CN106841358B - A kind of sulfurated hydrogen detection sensor and its manufacturing method - Google Patents
A kind of sulfurated hydrogen detection sensor and its manufacturing method Download PDFInfo
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Abstract
The present invention relates in sensor field a kind of sulfurated hydrogen detection sensor and its manufacturing method, sensor include the top substrate layer being mutually bonded and underlying substrate；Top substrate layer is equipped with several honeycomb holes through top substrate layer, and the upper surface of top substrate layer is coated with Na3Zr2Si2PO12The spray coating that material is formed, spray coating upper surface is embedded with spun gold net, one upper side of spun gold net is equipped with strip Au reference electrode, the working electrode of strip is equipped with above the other side of spun gold net, Pt lead is drawn to substrate outside respectively between spun gold net and reference electrode, between spun gold net and working electrode, working electrode is by CoNi0.6Cr0.8Mn1.6O5Material spraying is online in spun gold and is made.Quickly, detection accuracy is good, and has anti-jamming effectiveness for sensor response speed.
Description
Technical field
The present invention relates to a kind of gas content detection sensor and its manufacturing method, in particular to hydrogen sulfide gas content
Detection sensor and its manufacturing method, belong to sensor technical field.
Background technique
In the prior art, there is a kind of hydrogen sulfide sensing detection equipment, including hydrogen sulfide sensor acquires equipment, and therewith
The amplifying circuit and filter circuit of connection, the filter circuit output end connect main control chip；There is AD conversion in main control chip
Circuit, digital filtering module, concentration curve temperature compensation module, Concentration Algorithm parsing module and serial communication cache module；It is main
Control the interior also Pulse width modulation module of chip；Concentration parsing module is bi-directionally connected with EEPROM data accumulating module；Master control core
Piece is also bi-directionally connected with serial communication module and input/output module respectively.The device is by filtering and amplifying circuit, A/D converter circuit
With control processing integrated chip in one, is realized by data accumulating module and save hydrogen sulfide gas algorithm data, by serial
Interface is used for developer, has good versatility and portability.Disadvantage is that: the program fails to disclose how to obtain
Obtain highly sensitive sensor.
A kind of hydrogen sulfide electrochemical transducer of 102621205 A of Publication No. CN, including by acidic electrolysis bath formed from
The working electrode of son conducting, reference electrode and to electrode, working electrode is containing reference electrode, and working electrode is relative to reference electrode
Current potential within the scope of ± 40mV, reference electrode is to alcohols without adsorption electrode, wherein the reference electrode be selected from carbon carry ruthenium electricity
Pole, carbon carry rhodium electrode, graphite electrode, carbon supported noble metal oxide electrode, pallium-on-carbon and close reference electrode, Publication No. US 2010/
A kind of good hydrogen sulfide sensor of selectivity is given in 0012494 U.S. Patent application, by molten containing transition metal salt
Intermediary's electrolyte system of liquid reaches and improves H2The purpose of S selectivity.The sensor also has methanol, ethyl alcohol preferable anti-dry
Immunity.But this sensor is approximately 0.2uA/ppm, H to the interference value of methanol2The sensitivity of S is 3uA/ppm, and anti-with alcohols
Concentration when freezing agent, hand cleanser is all larger, usually percent concentration, by taking second methanol 2% as an example, then being equivalent to H2S's is dense
Degree is 1333ppm, will cause false alarm.Meanwhile the sensor is with intermediary's electrolyte system, electrolyte system is more multiple
It is miscellaneous, and be consumption-type electrolyte, there is certain capacity service life.
United States Patent (USP) US7615139B2 gives a kind of sensor, partially covered with guard electrode reference electrode to
Allow reference electrode that there is stable current potential.But alcohols is a kind of and the enough substances to mix mutually of water energy, if the concentration of alcohols
Bigger, e.g. percent concentration is diffused into reference electricity by electrolyte then alcohols still is possible to incomplete reaction again
Pole, so as to cause reference potential drift.And such device is four electrode systems, electrode system and circuit structure are more complicated.
