CN104769727A - Method and device for supplying hydrogen-selenide mixed gas - Google Patents
Method and device for supplying hydrogen-selenide mixed gas Download PDFInfo
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- CN104769727A CN104769727A CN201380052051.2A CN201380052051A CN104769727A CN 104769727 A CN104769727 A CN 104769727A CN 201380052051 A CN201380052051 A CN 201380052051A CN 104769727 A CN104769727 A CN 104769727A
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- hydrogen selenide
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- 229910000058 selane Inorganic materials 0.000 title claims abstract description 328
- SPVXKVOXSXTJOY-UHFFFAOYSA-N selane Chemical compound [SeH2] SPVXKVOXSXTJOY-UHFFFAOYSA-N 0.000 title claims abstract 35
- 238000000034 method Methods 0.000 title claims description 86
- 239000007789 gas Substances 0.000 claims abstract description 417
- 239000003595 mist Substances 0.000 claims description 196
- 238000004519 manufacturing process Methods 0.000 claims description 130
- 238000005259 measurement Methods 0.000 claims description 59
- 239000011261 inert gas Substances 0.000 claims description 47
- 238000012937 correction Methods 0.000 claims description 33
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 307
- 230000008569 process Effects 0.000 description 49
- 238000009434 installation Methods 0.000 description 35
- 239000011669 selenium Substances 0.000 description 14
- 229910052711 selenium Inorganic materials 0.000 description 13
- 238000011144 upstream manufacturing Methods 0.000 description 13
- 238000002425 crystallisation Methods 0.000 description 12
- 230000008025 crystallization Effects 0.000 description 12
- 102000003712 Complement factor B Human genes 0.000 description 11
- 108090000056 Complement factor B Proteins 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 238000009826 distribution Methods 0.000 description 8
- 238000001556 precipitation Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 238000010926 purge Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000012790 confirmation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000002571 modificatory effect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- DVRDHUBQLOKMHZ-UHFFFAOYSA-N chalcopyrite Chemical compound [S-2].[S-2].[Fe+2].[Cu+2] DVRDHUBQLOKMHZ-UHFFFAOYSA-N 0.000 description 1
- 229910052951 chalcopyrite Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000004087 circulation Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 229910052756 noble gas Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5846—Reactive treatment
- C23C14/5866—Treatment with sulfur, selenium or tellurium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/04—Binary compounds including binary selenium-tellurium compounds
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01F—MEASURING VOLUME, VOLUME FLOW, MASS FLOW OR LIQUID LEVEL; METERING BY VOLUME
- G01F25/00—Testing or calibration of apparatus for measuring volume, volume flow or liquid level or for metering by volume
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01F—MEASURING VOLUME, VOLUME FLOW, MASS FLOW OR LIQUID LEVEL; METERING BY VOLUME
- G01F25/00—Testing or calibration of apparatus for measuring volume, volume flow or liquid level or for metering by volume
- G01F25/10—Testing or calibration of apparatus for measuring volume, volume flow or liquid level or for metering by volume of flowmeters
- G01F25/15—Testing or calibration of apparatus for measuring volume, volume flow or liquid level or for metering by volume of flowmeters specially adapted for gas meters
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
- H01L31/0322—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312 comprising only AIBIIICVI chalcopyrite compounds, e.g. Cu In Se2, Cu Ga Se2, Cu In Ga Se2
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/186—Particular post-treatment for the devices, e.g. annealing, impurity gettering, short-circuit elimination, recrystallisation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/541—CuInSe2 material PV cells
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Organic Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Electromagnetism (AREA)
- Metallurgy (AREA)
- Computer Hardware Design (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Fluid Mechanics (AREA)
- Chemical Vapour Deposition (AREA)
- Photovoltaic Devices (AREA)
- Flow Control (AREA)
- Fuel Cell (AREA)
Abstract
A calibration gas is caused to flow, at the same flow rate, through a flow control means that has been disposed in a feed gas supply channel and that controls the flow rate of hydrogen selenide gas which is a feed gas and through a flow rate measuring means for calibration. The set value of the flow rate of the hydrogen selenide gas which is caused to flow by the flow control means is corrected in accordance with the difference between the calibration-gas flow rate amounts measured respectively by the flow control means and the flow rate measuring means.
Description
Technical field
The present invention relates to supply method and the feedway of hydrogen selenide mist.
The application requires priority based on October 22nd, 2012 in No. 2012-232832, the Patent of Japanese publication, and here cites its content.
Background technology
In recent years, due to environmental pollution, global warming, fossil fuel these problems exhausted, solar cell receives publicity as substitute energy source for petroleum.The main flow of current solar cell is following compound solar cell: it comprises copper, indium, gallium and selenium, and uses by using hydrogen selenide (H
2se) the chalcopyrite light absorbing zone formed.The manufacturing installation to this compound solar cell is needed to supply the hydrogen selenide mist that adjusted is normal concentration.
But, in order to realize a large amount of productions of compound solar cell, need a large amount of hydrogen selenide mists to be supplied to solar cell manufacturing installation.Therefore, when use be filled with the gas bomb of the mist that adjusted is normal concentration time, there is replacement frequency because of gas bomb many and the problem of enough gas delivery volumes cannot be guaranteed.
In order to solve the problem, used the feedway (hereinafter simply referred to as " feedway ") 201 of hydrogen selenide mist as shown in Figure 4 in the past.Basic gas supplying path L101 and unstrpped gas feed path L102 is provided with in feedway 201.The hydrogen selenide gas of inert gas and concentration 100% (after, be only called " hydrogen selenide gas ") can circulate in each path respectively.In addition, on basic gas supplying path L101 and unstrpped gas feed path L102, basic gas flow rate control unit 106 and raw material gas flow control unit 111 is respectively arranged with.And, in the downstream of basic gas supplying path L101 and unstrpped gas feed path L102, be provided with the surge tank 118 for storing inert gas and the mixed hydrogen selenide mist of hydrogen selenide gas.
(following at the supply method of the hydrogen selenide mist using feedway 201, be only called " supply method ") in, utilize basic gas flow rate control unit 106 and raw material gas flow control unit 111 to control the flow of inert gas and hydrogen selenide gas respectively, make the hydrogen selenide concentration of hydrogen selenide mist be setting.Afterwards, the inert gas after controlling by blender 117 mixed traffic and hydrogen selenide gas, thereafter, be stored in the hydrogen selenide mist obtained in surge tank 118.The hydrogen selenide mist being stored in the regulation hydrogen selenide concentration in surge tank 118 is supplied by the continuous manufacturing installation to solar cell.
But, in feedway 201, there is following problem.That is, there is the problem in unstrpped gas supply line L102, open and close valve 109,113 and the raw material gas flow control unit 111 etc. that selenium (Se) crystallization that the selfdecomposition because of hydrogen selenide causes flows through to hydrogen selenide gas.Especially, there is following problem: because selenium crystallization is in raw material gas flow control unit 111, thus the flow measurement precision of raw material gas flow control unit 111 and flow control accuracy reduce, its result, the concentration set point of the hydrogen selenide mist preset and the difference comparatively large (being referred to as shift phenomenon) of the concentration measured value of the actual hydrogen selenide mist adjusted by feedway 201.
As the technology suppressing this shift phenomenon, such as, Patent Document 1 discloses supply method and the feedway of the hydrogen selenide mist that stably can supply concentration set point.As shown in Figure 5, the feedway 202 of patent documentation 1, on the architecture basics of the feedway 201 shown in Fig. 4, possesses the bypass flow path L105 be communicated with unstrpped gas supply line L102 by basic gas supply line L101.And, Patent Document 1 discloses following supply method: under the state not using bypass flow path L105, manufacture mist and after being stored into surge tank 118, the hydrogen selenide gas of ormal weight is exported to surge tank 118 from unstrpped gas supply line L102, further, via bypass flow path L105, the inert gas of ormal weight is derived from unstrpped gas supply line L102, make the hydrogen selenide mist of regulation hydrogen selenide concentration thus, and the volumetric concentration making hydrogen selenide residual in unstrpped gas supply line L102 is less than 10%.
Patent documentation 1: No. 2011/045983A1st, International Publication
But, in the supply method that patent documentation 1 is recorded, there is following problem: when via bypass flow path L105, when deriving the hydrogen selenide gas in unstrpped gas supply line L102 with inert gas, such as requirement as the careful instrumentation with 0.1 second unit enforcement valve events.In addition now, vary to significantly close to 0% from the hydrogen selenide concentration of unstrpped gas supply line L102 effluent air from 100%.Therefore, if having the variation wanting the hydrogen selenide concentration suppressed in surge tank, then the problem of jumbo surge tank is needed.
Further, in the method for document 1, only when not supplying hydrogen selenide mist to unstrpped gas supply line L102, the volumetric concentration that can make hydrogen selenide residual in unstrpped gas supply line L102 is less than 10%, when supplying hydrogen selenide mist, the precipitation of selenium crystallization in unstrpped gas supply line L102 cannot be prevented completely.Therefore, make feedway 202 long-term work if had, occur the problem of shift phenomenon.
