CN107831197A - Sensor, the preparation method of sensor, gas detecting system and detection method - Google Patents
Sensor, the preparation method of sensor, gas detecting system and detection method Download PDFInfo
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- CN107831197A CN107831197A CN201711112890.5A CN201711112890A CN107831197A CN 107831197 A CN107831197 A CN 107831197A CN 201711112890 A CN201711112890 A CN 201711112890A CN 107831197 A CN107831197 A CN 107831197A
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- G—PHYSICS
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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Abstract
The invention discloses a kind of sensor, the preparation method of sensor, gas detecting system and detection method, the sensor includes zone of heating, solid electrolyte basic unit and the electrode layer set gradually from top to bottom, zone of heating and solid electrolyte basic unit are cubic shaped, solid electrolyte basic unit is formed using yttrium stable zirconium oxide ceramic chips sintering, and solid electrolyte basic unit is adhered to zone of heating upper surface；Advantage is when detection includes the mixed gas of multiple gases, by changing the bias voltage being carried between first electrode line and the 3rd electrode wires, make to export the response current signal under corresponding bias voltage between second electrode line and the 3rd electrode wires, the detection of gas with various can be achieved, thus sensor of the invention need not set the sensing unit of multiple different sizes, simple in construction, small volume, cost are relatively low, can detect multiple gases.
Description
Technical field
The present invention relates to a kind of sensor, is detected more particularly, to a kind of sensor, the preparation method of the sensor, gas
System and method.
Background technology
With industrial fast development, a large amount of pernicious gases such as hydrocarbons, oxycarbide and nitrogen oxides are to big
Discharged in gas.When human body contacts with these pernicious gases for a long time, the damage and canceration of human organ and nervous system can be triggered.
For this reason, it may be necessary to often to air, these toxic gases are monitored, to reduce its injury to human body.
At present, the monitoring of toxic gas is mainly realized by gas detecting system.Existing gas detecting system
The main PCA analysis modules included for the sensor of detection gas and for analyze data, tested gas is placed in by sensor
In, sensor, which gathers gas information and generates corresponding response, is sent to PCA analysis modules, and PCA analysis modules are to response
Analyzed, draw the species of gas.Because tested gas is generally all mixed gas, gas of the inside containing Multiple components,
In order to identify these toxic gases respectively, existing sensor generally includes multiple sensing units for being used to detect gas with various,
These sensing units discharge along array, and Each performs its own functions, export different response signals, thus cause existing sensor construction to be answered
Miscellaneous, volume is larger, and cost of manufacture is higher, and also more complicated using the method for the sensor detection gas, and cost is also higher.
The content of the invention
It is relatively low that one of technical problems to be solved by the invention are to provide a kind of simple in construction, small volume, cost, can
For detecting the sensor of multiple gases.
Technical scheme is used by the present invention solves one of above-mentioned technical problem：A kind of sensor, including from top to bottom
Zone of heating, solid electrolyte basic unit and the electrode layer set gradually, described zone of heating and described solid electrolyte basic unit are equal
For cubic shaped, described solid electrolyte basic unit is formed using yttrium stable zirconium oxide ceramic chips sintering, described solid electricity
Xie Zhi basic units are adhered to described zone of heating upper surface, and the length of described solid electrolyte basic unit is designated as into l, and width is designated as d,
Thickness is designated as h, wherein, length l span is 15-20mm, and width d span is 5-10mm, the value model of thickness h
Enclose and be equal to the length of described solid electrolyte basic unit for 0.3-1.5mm, the length of described zone of heating, described zone of heating
Width is equal to the width of described solid electrolyte basic unit, and described zone of heating and described solid electrolyte basic unit are perfectly aligned
Fitting；Described electrode layer includes reference electrode, to electrode and sensitive electrode, described reference electrode, it is described to electrode and
Described sensitive electrode is respectively size dimension identical cubic shaped, and the length of described reference electrode is designated as into l1, it is wide
Degree is designated as d1, thickness is designated as h1, wherein, length l1Span beWidth d1Span beThickness
It is designated as h1Span beIt is described reference electrode, described to electrode and described sensitive electrode is along institute
The length direction of the solid electrolyte basic unit stated is disposed on the upper surface of described solid electrolyte basic unit successively, described
The center to electrode it is overlapping with the center of described solid electrolyte basic unit, described reference electrode with it is described to electrode it
Between spacing be equal to the spacing to electrode between described sensitive electrode, and the span of the spacing be 1.mm~
2.5mm；First electrode line is provided with described reference electrode, it is described to being provided with second electrode line on electrode, it is described
The 3rd electrode wires are provided with sensitive electrode；When detection includes the mixed gas of multiple gases, it is carried in by change described
First electrode line and the 3rd described electrode wires between bias voltage, make described second electrode line and the described the 3rd electricity
The response current signal under corresponding bias voltage is exported between polar curve, is achieved in the detection of gas with various.
