CN104769727B - The supply method of Selenium hydride. mixed gas and feedway - Google Patents
The supply method of Selenium hydride. mixed gas and feedway Download PDFInfo
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- CN104769727B CN104769727B CN201380052051.2A CN201380052051A CN104769727B CN 104769727 B CN104769727 B CN 104769727B CN 201380052051 A CN201380052051 A CN 201380052051A CN 104769727 B CN104769727 B CN 104769727B
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- gas
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- selenium hydride
- supply line
- mixed gas
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- 229910000058 selane Inorganic materials 0.000 title claims abstract description 315
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 244
- 238000000034 method Methods 0.000 title claims abstract description 86
- 239000007789 gas Substances 0.000 claims abstract description 603
- SPVXKVOXSXTJOY-UHFFFAOYSA-N selane Chemical compound [SeH2] SPVXKVOXSXTJOY-UHFFFAOYSA-N 0.000 claims abstract description 87
- 238000005259 measurement Methods 0.000 claims abstract description 57
- 238000012937 correction Methods 0.000 claims abstract description 55
- 238000004519 manufacturing process Methods 0.000 claims description 116
- 229910052756 noble gas Inorganic materials 0.000 claims description 42
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 239000008246 gaseous mixture Substances 0.000 claims description 4
- 230000008569 process Effects 0.000 description 49
- 239000011669 selenium Substances 0.000 description 17
- 229910052711 selenium Inorganic materials 0.000 description 16
- 238000011144 upstream manufacturing Methods 0.000 description 13
- 239000002994 raw material Substances 0.000 description 11
- 102000003712 Complement factor B Human genes 0.000 description 10
- 108090000056 Complement factor B Proteins 0.000 description 10
- 238000002425 crystallisation Methods 0.000 description 10
- 230000008025 crystallization Effects 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- 238000009826 distribution Methods 0.000 description 8
- 230000033228 biological regulation Effects 0.000 description 7
- 230000008859 change Effects 0.000 description 7
- 238000001556 precipitation Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 238000010926 purge Methods 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 230000003139 buffering effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 230000002571 modificatory effect Effects 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 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
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000001629 suppression 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
- 239000000470 constituent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 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
- 239000011261 inert gas Substances 0.000 description 1
- 230000007774 longterm Effects 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
- 239000002244 precipitate Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
Abstract
The supply method of a kind of Selenium hydride. mixed gas and feedway, the calibration gas making same flow flows through flow controlling unit and the flow controlling unit of correction of the flow being arranged at unstrpped gas supply line to control the hydrogen selenide gas as unstrpped gas, and the difference of the flow value according to the calibration gas measured respectively by flow controlling unit and airflow measurement unit, the setting value of the flow of the hydrogen selenide gas that modified flow rate control unit flows out.
Description
Technical field
The present invention relates to supply method and the feedway of Selenium hydride. mixed gas.
The application claimed priority in the Patent 2012-232832 of Japanese publication based on October 22nd, 2012, and
And here cite its content.
Background technology
In recent years, due to environmental pollution, global warming, Fossil fuel these problems exhausted, solaode is as stone
Oil alternative energy source and receive publicity.The main flow of current solaode is following compound solar cell: it comprises
Copper, indium, gallium and selenium, and use by using Selenium hydride. (H2Se) the chalcopyrite light absorbing zone formed.Need
The Selenium hydride. mixed gas of normal concentration has been adjusted to the unit feeding that manufactures of this compound solar cell.
But, in order to realize a large amount of productions of compound solar cell, need to supply substantial amounts of Selenium hydride. mixed gas
It is given to solaode and manufactures device.Therefore, when using the gas storage being filled with the mixed gas being adjusted to normal concentration
During bottle, there is the problem that cannot guarantee enough gas delivery volumes because the replacement frequency of gas bomb is many.
In order to solve the problems referred to above, the feedway of use Selenium hydride. mixed gas as shown in Figure 4 was (below, in the past
It is only called " feedway ") 201.Basic gas supplying path L101 and raw material it is provided with in feedway 201
Gas supplying path L102.The hydrogen selenide gas of noble gas and concentration 100% (after, it is only called " selenizing hydrogen
Body ") can circulate in each path respectively.It addition, supply at basic gas supplying path L101 and unstrpped gas
On the L102 of path, it is respectively arranged with basic gas flow rate control unit 106 and raw material gas flow control unit 111.
And, in basic gas supplying path L101 and the downstream of unstrpped gas feed path L102, it is provided with for storing up
Deposit the surge tank 118 of noble gas Yu hydrogen selenide gas mixed Selenium hydride. mixed gas.
Supply method (hereinafter simply referred to as " supply method ") in the Selenium hydride. mixed gas using feedway 201
In, utilize basic gas flow rate control unit 106 and raw material gas flow control unit 111 to control noble gas respectively
Flow with hydrogen selenide gas so that the Selenium hydride. concentration of Selenium hydride. mixed gas is setting.Afterwards, blender is used
Noble gas after 117 mixed traffics controls and hydrogen selenide gas, thereafter, the Selenium hydride. mixed gas that will obtain stores
In surge tank 118.The Selenium hydride. mixed gas of the regulation Selenium hydride. concentration being stored in surge tank 118 by continuously to
The manufacture unit feeding of solaode.
But, in feedway 201, there is following problem.That is, have because the selfdecomposition of Selenium hydride. causes
Selenium (Se) crystallization to hydrogen selenide gas flow pass through unstrpped gas supply line L102, open and close valve 109,113
With the problem in raw material gas flow control unit 111 grade.Especially, there is following problem: due to selenium crystallization
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 reduces, its result, and the concentration set point of Selenium hydride. mixed gas set in advance and reality are by supplying
The difference of the concentration measured value of the Selenium hydride. mixed gas that device 201 adjusts is relatively big (being referred to as shift phenomenon).
As the technology of this shift phenomenon of suppression, such as, Patent Document 1 discloses and concentration can be stably supplied
The supply method of the Selenium hydride. mixed gas of setting value and feedway.As it is shown in figure 5, the supply dress of patent documentation 1
Put 202 on the architecture basics of the feedway 201 shown in Fig. 4, possess by basic gas supply line L101 with
Bypass flow path L105 of unstrpped gas supply line L102 connection.And, Patent Document 1 discloses following confession
To method: after manufacturing mixed gas when not using bypass flow path L105 and 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 after, warp
By bypass flow path L105, the noble gas of ormal weight is derived from unstrpped gas supply line L102, thus make rule
Determine the Selenium hydride. mixed gas of Selenium hydride. concentration, and make the Selenium hydride. of residual in unstrpped gas supply line L102
Volumetric concentration is less than 10%.
Patent documentation 1: International Publication the 2011/045983A1st
But, have a problem in that in the supply method that patent documentation 1 is recorded when via bypass flow path L105, using
When noble gas derives the hydrogen selenide gas in unstrpped gas supply line L102, such as, require as real with 0.1 second unit
Execute the careful instrumentation of valve events.The most now, from the selenium of unstrpped gas supply line L102 effluent air
Change hydrogen concentration to vary to significantly close to 0% from 100%.Therefore, have if it is intended to Selenium hydride. in suppressing surge tank
The variation of concentration, then the problem needing jumbo surge tank.
Further, in the method for document 1, only when not to the supply Selenium hydride. mixing of unstrpped gas supply line L102
During gas, can make the volumetric concentration of the Selenium hydride. of residual in unstrpped gas supply line L102 is less than 10%, works as confession
During to Selenium hydride. mixed gas, it is impossible to be entirely prevented from selenium crystallization precipitation in unstrpped gas supply line L102.Cause
This, make feedway 202 long-term work, problem shift phenomenon occur if had.
Summary of the invention
Therefore, it is an object of the invention to provide supply method and the feedway of a kind of Selenium hydride. mixed gas, it is not
Need careful instrumentation and jumbo surge tank, it is possible to suppress shift phenomenon for a long time, to supply stable selenizing
The Selenium hydride. mixed gas of hydrogen concentration.
In order to solve the problems referred to above, as the 1st aspect of the present invention, it is provided that method below.
