CN108169293A - High-precision film resistor hydrogen gas sensor calibration device and Calibration Method - Google Patents
High-precision film resistor hydrogen gas sensor calibration device and Calibration Method Download PDFInfo
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- CN108169293A CN108169293A CN201810140847.8A CN201810140847A CN108169293A CN 108169293 A CN108169293 A CN 108169293A CN 201810140847 A CN201810140847 A CN 201810140847A CN 108169293 A CN108169293 A CN 108169293A
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 112
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000007789 gas Substances 0.000 claims abstract description 66
- 239000001257 hydrogen Substances 0.000 claims abstract description 60
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 60
- 238000012360 testing method Methods 0.000 claims abstract description 29
- 230000004044 response Effects 0.000 claims abstract description 17
- 239000010408 film Substances 0.000 claims description 61
- 238000009413 insulation Methods 0.000 claims description 19
- 150000002431 hydrogen Chemical class 0.000 claims description 12
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- 238000005485 electric heating Methods 0.000 claims description 2
- 239000010409 thin film Substances 0.000 claims description 2
- 238000011088 calibration curve Methods 0.000 abstract description 7
- 230000003068 static effect Effects 0.000 abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 230000035945 sensitivity Effects 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000009021 linear effect Effects 0.000 description 2
- 229920001342 Bakelite® Polymers 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000004637 bakelite Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000000205 computational method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000003550 marker Substances 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 230000009022 nonlinear effect Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000002277 temperature effect Effects 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
Abstract
The invention discloses a kind of high-precision film resistor hydrogen gas sensor calibration device, the gas flow controller and constant temperature atmosphere test chamber including connection of mutually ventilating and the resistance instrument for the temperature controller that temperature is controlled for constant temperature atmosphere test chamber and for testing output resistance.The invention discloses the Calibration Method that a kind of high-precision film resistor hydrogen gas sensor calibration device uses, including obtaining temperature characteristics and obtaining hydrogen response characteristic curve.It can arbitrarily adjustment criteria gas concentration value and flow by the present invention, the wide precision of concentration adjustable range is high, the influence of ambient temperature interference and gas flowing to calibration can be greatly reduced when demarcating density of hydrogen calibration curve, so that it is guaranteed that sensing unit output resistance and density of hydrogen standard value correspondence are accurately obtained, convenient for every Static State Index of accurate analysed film resistance hydrogen gas sensor；The temperature calibration curve of film resistor hydrogen gas sensor can also be obtained by the present invention.
Description
Technical field
The present invention relates to a kind of hydrogen gas sensor calibration device and Calibration Methods more particularly to one kind to obtain film to be accurate
Resistor-type hydrogen gas sensor hydrogen inductive reactance changing value and standard density of hydrogen value correspondence and the high-precision film designed
Resistance hydrogen gas sensor calibration device and Calibration Method.
Background technology
Hydrogen gas sensor type is various, and variety classes sensor characteristics is different, therefore respectively has advantage and disadvantage.It is wherein adjoint partly to lead
Preparation process maturation and aftertreatment technology constantly improve develop rapidly a kind of film resistor hydrogen gas sensor.
The main operational principle of film resistor hydrogen gas sensor is hydrogen adsorption, infiltration when sensor is exposed in hydrogen
The quick material-sensitive layer resistance of hydrogen in sensor can be made to become larger, when sensor is removed from hydrogen, hydrogen can be detached from the quick material of hydrogen, make
The quick resistance of hydrogen reduces and is restored to zero mark resistance.Due to it with micro-volume, range is big, reproducible, back end test equipment
With measuring technology it is ripe the advantages that there is good future in engineering applications, but it has strong non-linear, temperature sensitivity simultaneously
Etc. characteristics, these characteristics the atmosphere sensor Calibration Method in national standard is not applied to, therefore film resistor hydrogen sense
The calibration of device is always a problem.Because sensor Calibration Method be directly related to sensor measurement accuracy and calibration it is accurate
Property, special calibration device is devised for its key property thus, and have studied Calibration Method and greatly improve calibration precision.
The calibration of sensor, exactly by testing the relationship set up between sensor input and output quantity, while
It can determine that the error relationship under different use conditions obtains its static characteristic.The static characteristic of sensor, specifically mainly
Finger depicts the calibration curve between sensor input and output quantity by a series of experiments data, can therefrom analyze weight
Want static characteristic index, such as the linearity, lag error, repeatability error and precision, sensitivity.
