CN104215673A - Preparation method of Zr-based nitric oxide sensor with high selectivity - Google Patents
Preparation method of Zr-based nitric oxide sensor with high selectivity Download PDFInfo
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- CN104215673A CN104215673A CN201410430029.3A CN201410430029A CN104215673A CN 104215673 A CN104215673 A CN 104215673A CN 201410430029 A CN201410430029 A CN 201410430029A CN 104215673 A CN104215673 A CN 104215673A
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- zirconium
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Abstract
The invention discloses a preparation method of a Zr-based nitric oxide sensor with high selectivity. The method comprises the following steps: preparing a raw YSZ ceramic chip by virtue of a tape casting technique; degluing and sintering the raw YSZ ceramic chip so as to obtain a Zr-based solid electrolyte substrate; mixing potassium dichromate, formaldehyde and citric acid according to a molar ratio of 1 to 6 to 0.6, dissolving the mixture in deionized water, reacting and drying so as to obtain Cr2O3 powder; calcining the Cr2O3 powder to obtain flaky Cr2O3 powder; dissolving the flaky Cr2O3 powder in a polymer chemical reagent to obtain Cr2O3 electrode slurry; then preparing a porous and flaky Cr2O3 sensitive electrode by virtue of a screen printing technique and leading an electrode leading wire out; preparing a porous Pt reference electrode by virtue of the screen printing technique and leading the electrode leading wire out; and finally, sintering and molding so as to obtain the Zr-based nitric oxide sensor. The method is simple in process, by taking flaky Cr2O3 as the sensitive electrode, the sensor prepared by the method is simple and exquisite in structure, and has the high selectivity to nitric oxide gas in medium and high temperature environments, so that the prepared sensor is high in measurement sensitivity.
Description
Technical field
The present invention relates to a kind of nitric oxide sensor, especially a kind of preparation method of high selectivity zirconium base nitric oxide sensor, specifically a kind of based on flake nano pattern Cr
2o
3the preparation method of the zirconium base nitrogen monoxide gas sensor of sensitive electrode.
Background technology
China's urban atmosphere pollutes and just pollutes development by coal-smoke pollution to vehicle exhaust type; The oxynitrides (NOx) of motor vehicle emission, the pollutant severe overweights such as carbon monoxide (CO) and hydrocarbon (HCs), wherein the excess emissions of NOx is the one of the main reasons producing haze and acid rain problem.
At present based on yttrium stable zirconium oxide (Yttria Stablilzed Zirconia, be called for short YSZ or zirconium base) electrolytical NOx sensor owing to being applicable to extreme environment and its relatively high sensitivity and extensively concerned, wherein to be equipped with chromium oxide sensitive electrode (Cr
2o
3-SE) the research of zirconium base NOx sensor the most extensive.But the NOx sensor developed at present is subject to the interference of other co-existing gases to the response of NOx more, the multipair nitrogen dioxide (NO of these NOx sensor in addition
2) present better sensitivity, and the principal ingredient under high temperature in oxynitrides gas is nitrogen monoxide (NO).Therefore be necessary to develop a kind of can in extreme circumstances to the NO sensor of NO high selectivity response.
Summary of the invention
Technical matters to be solved by this invention is for above-mentioned prior art present situation, and provides preparation technology the preparation method of simple a kind of high selectivity zirconium base nitric oxide sensor; The sensor obtained by this preparation method adopts sheet-like morphology Cr
2o
3as sensitive electrode, structure is simple, small and exquisite, in middle hot environment, have high selectivity to nitric oxide gas, measures sensitivity high.
The present invention solves the problems of the technologies described above adopted technical scheme:
A preparation method for high selectivity zirconium base nitric oxide sensor, comprises the following steps:
Step one, employing flow casting molding technology make YSZ ceramic chips, after YSZ ceramic chips is carried out binder removal in atmosphere, put into sintering furnace and sinter, obtain Zirconium-base solid electrolyte basic unit;
Step 2, by being dissolved in deionized water after the 1:6:0.6 mixing in molar ratio of potassium dichromate, formaldehyde, citric acid, mixed solution being proceeded to reaction kettle for reaction and obtains gel, after the washing of the gel that obtains, drying obtains Cr
2o
3powder, then by Cr
2o
3powder calcining obtains sheet Cr
2o
3powder, then by sheet Cr
2o
3powder dissolves in high polymer chemistry reagent, makes Cr
2o
3electrode slurry;
Step 3, the Cr will prepared in step 2
2o
3electrode slurry, flake porous Cr is made in the side of the Zirconium-base solid electrolyte basic unit adopting screen printing technique step one to obtain
2o
3after sensitive electrode, put into drying box drying;
Step 4, at flake porous Cr
2o
3on sensitive electrode, spot printing Pt starches, and extraction electrode lead-in wire;
Step 5, opposite side in Zirconium-base solid electrolyte basic unit, adopt screen printing technique that platinum slurry is made porous Pt contrast electrode, and extraction electrode lead-in wire;
Step 6, will make flake porous Cr
2o
3the Zirconium-base solid electrolyte basic unit sinter molding of sensitive electrode and porous Pt contrast electrode, obtains zirconium base nitric oxide sensor.
