CN108593726A - A kind of open fast-response electrochemical gas sensor - Google Patents
A kind of open fast-response electrochemical gas sensor Download PDFInfo
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- CN108593726A CN108593726A CN201810374909.1A CN201810374909A CN108593726A CN 108593726 A CN108593726 A CN 108593726A CN 201810374909 A CN201810374909 A CN 201810374909A CN 108593726 A CN108593726 A CN 108593726A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
Abstract
A kind of open fast-response electrochemical gas sensor, is related to a kind of sensor.Purpose is to solve the problems, such as existing electrochemical gas sensor response time length, poor selectivity and be vulnerable to the interference of other gases.Sensor is made of ceramic substrate, electrode, electrolyte and porous carrier layer；Electrode is set to porous carrier layer upper surface, and porous carrier layer inside is immobilized electrolyte；Preparation method：Porous slurry is printed on ceramic substrate surface, and high temperature sintering porous carrier layer prints electrode, and electrolyte is added dropwise in electrode sintering, electrode leads to client welding lead.The present invention produces the sensor with Open architecture by the structure design of the electrochemical gas sensor to cofiring structure, and the selective enumeration method to multiple gases may be implemented；Response time is short, and selectivity is good, and service life is long.The present invention is suitable for preparing electrochemical gas sensor.
Description
Technical field
The present invention relates to a kind of sensors.
Background technology
Electrochemical gas sensor is that target gas is carried out oxidation or reduction reaction in electrode surface, measures work
Make electrode and the electric current between electrode, and then realize the measurement to target gas concentration, generally include working electrode and
Induction electrode.Electrochemical gas sensor has been widely used for the gaseous species such as industrial environment, closed environment, air and concentration
Detection.Common electrochemical gas sensor is mostly chamber structure on the market at present, there is two electrodes, three electrodes and four electrode bodies
System, wherein two electrodes and three-electrode structure are relatively conventional.Electrochemical gas sensor relies primarily on gas molecule electrolytic potential
Different instructions gas with various, therefore gas similar in electrolytic potential cannot be distinguished, such as H2CO can be had an impact, two kinds of gas
Body electrode potential is close, it is more difficult to and it distinguishes, in turn results in the poor selectivity of electrochemical gas sensor, electrochemical gas sensor
Poor selectivity is current urgent problem.Chamber structure causes gas to be spread in electrolytic cell slowly, in turn results in electrochemistry
The response time of gas sensor is long, the response time τ of presently commercially available electrochemical gas sensor90≤60s；Therefore, existing electricity
Sensor of chemical gas common problem is in response to time length, poor selectivity, is vulnerable to the interference of other gases.
Invention content
The present invention is in order to solve long existing electrochemical gas sensor response time, poor selectivity and be vulnerable to other gases
The problem of interference, a kind of open fast-response electrochemical gas sensor of proposition and preparation method thereof.
The open fast-response electrochemical gas sensor of the present invention is by ceramic substrate, electrode, electrolyte and porous carrier layer
It constitutes；The porous carrier layer is set to ceramic substrate upper surface, and electrode is set to porous carrier layer upper surface, the extraction of electrode
End extends to ceramic substrate upper surface；It is immobilized inside porous carrier layer to have electrolyte；
The electrode is by working electrode and two electrode systems that are constituted to electrode, or by working electrode, to electrode and ginseng
Than the three electrode polar body systems that electrode is constituted, or four electrode systems that are made of a pair of of current electrode and a pair of of measuring electrode；
The electrolyte is ionic liquid, and ionic liquid is made of cation and anion；Cation in ionic liquid
For quaternary ammonium salt, imidazoles (Im+), pyridine (py+) or pyrroles's cationoid；Anion in ionic liquid is PF6 -、BF4 -、
CF3COO-、C3F7COO-Or N (C2F5SO2)2-Anion；
The material of the working electrode is noble metal or noble metal composite-material；Noble metal is Pt or Au, and noble metal is compound
Material is Pt/C or Pt/Ru；
The material to electrode is noble metal or noble metal composite-material, noble metal Pt, Au, Ag or Ru, noble metal
Composite material is Ag/Pd；
The material of the reference electrode is noble metal or noble metal composite-material, noble metal Pt, Au, Ag or Ru, your gold
Category composite material is Ag/Pd；
The material of the current electrode is noble metal or noble metal composite-material, noble metal Pt, Au, Ag or Ru, your gold
Category composite material is Ag/Pd；
The material of the measuring electrode is noble metal or noble metal composite-material, noble metal Pt, Au, Ag or Ru, your gold
