WO2014181527A1 - 原料流体濃度検出器 - Google Patents
原料流体濃度検出器 Download PDFInfo
- Publication number
- WO2014181527A1 WO2014181527A1 PCT/JP2014/002376 JP2014002376W WO2014181527A1 WO 2014181527 A1 WO2014181527 A1 WO 2014181527A1 JP 2014002376 W JP2014002376 W JP 2014002376W WO 2014181527 A1 WO2014181527 A1 WO 2014181527A1
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- Prior art keywords
- light
- raw material
- detector
- recess
- material fluid
- Prior art date
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- 239000012530 fluid Substances 0.000 title claims abstract description 110
- 239000002994 raw material Substances 0.000 title claims abstract description 81
- 238000001514 detection method Methods 0.000 claims abstract description 59
- 230000005540 biological transmission Effects 0.000 claims abstract description 50
- 230000010355 oscillation Effects 0.000 claims abstract description 37
- 238000003780 insertion Methods 0.000 claims description 21
- 230000037431 insertion Effects 0.000 claims description 21
- 229910052594 sapphire Inorganic materials 0.000 claims description 19
- 239000010980 sapphire Substances 0.000 claims description 19
- 239000013307 optical fiber Substances 0.000 claims description 11
- 238000007789 sealing Methods 0.000 claims description 7
- 230000002093 peripheral effect Effects 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 abstract description 4
- 239000007789 gas Substances 0.000 description 28
- 230000003287 optical effect Effects 0.000 description 23
- 239000000463 material Substances 0.000 description 13
- 239000004065 semiconductor Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 8
- 238000005259 measurement Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 238000005219 brazing Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- 229910052737 gold Inorganic materials 0.000 description 4
- 239000003566 sealing material Substances 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229920003002 synthetic resin Polymers 0.000 description 3
- 239000000057 synthetic resin Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000011481 absorbance measurement Methods 0.000 description 1
- 230000004308 accommodation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
- G01N21/05—Flow-through cuvettes
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/59—Transmissivity
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
- G01N9/24—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity by observing the transmission of wave or particle radiation through the material
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
- G01N21/85—Investigating moving fluids or granular solids
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2201/00—Features of devices classified in G01N21/00
- G01N2201/08—Optical fibres; light guides
Definitions
- the present invention relates to an improvement of a process fluid concentration meter used in a raw material fluid supply device or the like of a semiconductor manufacturing apparatus, and in particular, to achieve downsizing and an in-line type sensor unit of the concentration meter, as well as high precipitation and high photoreaction.
- In-line photoanalytical raw material fluid that can maintain high transparency of the light transmission window and high cleanliness (particle resistance) inside the sensor for long periods of time even for corrosive and corrosive raw material fluids
- the present invention relates to a concentration detector.
- a photometric densitometer 22 is provided in the vicinity of the raw material vapor outlet of the temperature-controlled raw material tank 21, By adjusting the temperature of the raw material tank 21, the flow rate of the carrier gas CG, the in-tank vapor pressure Po, etc. according to the concentration detection signal from the concentration meter 22, a process gas 24 (for example, a tank) having a predetermined raw material concentration is supplied to the reaction furnace 23.
- the process gas containing an organic metal material vapor such as trimethylgallium TMGa stored in the gas 21 is supplied.
- 25 is a thermal mass flow controller
- 26 is a pressure adjusting device for tank internal pressure.
- FIG. 10 Japanese Unexamined Patent Application Publication No. 2004-108981
- an optical cell (gas cell) 27 in which the gas G to be measured flows a light source 28 for irradiating the optical cell 27 with a light beam
- a light receiving device for the light beam that has passed through the optical cell 27 a light receiving device for the light beam that has passed through the optical cell 27
- an arithmetic unit 30 for calculating the concentration of the raw material by obtaining the absorbance from the signal of the light receiving device 29, and the like.
- 31 is a main pipeline and 32 is a branch pipeline.
- the so-called absorbance of the gas in the optical cell 27 is measured, and the gas concentration is calculated by applying Lambert-Beer's law to the absorbance measurement result.
- an in-line sensor 33 incorporating an optical cell is fixed to a conduit 31, and the light intensity of the light transmitted through the optical cell is measured. Like to do.
- the inline sensor 33 incorporating the photometric densitometer 22 and the optical cell (absorption cell) 27 is publicly known, and a detailed description thereof is omitted here.