Compared with prior art, a kind of sensor is the advantages of sensor of the invention, it is characterised in that including passing through
The zone of heating, solid electrolyte basic unit and the electrode layer that set gradually from top to bottom builds sensor construction, zone of heating and solid
Electrolyte basic unit is cubic shaped, and solid electrolyte basic unit is formed using yttrium stable zirconium oxide ceramic chips sintering, solid electricity
Xie Zhi basic units are adhered to zone of heating upper surface, and the length of solid electrolyte basic unit is designated as into l, and width is designated as d, and thickness is designated as h, its
In, length l span is 15-20mm, and width d span is 5-10mm, and the span of thickness h is 0.3-
1.5mm, the length of zone of heating are equal to the length of solid electrolyte basic unit, and the width of zone of heating is equal to the width of solid electrolyte basic unit
Degree, zone of heating with solid electrolyte basic unit is perfectly aligned is bonded；Electrode layer includes reference electrode, to electrode and sensitive electrode, ginseng
It is respectively size dimension identical cubic shaped than electrode, to electrode and sensitive electrode, the length of reference electrode is designated as l1,
Width is designated as d1, thickness is designated as h1, wherein, length l1Span beWidth d1Span beIt is thick
Degree is designated as h1Span beReference electrode, to the length of electrode and sensitive electrode along solid electrolyte basic unit
Degree direction is disposed on the upper surface of solid electrolyte basic unit successively, in the center and solid electrolyte basic unit to electrode
The heart is overlapping, reference electrode and the spacing between electrode is equal to the spacing between electrode and sensitive electrode, and the spacing takes
Value scope is 1.5mm~2.5mm；First electrode line is provided with reference electrode, it is sensitive to being provided with second electrode line on electrode
The 3rd electrode wires are provided with electrode；When detection includes the mixed gas of multiple gases, first electrode is carried in by changing
Bias voltage between line and the 3rd electrode wires, make to export under corresponding bias voltage between second electrode line and the 3rd electrode wires
Response current signal, you can realize the detection of gas with various, thus sensor of the invention need not set multiple different sizes
Sensing unit, simple in construction, small volume, cost are relatively low, can detect multiple gases.
The two of the technical problems to be solved by the invention are to provide a kind of preparation method of sensor, prepared by the preparation method
Obtained sensor construction is simple, small volume, cost are relatively low, can detect multiple gases.
Technical scheme is used by the two of present invention solution above-mentioned technical problem：A kind of sensing described in claim 1
The preparation method of device, comprises the following steps：
(1) according to Sizing requirements, the zone of heating and yttrium stable zirconium oxide ceramic chips of corresponding size are chosen；
(2) yttrium stable zirconium oxide ceramic chips are sintered to form solid electrolyte basic unit；
(3) reference electrode is prepared, specific preparation process is：First manganese oxide electrode slurry is printed using screen printing technique
In the upper surface corresponding position of described solid electrolyte basic unit, it is then placed in drying box, 10 is dried under the conditions of 100 DEG C
Hour, it is subsequently placed into high temperature furnace and is calcined 2 hours under the conditions of 1400 DEG C, described ginseng is formed after finally naturally cooling to room temperature
Than electrode, described manganese oxide electrode slurry is formed by the way that manganese oxide powder is dissolved in polymer chemistry reagent, wherein aoxidizing
The mass ratio of manganese powder body and polymer chemistry reagent is 1：1.5；
(4) prepare and be to electrode, specific preparation process：Pt is first printed on institute to electrode slurry by screen printing technique
The upper surface corresponding position of the solid electrolyte basic unit stated, is then placed in drying box, and it is small that 10 are dried under the conditions of 100 DEG C
When, place into high temperature furnace and calcined 2 hours under the conditions of 1200 DEG C, naturally cool to after room temperature formed it is described to electrode, institute
The Pt stated is formed to electrode slurry by the way that Pt slurries are dissolved in polymer chemistry reagent, and wherein Pt slurries try with polymer chemistry
The mass ratio of agent is 1：1；
(5) sensitive electrode, first electrode line, second electrode line and the 3rd electrode wires are prepared, specific preparation process is：Will be quick
Sense electrode slurry is printed on the upper surface corresponding position of described solid electrolyte basic unit, Ran Hou using screen printing technique
A Pt wire is drawn as the 3rd electrode wires in its surface, and a Pt wire is drawn on described reference electrode surface as first
Electrode wires, and second electrode line is used as by a Pt slurries piece Pt wire of extraction to electrode surface described, it is subsequently placed into
Dried 10 hours under the conditions of 100 DEG C in drying box, place into high temperature furnace and calcined 2 hours at 800-1200 DEG C, natural cooling
To room temperature, now sensitive electrode, first electrode line, second electrode line and the 3rd electrode wires are formed, described sensitive electrode slurry
Formed by the way that the mixture of zinc oxide and indium oxide powder is dissolved into polymer chemistry reagent, described zinc oxide and oxidation
The mixture of indium powder is made up of 5-40wt% zinc oxide and 60-95wt% indium oxide, zinc oxide and indium oxide powder
The mass ratio of mixture and polymer chemistry reagent is 1：1.5.
(6) lower surface of described solid electrolyte basic unit and described zone of heating upper surface are glued using refractory ceramics glue
It is combined, prepared by sensor completes.
Described polymer chemistry reagent is by 20wt%~30wt% ethyl cellulose and 77wt%~80wt% pine
Oleyl alcohol is mixed to form.
Compared with prior art, the zone of heating and yttrium for choosing corresponding size first are the advantages of preparation method of the invention
Stabilizing zirconia ceramic chips, then yttrium stable zirconium oxide ceramic chips are sintered to form solid electrolyte basic unit, then
It is sequentially prepared reference electrode, to electrode, sensitive electrode, first electrode line, second electrode line and the 3rd electrode wires, will finally uses
The lower surface of solid electrolyte basic unit and zone of heating upper surface are bonded together by refractory ceramics glue, and prepared by sensor completes, ginseng
The dense oxide manganese insensitive to all gas is used than electrode, can be by reference electrode and sensitive electrode simultaneously exposed to be measured
In gas, the volume of sensor is reduced, simplifies preparation technology, traditional Pt slurries are used to electrode, can be by effectively
Reference electrode is protected, is the polarization that will not cause reference electrode in applying bias voltage；Sensitive electrode is by zinc oxide and indium oxide
It is compound to be prepared, electrochemical catalysis activity is improved, so as to improve the susceptibility to gas, the sensor need not be set
The sensing unit of multiple different sizes, simple in construction, small volume, cost are relatively low, and the gaseous mixture of multiple gases is included in detection
During body, by changing the bias voltage being carried between first electrode line and the 3rd electrode wires, make second electrode line and the 3rd electricity
The response current signal under corresponding bias voltage is exported between polar curve, you can realize the detection of gas with various.
