CN104391025B - Preparation method of electrochemical carbon oxide gas sensor electrode - Google Patents
Preparation method of electrochemical carbon oxide gas sensor electrode Download PDFInfo
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Abstract
The invention relates to a preparation method of an electrochemical carbon oxide gas sensor electrode. A catalyst used by the electrode is a superconduction carbon-loaded cerium oxide-copper oxide (CeO-CuO) catalyst, and a base material of the catalyst is a perfluorosulfonic acid ion exchanging membrane (Nafion membrane). The preparation method is characterized by comprising the steps of transferring Ce(NO3)3.6H2O/Cu(NO3)2.3H2O and oxalic acid into a beaker; carrying out ball milling, drying, weighing superconduction carbon the mass of which is equal to that of a mixture obtained by ball milling, dropping ammonia water, stirring, carrying out water bath, and taking out the colloid which is dried out in the beaker; preserving heat, grinding, adding 5 percent of a Nafion solution to obtain a catalyst material, and uniformly smearing a waterproof breathable film with the catalyst; placing the processed Nafion film into the water bath; laminating the waterproof breathable film which is coated with the catalyst as well as a reference electrode and a counter electrode which are prepared by using an identical method onto the Nafion film for hot pressing, storing the pressed Nafion film at room temperature to obtain the electrochemical carbon oxide gas sensor electrode. The sensor is high in sensitivity, short in response time and good in output linearity.
Description
Technical field
The invention belongs to areas of information technology, specifically, belong to sensor field, be a kind of electrochemistry co gas sensor
Electrode preparation method.
Background technology
In gas sensor domain, electrochemical sensor can meet the sensitivity and accuracy required for general detection,
Have again small volume, simple to operate, easy to carry, can be used for field monitoring and cheap, can be in detection by quantitative air
The advantages of gas pollutant, detected gas species are many, concentration range width, small volume, certainty of measurement are high, thus existing at present
Critically important status is occupied, in environmental monitoring with industrial obtained substantial amounts of application in all kinds of gas sensors.Traditional electricity
Chemical sensor adopts liquid electrolyte, the evaporation of electrolyte or pollution to lead to sensor signal to reduce, and service life is short.Institute
So that researcher directs one's energies to solid electrolyte, and for solid electrolyte, and catalyst and membrane treatment process just seem ten
Divide important.Therefore, the pass that preparation catalysis activity is high, the catalyst-nafion membrane electrode of stable performance is impact sensor performance
Key.
The sensitivity of sensor and response time depend on working electrode and to electrode.And working electrode and the property to electrode
Can determine, the activity improving catalyst is key problem in technology by the activity of catalyst.What general electrochemical sensor used urges
Agent material mostly is the noble metal powder binding agent such as platinum or gold or platinum-ruthenium alloys and is adhered to shape on solid dielectric film base material
Become electrode.It is to cause high cost using noble metal powder in a large number that such shortcoming mainly has two: the first；Second is bonding agent
Use can reduce the specific surface area of catalyst granules, reduce the activity of catalyst.The present invention is prepared for a kind of structure and property
Good c load ceo-cuo catalyst of fine quality it is achieved that the high catalytic effect to co gas in electrochemical system, with c as load
Material, and there is no the use of noble metal, considerably reduce cost, there is very high application prospect.
Content of the invention
For overcoming the deficiencies in the prior art, the present invention provides a kind of preparation side preparing electrochemistry co gas sensors electrode
Method.
