detection part 10), represents molar absorbance coefficient of the raw material, Cd represents the raw material concentration, and A represents the absorbance.

(40) Referring to FIG. 5 (a), the mixed light of the three types of ultraviolet lights respectively having the wavelengths of .sub.1, .sub.2, and .sub.3 with the phase differences is entered to the light incident part 9 of the detecting unit 2 and then radiated into the raw material gas G from the light incident part 9.

(41) The three types of ultraviolet lights having the wavelengths of .sub.1, .sub.2, and .sub.3 with the phase differences that have passed through the raw material gas G are intensity-modulated and the three lights are mixed by the beam combiner 1a.sub.4. Then the mixed light reaches to the light detection parts 10a and 10b. While passing through the raw material gas G, a certain wavelength of the mixed incident light is absorbed by the gas G, and the intensity of the mixed light entered to the light detection parts is detected by the respective photo diodes 12. FIG. 5 (b) shows an example of the detection value of the light intensity. Change of the intensity is measured after the absorption of the light by the organic raw material gas.

(42) Here, the light intensities of the mixed light after the absorption of the light detected by the respective light detection parts 10a and 10b vary depending on the location of the detection of the light, the wavelength of the light, the concentration of the raw material gas, length of the transmitted light path and the like, and the detection value draws a curb like a curb S in the graph of FIG. 5 (b).

(43) The respective detection value S of light intensities detected by the light detection parts 10a and 10b are input to the computing processor unit 3, and then frequency analyses through fast Fourier transformation and/or computing analyses of the intensities in the three frequency ranges (i.e. intensities corresponding to the absorbances) are conducted for computing the concentration of the raw material gas by applying Beer-Lambert law.

(44) FIG. 5 (c) is a graph showing variations of the intensities of the ultraviolet lights having the wavelengths of .sub.1, .sub.2, and .sub.3 in the three frequency ranges which are examples of the intensities corresponding to the absorbances that are basis for computation of the raw material concentration.

(45) Subsequently, from the results of the frequency analyses through FFT (fast Fourier transformation) and/or the computed results of the variations of the light intensities corresponding to the absorbances in the respective frequency ranges (the three frequency ranges in the embodiment), the respective light absorption matrixes , , and shown in FIG. 5 (d) are obtained in the computing processor unit 3, and then the concentration of the raw material gas G is continuously computed in real time based on the light absorption matrixes , , and by using a prepared algorithm for computing the raw material gas concentration.

(46) Adjustment of a zero point and diagnosis of abnormality, for example, detection of fogging of the sapphire made light transmitting window 9a, of the concentration meter are also conducted based on the changes of the light absorption matrixes shown in FIG. 5 (d). It has been confirmed that the present invention may realize higher measurement precision as well as measurement reproducibility, significantly reduce time required for concentration measurement, and lower a cost of the device comparing with conventional gas analyzers for F.sub.2 gas using ultraviolet light.

(47) FIG. 6 shows an application example of the gas concentration meter GD according to the present invention, and the concentration of the raw material gas G is maintained at a certain level by feedback-controlling a tank pressure regulator 13 and/or a mass flow controller 14 of career gas CG based on the detection value of the concentration detected by the gas concentration meter GD.

(48) Here, because a structure of a raw material gas generator 15 is almost the same as in the case of the conventional technology shown in FIG. 7, description of the structure is omitted herein.

INDUSTRIAL APPLICABILITY

(49) A concentration meter according to the present invention may continuously detect a concentration of raw material fluid in a pipeline regardless of an original form, such as liquid or sublimable solid, of the raw material as long as the fluid has a light absorption characteristic, particularly an ultraviolet light absorption characteristic, and may be used for continuous fluid concentration detection not only in gas supply systems for semiconductor manufacturing but also in any fluid-supply pipelines and/or fluid-use apparatuses that are used with precipitating fluids, photoreactive fluids and/or corrosive fluids.

A REFERENCE SIGNS LIST

(50) 1 light source unit 1a LED light source 1a.sub.1 to 1a.sub.3 LED light source 1a.sub.4 beam combiner 1b reflect mirror 2 detecting unit 3 computing processor unit 3a fluid passage 3b coupling part 4 recording/displaying unit 5 optical fiber 6 detector body 6a fluid passage 6b leakage inspection hole 6c light incident part fixation hole 6d light detection part fixation hole 7 inlet block 8 outlet block 9 light incident part 9a sapphire made light transmitting window 9b flange reception hole 9c holding-fixing body 9d first fixation flange 9e second fixation flange 10 light detection part 10a and 10b light detection part 11 gasket-type seal 12 photo diode 13 tank pressure regulator 14 mass flow controller 15 gas generator GD gas concentration meter phase difference .sub.1 to .sub.3 wavelength S curb of light intensity detected by light detection part E1 to E3 curb of ultraviolet light transmittance of organic raw material A.sub.1 to A.sub.3 light intensity variation of ultraviolet light with wavelength of 1 to 3 , , light absorption matrix