That is, (1) supply method of a kind of Selenium hydride. mixed gas is provided, have: will supply from basic gas supply line
The noble gas given mixes with the hydrogen selenide gas supplied from unstrpped gas supply line, manufactures and is configured to normal concentration
The operation of Selenium hydride. mixed gas；With the operation of the described mixed gas of supply, the supply of described Selenium hydride. mixed gas
Method is characterised by, during further including at the operation stopping manufacturing Selenium hydride. mixed gas, revises unstrpped gas
The operation of flow setting value, described correction operation includes: make the calibration gas of same flow flow through be arranged at described
Unstrpped gas supply line is to control flow controlling unit and the flow-control of correction of the flow of described hydrogen selenide gas
The operation of unit；Obtain the described correction measured respectively by described flow controlling unit and described airflow measurement unit to use
The operation of the difference of the flow value of gas；With according to described difference, revise the described selenium that described flow controlling unit flows out
Change the operation of the flow value of hydrogen.
The mode of above-mentioned (1) preferably has following feature.
(2) described calibration gas is made to continue to flow through described flow controlling unit and described flow measurement list by different order
Unit.
(3) described flow controlling unit and described airflow measurement unit are used the flow-measuring method of same specification.
(4), in the either type in above-mentioned (1) to (3), use described noble gas as described correction gas
Body.
(5), in the either type in above-mentioned (1) to (4), when manufacturing described Selenium hydride. mixed gas, do not make
Described hydrogen selenide gas flows through the described airflow measurement unit of correction.
(6) as the 2nd aspect of the present invention, it is provided that device below.
That is, the feedway of a kind of Selenium hydride. mixed gas, by the noble gas that supplies from basic gas supply line with
From the hydrogen selenide gas mixing of unstrpped gas supply line supply, manufacture the Selenium hydride. gaseous mixture being configured to normal concentration
Body, supplies this Selenium hydride. mixed gas afterwards,
The feedway of described Selenium hydride. mixed gas is characterised by possessing: flow controlling unit, is arranged at described
Unstrpped gas supply line is to control the flow of described hydrogen selenide gas；Calibration gas supply line, when stopping manufacturing
During described Selenium hydride. mixed gas, by calibration gas to the described flow controlling unit of described unstrpped gas supply line
Primary side supply；The airflow measurement unit of correction, is arranged at when stopping manufacturing described Selenium hydride. mixed gas time institute
State calibration gas flow through and when manufacture described Selenium hydride. mixed gas time described hydrogen selenide gas without flow through stream
On；And control unit, when the described calibration gas making same flow flows through described flow controlling unit and described flow
During measuring unit, according to the difference of the flow value of the calibration gas measured respectively, modified flow rate control unit flows out
The flow value of described hydrogen selenide gas.
(7) in above-mentioned (6), described calibration gas supply line is provided with the first open and close valve, described
One open and close valve when manufacture described Selenium hydride. mixed gas time be closed mode, when by described calibration gas from described correction
It is open mode by gas supply line when described unstrpped gas supply line supplies, supplies at described calibration gas
The primary side of described first open and close valve of stream is provided with described airflow measurement unit.
(8) in above-mentioned (6), described calibration gas supply line is for by described basic gas supply line and institute
The bypass flow path that the primary side of the described flow controlling unit stating unstrpped gas supply line connects.
(9) in above-mentioned (8), being provided with the first open and close valve in described bypass flow path, described first open and close valve is worked as
Be closed mode when manufacturing described Selenium hydride. mixed gas, when using described noble gas as calibration gas from described base
This gas supply line is open mode when described unstrpped gas supply line supplies, described in described bypass flow path
The primary side of the first open and close valve is provided with described airflow measurement unit.
(10) in above-mentioned (6) or (8), at the described flow controlling unit of described unstrpped gas supply line
Primary side is provided with branch flow passage, is provided with the second open and close valve on described branch flow passage, and described second open and close valve is when system
Be closed mode when making described Selenium hydride. mixed gas, when using described noble gas as calibration gas from described substantially
Gas supply line is open mode when described unstrpped gas supply line supplies, at described the of described branch flow passage
The primary side of two open and close valves is provided with described airflow measurement unit.
(11) in the either type in above-mentioned (6) to (10), described flow controlling unit and described flow measurement
Unit is the flow-measuring method of same specification.
The supply method of the Selenium hydride. mixed gas according to the present invention, makes the calibration gas of same flow flow through and is arranged at
As the hydrogen selenide gas supply line of unstrpped gas to control the flow controlling unit of flow and the correction of hydrogen selenide gas
Airflow measurement unit.And, according to the correction measured respectively by flow controlling unit and airflow measurement unit
By the difference of the flow value of gas, the composition of the flow value of the hydrogen selenide gas that modified flow rate control unit flows out.According to
This composition, it is possible to utilize calibration gas, by the hydrogen selenide gas of delay in unstrpped gas supply line from described raw material
Derive in gas supply line.Therefore, it is possible to reduce the precipitation of the selenium crystallization caused by the selfdecomposition of Selenium hydride..It addition,
Can be based on the flow value of the calibration gas measured by the airflow measurement unit of correction, modified flow rate control unit
The flow value of the hydrogen selenide gas flowed out.Therefore, it is possible to the flow measurement greatly reduced in unstrpped gas supply line is by mistake
Difference and flow-control error, thus suppress shift phenomenon.Therefore, there is no need to the slow of careful instrumentation and big volume
Rush tank, it is possible to chronically the Selenium hydride. mixed gas of stable Selenium hydride. concentration is supplied in solaode manufacture
In the consumer device of the primary side of device etc..
It addition, the feedway of the Selenium hydride. mixed gas of the present invention has structures below.That is, possess: flow control
Unit processed, is arranged at unstrpped gas supply line to control the flow of hydrogen selenide gas；Bypass flow path, when stopping manufacturing
During Selenium hydride. mixed gas, noble gas is supplied to unstrpped gas as calibration gas from basic gas supply line
The primary side supply of the flow controlling unit of stream；The airflow measurement unit of correction, is arranged at when stopping manufacture selenizing
During hydrogen mixed gas, calibration gas flows through, when manufacture Selenium hydride. mixed gas time hydrogen selenide gas without flow through stream on；
And control unit, when the calibration gas making same flow flows through flow controlling unit and airflow measurement unit, according to
The difference of the flow value of the calibration gas measured respectively, the stream of the hydrogen selenide gas that modified flow rate control unit flows out
The setting value of amount.Above-mentioned supply method can be implemented by possessing the feedway of described structure.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the feedway 101 of the Selenium hydride. mixed gas being denoted as one embodiment of the present invention.
Fig. 2 is the figure of the service time representing the Selenium hydride. mixed gas in embodiment and the relation of Selenium hydride. concentration.
Fig. 3 is the figure of the service time representing the Selenium hydride. mixed gas in embodiment and the relation of flow error A.
Fig. 4 is the schematic diagram of the feedway 201 representing existing Selenium hydride. mixed gas.
Fig. 5 is the schematic diagram of the feedway 202 representing another Selenium hydride. mixed gas existing.
Fig. 6 is the signal of the feedway 102 of the Selenium hydride. mixed gas being denoted as another embodiment of the present invention
Figure.
Fig. 7 is the signal of the feedway 103 of the Selenium hydride. mixed gas being denoted as another embodiment of the present invention
Figure.
Detailed description of the invention
Below, utilize accompanying drawing to the supply method as the Selenium hydride. mixed gas applying one embodiment of the present invention
And the feedway of Selenium hydride. mixed gas is described in detail.
Additionally, in the accompanying drawing that following explanation is used, for ease of understanding feature, amplify the most for convenience
Representing the part of constitutive characteristic, the dimensional ratios of each structural element etc. may not be identical with reality.It addition, the present invention is not
Only it is defined in the examples below.Can also carry out as required changing within the scope of the invention, omit, convert and/
Or add.The quantity of device and position can also be changed as required.It addition, about being adopted in this manual
Unit, concentration represents volumetric concentration, pressure representative gauge pressure, and flow represents volume flow.And then, in this explanation
Volume shown in book is the volume under standard state (0 DEG C, 1atm (atmospheric pressure)).It addition, in the present invention,
The record of so-called " unit " can represent device, operation, parts, system and part etc..
(feedway of Selenium hydride. mixed gas)
First, as the feedway towards solaode manufacture device, the Selenium hydride. for present embodiment mixes
The structure of the feedway (hereinafter simply referred to as feedway) 101 of gas illustrates while with reference to Fig. 1.