For optimizing technique scheme, the measure taked also comprises:
In above-mentioned step one, the thickness of YSZ ceramic chips is 0.3mm to 1mm.
In above-mentioned step one, dump temperature is 350 to 400 DEG C, and the binder removal time is 20 hours.
In above-mentioned step one, sintering temperature is 1200 DEG C to 1400 DEG C, and sintering time is 2 hours.
In above-mentioned step 2, temperature of reaction is in a kettle. 180 DEG C, and the reaction time is 1 hour.
In above-mentioned step 2, baking temperature is 140 DEG C.
In above-mentioned step 2, calcining heat is 1000 DEG C, and calcination time is 2 hours.
Above-mentioned high polymer chemistry reagent is isoamylol.
It is 2 hours in the time of drying box drying in above-mentioned step 3.
In above-mentioned step 6, sintering temperature is 900 to 1000 DEG C, and sintering time is 2 hours.
Compared with prior art, sensor of the present invention adopts a kind of flake nano pattern Cr
2o
3material, as sensitive electrode, makes under middle high temperature, to have very high selectivity based on zirconium base nitric oxide sensor to nitric oxide production response, and comparatively strong to other gas antijamming capabilities, prepared sensor construction is simple, volume is little, preparation technology is simple.And this zirconium base nitric oxide sensor belongs to mixed potential type sensor, contrast electrode and sensitive electrode can be exposed in atmosphere to be measured simultaneously, can achieve good measurement effect under 0-500 ppm gasmetry scope.
Accompanying drawing explanation
Fig. 1 is the flake porous Cr of sensor of the present invention
2o
3the shape appearance figure of sensitive electrode;
Fig. 2 is the cross-sectional view of sensor of the present invention;
Fig. 3 is sensor of the present invention response results figure to various gas under optimum working temperature;
Fig. 4 is the ladder response curve of sensor of the present invention.
Embodiment
Below in conjunction with accompanying drawing, embodiments of the invention are described in further detail.
Reference numeral is wherein: Zirconium-base solid electrolyte basic unit 1, flake porous Cr
2o
3sensitive electrode 2, porous Pt contrast electrode 3, Pt slurry 4, contact conductor 5.
Embodiment one,
The preparation method of a kind of high selectivity zirconium of the present invention base nitric oxide sensor, comprises the following steps:
Step one, employing flow casting molding technology make the YSZ ceramic chips that thickness is 0.3mm, YSZ ceramic chips are carried out in atmosphere 350 DEG C of binder removals after 20 hours, put into sintering furnace and sinter 2 hours at 1200 DEG C of temperature, obtain Zirconium-base solid electrolyte basic unit 1;
Step 2, will 2.94g potassium dichromate, 1.65ml formaldehyde, 0.12g citric acid mixing after be dissolved in 35ml deionized water, the mol ratio of potassium dichromate, formaldehyde, citric acid is 1:6:0.6; Proceeded to by mixed solution in 50ml reactor, at 180 DEG C of temperature, reaction obtains gel in 1 hour, and after the gel washing obtained, at 140 DEG C of temperature, drying obtains Cr
2o
3powder, then by Cr
2o
3powder obtains sheet Cr in 2 hours at 1000 DEG C of temperature lower calcinations
2o
3powder, then by sheet Cr
2o
3powder dissolves in high polymer chemistry reagent isoamylol, makes Cr
2o
3electrode slurry;
Step 3, the Cr will prepared in step 2
2o
3electrode slurry, flake porous Cr is made in 140 DEG C, side, the oven dry in 1 hour of the Zirconium-base solid electrolyte basic unit 1 adopting screen printing technique step one to obtain
2o
3after sensitive electrode, put into drying box dry 2 hours;
Step 4, at described flake porous Cr
2o
3on sensitive electrode 2, spot printing Pt starches 4, and extraction electrode lead-in wire 5;
Step 5, opposite side in described Zirconium-base solid electrolyte basic unit 1, adopt screen printing technique that platinum slurry is made porous Pt contrast electrode 3, and extraction electrode lead-in wire 5;
Step 6, will make flake porous Cr
2o
3the Zirconium-base solid electrolyte basic unit 1 of sensitive electrode 2 and porous Pt contrast electrode 3 puts into high temperature furnace, at 900 DEG C of temperature sinter 2 hours shaping, obtain zirconium base nitric oxide sensor.