Summary of the invention
Therefore, the object of the present invention is to provide a kind of supply method and feedway of hydrogen selenide mist, it does not need careful instrumentation and jumbo surge tank, can suppress shift phenomenon for a long time, to supply the hydrogen selenide mist of stable hydrogen selenide concentration.
In order to solve the problem, as the 1st aspect of the present invention, provide method below.
Namely, (1) a kind of supply method of hydrogen selenide mist is provided, have: the inert gas from basic gas supply line supply is mixed with the hydrogen selenide gas supplied from unstrpped gas supply line, manufactures the operation of the hydrogen selenide mist being mixed with normal concentration; With the operation of the described mist of supply, the feature of the supply method of described hydrogen selenide mist is, during being included in the operation stopping manufacturing hydrogen selenide mist further, revise the operation of the flow setting value of unstrpped gas, described correction operation comprises: the calibration gas of same flow is flow through and is arranged at described unstrpped gas supply line with the operation of the flow controlling unit of the flow controlling unit and correction that control the flow of described hydrogen selenide gas; Obtain the operation of the difference of the flow value of the described calibration gas measured respectively by described flow controlling unit and described airflow measurement unit; With according to described difference, revise the operation of flow value of the described hydrogen selenide gas that described flow controlling unit flows out.
The mode of above-mentioned (1) preferably has feature below.
(2) described calibration gas is made to continue to flow through described flow controlling unit and described airflow measurement unit by different order.
(3) described flow controlling unit and described airflow measurement unit are used to the flow-measuring method of same specification.
(4) in above-mentioned (1) in the either type in (3), use described inert gas as described calibration gas.
(5) in above-mentioned (1) in the either type in (4), when manufacture described hydrogen selenide mist time, do not make described hydrogen selenide gas flow through correct described airflow measurement unit.
(6) as the 2nd aspect of the present invention, device is below provided.
Namely, a feedway for hydrogen selenide mist, mixes the inert gas from basic gas supply line supply with the hydrogen selenide gas supplied from unstrpped gas supply line, manufactures the hydrogen selenide mist being mixed with normal concentration, supply this hydrogen selenide mist afterwards
The feature of the feedway of described hydrogen selenide mist is to possess: flow controlling unit, is arranged at described unstrpped gas supply line to control the flow of described hydrogen selenide gas; Calibration gas supply line, when stopping manufacturing described hydrogen selenide mist, supplies the primary side of calibration gas to the described flow controlling unit of described unstrpped gas supply line; The airflow measurement unit corrected, is arranged at the described calibration gas when stopping manufacturing described hydrogen selenide mist and flows through and when the described hydrogen selenide mist of manufacture on the stream that do not flow through of described hydrogen selenide gas; And control unit, when making the described calibration gas of same flow flow through described flow controlling unit and described airflow measurement unit, according to the difference of the flow value of the calibration gas measured respectively, the flow value of the described hydrogen selenide gas that modified flow rate control unit flows out.
(7) in above-mentioned (6), described calibration gas supply line is provided with the first open and close valve, described first open and close valve is closed condition when manufacturing described hydrogen selenide mist, be open mode when described calibration gas is supplied to described unstrpped gas supply line from described calibration gas supply line, the primary side of described first open and close valve of described calibration gas supply line is provided with described airflow measurement unit.
(8) in above-mentioned (6), described calibration gas supply line is the bypass flow path described basic gas supply line be connected with the primary side of the described flow controlling unit of described unstrpped gas supply line.
(9) in above-mentioned (8), described bypass flow path is provided with the first open and close valve, described first open and close valve is closed condition when manufacturing described hydrogen selenide mist, be open mode when described inert gas is supplied to described unstrpped gas supply line as calibration gas from described basic gas supply line, the primary side of described first open and close valve of described bypass flow path is provided with described airflow measurement unit.
(10) in above-mentioned (6) or (8), the primary side of the described flow controlling unit of described unstrpped gas supply line is provided with branch flow passage, described branch flow passage is provided with the second open and close valve, described second open and close valve is closed condition when manufacturing described hydrogen selenide mist, be open mode when described inert gas is supplied to described unstrpped gas supply line as calibration gas from described basic gas supply line, the primary side of described second open and close valve of described branch flow passage is provided with described airflow measurement unit.
(11) in above-mentioned (6) in the either type in (10), described flow controlling unit and described airflow measurement unit are the flow-measuring method of same specification.
According to the supply method of hydrogen selenide mist of the present invention, the calibration gas of same flow is flow through be arranged at hydrogen selenide gas supply line as unstrpped gas with the flow controlling unit controlling the flow of hydrogen selenide gas and the airflow measurement unit corrected.And, be the formation of the difference of the flow value according to the calibration gas measured respectively by flow controlling unit and airflow measurement unit, the flow value of the hydrogen selenide gas that modified flow rate control unit flows out.According to this formation, can calibration gas be utilized, the hydrogen selenide gas of being detained in unstrpped gas supply line is derived in described unstrpped gas supply line.Therefore, it is possible to reduce the precipitation of the selenium crystallization caused by the selfdecomposition of hydrogen selenide.In addition, can based on the flow value of the calibration gas measured by the airflow measurement unit corrected, the flow value of the hydrogen selenide gas that modified flow rate control unit flows out.Therefore, it is possible to the flow measurement error greatly reduced in unstrpped gas supply line and flow control error, thus suppress shift phenomenon.Therefore, do not need the surge tank of careful instrumentation and large volume, can chronically the hydrogen selenide mist of stable hydrogen selenide concentration be supplied in the consumer device of the primary side of solar cell manufacturing installation etc.
In addition, the feedway of hydrogen selenide mist of the present invention has structure below.That is, possess: flow controlling unit, be arranged at unstrpped gas supply line to control the flow of hydrogen selenide gas; Bypass flow path, when stopping manufacturing hydrogen selenide mist, supplies inert gas from basic gas supply line to the primary side of the flow controlling unit of unstrpped gas supply line as calibration gas; The airflow measurement unit corrected, is arranged at the calibration gas when stopping manufacturing hydrogen selenide mist and flows through, on the stream that hydrogen selenide gas does not flow through when manufacturing hydrogen selenide mist; And control unit, when making the calibration gas of same flow flow through flow controlling unit and airflow measurement unit, according to the difference of the flow value of the calibration gas measured respectively, the set point of the flow of the hydrogen selenide gas that modified flow rate control unit flows out.Above-mentioned supply method can be implemented by the feedway possessing described structure.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the feedway 101 of the hydrogen selenide mist represented as one embodiment of the present invention.
Fig. 2 is the figure of the service time of the hydrogen selenide mist represented in embodiment and the relation of hydrogen selenide concentration.
Fig. 3 is the figure of the service time of the hydrogen selenide mist represented in embodiment and the relation of flow error A.
Fig. 4 is the schematic diagram of the feedway 201 representing existing hydrogen selenide mist.
Fig. 5 is the schematic diagram of the feedway 202 representing another hydrogen selenide mist existing.
Fig. 6 is the schematic diagram of the feedway 102 of the hydrogen selenide mist represented as another embodiment of the present invention.
Fig. 7 is the schematic diagram of the feedway 103 of the hydrogen selenide mist represented as another embodiment of the present invention.
Embodiment
Below, accompanying drawing is utilized to be described in detail to as the supply method of hydrogen selenide mist and the feedway of hydrogen selenide mist that apply one embodiment of the present invention.
In addition, in the accompanying drawing that explanation below uses, for ease of understanding feature, sometimes amplify the part representing constitutive characteristic for simplicity, the dimensional ratios of each structural element etc. may not be identical with reality.In addition, the present invention is not limited to example below.Also can within the scope of the invention, carry out as required changing, omit, convert and/or adding.The quantity of device and position also can be changed as required.In addition, about unit adopted in this manual, concentration represents volumetric concentration, and pressure representative gauge pressure, flow represents volume flow.And then the volume is in this manual the volume under standard state (0 DEG C, 1atm (atmospheric pressure)).In addition, in the present invention, the record of so-called " unit " can indication device, operation, parts, system and part etc.
(feedway of hydrogen selenide mist)
First, as the feedway towards solar cell manufacturing installation, the structure for the feedway (hereinafter simply referred to as feedway) 101 of the hydrogen selenide mist of present embodiment is being described with reference to while Fig. 1.In addition, the feedway towards solar cell manufacturing installation is described at this, if but feedway of the present invention is the feedway of the device towards consumption hydrogen selenide mist, is not particularly limited, thus the feedway of any device towards consumption hydrogen selenide mist can be used in.Such as, the feedway etc. towards semiconductor-fabricating device consumed as impurity gas by hydrogen selenide mist is listed as an example.In addition, about statements such as " the device B of facing device A ", the device B prepared separately with device A can be represented, or also can represent the part as device A and the device B comprised.