Additionally, describe the feedway manufacturing device towards solaode at this, if but the feedway of the present invention is face
The feedway of device to consumption Selenium hydride. mixed gas is then not particularly limited, such that it is able to be used in any towards
The feedway of the device of consumption Selenium hydride. mixed gas.Such as, list Selenium hydride. mixed gas work as an example
The feedway etc. towards semiconductor-fabricating device consumed for impurity gas.Additionally, about " facing device A's
Device B " etc. statement, the device B prepared separately with device A can be represented, maybe can also be denoted as device A's
A part and the device B that includes.
As it is shown in figure 1, feedway 101 is the condition of production manufacturing device (not shown) according to solaode,
Manufacture and manufacture, to solaode, the device that unit feeding has been formulated as the Selenium hydride. mixed gas of normal concentration.Tool
From the point of view of body, feedway 101 is substantially configured to possess: 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
Bright, then feedway 101 is substantially configured to possess: basic gas supply line L1, is used for supplying basic gas；
Unstrpped gas supply line L2, for base feed gas；Mass flow controller 6, for controlling basic gas
Flow；Mass flow controller 11, for controlling the flow of unstrpped gas；Blender 2, for mixed traffic control
After unstrpped gas and basic gas；With surge tank 3, store the unstrpped gas and basic gas mixed by blender 2
Selenium hydride. mixed gas.
More specifically, feedway 101 is further equipped with bypass flow path L3, mass flowmenter (airflow measurement unit)
16 and control unit 19.Be more particularly described, then feedway 101 is characterised by possessing: bypass flow path L3,
When stop manufacture Selenium hydride. mixed gas time, for using basic gas as calibration gas from basic gas supply line
Primary side (upstream side) supply of L1 mass flow controller 11 in unstrpped gas supply line L2；Quality stream
Gauge 16, when manufacture Selenium hydride. mixed gas time, for measure be supplied to unstrpped gas without flow through stream correction use
The flow of gas；With control unit 19, when the calibration gas making same flow flows through mass flow controller 11 He
During mass flowmenter 16, for the difference of the flow value according to the calibration gas measured respectively, revise and flow through quality
The flow value of the unstrpped gas of flow controller 11.
(basic gas supply line L1)
One end of basic gas supply line L1 is connected with not shown basic gas supply source, the other end and blender 2
Connect.If basic gas is the noble gas for dilution, it is not particularly limited.Lazy as used in the present invention
Property gas, can enumerate such as nitrogen (N2) rare gas etc. such as gas or argon (Ar), helium (He) and neon (Ne).
In basic gas supply line L1, from upstream side towards downstream, it is disposed with open and close valve 4, pressure tune
Whole device 5, mass flow controller 6, check-valves 7 and automatic valve 8.In addition it is also possible to as required, adjust at pressure
Upstream side and the downstream of whole device 5 arrange not shown Pressure gauge.By arranging this Pressure gauge, it is possible to pressure is adjusted
Pressure before and after whole device 5 is visually confirmed to be.
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 noble gas that supplies from basic gas supply source to hope
Pressure.In the feedway 101 of present embodiment, pressure regulator 5 is in basic gas supply line L1
It is provided only with one.But, it being not limited to one, pressure regulator 5 can also be in any selection of stream L1
Position two or more is set.
Additionally, the pressure of the gas that will arrive in the stream L1 before mass flow controller 6 can be according to the sun
The supply pressure of energy battery producing device suitably sets.Such as, as will arrive mass flow controller 6 it
The pressure of front gas, can be set to the scope of 0.3～0.8MPa.
Mass flow controller 6 is to measure the mass flow of basic gas and carry out the flow-control instrument of flow-control,
It is arranged for high-precision flow measurement and control.
It addition, mass flow controller 6 controls the flow of noble gas so that the Selenium hydride. mixed by blender 2 mixes
The Selenium hydride. concentration closed in gas maintains setting.
Exemplified with the feed unit being provided with a mass flow controller 6 in basic gas supply line L1 in Fig. 1
101, but the present invention is not limited to this.For example, it is also possible to be set up in parallel two in basic gas supply line L1
Above mass flow controller 6.
It is mounted with mass flow sensor in mass flow controller 6.It is loaded into the quality of mass flow controller 6
Flow transducer is not particularly limited, such as, thermal type mass flow sensor, differential pressure type mass flow can be used to sense
The common mass flow sensors such as device and Coriolis formula mass flow sensor.
Noble gas after check-valves 7 makes by mass flow controller 6 flow-control only moves from upstream side downstream effluent,
And prevent the adverse current of noble gas lateral upstream side downstream.Thereby, it is possible to alleviate basic gas supply line L1
The variation of interior basic gas flow.
Automatic valve 8 is arranged for controlling whether to be supplied by the noble gas after mass flow controller 6 flow-control
To blender 2.When automatic valve 8 is open mode, the noble gas after flow-control is discharged to automatic valve 8
Downstream, and it is supplied to blender 2.On the other hand, when automatic valve 8 is closed mode, stop noble gas to
The supply in the downstream of automatic valve 8, noble gas will not be supplied to blender 2.The open and-shut mode of automatic valve 8 according to
The pressure of the surge tank 3 measured by Pressure gauge 22 and switch.
(unstrpped gas supply line L2)
One end of unstrpped gas supply line L2 is connected with not shown unstrpped gas supply source, the other end and blender 2
Connect.Unstrpped gas is hydrogen selenide gas.
Unstrpped gas supply line L2 is provided with mass flow controller 11, and is being positioned at mass flow control
In unstrpped gas supply line L2 of the primary side (downstream) of device 11, connection has from unstrpped gas supply line L2
The branch flow passage L4 branched out.
It addition, in 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.With basic gas supply line
L1 is identical, it is also possible to upstream side and downstream at pressure regulator 10 arrange not shown any amount as required
Pressure gauge.By arranging this Pressure gauge, it is possible to the pressure before and after pressure regulator 10 is visually confirmed to be.
About automatic valve 9, pressure regulator 10, check-valves 12 and the explanation of automatic valve 13, supply with by basic gas
To the inert gas replacement in the explanation of the open and close valve 4 of stream L1, pressure regulator 5, check-valves 7 and automatic valve 8
For almost identical after hydrogen selenide gas, therefore omit the description.
Mass flow controller 11 is that metering is flow through the mass flow of the hydrogen selenide gas of stream L2 and carries out flow-control
Flow-control instrument, be arranged for carrying out high-precision flow measurement and control.
It addition, mass flow controller 11 controls the flow of hydrogen selenide gas so that the Selenium hydride. mixed by blender 2
Selenium hydride. concentration in mixed gas is setting.
It addition, utilize mass flow controller 11, when stopping manufacturing Selenium hydride. mixed gas, carry out via bypass stream
The flow-control of the calibration gas that road L3 supplies to the primary side (upstream side) of mass flow controller 11 and quality
Flow measurement.
Further, mass flow controller 11 is connected by distribution E1 described later control unit 19, can correction be used
The measurement result (flow measurements) of the flow of gas sends to control unit 19 from mass flow controller 11.?
In control unit 19 when obtain required for information time perform operation, it is possible to make its result reflect mass flow
In the control of controller 11.
Fig. 1 fills exemplified with the supply being provided with a mass flow controller 11 in unstrpped gas supply line L2
Put 101, but the present invention is not limited to this.For example, it is also possible to be set up in parallel two in unstrpped gas supply line L2
Individual above mass flow controller 11.
It is mounted with mass flow sensor in mass flow controller 11.It is loaded into the matter of mass flow controller 11
Amount flow transducer is not particularly limited, such as, thermal type mass flow sensor, differential pressure type mass flow can be used to pass
The common mass flow sensors such as sensor and Coriolis formula mass flow sensor.Furthermore it is preferred that mass flow control
Device 11 processed utilizes the hydrogen selenide gas as unstrpped gas to carry out flux modification, but is not particularly limited to this, it is also possible to
The gas beyond hydrogen selenide gas is utilized to be corrected.
(blender 2)
Blender 2 is arranged at another of the other end of basic gas supply line L1 and unstrpped gas supply line L2
The position at end interflow.Blender 2 can mix the noble gas by the supply of basic gas supply line L1 and pass through
The hydrogen selenide gas of unstrpped gas supply line L2 supply manufactures the Selenium hydride. mixed gas being adjusted to normal concentration,
And the gas produced is supplied to downstream, it is not particularly limited, it is possible to arbitrarily select.By blender 2,
Prevent the noble gas inflow to unstrpped gas supply line L2 and hydrogen selenide gas to basic gas supply line L1
Flow into.