- the transparency of the light transmission window of the optical cell 27 needs to be stable over a long period of time, and when the transparency changes over time. Makes it difficult to measure the gas concentration stably.
- quartz glass is often used as a constituent material of the light transmission window, so the light transmission window is corroded when measuring the concentration of organic source gas having high corrosivity or high precipitation.
- the transparency of the raw material is lowered at an early stage due to the deposition of the raw material, and there remains a problem that a stable raw material gas concentration cannot be measured.
- various structures inside the optical cell 27 need to be firmly fixed and held on the main body of the optical cell 27 with high airtightness. Therefore, various synthetic resin sealing materials, silver brazing, gold brazing, and the like are used in the optical cell 27.
- the synthetic resin sealing material, silver brazing, and gold brazing members in the optical cell 27 are emission sources for releasing the gas and particles contained in each member itself into the organic raw material gas. There is a danger that there is a problem that the gas purity is actually lowered due to emission of particles. Therefore, it is not desirable to use silver brazing or gold brazing in the gas supply system for manufacturing semiconductors.
- the above-mentioned problem in the raw material concentration meter used in the conventional raw material fluid supply device that is, (I) simplification and downsizing of the concentration meter, and reduction in product cost cannot be easily achieved.
- the first aspect of the raw material fluid concentration detector is a photoanalytical raw material fluid comprising a detector body 2 and a light oscillation unit 5a and a light detection unit 5b provided on the upper surface or the lower surface of the detector body 2.
- the concentration detector at least one recess 17 is formed on the upper surface and the lower surface of the detector body 2, and the fluid channel 2 a communicating from the fluid inlet of the detector body 2 to the recess 17 is communicated with the recess 17.
- a fluid passage 2b that communicates with the fluid outlet of the detector body 2 from the concave portion 17, and the light oscillation portion 5a is disposed in at least one concave portion, and the light detection portion 5b is disposed in the remaining concave portion.
- the light oscillation unit includes a light transmission plate, a light intensity detection photodiode, and a light oscillation light source (optical fiber).
- the light detection unit includes a light transmission plate and a light intensity detection photodiode.
- the light transmission plate disposed in the recess formed in the detector main body is hermetically fixed using a gasket type seal.
- a fourth aspect of the raw material fluid concentration detector includes a detector body 2, a light oscillation unit 5a provided on the upper surface of the detector body 2, and a light detection unit 5b provided on the lower surface of the detector body 2.
- An optical analysis type raw material fluid concentration detector comprising: a recess 17 provided on the upper and lower surfaces of the detector body 2 and communicated by a fluid passage 2b; a gasket-type seal 6 mounted in the recess 17; A first fixing flange 14 and a second fixing flange 16 which are arranged opposite to the mold seal 6 and which are airtightly sandwiched and fixedly bonded with a light transmission plate 11a; an optical fiber 9 provided in the second fixing flange 16; A photodiode 10 and a holding fixture 12 that hermetically fixes the joint-fixed flanges 14 and 16 into the recess of the detector body 2 via the gasket-type seal 6 are provided.
- the fifth aspect of the raw material fluid concentration detector according to the present invention includes a detector body 2, a light oscillation unit 5a provided on the upper surface of the detector body 2, and a light detection unit 5b provided on the lower surface of the detector body 2.
- the detector main body 2 includes a recess 17 provided on the upper surface and the lower surface, a fluid passage 2b communicating between both the recesses 17, a fluid inlet, and an upper surface, respectively.
- a gasket housing portion 17a that includes a fluid passage 2a that communicates between the recess portions 17 and a fluid passage 2c that communicates between the fluid outlet and the recess portion 17 on the lower surface, and the light oscillation portion 5a and the light detection portion 5b are connected to the recess portion 17.
- the light transmitting plate 11a and the protruding portion 16b having a stepped outer peripheral surface are inserted into the insertion concave portion 14b of the first fixing flange 14, and the light transmitting plate 11a is interposed between the light transmitting plate 11a and the insertion concave portion 14b.
- the second fixing flange 16, the light intensity detecting photodiode 10 disposed and fixed outside the light transmitting plate 11 a in the second fixing flange 16, and the both fixing flanges 14 and 16 fitted and fixed are accommodated.
- the flange housing portion 12a is provided in the center, and the two fixing flanges 14 and 16 housed in the flange housing portion 12a by tightening the fixing bolt 8 are hermetically fixed to the detector body 2 via the gasket type seal 6.