In addition, in H2S is detected in environment, often there is the presence of CO interference gas.The beauty of Patent No. US4042464
State's patent gives a kind of sensor, is worked electrode with Au/C, does reference electrode with Pt, have lesser interference to CO, but
It is that the sensor but has very big interference to methanol, and cannot restore the performance of sensor for a long time.
Therefore, it is necessary to the interference of a kind of not only anti-alcohols, but also the H of anti-CO interference2S sensor.Lack in the prior art in this way
Technical solution.
Summary of the invention
The object of the present invention is to provide a kind of sulfurated hydrogen detection sensors, can be using solid solution electrolyte to hydrogen sulfide
Gas content is detected, and quickly, detection accuracy is good for response speed, and has anti-jamming effectiveness.
The object of the present invention is achieved like this: a kind of sulfurated hydrogen detection sensor, including the square being made of ceramic materials
Shape top substrate layer and underlying substrate are mutually bonded between two-layer substrate through adhesive, are equipped in parallel in the upper surface of underlying substrate
Several grooves, groove is interior to be equipped with heating wire；Top substrate layer is equipped with several honeycomb holes through top substrate layer, the aperture of honeycomb hole
Upper surface for 0.1 ~ 0.25mm, top substrate layer is coated with Na3Zr2Si2PO12The spray coating that material is formed, spray coating upper surface are embedding
Equipped with spun gold net, spun gold net is in rectangle net trellis, and a upper side of spun gold net is equipped with strip Au reference electrode, spun gold net it is another
Upper side is equipped with the working electrode of strip, the reference electrode and the parallel setting of working electrode, spun gold net and reference electrode it
Between, between spun gold net and working electrode respectively to drawing Pt lead on the outside of substrate, the working electrode by
CoNi0.6Cr0.8Mn1.6O5Material spraying is online in spun gold and is made.
When the invention works, spray coating is trigonal system structure, wherein ZrO6For octahedral structure, with Si (P) O4Four
Face body is connected with apex angle, forms three-dimensional framework, and sodium ion is in interstitial site, forms the electrolyte of solid solution.It is at 300 DEG C
When, conductivity is up to 10-1S·cm-1.Carrying out H2When S is detected, carried out by following reaction formula:
H2S+4Na2O→ 8Na++H2SO4+8e-
8Na++4O2+8e- → 4Na2O
Above-mentioned two reaction can form potential difference between reference electrode and working electrode, using the potential difference, can survey
Obtain the H in gas2S content, working electrode is by CoNi0.6Cr0.8Mn1.6O5Material is made, and is used as sensitive electrode materials'use, can
Accelerate the electron-transport efficiency with contact with hydrogen sulfide interface, and then improve the speed of electrochemical reaction, so that H2S gas detection
Fast response time.The adhesive fastness of the material of coating and spraying can be enhanced in cellular structure, and spun gold net can guarantee to be formed
Stationary field avoids the influence of the monopole in field domain, makes it have jamproof effect, avoids doing caused by external drive
It disturbs.It is not also influenced simultaneously by CO, the alcohol in external environment, detection accuracy is high.The sensor is exclusively used in detection H2S gas contains
Amount.
It is as a further improvement of the present invention, the width of the reference electrode is 0.65 ~ 0.85mm, with a thickness of 45 ~
60μm；The width of working electrode is 2.0 ~ 2.5mm, with a thickness of 90 ~ 120 μm.The spray coating with a thickness of 45 ~ 60 μm.It is described
The sealike colour of spun gold net is 15 ~ 25 μm.The top substrate layer with a thickness of 0.8 ~ 1.2mm.
It is as the machine that further changes of the invention, described adhesive is to be mixed with Al2O3The Na of powder2SiO3Go from
Sub- aqueous solution, wherein the weight ratio of each component is Al2O3: Na2SiO3: H2O=1:(3 ~ 5): (10 ~ 15), Al2O3The partial size of powder
It is 40 ~ 80 μm.