(stream L5)
Blender 2 and surge tank 3 are connected by stream L5.In addition it is also possible to arrange not shown on stream L5
Open and close valve.
In Fig. 1 exemplified with one end of basic gas supply line L1 and one end of unstrpped gas supply line L2 with mix
Device 2 connects, and arranges the feedway 101 of stream L5 between blender 2 and surge tank 3.But, the present invention
It is not limited to this.For example, it is also possible to be the feedway not having blender 2, or can also be there is no blender
2 and stream L5 and basic gas supply line L1 and unstrpped gas supply line L2 one end the most directly with buffering
The feedway that tank 3 connects.I.e., it is also possible in tank, carry out the mixing of gas.
(surge tank 3)
Surge tank 3 is the accumulator tank for storing the Selenium hydride. mixed gas being adjusted to normal concentration by blender 2.
The internal volume of surge tank 3 is not particularly limited, it is possible to manufacture device according to Selenium hydride. mixed gas to solaode
Quantity delivered suitably selects.Can be according to the internal volume of surge tank 3 and Selenium hydride. mixed gas to solaode system
The quantity delivered of manufacturing apparatus suitably selects Selenium hydride. mixed gas storage capacity in surge tank 3.Such as, to solar energy
In the case of the Selenium hydride. mixed gas quantity delivered of battery producing device is 100～200L/min, can be by surge tank inner capacities
It is set to 20～400L.
Pressure upper limit and the threshold pression of surge tank 3 are not particularly limited, it is possible to according to Selenium hydride. mixed gas in buffering
Storage capacity and Selenium hydride. mixed gas in tank 3 suitably select to the quantity delivered of solaode manufacture device.Example
As, the pressure store of the Selenium hydride. mixed gas in surge tank 3 can be set to the scope of 0.1～0.5Mpa.
(stream L6)
Connecting on surge tank 3 and have one end of stream L6, the other end of stream L6 is the outlet of mixed gas, and this goes out
Mouth manufactures device with solaode and is connected.Thereby, it is possible to manufacture unit feeding selenium from surge tank 3 to solaode
Change hydrogen mixed gas.It addition, the upstream position of the outlet at stream L6, i.e. the supply mouth side at stream L6 are provided with
Open and close valve 21.
When Selenium hydride. mixed gas is supplied to solaode manufacture device from surge tank 3, open open and close valve 21.
On the other hand, when Selenium hydride. mixed gas not being supplied to solaode manufacture device from surge tank 3, make and break is closed
Valve closing 21.
Additionally, when Selenium hydride. mixed gas is supplied to solaode manufacture device with constant pressure, it is also possible to
Not shown pressure regulator is set on stream L6.
It addition, when Selenium hydride. mixed gas being supplied to multiple solaode and manufacturing device, it is also possible to arrange two
Above open and close valve 21.At this point it is possible to make stream L6 branch.
(stream L7)
Having one end of stream L7 it addition, connect on surge tank 3, the other end of stream L7 is connected with Pressure gauge 22.
Pressure gauge 22 can be utilized to measure the pressure of the Selenium hydride. mixed gas in surge tank 3.It addition, set on stream L7
It is equipped with open and close valve 23.Open and close valve 23 is normally open.
Further, preferably on surge tank 3, connection has not shown vacuum pump etc..Thus, in removing surge tank 3
During the purging gases such as the nitrogen of residual, it is possible to by vacuum pump, purging gas is exhausted.
(omission of surge tank)
In addition it is also possible to omit surge tank 3 in the present invention.Confession to the present embodiment not using surge tank 3
For device (not shown), the stream L5 shown in Fig. 1 and stream L6 is directly connected to, thus can also be not provided with
Stream L7, Pressure gauge 22 and the open and close valve 23 being connected with surge tank 3.
(bypass flow path L3)
One end of bypass flow path L3 is connected with basic gas supply source or basic gas supply line L1, the other end and position
Connect in the stream L2 of the primary side (upstream side) of 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 mode when manufacturing Selenium hydride. mixed gas, and is stopping
It is open mode during manufacture Selenium hydride. mixed gas.When automatic valve 14 is open mode, calibration gas is from basic gas
Body supply line L1 supplies to unstrpped gas supply line L2 via bypass flow path L3.
By arranging bypass flow path L3 and automatic valve 14, when stopping manufacturing Selenium hydride. mixed gas, unstrpped gas supplies
Connect with basic gas supply line L1 to stream L2.When manufacturing Selenium hydride. mixed gas, unstrpped gas supply stream
Road L2 does not connects with basic gas supply line L1.Therefore, when manufacturing Selenium hydride. mixed gas, due to unstripped gas
Body supply line L2 does not connects with basic gas supply line L1, and therefore hydrogen selenide gas will not flow to bypass flow path
The primary side (upstream side) of the automatic valve 14 of L3.
Calibration gas is the gas of the hydrogen selenide gas not comprising high concentration, then be not particularly limited.Can appoint
Meaning selects calibration gas.As calibration gas, such as preferably noble gas or with noble gas component as main constituent
Gas.Additionally, in FIG exemplified with being supplied to basic gas supply line L1 from basic gas supply source
Noble gas is used as the structure of calibration gas.However, it is also possible to one end of bypass flow path L3 is connected to not shown
The calibration gas supply source that arranges separately or the noble gas supply source shared with other devices, from these supply sources to
Bypass flow path L3 supply calibration gas (with reference to Fig. 7).But, in order to prevent the maximization of feedway 101 also
And need not the one end adding calibration gas supply source, preferably bypass flow path L3 with basic gas supply line L1 even
Connect.
It addition, the link position of one end of bypass flow path L3 and basic gas supply line L1 is not particularly limited.So
And, one end of bypass flow path L3 is preferably to be connected in the way of the position of basic gas supply source and basic gas
Supply line L1 connects.According to this structure, when calibration gas flows through basic gas supply line L1, it is possible to anti-
Only impurity is mixed in calibration gas.
Further, it is also possible to not shown pressure regulator is set in bypass flow path L3.
(branch flow passage L4)
One end of branch flow passage L4 supplies stream with the unstrpped gas of the primary side (downstream) of mass flow controller 11
Road L2 connects, and the other end is connected with not shown discharge duct.On branch flow passage L4, from upstream side towards downstream
Side, is disposed with automatic valve (the second open and close valve) 15 and mass flowmenter 16.Automatic valve 15 is manufacturing Selenium hydride.
It is closed mode during mixed gas, and is open mode when stopping manufacturing Selenium hydride. mixed gas.When automatic valve 15
For (when stopping manufacturing Selenium hydride. mixed gas) during open mode, calibration gas is from basic gas supply line L1
Supply to branch flow passage L4 via bypass flow path L3 and unstrpped gas supply line L2.
When manufacturing Selenium hydride. mixed gas, branch flow passage L4 and unstrpped gas supply line L2 are by automatic valve 15 sections
Disconnected.Further, when stop manufacture Selenium hydride. mixed gas time, branch flow passage L4 and unstrpped gas supply line L2 not by
Automatic valve 15 blocks, i.e. branch flow passage L4 connects with unstrpped gas supply line L2.When manufacturing Selenium hydride. gaseous mixture
During body, owing to branch flow passage L4 and unstrpped gas supply line L2 are truncated, therefore hydrogen selenide gas will 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, it is set
The flow of the calibration gas of mass flow controller 11 is flow through for metering.
It addition, in order to revise hydrogen selenide gas flow value in mass flow controller 11, this embodiment party more accurately
The mass flow controller 16 of formula be preferably positioned on when manufacture Selenium hydride. mixed gas time hydrogen selenide gas without flow through
On stream.It is prevented from selenium crystallization to separate out to mass flowmenter 16.Specifically, as it is shown in figure 1, mass flowmenter
16 primary side (downstream) being preferably positioned on when manufacturing Selenium hydride. mixed gas the automatic valve 15 being closed mode.
Utilize mass flowmenter 16, when stopping manufacturing Selenium hydride. mixed gas, measure via bypass flow path L3 and former
The mass flow of the calibration gas that material gas supply line L2 supplies to branch flow passage L4.This calibration gas is when stream
When crossing unstrpped gas supply line L2, flow through mass flow controller 11.
Preferably in mass flowmenter 16, it is mounted with mass flow sensor.
The mass flow sensor being loaded into mass flowmenter 16 is not particularly limited, such as, can use thermal mass stream
The mass flow biography that quantity sensor, differential pressure type mass flow sensor and Coriolis formula mass flow sensor etc. are common
Sensor.
