CN104897763A - Nitrogen-oxygen sensor and tail gas NOx content measurement method - Google Patents
Nitrogen-oxygen sensor and tail gas NOx content measurement method Download PDFInfo
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Abstract
The invention discloses a nitrogen-oxygen sensor and a tail gas NOx content measurement method. The nitrogen-oxygen sensor comprises a first substrate, a second substrate, a third substrate, a forth substrate, a fifth substrate, a sixth substrate, a seventh substrate, an eighth substrate and a ninth substrate. A circular main electrode is arranged on the upper surface of the first substrate, the first substrate contains a first diffusion barrier layer, an oxygen determination chamber is arranged in the second substrate, a circular oxygen determination electrode is arranged in the oxygen determination chamber, a second diffusion barrier layer is arranged in the third substrate, the forth substrate comprises a reduction chamber, a comparison electrode and a measurement electrode are arranged in the reduction chamber, the fifth substrate comprises a reference chamber, a reference electrode is arranged in the reference chamber, and a heating electrode is arranged between the seventh substrate and the eighth substrate. The method reduces time of gas diffusion into the measurement chamber, improves nitrogen-oxygen sensor response time and has the advantages of simple processes, production easiness, low production cost and long service life.
Description
Technical field
The invention belongs to sensor technical field, more specifically, relate to a kind of nitrogen oxide sensor and measure the method for NOx content in tail gas.
Background technology
The tail gas of motor vehicle emission has become the main source of air NOx pollutant, due to the raising of national exhaust emission standard, need to detect in real time the NOx discharge in tail gas and process, and nitrogen oxide sensor is one of core component in this detection system.
Traditional nitrogen oxide sensor is schistose texture, and adopt multilayer zirconia ceramics sheet to be formed by stacking, combined by electrochemical layer and zone of heating, electrochemical layer mainly completes a series of galvanochemistry and cartalytic decomposition effect, to realize the measurement to NOx gas; Zone of heating mainly to nitrogen oxide sensor heating, makes it to reach the temperature needed for electrochemical layer galvanochemistry and catalytic reaction.The electrode of traditional nitrogen oxide sensor adopts the metal material Au to oxynitrides almost catalytically inactive.Nitrogen oxide sensor chip is in course of normal operation, and the heating electrode temperatures as high of zone of heating 1000 DEG C, very close to the fusing point 1064 DEG C of Au, affect the heating effect of nitrogen oxide sensor, therefore adopt traditional Au as electrode, effect is unsatisfactory.
Containing multiple chamber in its inner structure of traditional nitrogen oxide sensor, manufacturing process is complicated, and decreases the contact area of two zirconia ceramics sheets around chamber, reduces the structural strength of the nitrogen oxide sensor head at chamber place.
Internal electrode many employings rectangle structure of traditional nitrogen oxide sensor, easily there is the phenomenon that stress is concentrated in the sharp corner in process near nitrogen oxide sensor internal electrode, so nitrogen oxide sensor in the course of the work, extremely easily there is problems of crack in the sharp corner near its internal electrode, greatly reduces the serviceable life of nitrogen oxide sensor.
The decomposition of potential electrode to NOx of traditional nitrogen oxide sensor is slower, therefore the NOx concentration difference inside and outside nitrogen oxide sensor is not very large, NOx diffuses into reduction chamber speed from outside is comparatively slow, then the electric current of NOx decomposition generation is less, and sensitivity is not high.
Summary of the invention
For the defect of prior art, the object of the present invention is to provide a kind of nitrogen oxide sensor, be intended to solve the material due to traditional nitrogen oxide sensor internal chamber structure and potential electrode and heating electrode of the prior art and shape, cause nitrogen oxide sensor manufacturing process complicated, head strength is lower, ate electrode goes out easily existing cracking, and heating electrode heating effect is not good enough, the technical matters that sensitivity is not high.