- the sixth aspect of the raw material fluid concentration detector according to the present invention is the same as the fifth aspect described above in that the tip surface 16d of the protruding portion 16b of the second fixing flange 16 and the bottom surface 14c of the insertion recess 14b of the first fixing flange 14 are provided.
- a seventh aspect of the raw material fluid concentration detector according to the present invention is such that, in the fifth aspect, the bottom surface 14e of the gasket housing portion 14d of the first fixing flange 14 is used as a gasket seal surface.
- an optical fiber insertion hole 9a is provided in the second fixing flange 16 of the light oscillating portion 5a, and the photodiode 10 is replaced with a light transmitting plate. This is a photodiode for detecting the intensity of reflected light from 11a.
- the photodiode 10 provided on the second fixed flange 16 of the light detection unit 5b has a transmitted light intensity from the light transmission plate 11a. This is a detection photodiode.
- the tenth aspect of the raw material fluid concentration detector according to the present invention is the same as the fifth aspect described above, in which another light detector 5b is provided at an interval on the upper surface of the detector body 2, and the lower surface of the detector body 2
- the concave portion 17 of the light detecting portion 5b provided on the lower surface and the concave portion 17 of the other light detecting portion 5b communicate with each other through the fluid passage 2c, and the reflected light intensity from the light transmitting plate 11a of the light detecting portion 5b provided on the lower surface is determined. This is configured to be detected by the other light detection unit 5b.
- An eleventh aspect of the raw material fluid concentration detector according to the present invention is that in the fifth aspect, the raw material fluid is an organic raw material vapor having precipitation, high reactivity, or corrosiveness.
- the light transmission plate 11a is made of sapphire in the fifth aspect.
- At least one recess 17 is formed on the upper surface and the lower surface of the detector body 2, and a fluid flow path 2 a that communicates from the fluid inlet of the detector body 2 to the recess 17 and a fluid passage that communicates between the recesses 17. 2b and a fluid flow path 2c communicating from the recess 17 to the fluid outlet of the detector body 2, the light oscillation unit 5a is disposed in at least one recess, and the light detection unit 5b is disposed in the remaining recess. Therefore, the raw material concentration detector can be an in-line type and has a very simple configuration.
- the light oscillation part 5a and the light detection part 5b include a gasket-type seal 6 mounted in the gasket housing part 17a, a first fixing flange 14 having an insertion concave part 14b disposed opposite thereto, and an insertion concave part 14b.
- a second fixed flange 16 that is hermetically joined and fixed to the first fixed flange 14 by press-fitting into the first fixed flange 14; a sapphire light transmitting plate 11a that is hermetically sandwiched between the two flanges; Since the holding fixing body 12 that is pressed and fixed to the detector main body 2 is provided, the structures of the light oscillating portion 5a and the light detecting portion 5b can be simplified, and high airtightness can be maintained.
- the light transmission window 11 is made of sapphire, the light transmittance does not decrease even if it is a depositing, reactive or corrosive fluid, and stable and highly accurate concentration measurement is possible. Further, since the gasket type seal is used, it is possible to eliminate impurities from entering the fluid as compared with a seal structure using other synthetic resin sealing materials, silver wax materials, gold wax materials, or the like.
- a light transmission window which is a plate material 11 made of a brittle fracture material, is sandwiched between the first fixing flange 14 and the second fixing flange 16, and both flanges are hermetically bonded and fixed, and the light transmission window is mounted. Since the two flanges that are airtightly joined and fixed are hermetically inserted into the recess 17 by the holding fixing body 12 fixed to the main body 2, the light transmission window can be easily and highly airtight without using a sealing material. And can be firmly held and fixed.
- the raw material fluid concentration detector of the present invention has excellent effects in terms of downsizing the equipment, reducing equipment costs, maintaining airtightness, ensuring stability of concentration measurement accuracy, and maintaining high gas purity. Play.
- concentration detector which concerns on embodiment of this invention. It is a top view of the raw material fluid density
- the raw material fluid concentration detector 1 has a detector main body 2 and inlets fixed to both sides thereof.
- the detector body 2, the inlet block 3, and the outlet block 4 are made of stainless steel or the like, and fluid passages 2a, 2b, 2c, 3a, and 4a are provided in communication with each other.