As shown in Figure 1, feedway 101 is the conditions of production according to solar cell manufacturing installation (not shown), manufactures and supplies the device being formulated as the hydrogen selenide mist of normal concentration to solar cell manufacturing installation.Specifically, feedway 101 is configured to possess substantially: basic gas supply line L1, unstrpped gas supply line L2, mass flow controller (flow controlling unit) 6 and 11, blender 2 and surge tank 3.More specifically illustrate, then feedway 101 is configured to possess substantially: basic gas supply line L1, for supplying basic gas; Unstrpped gas supply line L2, for base feed gas; Mass flow controller 6, for controlling the flow of basic gas; Mass flow controller 11, for controlling the flow of unstrpped gas; Blender 2, the unstrpped gas after controlling for mixed traffic and basic gas; With surge tank 3, store the hydrogen selenide mist of unstrpped gas and the basic gas mixed by blender 2.
More specifically, feedway 101 possesses bypass flow path L3, mass flowmenter (airflow measurement unit) 16 and control unit 19 further.More specifically illustrate, then the feature of feedway 101 is, possess: bypass flow path L3, when stopping manufacturing hydrogen selenide mist, for basic gas is supplied as calibration gas from basic gas supply line L1 to the primary side (upstream side) of the mass flow controller 11 unstrpped gas supply line L2; Mass flowmenter 16, when manufacturing hydrogen selenide mist, for measuring the flow of the calibration gas being supplied to the stream that unstrpped gas does not flow through; With control unit 19, when making the calibration gas of same flow flow through mass flow controller 11 and mass flowmenter 16, for the difference of the flow value according to the calibration gas measured respectively, revise the flow value flowing through the unstrpped gas of mass flow controller 11.
(basic gas supply line L1)
One end of basic gas supply line L1 is connected with not shown basic supplies for gas, and the other end is connected with blender 2.If basic gas is the inert gas for diluting, be not particularly limited.As the inert gas used in the present invention, such as nitrogen (N can be enumerated
2) rare gas etc. such as gas or argon (Ar), helium (He) and neon (Ne).
On basic gas supply line L1, from upstream side towards downstream, be disposed with open and close valve 4, pressure regulator 5, mass flow controller 6, check-valves 7 and automatic valve 8.In addition, also can as required, at the upstream side of pressure regulator 5 and downstream, not shown Pressure gauge is set.By arranging this Pressure gauge, visual confirmation can be carried out to the pressure of the front and back of pressure regulator 5.
Open and close valve 4 is opened when basic gas is supplied to the downstream of open and close valve 4, and is closed when not supplying.
Pressure regulator 5 is arranged for the pressure of inert gas that supplies from basic supplies for gas to the pressure of hope.In the feedway 101 of present embodiment, pressure regulator 5 is only provided with one on basic gas supply line L1.But be not limited to one, pressure regulator 5 also can arrange two or more at the optional position of stream L1.
In addition, the pressure being about to the gas arrived in the stream L1 before mass flow controller 6 suitably can set according to the supply pressure to solar cell manufacturing installation.Such as, as the pressure being about to the gas arrived before mass flow controller 6, the scope of 0.3 ~ 0.8MPa can be set to.
Mass flow controller 6 be measure basic gas mass flow and carry out the flow control instrument of flow control, be arranged for high-precision flow measurement and control.
In addition, mass flow controller 6 controls the flow of inert gas, makes the hydrogen selenide concentration in the hydrogen selenide mist mixed by blender 2 maintain setting.
Exemplified with the feed unit 101 being provided with a mass flow controller 6 on basic gas supply line L1 in Fig. 1, but the present invention is not limited thereto.Such as, also two or more mass flow controller 6 can be set up in parallel on basic gas supply line L1.
Mass flow sensor is mounted with in mass flow controller 6.The mass flow sensor being loaded into mass flow controller 6 is not particularly limited, such as, can adopt the mass flow sensor that thermal type mass flow sensor, differential pressure type mass flow transducer and Coriolis formula mass flow sensor etc. are common.
Check-valves 7 makes the inert gas after by mass flow controller 6 flow control only move from upstream side to downstream effluent, and prevents the adverse current of inert gas upstream side from downstream.Thereby, it is possible to alleviate the variation of the basic gas flow in basic gas supply line L1.
Automatic valve 8 is arranged for control and whether is supplied to blender 2 by by the inert gas after mass flow controller 6 flow control.When automatic valve 8 is open mode, the inert gas after flow control is discharged to the downstream of automatic valve 8, and is supplied to blender 2.On the other hand, when automatic valve 8 is closed condition, stop inert gas to the supply in the downstream of automatic valve 8, inert gas can not be supplied to blender 2.The open and-shut mode of automatic valve 8 switches according to the pressure of the surge tank 3 measured by Pressure gauge 22.
(unstrpped gas supply line L2)
One end of unstrpped gas supply line L2 is connected with not shown unstrpped gas supply source, and the other end is connected with blender 2.Unstrpped gas is hydrogen selenide gas.
Unstrpped gas supply line L2 is provided with mass flow controller 11, and is connected with the branch flow passage L4 branched out from unstrpped gas supply line L2 on the unstrpped gas supply line L2 of primary side (downstream) being positioned at mass flow controller 11.
In addition, on unstrpped gas supply line L2, from upstream side towards downstream, be disposed with automatic valve 9, pressure regulator 10, mass flow controller 11, check-valves 12 and automatic valve 13.Identical with basic gas supply line L1, the Pressure gauge of not shown any amount also can be set at the upstream side of pressure regulator 10 and downstream as required.By arranging this Pressure gauge, visual confirmation can be carried out to the pressure of the front and back of pressure regulator 10.
About the explanation of automatic valve 9, pressure regulator 10, check-valves 12 and automatic valve 13, with be almost identical after hydrogen selenide gas by the open and close valve 4 of basic gas supply line L1, pressure regulator 5, check-valves 7 and the inert gas replacement in the explanation of automatic valve 8, therefore omit the description.
Mass flow controller 11 measures the mass flow the flow control instrument carrying out flow control that flow through the hydrogen selenide gas of stream L2, is arranged for and carries out high-precision flow measurement and control.
In addition, mass flow controller 11 controls the flow of hydrogen selenide gas, makes the hydrogen selenide concentration in the hydrogen selenide mist mixed by blender 2 be setting.
In addition, utilizing mass flow controller 11, when stopping manufacturing hydrogen selenide mist, carrying out flow control and the mass flow metering of the calibration gas supplied to the primary side (upstream side) of mass flow controller 11 via bypass flow path L3.
Further, mass flow controller 11 is connected with control unit 19 by distribution E1 described later, the measurement result of the flow of calibration gas (flow measurements) can be sent to control unit 19 from mass flow controller 11.In control unit 19 when obtain required for information time perform operation, its result can be made to be reflected in the control of mass flow controller 11.
Exemplified with the feedway 101 being provided with a mass flow controller 11 on unstrpped gas supply line L2 in Fig. 1, but the present invention is not limited thereto.Such as, also two or more mass flow controller 11 can be set up in parallel on unstrpped gas supply line L2.
Mass flow sensor is mounted with in mass flow controller 11.The mass flow sensor being loaded into mass flow controller 11 is not particularly limited, such as, can adopt the mass flow sensor that thermal type mass flow sensor, differential pressure type mass flow transducer and Coriolis formula mass flow sensor etc. are common.In addition, preferred mass flow controller 11 utilizes the hydrogen selenide gas as unstrpped gas to carry out flux modification, but is not particularly limited to this, and the gas beyond hydrogen selenide gas also can be utilized to correct.
(blender 2)
The position that the other end of the other end and unstrpped gas supply line L2 that blender 2 is arranged at basic gas supply line L1 collaborates.Blender 2 can mix by the inert gas of basic gas supply line L1 supply and manufacture by the hydrogen selenide gas that unstrpped gas supply line L2 supplies the hydrogen selenide mist that adjusted is normal concentration, and the gas produced is supplied to downstream, be not particularly limited, can select arbitrarily.By blender 2, prevent inert gas to the inflow of unstrpped gas supply line L2 and hydrogen selenide gas to the inflow of basic gas supply line L1.
(stream L5)
Blender 2 is connected by stream L5 with surge tank 3.In addition, also not shown open and close valve can be set on stream L5.
Be connected with blender 2 with one end of unstrpped gas supply line L2 exemplified with one end of basic gas supply line L1 in Fig. 1, and the feedway 101 of stream L5 is set between blender 2 and surge tank 3.But the present invention is not limited thereto.Such as, also can be the feedway not having blender 2, or also can be do not have blender 2 with stream L5 and the feedway that is directly connected with surge tank 3 respectively with one end of unstrpped gas supply line L2 of basic gas supply line L1.That is, the mixing of gas also can be carried out in tank.