The invention provides a kind of nitrogen oxide sensor, comprise laminate successively from top to bottom ground floor substrate, second layer substrate, third layer substrate, the 4th layer of substrate, layer 5 substrate, layer 6 substrate, layer 7 substrate, the 8th layer of substrate and the 9th layer of substrate; The upper surface of described ground floor substrate is provided with the central electrode of annular, and includes the first diffusion barrier layer in described ground floor substrate, and vehicle exhaust enters nitrogen oxide sensor by described first diffusion barrier layer; Be provided with in described second layer substrate and tubularly determine oxygen chamber, describedly determine to be provided with annular in oxygen chamber and determine oxygen electrode; The second diffusion barrier layer is included in described third layer substrate; Include tubular reduction chamber in described 4th layer of substrate, be provided with in described reduction chamber and compare electrode and potential electrode; Comprise with reference to chamber in described layer 5 substrate, described is the reference gas channel be connected with air with reference to chamber, and described reference cavity indoor are provided with reference electrode; Heating electrode is provided with between described layer 7 substrate and described 8th layer of substrate.
Further, the material of described central electrode is to the metallic ceramics of NOx compound without catalytic action.
Further, described metallic ceramics is made up of Pt, YSZ (yttria-stabilized zirconia).
Further, the material of described first diffusion barrier layer is the mixing of aluminium oxide and graphite, and the percent by volume of graphite is 5% ~ 25%Vol, because graphite can be sintered in nitrogen oxide sensor manufacturing process, therefore diffusion barrier has certain hole, allows gas to pass through.
Further, the material of described heating electrode is platinum.
Further, the material of described potential electrode is the compound substance be made up of NiO, CuO and YSZ, and in described compound substance, the percent by volume of YSZ is the percent by volume of 5% ~ 30%Vol, CuO is 7% ~ 38%Vol.
Further, described potential electrode is attached with an overlayer, described tectal material is the crystalline substance point stone containing Mn element 0% ~ 10%Vol.
Present invention also offers a kind of method measuring NOx content in tail gas based on above-mentioned nitrogen oxide sensor, comprise the steps:
(1) by described heating electrode, nitrogen oxide sensor is heated, the oxygen in each chamber of nitrogen oxide sensor is pumped from each chamber interior with the form of oxonium ion; When gas to be measured by the first diffusion barrier layer enter determine oxygen chamber time, by central electrode with determine to apply main pump voltage between oxygen electrode, make to determine the oxygen in oxygen chamber and pump with the form of oxonium ion; Remaining gas enters reduction chamber through the second diffusion barrier layer, by regulating main pump voltage, control the pump output of determining oxygen in oxygen chamber, make reference voltage Vc remain on about 450mv, thus make the oxygen concentration of reducing in chamber remain on the level of 1 ~ 5ppm; By applying the voltage of-2v ~+2v between potential electrode and central electrode, the O2 decomposing out constantly being pumped, producing pump electric current I p1;
(2) pump electric current I p1 is gathered;
(3) content of NOx in gas to be measured is obtained according to described pump electric current I p1.
Wherein, main pump voltage is-2v ~+2v.
Wherein, step S3 is specially: be pump electric current I p1 under the NOx condition of 1000ppm ~ 3000ppm by measuring NOx that concentration is 0ppm and full journey respectively, the proportionate relationship between the content of different N Ox and pump electric current I p1 can be drawn, thus the content of NOx can be obtained according to any current value Ip1 recorded.
The present invention can realize following technique effect: (1) structurally nitrogen oxide sensor inside of the present invention only has altogether 3 chambers, and 5 chambers of traditional nitrogen oxide sensor of comparing reduce by 2 chambers.Due to the minimizing that chamber takes up space, which increases the contact area between the zirconia ceramics substrate around chamber, improve the structural strength of the nitrogen oxide sensor head at chamber place.In addition the present invention also simplify the structure of nitrogen oxide sensor, thus makes the manufacture craft of whole nitrogen oxide sensor become more simple, is easy to produce, and reduces production cost.(2) in the present invention, the determining oxygen chamber and measure chamber of nitrogen oxide sensor is right cylinder, central electrode, potential electrode, compares electrode and is annular.Compared to rectangular parallelepiped chamber and the rectangular electrodes of traditional nitrogen oxide sensor, the wedge angle of inside of the present invention all adopts circular arc excessive, and the stress significantly reducing sensor internal is concentrated, and greatly reduces the possibility of its internal cleavage, thus improves its serviceable life.(3) in the present invention, heating electrode is metal platinum, and the fusing point of platinum is 1772 DEG C, and far above heating-up temperature 1000 DEG C, being compared to metallic gold is electrode, and can't appear at the problem such as hardness decline, volatilization in heating process, its heating effect is good.(4), in the present invention, potential electrode is made up of the compound substance of NiO, CuO and YSZ.In compound substance, the percent by volume of YSZ is the percent by volume of 5% ~ 30%Vol, CuO is 7% ~ 38%Vol.Potential electrode has an overlayer, tectal material is the crystalline substance point stone containing Mn element 0% ~ 10%Vol.Compared to traditional nitrogen oxide sensor potential electrode material, this material can improve the decomposition rate of NOx in potential electrode, thus make the concentration of the NOx of reduction chamber lower, the NOx accelerating determine oxygen chamber diffuses into reduction chamber, and then the NOx of acceleration nitrogen oxide sensor outside diffuses into and determines oxygen chamber.Due to diffuse faster, then decompose by NOx the electric current produced and increase, and then increase the sensitivity of NOx measurement.