- the inlet block 3 and the outlet block 4 are hermetically fixed to both sides of the detector main body 2 by bolts (not shown) via gasket type seals 6.
- 3b and 4b are joint parts
- 7 is a leak inspection hole
- 8 is a fixing bolt for the light oscillation part 5a.
- the light detection unit 5b is also fixed by a fixing bolt 8 (not shown) in the same manner as the light oscillation unit 5a.
- the light oscillating unit 5a and the light detecting unit 5b are juxtaposed on the upper surface side of the detector body 2 with a space therebetween, and a visible region from a light source device (not shown) including a light source, a diffraction grating, a mirror, and the like.
- a light source device including a light source, a diffraction grating, a mirror, and the like.
- Light having a predetermined wavelength in the ultraviolet region is incident on a light transmission plate 11a made of a brittle fracture material, that is, a light transmission plate material made of sapphire, through the optical fiber 9 in the light oscillation section 5a.
- the incident light passes through the sapphire light transmission plate 11a and enters the fluid passage 2a, but a part of the incident light is reflected by the sapphire light transmission plate 11a.
- the intensity of the reflected light is detected by the photodiode 10.
- the light detection unit 5b is provided on the lower surface side of the detector body 2 obliquely below the light oscillation unit 5a so as to face the light oscillation unit 5a, and light incident from the light oscillation unit 5a through the fluid passage 2b. Is incident on the photodiode 10 in the light detector 5b through the sapphire light transmission plate 11a, and the light intensity of the incident light is detected.
- a part of the incident light is also reflected by the sapphire light transmission plate 11a in the light detection section 5b on the lower surface side of the detector main body 2, but this reflected light passes through the fluid passage 2c. 2 is incident on the light detection unit 5b on the upper surface side, and the light detection unit 5b detects the intensity of the reflected light from the light detection unit 5b on the lower surface side.
- the light intensity detected by the light detecting unit 5b on the lower surface side changes depending on the concentration of the raw material fluid (process fluid) flowing in the fluid passage 2b, and the detected light intensity signal is sent to a computing device (not shown).
- the raw material concentration in the raw material fluid is calculated.
- the raw material concentration C is basically calculated by the following equation (1) based on the absorbance A obtained with a spectrophotometer.
- I 0 is the incident light intensity from the light oscillation unit 5a
- I is the transmitted light intensity (incident light intensity to the photodiode 10 of the light detection unit 5b)
- ⁇ is the molar absorption coefficient of the raw material
- C is the raw material concentration
- A is the absorbance.
- the light transmission characteristics of the light oscillation unit 5a and the light detection unit 5b change due to secular change or the like.
- This change in the light transmission characteristic is caused by a photo of the light oscillation unit 5a on the upper surface side that detects reflected light. It appears as a change in the detection value of the diode 10 or the photodiode 10 of the light detection unit 5b on the upper surface side. Therefore, the incident light intensity I 0 and the transmitted light intensity I in the above equation (1) are corrected using the detection values of the photodiodes 10 of the light oscillation unit 5a and the light detection unit 5b on the upper surface side.
- the light oscillating part 5a and the light detecting part 5b are identical in structure, and as shown in FIG. 3, a holding and fixing body 12 having a flange receiving hole 12a in the center made of stainless steel, and a detector A first fixing flange 14 provided on the outer surface of the main body 2, a second fixing flange 16, a sapphire light transmission plate 11 a that is hermetically sandwiched and fixed between both flanges 14, 16, and a position above the light transmission plate 11 a
- the photodiode 10 is fixed to the second fixing flange 16.
- the second fixing flange 16 and the first fixing flange 14 press-fit the protruding portion 16b of the second fixing flange 16 into the insertion recess 14b of the first fixing flange 14 with a force of 8 to 12N, as will be described later. Accordingly, the sapphire light transmissive plate 11a is sandwiched and fixed in an airtight manner with the tip surface 16d of the protruding portion 16b and the bottom surface 14c of the insertion recess 14b as a sealing surface.
- the light oscillation unit 5 a and the light detection unit 5 b are hermetically fixed to the detector main body 2 by being installed and pressed and fixed to the detector main body 2.
- 17 is a recess formed in the outer surface of the detector body 2
- 6a is a gasket
- 13 is a sealing surface between the two fixing flanges 14 and 16
- 14e is a seal between the gasket 6a and the first fixing flange 14.