From the point of view of meterological, measurement error has quite stringent definition, it characterize measured value and actual value it
Between difference, can not generally directly obtain actual measured value, but can add by using appropriate standard value and using statistics
With estimation.Usual method is as standard value output device, such as metrological service one using the high device of ratio of precision design objective
As first select 3~5 values in the range of working sensor, then select high-purity gas cylinder of configured good concentration in room temperature according to them
It is lower to provide standard density of hydrogen value to tested sensor, sensor is demarcated according to sensor output value.This tradition
Method is only applicable to the sensor of linearity height, fast response time, temperature-insensitive, for film resistor hydrogen gas sensor,
It is primarily present 3 aspect major defects：1) statistical sample quantity is far from enough, and the larger non-linear property of sensor can cause greatly
Calibration error, the calibration precision of calibration curve obtained using the method is low, therefore can also be brought to sensor test greatly
Measurement error；2) it is larger that calibration experiment environmental temperature fluctuation is carried out at room temperature, for this kind of temperature of film resistor hydrogen gas sensor
The high sensor of sensibility, measurement error caused by environmental temperature fluctuation is even considerably beyond hydrogen response background values；3) in addition,
In addition to Static State Index, other characteristics such as response time, response speed, gas-selectively, temperature characterisitic of sensor can not also lead to
Calibration experimental provision is crossed to obtain, it is also necessary to which other devices are completed with experiment.More than reason is based on, for film resistor hydrogen
The special high-accuracy calibration device and Calibration Method of Sensor Design have accurate obtain of its properties and calibration curve
Significance.
In conclusion since the sensing chip of film resistor hydrogen gas sensor generally selects palladium-base alloy to do the quick material of hydrogen,
With good invertibity and gas-selectively, but the quick resistance value of hydrogen has strong non-linear relation with extraneous density of hydrogen value,
And the quick resistance value of hydrogen not only also changes with density of hydrogen variation with ambient temperature value, and temperature control is even higher than hydrogen
Sensitivity, therefore the coupled relation of temperature and density of hydrogen must be reduced during calibration to improve calibration precision, hydrogen is calibrated respectively
After gas concentration and temperature are to the response curve of sensor, then hydrogen gas sensor mark can be greatly improved using the method for temperature-compensating
School and measurement accuracy；But traditional calibration device and Calibration Method method can not realize this purpose.
Invention content
The purpose of the present invention is that solve the above-mentioned problems and provides a kind of high-precision film resistor hydrogen gas sensor
Calibration device and Calibration Method.
The present invention is achieved through the following technical solutions above-mentioned purpose：
A kind of high-precision film resistor hydrogen gas sensor calibration device is tested including gas flow controller, constant temperature atmosphere
Chamber, temperature controller and resistance instrument, the gas flow controller include at least two input ports and a delivery outlet, Mei Gesuo
It states input port and the delivery outlet connects a program-controlled mass flowmenter respectively；The constant temperature atmosphere test chamber include housing and
Temperature sensor, film resistor hydrogen gas sensor, the electric heater being placed in the inner cavity of the housing, the housing, which is equipped with, to be divided
The air inlet not communicated with the inner cavity of the housing and gas outlet；The delivery outlet of the gas flow controller and the constant temperature gas
The air inlet connection of atmosphere test chamber, the gas outlet of the constant temperature atmosphere test chamber are communicated with air, the letter of the temperature sensor
The power input of number output terminal and the electric heater respectively with the signal input part and computer heating control of the temperature controller
Output terminal connects, and the signal output end of the film resistor hydrogen gas sensor is connect with the signal input part of the resistance instrument.