(control unit 19 and distribution E1 and E2)
Mass flowmenter 16 is connected with control unit 19 by distribution E2.That is, to the correction of branch flow passage L4 supply
Can be sent to control unit 19 from mass flowmenter 16 by distribution E2 by the flow measurements of gas.
Additionally, it has been observed that be also associated with the distribution E1 being connected with mass flow controller 11 in control unit 19.
The flow value of calibration gas is measured respectively, concurrently in mass flow controller 11 and mass flowmenter 16
Deliver 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 the data for revising to mass flow controller 11.So, utilize the difference obtained,
When recovering the manufacture of Selenium hydride. mixed gas, revise and flow to the primary side (downstream) of mass flow controller 11
The flow value of hydrogen selenide gas.Mass flow controller 11 and mass flowmenter 16 more preferably flow measurement range
Identical mass flow sensor, the most particularly preferably carries out the quality stream of flux modification with the gas of same composition
Quantity sensor.
Such as, if mass flow controller 11 is mounted with thermal type mass flow sensor, and it is corrected with Selenium hydride.
The gamut of flow measurement is the specification of 10 [L/min], then particularly preferably use identical for mass flowmenter 16,
That is, it is mounted with thermal type mass flow sensor and the gamut of flow measurement that is corrected with Selenium hydride. is 10 [L/min]
Specification.
As mass flow controller 11 and the instrument of mass flowmenter 16, by so selecting similar or phase
Same instrument, it is possible to obtain following effect.That is, survey about by mass flow controller 11 and mass flowmenter 16
The flow measurements of the calibration gas measured, it is not necessary to flow rate conversion required when carrying out use heterogeneous gas processes,
After measuring calibration gas, it is possible to directly utilize control unit 19, calculate selenizing for mass flow controller 11
The correction of the flow value of hydrogen or the flow value of revised hydrogen selenide gas.
Control unit 19 receives the calibration gas each measured by mass flow controller 11 and mass flowmenter 16
Flow value.It addition, control unit 19 is according to the difference of the flow value of each calibration gas received, calculate by
The correction of the flow value of the hydrogen selenide gas that mass flow controller 11 sets or the stream of revised hydrogen selenide gas
Value, and pass to mass flow controller 11.
Additionally, when stopping manufacturing Selenium hydride. mixed gas, mass flow controller 11 and mass flowmenter 16 survey
Measure the flow measurements of calibration gas.Afterwards, when recovering the manufacture of Selenium hydride. mixed gas, selenizing will be added
The flow value of the correction of hydrogen is as the flow setting value of mass flow controller 11.
Control unit 19 can calculate correction or the stream of revised hydrogen selenide gas of the flow value of hydrogen selenide gas
Value, is not particularly limited.Can arbitrarily select to use arithmetic unit or system.As this control unit 19,
Such as can use common computer or the programmable logic controller with central operation processing means.
(supply method of Selenium hydride. mixed gas)
Below, to the supply method of the Selenium hydride. mixed gas of the present embodiment using feedway 101 (following,
It is only called " supply method ") illustrate.
The supply method of present embodiment includes following process.
First, by by the noble gas of mass flow controller 6 flow-control and by mass flow control in blender 2
The mixed raw material gas mixing of device 11 processed flow-control, to become the Selenium hydride. concentration set point of regulation, thus manufactures
Selenium hydride. mixed gas.And, the mixed gas produced is stored in surge tank 3 (Selenium hydride. mixed gas
Manufacture process (I)).
That afterwards, be supplied to this Selenium hydride. mixed gas in surge tank 3 to be arranged at the back segment of feedway 101,
(the supply process of Selenium hydride. mixed gas in the consumer device being positioned at primary side of solaode manufacture device etc.
(Ⅲ))。
After the manufacture process of Selenium hydride. mixed gas, i.e. after stopping the manufacture of Selenium hydride. mixed gas, make
The calibration gas of same flow, preferably makes identical calibration gas, and flowing is by mass flow controller 11 and matter
Amount effusion meter 16.According to the calibration gas measured respectively by mass flow controller 11 and mass flowmenter 16
The difference of flow value, revises the flow value (flow of unstrpped gas of the hydrogen selenide gas flowing through mass flow controller 11
The makeover process (II) of setting value).
Here, as the consumer device of the primary side (downstream) being positioned at Selenium hydride. mixed gas, describe solar energy
Battery producing device, but can be the device of any consumption Selenium hydride. mixed gas.For example, it is possible to enumerate consumption selenizing
Hydrogen mixed gas is as the semiconductor-fabricating device etc. of impurity gas.
(manufacture set-up procedure)
First, the preparation before the manufacture of Selenium hydride. mixed gas is carried out.Specifically, the supply dress shown in Fig. 1 is prepared
Put 101, in the apparatus, while open and close valve 4,21,23 and automatic valve 9 are carried out opening and closing operations, make nitrogen etc. blow
Scavenging body circulates, and carries out the purging in stream.After completing above-mentioned purging, it is set to automatic valve 14,15 close shape
State, and all of open and close valve in addition to automatic valve 14,15 and automatic valve are set to open mode, complete to manufacture standard
Standby.
Furthermore it is preferred that remove the nitrogen etc. remained in surge tank 3 in advance to purge gas.For example, it is preferable to use not shown
Vacuum pumps etc. carry out vacuum exhaust from the not shown vacuum exhaust valve etc. being connected with surge tank 3.
(manufacture process (I) of Selenium hydride. mixed gas)
Then, noble gas is supplied from basic gas supply line L1 to blender 2, from unstrpped gas supply line
L2 supplies hydrogen selenide gas to blender 2.That is, by flow (the flow setting value V of noble gas1[L/min]) and
Flow (the flow setting value V of hydrogen selenide gas2[L/min]) control to supply while flow set in advance.
More specifically, control the flow of noble gas and the flow of hydrogen selenide gas respectively so that become from presetting
, the setting value (Selenium hydride. of Selenium hydride. concentration in the Selenium hydride. mixed gas being supplied to solaode and manufacturing device
Concentration C [%], C=V2/(V1+V2) × 100) in each flow of determining.So, from basic gas supply line
L1 supplies noble gas to blender 2, supplies hydrogen selenide gas from unstrpped gas supply line L2 to blender 2.
Be more particularly described, then noble gas is supplied to basic gas supply line L1 from basic gas supply source.Indifferent gas
After body reduces pressure into authorized pressure by pressure regulator 5 in basic gas supply line L1, to mass flow control
Import in device 6 processed.In mass flow controller 6, preset the flow setting value V of noble gas1[L/min]。
That is, the flow of noble gas is controlled at V by mass flow controller 61[L/min].And, when automatic valve 8 is for beat
During open state, via mass flow controller 6, it is stipulated that flow (V1) noble gas supply to blender 2.
It addition, hydrogen selenide gas is supplied to unstrpped gas supply line L2 from unstrpped gas supply source.Hydrogen selenide gas exists
After unstrpped gas supply line L2 reduces pressure into authorized pressure by pressure regulator 10, to mass flow controller
Import in 11.In mass flow controller 11, preset the flow setting value V of hydrogen selenide gas2[L/min]。
That is, the flow of hydrogen selenide gas is controlled at V by mass flow controller 112[L/min].And, when automatic valve 13
During for open mode, via mass flow controller 11, it is stipulated that flow (V2) hydrogen selenide gas to blender 2
Supply.
Secondly, utilize blender 2 to mix the noble gas with the supply of regulation flow and hydrogen selenide gas, thus manufacture rule
Determine concentration C=V2/(V1+V2) × 100) the Selenium hydride. mixed gas of [%].
Here, the concentration of Selenium hydride. mixed gas is not particularly limited, it is possible to manufacture wanting of device according to solaode
Ask and suitably select.Specifically, such as, the concentration of the Selenium hydride. in Selenium hydride. mixed gas can be set to
5～20vol%.
Then, via stream L5, the Selenium hydride. mixed gas being mixed into regulation Selenium hydride. concentration is stored in surge tank 3
In.The pressure of the Selenium hydride. mixed gas stored can be measured with Pressure gauge 22.Manufacture Selenium hydride. mixed gas, and
And be supplied to surge tank 3 by stream L5, until the pressure of the Selenium hydride. mixed gas stored arrives set in advance
Pressure upper limit.When the pressure measured by Pressure gauge 22 arrives pressure upper limit, by all of automatic valve 8,9 and 13
It is set to off closed state, stops the supply to surge tank 3, thus stop the manufacture of Selenium hydride. mixed gas.Additionally, from
Dynamic valve 9 is also switched off, and this is to implement makeover process described later.