Category composite material is Ag/Pd；
The preparation method of above-mentioned open fast-response electrochemical gas sensor carries out according to the following steps：
One, porous slurry is printed on ceramic substrate surface by the way of silk-screen printing, is printed electrode using Gold conductor
Exit；
The porous slurry is commercial goods, is bought in ESL companies of the U.S., model 4550；
The Gold conductor is commercial goods, is bought in ESL companies of the U.S., model 1901-Au；
Two, high temperature sintering obtains the porous carrier layer for immobilized electrolyte；
Length, the width and thickness of the porous carrier layer be respectively 3~8mm, 3~8mm and 10~50 μm；
The high-sintering process is：It is 1000~1250 DEG C of 2~3h of heat preservation in temperature；
Three, it uses metal paste in porous carrier layer print electrode on surface by the way of silk-screen printing, and makes printing
Electrode covers corresponding electrode leads to client；
Four, electrode is sintered；
The sintering temperature of the sintered electrode is 100~125 DEG C；Sintering time is 45~60min；The purpose of electrode sintering
It is that electrode is made to cure, the organic matter burning-off in metal paste is removed, metal electrode layer is only left in porous layer surface；
Five, in electrode leads to client welding lead, the sensor electrolytic cell being made of electrode, lead and porous carrier layer is obtained
Structure；
Six, electrolyte is added dropwise to porous carrier layer surface using pipettor, then vacuumize process 10min, then weighs again
Electrolyte and vacuumize process is added dropwise twice again, that is, completes the system of open fast-response electrochemical gas sensor sensing unit
It is standby；
The amount of the electrolyte being added dropwise every time to porous carrier layer surface is 2~5 μ L/cm3；
The pressure ＜ 0.1MPa of the vacuumize process；
Seven, several open fast-response electrochemical gas sensor sensing units are prepared on the same ceramic substrate, i.e.,
Complete the preparation of open fast-response electrochemical gas sensor；
The present invention is produced by the structure design of the electrochemical gas sensor to cofiring structure with Open architecture
Sensor, the principle of the invention and have the beneficial effect that：
1, chamber structure is not present in inventive sensor, therefore easy to be integrated with other sensors, and easily realizes
Sensor is miniaturized；The present invention can make several identical sensor sensing units on same substrate ceramic substrate, realize electricity
It is the array of chemical sensor, integrated；According to the difference of the oxidation-reduction potential of gas in the electrolytic solution, in porous carrier layer
Upper immobilized different types of electrolyte and the working electrode for printing different materials, and apply different operating voltage respectively, it can
Realize the selective enumeration method to multiple gases；Present invention gas that can be detected includes inorganic gas such as H2、O2、HCl、H2S、
HCN、SO2、CO、CO2、NH3、F2、Cl2、NOxDeng it is organic that a variety of aromatic series, hydro carbons, aldehydes, ketone, alcohols etc. can also be detected
Gas；
2, the present invention is Open architecture, and without ventilated membrane, electrode and electrolyte are exposed for electrode and electrolyte carrier surface
In air, it can occasionally directly be contacted with detected gas, shorten response time, the response time τ of inventive sensor90≤
30s；
3, the preparation of sensor of the invention electrolyser construction is realized using silk-screen printing, the consistency of the product of preparation
It is good；
4, present invention uses ionic liquids as electrolyte, and ionic liquid has different solubility to gas with various, because
This present invention improves the selectivity of electrochemical gas sensor；Sensor realizes the selection to gas using two methods simultaneously
Identification utilizes the electrolytic potential difference of object gas to be identified to the selection of gas and using object gas in the molten of ionic liquid
Solution property difference identifies that classic water-soluble electrolyte system realizes the choosings of gases mainly by the difference of electrolytic potential to the selection of gas
Selecting property identifies, for gas similar in electrolytic potential with regard to None- identified.Therefore the selectivity of inventive sensor is good；
5, traditional electrolyte is water solution system, and the electrochemical window of the electrolytic potential 1.23V of water, ionic liquid are -3V
~3V, therefore water solution system is easily decomposed；In addition, ionic liquid body saturated vapour pressure is small, it is not volatile, therefore electrolyte
It is not easy to dry up, the stability of electrolyte is good；Electrode of the present invention does electrode using noble metal simultaneously, is not easy that corruption occurs in the electrolytic solution
Erosion, porous carrier layer is ceramic material, and chemical property is more stable, therefore the electrolyser construction performance of the present invention is stablized, and is extended
The service life of sensor.