The invention also discloses a kind of manufacturing methods of sulfurated hydrogen detection sensor, include the following steps:
1) by Na3Zr2Si2PO12Powder made of material and 2- (4- methyl -3- cyclohexenyl group) -2- propyl alcohol are mixed into paste
Shape is sprayed in top substrate layer, and fills up honeycomb hole；
2) it is embedded in spun gold net in top substrate layer, the upper surface of spun gold net is kept to be higher by the spray coating；
3) it is sintered 2 ~ 3 hours at 850 ~ 880 DEG C；The purpose of sintering is to remove 2- (4- methyl -3- cyclohexenyl group) -2-
Propyl alcohol, and make Na3Zr2Si2PO12Material solidification, spun gold net are fixed；
4) Pt lead is drawn respectively in spun gold net two sides, then coat gold paste in spun gold net side, form reference electrode；?
The spun gold net other side sprays CoNi0.6Cr0.8Mn1.6O5Slurry forms working electrode；Gold paste and CoNi0.6Cr0.8Mn1.6O5Slurry is equal
It is formed by corresponding dusty material and ethylene glycol mixing preparation；It is put under infrared lamp after drying, then applies after coating and spraying every time
Next layer is covered and sprays, until the width of the reference electrode is 0.65 ~ 0.85mm, with a thickness of 45 ~ 60 μm；The width of working electrode
Degree is 2.0 ~ 2.5mm, with a thickness of 90 ~ 120 μm；
5) it is taken out after being sintered 4 ~ 6 hours at 600 ~ 650 DEG C, removal ethylene glycol is sintered by this；
6) adhesive is prepared, by Al2O3、Na2SiO3With deionized water according to 1:(3 ~ 5): the ratio mixing of (10 ~ 15) is equal
It is even, Na2SiO3Using Na2SiO3•9H2O is converted into deionized water and is measured as raw material, the crystallization water therein；
8) it is coated between top substrate layer and underlying substrate with adhesive, then top substrate layer and underlying substrate is bonded in one
It rises；
7) in CO2Under environment, 4 ~ 5 hours are kept the temperature in 160 ~ 250 DEG C, keeps top substrate layer Nian Jie with underlying substrate securely；Water
Glass curable rock-steady structure for forming Si-O-Si at 130 DEG C or more, in CO2Under environment, this process can be accelerated, make it
Solidification is rapid, bonding is secured；
8) finally, heating wire is mounted in the groove of underlying substrate.
This method manufactures sulfurated hydrogen detection sensor, and method is simple, easy to implement, high yield rate.
Detailed description of the invention
Fig. 1 is schematic structural view of the invention.
Fig. 2 is the corresponding relationship of concentration of hydrogen sulfide and potential difference.
Wherein, 1Pt lead, 2 reference electrodes, 3 honeycomb holes, 4 working electrodes, 5 spray coatings, 6 top substrate layers, 7 adhesive layers, 8
Underlying substrate, 9 spun gold nets, 10 grooves, 11 heating wire.
Specific embodiment
Embodiment 1
As shown in Figure 1, being a kind of sulfurated hydrogen detection sensor, including the top substrate layer and lower layer's base in rectangle and insulation
Plate, top substrate layer 6 and underlying substrate 8 are made of ceramic materials, and are mutually bonded between two-layer substrate through adhesive, and adhesive layer is formed
7, it is equipped with several grooves 10 in parallel in the upper surface of underlying substrate, is equipped with heating wire 11 in groove 10；If top substrate layer is equipped with
The aperture of the dry honeycomb hole 3 through top substrate layer, honeycomb hole 3 is 0.1 ~ 0.25mm, and the upper surface of top substrate layer is coated with
Na3Zr2Si2PO12The spray coating 5 that material is formed, 5 upper surface of spray coating are embedded with spun gold net 9, and spun gold net 9 is in rectangle net trellis,
One upper side of spun gold net 9 is equipped with strip Au reference electrode 2, and the working electrode 4 of strip is equipped with above the other side of spun gold net 9,
The reference electrode 2 and the parallel setting of working electrode 4, between spun gold net 9 and reference electrode 2, spun gold net 9 and working electrode 4
Between respectively to drawing Pt lead 1 on the outside of substrate, the working electrode 4 is by CoNi0.6Cr0.8Mn1.6O5Material spraying is in spun gold net
It is made on 9.