Afterwards, the pressure of the Selenium hydride. mixed gas in utilizing Pressure gauge 22 to detect surge tank 3 arrives and presets
Threshold pression below time, the automatic valve 8,9,13 being closed is set to open mode, starts mixed gas to buffering
The supply of tank 3, i.e. starts the manufacture of Selenium hydride. mixed gas.Afterwards, when utilizing Pressure gauge 22 to detect surge tank 3
Pressure when arriving more than pressure upper limit, all of automatic valve 8,9,13 is set to off closed state, stops mixed gas
To the supply of surge tank 3, i.e. stop the manufacture of Selenium hydride. mixed gas.Afterwards, according to the pressure of surge tank 3, depend on
Manufacture and the manufacture of secondary repetition Selenium hydride. mixed gas stop.
(the supply process (III) of Selenium hydride. mixed gas)
The Selenium hydride. mixed gas being stored in surge tank 3 is manufactured according to solaode the Selenium hydride. mixing in device
The condition of consumption of gas manufactures unit feeding to solaode.
Additionally, in not using the supply method of present embodiment of surge tank 3, be not according to being measured by Pressure gauge 22
Force value in the surge tank 3 gone out carries out manufacturing or manufacturing the switching stopped of Selenium hydride. mixed gas, but can basis
The condition of consumption of the Selenium hydride. mixed gas in solaode manufacture device carries out manufacture or the system of Selenium hydride. mixed gas
Make the switching of stopping.Such as, the manufacture of mixed gas can be stopped when not consuming, and/or, when consuming
Time can manufacture.
So, Selenium hydride. mixed gas stable for Selenium hydride. concentration is continuously fed to solaode manufacture in device.
(makeover process (II) of the flow setting value of unstrpped gas)
Stopping after the manufacture of the Selenium hydride. mixed gas of surge tank 3, carrying out unstrpped gas described below
The makeover process of flow setting value.By this makeover process, revise to the primary side (downstream of mass flow controller 11
Side) flow, the flow setting value of hydrogen selenide gas.
Specifically, make the calibration gas of same flow flow through be arranged at unstrpped gas supply line L2 and control selenizing
The mass flow controller 11 of the flow of hydrogen and the mass flowmenter 16 of correction.Flow continuously in respective position measurement
The flowing of dynamic calibration gas.And, measure respectively according to by mass flow controller 11 and mass flowmenter 16
The difference of the flow value of the calibration gas gone out, the flow revising the hydrogen selenide gas flowing through mass flow controller 11 sets
Definite value.
Further makeover process is illustrated.
First, automatic valve 9 is set to off closed state, stops the supply of hydrogen selenide gas.It is also switched off automatic valve 8 and 13.
Then, automatic valve 14,15 is set to open mode.It is as a result, it is possible to make the noble gas as basic gas
Continue to flow through by bypass flow path L3, from bypass flow path L3 and unstrpped gas supply line L2 from basic gas supply source
Link position to the unstrpped gas supply stream between the link position of branch flow passage L4 and unstrpped gas supply line L2
Stream that road L2 and branch flow passage L4 are constituted (after, this continuous print stream is referred to as " calibration gas stream ").
This noble gas can use the gas identical with basic gas.The noble gas used plays the merit of calibration gas
Energy.According to this process, it is possible to make the calibration gas of same flow continuously flow through setting on calibration gas stream
Mass flow controller 11 and mass flowmenter 16.
Then, mass flow controller 11 and mass flowmenter 16 by arranging on calibration gas stream are surveyed respectively
Measure the flow value of calibration gas.Use these measured values to carry out calculation process by control unit 19, and tie with it
Based on Guo, revise when recovering the manufacture of Selenium hydride. mixed gas, the Selenium hydride. of mass flow controller 11 outflow
The flow value of gas.
Additionally, gas when timing and mixed gas manufacture diverse in the case of, or ought be as required
Carry out mass flow controller and the respective timing of mass flowmenter separately, gas when timing and flow measurement
In the case of diverse, preferably before calculating flow error, use the flow modificatory coefficient being referred to as conversion factor
Reduced discharge.
In more detail, calculating of the flow error in the present invention is illustrated.
When calculating flow error, first, mass flow controller 11 is utilized to be corrected the control with the flow of gas,
Further, measure the flow V of calibration gas simultaneously3[L/min].Further, utilization is positioned at the quality in downstream simultaneously
The flow V of calibration gas measured by effusion meter 164[L/min]。
When manufacturing Selenium hydride. mixed gas, if selenium crystallization more precipitate into the raw material comprising mass flow controller 11
In gas supply line L2, then the flow control accuracy of mass flow controller 11 reduces.Now, crystallize due to selenium
Existence, therefore there is the correction measured by mass flow controller 11 when stopping manufacturing Selenium hydride. mixed gas and use
The flow V of gas3[L/min] is less than the tendency of the flow of the calibration gas originally should measured.
In contrast, mass flowmenter 16 be configured in when manufacture Selenium hydride. mixed gas time hydrogen selenide gas without flow through
Position.Therefore, mass flowmenter 16 the flow V of the calibration gas measured4[L/min] with originally should measure
The flow of calibration gas equal.
So, when stopping manufacturing Selenium hydride. mixed gas, by mass flow controller 11 and mass flowmenter 16 points
The flow value V of the calibration gas do not measured3、V4The difference of [L/min] represents mass flow controller exactly
The reduction situation of the flow control accuracy of 11, represents the raw material comprising mass flow controller 11 the most exactly
The degree of the amount of precipitation of the selenium crystallization of gas supply line L2.
Additionally, describe the flow V of the calibration gas measured by mass flow controller 11 at this3[L/min] is little
Situation in the flow of the calibration gas originally should measured.But, even if more than the correction originally should measured
In the case of the flow of gas, it is also possible to process equally, i.e. it is modified.
Afterwards, the flow measurement value of calibration gas that will be obtained by mass flow controller 11 and mass flowmenter 16
V3、V4[L/min] passes to control unit 19 via distribution E1, E2 respectively.
Then, according to flow measurements V of the calibration gas obtained by mass flow controller 113[L/min] with by
Flow measurements V of the calibration gas that mass flowmenter 16 obtains4The difference of [L/min], calculates mass flow control
The correction of the flow setting value of the hydrogen selenide gas in device 11.
Specifically, according to following formula, by flow measurements V3、V4[L/min] calculates flow error A and correction factor B.
Flow error A=(V3-V4∣/V4) × 100 [%]
Correction factor B=V4/V3
But, for mass flow controller, at timing and gas diverse when manufacturing mixed gas
In the case of, or the timing of mass flow controller ought be carried out the most separately, made when timing and flow measurement
The kind of gas inconsistent in the case of, need to utilize the flow modificatory coefficient being referred to as conversion factor to be modified.
Using flow modificatory coefficient by V3And V4After being modified to the flow value of kind based on calibration gas, calculate stream
Amount error A and correction factor B.
After calculating flow error A and correction factor B, according to following formula, calculate to mass flow controller 11
The flow setting value V of hydrogen selenide gas that send, revised5[L/min]。
Flow setting value V5[L/min]=B × V2[L/min]
Then, the flow setting value V of hydrogen selenide gas that will calculate5[L/min] sends to mass flow via distribution E1
Controller 11.Flow setting value V5The manufacture process of the Selenium hydride. mixed gas carried out thereafter uses.So,
After the makeover process of the flow setting value of unstrpped gas, used during the manufacture of the Selenium hydride. mixed gas that is restored
Correction value.That is, the flow of the hydrogen selenide gas flowed to the primary side (downstream) of mass flow controller 11 sets
Definite value is corrected for the correction calculated by control unit 19.
According to above process, complete after using according to the amount of precipitation correction of the selenium crystallization in mass flow controller 11
The flow setting value V of Selenium hydride.5[L/min], be suitable for being given to solaode and manufacture device, for manufacturing
The preparation of the Selenium hydride. mixed gas of regulation Selenium hydride. concentration.Afterwards, automatic valve 14,15 can be closed and open automatic valve
9.That is, by so opening, can by from the link position of bypass flow path L3 and unstrpped gas supply line L2 to point
Exist in unstrpped gas supply line L2 between the link position of Zhi Liulu L4 and unstrpped gas supply line L2
Calibration gas is replaced into hydrogen selenide gas.Now, automatic valve 15 can be opened, or can also regulation time
Machine is opened.
