CN110455889A - Based on YSZ and NiTiO3Sensitive electrode blendes together electric potential type acetaldehyde sensor and preparation method thereof - Google Patents
Based on YSZ and NiTiO3Sensitive electrode blendes together electric potential type acetaldehyde sensor and preparation method thereof Download PDFInfo
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- CN110455889A CN110455889A CN201910747230.7A CN201910747230A CN110455889A CN 110455889 A CN110455889 A CN 110455889A CN 201910747230 A CN201910747230 A CN 201910747230A CN 110455889 A CN110455889 A CN 110455889A
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- G—PHYSICS
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- 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
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Abstract
One kind being based on YSZ and NiTiO3Sensitive electrode blendes together electric potential type acetaldehyde sensor and preparation method thereof, belongs to gas sensor technical field.From bottom to up successively by the Al with Pt heating electrode2O3Ceramic wafer, YSZ substrate, Pt reference electrode and NiTiO3Sensitive electrode composition；Pt reference electrode and NiTiO3Sensitive electrode is separate and symmetrically prepares in the both ends of YSZ upper surface of base plate, YSZ base lower surface and the Al with Pt heating electrode2O3Ceramic wafer is bonded together.The present invention utilizes the NiTiO with high electrochemical catalytic activity using stabilizing zirconia (YSZ) as ion conductive layer3Composite oxide material is sensitive electrode, changes the microscopic appearance of sensitive electrode layer by different calcination temperatures (800 DEG C~1200 DEG C), achievees the purpose that improve acetaldehyde sensitivity characteristic.
Description
Technical field
The invention belongs to gas sensor technical fields, and in particular to one kind is based on YSZ and NiTiO3Sensitive electrode mixes
At electric potential type acetaldehyde sensor and preparation method thereof, it is mainly used for the quick detection of volatile aldehyde.
Background technique
Acetaldehyde is one of most important aldehyde material in volatile organic compounds, colourless and have pungent smell, In
It can all be produced in the burning of indoor (construction material, wood varnish etc.) and outdoor (tail gas of automobiles and other vehicles) and discharge process
Raw acetaldehyde.In addition, acetaldehyde is classified as level-one carcinogen by international cancer research institution (IARC), not only played in environmental pollution
Important function, and threaten the health of the mankind.According to the regulation of Occupational Safety and Health Administration (OSHA), the maximum of acetaldehyde
Permission exposure concentrations are 25ppm, working time 8h.A variety of influences harmful to health can be generated by being exposed in acetaldehyde for a long time, such as
The problems such as eye irritation, headache, DNA damage, red blood cell structure change.Therefore, exploitation has highly sensitive, highly selective and high
Real-time, quick, the portable and inexpensive aldehydes gas sensor of stability has vital meaning.
So far, many research teams are using various methods detection aldehydes gas in different applications, such as liquid phase color
Spectrometry, ampere electrochemical cell, molecular imprinting technology, metal oxide semiconductor sensor.Wherein, solid electrolyte type gas
Sensor has many advantages, such as simple at low cost, fast response time, structure, chemistry and good mechanical stability, it is considered to be most has latent
The detection technique of power.Currently, blending together type solid-state electrochemistry gas based on stabilizing zirconia (YSZ) and metal oxide sensitive electrode
Body sensor has been exploited for the toxic gases such as detection VOCs.However, for realizing quick detection acetaldehyde based on blending together
There is not been reported for the YSZ base gas sensor of electric potential type, therefore, develops and find a kind of sensitive electrode suitable for detecting acetaldehyde
Material is extremely important.
Summary of the invention
The object of the present invention is to provide one kind to be based on YSZ and NiTiO3Sensitive electrode blend together electric potential type acetaldehyde sensor and
Preparation method to realize the needs of quickly detection acetaldehyde, and effectively improves transducer sensitivity, reduces the property such as Monitoring lower-cut
Can, promote this sensor in the practical application of volatile aldehyde detection field.The obtained sensor of the present invention is in addition to tool
Have outside rapid response speed and high sensitivity, also there is lower Monitoring lower-cut, good selectivity and stability.
The acetaldehyde sensor of super fast response according to the present invention be based on stabilizing zirconia (YSZ) solid electrolyte and
NiTiO3It is novel constructed by composite oxides sensitive electrode to blend together electric potential type aldehydes gas sensor, YSZ (stabilized with yttrium oxide oxygen
Change zirconium (8%mol Y2O3-ZrO2)) it is used as ion conductive layer.