Accompanying drawing explanation
Fig. 1 is the cross section view of the nitrogen oxide sensor that the embodiment of the present invention provides.
Fig. 2 is the three-dimensional structure view of the nitrogen oxide sensor that the embodiment of the present invention provides.
Fig. 3 is the nitrogen oxide sensor schematic diagram that the embodiment of the present invention provides.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Nitrogen oxide sensor provided by the invention can measure the content of NOx in tail gas, is applicable to the measurement of nitrogen oxide in automobile exhaust gas.Fig. 1 shows the cross section view of the nitrogen oxide sensor that the embodiment of the present invention provides, for convenience of explanation, illustrate only the part relevant to the embodiment of the present invention, details are as follows: nitrogen oxide sensor provided by the invention is formed by zirconia ceramics substrate layer is folded, comprises ground floor substrate, second layer substrate, third layer substrate, the 4th layer of substrate, layer 5 substrate, layer 6 substrate, layer 7 substrate, the 8th layer of substrate and the 9th layer of substrate laminate from top to bottom successively.Ground floor substrate upper surface is provided with annular central electrode 1, includes the first diffusion barrier layer 2 in ground floor substrate, and vehicle exhaust enters nitrogen oxide sensor by this diffusion barrier layer 2; Be provided with certain oxygen chamber 4 in second layer substrate, determine in oxygen chamber 4, to be provided with annular and determine oxygen electrode 3; The second diffusion barrier layer 5 is included in third layer substrate; Include reduction chamber 7 in 4th layer of substrate, be provided with in reduction chamber 7 and compare electrode 6 and potential electrode 8; Comprising with reference to chamber 10 in layer 5 substrate, is the reference gas channels be connected with air with reference to chamber 10, is provided with reference electrode with reference in chamber 10; Heating electrode is included between layer 7 and the 8th layer of substrate.
In embodiments of the present invention; central electrode 1 can be to the metallic ceramics of NOx compound without catalytic action with the material comparing electrode 6; mainly be made up of Pt, YSZ (yttria-stabilized zirconia); central electrode 1 outside surface covers layer protective layer, and the material of protective seam can be aluminium oxide.
In embodiments of the present invention, the material spreading barrier layer (2,5) can be the aluminium oxide having certain porosity.
In embodiments of the present invention, the material of potential electrode can be platinum rhodium and YSZ (yttria-stabilized zirconia), responsive to the oxynitrides in vehicle exhaust.
As one embodiment of the present of invention, the upper and lower surface of zone of heating is all coated with insulation course.Heating electrode material can be platinum.
As one embodiment of the present of invention, the material of insulation course can be fine and close aluminium oxide.
Beneficial effect of the present invention is specifically: structurally nitrogen oxide sensor inside of the present invention only has altogether 3 chambers, and 5 chambers of traditional nitrogen oxide sensor of comparing, reduce by 2 chambers.Gas in such tail gas directly can be entered by diffusion barrier determines oxygen chamber, accelerates gas and is diffused into the time of measuring chamber, thus improve the response time of nitrogen oxide sensor.In addition the present invention also simplify the structure of nitrogen oxide sensor, thus makes the manufacture craft of whole nitrogen oxide sensor become more simple, is easy to produce, and reduces production cost.