The width of reference electrode 2 is 0.65mm, with a thickness of 45 μm；The width of working electrode 4 is 2.0mm, with a thickness of 90 μm.
Spray coating 5 with a thickness of 45 μm.The sealike colour of spun gold net 9 is 15 μm.Top substrate layer 7 with a thickness of 0.8mm, underlying substrate master
It plays a supportive role, thickness is to meet intensity requirement.
When the manufacture of the sulfurated hydrogen detection sensor, carry out as follows:
1) by Na3Zr2Si2PO12Powder made of material and 2- (4- methyl -3- cyclohexenyl group) -2- propyl alcohol are mixed into paste
Shape is sprayed in top substrate layer, and fills up honeycomb hole；
2) it is embedded in spun gold net in top substrate layer, the upper surface of spun gold net is kept to be higher by the spray coating；
3) it is sintered 2 hours at 850 ~ 880 DEG C；The purpose of sintering is to remove 2- (4- methyl -3- cyclohexenyl group) -2- third
Alcohol, and make Na3Zr2Si2PO12Material solidification, spun gold net are fixed；
4) Pt lead is drawn respectively in spun gold net two sides, then coat gold paste in spun gold net side, form reference electrode；?
The spun gold net other side sprays CoNi0.6Cr0.8Mn1.6O5Slurry forms working electrode；Gold paste and CoNi0.6Cr0.8Mn1.6O5Slurry is equal
It is formed by corresponding dusty material and ethylene glycol mixing preparation；It is put under infrared lamp after drying, then applies after coating and spraying every time
Next layer is covered and sprays, until the width of the reference electrode is 0.65mm, with a thickness of 45 μm；The width of working electrode is
2.0mm, with a thickness of 90 μm；
5) it is taken out after being sintered 4 hours at 600 ~ 650 DEG C, removal ethylene glycol is sintered by this；
6) adhesive is prepared, by Al2O3、Na2SiO3It is uniformly mixed with deionized water according to the ratio of 1:3:10,
Na2SiO3Using Na2SiO3•9H2O is converted into deionized water and is measured as raw material, the crystallization water therein； Al2O3Powder
Partial size is 40 ~ 80 μm；
8) it is coated between top substrate layer and underlying substrate with adhesive, then top substrate layer and underlying substrate is bonded in one
It rises；
7) in CO2Under environment, 5 hours are kept the temperature in 160 DEG C, keeps top substrate layer Nian Jie with underlying substrate securely；Waterglass exists
The curable rock-steady structure for forming Si-O-Si at 130 DEG C or more, in CO2Under environment, this process can be accelerated, keep its solidification fast
Speed, bonding are secured；
8) finally, heating wire is mounted in the groove of underlying substrate.
The sulfurated hydrogen detection sensor obtained using this method, when being detected, in reference electrode and working electrode
Between potential difference as shown in Fig. 2, be directed to various concentration H2S has preferable corresponding relationship, especially H2The concentration of S is in 30ppm
When following, substantially linearly, measured value is very accurate.
Embodiment 2
Difference from example 1 is that the width of reference electrode is 0.85mm, with a thickness of 60 μm；Working electrode
Width is 2.5mm, with a thickness of 120 μm.Spray coating with a thickness of 60 μm.The sealike colour of spun gold net is 25 μm.
When the manufacture of the sulfurated hydrogen detection sensor, carry out as follows:
1) by Na3Zr2Si2PO12Powder made of material and 2- (4- methyl -3- cyclohexenyl group) -2- propyl alcohol are mixed into paste
Shape is sprayed in top substrate layer, and fills up honeycomb hole；
2) it is embedded in spun gold net in top substrate layer, the upper surface of spun gold net is kept to be higher by the spray coating；
3) it is sintered 3 hours at 850 ~ 880 DEG C；The purpose of sintering is to remove 2- (4- methyl -3- cyclohexenyl group) -2- third
Alcohol, and make Na3Zr2Si2PO12Material solidification, spun gold net are fixed；
4) Pt lead is drawn respectively in spun gold net two sides, then coat gold paste in spun gold net side, form reference electrode；?