(surge tank 3)
Surge tank 3 is the accumulator tank for storing the hydrogen selenide mist being adjusted to normal concentration by blender 2.The internal volume of surge tank 3 is not particularly limited, and suitably can select according to the quantity delivered of hydrogen selenide mist to solar cell manufacturing installation.The storage capacity of hydrogen selenide mist in surge tank 3 can be suitably selected to the quantity delivered of solar cell manufacturing installation according to the internal volume of surge tank 3 and hydrogen selenide mist.Such as, when being 100 ~ 200L/min to the hydrogen selenide mist quantity delivered of solar cell manufacturing installation, surge tank inner capacities can be set to 20 ~ 400L.
Pressure upper limit and the threshold pression of surge tank 3 are not particularly limited, and suitably can select according to the storage capacity of hydrogen selenide mist in surge tank 3 and hydrogen selenide mist to the quantity delivered of solar cell manufacturing installation.Such as, the pressure store of the hydrogen selenide mist in surge tank 3 can be set to the scope of 0.1 ~ 0.5Mpa.
(stream L6)
Surge tank 3 is connected with one end of stream L6, and the other end of stream L6 is the outlet of mist, and this outlet is connected with solar cell manufacturing installation.Thereby, it is possible to supply hydrogen selenide mist from surge tank 3 to solar cell manufacturing installation.In addition, at the upstream position of the outlet of stream L6, namely the supply port side of stream L6 is provided with open and close valve 21.
When hydrogen selenide mist is supplied to solar cell manufacturing installation from surge tank 3, open open and close valve 21.On the other hand, when hydrogen selenide mist not being supplied to solar cell manufacturing installation from surge tank 3, close open and close valve 21.
In addition, when hydrogen selenide mist is supplied to solar cell manufacturing installation with constant pressure, also not shown pressure regulator can be set on stream L6.
In addition, when hydrogen selenide mist is supplied to multiple solar cell manufacturing installation, also two or more open and close valve 21 can be set.Now, stream L6 branch can be made.
(stream L7)
In addition, surge tank 3 is connected with one end of stream L7, the other end of stream L7 is connected with Pressure gauge 22.Pressure gauge 22 can be utilized to measure the pressure of the hydrogen selenide mist in surge tank 3.In addition, stream L7 is provided with open and close valve 23.Open and close valve 23 opens usually.
Further, preferably on surge tank 3, not shown vacuum pump etc. is connected with.Thus, when removing the purge gas such as nitrogen residual in surge tank 3, can be exhausted purge gas by vacuum pump.
(omission of surge tank)
In addition, also surge tank 3 can be omitted in the present invention.Concerning not adopting the feedway of the present embodiment of surge tank 3 (not shown), the stream L5 shown in Fig. 1 is directly connected with stream L6, thus also can not arrange the stream L7, Pressure gauge 22 and the open and close valve 23 that are connected with surge tank 3.
(bypass flow path L3)
One end of bypass flow path L3 is connected with basic supplies for gas or basic gas supply line L1, and the other end is connected with the stream L2 of the primary side (upstream side) being positioned at mass flow controller 11.Bypass flow path L3 is provided with automatic valve (the first open and close valve) 14.Automatic valve 14 is closed condition when manufacturing hydrogen selenide mist, and is open mode stopping when manufacturing hydrogen selenide mist.When automatic valve 14 is open mode, calibration gas supplies to unstrpped gas supply line L2 from basic gas supply line L1 via bypass flow path L3.
By arranging bypass flow path L3 and automatic valve 14, when stopping manufacturing hydrogen selenide mist, unstrpped gas supply line L2 is communicated with basic gas supply line L1.When manufacturing hydrogen selenide mist, unstrpped gas supply line L2 is not communicated with basic gas supply line L1.Therefore, when manufacturing hydrogen selenide mist, because unstrpped gas supply line L2 is not communicated with basic gas supply line L1, therefore hydrogen selenide gas can not flow to the primary side (upstream side) of the automatic valve 14 of bypass flow path L3.
Calibration gas is the gas of the hydrogen selenide gas not comprising high concentration, be then not particularly limited.Calibration gas can be selected arbitrarily.As calibration gas, such as preferred inert gas or take noble gas component as the gas of principal component.In addition, in FIG exemplified with the structure inert gas being supplied to basic gas supply line L1 from basic supplies for gas being used as calibration gas.But, also can one end of bypass flow path L3 inert gas supply source of being connected to the not shown calibration gas supply source arranged separately or sharing with other devices, calibration gas (with reference to Fig. 7) is supplied from these supply sources to bypass flow path L3.But in order to prevent the maximization of feedway 101 and not need additional calibration gas supply source, one end of preferred bypass flow path L3 is connected with basic gas supply line L1.
In addition, one end of bypass flow path L3 and the link position of basic gas supply line L1 are not particularly limited.But one end of bypass flow path L3 is preferably connected with basic gas supply line L1 in the mode be connected near the position of basic supplies for gas.According to this structure, when calibration gas flows through basic gas supply line L1, impurity can be prevented to be mixed in calibration gas.
Further, also can not shown pressure regulator be set on bypass flow path L3.
(branch flow passage L4)
One end of branch flow passage L4 is connected with the unstrpped gas supply line L2 of the primary side (downstream) of mass flow controller 11, and the other end is connected with not shown discharge duct.On branch flow passage L4, from upstream side towards downstream, be disposed with automatic valve (the second open and close valve) 15 and mass flowmenter 16.Automatic valve 15 is closed condition when manufacturing hydrogen selenide mist, and is open mode stopping when manufacturing hydrogen selenide mist.When automatic valve 15 is open mode (when stopping manufacturing hydrogen selenide mist), calibration gas supplies to branch flow passage L4 from basic gas supply line L1 via bypass flow path L3 and unstrpped gas supply line L2.
When manufacturing hydrogen selenide mist, branch flow passage L4 and unstrpped gas supply line L2 is blocked by automatic valve 15.Further, when stopping manufacturing hydrogen selenide mist, branch flow passage L4 and unstrpped gas supply line L2 is not blocked by automatic valve 15, and namely branch flow passage L4 is communicated with unstrpped gas supply line L2.When manufacturing hydrogen selenide mist, because branch flow passage L4 and unstrpped gas supply line L2 is truncated, therefore hydrogen selenide gas can not flow to the primary side of the automatic valve 15 of branch flow passage L4.
Mass flowmenter 16 is the flowrate measuring tool of the mass flow of metering calibration gas.Specifically, the flow that the calibration gas of mass flow controller 11 is flow through in metering is arranged for.
In addition, in order to revise the flow value of hydrogen selenide gas in mass flow controller 11 more accurately, the mass flow controller 16 of present embodiment is preferably arranged on the stream that hydrogen selenide gas does not flow through when manufacturing hydrogen selenide mist.Can prevent selenium crystallization from separating out to mass flowmenter 16.Specifically, as shown in Figure 1, mass flowmenter 16 is preferably arranged on when manufacturing hydrogen selenide mist is the primary side (downstream) of the automatic valve 15 of closed condition.
Utilizing mass flowmenter 16, when stopping manufacturing hydrogen selenide mist, measuring the mass flow of the calibration gas supplied to branch flow passage L4 via bypass flow path L3 and unstrpped gas supply line L2.This calibration gas, when flowing through unstrpped gas supply line L2, flows through mass flow controller 11.
Preferably in mass flowmenter 16, be mounted with mass flow sensor.
The mass flow sensor being loaded into mass flowmenter 16 is not particularly limited, such as, can adopt the mass flow sensor that thermal type mass flow sensor, differential pressure type mass flow transducer and Coriolis formula mass flow sensor etc. are common.
(control unit 19 and distribution E1 and E2)
Mass flowmenter 16 is connected with control unit 19 by distribution E2.That is, the flow measurements to the calibration gas of branch flow passage L4 supply can be sent to control unit 19 from mass flowmenter 16 by distribution E2.
In addition, as aforementioned, control unit 19 is also connected with the distribution E1 be connected with mass flow controller 11.
In mass flow controller 11 and mass flowmenter 16, measure the flow value of calibration gas respectively, and be sent to control unit 19.Therefore, in control unit 19, obtain the difference of the flow value of the calibration gas measured.Control unit 19 can send data for revising to mass flow controller 11.So, utilizing the difference that obtains, when recovering the manufacture of hydrogen selenide mist, revising the flow value of the hydrogen selenide gas that the primary side (downstream) to mass flow controller 11 flows.Mass flow controller 11 and mass flowmenter 16 are more preferably the identical mass flow sensor of flow measurement range, are particularly preferably the mass flow sensor carrying out flux modification with the gas of same composition further.
Such as, if mass flow controller 11 is mounted with thermal type mass flow sensor, and the gamut carrying out the flow measurement corrected with hydrogen selenide is the specification of 10 [L/min], then particularly preferably use identical for mass flowmenter 16, that is, thermal type mass flow sensor is mounted with and the gamut carrying out the flow measurement corrected with hydrogen selenide is the specification of 10 [L/min].