- the surface 9a is an optical fiber insertion hole.
- the light oscillating portion 5a and the light detecting portion 5b are provided on the upper surface side of the detector body 2 at intervals, but the light detecting portion 5b on the upper surface side is omitted.
- the concave portion 17 of the light detecting portion 5b on the lower surface side and the fluid outlet side may be directly communicated with each other through the fluid passage 2c.
- the light detection unit 5b is provided on the upper surface side of the detector main body 2, and the light oscillation unit 5a is provided on the lower surface side. That is, the light oscillation unit 5a is disposed in another recess in addition to being disposed in the recess closest to the entrance. It is also possible to use other materials such as quartz glass in place of the sapphire light transmission plate 11a.
- the holding and fixing body 12 is provided with a flange accommodating hole 12a in the center of a square steel plate having a thickness of 12 to 15 mm, and fixing bolts 8 on both sides thereof. Insertion hole 12b is provided. Further, a lower end portion of the holding and fixing body 12 is formed with a step portion 12c that fits and presses the upper surface of the outer peripheral portion of the first fixing flange 14, and the lower portion of the flange accommodation hole 12a has an enlarged diameter. And formed in the accommodating portion of the first fixed flange 14.
- the second fixed flange 16 is formed in a short cylindrical body made of stainless steel, and a central portion on one side thereof is a protrusion whose diameter is reduced in a stepped manner by two step portions 16a. It is formed in the part 16b. Further, the distal end surface 16d of the distal end portion of the projecting portion 16b having a reduced diameter is a seal surface that comes into contact with the thin light transmission plate 11a having a thickness of about 0.8 to 1.5 mm.
- the first fixed flange 14 is formed in a disc shape from stainless steel, and is formed in an insertion recess 14b whose diameter is reduced stepwise by a three-step step portion 14a in the center portion. Yes.
- the insertion recess 14 b is formed in a penetrating manner and communicates with the recess 17 of the detector body 2.
- an intermediate portion of the three step portions 14a constitutes a housing portion for the sapphire light transmission plate 11a, on which the sapphire light transmission plate 11a is placed and fixed.
- An accommodating portion 14d of the gasket 6a is formed on the lower surface side of the first fixing flange 14, and the upper half portion of the gasket type seal 6 is inserted and fixed therein.
- the gasket type seal 6 includes a gasket housing portion 14d of the first fixing flange 14, a gasket housing portion 17a on the detector body 2 side, a ring-shaped gasket 6a, and a ring-shaped retainer 6b. And a ring-shaped guide ring 6c and the like, and is configured to be double-sealed by the seal surfaces 15 and 15.
- the light transmission plate 11a made of sapphire constituting the light transmission window made of the plate material 11 made of the brittle fracture material is a so-called high-purity alumina (Al 2 O 3 ) single crystal having a thickness of 0.8 to 1.5 mm. It is formed and has excellent wear resistance, corrosion resistance (chemical resistance), heat resistance, etc., and it is used for semiconductor manufacturing and is corroded and altered by organic raw material gas. It has been confirmed that there is no.
- the gasket-type seal 6, the sapphire light transmission plate 11a, the photodiode 10, and the like are well-known, and detailed description thereof is omitted here.
- the raw material fluid concentration detector 1 is connected in-line to a process gas (organic raw material TMGa vapor) supply line for a semiconductor manufacturing apparatus, and light is oscillated from the light source device 18 through the optical fiber 9. Light was incident on the part 5a.
- the photodiodes 10 of the light oscillating unit 5a and the light detecting unit 5b are selected to have a light receiving surface of 1.0 mm ⁇ 1.1 mm, a diameter of 504 mm, and a height of 3.6 mm, and the sapphire light transmitting plate 11a has a thickness. Further, the length of the flow path 2b between the light oscillation section 5a and the light detection section 5b is set to 30 mm, and the inner diameter of the flow path is set to 4.0 mm ⁇ .
- the detection output from the photodiode 10 of the light oscillating unit 5a is input to the arithmetic unit 19 via the reflected light detection device 18a, and the detection from the photodiode 10 of the light detection unit 5b.
- the output is input to the arithmetic device 19 via the output light detection device 18b.
- the concentration of the organic raw material TMGa vapor flowing in the fluid passage 2a is set at a predetermined time interval using the equation (1). Calculate and record and display the result.