The spun gold net other side sprays CoNi0.6Cr0.8Mn1.6O5Slurry forms working electrode；Gold paste and CoNi0.6Cr0.8Mn1.6O5Slurry is equal
It is formed by corresponding dusty material and ethylene glycol mixing preparation；It is put under infrared lamp after drying, then applies after coating and spraying every time
Next layer is covered and sprays, until the width of the reference electrode is 0.85mm, with a thickness of 60 μm；The width of working electrode is
2.5mm, with a thickness of 120 μm；
5) it is taken out after being sintered 6 hours at 600 ~ 650 DEG C, removal ethylene glycol is sintered by this；
6) adhesive is prepared, by Al2O3、Na2SiO3It is uniformly mixed with deionized water according to the ratio of 1:5:15,
Na2SiO3Using Na2SiO3•9H2O is converted into deionized water and is measured as raw material, the crystallization water therein； Al2O3Powder
Partial size is 40 ~ 80 μm；
8) it is coated between top substrate layer and underlying substrate with adhesive, then top substrate layer and underlying substrate is bonded in one
It rises；
7) in CO2Under environment, 4 hours are kept the temperature in 250 DEG C, keeps top substrate layer Nian Jie with underlying substrate securely；Waterglass exists
The curable rock-steady structure for forming Si-O-Si at 130 DEG C or more, in CO2Under environment, this process can be accelerated, keep its solidification fast
Speed, bonding are secured；
8) finally, heating wire is mounted in the groove of underlying substrate.
Embodiment 3
Difference from example 1 is that the width of reference electrode is 0.70mm, with a thickness of 60 μm；Working electrode
Width is 2.0mm, with a thickness of 100 μm.Spray coating with a thickness of 50 μm.The sealike colour of spun gold net is 20 μm.
Embodiment 4
Difference from example 1 is that the width of reference electrode is 0.85mm, with a thickness of 45 μm；Working electrode
Width is 2.0mm, with a thickness of 120 μm.Spray coating with a thickness of 45 μm.The sealike colour of spun gold net is 15 μm.
In short, being carried out as follows when the manufacture of the sulfurated hydrogen detection sensor:
1) by Na3Zr2Si2PO12Powder made of material and 2- (4- methyl -3- cyclohexenyl group) -2- propyl alcohol are mixed into paste
Shape is sprayed in top substrate layer, and fills up honeycomb hole；
2) it is embedded in spun gold net in top substrate layer, the upper surface of spun gold net is kept to be higher by the spray coating；
3) it is sintered 2 ~ 3 hours at 850 ~ 880 DEG C；The purpose of sintering is to remove 2- (4- methyl -3- cyclohexenyl group) -2-
Propyl alcohol, and make Na3Zr2Si2PO12Material solidification, spun gold net are fixed；
4) Pt lead is drawn respectively in spun gold net two sides, then coat gold paste in spun gold net side, form reference electrode；?
The spun gold net other side sprays CoNi0.6Cr0.8Mn1.6O5Slurry forms working electrode；Gold paste and CoNi0.6Cr0.8Mn1.6O5Slurry is equal
It is formed by corresponding dusty material and ethylene glycol mixing preparation；It is put under infrared lamp after drying, then applies after coating and spraying every time
Next layer is covered and sprays, until the width of the reference electrode is 0.65 ~ 0.85mm, with a thickness of 45 ~ 60 μm；The width of working electrode
Degree is 2.0 ~ 2.5mm, with a thickness of 90 ~ 120 μm；
5) it is taken out after being sintered 4 ~ 6 hours at 600 ~ 650 DEG C, removal ethylene glycol is sintered by this；
6) adhesive is prepared, by Al2O3、Na2SiO3With deionized water according to 1:(3 ~ 5): the ratio mixing of (10 ~ 15) is equal
It is even, Na2SiO3Using Na2SiO3•9H2O is converted into deionized water and is measured as raw material, the crystallization water therein； Al2O3Powder
The partial size at end is 40 ~ 80 μm；
8) it is coated between top substrate layer and underlying substrate with adhesive, then top substrate layer and underlying substrate is bonded in one
It rises；
7) in CO2Under environment, 4 ~ 5 hours are kept the temperature in 160 ~ 250 DEG C, keeps top substrate layer Nian Jie with underlying substrate securely；Water
Glass curable rock-steady structure for forming Si-O-Si at 130 DEG C or more, in CO2Under environment, this process can be accelerated, make it
Solidification is rapid, bonding is secured；
8) finally, heating wire is mounted in the groove of underlying substrate.