As the instrument being used as mass flow controller 11 and mass flowmenter 16, by so selecting similar or identical instrument, following effect can be obtained.Namely, about the flow measurements of the calibration gas measured by mass flow controller 11 and mass flowmenter 16, flow rate conversion process required when not needing to carry out using heterogeneous gas, after measurement update gas, can directly utilize control unit 19, for mass flow controller 11 calculates the correction of the flow value of hydrogen selenide gas or the flow value of revised hydrogen selenide gas.
Control unit 19 receives the flow value of the calibration gas measured separately by mass flow controller 11 and mass flowmenter 16.In addition, control unit 19 is according to the difference of the flow value of each calibration gas received, calculate the correction of the flow value of the hydrogen selenide gas set by mass flow controller 11 or the flow value of revised hydrogen selenide gas, and pass to mass flow controller 11.
In addition, when stopping manufacturing hydrogen selenide mist, the flow measurements of calibration gas is measured by mass flow controller 11 and mass flowmenter 16.Afterwards, when recovering the manufacture of hydrogen selenide mist, the flow setting value of flow value as mass flow controller 11 of the correction of hydrogen selenide gas will be added.
Control unit 19 can calculate the correction of the flow value of hydrogen selenide gas or the flow value of revised hydrogen selenide gas, is not particularly limited.Can choice for use arithmetic unit or system arbitrarily.As this control unit 19, such as, can use the common computer or programmable logic controller with central operation processing unit.
(supply method of hydrogen selenide mist)
Below, the supply method (hereinafter simply referred to as " supply method ") of the hydrogen selenide mist using the present embodiment of feedway 101 is described.
The supply method of present embodiment comprises following process.
First, in blender 2, the inert gas by mass flow controller 6 flow control is mixed with the mixed raw material gas by mass flow controller 11 flow control, to become the hydrogen selenide concentration set point of regulation, thus manufacture hydrogen selenide mist.And, the mist produced is stored in (manufacture process (I) of hydrogen selenide mist) in surge tank 3.
Afterwards, this hydrogen selenide mist in surge tank 3 is supplied to the consumer device (the supply process (III) of hydrogen selenide mist) being arranged in primary side that be arranged at the back segment of feedway 101, solar cell manufacturing installation etc.
After the manufacture process of hydrogen selenide mist, that is, after the manufacture stopping hydrogen selenide mist, make the calibration gas of same flow, preferably make identical calibration gas, flow through mass flow controller 11 and mass flowmenter 16.According to the difference of the flow value of the calibration gas measured respectively by mass flow controller 11 and mass flowmenter 16, revise the flow value (makeover process (II) of the flow setting value of unstrpped gas) flowing through the hydrogen selenide gas of mass flow controller 11.
At this, as the consumer device of primary side (downstream) being positioned at hydrogen selenide mist, describe solar cell manufacturing installation, but can be the device of any consumption hydrogen selenide mist.Such as, the semiconductor-fabricating device etc. of consumption hydrogen selenide mist as impurity gas can be enumerated.
(manufacture set-up procedure)
First, the preparation before the manufacture of hydrogen selenide mist is carried out.Specifically, the feedway 101 shown in set-up dirgram 1, in the apparatus, makes the purge gas circulations such as nitrogen, carry out the purging in stream to open and close valve 4,21,23 and automatic valve 9 while carrying out opening and closing operations.After completing above-mentioned purging, automatic valve 14,15 is set to closed condition, and all open and close valves except automatic valve 14,15 and automatic valve are set to open mode, complete to manufacture preparing.
In addition, preferably the purge gas such as nitrogen residual in surge tank 3 are removed in advance.Such as, not shown vacuum pump etc. is preferably used to carry out vacuum exhaust from the not shown vacuum exhaust valve etc. be connected with surge tank 3.
(manufacture process (I) of hydrogen selenide mist)
Then, supply inert gas from basic gas supply line L1 to blender 2, supply hydrogen selenide gas from unstrpped gas supply line L2 to blender 2.That is, by flow (the flow setting value V of inert gas
1[L/min]) and flow (the flow setting value V of hydrogen selenide gas
2[L/min]) control to supply while the flow preset.
More specifically, control the flow of inert gas and the flow of hydrogen selenide gas respectively, make to become from preset, set point (hydrogen selenide concentration C [%], the C=V of hydrogen selenide concentration the hydrogen selenide mist that is supplied to solar cell manufacturing installation
2/ (V
1+ V
2) × 100) in each flow of determining.So, supply inert gas from basic gas supply line L1 to blender 2, supply hydrogen selenide gas from unstrpped gas supply line L2 to blender 2.
More specifically illustrate, then inert gas is supplied to basic gas supply line L1 from basic supplies for gas.After inert gas reduces pressure into authorized pressure by pressure regulator 5 in basic gas supply line L1, import in mass flow controller 6.In mass flow controller 6, preset the flow setting value V of inert gas
1[L/min].That is, the flow of inert gas is controlled at V by mass flow controller 6
1[L/min].And, when automatic valve 8 is open mode, via mass flow controller 6, the flow (V of regulation
1) inert gas supply to blender 2.
In addition, hydrogen selenide gas is supplied to unstrpped gas supply line L2 from unstrpped gas supply source.After hydrogen selenide gas reduces pressure into authorized pressure by pressure regulator 10 in unstrpped gas supply line L2, import in mass flow controller 11.In mass flow controller 11, preset the flow setting value V of hydrogen selenide gas
2[L/min].That is, the flow of hydrogen selenide gas is controlled at V by mass flow controller 11
2[L/min].And, when automatic valve 13 is open mode, via mass flow controller 11, the flow (V of regulation
2) hydrogen selenide gas supply to blender 2.
Secondly, utilize blender 2 to mix with the inert gas of regulation flow supply and hydrogen selenide gas, thus manufacture normal concentration C=V
2/ (V
1+ V
2) × 100) the hydrogen selenide mist of [%].
At this, the concentration of hydrogen selenide mist is not particularly limited, and suitably can select according to the requirement of solar cell manufacturing installation.Specifically, such as, the concentration of the hydrogen selenide in hydrogen selenide mist can be set to 5 ~ 20vol%.
Then, via stream L5, the hydrogen selenide mist being mixed into regulation hydrogen selenide concentration is stored in surge tank 3.The pressure of the hydrogen selenide mist stored can be measured with Pressure gauge 22.Manufacture hydrogen selenide mist, and be supplied to surge tank 3 by stream L5, until the pressure of the hydrogen selenide mist stored arrives the pressure upper limit preset.When the pressure measured by Pressure gauge 22 arrives pressure upper limit, all automatic valves 8,9 and 13 are set to closed condition, stop the supply to surge tank 3, thus stop the manufacture of hydrogen selenide mist.In addition, automatic valve 9 is also closed, and this is to implement makeover process described later.
Afterwards, when utilizing Pressure gauge 22 to detect that the pressure of the hydrogen selenide mist in surge tank 3 arrives below the threshold pression that presets, the automatic valve 8,9,13 be closed is set to open mode, starts mist to the supply of surge tank 3, namely start the manufacture of hydrogen selenide mist.Afterwards, when utilizing Pressure gauge 22 to detect that the pressure of surge tank 3 arrives more than pressure upper limit, all automatic valves 8,9,13 being set to closed condition, stopping mist to the supply of surge tank 3, namely stopping the manufacture of hydrogen selenide mist.Afterwards, according to the pressure of surge tank 3, repeat the manufacture of hydrogen selenide mist successively and manufacture stopping.
(the supply process (III) of hydrogen selenide mist)
The hydrogen selenide mist be stored in surge tank 3 is supplied to solar cell manufacturing installation according to the condition of consumption of the hydrogen selenide mist in solar cell manufacturing installation.
In addition, in the supply method of present embodiment not adopting surge tank 3, not carry out the manufacture of hydrogen selenide mist according to the force value in the surge tank 3 measured by Pressure gauge 22 or manufacture the switching stopped, but can the manufacture of hydrogen selenide mist be carried out according to the condition of consumption of the hydrogen selenide mist in solar cell manufacturing installation or manufacture the switching stopped.Such as, the manufacture of mist can be stopped when not consuming, and/or, can manufacture when consuming.
So, the hydrogen selenide mist of hydrogen selenide concentration stabilize is supplied in solar cell manufacturing installation continuously.
(makeover process (II) of the flow setting value of unstrpped gas)
After stopping the manufacture to the hydrogen selenide mist of surge tank 3, carry out the makeover process of the flow setting value of following illustrated unstrpped gas.By this makeover process, flow setting value that the primary side (downstream) revised to mass flow controller 11 flows, hydrogen selenide gas.