Preferably, the constant temperature atmosphere test chamber further includes chip mounting circuit boards, pinboard, connecting plate, thermal insulation layer
And head cover, the electric heater are electric network, the thermal insulation layer is set on the interior cavity wall of the housing, and the electric network is set on
The outside of the thermal insulation layer, the chip mounting circuit boards are installed on the inner cavity middle position of the housing, the film resistor
Hydrogen gas sensor is installed in the chip mounting circuit boards, and the upper surface of the chip mounting circuit boards is equipped with double socket bottom
Seat or double socket contact pin, the pinboard are installed on the surface of the chip mounting circuit boards, the following table of the pinboard
Face is equipped with the double socket contact pin being electrically connected with the chip mounting circuit boards or double socket pedestal, the temperature sensor
The lower surface of pinboard is installed on, the head cover is installed on the upper end of the housing and equipped with connection plate interface, the connecting plate
It is embedded in the head cover, top pads and bottom land, the top weldering is respectively equipped at the top and bottom of the connecting plate
Disk is used to be electrically connected with the temperature controller and the resistance instrument, and the bottom land is used for and pair on the pinboard
It arranges socket contact pin or the output signal line of double socket pedestal and the temperature sensor is electrically connected；On the housing into
Gas port is located at the lower section of the chip mounting circuit boards, and the gas outlet on the housing is located at the top of the connecting plate.
Further, multiple vertical support column vias are respectively equipped on the chip mounting circuit boards and the pinboard,
The lower end of multiple vertical support columns is fixed in the intracavity bottom cavity wall of the housing, and the upper end of the support column is worn successively
The support column via in the chip mounting circuit boards and the pinboard is crossed, insulation sleeve is set with outside the support column.
The Calibration Method that a kind of high-precision film resistor hydrogen gas sensor calibration device uses, it is bent including obtaining temperature characterisitic
Line and acquisition hydrogen response characteristic curve, wherein, the method for the acquisition temperature characteristics is：The inner cavity of the housing is from room
Temperature starts gradually to be heated to 40 DEG C, and temperature point is：Room temperature, 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C, the high-precision film resistor hydrogen
Gas sensor calibration device is placed at room temperature more than half an hour, passes through the temperature sensor, the electric heater and described
Temperature controller controls the temperature in the inner cavity of the housing, temperature error is made to be less than ± 0.3 DEG C, each temperature point is kept
20-30 minutes, obtain the temperature characteristics of film resistor hydrogen gas sensor and temperature sensor；It is bent to obtain hydrogen response characteristic
The method of line is：The inner cavity temperature of the housing is maintained at certain steady temperature, constant temperature passes through gas flow after 20-30 minutes
Controller is passed through normal concentration hydrogen, and the resistance that film resistor hydrogen gas sensor is measured using resistance instrument is changed, and divides three sections
Concentration range is demarcated respectively, and 40000ppm is risen to from 0ppm when being flushed with hydrogen, and 0-2000ppm super low concentration section measuring points are：100、
200th, 300,600,900,1200ppm, 2000ppm-10000ppm low concentration sections measuring point is stepping 2000ppm, 10000ppm-
40000ppm high concentration sections stepping-in amount is 5000ppm, is flushed with hydrogen to 40000ppm, is gradually reduced from 40000ppm by similary measuring point
To zero-dose, when replacing measuring point every time, first filled 3-5 minutes using the new concentration value gas of big flow, it is gentle that Rapid replacement falls cavity
Original concentration hydrogen gas in pipe, then low discharge reduction gas flowing and influence of the temperature fluctuation to calibration are transferred to, obtain hydrogen response
Characteristic curve, with the characteristic of this analysed film resistance hydrogen gas sensor.
The beneficial effects of the present invention are：
The present invention by will be used to controlling the gas flow controller of density of hydrogen and flow, for providing steady temperature
Constant temperature atmosphere test chamber and temperature controller and whole for measuring the resistance instrument of the output signal of film resistor hydrogen gas sensor
It being combined, is capable of providing arbitrary gas concentration multiple spot standard value, configuration and the control of increase and decrease standard density of hydrogen are easy to operate,
Can arbitrarily adjustment criteria gas concentration value and flow, the wide precision of concentration adjustable range is high, can when demarcating density of hydrogen calibration curve
Greatly to reduce the influence of ambient temperature interference and gas flowing to calibration, so that it is guaranteed that accurately obtaining sensing unit output electricity
Resistance and density of hydrogen standard value correspondence, consequently facilitating every Static State Index of accurate analysed film resistance hydrogen gas sensor；
It, can be easily by multiple signals from constant temperature by the way that chip mounting circuit boards, pinboard, connecting plate to be combined and be electrically connected
It is sent out in atmosphere test chamber, increases cavity volume without using bulky adapter, connection is easy and of low cost
Cheaply.
The temperature calibration curve of film resistor hydrogen gas sensor can also be obtained by the present invention, analyzes its temperature spy
Property, in order to which the method for temperature-compensating is used to realize high-acruracy survey from now on；Film resistor hydrogen can also be directed to by the present invention
The response time of gas sensor, selectivity, resists other characteristics such as other atmosphere cross jammings to be detected at resolution ratio.
