CN104897761A - YSZ base mixed-potential type NO2 sensor based on hierarchical In2O3 sensing electrode and preparation method - Google Patents
YSZ base mixed-potential type NO2 sensor based on hierarchical In2O3 sensing electrode and preparation method Download PDFInfo
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Abstract
The invention belongs to the technical field of gas sensors, and particularly relates to a YSZ base mixed-potential type NO2 sensor based on a hierarchical In2O3 sensing electrode and a preparation method of the YSZ base mixed-potential type NO2 sensor. The sensor can be mainly applied to the detection of automobile exhaust, and sequentially comprises an Al2O3 ceramic plate with a Pt heating electrode, a YSZ baseplate, a reference electrode and a sensing electrode, wherein the reference electrode is strip Pt; the sensing electrode is strip In2O3; the reference electrode and the sensing electrode are discrete with each other and symmetrically arranged at the two ends of the upper surface of the YSZ baseplate; the lower surface of the YSZ baseplate is bonded with the Al2O3 ceramic plate with a Pt heating electrode. According to the invention, the YSZ baseplate is used as an ion conducting layer, In2O3 with high electrochemicalcatalytic activity is used as the sensing electrode, and the micro appearance of the sensing electrode material is changed through different calcination temperatures (800 DEG C to 1200 DEG C), so that the purpose of improving the sensitive property is achieved.
Description
Technical field
The invention belongs to gas sensor technical field, be specifically related to a kind of based on graduation In
2o
3the YSZ base of sensitive electrode blendes together electric potential type NO
2sensor and preparation method thereof, this sensor mainly can be used for the detection of vehicle exhaust.
Background technology
NO
2as a group high activity reacting gas (NO
x) one, be mainly derived from burning and exhausting process, especially an on-highway motor vehicle exhaust emissions.The NO emitted in a large number
2not only can cause the atmosphere polluting problem that such as acid rain, greenhouse effect, depletion of the ozone layer etc. are serious, and severe injury is caused to the respiratory system of the mankind.In order to effectively solve relevant pollution problem from source, the protection mankind's is healthy, develops cheap, miniature, responsive, reliable gas sensor and is used for monitor and forecast NO
xit is exigence.Because automobile engine tail gas discharge is in typical long term high temperature, high humidity and multiple gases coexisted environment, require that the sensor of normal work in such a case must have good sensitivity characteristic.In more than ten years in the past, the electric potential type gas sensor that blendes together based on solid electrolyte (YSZ) and sensitive oxide electrode meets above requirement, for the application in automobile emission gas analyzer, be proved to be one equipment very reliably, and become the class new gas sensor got most of the attention.
Stabilizing zirconia base blendes together electric potential type NO
2the sensitive mechanism of sensor is: NO in atmosphere
2spread to three-phase reaction interface by sensitive electrode layer, due to react (1) in diffusion process, NO
2concentration can reduce gradually, the poriness of sensitive oxide electrode can determine NO
2the reduction degree of concentration.At the three phase boundary place of gas/sensitive electrode/YSZ, there is NO simultaneously
2electrochemical reducting reaction and the electrochemical oxidation reactions of oxygen, reaction (2) and (3) forms a local cell, when both reaction rates are equal, reaction reaches balance, sensitive electrode is formed and blendes together current potential, the potential difference (PD) of it and reference electrode is as the detection signal of sensor.Detection signal size is decided by the speed of electrochemical reaction (2) and (3), and reaction rate depends on the galvanochemistry of sensitive electrode material and chemical catalysis is active, electrode material micromechanism (poriness, granularity, pattern etc. of such as material).
Reaction equation is as follows:
NO
2→NO+1/2O
2(1)
NO
2+2e
-→NO+O
2-(2)
O
2-→1/2O
2+2e
-(3)
At present, in order to prepare the sensor of higher sensitivity characteristic, domestic and international most researchers is devoted to the research of sensitive electrode material.Such as, this seminar make with Cr
2o
3-WO
3for the YSZ base of sensitive electrode material blendes together electric potential type NO
2sensor is to 100ppm NO
2the potential value that blendes together be 52mV (Quan Diao, Chengguo Yin, Yingwei Liu, Jianguo Li, Xun Gong, Xishuang Liang, Shiqi Yang, Hong Chen, Geyu Lu, Mixed-potential-type NO
2sensor using stabilized zirconia and Cr
2o
3-WO
3nanocomposites, Sensor and Actuators B 180 (2013) 90-95).This type of NO
2the shortcoming of sensor is that response is low, insufficient sensitivity is high, does not reach practical requirement.In addition, because the pattern of electrode material can affect NO
2in the diffusion process of electrode layer, thus affecting the electrochemical reaction of gas at three phase boundary place, the sensitivity characteristic (sensitivity, response, selectivity, stability etc.) that the poriness sensitive electrode material that therefore exploitation has a special appearance improves sensor further has great importance.