- the detection output from the reflected light detection device 18a is used for correction of the raw material concentration detection value in the arithmetic device 19, whereby the so-called fluctuation of the incident light from the light source device 18 and the light of the sapphire light transmission plate 11a.
- the measurement error of the raw material concentration caused by the secular change of transmittance is corrected.
- the raw material fluid concentration detector according to the present invention can perform highly accurate concentration measurement that is not inferior to a conventional expensive concentration detector.
- the present invention can be used for continuous detection of fluid concentration not only in semiconductor manufacturing gas supply systems, but also in all fluid supply pipelines and fluid handling equipment that handle precipitation, photoreactivity, and corrosive fluids. is there.
- Optical oscillation part 5b is a light detection part 6 is a gasket type seal 6a is a gasket 6b is a ring-shaped retainer 6c is a guide ring 7 is a leak inspection hole 8 is a fixing bolt 9 is an optical fiber 9a is an optical fiber insertion hole 10 is a photodiode 11 is a plate made of a brittle fracture material (light transmission window).
- 11a is a light transmission plate made of sapphire 12 is a holding and fixing body 12a is a flange housing portion 12b is a bolt insertion hole 12c is a stepped portion 13 is a sealing surface 14 is a first fixing flange 14a is a stepped portion 14b is an insertion recess 14c is a bottom surface of the recess ( Seal surface) 14d is a gasket housing portion 16 is a second fixing flange 16a is a stepped portion 16b is a projecting portion 16c is a photodiode housing recess 16d is a tip surface (seal surface) of the projecting portion
- Reference numeral 17 denotes a recess 17a denotes a gasket housing part 18 denotes a light source device 18a denotes a reflected light detection device 18b denotes an output light detection device 19 denotes an arithmetic device 20 denotes a standard densitometer
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Abstract
Description
そのため、従前のこの種原料流体供給装置、例えば図9に示す如きバブリング型原料流体供給装置においては、温度制御された原料タンク21の原料蒸気出口の近傍に光分析方式の濃度計22を設け、当該濃度計22からの濃度検出信号によって原料タンク21の温度、キャリアガスCGの流量、タンク内蒸気圧力Po等を調整することにより、反応炉23へ所定の原料濃度のプロセスガス24(例えば、タンク21内に貯留したトリメチルガリウムTMGa等の有機金属材料蒸気を含んだプロセスガス)が供給されて行く。
尚、図9において、25は熱式マスフローコントローラ、26はタンク内圧の圧力調整装置である。