It is of the present invention to be based on YSZ and NiTiO3Sensitive electrode blendes together electric potential type acetaldehyde sensor, as shown in Figure 1,
From bottom to up successively by the Al with Pt heating electrode2O3Ceramic wafer, YSZ substrate, Pt reference electrode and sensitive electrode composition；Ginseng
Examine electrode and sensitive electrode be separate and symmetrically prepare at the both ends of YSZ upper surface of base plate, YSZ base lower surface with have
The Al of Pt heating electrode2O3Ceramic wafer is bonded together；Sensitive electrode material is NiTiO3, which is prepared by the following method
It arrives,
By Ni (NO3)2·6H2O is dissolved in ethyl alcohol, at room temperature stirring and dissolving；Butyl titanate is added to above-mentioned solution
In, continue to stir evenly, add citric acid and water, is stirred at room temperature to uniform colloidal sol is formed, stand 20~30 hours and obtain
Gel；Ni(NO3)2·6H2O, butyl titanate, citric acid dosage molar ratio be 1:1:2；By obtained gel 80~90
It is dried 12~24 hours under DEG C vacuum condition and obtains xerogel, xerogel is finally sintered to 1~3h at 800~1200 DEG C, from
And obtain NiTiO of the present invention3Sensitive electrode material；
It is of the present invention a kind of based on YSZ and NiTiO3The preparation side for blending together electric potential type acetaldehyde sensor of sensitive electrode
Method, its step are as follows:
(1) it makes Pt reference electrode: being referred in one end of YSZ upper surface of base plate using the Pt of Pt slurry 15~20 μ m-thicks of production
Electrode, while will be sticked to after a Pt doublings on reference electrode middle position as contact conductor, then by YSZ substrate 90
It is toasted 1~2 hour under the conditions of~120 DEG C, then YSZ substrate is sintered 1~2 hour at 1000~1100 DEG C, excluded in platinum slurry
Terpinol, be finally down to room temperature；
(2) NiTiO is made3Sensitive electrode: by NiTiO3Sensitive electrode material is slurred material, mass concentration with deionized water
It is 2~20%；Use NiTiO3Slurry is preparing 20~30 μ m-thicks with the other end of the symmetrical YSZ upper surface of base plate of reference electrode
Sensitive electrode will be equally sticked on sensitive electrode as contact conductor after a platinum filament doubling；
(3) the YSZ substrate that step (2) is prepared with reference electrode and sensitive electrode is sintered 1 under the conditions of 800~1000 DEG C
~3 hours；Heating rate when high temperature sintering is 1~2 DEG C/min；
(4) it prepares inorganic bond: measuring waterglass (Na2SiO3·9H2O) 2~4mL, and weigh Al2O3Powder 0.7~
1.0g, by waterglass and Al2O3Powder is mixed and stirred for uniformly, inorganic bond being made；
(5) Al of electrode is heated using inorganic bond by YSZ base lower surface and with Pt2O3Ceramic wafer is bonded in one
It rises；
Wherein, the Al with Pt heating electrode2O3Ceramic wafer is in Al2O3It is obtained on ceramic wafer by silk-screen printing Pt, band
There is the Al of Pt heating electrode2O3Ceramic wafer is used as the heating plate of sensor；
(6) step (5) is obtained device to be welded, encapsulate, to obtain of the present invention based on YSZ and NiTiO3
Sensitive electrode blendes together electric potential type acetaldehyde sensor.
The present invention is using stabilizing zirconia (YSZ) as ion conductive layer, using with high electrochemical catalytic activity
NiTiO3Composite oxide material is sensitive electrode, changes sensitive electrode by different calcination temperatures (800 DEG C~1200 DEG C)
The microscopic appearance of layer achievees the purpose that improve acetaldehyde sensitivity characteristic.
Advantages of the present invention:
(1) typical solid electrolyte -- stabilizing zirconia (YSZ) is utilized, there is good thermal stability and chemical stabilization
Property, acetaldehyde can be detected in complex environment；
(2) high-performance composite oxide NiTiO is prepared using simple sol-gel method3As sensor sensing electrode,
Preparation method is simple, conducive to the industrial production of mass.
(3) by changing the different calcination temperatures (800 DEG C~1200 DEG C) of material, obtaining has the quick of different cellular structures
It is anti-quickly to reach three phase boundary participation electrochemistry conducive under test gas to optimize the microstructure of sensitive electrode for sense electrode layer
It answers, to improve the response speed and sensitivity of sensor.
Detailed description of the invention
Fig. 1: YSZ base of the present invention blendes together the structural schematic diagram of electric potential type acetaldehyde sensor.
Each section title: Pt silk 1, NiTiO3Sensitive electrode 2, YSZ substrate 3, Pt reference electrode 4, Pt point are (for gluing electrode
Lead) 5, inorganic bond 6, the Al with Pt heating electrode2O3Ceramic wafer 7.