Description of the drawings
Fig. 1 is the structural schematic diagram of open fast-response electrochemical gas sensor prepared by embodiment 1；
Fig. 2 is output current measured drawing of the ammonia gas sensor under different ammonia concentration concentration in embodiment 1；
The ammonia concentration that Fig. 3 is done by the corresponding test datas of Fig. 2-output current relational graph.
Specific implementation mode：
Technical solution of the present invention is not limited to act specific implementation mode set forth below, further includes between each specific implementation mode
Arbitrary reasonable combination.
Specific implementation mode one：The open fast-response electrochemical gas sensor of present embodiment is by ceramic substrate 1, electrode
2, electrolyte and porous carrier layer 3 are constituted；The porous carrier layer 3 is set to 1 upper surface of ceramic substrate, and electrode 2 is set to more
The exit of 3 upper surface of hole carrier layer, electrode 2 extends to 1 upper surface of ceramic substrate；3 inside of porous carrier layer is immobilized electrolysis
Liquid.
Present embodiment has following advantageous effect：
1, chamber structure is not present in present embodiment sensor, therefore is easy integrated with other sensors and easy
Realize sensor micromation；Present embodiment can make several identical sensor sensing lists on same substrate ceramic substrate
Member realizes the array, integrated of electrochemical sensor；The difference of the oxidation-reduction potential of foundation gas in the electrolytic solution,
The working electrode of immobilized different types of electrolyte and printing different materials on porous carrier layer, and apply different operating electricity respectively
Pressure, can realize the selective enumeration method to multiple gases；Present embodiment gas that can be detected includes inorganic gas such as H2、
O2、HCl、H2S、HCN、SO2、CO、CO2、NH3、F2、Cl2、NOxDeng, can also detect a variety of aromatic series, hydro carbons, aldehydes, ketone,
The organic gas such as alcohols；
2, present embodiment is Open architecture, and electrode and electrolyte carrier surface are without ventilated membrane, electrode and electrolyte
It is exposed occasionally directly to be contacted in air with detected gas, the response time is shortened, when the response of present embodiment sensor
Between τ90≤30s；
3, the preparation of the sensor electrolyser construction of present embodiment using silk-screen printing realize, the product of preparation it is consistent
Property is good；
4, present embodiment has used ionic liquid as electrolyte, and ionic liquid has different dissolvings to gas with various
Degree, therefore present embodiment improves the selectivity of electrochemical gas sensor；Sensor is simultaneously using two methods realization pair
The selection of gas identifies, that is, utilize the electrolytic potential difference of object gas the selection of gas is identified and using object gas from
The dissolubility difference of sub- liquid identifies the selection of gas classic water-soluble electrolyte system is real mainly by the difference of electrolytic potential
The Selective recognition of existing gas, for gas similar in electrolytic potential with regard to None- identified.Therefore the choosing of present embodiment sensor
Selecting property is good；
5, traditional electrolyte is water solution system, and the electrochemical window of the electrolytic potential 1.23V of water, ionic liquid are -3V
~3V, therefore water solution system is easily decomposed；In addition, ionic liquid body saturated vapour pressure is small, it is not volatile, therefore electrolyte
It is not easy to dry up, the stability of electrolyte is good；Present embodiment electrode does electrode using noble metal simultaneously, is not easy to send out in the electrolytic solution
Raw corrosion, porous carrier layer is ceramic material, and chemical property is more stable, therefore the electrolyser construction performance of present embodiment is steady
It is fixed, extend the service life of sensor.
Specific implementation mode two：The present embodiment is different from the first embodiment in that：The electrode is by work electricity
Pole and two electrode systems that electrode is constituted, or by working electrode, the three electrode polar body systems constituted to electrode and reference electrode, or
Four electrode systems being made of a pair of of current electrode and a pair of of measuring electrode.Other steps and parameter and one phase of specific implementation mode
Together.
Specific implementation mode three：The present embodiment is different from the first and the second embodiment in that：The electrolyte be from
Sub- liquid, ionic liquid are made of cation and anion；Cation in ionic liquid is quaternary ammonium salt, imidazoles Im+, pyridine py+
Or pyrroles's cationoid；Anion in ionic liquid is PF6 -、BF4 -、CF3COO-、C3F7COO-Or N (C2F5SO2)2-Anion.