又、後者の特開2004-108981号においては、図11に示すように、光学セル(吸光セル)を内蔵したインラインセンサー33を管路31へ固定し、前記光学セルを透過した光の光度測定を行うようにしている。
しかし、光学セル27内の合成樹脂製シール材や銀蝋付け、金蝋付け等の部材は、各部材自体の内部に含有されているガスやパーティクルを有機原料ガス内へ放出する放出源になる危険性があり、現実に、パーティクルの放出によるガス純度の低下が生ずると云う問題がある。そのため、半導体製造用ガス供給系に於いては、銀蝋付けや金蝋付けの使用は望ましいことでない。
また、ガスケット型シールを用いているため、他の合成樹脂製シール材や銀蝋材、金蝋材等を用いるシール構造に比較して、流体内への不純物の混入を皆無にすることが出来る。
図1及び図2は、本発明の第1実施形態に係る原料流体濃度検出器1を示すものであり、当該原料流体濃度検出器1は、検出器本体2と、その両側部に固定した入口ブロック3及び出口ブロック4と、検出器本体2の上面側に並列状に設けた光発振部5a及び光検出部5bと、検出器本体2の下面側に設けた光検出部5b等から構成されている。
尚、原料濃度Cは、基本的には、分光光度計で求めた吸光度Aを基にして、次の(1)式により演算される。
A=log10(I0/I)=ε×C×I・・・(1)
但し、(1)式において、I0は光発振部5aからの入射光強度、Iは透過光強度(光検出部5bのフォトダイオード10への入射光強度)、εは原料のモル吸光係数、Cは原料濃度、Aは吸光度である。
そして、この第二固定フランジ16と第一固定フランジ14を一体化したものを保持固定体12のフランジ収容孔12a内へ挿入し、保持固定体12を固定用ボルト8によりガスケット型シール6を介設して検出器本体2へ押圧固定することにより、光発振部5a及び光検出部5bは検出器本体2へ気密に固定されている。
また、前記図1の実施形態においては、検出器本体2の上面側に光発振部5a及び光検出部5bを間隔を置いて設けるようにしているが、上面側の光検出部5bを省略し、且つ下面側の光検出部5bの凹部17と流体出口側とを流体通路2cにより直接連通しても良いことは勿論である。
更に、検出器本体2の上面側に光検出部5bを、下面側に光発振部5aを設ける、つまり、光発振部5aは入口に最も近い凹部に配置する以外に、別の凹部に設置することも可能であり、また、前記サファイア製光透過板11aに代えて、その他の材質、例えば石英ガラス等を使用することも可能である。
また、保持固定体12の下端部には、第一固定フランジ14の外周部上面に嵌合してこれを押圧するための段部12cが形成されており、フランジ収容孔12aの下方は拡径されて、第一固定フランジ14の収容部に形成されている。
又、縮径された突出部16bの先端部の先端面16dは、厚さ0.8~1.5mm程度の薄い光透過板11aに当接するシール面になっている。
更に、前記3段の段部14aの中間部は、サファイア製光透過板11aの収納部を成しており、ここにサファイア製光透過板11aが載置固定されている。
尚、第一固定フランジ14の下面側にはガスケット6aの収容部14dが形成されており、ここにガスケット型シール6の上半部が挿入固定される。
先ず、図8に示すように、半導体製造装置用のプロセスガス(有機原料TMGa蒸気)の供給管路へ原料流体濃度検出器1をインライン状に接続し、光源装置18より光ファイバ9を通して光発振部5aへ光を入射した。尚、光発振部5a及び光検出部5bのフォトダイオード10は、受光面1.0mm×1.1mm、直径504mm、高さ3.6mmに選定されている、また、サファイア製光透過板11aは、厚さ1.0mm、直径8.0mm、であり、更に、光発振部5aと光検出部5b間の流通路2bの長さは30mm、流路の内径は4.0mmΦに設定されている。
前記反射光検出装置18aからの検出出力は、演算装置19に於ける原料濃度検出値の補正に用いられ、これにより、光源装置18からの入射光の所謂揺らぎやサファイア製光透過板11aの光透過率の経年変化等により生ずる原料濃度の測定誤差が補正される。
2は検出器本体
2aは流体通路
2bは流体通路
2cは流体通路
3は入口ブロック
3aは流体通路
3bは継手部
4は出口ブロック
4aは流体通路
4bは継手部
5aは光発振部
5bは光検出部
6はガスケット型シール
6aはガスケット
6bはリング状リテイナー
6cはガイドリング
7は漏洩検査用孔
8は固定用ボルト
9は光ファイバ
9aは光ファイバ挿入孔
10はフォトダイオード
11は脆性破壊材料から成る板材(光透過窓)
11aはサファイア製光透過板
12は保持固定体
12aはフランジ収納部
12bはボルト挿入孔
12cは段部
13はシール面
14は第一固定フランジ
14aは階段部
14bは挿入凹部
14cは凹部の底面(シール面)
14dはガスケット収容部
16は第二固定フランジ
16aは階段部
16bは突出部
16cはフォトダイオード収納凹部
16dは突出部の先端面(シール面)
17は凹部
17aはガスケット収容部
18は光源装置
18aは反射光検出装置
18bは出力光検出装置
19は演算装置
20は標準濃度計
Claims (12)
- 検出器本体と、検出器本体の上面または下面に設けた光発振部及び光検出部とを備える光分析式原料流体濃度検出器であって、検出器本体には上面及び下面の其々に少なくとも一つの凹部が形成され、検出器本体の流体入口から凹部に連通する流体流路と、凹部間を連通する流体通路と、凹部から検出器本体の流体出口に連通する流体流路とを備え、少なくとも1つの凹部に光発振部が配置され、残りの凹部に光検出部が配置された、原料流体濃度検出器。