It is relatively low that the three of the technical problems to be solved by the invention are to provide a kind of simple in construction, small volume, cost, can
Detect the gas detecting system of multiple gases.
Technical scheme is used by the three of present invention solution above-mentioned technical problem：A kind of gas detecting system, including pass
Sensor, mass flowmenter, test cabinet, at the electrochemical workstation and PCA data that regulate and control for gathered data and bias voltage
Manage module；Described sensor includes zone of heating, solid electrolyte basic unit and the electrode layer set gradually from top to bottom, described
Zone of heating and described solid electrolyte basic unit are cubic shaped, and described solid electrolyte basic unit aoxidizes using yttrium is stable
Zirconium ceramic chips sintering forms, and described solid electrolyte basic unit is adhered to described zone of heating upper surface, by described solid electricity
The length of Xie Zhi basic units is designated as l, and width is designated as d, and thickness is designated as h, wherein, length l span is 15-20mm, width d's
Span is 5-10mm, and the span of thickness h is 0.3-1.5mm, and the length of described zone of heating is equal to described solid
The length of electrolyte basic unit, the width of described zone of heating are equal to the width of described solid electrolyte basic unit, described heating
Layer with described solid electrolyte basic unit is perfectly aligned is bonded；Described electrode layer includes reference electrode, to electrode and sensitive electrical
Pole, it is described reference electrode, described to electrode and described sensitive electrode is respectively size dimension identical cubic shaped,
The length of described reference electrode is designated as l1, width is designated as d1, thickness is designated as h1, wherein, length l1Span beWidth d1Span beThickness is designated as h1Span beDescribed reference electricity
Pole, described electrode is disposed on successively with length direction of the described sensitive electrode along described solid electrolyte basic unit
On the upper surface of described solid electrolyte basic unit, the center to electrode and the center of described solid electrolyte basic unit
It is overlapping, described reference electrode and the spacing between electrode be equal to it is described to electrode and described sensitive electrode it
Between spacing, and the span of the spacing is 1.5mm~2.5mm；First electrode line, institute are provided with described reference electrode
State to being provided with second electrode line on electrode, the 3rd electrode wires are provided with described sensitive electrode；In detection comprising a variety of
During the mixed gas of gas, by changing the biased electrical being carried between described first electrode line and the 3rd described electrode wires
Pressure, makes to export the response current signal under corresponding bias voltage between described second electrode line and the 3rd described electrode wires；
Described test cabinet has air inlet and gas outlet, and described mass flowmenter is arranged at the air inlet of described test cabinet,
For controlling the flow velocity of the gas flowed into described test cabinet；Described electrochemical workstation and described first electrode line,
Described second electrode line connects with the 3rd described electrode wires, for controlled loading in described first electrode line and described
Bias voltage between 3rd electrode wires, while gather caused by between described second electrode line and the 3rd described electrode wires
Response current signal；It is previously stored with described PCA data processing module by testing each reference gas got in phase
Answer under bias voltage, the term of reference of the response current signal of described sensor output, described PCA data processing module pair
The response current signal for receiving described sensor output is identified, and obtains each gas componant in mixed gas to be measured.
Compared with prior art, it is the advantages of gas detecting system of the invention by sensor, mass flowmenter, survey
Examination room, the electrochemical workstation regulated and controled for gathered data and bias voltage and PCA data processing module are examined to build gas
Survey, sensor includes zone of heating, solid electrolyte basic unit and electrode layer, zone of heating and the solid electrolytic set gradually from top to bottom
Matter basic unit is cubic shaped, and solid electrolyte basic unit is formed using yttrium stable zirconium oxide ceramic chips sintering, solid electrolyte
Basic unit is adhered to zone of heating upper surface, and the length of solid electrolyte basic unit is designated as into l, and width is designated as d, and thickness is designated as h, wherein,
Length l span is 15-20mm, and width d span is 5-10mm, and the span of thickness h is 0.3-1.5mm,
The length of zone of heating is equal to the length of solid electrolyte basic unit, and the width of zone of heating is equal to the width of solid electrolyte basic unit, added
Thermosphere with solid electrolyte basic unit is perfectly aligned is bonded；Electrode layer includes reference electrode, to electrode and sensitive electrode, reference electricity
Pole, it is respectively size dimension identical cubic shaped to electrode and sensitive electrode, the length of reference electrode is designated as l1, width
It is designated as d1, thickness is designated as h1, wherein, length l1Span beWidth d1Span beThickness is remembered
For h1Span beReference electrode, to the length side of electrode and sensitive electrode along solid electrolyte basic unit
To being disposed on successively on the upper surface of solid electrolyte basic unit, center and the center weight of solid electrolyte basic unit to electrode
It is folded, reference electrode and the spacing between electrode is equal to the spacing between electrode and sensitive electrode, and the value model of the spacing
Enclose for 1.5mm~2.5mm；First electrode line is provided with reference electrode, to being provided with second electrode line, sensitive electrode on electrode
On be provided with the 3rd electrode wires；Detection comprising multiple gases mixed gas when, by change be carried in first electrode line and
Bias voltage between 3rd electrode wires, make to export the response under corresponding bias voltage between second electrode line and the 3rd electrode wires
Current signal；Test cabinet has air inlet and gas outlet, and mass flowmenter is arranged at the air inlet of test cabinet, for controlling stream
Enter the flow velocity of the gas in test cabinet；Electrochemical workstation is connected with first electrode line, second electrode line and the 3rd electrode wires, is used
In bias voltage of the controlled loading between first electrode line and the 3rd electrode wires, while gather second electrode line and the 3rd electrode
Caused response current signal between line；It is previously stored with PCA data processing module by testing each reference gas got
Body is under corresponding bias voltage, and the term of reference of the response current signal of sensor output, PCA data processing module is to receiving
The response current signal of sensor output is identified, and obtains each gas componant in mixed gas to be measured, simple in construction, volume
Smaller, cost of manufacture is relatively low.