Fig. 2: NiTiO obtained by present invention difference sintering temperature3(wherein, abscissa is the XRD diagram of sensitive electrode material
Angle, ordinate are intensity).
As shown in Fig. 2, being different sintering temperature NiTiO3The XRD diagram of sensitive electrode material, by being compared with standard spectrogram,
It is sintered obtained material and NiTiO3Standard card JCPDS (File No.76-334) is consistent.Show that we invent preparation
Sensitive electrode material is NiTiO3Material.
Fig. 3: the SEM figure of sensitive electrode material prepared by present invention difference sintering temperature.
As shown in figure 3, a:800 DEG C, b:1000 DEG C, the NiTiO of c:1200 DEG C of sintering3The SEM of sensitive electrode material schemes, from
It can be seen that the raising with sintering temperature in figure, granular size is gradually increased, and the sintering temperature for changing sensitive material can change
The microscopic appearance for becoming sensitive electrode, forms loose porous structure, and the porosity of electrode is conducive to the diffusion of gas.
Fig. 4: the NiTiO being sintered at 800 DEG C, 1000 DEG C and 1200 DEG C respectively is utilized3Biography as sensitive electrode material
Response curve of the sensor to 50ppm acetaldehyde (wherein, abscissa is the time, and ordinate is potential difference values).
As shown in figure 4, being device made by embodiment 1,2,3 to the potential difference Δ V (response of device of 50ppm acetaldehyde
Indicated with potential difference Δ V), it can be seen from the figure that the response of 1,2,3 pair of 50ppm acetaldehyde of embodiment respectively -16mV, -
43mV and -3mV.It can be seen that the NiTiO being sintered at 1000 DEG C3YSZ base as sensitive electrode material blendes together electric potential type acetaldehyde
Sensor has highest response.
Fig. 5: the NiTiO being sintered at 1000 DEG C is utilized3Sensor continuous response curve (a) as sensitive electrode material
(wherein, abscissa is the time, and ordinate is potential difference values.Operating temperature is 575 degree) and sensitivity curve (b, c) (wherein, cross
Coordinate is acetaldehyde concentration, and ordinate is potential difference values.Operating temperature is 575 degree).
As shown in figure 5, being NiTiO3(1000℃)The continuous response curve of device, it can be seen from the figure that device is to 50ppm
The response of acetaldehyde is -43mV, the minimum acetaldehyde that can detecte 200ppb, this sensor show ultrafast response speed and
Lower Monitoring lower-cut.
Fig. 6: the NiTiO being sintered at 1000 DEG C is utilized3The selective bar chart of sensor as sensitive electrode material.
(wherein, abscissa is potential difference values, and ordinate is test gas: being from top to bottom respectively ethylene, nitric oxide, ammonia, dioxy
Change nitrogen, carbon monoxide, benzene, toluene, acetic acid, dimethylbenzene, formaldehyde, ethyl alcohol, methanol, n-butanal)；
As shown in fig. 6, being NiTiO3(1000℃)The selectivity of device, it can be seen from the figure that device shows acetaldehyde
Maximum sensitivity characteristic, it can be seen that, device has selectivity well.
Fig. 7: the NiTiO being sintered at 1000 DEG C is utilized3Humidity influence curve (its of sensor as sensitive electrode material
In, abscissa is relative humidity, and ordinate is potential difference values).
As shown in fig. 7, being NiTiO3(1000℃)Response of the device under different humidity to 100ppm acetaldehyde, can be with from figure
Find out, device is smaller to the response variation of 100ppm acetaldehyde in 20~98% humidity range, and showing sensor has very
Good moisture-proof.
Fig. 8: the NiTiO being sintered at 1000 DEG C is utilized3The stability curve of sensor as sensitive electrode material.(its
In, abscissa is the time, and the ordinate of upper and lower two figure is respectively potential difference values and potential difference knots modification)
As shown in figure 8, being NiTiO3(1000℃)Stability test of the device in 20 days, it can be seen from the figure that device exists
In 20 days, the fluctuation range of response is smaller, shows that this device has good stability.
Specific embodiment
Embodiment 1:
NiTiO is prepared with sol-gel method3Material, the NiTiO that 1000 DEG C are sintered3(1000℃)As sensitive electrode material
Production YSZ base blendes together electric potential type acetaldehyde sensor, and tests sensor air-sensitive performance, and detailed process is as follows:
1. production Pt reference electrode: being starched in one end of the YSZ upper surface of base plate of 2 × 2mm of length and width, thickness 0.2mm using Pt
Make the Pt reference electrode of one layer of 0.5mm × 2mm size, 15 μ m-thicks, while with being sticked in reference electrode after a Pt doublings
Between extraction electrode lead on position；Then YSZ substrate is toasted 1.5 hours under the conditions of 100 DEG C, then by YSZ substrate 1000
It is sintered 1 hour at DEG C, to exclude the terpinol in platinum slurry, is finally down to room temperature.