- 光発振部が、光透過板と、光強度検出用のフォトダイオードと、光発振用の光源(光ファイバ)とを備え、光検出部が、光透過板と、光強度検出用のフォトダイオードと、を備える、請求項1に記載の原料流体濃度検出器。
- 検出器本体に形成した凹部に配置する光透過板は、ガスケット型シールを用いて気密に固定されるようにした、請求項2に記載の原料流体濃度検出器。
- 検出器本体と、検出器本体の上面に設けた光発振部及び検出器本体の下面に設けた光検出部とを備える光分析式原料流体濃度検出器であって、検出器本体の上面及び下面に設けられ流体通路により連通された凹部と、当該凹部内に装着したガスケット型シールと、ガスケット型シールと対向して配置され、光透過板を気密に挟着して接合固定した第一固定フランジ及び第二固定フランジと、第二固定フランジ内に設けた光ファイバ及びフォトダイオードと、前記接合固定した両固定フランジをガスケット型シールを介して検出器本体の凹部内へ気密に固定する保持固定体と、を備える原料流体濃度検出器。
- 検出器本体と、検出器本体の上面に設けた光発振部と、検出器本体の下面に設けた光検出部とを備えた光分析式原料流体濃度検出器であって、前記検出器本体が、上面及び下面に夫々設けた凹部と、両凹部間を連通する流体通路と、流体入口と上面の凹部間を連通する流体通路と、流体出口と下面の凹部間を連通する流体通路を備え、また、前記光発振部及び光検出部の各々が、前記凹部に繋がるガスケット収容部内に装着したガスケット型シールと、内周面が階段状に縮径した挿入凹部を有し、前記ガスケット型シールと対向状に配置した第一固定フランジと、前記第一固定フランジの挿入凹部の最奥部に配置した光透過板と、前記第一固定フランジの挿入凹部内に階段状外周面を有する突出部を挿入して前記光透過板を挟んで前記第一固定フランジへ気密に接合固定した第二固定フランジと、第二固定フランジ内の前記光透過板の外側に配設固定した光強度検出用のフォトダイオードと、前記接合固定した両固定フランジを収容するフランジ収納部を中央に備え、固定用ボルトの締め込みによりフランジ収納部内に収納した両固定フランジをガスケット型シールを介して検出器本体へ気密に固定する保持固定体と、を備える原料流体濃度検出器。
- 第二固定フランジの突出部の先端面と、第一固定フランジの挿入凹部の底面を光透過板のシール面とした請求項5に記載の原料流体濃度検出器。
- 第一固定フランジのガスケット収容部の底面をガスケットシール面とした請求項5に記載の原料流体濃度検出器。
- 光発振部の第二固定フランジに光ファイバ挿入孔を設けると共に、フォトダイオードを光透過板からの反射光強度の検出用フォトダイオードとした請求項5に記載の原料流体濃度検出器。
- 光検出部の第二固定フランジに設けたフォトダイオードを光透過板からの透過光強度の検出用フォトダイオードとした請求項5に記載の原料流体濃度検出器。
- 検出器本体の上面に間隔を置いて他の光検出部を設けると共に、検出器本体の下面に設けた光検出部の凹部と前記他の光検出部の凹部間を流体通路により連通し、前記下面に設けた光検出部の光透過板からの反射光強度を前記他の光検出部にて検出するようにした請求項5に記載の原料流体濃度検出器。
- 原料流体を、析出性又は高反応性若しくは腐食性の有機原料蒸気とした請求項5に記載の原料流体濃度検出器。
- 光透過板をサファイア製光透過板とした請求項5に記載の原料流体濃度検出器。
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JPH11280967A (ja) * | 1998-03-31 | 1999-10-15 | Fujikin Inc | 流体継手 |
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JP3155842U (ja) * | 2009-09-18 | 2009-12-03 | テルモ株式会社 | 成分測定装置 |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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JPWO2016017122A1 (ja) * | 2014-07-29 | 2017-04-27 | 国立大学法人徳島大学 | インライン型濃度計測装置 |
KR20230140581A (ko) | 2021-07-31 | 2023-10-06 | 가부시키가이샤 후지킨 | 농도 측정 장치 |
Also Published As
Publication number | Publication date |
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KR20150093232A (ko) | 2015-08-17 |
TWI515421B (zh) | 2016-01-01 |
CN105247344B (zh) | 2018-11-13 |
TW201510501A (zh) | 2015-03-16 |
CN105247344A (zh) | 2016-01-13 |
KR101722013B1 (ko) | 2017-03-31 |
JP6326284B2 (ja) | 2018-05-16 |
US20160061704A1 (en) | 2016-03-03 |
US9651467B2 (en) | 2017-05-16 |
JP2014238391A (ja) | 2014-12-18 |
SG11201509120VA (en) | 2015-12-30 |
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