Embodiment two,
The preparation method of a kind of high selectivity zirconium of the present invention base nitric oxide sensor, comprises the following steps:
Step one, employing flow casting molding technology make the YSZ ceramic chips that thickness is 1mm, YSZ ceramic chips are carried out in atmosphere 400 DEG C of binder removals after 20 hours, put into sintering furnace and sinter 2 hours at 1400 DEG C of temperature, obtain Zirconium-base solid electrolyte basic unit 1;
Step 2, will 2.94g potassium dichromate, 1.65ml formaldehyde, 0.12g citric acid mixing after be dissolved in 35ml deionized water, the mol ratio of potassium dichromate, formaldehyde, citric acid is 1:6:0.6; Proceeded to by mixed solution in 50ml reactor, at 180 DEG C of temperature, reaction obtains gel in 1 hour, and after the gel washing obtained, at 140 DEG C of temperature, drying obtains Cr
2o
3powder, then by Cr
2o
3powder obtains sheet Cr in 2 hours at 1000 DEG C of temperature lower calcinations
2o
3powder, then by sheet Cr
2o
3powder dissolves in high polymer chemistry reagent isoamylol, makes Cr
2o
3electrode slurry;
Step 3, the Cr will prepared in step 2
2o
3electrode slurry, flake porous Cr is made in 140 DEG C, side, the oven dry in 1 hour of the Zirconium-base solid electrolyte basic unit 1 adopting screen printing technique step one to obtain
2o
3after sensitive electrode, put into drying box dry 2 hours;
Step 4, at described flake porous Cr
2o
3on sensitive electrode 2, spot printing Pt starches 4, and extraction electrode lead-in wire 5;
Step 5, opposite side in described Zirconium-base solid electrolyte basic unit 1, adopt screen printing technique that platinum slurry is made porous Pt contrast electrode 3, and extraction electrode lead-in wire 5;
Step 6, will make flake porous Cr
2o
3the Zirconium-base solid electrolyte basic unit 1 of sensitive electrode 2 and porous Pt contrast electrode 3 puts into high temperature furnace, at 1000 DEG C of temperature sinter 2 hours shaping, obtain zirconium base nitric oxide sensor.
Embodiment three,
The preparation method of a kind of high selectivity zirconium of the present invention base nitric oxide sensor, comprises the following steps:
Step one, employing flow casting molding technology make the YSZ ceramic chips that thickness is 0.6mm, YSZ ceramic chips are carried out in atmosphere 380 DEG C of binder removals after 20 hours, put into sintering furnace and sinter 2 hours at 1300 DEG C of temperature, obtain Zirconium-base solid electrolyte basic unit 1;
Step 2, will 2.94g potassium dichromate, 1.65ml formaldehyde, 0.12g citric acid mixing after be dissolved in 35ml deionized water, the mol ratio of potassium dichromate, formaldehyde, citric acid is 1:6:0.6; Proceeded to by mixed solution in 50ml reactor, at 180 DEG C of temperature, reaction obtains gel in 1 hour, and after the gel washing obtained, at 140 DEG C of temperature, drying obtains Cr
2o
3powder, then by Cr
2o
3powder obtains sheet Cr in 2 hours at 1000 DEG C of temperature lower calcinations
2o
3powder, then by sheet Cr
2o
3powder dissolves in high polymer chemistry reagent isoamylol, makes Cr
2o
3electrode slurry;
Step 3, the Cr will prepared in step 2
2o
3electrode slurry, flake porous Cr is made in 140 DEG C, side, the oven dry in 1 hour of the Zirconium-base solid electrolyte basic unit 1 adopting screen printing technique step one to obtain
2o
3after sensitive electrode, put into drying box dry 2 hours;
Step 4, at described flake porous Cr
2o
3on sensitive electrode 2, spot printing Pt starches 4, and extraction electrode lead-in wire 5;
Step 5, opposite side in described Zirconium-base solid electrolyte basic unit 1, adopt screen printing technique that platinum slurry is made porous Pt contrast electrode 3, and extraction electrode lead-in wire 5;
Step 6, will make flake porous Cr
2o
3the Zirconium-base solid electrolyte basic unit 1 of sensitive electrode 2 and porous Pt contrast electrode 3 puts into high temperature furnace, at 950 DEG C of temperature sinter 2 hours shaping, obtain zirconium base nitric oxide sensor.