In the present invention, the determining oxygen chamber and measure chamber of nitrogen oxide sensor is right cylinder, central electrode, potential electrode, compares electrode and is annular.Compared to rectangular parallelepiped chamber and the rectangular electrodes of traditional nitrogen oxide sensor, the wedge angle of inside of the present invention all adopts circular arc excessive, and the stress significantly reducing sensor internal is concentrated, and greatly reduces the possibility of its internal cleavage, thus improves its serviceable life.
In the embodiment of the present invention, heating electrode can be metal platinum, and the fusing point of platinum is 1772 DEG C, and far above heating-up temperature 1000 DEG C, being compared to metallic gold is electrode, and can't appear at the problem such as hardness decline, volatilization in heating process, its heating effect is good.
In order to the nitrogen oxide sensor that the further description embodiment of the present invention provides, existing details are as follows by reference to the accompanying drawings:
Fig. 1 is the NOx sensor section of structure of the embodiment of the present invention.As shown in Figure 1, nitrogen oxide sensor of the present invention is formed by nine layers of zirconia ceramics substrate layer are folded.Ground floor substrate upper surface is provided with central electrode 1, includes the first diffusion barrier layer 2 in ground floor substrate, and vehicle exhaust enters nitrogen oxide sensor by this diffusion barrier layer; Be provided with certain oxygen chamber 4 in second layer substrate, determine to be provided with in oxygen chamber to determine oxygen electrode 3; The second diffusion barrier layer 5 is included in third layer substrate; Include reduction chamber 7 in 4th layer of substrate, be provided with in reduction chamber 7 and compare electrode 6 and potential electrode 8; Comprising with reference to chamber 10 in layer 5 substrate, is the reference gas channels be connected with air with reference to chamber 10, is provided with reference electrode 9 with reference in chamber 10; Heating electrode 11 is included between layer 7 and the 8th layer of substrate.
In embodiments of the present invention; central electrode and to compare the material that electrode is all be to the metallic ceramics of NOx compound without catalytic action; mainly be made up of Pt, YSZ (yttria-stabilized zirconia), central electrode outside surface covers layer protective layer, and material is aluminium oxide.The material of diffusion barrier layer has certain porosity alumina.The material of potential electrode is made up of the compound substance of NiO, CuO and YSZ.In compound substance, the percent by volume of YSZ is the percent by volume of 5% ~ 30%Vol, CuO is 7% ~ 38%Vol.Potential electrode has an overlayer, tectal material is the crystalline substance point stone containing Mn element 0% ~ 10%Vol.Zone of heating upper and lower surface is all coated with insulation course.The material of insulation course is fine and close aluminium oxide.Heating electrode material is platinum.Accurately to record NOx content in gas just must first the oxygen of nitrogen oxide sensor internal chamber be discharged, remove the interference that there is oxygen in gas Central Plains, then by measuring the O2 content that NOx decomposes out, calculating the content of the NOx in gas, namely completing the measurement of nitrogen oxide sensor to NOx gas.During measurement, by heating electrode 11 pairs of nitrogen oxide sensor heating, utilize the electrolyte characteristics that zirconia ceramics at high temperature presents, oxygen can be made to pump from nitrogen oxide sensor chamber interior with the form of oxonium ion.
As shown in Figure 3, the electrode of nitrogen oxide sensor inside forms four loops.Wherein compare electrode 6 and reference electrode 9 forms the first loop, poor with the oxygen concentration with reference to chamber 10 for measuring reduction chamber 7;
Central electrode 1 and determine oxygen electrode 3 and form second servo loop, controls the pump oxygen amount of determine oxygen chamber, make the oxygen concentration of determining oxygen chamber 4 and reducing chamber 7 at 1 ~ 5ppm, thus the guarantee voltage compared between electrode 6 and reference electrode 9 is about 450mv.
Potential electrode 8 and central electrode 1 form tertiary circuit, for measuring the content of the NOx decomposed in potential electrode 8, the content of the NOx namely in gas.
Heating electrode 11 forms the 4th loop, for being nitrogen oxide sensor heating heating, thus acquisition zirconia ceramics electrolyte characteristics at high temperature, oxygen is pumped with the form of oxonium ion.