Other steps and parameter are the same as one or two specific embodiments.
Specific implementation mode four：Unlike one of present embodiment and specific implementation mode one to three：The work electricity
The material of pole is noble metal or noble metal composite-material；Noble metal is Pt or Au, and noble metal composite-material is Pt/C or Pt/Ru.
Other steps and parameter are identical as one of specific implementation mode one to three.
Specific implementation mode five：Unlike one of present embodiment and specific implementation mode one to four：It is described to electrode
Material be noble metal or noble metal composite-material, noble metal Pt, Au, Ag or Ru, noble metal composite-material Ag/Pd.Its
His step and parameter are identical as one of specific implementation mode one to four.
Specific implementation mode six：Unlike one of present embodiment and specific implementation mode one to five：The reference electricity
The material of pole is noble metal or noble metal composite-material, noble metal Pt, Au, Ag or Ru, noble metal composite-material Ag/Pd.
Other steps and parameter are identical as one of specific implementation mode one to five.
Specific implementation mode seven：Unlike one of present embodiment and specific implementation mode one to six：The power supply electricity
The material of pole is noble metal or noble metal composite-material, noble metal Pt, Au, Ag or Ru, noble metal composite-material Ag/Pd.
Other steps and parameter are identical as one of specific implementation mode one to six.
Specific implementation mode eight：Unlike one of present embodiment and specific implementation mode one to seven：The measurement electricity
The material of pole is noble metal or noble metal composite-material, noble metal Pt, Au, Ag or Ru, noble metal composite-material Ag/Pd.
Other steps and parameter are identical as one of specific implementation mode one to seven.
Specific implementation mode nine：The preparation method of the open fast-response electrochemical gas sensor of present embodiment is by following
Step carries out：
One, porous slurry is printed on ceramic substrate surface by the way of silk-screen printing, is printed electrode using Gold conductor
Exit；
Two, high temperature sintering obtains the porous carrier layer for immobilized electrolyte；
Length, the width and thickness of the porous carrier layer be respectively 3~8mm, 3~8mm and 10~50 μm；
The high-sintering process is：It is 1000~1250 DEG C of 2~3h of heat preservation in temperature；
Three, it uses metal paste in porous carrier layer print electrode on surface by the way of silk-screen printing, and makes printing
Electrode covers corresponding electrode leads to client；
Four, electrode is sintered；
The sintering temperature of the sintered electrode is 100~125 DEG C；Sintering time is 45~60min；
Five, in electrode leads to client welding lead, the sensor electrolytic cell being made of electrode, lead and porous carrier layer is obtained
Structure；
Six, electrolyte is added dropwise to porous carrier layer surface using pipettor, then vacuumize process 10min, then weighs again
Electrolyte and vacuumize process is added dropwise twice again, that is, completes the system of open fast-response electrochemical gas sensor sensing unit
It is standby；
The pressure ＜ 0.1MPa of the vacuumize process；
Seven, several open fast-response electrochemical gas sensor sensing units are prepared on the same ceramic substrate, i.e.,
Complete the preparation of open fast-response electrochemical gas sensor.