The four of the technical problems to be solved by the invention are to provide a kind of gas detection method, and the gas detection method uses
Simple in construction, small volume and the realization of lower-cost gas detecting system, can detect multiple gases.
Technical scheme is used by the four of present invention solution above-mentioned technical problem：A kind of detection side of gas detecting system
Method, comprise the following steps：
S1：The zone of heating of described sensor is connected with external power source, the first electrode line of described sensor,
Two electrode wires and the 3rd electrode wires are connected with described electrochemical workstation respectively, and described sensor is placed in described survey
Examination is indoor；Test cabinet has air inlet and gas outlet, and described mass flowmenter is arranged on to the air inlet of described test cabinet
Place；
S2：Open external power source to heat described heating plate, described heating plate is heated to 420~470 DEG C
After keep constant；
S3：Set by described electrochemical workstation and be carried in described first electrode line and the 3rd described electrode wires
Between initial bias, initial bias be -150mV~+150mV in any voltage value；
S4：The flow velocity of described mass flowmenter is set as 5~200sccm, basic gas is passed through into described quality stream
Gauge is filled with described test cabinet, and the gas outlet of described test cabinet is opened, and keeps having gas flowing always in test cabinet,
And calculate basic gas is filled with the time, when the time is 5 minutes, stopping is filled with basic gas, and at the same time starting will be to be measured
Gas is filled with by described mass flowmenter in described test cabinet, and calculate under test gas is filled with the time, is 5 when the time
During minute, stopping is filled with test gas, at the same time starts again at basic gas being filled with institute by described mass flowmenter
In the test cabinet stated, so repeatedly 3 times, after terminating, acquired from electrochemical workstation under initial bias, it is described
The response current signal of the 1st output of sensor；
S5：By described electrochemical workstation to be carried in described first electrode line and the 3rd described electrode wires it
Between bias voltage carry out the t time adjustment, t=1,2 ... T, T be more than or equal to 4 and be less than or equal to 10 integer, obtain the t times
Under bias voltage conditions after adjustment, the response current signal of the 1st output of described sensor, wherein, every time after adjustment
Bias voltage is also respectively a certain magnitude of voltage in -150mV~+150mV, and the biasing after initial bias, the 1st adjustment
In bias voltage after t adjustment of voltage~the, the absolute value of the difference of any two bias voltage is between 15-20mV；
S6：Under identical testing conditions, 3~step 5 of repeat step twice, under the conditions of getting initial bias,
The response current signal of the 2nd output of described sensor and the response current signal of the 3rd output, and after the t times adjustment
Bias voltage conditions under, the response current letter of the response current signal of the output of described sensor the 2nd time and the 3rd output
Number；
S7：Under the conditions of calculating initial bias, the response current signal of the output of described sensor the 1st time, the 2nd time it is defeated
The average value of the response current signal gone out and the response current signal of the 3rd output, using the average value as initial bias
Under the conditions of, response current signal caused by described sensor；It is inclined after the t times adjustment under the conditions of calculating initial bias
Put under voltage conditions, the response current signal of the 1st output of described sensor, the response current signal and the 3rd of the 2nd output
The average value of the response current signal of secondary output, using the average value as the t times adjustment after bias voltage conditions under, it is described
Response current signal caused by sensor；
S8：After response current signal caused by sensor described under the conditions of initial bias and the t times adjustment
Bias voltage conditions under response current signal caused by described sensor be input in described PCA data processing module,
Described PCA data processing module by its to each reference gas prestored under corresponding bias voltage, described sensor
The term of reference of the response current signal of output is compared, and obtains each gas componant under test gas.
Compared with prior art, it is that by setting the flow velocity of mass flowmenter be 5 the advantages of detection method of the invention
~200sccm, and the bias voltage being carried between first electrode line and the 3rd electrode wires is carried out by electrochemical workstation
Set and adjustment, obtain under different bias voltage conditions, the response current signal of the output of sensor, then by will be variant
Under bias voltage conditions, for the response current signal output of sensor into PCA data processing module, PCA data processing module will
To each reference gas prestored under corresponding bias voltage, the term of reference of the response current signal of sensor output enters for it
Row compares, and obtains each gas componant under test gas, detection process is simple, and cost is relatively low.
Brief description of the drawings
Fig. 1 is the structure chart of sensor of the invention；
Fig. 2 is for detection method of the invention to three kinds of 100ppm carbon monoxide, propylene and nitrogen dioxide calibrating gas not
With being detected under bias voltage, each gas responds output current and the relation of time (I-t) curve；
Fig. 3 is for detection method of the invention to three kinds of carbon monoxide, propylene and nitrogen dioxide calibrating gas in various concentrations
With the synthesis recognition effect figure for detecting to obtain under different bias voltages.
Embodiment
The present invention is described in further detail below in conjunction with accompanying drawing embodiment.
The invention provides a kind of sensor, sensor of the invention is made below in conjunction with accompanying drawing embodiment further detailed
Description.