2. making NiTiO3Sensitive electrode: the Ni (NO of 5mmol is weighed3)2·6H2O is dissolved in the ethyl alcohol of 15mL, room temperature
Stirring is extremely dissolved；The butyl titanate of 5mmol is added in the above solution, continues to stir evenly, be added 10mmol citric acid and
The water of 15mL is stirred at room temperature to uniform colloidal sol is formed, stands 24 hours；Obtained gel is dried 24 under 80 DEG C of vacuum conditions
Hour obtains xerogel, is finally sintered 3 hours under the conditions of 1000 DEG C, obtains NiTiO3Sensitive electrode material.
Take 5mg NiTiO3Powder is tuned into slurry with deionized water 100mg, by NiTiO3Slurry is symmetrical with reference electrode
The other end of YSZ upper surface of base plate coats the sensitive electrode of one layer of 0.5mm × 2mm size, 20 μ m-thicks, a same platinum filament pair
Extraction electrode lead on sensitive electrode is sticked to after folding.
The YSZ substrate with reference electrode and sensitive electrode made is warming up to 800 with the heating rate of 2 DEG C/min
DEG C and be down to room temperature after keeping 2h.
3. bonding the ceramic wafer with heating electrode.Use inorganic bond (Al2O3With waterglass Na2SiO3·9H2O, matter
Amount volume ratio is 1g:4mL) Pt that has of the lower surface (side of uncoated electrode) of YSZ substrate and same size is heated into electricity
The Al of pole2O3Ceramic wafer (2 × 2mm of length and width, thickness 0.2mm) is bonded.
4. device welding, encapsulation.Device is welded on hexagonal tube socket, shield is put on, completes and blendes together electric potential type
Acetaldehyde sensor.
Embodiment 2:
The NiTiO being sintered with 800 DEG C3Material makes acetaldehyde sensor, manufacturing process as sensitive electrode material are as follows:
By NiTiO prepared by preceding method3800 DEG C of sintering obtain sensitive electrode material in Muffle furnace
NiTiO3(800℃), device fabrication processes are same as Example 1.
Embodiment 3:
The NiTiO being sintered with 1200 DEG C3Material makes acetaldehyde sensor, manufacturing process as sensitive electrode material are as follows:
By NiTiO prepared by preceding method31200 DEG C of sintering obtain sensitive electrode material in Muffle furnace
NiTiO3(1200℃), device fabrication processes are same as Example 1.
Sensor is connected on Rigol signal tester, respectively by sensor be placed in air, 200ppb acetaldehyde,
500ppb acetaldehyde, 1ppm acetaldehyde, 2ppm acetaldehyde, 5ppm acetaldehyde, 10ppm acetaldehyde, 20ppm acetaldehyde, 50ppm acetaldehyde, 100ppm second
Aldehyde, 200ppm acetaldehyde atmosphere in carry out voltage signal test.The response size of device indicates with Δ V, value VUnder test gas-
VAir。
Table 1: with NiTiO3(800℃)、NiTiO3(1000℃)And NiTiO3(1200℃)For sensitive electrode material sensor to 50ppm
Acetaldehyde responds Value Data
Table 2: with NiTiO3(1000℃)For sensitive electrode material sensor Δ V with acetaldehyde concentration delta data
| The concentration (ppm) of acetaldehyde | Sensitive electrode and reference electrode potential difference Δ V (mV) |
| 0.2 | -4.5 |
| 0.5 | -7.5 |
| 1 | -3.5 |
| Sensitivity (mV/decade) | -3 |
| 1 | -3.5 |
| 2 | -9 |
| 5 | -12 |
| 10 | -25 |
| 20 | -34 |
| 50 | -43 |
| 100 | -54.5 |
| 200 | -62.5 |
| Sensitivity (mV/decade) | -26.5 |
It is listed in table 1 respectively with NiTiO3(800℃)、NiTiO3(1000℃)And NiTiO3(1200℃)For the biography of sensitive electrode material
Sensor is to 50ppm acetaldehyde response size.It can be seen that, three kinds of devices have good response characteristic to acetaldehyde from table,
Wherein use NiTiO3(1000℃)It is -43mV for the response highest of the device of sensitive electrode material.In addition, can from table 2
Out, NiTiO3(1000℃)Device reaches 200ppb to the Monitoring lower-cut of acetaldehyde.Sensitivity to 0.2-1ppm and 1-200ppm acetaldehyde
For -3mV/decade and -26.5mV/decade.It can be seen that the Copper diethlydithiocarbamate that blendes together currently constructed shows acetaldehyde
Good sensitivity characteristic has good potential application foreground in atmospheric environment detection field.