Above-mentioned data area can be with capping value, lower limit value and intermediate arbitrary value.
The present invention is not limited to the above embodiments, on the basis of technical solution disclosed by the invention, the skill of this field
For art personnel according to disclosed technology contents, one can be made to some of which technical characteristic by not needing creative labor
A little replacements and deformation, these replacements and deformation are within the scope of the invention.
Claims (1)
1. a kind of manufacturing method of sulfurated hydrogen detection sensor, it is characterised in that include the following steps:
1) by Na3Zr2Si2PO12Powder made of material and 2- (4- methyl -3- cyclohexenyl group) -2- propyl alcohol are mixed into paste, spray
It is coated in top substrate layer, and fills up honeycomb hole；It is arranged if the honeycomb hole is equipped with dry doubling through top substrate layer, the aperture of honeycomb hole
For 0.1 ~ 0.25mm；
2) it is embedded in spun gold net in top substrate layer, the upper surface of spun gold net is kept to be higher by the spray coating；
3) it is sintered 2 ~ 3 hours at 850 ~ 880 DEG C；
4) Pt lead is drawn respectively in spun gold net two sides, then coat gold paste in spun gold net side, form reference electrode；In spun gold
It nets the other side and sprays CoNi0.6Cr0.8Mn1.6O5Slurry forms working electrode；Gold paste and CoNi0.6Cr0.8Mn1.6O5Slurry is by phase
Dusty material is answered to form with ethylene glycol mixing preparation；Be put under infrared lamp after coating and spraying every time it is dry after, re-coating and
Next layer is sprayed, until the width of the reference electrode is 0.65 ~ 0.85mm, with a thickness of 45 ~ 60 μm；The width of working electrode is
2.0 ~ 2.5mm, with a thickness of 90 ~ 120 μm；
5) it is taken out after being sintered 4 ~ 6 hours at 600 ~ 650 DEG C；
6) adhesive is prepared, by Al2O3、Na2SiO3With deionized water according to 1:(3 ~ 5): the ratio of (10 ~ 15) is uniformly mixed,
Na2SiO3Using Na2SiO3•9H2O is converted into deionized water and is measured as raw material, the crystallization water therein；
8) it is coated between top substrate layer and underlying substrate with adhesive, then top substrate layer and underlying substrate is bonded together；
7) in CO2Under environment, 4 ~ 5 hours are kept the temperature in 160 ~ 250 DEG C, keeps top substrate layer Nian Jie with underlying substrate securely；
8) heating wire is mounted in the groove of underlying substrate.
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| JPWO2003091719A1 (en) * | 2002-04-25 | 2005-09-02 | 独立行政法人科学技術振興機構 | Nitrogen oxide sensing electrode and nitrogen oxide sensor using the same |
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| CN201141848Y (en) * | 2008-01-14 | 2008-10-29 | 吉林大学 | Integrated dual-function NASICON solid electrolyte gas sensor |
| CN102866189A (en) * | 2012-08-26 | 2013-01-09 | 吉林大学 | NASICON-based H2S sensor using composite metallic oxide as sensitive electrode |
| CN103604853A (en) * | 2013-11-21 | 2014-02-26 | 吉林大学 | Mixed-potential type NO2 sensor with mesh-strip structured YSZ (yttria-stabilized zirconia) substrate serving as conductive layer and preparation method for mixed-potential type NO2 sensor |
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