Embodiment：As shown in figure 1, a kind of sensor, including zone of heating 1, the solid electrolyte set gradually from top to bottom
Basic unit 2 and electrode layer, zone of heating 1 and solid electrolyte basic unit 2 are cubic shaped, and solid electrolyte basic unit 2 is steady using yttrium
Determine zirconium oxide ceramic chips sintering to form, solid electrolyte basic unit 2 is adhered to the upper surface of zone of heating 1, by solid electrolyte basic unit 2
Length is designated as l, and width is designated as d, and thickness is designated as h, wherein, length l span is 15-20mm, and width d span is
5-10mm, the span of thickness h is 0.3-1.5mm, and the length of zone of heating 1 is equal to the length of solid electrolyte basic unit 2, heating
The width of layer 1 is equal to the width of solid electrolyte basic unit 2, zone of heating 1 with solid electrolyte basic unit 2 is perfectly aligned is bonded；Electrode
Layer includes reference electrode 3, to electrode 4 and sensitive electrode 5, reference electrode 3, is respectively size dimension to electrode 4 and sensitive electrode 5
Identical cubic shaped, the length of reference electrode 3 is designated as l1, width is designated as d1, thickness is designated as h1, wherein, length l1Take
Value scope isWidth d1Span beThickness is designated as h1Span beReference electricity
Pole 3, solid electrolyte basic unit is disposed on successively to the length direction of electrode 4 and sensitive electrode 5 along solid electrolyte basic unit 2
It is overlapping with the center of solid electrolyte basic unit 2 to the center of electrode 4 on 2 upper surface, reference electrode 3 and between electrode 4
Spacing is equal to the spacing between electrode 4 and sensitive electrode 5, and the span of the spacing is 1.5mm~2.5mm；Reference electricity
First electrode line is provided with pole 3, to being provided with second electrode line on electrode 4, the 3rd electrode wires are provided with sensitive electrode 5；
When detection includes the mixed gas of multiple gases, by changing the biasing being carried between first electrode line and the 3rd electrode wires
Voltage, make to export the response current signal under corresponding bias voltage between second electrode line and the 3rd electrode wires, be achieved in not
With the detection of gas.
Present invention also offers the preparation method of the sensor, below in conjunction with accompanying drawing embodiment to sensor of the invention
Preparation method be described in further detail.
Embodiment：As shown in figure 1, a kind of preparation method of sensor, comprises the following steps：
(1) according to Sizing requirements, the zone of heating 1 and yttrium stable zirconium oxide ceramic chips of corresponding size are chosen；
(2) yttrium stable zirconium oxide ceramic chips are sintered to form solid electrolyte basic unit 2；
(3) reference electrode 3 is prepared, specific preparation process is：First manganese oxide electrode slurry is printed using screen printing technique
The upper surface corresponding position of solid electrolyte basic unit 2 is formed on, is then placed in drying box, it is small that 10 are dried under the conditions of 100 DEG C
When, it is subsequently placed into high temperature furnace and is calcined 2 hours under the conditions of 1400 DEG C, reference electrode 3 is formed after finally naturally cooling to room temperature,
Manganese oxide electrode slurry is formed by the way that manganese oxide powder is dissolved in polymer chemistry reagent, wherein manganese oxide powder and macromolecule
The mass ratio of chemical reagent is 1：1.5；
(4) prepare and be to electrode 4, specific preparation process：First Pt is printed on to the slurry of electrode 4 by screen printing technique
The upper surface corresponding position of solid electrolyte basic unit 2, is then placed in drying box, is dried 10 hours under the conditions of 100 DEG C, then
It is put into high temperature furnace and is calcined 2 hours under the conditions of 1200 DEG C, naturally cools to shape paired electrode 4 after room temperature, Pt is to the slurry of electrode 4
Formed by the way that Pt slurries are dissolved in polymer chemistry reagent, the mass ratio of wherein Pt slurries and polymer chemistry reagent is 2：1；
(5) sensitive electrode 5, first electrode line, second electrode line and the 3rd electrode wires are prepared, specific preparation process is：Will
The slurry of sensitive electrode 5 is printed on the upper surface corresponding position of solid electrolyte basic unit 2 using screen printing technique, then at it
A Pt wire is drawn as the 3rd electrode wires in surface, and a Pt wire is drawn on the surface of reference electrode 3 as first electrode line,
And it is used as second electrode line drawing a Pt wire by Pt slurries to the surface of electrode 4, it is subsequently placed into drying box 100
Dried 10 hours under the conditions of DEG C, place into high temperature furnace and calcined 2 hours at 800-1200 DEG C, naturally cool to room temperature, it is now quick
Sense electrode 5, first electrode line, second electrode line and the 3rd electrode wires are formed, and the slurry of sensitive electrode 5 is by by zinc oxide and oxidation
The mixture of indium powder is dissolved into polymer chemistry reagent and formed, and the mixture of zinc oxide and indium oxide powder is by 5-40wt%
Zinc oxide and 60-95wt% indium oxide composition, mixture and the polymer chemistry reagent of zinc oxide and indium oxide powder
Mass ratio is 1：1.5.
(6) lower surface of solid electrolyte basic unit 2 and the upper surface of zone of heating 1 are bonded together using refractory ceramics glue,
Prepared by sensor completes.
In the present embodiment, polymer chemistry reagent by 20wt%~30wt% ethyl cellulose and 77wt%~80wt%
Terpinol be mixed to form.
Present invention also offers a kind of gas detecting system using the sensor, below in conjunction with accompanying drawing embodiment to this
The gas detecting system of invention is described in further detail.