It is suitable for other structures type such as optical fiber atmosphere sensor or other sensitive atmosphere sensings are such as
CO atmosphere sensors etc., nonstandard class atmosphere sensor calibration that these are easily affected by temperature, nonlinear object.
Description of the drawings
Fig. 1 is the structure diagram of high-precision film resistor hydrogen gas sensor calibration device of the present invention；
Fig. 2 is that the constant temperature atmosphere test chamber section view of high-precision film resistor hydrogen gas sensor calibration device of the present invention is stood
Body structure chart；
Fig. 3 is the three-dimensional structure diagram of the connecting plate of high-precision film resistor hydrogen gas sensor calibration device of the present invention；
Fig. 4 is the three-dimensional structure diagram of the pinboard of high-precision film resistor hydrogen gas sensor calibration device of the present invention；
Fig. 5 is the solid of the chip mounting circuit boards of high-precision film resistor hydrogen gas sensor calibration device of the present invention
Structure chart.
Specific embodiment
The invention will be further described below in conjunction with the accompanying drawings：
As Figure 1-Figure 5, high-precision film resistor hydrogen gas sensor calibration device of the present invention includes gas flow
Controller (not showing in Fig. 2-Fig. 5), constant temperature atmosphere test chamber, temperature controller (not showing in Fig. 2-Fig. 5) and resistance instrument (Fig. 2-figure
Do not show in 5), the gas flow controller includes three input ports and a delivery outlet, input port described in two of which are used for
Hydrogen and the nitrogen for adjusting density of hydrogen are passed through, another described input port can be passed through other gases or not have to, and increase
Multicomponent calibrating gas matches function, and 2 input ports and the delivery outlet for being passed through hydrogen and other gases connect one respectively
Program-controlled mass flowmenter, the latter are responsible for total flow control, and the input port for being passed through nitrogen directly connects diluent gas nitrogen and do not connect matter
Measure flowmeter；The constant temperature atmosphere test chamber includes housing 9 and the temperature sensor 17 being placed in the inner cavity of housing 9 (in Fig. 2 not
Show), film resistor hydrogen gas sensor 18 (not showing in Fig. 2), electric network 3, chip mounting circuit boards 5, pinboard 4, connecting plate 13
(not showing in Fig. 2) and thermal insulation layer 2, housing 9 are equipped with the air inlet 10 communicated respectively with the inner cavity of housing 9 and gas outlet 1, air inlet
Mouth 10 is located at the lower section of chip mounting circuit boards 5, and gas outlet 1 is located at the top of the connecting plate；Thermal insulation layer 2 is set on housing 9
On interior cavity wall, electric network 3 is set on the outside of thermal insulation layer 2, and electric network 3 keeps a fixed gap with chip mounting circuit boards 5, is convenient for
Gas permeates, and chip mounting circuit boards 5 are installed on the inner cavity middle position of housing 9, and the film resistor hydrogen gas sensor 18 is pacified
Loaded in chip mounting circuit boards 5, it is (or double that the upper surfaces of chip mounting circuit boards 5 is equipped with double socket pedestal 19
Socket contact pin), pinboard 4 is installed on the surface of chip mounting circuit boards 5, and the lower surface of pinboard 4 is equipped with installs with chip
The double socket contact pin 16 (or double socket pedestal) that circuit board 5 is electrically connected, double socket contact pin 16 is inserted into double
In socket pedestal 19, multiple vertical support column vias 15 are respectively equipped in chip mounting circuit boards 5 and pinboard 4, it is multiple perpendicular
To the lower end of support column 11 be fixed in the intracavity bottom cavity wall of housing 9, the upper end of support column 11 sequentially passes through chip peace
Support column via 15 on device, circuit board 5 and pinboard 4, support column 11 are set with insulation sleeve 6 outside；Temperature sensor 17 uses armour
The Pt100 platinum resistance of dress and the lower surface for being installed on pinboard 4, prevent hydrogen embrittlement effects temperature measurement accuracy, and head cover 7 is installed on shell
The upper end of body 9 is simultaneously equipped with connection plate interface 8, and connecting plate 13 is embedded in head cover 7, and the top and bottom of connecting plate 13 are respectively equipped with
Top pads 12 and bottom land 14, top pads 12 are electrically connected with the temperature controller and the resistance instrument, bottom weldering
Disk 14 is electrically connected with the double socket contact pin 16 on pinboard 4 and the output signal line of temperature sensor 17；The gas
The delivery outlet of flow controller is connect with the air inlet 10 of the constant temperature atmosphere test chamber, the air inlet 10 of constant temperature atmosphere test chamber
The position of chip mounting circuit boards 5, intracavitary port diameter 3mm are highly had to be lower than, bore excessive cannot prevent from being passed through gas flowing
Too quickly, height is low to be made to be passed through gas slowly and penetrates into more than 5 chip mounting circuit boards, prevents gas from chip being caused to be pacified when being passed through
Resistance of sensor fluctuation is excessive on device, circuit board 5 interferes, and the gas outlet 1 of the constant temperature atmosphere test chamber is communicated with air,
The signal output end of temperature sensor 17 and the power input of electric network 3 signal input part with the temperature controller respectively
It is connected with computer heating control output terminal, the signal output end of the film resistor hydrogen gas sensor 18 and the signal of the resistance instrument are defeated
Enter end connection.