Specifically, the calibration gas of same flow is flow through and be arranged at unstrpped gas supply line L2 and the mass flow controller 11 controlling the flow of hydrogen selenide and the mass flowmenter 16 corrected.In the flowing of the calibration gas of respective position measurement continuous flow.And, according to the difference of the flow value of the calibration gas measured respectively by mass flow controller 11 and mass flowmenter 16, revise the flow setting value flowing through the hydrogen selenide gas of mass flow controller 11.
Further makeover process is described.
First, automatic valve 9 is set to closed condition, stops the supply of hydrogen selenide gas.Also automatic valve 8 and 13 is closed.
Then, automatic valve 14,15 is set to open mode.Its result, the inert gas as basic gas can be made to continue to flow through by bypass flow path L3, the stream (after, be called " calibration gas stream " by this continuous print stream) that forms to the unstrpped gas supply line L2 between branch flow passage L4 and the link position of unstrpped gas supply line L2 and branch flow passage L4 from the link position of bypass flow path L3 and unstrpped gas supply line L2 from basic supplies for gas.This inert gas can use the gas identical with basic gas.The inert gas used plays the function of calibration gas.According to this process, the mass flow controller 11 that the calibration gas of same flow can be made to continuously flow through calibration gas stream is arranged and mass flowmenter 16.
Then, the flow value of calibration gas is measured respectively by mass flow controller 11 that calibration gas stream is arranged and mass flowmenter 16.Use these measured values to carry out calculation process by control unit 19, and based on its result, revise the flow value of hydrogen selenide gas when recovering the manufacture of hydrogen selenide mist, mass flow controller 11 outflow.
In addition, in the diverse situation of the gas when timing and mist manufacture, or mass flow controller and mass flowmenter timing separately ought be carried out as required separately, in the diverse situation of gas when timing and flow measurement, preferably before calculating flow error, use the flow modificatory coefficient reduced discharge being referred to as conversion factor.
In more detail, calculating of the flow error in the present invention is described.
When calculating flow error, first, mass flow controller 11 is utilized to carry out the control of the flow of calibration gas, and, measure the flow V of calibration gas simultaneously
3[L/min].Further, utilize the mass flowmenter 16 being positioned at downstream to measure the flow V of calibration gas simultaneously
4[L/min].
When manufacturing hydrogen selenide mist, comprise in the unstrpped gas supply line L2 of mass flow controller 11 if selenium crystallization more precipitate into, then the flow control accuracy of mass flow controller 11 reduces.Now, due to the existence of selenium crystallization, therefore there is the flow V when stopping the calibration gas being measured by mass flow controller 11 when manufacturing hydrogen selenide mist
3[L/min] is less than the tendency of the flow of the calibration gas originally should measured.
In contrast, mass flowmenter 16 is configured in the position that hydrogen selenide gas does not flow through when manufacturing hydrogen selenide mist.Therefore, the flow V of the calibration gas measured by mass flowmenter 16
4[L/min] is equal with the flow of the calibration gas originally should measured.
So, when stopping manufacturing hydrogen selenide mist, the flow value V of the calibration gas measured respectively by mass flow controller 11 and mass flowmenter 16
3, V
4the difference of [L/min] indicates the reduction situation of the flow control accuracy of mass flow controller 11 exactly, indicates the degree of the amount of precipitation of the selenium crystallization of the unstrpped gas supply line L2 comprising mass flow controller 11 further exactly.
In addition, the flow V of the calibration gas measured by mass flow controller 11 is described at this
3[L/min] is less than the situation of the flow of the calibration gas originally should measured.But, even if when being greater than the flow of the calibration gas originally should measured, also can processing equally, namely revising.
Afterwards, the flow measurement value V of calibration gas will obtained by mass flow controller 11 and mass flowmenter 16
3, V
4[L/min] passes to control unit 19 via distribution E1, E2 respectively.
Then, according to the flow measurements V of the calibration gas obtained by mass flow controller 11
3the flow measurements V of [L/min] and the calibration gas to be obtained by mass flowmenter 16
4the difference of [L/min], calculates the correction of the flow setting value of the hydrogen selenide gas in mass flow controller 11.
Specifically, according to following formula, by flow measurements V
3, V
4[L/min] calculates flow error A and correction factor B.
Flow error A=(∣ V
3-V
4∣/V
4) × 100 [%]
Correction factor B=V
4/ V
3
But, concerning mass flow controller, in the diverse situation of timing with gas during manufacture mist, or the timing of mass flow controller ought be carried out as required separately, when the kind of the gas used when timing and flow measurement is inconsistent, need to utilize the flow modificatory coefficient being referred to as conversion factor to revise.At use traffic correction factor by V
3and V
4after being modified to the flow value based on the kind of calibration gas, calculate flow error A and correction factor B.
After calculating flow error A and correction factor B, according to following formula, calculate flow setting value V that send to mass flow controller 11, revised hydrogen selenide gas
5[L/min].
Flow setting value V
5[L/min]=B × V
2[L/min]
Then, the flow setting value V of hydrogen selenide gas will calculated
5[L/min] is sent to mass flow controller 11 via distribution E1.Flow setting value V
5use in the manufacture process of the hydrogen selenide mist after this carried out.So, after the makeover process of the flow setting value of unstrpped gas, the correction value used during the manufacture of the hydrogen selenide mist that is restored.That is, the flow setting value of the hydrogen selenide gas flowed to the primary side (downstream) of mass flow controller 11 is corrected for the correction calculated by control unit 19.
According to above process, complete the flow setting value V used according to the revised hydrogen selenide of amount of precipitation of the selenium crystallization in mass flow controller 11
5[L/min], be applicable to be supplied to solar cell manufacturing installation, for the manufacture of the preparation of the hydrogen selenide mist of regulation hydrogen selenide concentration.Afterwards, automatic valve 14,15 can be closed and open automatic valve 9.Namely, by so opening, the calibration gas existed in from the link position of bypass flow path L3 and unstrpped gas supply line L2 to the unstrpped gas supply line L2 between branch flow passage L4 and the link position of unstrpped gas supply line L2 can be replaced into hydrogen selenide gas.Now, automatic valve 15 can be opened, or also can open on the opportunity of regulation.
In addition, only correction factor B is used when the flow control of hydrogen selenide gas.That is, when the flow measurement of calibration gas, the correction using correction factor B is not carried out to mass flow controller 11.
Afterwards, automatic valve 14,15 is set to closed condition, and all open and close valves except automatic valve 14,15 and automatic valve are set to open mode, carry out the hydrogen selenide mist manufacture process of above-mentioned explanation.In hydrogen selenide mist manufacture process after second time, flow setting value V that accurately revised by the raw material gas flow set point correct process before it, hydrogen selenide gas
5[L/min] is set in mass flow controller 11.Therefore, it is possible to flow out the flow V that originally should flow to the primary side (downstream) of mass flow controller 11
2the hydrogen selenide gas of [L/min].And, can by flow value V
2the hydrogen selenide gas of [L/min] is supplied to blender 2.
Afterwards, the makeover process (II) implementing the manufacture process (I) of hydrogen selenide mist and the flow setting value of unstrpped gas is alternately repeated.So, chronically and stably supply be suitable for from feedway 101 be supplied to solar cell manufacturing installation, the hydrogen selenide mist of regulation hydrogen selenide concentration.
As makeover process (II) of the flow setting value of the manufacture process (I) and unstrpped gas that alternately repeat enforcement more than twice hydrogen selenide mist, the flow setting value that also can change the calibration gas in the makeover process (II) of the flow setting value of unstrpped gas as required carrys out implementation process.When repeatedly, obtain the difference of the flow value of multiple calibration gas.Therefore, when changing the flow setting value of calibration gas, that obtain in the makeover process of the flow setting value of each unstrpped gas, so far obtained multiple correction factor B equalization can be made and use, or also can determine to be applicable to the correction factor B of range of flow to be set and use.
Such as, when makeover process (II) of the flow setting value of the manufacture process (I) and unstrpped gas that alternately repeat enforcement more than twice hydrogen selenide mist, the flow measurements for the first time in manufacture process is V
3a[L/min], is using the correction factor obtained in the makeover process of this value to be B
a, the flow measurements in second time manufacture process is V
3b[L/min], is using the correction factor obtained in the makeover process of this value to be B
b, and establish V
3a< V
3b.Now, in manufacture afterwards and makeover process, the flow measurements of hydrogen selenide gas is applicable to 0 ~ V
3athe correction factor of the situation of [L/min] is set to B
a, and the flow measurements of hydrogen selenide gas is applicable to V
3a~ V
3bthe correction factor of the situation of [L/min] is set to B
b.
In addition, as makeover process (II) of the flow setting value of the manufacture process (I) and unstrpped gas that alternately repeat enforcement more than twice hydrogen selenide mist, also can before the Pressure gauge 22 being connected to surge tank be lower than authorized pressure, and automatic valve 14,15 is set to closed condition after implementing by the makeover process of the flow setting value in unstrpped gas (II).In addition, the value of preferred flow error A in 5 ~ 30% scopes, but is not particularly limited to this scope, if practical no problem, can suitably select.