Embodiment：As shown in figure 1, a kind of gas detecting system, including sensor, mass flowmenter, test cabinet, for adopting
Collect the electrochemical workstation and PCA data processing module of data and bias voltage regulation and control；Sensor is included from top to bottom successively
Zone of heating 1, solid electrolyte basic unit 2 and the electrode layer of setting, zone of heating 1 and solid electrolyte basic unit 2 are cubic shaped,
Solid electrolyte basic unit 2 is formed using yttrium stable zirconium oxide ceramic chips sintering, and solid electrolyte basic unit 2 is adhered on zone of heating 1
Surface, the length of solid electrolyte basic unit 2 being designated as l, width is designated as d, and thickness is designated as h, wherein, length l span is
15-20mm, width d span are 5-10mm, and the span of thickness h is 0.3-1.5mm, and the length of zone of heating 1 is equal to
The length of solid electrolyte basic unit 2, the width of zone of heating 1 are equal to the width of solid electrolyte basic unit 2, zone of heating 1 and solid electricity
The 2 perfectly aligned fitting of Xie Zhi basic units；Electrode layer includes reference electrode 3, to electrode 4 and sensitive electrode 5, reference electrode 3, to electrode
4 and sensitive electrode 5 be respectively size dimension identical cubic shaped, the length of reference electrode 3 is designated as l1, width is designated as d1,
Thickness is designated as h1, wherein, length l1Span beWidth d1Span beThickness is designated as h1Take
Value scope isReference electrode 3, to length direction along solid electrolyte basic unit 2 of electrode 4 and sensitive electrode 5 according to
Minor tick is arranged on the upper surface of solid electrolyte basic unit 2, center and the center weight of solid electrolyte basic unit 2 to electrode 4
It is folded, reference electrode 3 and the spacing between electrode 4 is equal to the spacing between electrode 4 and sensitive electrode 5, and the spacing takes
Value scope is 1.5mm~2.5mm；First electrode line is provided with reference electrode 3, it is quick to being provided with second electrode line on electrode 4
The 3rd electrode wires are provided with sense electrode 5；When detection includes the mixed gas of multiple gases, the first electricity is carried in by changing
Bias voltage between polar curve and the 3rd electrode wires, make to export under corresponding bias voltage between second electrode line and the 3rd electrode wires
Response current signal；Test cabinet has air inlet and gas outlet, and mass flowmenter is arranged at the air inlet of test cabinet, is used for
The flow velocity for the gas that control is flowed into test cabinet；Electrochemical workstation and first electrode line, second electrode line and the 3rd electrode wires
Connection, for bias voltage of the controlled loading between first electrode line and the 3rd electrode wires, while gather second electrode line and
Caused response current signal between 3rd electrode wires；It is previously stored with what is got by experiment in PCA data processing module
Each reference gas is under corresponding bias voltage, the term of reference of the response current signal of sensor output, PCA data processing module
The response current signal for receiving sensor output is identified, obtains each gas componant in mixed gas to be measured.
In the present embodiment, the electrochemistry work for the model LK1100 that electrochemical workstation is produced using Tianjin Lan Like companies
Stand, PCA data processing module uses existing ripe product.
Present invention also offers a kind of detection method of above-mentioned gas detecting system, below in conjunction with accompanying drawing embodiment to this hair
Bright gas detection method is described in further detail.
Embodiment：A kind of detection method of gas detecting system, comprises the following steps：
S1：The zone of heating 1 of sensor is connected with external power source, the first electrode line of sensor, second electrode line and
3rd electrode wires are connected with electrochemical workstation respectively, and sensor is placed in test cabinet；Test cabinet has air inlet and gone out
Gas port, mass flowmenter is arranged at the air inlet of test cabinet；
S2：Open external power source to heat heating plate, heating plate is heated to keep constant after 420~470 DEG C；
S3：The initial bias being carried between first electrode line and the 3rd electrode wires electricity is set by electrochemical workstation
Pressure, initial bias are any voltage value in -150mV~+150mV；
S4：The flow velocity of mass flowmenter is set as 5~200sccm, basic gas is filled with test by mass flowmenter
Interior, the gas outlet of test cabinet is opened, keep having gas flowing always in test cabinet, and calculate when being filled with of basic gas
Between, when the time is 5 minutes, stopping is filled with basic gas, at the same time starts under test gas being filled with by mass flowmenter
In test cabinet, and calculate under test gas is filled with the time, and when the time is 5 minutes, stopping is filled with test gas, at the same time again
It is secondary to start basic gas being filled with test cabinet by mass flowmenter, so repeatedly 3 times, after terminating, from electrochemical workstation
In acquire under initial bias, the response current signal of the output of sensor the 1st time；
S5：The is carried out to the bias voltage that is carried between first electrode line and the 3rd electrode wires by electrochemical workstation
T adjustment, t=1,2 ... T, T are the integer more than or equal to 4 and less than or equal to 10, obtain the biased electrical press strip after the t times adjustment
Under part, the response current signal of the output of sensor the 1st time, wherein, every time the bias voltage after adjustment be also respectively -150mV~+
A certain magnitude of voltage in 150mV, and the biased electrical after the t adjustment of bias voltage~the after initial bias, the 1st adjustment
In pressure, the absolute value of the difference of any two bias voltage is between 15-20mV；
S6：Under identical testing conditions, 3~step 5 of repeat step twice, under the conditions of getting initial bias,
The response current signal of the 2nd output of sensor and the response current signal of the 3rd output, and the biasing after the t times adjustment
Under voltage conditions, the response current signal of the 2nd output of sensor and the response current signal of the 3rd output；
S7：Under the conditions of calculating initial bias, the response current signal of the 1st output of sensor, the sound of the 2nd output
Induced current signal and the 3rd time output response current signal average value, using the average value as initial bias under the conditions of,
Response current signal caused by sensor；Under the conditions of calculating initial bias, under the bias voltage conditions after the t times adjustment,
The response current letter of the response current signal of the 1st output of sensor, the response current signal of the 2nd output and the 3rd output
Number average value, using the average value as the t times adjustment after bias voltage conditions under, caused by sensor response current believe
Number；
S8：By response current signal caused by initial bias condition lower sensor and the biasing after the t times adjustment
Response current signal is input in PCA data processing module caused by voltage conditions lower sensor, PCA data processing module by its
To each reference gas prestored under corresponding bias voltage, the term of reference of the response current signal of sensor output is carried out
Compare, obtain each gas componant under test gas.
In the present embodiment, basic gas is air.
Using the detection method of the present invention to three kinds of 100ppm carbonoxides, propylene and nitrogen dioxide calibrating gas Bu Tong inclined
Put and detected under voltage, three kinds of gas response current signals and the relation of time (I-t) curve are as shown in Figure 2；Using this hair
Bright gas detection method is to three kinds of carbonoxide, propylene and nitrogen dioxide calibrating gas under various concentrations and different bias voltages
Detected, it is as shown in Figure 3 that it integrates recognition effect figure.Analysis chart 2 understands that the gas detection method in the present invention is to 15-
The object gas of 65ppm concentration, under different bias voltages, respondent behavior shows notable difference, different target gas
Body also shows different response characteristics under identical bias voltage.By Fig. 3 intuitively to find out, the present invention has to mixing
Gas carries out effective detection and the ability of identification.