Claims (4)
1. one kind is based on YSZ and NiTiO3Sensitive electrode blendes together electric potential type acetaldehyde sensor, from bottom to up successively by adding with Pt
The Al of thermode2O3Ceramic wafer, YSZ substrate, Pt reference electrode and sensitive electrode composition；Reference electrode and sensitive electrode divide each other
It stands and symmetrically prepares in the both ends of YSZ upper surface of base plate, YSZ base lower surface and the Al with Pt heating electrode2O3Ceramic wafer
It is bonded together；Sensitive electrode material is NiTiO3, which is prepared by the following method,
By Ni (NO3)2·6H2O is dissolved in ethyl alcohol, at room temperature stirring and dissolving；Butyl titanate is added in above-mentioned solution,
Continue to stir evenly, add citric acid and water, is stirred at room temperature to uniform colloidal sol is formed, stand 20~30 hours and coagulated
Glue；Ni(NO3)2·6H2O, butyl titanate, citric acid dosage molar ratio be 1:1:2；By obtained gel at 80~90 DEG C
It is dried 12~24 hours under vacuum condition and obtains xerogel, xerogel is finally sintered to 1~3h at 800~1200 DEG C, thus
Obtain NiTiO3Sensitive electrode material.
2. described in claim 1 a kind of based on YSZ and NiTiO3The preparation side for blending together electric potential type acetaldehyde sensor of sensitive electrode
Method, its step are as follows:
(1) Pt reference electrode is made: in one end of YSZ upper surface of base plate using the Pt of Pt slurry 15~20 μ m-thicks of production with reference to electricity
Pole, while will be sticked to after a Pt doublings on reference electrode middle position as contact conductor, then by YSZ substrate 90~
It is toasted 1~2 hour under the conditions of 120 DEG C, then YSZ substrate is sintered 1~2 hour at 1000~1100 DEG C, excluded in platinum slurry
Terpinol is finally down to room temperature；
(2) NiTiO is made3Sensitive electrode: by NiTiO3Sensitive electrode material is slurred material with deionized water, and mass concentration is 2~
20%；Use NiTiO3Slurry is in the sensitivity for preparing 20~30 μ m-thicks with the other end of the symmetrical YSZ upper surface of base plate of reference electrode
Electrode will be equally sticked on sensitive electrode as contact conductor after a platinum filament doubling；
(3) the YSZ substrate that step (2) is prepared with reference electrode and sensitive electrode is sintered 1~3 under the conditions of 800~1000 DEG C
Hour；
(4) it prepares inorganic bond: measuring 2~4mL of waterglass, and weigh Al2O30.7~1.0g of powder, by waterglass and Al2O3
Powder is mixed and stirred for uniformly, inorganic bond being made；
(5) Al of electrode is heated using inorganic bond by YSZ base lower surface and with Pt2O3Ceramic wafer is bonded together；
(6) step (5) is obtained device to be welded, encapsulate, to obtain based on YSZ and NiTiO3Sensitive electrode blendes together electricity
Bit-type acetaldehyde sensor.
3. as claimed in claim 2 a kind of based on YSZ and NiTiO3The preparation for blending together electric potential type acetaldehyde sensor of sensitive electrode
Method, it is characterised in that: heating rate when step (3) high temperature is sintered is 1~2 DEG C/min.
4. as claimed in claim 2 a kind of based on YSZ and NiTiO3The preparation for blending together electric potential type acetaldehyde sensor of sensitive electrode
Method, it is characterised in that: the Al with Pt heating electrode in step (5)2O3Ceramic wafer is in Al2O3Pass through silk screen on ceramic wafer
Printing Pt is obtained, the Al with Pt heating electrode2O3Ceramic wafer is used as the heating plate of sensor.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111413386A (en) * | 2020-04-09 | 2020-07-14 | 吉林大学 | Based on YSZ and MTiO3Mixed potential type acetylene sensor of sensitive electrode and preparation method thereof |
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| CN111413386A (en) * | 2020-04-09 | 2020-07-14 | 吉林大学 | Based on YSZ and MTiO3Mixed potential type acetylene sensor of sensitive electrode and preparation method thereof |
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Application publication date: 20191115 |