The supply method of present embodiment according to the above description, can utilize calibration gas to remove the hydrogen selenide gas of being detained in unstrpped gas supply line.Therefore, it is possible to significantly reduce the precipitation of selenium crystallization in unstrpped gas supply line L2 caused by the selfdecomposition of hydrogen selenide.In addition, flow V is made
2when the hydrogen selenide gas of [L/min] flows through mass flow controller 11, even if such as there is the precipitation of selenium crystallization, also the correction flow value can measured based on the mass flowmenter 16 of the correction that the stream do not flow through by hydrogen selenide gas is arranged, sends revised flow setting value V to mass flow controller 11
5[L/min].Therefore, it is possible to greatly reduce the flow control error of unstrpped gas supply line L2.
Therefore, the supply method of hydrogen selenide mist according to the present embodiment, do not carry out the volume expansion of the careful instrumentations such as the switching of the open and close valve of short cycle and surge tank, shift phenomenon is reduced for a long time compared with existing, thus can by the hydrogen selenide mist of stable hydrogen selenide concentration to supplies such as solar cell manufacturing installations.
In addition, in the feedway 101 of present embodiment, when stopping the manufacture of hydrogen selenide mist, the calibration gas of same flow flows through and is arranged at unstrpped gas supply line L2 and the mass flow controller 11 controlling the flow of hydrogen selenide gas and the mass flowmenter 16 corrected.According to this structure, remove the hydrogen selenide gas of being detained in unstrpped gas supply line with calibration gas, therefore, it is possible to reduce the precipitation of the selenium crystallization caused by the selfdecomposition of hydrogen selenide.
In addition, when manufacturing hydrogen selenide mist, the difference of the flow measurements of calibration gas that measure respectively according to the mass flowmenter 16 that the stream that the mass flow controller 11 that the unstrpped gas supply line L2 flow through by hydrogen selenide gas is arranged and hydrogen selenide gas do not flow through is arranged, that measure same flow, revises the flow setting value of the hydrogen selenide gas that mass flow controller 11 flows out.Thus, greatly reduce the flow control error of unstrpped gas supply line L2, thus suppress shift phenomenon.Its result, does not need careful instrumentation and the jumbo surge tanks such as the valve opening and closing of short cycle, to the hydrogen selenide mist of the stable hydrogen selenide concentration of the supply of long durations such as solar cell manufacturing installation.
In addition, technical scope of the present invention is not limited to above-mentioned execution mode, not departing from main scope of the present invention, can apply various change.
Such as, the feedway 101 of above-mentioned execution mode is the structure be arranged on by mass flowmenter 16 on branch flow passage L4.But the feedway 102 described in Fig. 6, also can be arranged on mass flowmenter 16 on the bypass flow path L3 of the primary side (upstream side) of automatic valve 14.As aforementioned, hydrogen selenide gas can not flow through the bypass flow path L3 of the primary side of automatic valve 14.Therefore, identical with above-mentioned feedway 101, the stream that can not flow through in hydrogen selenide gas arranges mass flowmenter 16.Therefore, also branch flow passage L4 can not be set, on the effect basis of above-mentioned execution mode, feedway can be made miniaturized.Its result, does not need careful instrumentation and the jumbo surge tanks such as the valve opening and closing of short cycle, to the hydrogen selenide mist of the stable hydrogen selenide concentration of the supply of long durations such as solar cell manufacturing installation.
In addition, as other embodiments, such as, when flow error A exceedes setting, to the exception of the operator notification mass flow controller 11 of feedway 101, the replacing of mass flow controller 11 can be carried out by operator.
Embodiment
Below, preferred object lesson of the present invention is shown.
(embodiment)
Use the feedway 101 shown in Fig. 1 to manufacture hydrogen selenide mist, and supply hydrogen selenide mist for a long time continuously to solar cell manufacturing installation.When carrying out the manufacture process of hydrogen selenide mist of feedway 101, use the condition of table 1.In addition, when carrying out the makeover process of flow setting value of unstrpped gas of feedway 101, the condition of table 2 is used.
[table 1]
[table 2]
Table 2 shows the flow measurements V when mass flow controller 11
3when the flow indication of makeover process middle controller is 10.0L/min, the actual nitrogen flow through is 13.0L/min.
" once " described in table 2 is correction in order to carry out a flow setting value and the combination number of times of the manufacture process of carrying out and makeover process, in the present embodiment the combination of repeatedly this manufacture process and makeover process.
While repeat manufacture and makeover process under the implementation condition shown in table 1,2, when supplying hydrogen selenide mist continuously to solar cell manufacturing installation, use the hydrogen selenide concentration analysis meter (not shown) that stream L6 is arranged, measure the rheological parameters' change with time of the hydrogen selenide concentration in hydrogen selenide mist.Time (number of days) interdependence being measured that measure, in hydrogen selenide mist hydrogen selenide concentration by hydrogen selenide concentration analysis has been shown in Fig. 2.In addition, time (number of days) interdependence of the flow error A when repeating manufacture and makeover process has been shown in Fig. 3.
(comparative example)
When the makeover process of the flow setting value of the unstrpped gas of enforcement feedway 101, except the flow setting value V of the hydrogen selenide to mass flow controller 11
2the correction of [L/min] does not use outside correction factor B, with embodiment at identical conditions, produce hydrogen selenide mist, and supply hydrogen selenide mist continuously to solar cell manufacturing installation.That is, although implement makeover process, in mass flow controller 11, do not use revised flow, and carry out manufacturing and supplying.Identical with embodiment, use the hydrogen selenide concentration analysis meter that stream L6 is arranged to measure the rheological parameters' change with time of the hydrogen selenide concentration in hydrogen selenide mist.Time (number of days) interdependence of the hydrogen selenide concentration in hydrogen selenide mist has now been shown in Fig. 2.
(comparison of the measurement result of embodiment and comparative example)
As shown in Figure 2, in a comparative example, until through about 40 days from measurement starts, the hydrogen selenide concentration in hydrogen selenide mist remains near normal concentration 10.0%.But, number of days further across, then hydrogen selenide concentration sharply increases.
In addition, concerning time (number of days) interdependence of the hydrogen selenide concentration of the flow error A shown in Fig. 3, the number of days from measuring and starting after about 40 days, flow error A sharply increases.Its result, in a comparative example, from measurement starts the 100th day, the hydrogen selenide concentration in hydrogen selenide mist reached 13.8%.
So, as the main cause that hydrogen selenide concentration rises, the reason that can be listed below: owing to not carrying out the flow setting value V of the hydrogen selenide of the mass flow controller 11 using correction factor B
2the correction of [L/min], therefore the flow control accuracy of mass flow controller 11 reduces.
Relative to comparative example, though in an embodiment from measurement starts through about 100 days, the hydrogen selenide concentration in hydrogen selenide mist is also stabilized near 10.0%.Therefore, in the present invention, confirming can clock like precision ground and reduce the flow control error of unstrpped gas supply line L2 long-time period of about at least 100 days.This is because, supply method and the feedway 101 of above-mentioned execution mode of the present invention can be utilized, the flow error A calculated according to the flow value based on the calibration gas measured by the mass flowmenter 16 corrected and correction factor B, will flow through the flow setting value V of the hydrogen selenide gas of mass flow controller 11
2[L/min] is modified to flow setting value V
5[L/min].
Utilizability in industry
In the supply method that the present invention is applicable to hydrogen selenide mist and feedway.Can provide a kind of supply method and feedway of hydrogen selenide mist, it does not need careful instrumentation and jumbo surge tank, while can shift phenomenon being suppressed, and the hydrogen selenide mist of supply of long duration hydrogen selenide concentration stabilize.
Description of reference numerals
2,117 ... blender
3,118 ... surge tank
4,21,23,104,114,115 ... open and close valve
5,10,105,110 ... pressure adjusting meter
6,11,106,111 ... mass flow controller (flow controlling unit)
7,12,107,112 ... check-valves
8,9,13,108,109,113 ... automatic valve
14,15 ... automatic valve (open and close valve)
16 ... mass flowmenter (airflow measurement unit)
19 ... control unit
22,116 ... Pressure gauge
L1, L101 ... basic gas supply line
L2, L102 ... unstrpped gas supply line
L3, L105 ... bypass flow path
L4 ... branch flow passage
L5, L6, L7, L103, L104 ... stream
E1, E2 ... distribution
101,102,103,201,202 ... feedway
Claims (11)
1. a supply method for hydrogen selenide mist, has: mixed with the hydrogen selenide gas supplied from unstrpped gas supply line by the inert gas from basic gas supply line supply, manufacture the operation of the hydrogen selenide mist being mixed with normal concentration; With the operation of the described mist of supply,
The feature of the supply method of described hydrogen selenide mist is,
During being included in the operation stopping manufacturing hydrogen selenide mist further, revise the operation of the flow setting value of unstrpped gas,
Described correction operation comprises:
The calibration gas of same flow is flow through and is arranged at described unstrpped gas supply line with the operation of the airflow measurement unit of the flow controlling unit and correction that control the flow of described hydrogen selenide gas;
Obtain the operation of the difference of the flow value of the described calibration gas measured respectively by described flow controlling unit and described airflow measurement unit; With
According to described difference, revise the operation of the flow value of the described hydrogen selenide gas that described flow controlling unit flows out.