With reference to Fig. 1-Fig. 5, the Calibration Method of high-precision film resistor hydrogen gas sensor calibration device use of the present invention,
Including obtaining temperature characteristics and obtaining hydrogen response characteristic curve, wherein, the method for the acquisition temperature characteristics is：
The inner cavity of housing 9 is gradually heated to 40 DEG C since room temperature, and temperature point is：Room temperature, 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C, it is described
The placement of high-precision film resistor hydrogen gas sensor calibration device more than half an hour, passes through temperature sensor 17, electric heating at room temperature
Temperature in the inner cavity of net 3 and temperature controller control housing 9, makes temperature error be less than ± 0.3 DEG C, each temperature point
It is kept for 20-30 minutes, obtains the temperature characteristics of film resistor hydrogen gas sensor 18 and temperature sensor 17；Hydrogen is obtained to ring
The characteristic method is answered to be：The inner cavity temperature of housing 9 is maintained at certain steady temperature, such as 25 DEG C, constant temperature 20-30 minutes
Afterwards, normal concentration hydrogen is passed through by the gas flow controller, measuring film resistor hydrogen using the resistance instrument senses
The resistance variation of device 18, point three sections of concentration ranges are demarcated respectively, and 40000ppm, 0- are risen to from 0ppm when being flushed with hydrogen
2000ppm super low concentration section measuring points are：100th, 200,300,600,900,1200ppm, 2000ppm-10000ppm low concentration sections
Measuring point is that stepping 2000ppm, 10000ppm-40000ppm high concentration section stepping-in amount is 5000ppm, is flushed with hydrogen to 40000ppm,
Zero-dose is stepped down to from 40000ppm by similary measuring point, when replacing measuring point every time, first using the new concentration value gas of big flow
It fills 3-5 minutes, Rapid replacement falls cavity and tracheae Central Plains beginning concentration hydrogen, then is transferred to low discharge reduction gas flowing and temperature wave
The dynamic influence to calibration obtains hydrogen response characteristic curve, with the characteristic of this analysed film resistance hydrogen gas sensor 18, thin-film electro
The hydrogen nonlinearity for hindering hydrogen gas sensor 18 is strong, high sensitivity during low concentration, during high concentration sensitivity gradually decline, but past
Return test repeatability it is good, sensing unit lag error is small, resolution ratio 100ppm；It may also be aware of by calibration experiment, when concentration is low
18 response time of film resistor hydrogen gas sensor is long, and response speed increases with density of hydrogen and accelerated.