Summary of the invention
The object of this invention is to provide a kind of based on graduation In
2o
3the YSZ base of sensitive electrode blendes together electric potential type NO
2sensor and preparation method, to improve NO
2sensor sensing performance, promotes practical in automobile emission gas analyzer field of this sensor.The sensor that the present invention obtains, except having high sensitivity, also has good selectivity, repeatability, stability.
NO involved in the present invention
2sensor is based on solid electrolyte YSZ and high electrochemical catalytic performance graduation In
2o
3novel NO constructed by sensitive electrode
2sensor, YSZ (Y
2o
3amount of substance doping ratio be the ZrO of 8%
2) as ion conductive layer.
One of the present invention is based on graduation In
2o
3the YSZ base of sensitive electrode blendes together electric potential type NO
2sensor, as shown in Figure 1, is characterized in that: successively by the Al with Pt heating electrode
2o
3ceramic wafer, YSZ substrate, reference electrode and sensitive electrode form; Reference electrode is strip Pt, and sensitive electrode is strip In
2o
3, two electrodes are separate and be prepared in the two ends of YSZ upper surface of base plate symmetrically, lower surface and the Al with fine strip shape Pt heating electrode of YSZ substrate
2o
3ceramic wafer is bonded together; Sensitive electrode material is by the In (NO of 1 ~ 2mmol
3)
34.5H
2o is dissolved in 30 ~ 60mL deionized water, stirs and makes it dissolve; Then 4 ~ 6mmol sucrose and 2.5 ~ 5mmol urea are joined In (NO
3)
3in solution, stir and make it dissolve; The mixed solution obtained is transferred in teflon reactor, after airtight, at 160 ~ 180 DEG C, react 12 ~ 18h, after reaction terminates, naturally cool to room temperature; In reactor product through centrifugal, washing, obtain prepolymer precipitation after drying, then sinter at 800 ~ 1200 DEG C and prepare for 2 ~ 4 hours.Wherein, as shown in Figure 3 a, classify In
2o
3be built by nanometer sheet with holes there is certain star topology, and nanometer sheet is made up of nano particle.
The present invention, using YSZ substrate as ion conductive layer, utilizes the In with high electrochemical catalytic activity
2o
3for sensitive electrode, changed the microscopic appearance of sensitive electrode material by different calcining heat (800 DEG C ~ 1200 DEG C), reach the object improving sensitivity characteristic.
One of the present invention is based on graduation In
2o
3the YSZ base of sensitive electrode blendes together electric potential type NO
2the preparation method of sensor, its step is as follows:
(1) Pt reference electrode is made: use Pt to starch the thick Pt reference electrode of making 15 ~ 20 μm in one end of YSZ upper surface of base plate, be bonded at after the doubling of a Pt silk on reference electrode centre position as contact conductor with Pt slurry simultaneously, then YSZ substrate is toasted 1 ~ 2 hour under 90 ~ 120 DEG C of conditions, again YSZ substrate is sintered 1 ~ 2 hour at 1000 ~ 1200 DEG C, get rid of the terpinol in Pt slurry, be finally down to room temperature;
(2) sensitive electrode is made: by aforementioned obtained sensitive electrode material deionized water furnishing slurry, mass concentration is 2 ~ 20%; Prepare 20 ~ 30 μm of thick sensitive electrodes with the slurry of sensitive electrode material at the other end of the YSZ upper surface of base plate with reference electrode symmetry, be bonded at after the doubling of a Pt silk on sensitive electrode as contact conductor with Pt slurry equally;
(3) the YSZ substrate of reference electrode and sensitive electrode above-mentioned preparation is had to sinter 1 ~ 3 hour at 800 ~ 1000 DEG C; Heating rate during preferred high temperature sintering is 1 ~ 2 DEG C/min;
(4) inorganic bond is prepared: measure water glass (Na
2siO
39H
2o) 2 ~ 4mL, and take Al
2o
3powder 0.7 ~ 1.0g, by the water glass that obtains and Al
2o
3powder mixes and stirs, obtained inorganic bond;
(5) use inorganic bond by the lower surface of YSZ substrate and the Al with Pt heating electrode
2o
3ceramic wafer is bonded together;
Wherein, with the Al of Pt heating electrode
2o
3ceramic wafer is at Al
2o
3ceramic wafer is obtained by serigraphy Pt, with the Al of Pt heating electrode
2o
3ceramic wafer together uses as the heating plate of device;
(6) device bonded is carried out welding, encapsulating, thus making obtains of the present invention with In
2o
3for the YSZ base of sensitive electrode blendes together Copper diethlydithiocarbamate.