Additionally, only use correction factor B when the flow-control of hydrogen selenide gas.That is, at the flow of calibration gas
During measurement, mass flow controller 11 does not carry out using the correction of correction factor B.
Afterwards, automatic valve 14,15 is set to off closed state, and all of in addition to automatic valve 14,15 is opened
Valve closing and automatic valve are set to open mode, carry out the Selenium hydride. mixed gas manufacture process of described above.Second time with
After Selenium hydride. mixed gas manufacture process in, the raw material gas flow set point correct process before it accurately revise
, the flow setting value V of hydrogen selenide gas5[L/min] is set in mass flow controller 11.Therefore, it is possible to stream
Go out originally should flow to the flow V of the primary side (downstream) of mass flow controller 112The selenizing hydrogen of [L/min]
Body.And, can be by flow value V2The hydrogen selenide gas of [L/min] is supplied to blender 2.
Afterwards, manufacture process (I) and the flow setting value of unstrpped gas of enforcement Selenium hydride. mixed gas it are alternately repeated
Makeover process (II).So, chronically and be stably supplied and be suitable to be supplied to solaode from feedway 101
Manufacture device, the Selenium hydride. mixed gas of regulation Selenium hydride. concentration.
When the flow being alternately repeated the manufacture process (I) and unstrpped gas of implementing more than twice Selenium hydride. mixed gas sets
During makeover process (II) of definite value, it is also possible to change the makeover process (II) of the flow setting value of unstrpped gas as required
In the flow setting value of calibration gas carry out implementation process.When repeatedly, obtain the stream of multiple calibration gas
The difference of value.Therefore, when changing the flow setting value of calibration gas, the flow of each unstrpped gas can be made to set
Multiple correction factor B equalizations obtained by that obtain in the makeover process of definite value, so far and use, or also may be used
To determine that the correction factor B being applicable to range of flow to be set uses.
Such as, the manufacture process (I) of more than twice Selenium hydride. mixed gas and unstrpped gas are implemented being alternately repeated
In the case of the makeover process (II) of flow setting value, the flow measurements in manufacture process is V for the first time3a[L/min],
Correction factor obtained by the makeover process using this value is Ba, the flow measurements in manufacture process is for the second time
V3b[L/min], correction factor obtained in the makeover process using this value is Bb, and set V3a＜ V3b.This
Time, in manufacture later and makeover process, the flow measurements of hydrogen selenide gas is applicable to 0～V3a[L/min's]
The correction factor of situation is set to Ba, and the flow measurements of hydrogen selenide gas is applicable to V3a～V3bThe feelings of [L/min]
The correction factor of condition is set to Bb。
It addition, implement the manufacture process (I) of more than twice Selenium hydride. mixed gas and unstrpped gas when be alternately repeated
During makeover process (II) of flow setting value, it is also possible to be connected to the Pressure gauge 22 of surge tank less than authorized pressure it
Before, and after makeover process (II) enforcement of the flow setting value in unstrpped gas, automatic valve 14,15 is set to off
Closed state.Furthermore it is preferred that the value of flow error A is in the range of 5～30%, but it is not particularly limited to this scope, if
In practicality no problem, can suitably select.
The supply method of present embodiment according to the above description, it is possible to utilize calibration gas to remove unstrpped gas supply
The hydrogen selenide gas being detained in stream.Crystallize former therefore, it is possible to significantly reduce the selenium caused by the selfdecomposition of Selenium hydride.
Precipitation in material gas supply line L2.It addition, make flow V2The hydrogen selenide gas of [L/min] flows through mass flow
In the case of controller 11, though such as exist selenium crystallization precipitation, it is also possible to based on by hydrogen selenide gas without flow through
The correction flow value that the mass flowmenter 16 of the correction arranged on stream is measured, to mass flow controller 11
Send revised flow setting value V5[L/min].Therefore, it is possible to greatly reduce the stream of unstrpped gas supply line L2
Amount controls error.
Therefore, according to the supply method of the Selenium hydride. mixed gas of present embodiment, the opening and closing of short cycle is not carried out
Instrumentation that the switching of valve etc. are careful and the volume expansion of surge tank, reduce shift phenomenon compared with existing for a long time, from
And the Selenium hydride. mixed gas of stable Selenium hydride. concentration can be manufactured the supplies such as device to solaode.
It addition, in the feedway 101 of present embodiment, when stopping the manufacture of Selenium hydride. mixed gas, same
The calibration gas of flow flows through the quality of the flow being arranged at unstrpped gas supply line L2 and control hydrogen selenide gas
Flow controller 11 and the mass flowmenter 16 of correction.According to this structure, remove unstrpped gas with calibration gas
The hydrogen selenide gas being detained in supply line, therefore, it is possible to reduce the precipitation of the selenium crystallization caused by the selfdecomposition of Selenium hydride..
It addition, when manufacturing Selenium hydride. mixed gas, according to unstrpped gas supply line L2 flow through by hydrogen selenide gas
The mass flow controller 11 of upper setting and hydrogen selenide gas without flow through stream on the mass flowmenter 16 that arranges respectively
That measure, measure the difference of the flow measurements of the calibration gas of same flow, revise mass flow controller 11
The flow setting value of the hydrogen selenide gas flowed out.Thus, the flow-control of unstrpped gas supply line L2 is greatly reduced
Error, thus suppress shift phenomenon.Itself result it is not necessary to the careful instrumentation such as valve opening and closing of short cycle and
Jumbo surge tank, manufactures the Selenium hydride. mixing of the stable Selenium hydride. concentration of the supply of long durations such as device to solaode
Gas.
Additionally, the technical scope of the present invention is not limited to above-mentioned embodiment, at the main scope without departing from the present invention
In, it is possible to apply various change.
Such as, the feedway 101 of above-mentioned embodiment is for be arranged on mass flowmenter 16 on branch flow passage L4
Structure.But, the feedway 102 as described in Fig. 6, it is also possible to mass flowmenter 16 is arranged on automatic valve 14
Primary side (upstream side) bypass flow path L3 on.It has been observed that hydrogen selenide gas does not flows through at the beginning of automatic valve 14
Bypass flow path L3 of level side.Therefore, identical with above-mentioned feedway 101, can hydrogen selenide gas without flow through
Mass flowmenter 16 is set on stream.Accordingly it is also possible to be not provided with branch flow passage L4, at above-mentioned embodiment
On the basis of effect, it is possible to make feedway miniaturization.It is result it is not necessary to the valve opening and closing etc. of short cycle is careful
Instrumentation and jumbo surge tank, manufacture the stable Selenium hydride. concentration of the supply of long durations such as device to solaode
Selenium hydride. mixed gas.
It addition, as other embodiments, such as when flow error A exceedes setting, can be to feedway 101
The exception of operator notification mass flow controller 11, operator carry out the replacing of mass flow controller 11.
Embodiment
Below, it is shown that the preferred object lesson of the present invention.
(embodiment)
Use the feedway 101 shown in Fig. 1 to manufacture Selenium hydride. mixed gas, and manufacture device to solaode
Supply Selenium hydride. mixed gas the most for a long time.Manufacture when the Selenium hydride. mixed gas carrying out feedway 101
Cheng Shi, uses the condition of table 1.It addition, the correction of the flow setting value when the unstrpped gas carrying out feedway 101
During process, use the condition of table 2.
[table 1]
[table 2]
Table 2 shows when flow measurements V of mass flow controller 113Flow at makeover process middle controller
When being shown as 10.0L/min, the actual nitrogen flow through is 13.0L/min.
" once " described in table 2 be the manufacture process that carries out to carry out the correction of a flow setting value with
The combination number of times of makeover process, the most repeatedly this manufacture process and the combination of makeover process.
When repeating to manufacture and while makeover process, to solaode system under the implementation condition shown in table 1,2
When manufacturing apparatus supplies Selenium hydride. mixed gas continuously, the Selenium hydride. concentration analysis meter arranged on stream L6 is used (not scheme
Show), measure the rheological parameters' change with time of Selenium hydride. concentration in Selenium hydride. mixed gas.Fig. 2 shows by Selenium hydride. concentration
Time (natural law) interdependence of the Selenium hydride. concentration in that analysis meter is measured, Selenium hydride. mixed gas.It addition, figure
Show in 3 when time (natural law) interdependence of the flow error A repeated when manufacturing with makeover process.