A kind of preparation method of Electrochemical carbon monoxide gas sensors electrode is it is characterised in that urging of being used of electrode
Agent is superconduction carbon Supporting cerium oxide-copper oxide (ceo-cuo) catalyst, and base material is perfluorinated sulfonic acid ion exchange membrane (nafion
Film), its preparation process comprises step in detail below:
Step 1, weighs ce (no3)3·6h2O powder is transferred in beaker, then weighs cu (no3)2·3h2O powder is transferred to
In same beaker, then weigh excessive oxalic acid and be transferred in same beaker；It is then transferred to ball milling in ball mill, after taking-up
It is dried at 120 DEG C, be then transferred in mortar grind uniformly, stand-by；
Step 2, weighs the product in step 1, then weighs the superconduction carbon of equal in quality, is placed in stand-by in same beaker；
Step 3, the ammonia instilling in the beaker of step 2, after being stirred until homogeneous, it is put in water-bath, the colloid in beaker
Become dry and take out；
Step 4, the catalyst powder that step 3 is taken out moves in pottery, is then incubated in Muffle furnace, to be cooled
After take out, be then transferred in agate mortar to be ground to uniformly, be transferred in ceramic crucible, after room temperature standing, be added thereto to
5% nafion solution, is stirred until homogeneous, and is just made for catalyst material, then this catalyst with weighing scoop uniform application extremely
On waterproof ventilated membrane；
Step 5, is placed with the nafion film processing in the beaker of deionized water, puts into insulation in water-bath, then drags for
Go out, stand-by；
Step 6, in step 4 scribble catalyst waterproof ventilated membrane and using same procedure make reference electrode and
To electrode paste hot pressing on the nafion film being formed after step 4, room temperature decentralization after hot pressing is put, and is so just made for electrochemistry
CO gas sensor electrode.
Ce (the no weighing described in step 13)3·6h2O powder and cu (no3)2·3h2The atomic percent of o powder is 1/
19～1/4, described in ball mill Ball-milling Time be 6～10 hours, drying time is dry 8～10 hours.
Ammonia volume described in step 3 is 30～40ml/g catalyst；The temperature of water-bath is constant temperature, and temperature is between 70
～90 DEG C, the retention time is 6～8 hours.
The temperature of Muffle furnace described in step 4 is 500 DEG C, and temperature retention time is 3～5 hours；Described room temperature time of repose is 8
～12 hours；Described is applied in colloid catalyst on waterproof ventilated membrane, for being applied on 3 waterproof ventilated membranes, makees respectively
Use for working electrode, to electrode and reference electrode, waterproof ventilated membrane used is perfluorinated sulfonic acid ion exchange membrane (eptfe)
Film.
The nafion film processing described in step 5, described process is to carry out pretreatment to nafion film, nafion
Film is first placed into the h of the 5% of boiling2o2Boil in solution 50 minutes, to remove contained organic impuritiess, be then dipped in temperature again
For 2 hours in 80 DEG C of dilute sulfuric acids, carry out the protonation of nafion film, after deionized water rinses out the remaining acid solution on film surface
Put in deionized water, then stand-by；The water-bath of described specified temp refers to the water-bath that temperature is 80～100 DEG C, and insulation 1 is little
When.
Described in step 6, the waterproof ventilated membrane being sprayed with catalyst is attached on nafion film, refers to three waterproof ventilated membranes
It is attached to the both sides of nafion film respectively, side pastes one, opposite side pastes two, form three-electrode system.
The transducer sensitivity being made using the present invention is high, and response time is fast, and output linearity degree spy is good.The method institute
The electrode of preparation is used for sensor, selectivity and long-time stability are good, sensitivity is higher.
Brief description
Fig. 1 three-electrode system schematic diagram, 1 working electrode, 2 reference electrodes, 3 pairs of electrodes.
Fig. 2 is the scanning electron microscope (SEM) photograph of the catalyst of preparation in embodiment 1.
Fig. 3 is the output characteristics figure of the sensor making according to embodiment 1.
Specific embodiment
Although present disclosure has been made to be discussed in detail by the above, but it should be appreciated that the description above is not
It is considered as limitation of the present invention.After those skilled in the art have read the above, multiple for the present invention repair
Change and substitute and all will be apparent from.Therefore, protection scope of the present invention should be limited to the appended claims.