Advantage of the present invention:
(1) sensor utilizes typical solid electrolyte---and stabilizing zirconia (YSZ), has good thermal stability and chemical stability, at high temperature (in vehicle exhaust) can detect NO
2.
(2) hydro-thermal method preparation graduation In is adopted
2o
3as sensor sensing electrode material, preparation method is simple, is beneficial to the suitability for industrialized production of mass.
(3) micromechanism of sensitive electrode material is optimized by changing different calcining heats (800 DEG C ~ 1200 DEG C), be beneficial to gas to be measured and arrive three phase boundary participation electrochemical reaction fast, reduce the consumption in diffusion process, thus make sensor have very high sensitivity.
Accompanying drawing explanation
Fig. 1: YSZ base of the present invention blendes together electric potential type NO
2the structural representation of sensor.
Each several part title: In
2o
3sensitive electrode 1, YSZ substrate 2, Pt reference electrode 3, Pt silk 4, Pt point 5, Al
2o
3ceramic wafer 6, Pt heating electrode 7, inorganic bond 8.
Fig. 2: the In prepared by the present invention
2o
3the XRD figure of sensitive electrode material.
As shown in Figure 2, be In
2o
3the XRD figure of sensitive electrode material, by contrasting with standard spectrogram, In prepared by the present invention
2o
3consistent with standard card JCPDS#65-3170, be cubic system In
2o
3.Show that sensitive electrode material prepared by the present invention is In
2o
3material.
Fig. 3: the SEM figure of the sensitive electrode material under the different calcining heats prepared by the present invention.
As shown in Figure 3, a:800 DEG C, b:1000 DEG C, the In of c:1200 DEG C of calcining
2o
3the SEM figure of sensitive electrode material, illustration is the enlarged drawing of regional area.As can be seen from the figure, along with the rising of calcining heat, the special appearance that material has fades away, grain size and duct size increase gradually, this shows, the sintering temperature changing sensitive material can change the microscopic appearance of sensitive electrode, and the poriness of electrode is beneficial to the diffusion of gas.
Fig. 4: sensor S800, S1000 and S1200 are to variable concentrations NO
2response log concentration curve.
As shown in Figure 4, the Electromotive Difference Of Potential Δ V of the device made by embodiment 1, embodiment 2 and embodiment 3 is with NO
2the change of concentration, as can be seen from the figure, Δ V and NO of three kinds of devices
2the logarithm of concentration all becomes good linear relationship, its slope is defined as the sensitivity of sensor, and the sensitivity of embodiment 1,2 and embodiment 3 is respectively 61,68 and 33mV/decade.As can be seen here, with the In of sintering at 1000 DEG C
2o
3ySZ base as sensitive electrode material blendes together electric potential type NO
2sensor S1000 has the highest sensitivity.
Fig. 5: with the In of sintering at 1000 DEG C
2o
3as the selectivity of the sensor S1000 of sensitive electrode material.
As shown in Figure 5, be the selectivity of sensor S1000, as can be seen from the figure, device is to NO
2with other gases co-existing gases sensitivity change less, as can be seen here, device is to NO
2there is good selectivity.
Fig. 6: sensor S1000 is to NO
2long-time stability.
As shown in Figure 6, for sensor S1000 at the test period of 30 days to 100ppm and 200ppm NO
2stability, as can be seen from the figure, device is to NO
2show good long-time stability.