(comparative example)
When implementing the makeover process of the flow setting value of unstrpped gas of feedway 101, except to mass flow control
The flow setting value V of the Selenium hydride. of device 11 processed2The correction of [L/min] does not use outside correction factor B, exists with embodiment
Under conditions of identical, produce Selenium hydride. mixed gas, and it is mixed to supply Selenium hydride. continuously to solaode manufacture device
Close gas.I.e., although enforcement makeover process, but in mass flow controller 11, do not use revised flow, and
Manufacture and supply.Identical with embodiment, use the Selenium hydride. concentration analysis meter arranged on stream L6 to measure
The rheological parameters' change with time of the Selenium hydride. concentration in Selenium hydride. mixed gas.Fig. 2 shows in Selenium hydride. mixed gas now
Time (natural law) interdependence of Selenium hydride. concentration.
(comparison of the measurement result of embodiment and comparative example)
As in figure 2 it is shown, in a comparative example, from measurement start until through about 40 days, in Selenium hydride. mixed gas
Selenium hydride. concentration is maintained near normal concentration 10.0%.But, natural law further across, then Selenium hydride. concentration is drastically
Increase.
It addition, for time (natural law) interdependence of the Selenium hydride. concentration of the flow error A shown in Fig. 3, from survey
Amount has started the natural law after about 40 days, and flow error A sharply increases.Its result, in a comparative example, from
Measurement has started the 100th day, and the Selenium hydride. concentration in Selenium hydride. mixed gas reaches 13.8%.
So, the main cause risen as Selenium hydride. concentration, the reason that can be listed below: owing to not using
The flow setting value V of the Selenium hydride. of the mass flow controller 11 of correction factor B2The correction of [L/min], therefore quality
The flow control accuracy of flow controller 11 reduces.
Relative to comparative example, though in an embodiment from measurement start through about 100 days, in Selenium hydride. mixed gas
Selenium hydride. concentration be also stabilized near 10.0%.Therefore, in the present invention, confirm can clock like precision ground and
The long-time period of about at least 100 days reduces the flow-control error of unstrpped gas supply line L2.This is because,
Supply method and the feedway 101 of the above-mentioned embodiment of the present invention can be utilized, according to based on the matter by correction
Flow error A that the flow value of calibration gas that amount effusion meter 16 is measured calculates and correction factor B, will flow through
The flow setting value V of the hydrogen selenide gas of mass flow controller 112[L/min] is modified to flow setting value
V5[L/min]。
Industrial applicability
Present invention can be suitably applied in supply method and the feedway of Selenium hydride. mixed gas.A kind of Selenium hydride. can be provided
The supply method of mixed gas and feedway, it need not careful instrumentation and jumbo surge tank, it is possible to
While suppression shift phenomenon, the Selenium hydride. mixed gas that supply of long duration Selenium hydride. concentration is stable.
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 adjusts 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 (8)
1. a supply method for Selenium hydride. mixed gas, has: the indifferent gas that will supply from basic gas supply line
Body mixes with the hydrogen selenide gas supplied from unstrpped gas supply line, manufacture be configured to normal concentration Selenium hydride. mix
Close the operation of gas；With supply described mixed gas operation,
The supply method of described Selenium hydride. mixed gas is characterised by,
During further including at the operation stopping manufacturing Selenium hydride. mixed gas, revise the flow setting value of unstrpped gas
Operation,
Described correction operation includes:
The calibration gas making same flow flows through and is arranged at described unstrpped gas supply line to control described selenizing hydrogen
The flow controlling unit of the flow of body and the operation of the airflow measurement unit of correction；
Obtain the stream of the described calibration gas measured respectively by described flow controlling unit and described airflow measurement unit
The operation of the difference of value；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,
Described calibration gas is from the described stream by described basic gas supply line Yu described unstrpped gas supply line
The described noble gas of the bypass flow path supply that the primary side of amount control unit connects.
The supply method of Selenium hydride. mixed gas the most according to claim 1, it is characterised in that make described correction
Described flow controlling unit and described airflow measurement unit is continued to flow through by different order with gas.
The supply method of Selenium hydride. mixed gas the most according to claim 1, it is characterised in that to described flow
Control unit and described airflow measurement unit use the flow-measuring method of same specification.
The supply method of Selenium hydride. mixed gas the most according to claim 1, it is characterised in that described when manufacturing
During Selenium hydride. mixed gas, described hydrogen selenide gas is not made to flow through described airflow measurement unit.
5. a feedway for Selenium hydride. mixed gas, by the noble gas that supplies from basic gas supply line with from
The hydrogen selenide gas mixing of unstrpped gas supply line supply, manufactures the Selenium hydride. mixed gas being configured to normal concentration,
Supply this Selenium hydride. mixed gas afterwards,
The feedway of described Selenium hydride. mixed gas is characterised by possessing:
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 Selenium hydride. mixed gas, by calibration gas to described
The primary side supply of the described flow controlling unit of unstrpped gas supply line；
The airflow measurement unit of correction, is arranged at the described correction gas when stopping manufacturing described Selenium hydride. mixed gas
Body flow through and when manufacture described Selenium hydride. mixed gas time described hydrogen selenide gas without flow through stream on；With
Control unit, when the described calibration gas making same flow flows through described flow controlling unit and the survey of described flow
During amount unit, according to the difference of the flow value of the calibration gas measured respectively, revise described flow controlling unit stream
The flow value of the described hydrogen selenide gas gone out,
Described calibration gas supply line is by described basic gas supply line and described unstrpped gas supply line
The bypass flow path that the primary side of described flow controlling unit connects.
The feedway of Selenium hydride. mixed gas the most according to claim 5, it is characterised in that
Being provided with the first open and close valve in described bypass flow path, described first open and close valve is when manufacturing described Selenium hydride. gaseous mixture
Be closed mode during body, when using described noble gas as calibration gas from described basic gas supply line to described
It is open mode during the supply of unstrpped gas supply line,
Primary side at described first open and close valve of described bypass flow path is provided with described airflow measurement unit.
The feedway of Selenium hydride. mixed gas the most according to claim 5, it is characterised in that
Primary side at the described flow controlling unit of described unstrpped gas supply line is provided with branch flow passage,
Being provided with the second open and close valve on described branch flow passage, described second open and close valve is when manufacturing described Selenium hydride. gaseous mixture
Be closed mode during body, when using described noble gas as calibration gas from described basic gas supply line to described
It is open mode during the supply of unstrpped gas supply line,
Primary side at described second open and close valve of described branch flow passage is provided with described airflow measurement unit.
The feedway of Selenium hydride. mixed gas the most according to claim 5, it is characterised in that described flow control
Unit processed and the flow-measuring method that described airflow measurement unit is 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 CN104769727A (en) | 2015-07-08 |
| CN104769727B true CN104769727B (en) | 2016-12-07 |
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| 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) |
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| DE102016003875A1 (en) * | 2016-03-31 | 2017-10-05 | Linde Aktiengesellschaft | Volumetric and gravimetric level for the production of gas mixtures |
| JP6904231B2 (en) * | 2017-12-13 | 2021-07-14 | 東京エレクトロン株式会社 | Substrate processing method, storage medium and raw material gas supply device |
| 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 |
| US20220157599A1 (en) * | 2019-11-12 | 2022-05-19 | Showa Denko K.K. | Adhered substance removing method and film-forming method |
| 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 |
| 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 |
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| 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 |
| JP5518404B2 (en) * | 2009-09-04 | 2014-06-11 | 大陽日酸株式会社 | Method and apparatus for supplying hydrogen selenide mixed gas for solar cell |
| JP5548208B2 (en) * | 2009-09-04 | 2014-07-16 | 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 CN CN201380052051.2A patent/CN104769727B/en not_active Expired - Fee Related
- 2013-10-21 KR KR1020157006775A patent/KR101661483B1/en active IP Right Grant
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| Publication number | Publication date |
|---|---|
| WO2014065233A1 (en) | 2014-05-01 |
| CN104769727A (en) | 2015-07-08 |
| KR20150044437A (en) | 2015-04-24 |
| JP6065329B2 (en) | 2017-01-25 |
| TWI618672B (en) | 2018-03-21 |
| JPWO2014065233A1 (en) | 2016-09-08 |
| TW201427896A (en) | 2014-07-16 |
| KR101661483B1 (en) | 2016-09-30 |
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