The zirconium base nitric oxide sensor prepared by above-mentioned preparation method, have employed flake nano pattern Cr
2o
3(shown in Fig. 1) is as sensitive electrode.The Cr of sheet-like morphology
2o
3the zirconium base nitric oxide sensor of preparation is made to have high selectivity to NO; Through experimental studies have found that, adopt the chromium oxide of other pattern (such as the chromium oxide of cubic pattern), the sensor of preparation also has response to HCs, is very easily subject to the interference of HCs in testing process.And the Cr of sheet-like morphology
2o
3very weak but very strong to the electrochemical activity of NO to the electrochemical activity of HCs, thus realize responding the high selectivity of NO.
According to gas sensor domain acquiescence regulation, if sensor to the response signal of object gas higher than 3 times to other gas response signals, then can be described as this sensor to this gas have high selectivity response.The response signal of zirconium base nitric oxide sensor to 200 ppm NO of inventing in this patent is 16.9 millivolts, and be no more than 2 millivolts to the response signal of same other gases of concentration, relative signal ratio is about 8 times, and therefore the response of this sensor to NO has high selectivity.
Sensor operating principles is as follows:
Flake porous Cr
2o
3define three phase boundary between sensitive electrode 2 and Zirconium-base solid electrolyte basic unit 1, before gas enters into sensor three phase boundary, have part gas to be measured to there occurs gas-phase reaction, when gas to be measured enters flake porous Cr
2o
3there occurs following electrochemical reaction behind sensitive electrode 2 and three phase boundary place of Zirconium-base solid electrolyte basic unit 1 to react:
Anode reaction:
Cathode reaction:
;
As NO anode current and O
2mixed potential can be obtained when cathode current is equal, and the response of sensor to gas can be obtained thus, and the log concentration of the response of sensor and gas to be measured is linear, the concentration of gas to be measured so just can be obtained by the response of sensor.
Figure 3 shows that the response of sensor to various gas under optimum working temperature (475 DEG C).Can see: have good selective response at 475 DEG C of lower sensors to NO.
When Fig. 4 is 475 DEG C under variable concentrations NO (40-500 ppm), the ladder response diagram of sensor.Can obviously see: this sensor sheet reveals well repeatability and stability, and the logarithm of this sensor response and gas concentration presents good linear relationship.
Most preferred embodiment of the present invention is illustrated, and the various change made by those of ordinary skill in the art or remodeling all can not depart from the scope of the present invention.
Claims (10)
1. a preparation method for high selectivity zirconium base nitric oxide sensor, is characterized in that: comprise the following steps:
Step one, employing flow casting molding technology make YSZ ceramic chips, after YSZ ceramic chips is carried out binder removal in atmosphere, put into sintering furnace and sinter, obtain Zirconium-base solid electrolyte basic unit (1);
Step 2, by being dissolved in deionized water after the 1:6:0.6 mixing in molar ratio of potassium dichromate, formaldehyde, citric acid, mixed solution being proceeded to reaction kettle for reaction and obtains gel, after the washing of the gel that obtains, drying obtains Cr
2o
3powder, then by Cr
2o
3powder calcining obtains sheet Cr
2o
3powder, then by sheet Cr
2o
3powder dissolves in high polymer chemistry reagent, makes Cr
2o
3electrode slurry;
Step 3, the Cr will prepared in step 2
2o
3electrode slurry, flake porous Cr is made in the side of the Zirconium-base solid electrolyte basic unit (1) adopting screen printing technique step one to obtain
2o
3after sensitive electrode, put into drying box drying;
Step 4, at described flake porous Cr
2o
3the upper spot printing Pt of sensitive electrode (2) starches (4), and extraction electrode lead-in wire (5);
Step 5, opposite side in described Zirconium-base solid electrolyte basic unit (1), adopt screen printing technique that platinum slurry is made porous Pt contrast electrode (3), and extraction electrode lead-in wire (5);
Step 6, will make flake porous Cr
2o
3zirconium-base solid electrolyte basic unit (1) sinter molding of sensitive electrode (2) and porous Pt contrast electrode (3), obtains zirconium base nitric oxide sensor.