Embodiment
Embodiment 1:
In is prepared by hydro-thermal method
2o
3material, by In
2o
3make YSZ base as sensitive electrode material and blend together electric potential type NO
2sensor, and testing sensor air-sensitive performance, detailed process is as follows:
1. make Pt reference electrode: using in one end of the YSZ upper surface of base plate of length and width 2 × 2mm, thickness 0.2mm Pt slurry to make one deck 0.5mm × 2mm size, 15 μm of thick Pt reference electrodes, going between with being bonded at extraction electrode on reference electrode centre position with Pt slurry after the doubling of a Pt silk simultaneously; Then YSZ substrate is toasted 1.5 hours under 100 DEG C of conditions, then YSZ substrate is sintered 1.5 hours at 1000 DEG C, thus get rid of the terpinol in platinum slurry, be finally down to room temperature.
2. make In
2o
3sensitive electrode: first prepare In by hydro-thermal method
2o
3material.By the In (NO of 1mmol
3)
34.5H
2o is dissolved in 30mL deionized water, stirs and makes it dissolve; Then 4mmol sucrose and 2.5mmol urea are joined In (NO
3)
3in solution, stir and make it dissolve; Transferred to by the mixed solution obtained in teflon reactor, sealing is closely placed in 160 DEG C of baking ovens and reacts 12h, naturally cools to room temperature after reaction terminates.Prepolymer precipitation is obtained through centrifugal, washing drying.Finally by obtain be deposited in 800 DEG C at sintering 2 hours, heating rate 2 DEG C/min, thus obtain In
2o
3sensitive electrode material.
Get 5mg In
2o
3powder deionized water 100mg furnishing slurry, by In
2o
3slurry applies one deck 0.5mm × 2mm size, 20 μm of thick sensitive electrodes at the other end of the YSZ upper surface of base plate with reference electrode symmetry, goes between with being bonded at extraction electrode on sensitive electrode with Pt slurry after a platinum filament doubling equally.
The YSZ substrate with reference electrode and sensitive electrode made is warming up to 800 DEG C with the heating rate of 2 DEG C/min and is down to room temperature after keeping 2h.
3. bonding has the ceramic wafer of heating electrode.Use inorganic bond (Al
2o
3with water glass Na
2siO
39H
2o, quality is about than 5:1 preparation) by the lower surface (side of uncoated electrode) of YSZ substrate and the Al with Pt heating electrode of same size
2o
3ceramic wafer (length and width 2 × 2mm, thickness 0.2mm) bonds;
4. device welding, encapsulation.Device is welded on hexagonal base, puts protective cover, complete and blend together electric potential type NO
2sensor, is labeled as sensor S800.
Embodiment 2:
With the In of 1200 DEG C of sintering
2o
3material, as sensitive electrode material, makes NO
2sensor, its manufacturing process is:
By the In prepared by preceding method
2o
3in muffle furnace, 1200 DEG C of sintering obtain sensitive electrode material In
2o
3(1200 DEG C), device fabrication processes is identical with embodiment 1, is labeled as sensor S1200.
Embodiment 3:
With the In of 1000 DEG C of sintering
2o
3material, as sensitive electrode material, makes NO
2sensor, its manufacturing process is:
By the In prepared by preceding method
2o
3in muffle furnace, 1000 DEG C of sintering obtain sensitive electrode material In
2o
3(1000 DEG C), device fabrication processes is identical with embodiment 1, is labeled as sensor S1000.
Sensor is connected on Rigol signal tester, sensor is placed in air, 5ppm NO respectively
2, 10ppm NO
2, 20ppm NO
2, 50ppm NO
2, 100ppm NO
2, 200ppm NO
2, 300ppm NO
2atmosphere in carry out voltage signal test.
List in table 1 respectively with In
2o
3 (800 DEG C), In
2o
3 (1000 DEG C)and In
2o
3 (1200 DEG C)the YSZ base made for sensitive electrode material blendes together Copper diethlydithiocarbamate at variable concentrations NO
2electromotive force in atmosphere and in the difference of the heavy electromotive force of air with NO
2the changing value of concentration.Can see from table, three kinds of devices are all to NO
2have good response characteristic, wherein the sensitivity (slope) of device S1000 is the highest, is 68mV/decade, is greater than the 61mV/decade of device S800 and the 33mV/decade of device S1200.And device S1000 is to each concentration NO
2response all maximum, show the highest sensitivity.As can be seen here, there is the graduation In of special appearance
2o
3the device that sensitive electrode material is constructed is to NO
2there is good sensitivity characteristic, change the active and poriness of the electrochemical catalysis of sensitive material by the sintering temperature changing sensitive electrode material, thus the electrode reaction efficiency improving sensor obtains and has highly sensitive YSZ base and blend together electric potential type NO
2sensor.