Claims (5)
1. a kind of sensor, it is characterised in that including zone of heating, solid electrolyte basic unit and the electrode set gradually from top to bottom
Layer, described zone of heating and described solid electrolyte basic unit are cubic shaped, and described solid electrolyte basic unit uses
Yttrium stable zirconium oxide ceramic chips sintering forms, and described solid electrolyte basic unit is adhered to described zone of heating upper surface, by institute
The length of the solid electrolyte basic unit stated is designated as l, and width is designated as d, and thickness is designated as h, wherein, length l span is 15-
20mm, width d span are 5-10mm, and the span of thickness h is 0.3-1.5mm, the length of described zone of heating etc.
In the length of described solid electrolyte basic unit, the width of described zone of heating is equal to the width of described solid electrolyte basic unit
Degree, described zone of heating with described solid electrolyte basic unit is perfectly aligned is bonded；
Described electrode layer includes reference electrode, to electrode and sensitive electrode, described reference electrode, described to electrode and institute
The sensitive electrode stated is respectively size dimension identical cubic shaped, and the length of described reference electrode is designated as into l1, width
It is designated as d1, thickness is designated as h1, wherein, length l1Span beWidth d1Span beThickness is remembered
For h1Span beIt is described reference electrode, described to electrode and described sensitive electrode is described in
The length direction of solid electrolyte basic unit be disposed on successively on the upper surface of described solid electrolyte basic unit, it is described
It is overlapping with the center of described solid electrolyte basic unit to the center of electrode, described reference electrode and described between electrode
Spacing be equal to the spacing to electrode between described sensitive electrode, and the span of the spacing be 1.5mm~
2.5mm；First electrode line is provided with described reference electrode, it is described to being provided with second electrode line on electrode, it is described
The 3rd electrode wires are provided with sensitive electrode；
When detection includes the mixed gas of multiple gases, described first electrode line and the described the 3rd is carried in by changing
Bias voltage between electrode wires, make to export corresponding bias voltage between described second electrode line and the 3rd described electrode wires
Under response current signal, be achieved in the detection of gas with various.
2. the preparation method of the sensor described in a kind of claim 1, it is characterised in that comprise the following steps：
(1) according to Sizing requirements, the zone of heating and yttrium stable zirconium oxide ceramic chips of corresponding size are chosen；
(2) yttrium stable zirconium oxide ceramic chips are sintered to form solid electrolyte basic unit；
(3) reference electrode is prepared, specific preparation process is：Manganese oxide electrode slurry is first printed on institute using screen printing technique
The upper surface corresponding position of the solid electrolyte basic unit stated, is then placed in drying box, and it is small that 10 are dried under the conditions of 100 DEG C
When, it is subsequently placed into high temperature furnace and is calcined 2 hours under the conditions of 1400 DEG C, described reference is formed after finally naturally cooling to room temperature
Electrode, described manganese oxide electrode slurry are formed by the way that manganese oxide powder is dissolved in polymer chemistry reagent, wherein manganese oxide
The mass ratio of powder and polymer chemistry reagent is 1：1.5；
(4) prepare and be to electrode, specific preparation process：First Pt is printed on to electrode slurry by screen printing technique described
The upper surface corresponding position of solid electrolyte basic unit, is then placed in drying box, is dried 10 hours under the conditions of 100 DEG C, then
Be put into high temperature furnace and calcined 2 hours under the conditions of 1200 DEG C, naturally cool to after room temperature formed it is described to electrode, described Pt
Electrode slurry is formed by the way that Pt slurries are dissolved in polymer chemistry reagent, wherein the matter of Pt slurries and polymer chemistry reagent
Amount is than being 2：1；
(5) sensitive electrode, first electrode line, second electrode line and the 3rd electrode wires are prepared, specific preparation process is：By sensitive electrical
Pole slurry is printed on the upper surface corresponding position of described solid electrolyte basic unit using screen printing technique, then in its table
A Pt wire is drawn as the 3rd electrode wires in face, and a Pt wire is drawn on described reference electrode surface as first electrode
Line, and second electrode line is used as by a Pt slurries piece Pt wire of extraction to electrode surface described, it is subsequently placed into drying
Dried 10 hours under the conditions of 100 DEG C in case, place into high temperature furnace and calcined 2 hours at 800-1200 DEG C, naturally cool to room
Temperature, now sensitive electrode, first electrode line, second electrode line and the 3rd electrode wires formed, described sensitive electrode slurry passes through
The mixture of zinc oxide and indium oxide powder is dissolved into polymer chemistry reagent and formed, described zinc oxide and indium oxide powder
The mixture of body is made up of 5-40wt% zinc oxide and 60-95wt% indium oxide, the mixing of zinc oxide and indium oxide powder
The mass ratio of thing and polymer chemistry reagent is 1：1.5.
(6) lower surface of described solid electrolyte basic unit and described zone of heating upper surface are bonded in using refractory ceramics glue
Together, prepared by sensor completes.
A kind of 3. preparation method of sensor according to claim 2, it is characterised in that described polymer chemistry reagent
It is mixed to form by 20wt%~30wt% ethyl cellulose and 77wt%~80wt% terpinol.