2. a preparation method for a kind of high selectivity zirconium base nitric oxide sensor according to claim 1, is characterized in that: in described step one, the thickness of YSZ ceramic chips is 0.3mm to 1mm.
3. a preparation method for a kind of high selectivity zirconium base nitric oxide sensor according to claim 2, is characterized in that: in described step one, dump temperature is 350 DEG C to 400 DEG C, and the binder removal time is 20 hours.
4. a preparation method for a kind of high selectivity zirconium base nitric oxide sensor according to claim 3, is characterized in that: in described step one, sintering temperature is 1200 DEG C to 1400 DEG C, and sintering time is 2 hours.
5. a preparation method for a kind of high selectivity zirconium base nitric oxide sensor according to claim 4, is characterized in that: in described step 2, temperature of reaction is in a kettle. 180 DEG C, and the reaction time is 1 hour.
6. a preparation method for a kind of high selectivity zirconium base nitric oxide sensor according to claim 5, is characterized in that: in described step 2, baking temperature is 140 DEG C.
7. a preparation method for a kind of high selectivity zirconium base nitric oxide sensor according to claim 6, it is characterized in that: in described step 2, calcining heat is 1000 DEG C, calcination time is 2 hours.
8. a preparation method for a kind of high selectivity zirconium base nitric oxide sensor according to claim 7, is characterized in that: described high polymer chemistry reagent is isoamylol.
9. a preparation method for a kind of high selectivity zirconium base nitric oxide sensor according to claim 8, is characterized in that: be 2 hours in the time of drying box drying in described step 3.
10. a preparation method for a kind of high selectivity zirconium base nitric oxide sensor according to claim 9, it is characterized in that: in described step 6, sintering temperature is 900 to 1000 DEG C, sintering time is 2 hours.
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CN104950028A (en) * | 2015-06-16 | 2015-09-30 | 宁波大学 | Zr-based amperometric three-electrode slice NO gas sensor and preparation method thereof |
CN106198677A (en) * | 2016-06-23 | 2016-12-07 | 宁波大学 | A kind of method using zirconio sensor detection organic volatile |
CN104792846B (en) * | 2014-12-10 | 2017-10-03 | 中国第一汽车股份有限公司 | Available for NOXThe Multi-function protective cover and its coating production of sensor |
CN111089882A (en) * | 2020-01-02 | 2020-05-01 | 宁波大学 | Hydrogen sensor structure and preparation method thereof |
CN114402194A (en) * | 2019-09-24 | 2022-04-26 | 独立行政法人国立高等专门学校机构 | Gas sensor and method for producing alkaline earth ferrite |
CN115950939A (en) * | 2023-03-10 | 2023-04-11 | 华北理工大学 | YSZ-NiO porous layer-based sensor and preparation method and application thereof |
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CN104749235A (en) * | 2015-03-12 | 2015-07-01 | 宁波大学 | High-selectivity compensation type CO sensor and preparation method thereof |
CN104749235B (en) * | 2015-03-12 | 2018-12-04 | 宁波大学 | A kind of highly selective setoff type CO sensor and preparation method thereof |
CN104950028A (en) * | 2015-06-16 | 2015-09-30 | 宁波大学 | Zr-based amperometric three-electrode slice NO gas sensor and preparation method thereof |
CN106198677A (en) * | 2016-06-23 | 2016-12-07 | 宁波大学 | A kind of method using zirconio sensor detection organic volatile |
CN114402194A (en) * | 2019-09-24 | 2022-04-26 | 独立行政法人国立高等专门学校机构 | Gas sensor and method for producing alkaline earth ferrite |
CN114402194B (en) * | 2019-09-24 | 2024-02-13 | 独立行政法人国立高等专门学校机构 | Gas sensor and method for producing alkaline earth ferrite |
CN111089882A (en) * | 2020-01-02 | 2020-05-01 | 宁波大学 | Hydrogen sensor structure and preparation method thereof |
CN111089882B (en) * | 2020-01-02 | 2022-09-02 | 宁波大学 | Hydrogen sensor structure and preparation method thereof |
CN115950939A (en) * | 2023-03-10 | 2023-04-11 | 华北理工大学 | YSZ-NiO porous layer-based sensor and preparation method and application thereof |
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