For a better understanding of the present invention, the making and use of the present invention are described further below：
First, the composing method of constant temperature atmosphere test chamber is：A) by the housing 9 of the constant temperature atmosphere test chamber of included support base
It is horizontal positioned, suitable length is cut out with reference to constant temperature atmosphere test chamber internal diameter and height dimension using the sheathing paper of 2-3mm thickness
Square configuration is curled into cylindrical shape and is put into intracavitary, is close to the inner cavity cavity wall of housing 9, and cannot be overlapped, and forms thermal insulation layer 2；B) it uses
Marker pen is stretched into air inlet 10 and gas outlet 1, in the corresponding position marking of thermal insulation layer 2, then by thermal insulation layer 2 output with
The 1 matched hole of internal diameter size of air inlet 10 and gas outlet, as into outlet passageway；C) heating ribbon power uniform winding is being heated
Electric network 3 is formed on net outer wall, with leaving big gap at 1 corresponding position of air inlet 10 and gas outlet in order into outlet
Body, both ends are fixed and respectively reserve one section of 7-10mm length line after twining, to facilitate on the connection plate interface 8 on connection head cover 7
Cable switching circuit board；D) be placed sequentially in the interior intracavitary of housing 9 after making thermal insulation layer 2 and electric network 3, tapping with into
The position of gas port 10 and gas outlet 1 corresponds to, and the position of air inlet 10 has to be lower than chip mounting circuit boards 5, in this way can be effective
Influence of the airflow fluctuation to chip, can also reduce the calibrated error that different flow difference is brought when eliminating logical deflate；E) by 3 branch
Dagger 11 is rotated on the pedestal of housing 9 in three threaded holes, is fixed on the pedestal of housing 9, puts on 3 insulation sleeves 6, support
Column 11 is the threaded cylindrical aluminium rod of metal alloy of upper and lower ends, and insulation sleeve 6 is the bakelite cylindrical prism in Nei Dai gardens hole；F) it will pass
Film resistor hydrogen gas sensor 18 is inserted in chip mounting circuit boards 5, at most can once install 10 film resistor hydrogen sensings
Chip mounting circuit boards 5 are positioned on insulation sleeve 6 by device 18 after being plugged；G) mounting hole will be corresponded on pinboard 4 and passes through what is stretched out
Then support column 11 docks pinboard 4 with the respective socket in chip mounting circuit boards 5, fixed pinboard 4 using screw
On support column 11, respective sensor line on the pinboard 4, Pt100 standard platinum resistances, that is, temperature sensor on inner wall
17 and 3 line of electric network, it is welded in advance at connection plate interface 8 on mounted cable switching circuit board, convenient for by chamber
The data of the acquisition in need of internal institute of portion and measurement are spread out of；F) it is cut out using 1mm thickness polytetrafluoroethylene film or sheathing paper
2mm × 40mm square holes are opened in circular pattern, inside, and outer diameter is identical with the internal diameter of head cover 7, on the inner wall of head cover 7, for protecting
Temperature is heat-insulated；G) to reach better constant temperature effect, thick froth bed can be pasted on the outer wall of housing 9.So far constant temperature atmosphere chamber
It is completed, combination temperature controller, temperature-controlled precision is maintained within ± 0.1 DEG C~± 0.3 DEG C, could meet good calibration
Required precision.
Chip mounting circuit boards 5, pinboard 4, connecting plate 13 using Pcb circuit board makings after 2mm, are connected with each other method
It is as follows：A) tested film resistor hydrogen gas sensor 18 is plugged in chip mounting circuit boards 5, a film resistor hydrogen passes
At least 2 groups of resistance on sensor 18, one group is to survey hydrogen resistance, and another group is temperature detecting resistance, therefore film resistor hydrogen gas sensor
Visible 4 vias on 18, every 2 vias correspond to one group of resistance, upper four cores contact pin are welded at via；In chip mounting circuit boards 5
The via of corresponding film resistor hydrogen gas sensor 18, which is handled affairs, is first welded insert row pedestal, and film resistor hydrogen gas sensor 18 is plugged i.e.
Can, without bonding wire, reduce sensor cable line volume so that sensor grafting is convenient and can once install more films simultaneously
Resistance hydrogen gas sensor 18 synchronizes calibration, improves calibration efficiency, is convenient at former jointing holes being sensor bonding wire after calibration
Signal is drawn；B) standard Pt100 standard platinum resistances, that is, temperature sensor 17 is welded on to the downside of pinboard 4, for measuring
Temperature value between pinboard 4 and chip mounting circuit boards 5；C) 5 both ends of chip mounting circuit boards are welded with 2 groups of double socket bottoms
Seat 19 corresponds to 2 groups of double socket contact pins 16 being welded on pinboard 4, film resistor hydrogen gas sensor 18 and double socket bottom
19 unicom of seat, only need to be by the double socket of chip mounting circuit boards 5 in this way after film resistor hydrogen gas sensor 18 installs
Corresponding double socket contact pin 16 docks on pedestal 19 and pinboard 4, you can believes the output of film resistor hydrogen gas sensor 18
Number lead to pinboard 4；D) connecting plate 13 is embedded at the connection plate interface 8 of head cover 7, and bottom land 14 is used for line pinboard
Double socket contact pin 16 on 4, top pads 12 are connecting for the temperature controller outside line and high-precision resistance instrument
It also needs to reserve the interface channel of electric network 3 and the interface channel of temperature sensor 17 on plate 13.Due to being difficult to find tens tunnels on the market
The circuit connector of signal, therefore using the design of this three pieces of circuit boards, can will easily pass multiple signals and be surveyed from constant temperature atmosphere
It is sent out in examination chamber, it is easy and cheap.