Table 1 is respectively with In
2o
3(800 DEG C), In
2o
3(1000 DEG C) and In
2o
3the Δ V of sensor S800, S1000 and S1200 that (1200 DEG C) are sensitive electrode material is with NO
2the change of concentration
Claims (4)
1. one kind based on graduation In
2o
3the YSZ base of sensitive electrode blendes together electric potential type NO
2sensor, is characterized in that: successively by the Al with Pt heating electrode
2o
3ceramic wafer, YSZ substrate, reference electrode and sensitive electrode form; Reference electrode is strip Pt, and sensitive electrode is strip In
2o
3, two electrodes are separate and be prepared in the two ends of YSZ upper surface of base plate symmetrically, lower surface and the Al with fine strip shape Pt heating electrode of YSZ substrate
2o
3ceramic wafer is bonded together; Sensitive electrode material is by the In (NO of 1 ~ 2mmol
3)
34.5H
2o is dissolved in 30 ~ 60mL deionized water, stirs and makes it dissolve; Then 4 ~ 6mmol sucrose and 2.5 ~ 5mmol urea are joined In (NO
3)
3in solution, stir and make it dissolve; The mixed solution obtained is transferred in teflon reactor, after airtight, at 160 ~ 180 DEG C, react 12 ~ 18h, after reaction terminates, naturally cool to room temperature; In reactor product through centrifugal, washing, obtain prepolymer precipitation after drying, then sinter at 800 ~ 1200 DEG C and prepare for 2 ~ 4 hours.
2. one according to claim 1 is based on graduation In
2o
3the YSZ base of sensitive electrode blendes together electric potential type NO
2the preparation method of sensor, its step is as follows:
(1) Pt reference electrode is made: use Pt to starch the thick Pt reference electrode of making 15 ~ 20 μm in one end of YSZ upper surface of base plate, be bonded at after the doubling of a Pt silk on reference electrode centre position as contact conductor with Pt slurry simultaneously, then YSZ substrate is toasted 1 ~ 2 hour under 90 ~ 120 DEG C of conditions, again YSZ substrate is sintered 1 ~ 2 hour at 1000 ~ 1200 DEG C, get rid of the terpinol in Pt slurry, be finally down to room temperature;
(2) sensitive electrode is made: by aforementioned obtained sensitive electrode material deionized water furnishing slurry, mass concentration is 2 ~ 20%; Prepare 20 ~ 30 μm of thick sensitive electrodes with the slurry of sensitive electrode material at the other end of the YSZ upper surface of base plate with reference electrode symmetry, be also bonded at after the doubling of a Pt silk on sensitive electrode as contact conductor with Pt slurry equally;
(3) the YSZ substrate of reference electrode and sensitive electrode above-mentioned preparation is had to sinter 1 ~ 3 hour at 800 ~ 1000 DEG C;
(4) use inorganic bond by the lower surface of YSZ substrate and the Al with Pt heating electrode
2o
3ceramic wafer is bonded together;
(5) device bonded is carried out welding, encapsulating, thus prepare based on graduation In
2o
3the YSZ base of sensitive electrode blendes together electric potential type NO
2sensor.
3. as claimed in claim 2 a kind of based on graduation In
2o
3the YSZ base of sensitive electrode blendes together electric potential type NO
2the preparation method of sensor, is characterized in that: measure water glass Na
2siO
39H
2o 2 ~ 4mL, and take Al
2o
3powder 0.7 ~ 1.0g, by the water glass that obtains and Al
2o
3powder mixes and stirs, and namely prepares inorganic bond.
4. as claimed in claim 2 a kind of based on graduation In
2o
3the YSZ base of sensitive electrode blendes together electric potential type NO
2the preparation method of sensor, is characterized in that: with the Al of Pt heating electrode
2o
3ceramic wafer is at Al
2o
3ceramic wafer is obtained by serigraphy Pt.
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