During measurement, nitrogen oxide sensor is heated between 600 DEG C to 800 DEG C by heating electrode 11, and gas is entered is determined oxygen chamber 4 by the first diffusion barrier layer 2, central electrode 1 and determine to apply a main pump voltage between oxygen electrode 3, oxygen can be pumped from nitrogen oxide sensor inside.This main pump voltage is determined by the reference voltage Vc compared between electrode 6 and reference electrode 9.
Remaining gas enters reduction chamber 7 through the second diffusion barrier layer 5.Reference electrode one end is placed in air, reference electrode and compare between electrode exist a reference voltage Vc (this electric potential signal meets Nernst equation) determined by the difference in oxygen concentration of electrode place atmosphere.
Zirconia composition solid electrolyte in, can this spy (Nernst) equation be used for calculate electrolyte two ends due to oxygen concentration look into difference produce electromotive force.
Wherein, R is ideal gas constant; T is temperature; N is the electron transfer number of reaction equation; F is Faraday constant; Po is oxygen concentration in air, and p is reduction chamber oxygen concentration; At a certain temperature (600 ~ 800 DEG C), the oxygen concentration difference that air is different from reduction chamber just has a corresponding electromotive force and exports.
By regulating main pump voltage, control the pump output of determining oxygen in oxygen chamber 4, reference voltage Vc is made to remain on about 450mv, reference electrode and the difference in oxygen concentration comparing electrode place atmosphere can be ensured, thus ensure that the oxygen concentration in reduction chamber 7 remains on very little level (in 1 ~ 5PPM rank).
The material that potential electrode 8 in reduction chamber 7 adopts is the material to NOx sensitivity.In potential electrode 8, high temperature and catalyzer can allow NOx resolve into N2 and O2, an appropriate voltage is added between potential electrode 8 and central electrode 1, the O2 decomposed out is constantly pumped, produce pump electric current I p1, calculating the content of the NOx in gas by measuring pump current value Ip1, namely completing the measurement of nitrogen oxide sensor to NOx gas.In gas the content of NOx and the pump electric current I p1 of generation linearly proportional, be demarcate pump electric current I p1 value under the condition of the NOx of NOx and 2000ppm of 0ppm by measuring concentration respectively, the proportionate relationship between the content of NOx and the pump electric current I p1 of generation can be drawn, thus the content of NOx can be calculated according to any current value Ip1 value recorded.
Those skilled in the art will readily understand; the foregoing is only preferred embodiment of the present invention; not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a nitrogen oxide sensor, is characterized in that, comprise laminate successively from top to bottom ground floor substrate, second layer substrate, third layer substrate, the 4th layer of substrate, layer 5 substrate, layer 6 substrate, layer 7 substrate, the 8th layer of substrate and the 9th layer of substrate;
The upper surface of described ground floor substrate is provided with the central electrode (1) of annular, and in described ground floor substrate, including the first diffusion barrier layer (2), vehicle exhaust enters nitrogen oxide sensor by described first diffusion barrier layer (2);
Be provided with in described second layer substrate and tubularly determine oxygen chamber (4), describedly determine in oxygen chamber (4), to be provided with annular and determine oxygen electrode (3);
The second diffusion barrier layer (5) is included in described third layer substrate;
Include tubular reduction chamber (7) in described 4th layer of substrate, be provided with in described reduction chamber (7) and compare electrode (6) and potential electrode (8);
Comprise with reference to chamber (10) in described layer 5 substrate, described is the reference gas channel be connected with air with reference to chamber (10), is provided with reference electrode in described reference chamber (10);
Heating electrode is provided with between described layer 7 substrate and described 8th layer of substrate.
2. nitrogen oxide sensor as claimed in claim 1, it is characterized in that, the material of described central electrode (1) is to the metallic ceramics of NOx compound without catalytic action.
3. nitrogen oxide sensor as claimed in claim 2, it is characterized in that, described metallic ceramics is made up of Pt and YSZ.
4. nitrogen oxide sensor as claimed in claim 1, it is characterized in that, the material of described first diffusion barrier layer (2) is the potpourri of aluminium oxide and graphite, the percent by volume of graphite is 5% ~ 25%Vol, because graphite can be sintered in nitrogen oxide sensor manufacturing process, therefore diffusion barrier has certain hole, allows gas to pass through.