Gas flow controller uses three component flow controllers, and 3 mass flowmenters integrate, and pass through computer
Accurately gas concentration is matched in control to CPU.Wherein, the flowmeter total flow maximum 2000mL of output terminal, two flowmeters of input terminal are total
Maximum flow 8mL, maximum ratio 1：100, therefore H2、O2Distribution range 0.08mL~8mL.It is required that H2Concentration range 40ppm
During~40000ppm, concentration ratio 1：1000, O2During concentration range 40ppm~20000ppm, concentration ratio 1：500, proportioning is dense
Degree is lower, and total flow needs bigger, and calculation formula is as follows：
Assuming that two kinds of gas distributions, it is assumed that need to configure H2A concentration of x, by N2As diluent gas, H2Flow y and N2Stream
Amount q always meets following formula：
H2Flow：Y=(100x-0.004) × 1.98+0.08 (units：mL)
N2Flow：Z=y/x-y (units：mL)
Total flow：Q is total=y+z (units：mL)
Simpler computational methods assume that total gas flow rate in the range of equipment index, it is assumed that three kinds of gas mixing ratios, it is false
If total flow is set to 500mL (in the range of 2000mL), O2With gas concentration 0.5%, then O2Flow is 0.5% × 500=2.50mL,
H2With gas concentration 1%, then H21% × 500=5mL of flow.
The general pure H for using more than 99.99% purity2Or pure N2Distribution is set low when reduction total gas flow rate is needed to match again
During concentration, the proportioned low concentration standard hydrogen of metrological service may be used and be used as with air source.
After computer calculates and automatically controlled flow, it regard the gas for having matched concentration and flow as mark by connecting air flue
Quasi- concentration gases are exported to the air inlet 10 of constant temperature atmosphere test chamber, the gas outlet 1 of constant temperature atmosphere test chamber by hose with it is big
Gas leads to, for intracavity gas to be discharged into air.
Temperature controller and resistance instrument are then according to prior art choice accuracy matured product as high as possible, herein not
It is described specifically.
Above-described embodiment is presently preferred embodiments of the present invention, is not the limitation to technical solution of the present invention, as long as
Without the technical solution that creative work can be realized on the basis of above-described embodiment, it is regarded as falling into patent of the present invention
Rights protection scope in.
Claims (4)
1. a kind of high-precision film resistor hydrogen gas sensor calibration device, it is characterised in that：Including gas flow controller, constant temperature
Atmosphere test chamber, temperature controller and resistance instrument, the gas flow controller include at least two input ports and an output
Mouthful, each input port and the delivery outlet connect a program-controlled mass flowmenter respectively；The constant temperature atmosphere test chamber
Including housing and the temperature sensor, film resistor hydrogen gas sensor, the electric heater that are placed in the inner cavity of the housing, the shell
Body is equipped with the air inlet communicated respectively with the inner cavity of the housing and gas outlet；The delivery outlet of the gas flow controller with
The air inlet connection of the constant temperature atmosphere test chamber, the gas outlet of the constant temperature atmosphere test chamber are communicated with air, the temperature
The power input of the signal output end of sensor and the electric heater signal input part with the temperature controller respectively
It is connected with computer heating control output terminal, the signal output end of the film resistor hydrogen gas sensor and the signal of the resistance instrument input
End connection.