Present embodiment has following advantageous effect：
1, chamber structure is not present in sensor prepared by present embodiment, therefore easy to be integrated with other sensors,
And easily realize sensor micromation；It is quick that present embodiment can make several identical sensors on same substrate ceramic substrate
Feel unit, realizes the array, integrated of electrochemical sensor；Not according to the oxidation-reduction potential of gas in the electrolytic solution
Together, immobilized different types of electrolyte and the working electrode for printing different materials on porous carrier layer, and apply respectively different
Operating voltage can realize the selective enumeration method to multiple gases；Sensor gas that can be detected prepared by present embodiment
Body includes inorganic gas such as H2、O2、HCl、H2S、HCN、SO2、CO、CO2、NH3、F2、Cl2、NOxDeng a variety of fragrance can also be detected
The organic gas such as race, hydro carbons, aldehydes, ketone, alcohols；
2, sensor prepared by present embodiment is Open architecture, electrode and electrolyte carrier surface without ventilated membrane,
Electrode and electrolyte are exposed in air, can occasionally directly be contacted with detected gas, shorten the response time, and present embodiment passes
The response time τ of sensor90≤30s；
3, the preparation of the sensor electrolyser construction of sensor prepared by present embodiment is realized using silk-screen printing, is prepared
Product consistency it is good；
4, used ionic liquid as electrolyte in sensor prepared by present embodiment, ionic liquid has gas with various
There is different solubility, therefore present embodiment improves the selectivity of electrochemical gas sensor；Sensor uses two simultaneously
Kind method realizes that the selection to gas identifies, that is, utilizes the electrolytic potential difference of object gas to the selection identification and utilization of gas
Object gas identifies that classic water-soluble electrolyte system is mainly by electrolysis in the dissolubility difference of ionic liquid to the selection of gas
The different Selective recognitions for realizing gas of current potential, for gas similar in electrolytic potential with regard to None- identified.Therefore this embodiment party
The selectivity of formula sensor is good；
5, traditional electrolyte is water solution system, and the electrochemical window of the electrolytic potential 1.23V of water, ionic liquid are -3V
~3V, therefore water solution system is easily decomposed；In addition, ionic liquid body saturated vapour pressure is small, it is not volatile, therefore electrolyte
It is not easy to dry up, the stability of electrolyte is good；Present embodiment electrode does electrode using noble metal simultaneously, is not easy to send out in the electrolytic solution
Raw corrosion, porous carrier layer is ceramic material, and chemical property is more stable, therefore the electrolyser construction performance of present embodiment is steady
It is fixed, extend the service life of sensor.
Specific implementation mode ten：Present embodiment is unlike specific implementation mode nine：Every time to more described in step 6
The amount for the electrolyte that hole carrying layer surface is added dropwise is 2~5 μ L/cm3.Other steps and parameter are identical as specific implementation mode nine.
Beneficial effects of the present invention are verified using following embodiment：
Embodiment 1:
The open fast-response electrochemical gas sensor of the present embodiment is by ceramic substrate 1, electrode 2, electrolyte and porous load
Body layer 3 is constituted；The porous carrier layer 3 is set to 1 upper surface of ceramic substrate, and electrode 2 is set to 3 upper surface of porous carrier layer,
The exit of electrode 2 extends to 1 upper surface of ceramic substrate；3 inside of porous carrier layer is immobilized electrolyte；
The electrode is by working electrode, the three electrode polar body systems constituted to electrode and reference electrode；
The electrolyte is ionic liquid, and ionic liquid is made of cation and anion；Cation in ionic liquid
For imidazoles Im+；Anion in ionic liquid is PF6 -；
The material of the working electrode is noble metal；Noble metal is Pt；
The material to electrode is noble metal, noble metal Pt；
The material of the reference electrode is noble metal, noble metal Pt；
The preparation method of above-mentioned open fast-response electrochemical gas sensor carries out according to the following steps：
One, porous slurry is printed on ceramic substrate surface by the way of silk-screen printing, is printed electrode using Gold conductor
Exit；
The porous slurry is commercial goods, is bought in ESL companies of the U.S., model 4550；
The Gold conductor is commercial goods, is bought in ESL companies of the U.S., model 1901-Au；
Two, high temperature sintering obtains the porous carrier layer for immobilized electrolyte；
Length, the width and thickness of the porous carrier layer are respectively 6mm, 6mm and 10 μm；
The high-sintering process is：It is 1100 DEG C of heat preservation 2.5h in temperature；
Three, it uses metal paste in porous carrier layer print electrode on surface by the way of silk-screen printing, and makes printing
Electrode covers corresponding electrode leads to client；
Four, electrode is sintered；
The sintering temperature of the sintered electrode is 115 DEG C；Sintering time is 50min；The purpose of electrode sintering is to make electrode
Solidification, the organic matter burning-off in metal paste is removed, metal electrode layer is only left in porous layer surface；
Five, in electrode leads to client welding lead, the sensor electrolytic cell being made of electrode, lead and porous carrier layer is obtained
Structure；
Six, electrolyte is added dropwise to porous carrier layer surface using pipettor, then vacuumize process 10min, then weighs again
Electrolyte and vacuumize process is added dropwise twice again, that is, completes the system of open fast-response electrochemical gas sensor sensing unit
It is standby；
The amount of the electrolyte being added dropwise every time to porous carrier layer surface is 2 μ L/cm3；
The pressure ＜ 0.1MPa of the vacuumize process；
The present embodiment prepares 1 open fast-response electrochemical gas sensor sensing unit on the same ceramic substrate
Constitute open fast-response electrochemical gas sensor；The sensor prepared to embodiment 1 using electrochemical workstation is placed in close
It holds one's breath in room, various concentration NH is passed through into gas chamber3, operating voltage is 2V DC voltages, and measurement sensor output current obtains
Sensor is in various concentration NH3In time current curve.Fig. 2 is that ammonia gas sensor is dense in different ammonia concentrations in embodiment 1
Output current measured drawing under degree；Fig. 3 does ammonia concentration-output current relational graph by the corresponding test datas of Fig. 2.By Fig. 3
It is found that the working strategy of sensor is y=0.6708x+272.44 in embodiment 1, linearly dependent coefficient 0.9906 illustrates reality
It applies 1 linear sensor of example to export, sensor accuracy class is high.