2. the supply method of hydrogen selenide mist according to claim 1, is characterized in that, makes described calibration gas continue to flow through described flow controlling unit and described airflow measurement unit by different order.
3. the supply method of hydrogen selenide mist according to claim 1 and 2, is characterized in that, described flow controlling unit and described airflow measurement unit is used to the flow-measuring method of same specification.
4. the supply method of the hydrogen selenide mist according to any one in claims 1 to 3, is characterized in that, uses described inert gas as described calibration gas.
5. the supply method of the hydrogen selenide mist according to any one in Claims 1-4, is characterized in that, when manufacturing described hydrogen selenide mist, does not make described hydrogen selenide gas flow through described airflow measurement unit.
6. the feedway of a hydrogen selenide mist, inert gas from basic gas supply line supply is mixed with the hydrogen selenide gas supplied from unstrpped gas supply line, manufacture the hydrogen selenide mist being mixed with normal concentration, supply this hydrogen selenide mist afterwards
The feature of the feedway of described hydrogen selenide mist is to possess:
Flow controlling unit, is arranged at described unstrpped gas supply line to control the flow of described hydrogen selenide gas;
Calibration gas supply line, when stopping manufacturing described hydrogen selenide mist, supplies the primary side of calibration gas to the described flow controlling unit of described unstrpped gas supply line;
The airflow measurement unit corrected, is arranged at the described calibration gas when stopping manufacturing described hydrogen selenide mist and flows through and when the described hydrogen selenide mist of manufacture on the stream that do not flow through of described hydrogen selenide gas; With
Control unit, when making the described calibration gas of same flow flow through described flow controlling unit and described airflow measurement unit, according to the difference of the flow value of the calibration gas measured respectively, revise the flow value of the described hydrogen selenide gas that described flow controlling unit flows out.
7. the feedway of hydrogen selenide mist according to claim 6, is characterized in that,
Described calibration gas supply line is provided with the first open and close valve, described first open and close valve is closed condition when manufacturing described hydrogen selenide mist, be open mode when described calibration gas is supplied from described calibration gas supply line to described unstrpped gas supply line
The primary side of described first open and close valve of described calibration gas supply line is provided with described airflow measurement unit.
8. the feedway of hydrogen selenide mist according to claim 6, it is characterized in that, described calibration gas supply line is the bypass flow path described basic gas supply line be connected with the primary side of the described flow controlling unit of described unstrpped gas supply line.
9. the feedway of hydrogen selenide mist according to claim 8, is characterized in that,
Described bypass flow path is provided with the first open and close valve, described first open and close valve is closed condition when manufacturing described hydrogen selenide mist, be open mode when described inert gas is supplied as calibration gas from described basic gas supply line to described unstrpped gas supply line
The primary side of described first open and close valve of described bypass flow path is provided with described airflow measurement unit.
10. the feedway of the hydrogen selenide mist according to claim 6 or 8, is characterized in that,
The primary side of the described flow controlling unit of described unstrpped gas supply line is provided with branch flow passage,
Described branch flow passage is provided with the second open and close valve, described second open and close valve is closed condition when manufacturing described hydrogen selenide mist, be open mode when described inert gas is supplied as calibration gas from described basic gas supply line to described unstrpped gas supply line
The primary side of described second open and close valve of described branch flow passage is provided with described airflow measurement unit.
The feedway of 11. hydrogen selenide mists according to any one in claim 6 to 10, it is characterized in that, described flow controlling unit and described airflow measurement unit are the flow-measuring method of same specification.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2012-232832 | 2012-10-22 | ||
| JP2012232832 | 2012-10-22 | ||
| PCT/JP2013/078444 WO2014065233A1 (en) | 2012-10-22 | 2013-10-21 | Method and device for supplying hydrogen-selenide mixed gas |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104769727A true CN104769727A (en) | 2015-07-08 |
| CN104769727B CN104769727B (en) | 2016-12-07 |
Family
ID=50544613
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201380052051.2A Expired - Fee Related CN104769727B (en) | 2012-10-22 | 2013-10-21 | The supply method of Selenium hydride. mixed gas and feedway |
Country Status (5)
| Country | Link |
|---|---|
| JP (1) | JP6065329B2 (en) |
| KR (1) | KR101661483B1 (en) |
| CN (1) | CN104769727B (en) |
| TW (1) | TWI618672B (en) |
| WO (1) | WO2014065233A1 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109196442A (en) * | 2016-03-31 | 2019-01-11 | 林德股份公司 | For manufacturing the volume and weight occupied state of admixture of gas |
| CN109913853A (en) * | 2017-12-13 | 2019-06-21 | 东京毅力科创株式会社 | Substrate processing method using same, storage medium and material gas supply device |
| CN112097114A (en) * | 2020-08-07 | 2020-12-18 | 安徽亚格盛电子新材料有限公司 | Device for accurately preparing liquid MO source and hydrogen mixed gas |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20200050607A (en) | 2018-11-02 | 2020-05-12 | 알엠아이텍(주) | Method for producing hydrogen selenide based on zinc selenide |
| JP2020105577A (en) * | 2018-12-27 | 2020-07-09 | 株式会社フジキン | Fluid supply device |
| CN109865440B (en) * | 2019-03-29 | 2021-08-31 | 国网山东省电力公司电力科学研究院 | Standard gas preparation device |
| JPWO2021095608A1 (en) * | 2019-11-12 | 2021-05-20 | ||
| KR102431346B1 (en) * | 2022-02-11 | 2022-08-09 | 박재기 | Gas supply system that can replace the flow controller without interruption of the process |
| JP2024027372A (en) * | 2022-08-17 | 2024-03-01 | 大陽日酸株式会社 | Mixed gas supply device |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11265218A (en) * | 1998-03-18 | 1999-09-28 | Kokusai Electric Co Ltd | Automatic flow/flow ratio conversion data calibrating device and gas supplying device |
| JP2011057455A (en) * | 2009-09-04 | 2011-03-24 | Taiyo Nippon Sanso Corp | Method and apparatus for supplying hydrogen selenide-mixed gas for solar cell |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011027663A1 (en) * | 2009-09-04 | 2011-03-10 | 大陽日酸株式会社 | Method and apparatus for supplying hydrogen selenide mixed gas for solar cell |
| JP5663488B2 (en) | 2009-10-14 | 2015-02-04 | 大陽日酸株式会社 | Method and apparatus for supplying hydrogen selenide mixed gas for solar cell |
-
2013
- 2013-10-21 WO PCT/JP2013/078444 patent/WO2014065233A1/en active Application Filing
- 2013-10-21 JP JP2014543279A patent/JP6065329B2/en not_active Expired - Fee Related
- 2013-10-21 CN CN201380052051.2A patent/CN104769727B/en not_active Expired - Fee Related
- 2013-10-21 KR KR1020157006775A patent/KR101661483B1/en active IP Right Grant
- 2013-10-22 TW TW102138027A patent/TWI618672B/en not_active IP Right Cessation
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11265218A (en) * | 1998-03-18 | 1999-09-28 | Kokusai Electric Co Ltd | Automatic flow/flow ratio conversion data calibrating device and gas supplying device |
| JP2011057455A (en) * | 2009-09-04 | 2011-03-24 | Taiyo Nippon Sanso Corp | Method and apparatus for supplying hydrogen selenide-mixed gas for solar cell |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109196442A (en) * | 2016-03-31 | 2019-01-11 | 林德股份公司 | For manufacturing the volume and weight occupied state of admixture of gas |
| CN109913853A (en) * | 2017-12-13 | 2019-06-21 | 东京毅力科创株式会社 | Substrate processing method using same, storage medium and material gas supply device |
| CN112097114A (en) * | 2020-08-07 | 2020-12-18 | 安徽亚格盛电子新材料有限公司 | Device for accurately preparing liquid MO source and hydrogen mixed gas |
Also Published As
| Publication number | Publication date |
|---|---|
| KR101661483B1 (en) | 2016-09-30 |
| TWI618672B (en) | 2018-03-21 |
| JPWO2014065233A1 (en) | 2016-09-08 |
| WO2014065233A1 (en) | 2014-05-01 |
| KR20150044437A (en) | 2015-04-24 |
| JP6065329B2 (en) | 2017-01-25 |
| CN104769727B (en) | 2016-12-07 |
| TW201427896A (en) | 2014-07-16 |
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