2. high-precision film resistor hydrogen gas sensor calibration device according to claim 1, it is characterised in that：The constant temperature
Atmosphere test chamber further includes chip mounting circuit boards, pinboard, connecting plate, thermal insulation layer and head cover, and the electric heater is electric heating
Net, the thermal insulation layer are set on the interior cavity wall of the housing, and the electric network is set on the outside of the thermal insulation layer, the chip
Mounting circuit boards are installed on the inner cavity middle position of the housing, and the film resistor hydrogen gas sensor is installed on the chip peace
On device, circuit board, the upper surface of the chip mounting circuit boards is equipped with double socket pedestal or double socket contact pin, the switching
Plate is installed on the surface of the chip mounting circuit boards, and the lower surface of the pinboard is equipped with and the chip mounting circuit boards
The double socket contact pin or double socket pedestal being electrically connected, the temperature sensor is installed on the lower surface of pinboard, described
Head cover is installed on the upper end of the housing and equipped with connection plate interface, and the connecting plate is embedded in the head cover, the connection
Top pads and bottom land are respectively equipped at the top and bottom of plate, the top pads are used for and the temperature controller and institute
State the electric connection of resistance instrument, the bottom land be used for the double socket contact pin on the pinboard or double socket pedestal with
And the output signal line of the temperature sensor is electrically connected；Air inlet on the housing is located at the chip mounting circuit boards
Lower section, the gas outlet on the housing is located at the top of the connecting plate.
3. high-precision film resistor hydrogen gas sensor calibration device according to claim 2, it is characterised in that：The chip
Multiple vertical support column vias are respectively equipped in mounting circuit boards and the pinboard, the lower end of multiple vertical support columns is consolidated
Surely it is set in the intracavity bottom cavity wall of the housing, the upper end of the support column sequentially passes through the chip mounting circuit boards and institute
The support column via on pinboard is stated, insulation sleeve is set with outside the support column.
4. a kind of calibration side that high-precision film resistor hydrogen gas sensor calibration device as described in claim 1,2 or 3 uses
Method, it is characterised in that：Including obtaining temperature characteristics and obtaining hydrogen response characteristic curve, wherein, the acquisition temperature is special
The method of linearity curve is：The inner cavity of the housing is gradually heated to 40 DEG C since room temperature, and temperature point is：Room temperature, 25 DEG C, 30
DEG C, 35 DEG C, 40 DEG C, the high-precision film resistor hydrogen gas sensor calibration device is placed at room temperature more than half an hour, is passed through
The temperature sensor, the electric heater and the temperature controller control the temperature in the inner cavity of the housing, make temperature
Error is less than ± 0.3 DEG C, and each temperature point is kept for 20-30 minutes, obtains film resistor hydrogen gas sensor and temperature sensor
Temperature characteristics；Obtaining the characteristic method of hydrogen response is：It is constant that the inner cavity temperature of the housing is maintained at certain
Temperature, constant temperature are passed through normal concentration hydrogen after 20-30 minutes, by gas flow controller, and thin-film electro is measured using resistance instrument
The resistance variation of hydrogen gas sensor is hindered, point three sections of concentration ranges are demarcated respectively, and 40000ppm is risen to from 0ppm when being flushed with hydrogen,
0-2000ppm super low concentration section measuring points are：100th, 200,300,600,900,1200ppm, 2000ppm-10000ppm low concentrations
It is 5000ppm that section measuring point, which is stepping 2000ppm, 10000ppm-40000ppm high concentration section stepping-in amount, is flushed with hydrogen to 40000ppm
Afterwards, zero-dose is stepped down to from 40000ppm by similary measuring point, when replacing measuring point every time, first using the new concentration value gas of big flow
Body fills 3-5 minutes, and Rapid replacement falls cavity and tracheae Central Plains beginning concentration hydrogen, then is transferred to low discharge reduction gas flowing and temperature
The influence to calibration is fluctuated, hydrogen response characteristic curve is obtained, with the characteristic of this analysed film resistance hydrogen gas sensor.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110988272A (en) * | 2019-12-27 | 2020-04-10 | 中国原子能科学研究院 | Method for correcting measured values of a hydrogen sensor |
| CN111397660A (en) * | 2020-04-03 | 2020-07-10 | 天津大学 | Multifunctional photonic chip detection system |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110988272A (en) * | 2019-12-27 | 2020-04-10 | 中国原子能科学研究院 | Method for correcting measured values of a hydrogen sensor |
| CN111397660A (en) * | 2020-04-03 | 2020-07-10 | 天津大学 | Multifunctional photonic chip detection system |
| CN111397660B (en) * | 2020-04-03 | 2022-03-15 | 天津大学 | Multifunctional photonic chip detection system |
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