Embodiment 2：
As different from Example 1, the present embodiment prepares 4 sensor sensings to the present embodiment on the same ceramic substrate
Unit, constitutes integrated gas sensor, and 4 sensor sensing units are respectively：NO2Sensor sensing unit, CO sensors
Sensing unit, SO2Sensor sensing unit and H2Sensor sensing unit；The electrode of 4 sensor sensing units and embodiment 1
Identical, the electrolyte used in 4 sensor sensing units is as shown in table 1；
It is placed in integrated gas sensor is made in embodiment 2 in sealed gas chamber, NO is each led into gas chamber2, CO,
SO2And H2S, and apply the operating voltage of 1.0V, 0.5V, 1.4V and 0.7V respectively, using using Wan Tong companies of Switzerland
Autolab302N electrochemical workstations are to the NO that is passed through2, CO, SO2And H2S is detected.To NO2Sensor sensing unit, CO
Sensor sensing unit, SO2Sensor sensing unit and H2The operating voltage that sensor sensing unit applies is as shown in table 1；
Table 2 is testing result, from the data in table 2, it can be seen that 2 current output sensor of embodiment is nA grades, the response time is very fast
τ90≤ 20s, high certainty of measurement, precision non-linear≤± 1.5%FS.Response time and nonlinear indicator are higher than existing commercially available sensing
Device；The response time τ of existing commercial sensor90≤ 60s, precision non-linear≤± 3%FS.
Table 1
| Gaseous species | Operating voltage V | Electrolyte |
| NO2 | 1.0 | 1- butyl -3- methylimidazole bis-trifluoromethylsulfoandimide salt |
| CO | 0.5 | Chlorination 1- butyl -3- methylimidazoles |
| SO2 | 1.4 | 1- butyl -3- crassitude bis trifluoromethyl sulfonephthalein inferior amine salts |
| H2S | 0.7 | 1- ethyl-3-methylimidazole fluoroform sulphonates |
Table 2
Claims (10)
1. a kind of open fast-response electrochemical gas sensor, it is characterised in that：Open fast-response electrochemical gas sensing
Device is made of ceramic substrate (1), electrode (2), electrolyte and porous carrier layer (3)；The porous carrier layer (3) is set to ceramics
Substrate (1) upper surface, electrode (2) are set to porous carrier layer (3) upper surface, and the exit of electrode (2) extends to ceramic substrate
(1) upper surface；Porous carrier layer (3) inside is immobilized electrolyte.
2. open fast-response electrochemical gas sensor according to claim 1, it is characterised in that：The electrode is served as reasons
Working electrode and two electrode systems that electrode is constituted, or by working electrode, the three electrode poles constituted to electrode and reference electrode
System, or four electrode systems that are made of a pair of of current electrode and a pair of of measuring electrode.
3. open fast-response electrochemical gas sensor according to claim 1 or 2, it is characterised in that：The electrolysis
Liquid is ionic liquid, and ionic liquid is made of cation and anion；Cation in ionic liquid is quaternary ammonium salt, imidazoles, pyrrole
Pyridine or pyrroles's cationoid；Anion in ionic liquid is PF6 -、BF4 -、CF3COO-、C3F7COO-Or N (C2F5SO2)2-The moon from
Son.
4. open fast-response electrochemical gas sensor according to claim 3, it is characterised in that：The working electrode
Material be noble metal or noble metal composite-material；Noble metal is Pt or Au, and noble metal composite-material is Pt/C or Pt/Ru.