5. nitrogen oxide sensor as claimed in claim 1, it is characterized in that, the material of described heating electrode is platinum.
6. nitrogen oxide sensor as claimed in claim 1, it is characterized in that, the material of described potential electrode (8) is the compound substance be made up of NiO, CuO and YSZ, and in described compound substance, the percent by volume of YSZ is the percent by volume of 5% ~ 30%Vol, CuO is 7% ~ 38%Vol.
7. the nitrogen oxide sensor as described in claim 1 or 6, is characterized in that, described potential electrode is attached with an overlayer, and described tectal material is the crystalline substance point stone containing Mn element 0% ~ 10%Vol.
8. measure a method for NOx content in tail gas based on the nitrogen oxide sensor described in any one of claim 1-7, it is characterized in that, comprise the steps:
S1: heated nitrogen oxide sensor by described heating electrode, makes the oxygen in each chamber of nitrogen oxide sensor pump from each chamber interior with the form of oxonium ion; When gas to be measured by first diffusion barrier layer (2) enter determine oxygen chamber (4) time, by in central electrode (1) with determine to apply main pump voltage between oxygen electrode (3), the oxygen determined in oxygen chamber (4) is pumped with the form of oxonium ion; Remaining gas enters reduction chamber (7) through the second diffusion barrier layer (5), by regulating main pump voltage, control the pump output of determining oxygen in oxygen chamber (4), make reference voltage Vc remain on about 450mv, thus make the oxygen concentration of reducing in chamber (7) remain on the level of 1 ~ 5ppm; By applying the voltage of-2v ~+2v between potential electrode (8) and central electrode (1), the O2 decomposing out constantly being pumped, producing pump electric current I p1;
S2: gather pump electric current I p1;
S3: the content obtaining NOx in gas to be measured according to described pump electric current I p1.
9. method as claimed in claim 8, it is characterized in that, described main pump voltage is-2v ~+2v.
10. method as claimed in claim 8, it is characterized in that, step S3 is specially: be pump electric current I p1 under the NOx condition of 1000ppm ~ 3000ppm by measuring NOx that concentration is 0ppm and full journey respectively, the proportionate relationship between the content of different N Ox and pump electric current I p1 can be drawn, thus the content of NOx can be obtained according to any current value Ip1 recorded.
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| CN107328837A (en) * | 2017-07-24 | 2017-11-07 | 深圳安培龙科技股份有限公司 | A kind of structure improved nitrogen oxide sensor |
| CN108872482A (en) * | 2018-06-22 | 2018-11-23 | 西安创联电气科技（集团）有限责任公司 | A kind of diaphragm of nitrogen oxide sensor ceramic chip |
| CN109298057A (en) * | 2018-09-03 | 2019-02-01 | 上海长园维安电子线路保护有限公司 | A kind of nitrogen oxide sensor ceramic chip |
| CN109375513A (en) * | 2018-11-28 | 2019-02-22 | 华中科技大学 | A kind of nitrogen oxide sensor control system |
| CN109507262A (en) * | 2018-11-21 | 2019-03-22 | 温州百岸汽车零部件有限公司 | A kind of NOx sensor chip pumping current adjustment |
| CN110907522A (en) * | 2019-12-03 | 2020-03-24 | 湖北丹瑞新材料科技有限公司 | Method for improving measurement precision of nitrogen-oxygen sensor |
| CN112198206A (en) * | 2020-09-21 | 2021-01-08 | 苏州禾苏传感器科技有限公司 | Electrochemical gas sensor chip |
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| CN107328837A (en) * | 2017-07-24 | 2017-11-07 | 深圳安培龙科技股份有限公司 | A kind of structure improved nitrogen oxide sensor |
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| CN110907522A (en) * | 2019-12-03 | 2020-03-24 | 湖北丹瑞新材料科技有限公司 | Method for improving measurement precision of nitrogen-oxygen sensor |
| CN112198206A (en) * | 2020-09-21 | 2021-01-08 | 苏州禾苏传感器科技有限公司 | Electrochemical gas sensor chip |
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