A kind of 4. gas detecting system, it is characterised in that including sensor, mass flowmenter, test cabinet, for gathered data and
The electrochemical workstation and PCA data processing module of bias voltage regulation and control；
Described sensor includes zone of heating, solid electrolyte basic unit and the electrode layer set gradually from top to bottom, and described adds
Thermosphere and described solid electrolyte basic unit are cubic shaped, and described solid electrolyte basic unit uses yttrium stable zirconium oxide
Ceramic chips sintering forms, and described solid electrolyte basic unit is adhered to described zone of heating upper surface, by described solid electrolytic
The length of matter basic unit is designated as l, and width is designated as d, and thickness is designated as h, wherein, length l span is 15-20mm, and width d's takes
Value scope is 5-10mm, and the span of thickness h is 0.3-1.5mm, and the length of described zone of heating is equal to described solid electricity
The length of Xie Zhi basic units, the width of described zone of heating are equal to the width of described solid electrolyte basic unit, described zone of heating
With described solid electrolyte basic unit is perfectly aligned is bonded；Described electrode layer includes reference electrode, to electrode and sensitive electrode,
It is described reference electrode, described to electrode and described sensitive electrode is respectively size dimension identical cubic shaped, will
The length of described reference electrode is designated as l1, width is designated as d1, thickness is designated as h1, wherein, length l1Span be
Width d1Span beThickness is designated as h1Span beIt is described reference electrode, described
The length direction of electrode and described sensitive electrode along described solid electrolyte basic unit is disposed on successively it is described
On the upper surface of solid electrolyte basic unit, the center to electrode is overlapping with the center of described solid electrolyte basic unit,
Described reference electrode and the spacing between electrode be equal to it is described to electrode between described sensitive electrode
Spacing, and the span of the spacing is 1.5mm~2.5mm；First electrode line is provided with described reference electrode, it is described
To being provided with second electrode line on electrode, the 3rd electrode wires are provided with described sensitive electrode；Multiple gases are included in detection
Mixed gas when, by changing the bias voltage being carried between described first electrode line and the 3rd described electrode wires,
Make to export the response current signal under corresponding bias voltage between described second electrode line and the 3rd described electrode wires；
Described test cabinet has air inlet and gas outlet, and described mass flowmenter is arranged on the air inlet of described test cabinet
Place, for controlling the flow velocity of the gas flowed into described test cabinet；
Described electrochemical workstation connects with described first electrode line, described second electrode line and the 3rd described electrode wires
Connect, for bias voltage of the controlled loading between described first electrode line and the 3rd described electrode wires, while gather institute
Caused response current signal between the second electrode line stated and the 3rd described electrode wires；
It is previously stored with described PCA data processing module by testing each reference gas got in corresponding bias voltage
Under, the term of reference of the response current signal of described sensor output, described PCA data processing module is described to receiving
Sensor output response current signal be identified, obtain each gas componant in mixed gas to be measured.
5. the detection method of a kind of gas detecting system using described in claim 4, it is characterised in that comprise the following steps：
S1：The zone of heating of described sensor is connected with external power source, the first electrode line of described sensor, the second electricity
Polar curve and the 3rd electrode wires are connected with described electrochemical workstation respectively, and described sensor is placed in described test cabinet
It is interior；Test cabinet has air inlet and gas outlet, described mass flowmenter is arranged at the air inlet of described test cabinet；
S2：Open external power source to heat described heating plate, protected after described heating plate is heated into 420~470 DEG C
Hold constant；
S3：Set and be carried between described first electrode line and the 3rd described electrode wires by described electrochemical workstation
Initial bias, initial bias be -150mV~+150mV in any voltage value；
S4：The flow velocity of described mass flowmenter is set as 5~200sccm, basic gas is passed through into described mass flowmenter
It is filled with described test cabinet, the gas outlet of described test cabinet is opened, keeps having gas flowing always in test cabinet, and count
That calculates basic gas is filled with the time, and when the time is 5 minutes, stopping is filled with basic gas, at the same time starts under test gas
It is filled with by described mass flowmenter in described test cabinet, and calculate under test gas is filled with the time, is 5 minutes when the time
When, stopping is filled with test gas, at the same time start again at basic gas be filled with by described mass flowmenter it is described
In test cabinet, so repeatedly 3 times, after terminating, acquired from electrochemical workstation under initial bias, described sensing
The response current signal of the 1st output of device；
S5：By described electrochemical workstation to being carried between described first electrode line and the 3rd described electrode wires
Bias voltage carries out the t times adjustment, and t=1,2 ... T, T are the integer more than or equal to 4 and less than or equal to 10, obtains the t times adjustment
Under bias voltage conditions afterwards, the response current signal of the 1st output of described sensor, wherein, the biasing after adjustment every time
Voltage is also respectively a certain magnitude of voltage in -150mV~+150mV, and the bias voltage after initial bias, the 1st adjustment
In bias voltage after~the t times adjustment, the absolute value of the difference of any two bias voltage is between 15-20mV；
S6：Under identical testing conditions, 3~step 5 of repeat step is twice, described under the conditions of getting initial bias
The response current signal of the output of sensor the 2nd time and the response current signal of the 3rd output, it is and inclined after adjusting for the t time
Put under voltage conditions, the response current signal of the 2nd output of described sensor and the response current signal of the 3rd output；
S7：Under the conditions of calculating initial bias, the response current signal of the output of described sensor the 1st time, the 2nd output
The average value of response current signal and the response current signal of the 3rd output, using the average value as initial bias condition
Under, response current signal caused by described sensor；Under the conditions of calculating initial bias, the biased electrical after the t times adjustment
Under the conditions of pressure, the response current signal of the 1st output of described sensor, the response current signal of the 2nd output and the 3rd time are defeated
The average value of the response current signal gone out, using the average value as the t times adjustment after bias voltage conditions under, described sensing
Response current signal caused by device；
S8：Will be inclined after response current signal caused by sensor described under the conditions of initial bias and the t times adjustment
Response current signal caused by putting sensor described under voltage conditions is input in described PCA data processing module, described
PCA data processing module by its to each reference gas prestored under corresponding bias voltage, described sensor output
The term of reference of response current signal be compared, obtain each gas componant under test gas.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109001283A (en) * | 2018-09-27 | 2018-12-14 | 上海应用技术大学 | A kind of self-constant temperature electrochemistry sheet-type gas sensor and preparation method thereof |
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