5. open fast-response electrochemical gas sensor according to claim 1,2 or 4, it is characterised in that：It is described right
The material of electrode is noble metal or noble metal composite-material, noble metal Pt, Au, Ag or Ru, noble metal composite-material Ag/
Pd。
6. open fast-response electrochemical gas sensor according to claim 5, it is characterised in that：The reference electrode
Material be noble metal or noble metal composite-material, noble metal Pt, Au, Ag or Ru, noble metal composite-material Ag/Pd.
7. open fast-response electrochemical gas sensor according to claim 6, it is characterised in that：The current electrode
Material be noble metal or noble metal composite-material, noble metal Pt, Au, Ag or Ru, noble metal composite-material Ag/Pd.
8. open fast-response electrochemical gas sensor according to claim 7, it is characterised in that：The measuring electrode
Material be noble metal or noble metal composite-material, noble metal Pt, Au, Ag or Ru, noble metal composite-material Ag/Pd.
9. the preparation method of open fast-response electrochemical gas sensor as described in claim 1, it is characterised in that：The party
Method carries out according to the following steps：
One, porous slurry is printed on ceramic substrate surface by the way of silk-screen printing, is printed electrode extraction using Gold conductor
End；
Two, high temperature sintering obtains the porous carrier layer for immobilized electrolyte；
Length, the width and thickness of the porous carrier layer be respectively 3~8mm, 3~8mm and 10~50 μm；
The high-sintering process is：It is 1000~1250 DEG C of 2~3h of heat preservation in temperature；
Three, it uses metal paste in porous carrier layer print electrode on surface by the way of silk-screen printing, and makes the electrode of printing
Cover corresponding electrode leads to client；
Four, electrode is sintered；
The sintering temperature of the sintered electrode is 100~125 DEG C；Sintering time is 45~60min；
Five, in electrode leads to client welding lead, the sensor electrolytic cell knot being made of electrode, lead and porous carrier layer is obtained
Structure；
Six, electrolyte is added dropwise to porous carrier layer surface using pipettor, then vacuumize process 10min, then repeats drop
Add electrolyte and vacuumize process twice, that is, completes the preparation of open fast-response electrochemical gas sensor sensing unit；
The pressure ＜ 0.1MPa of the vacuumize process；
Seven, several open fast-response electrochemical gas sensor sensing units are prepared on the same ceramic substrate, that is, are completed
The preparation of open fast-response electrochemical gas sensor.
10. requiring the preparation method of the open fast-response electrochemical gas sensor described in 9 according to profit, it is characterised in that：Step
The amount of rapid six electrolyte being added dropwise every time to porous carrier layer surface is 2~5 μ L/cm3。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109557151A (en) * | 2019-01-15 | 2019-04-02 | 中国电子科技集团公司第四十九研究所 | The manufacturing method of sensing unit based on ceramic co-fired technique, the electrochemical gas sensor containing the sensing unit and sensing unit |
| CN110044989A (en) * | 2019-04-30 | 2019-07-23 | 四川轻化工大学 | A kind of multi-gas sensor and preparation method thereof |
| CN112697864A (en) * | 2020-12-16 | 2021-04-23 | 浙江大学 | Integrated four-electrode gas sensor and preparation method and application thereof |
| CN114594146A (en) * | 2022-02-28 | 2022-06-07 | 广州钰芯智能科技研究院有限公司 | Four-pin double-working high-precision photoelectric transparent interdigital electrode containing insulation protection film and application thereof in photoelectric joint detection |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109557151A (en) * | 2019-01-15 | 2019-04-02 | 中国电子科技集团公司第四十九研究所 | The manufacturing method of sensing unit based on ceramic co-fired technique, the electrochemical gas sensor containing the sensing unit and sensing unit |
| CN110044989A (en) * | 2019-04-30 | 2019-07-23 | 四川轻化工大学 | A kind of multi-gas sensor and preparation method thereof |
| CN110044989B (en) * | 2019-04-30 | 2022-02-01 | 四川轻化工大学 | Multi-gas sensor |
| CN112697864A (en) * | 2020-12-16 | 2021-04-23 | 浙江大学 | Integrated four-electrode gas sensor and preparation method and application thereof |
| CN112697864B (en) * | 2020-12-16 | 2022-04-01 | 浙江大学 | Integrated four-electrode gas sensor and preparation method and application thereof |
| CN114594146A (en) * | 2022-02-28 | 2022-06-07 | 广州钰芯智能科技研究院有限公司 | Four-pin double-working high-precision photoelectric transparent interdigital electrode containing insulation protection film and application thereof in photoelectric joint detection |
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