The embodiment that the present invention provides is as follows:
Embodiment 1: weigh 5.21 grams of ce (no3)3·6h2O powder, 0.73 gram of cu (no3)2·3h2O powder pours beaker into
In, then weigh 3.15 grams of oxalic acid and pour in same beaker, transfer to ball milling 8 hours in ball mill, then take out 120 DEG C and do
Dry 8 hours, be then transferred in mortar to be ground to uniformly, then weigh 0.1 gram of product and put in another container, thereto plus
The superconduction c powder entering 0.1 gram is poured in same beaker, till instilling 8ml ammonia, the colloid being stirred until homogeneous thereto, turns
Move to and keep in 70 DEG C of water-bath thoroughly vaporing away to ammonia for 8 hours, then cool down under room temperature, the powder body after cooling puts into porcelain boat
In, it is transferred in Muffle furnace 500 DEG C and be incubated 4 hours, then natural cooling, the powder after cooling is transferred in Achatess and is ground to all
Even, it is transferred in ceramic crucible, room temperature stands 8 hours, is added thereto to nation emulsion, stirs, uniform with weighing scoop
It is applied on three waterproof ventilated membranes；Nafion film is carried out with pretreatment again, first nafion film is first placed into seething with excitement 5%
h2o2Boil in solution 50 minutes, to remove contained organic impuritiess, be then dipped in the dilute sulfuric acid that temperature is 80 DEG C 2 less
When, carry out the protonation of nafion film, deionized water is put in deionized water after rinsing out the remaining acid solution on film surface, then turns
Move to the three waterproof ventilated membrane hot pressing taking out and being coated with catalyst after keeping 1 hour in the water-bath of boiling, form electrochemistry
Co gas sensor three-electrode system.Co gas is monitored, its response time is 11 seconds, sensitivity is 64.2na/ppm.
Fig. 2 is the scanning electron microscope (SEM) photograph of the catalyst electrode material done according to this embodiment, and Fig. 3 is the sensor in this, as electrode fabrication
Concentration-the current curve diagram of element.
Embodiment 2: weigh 7.38 grams of ce (no3)3·6h2O powder, 0.73 gram of cu (no3)2·3h2O powder pours beaker into
In, then weigh 3.78 grams of oxalic acid and pour in same beaker, transfer to ball milling 6 hours in ball mill, then take out 120 DEG C and do
Dry 9 hours, be then transferred in mortar to be ground to uniformly, then weigh 0.1 gram of product and put in another container, thereto plus
The superconduction c powder entering 0.1 gram is poured in same beaker, till instilling 7ml ammonia, the colloid being stirred until homogeneous thereto, turns
Move to and keep in 80 DEG C of water-bath thoroughly vaporing away to ammonia for 8 hours, then cool down under room temperature, the powder body after cooling puts into porcelain boat
In, it is transferred in Muffle furnace 500 DEG C and be incubated 4 hours, then natural cooling, the powder after cooling is transferred in Achatess and is ground to all
Even, it is transferred in ceramic crucible, room temperature stands 8 hours, is added thereto to nation emulsion, stirs, uniform with weighing scoop
It is applied on three waterproof ventilated membranes；Nafion film is carried out with pretreatment again, first nafion film is first placed into seething with excitement 5%
h2o2Boil in solution 50 minutes, to remove contained organic impuritiess, be then dipped in the dilute sulfuric acid that temperature is 80 DEG C 2 less
When, carry out the protonation of nafion film, deionized water is put in deionized water after rinsing out the remaining acid solution on film surface, then turns
Move to the three waterproof ventilated membrane hot pressing taking out and being coated with catalyst after keeping 1 hour in the water-bath of boiling, form electrochemistry
Co gas sensor three-electrode system.Co gas is monitored, its response time is 10 seconds, sensitivity is 68.7na/ppm.
Embodiment 3: weigh 37.13 grams of ce (no3)3·6h2O powder, 0.73 gram of cu (no3)2·3h2O powder pours beaker into
In, then weigh 11.22 grams of oxalic acid and pour in same beaker, transfer to ball milling 9 hours in ball mill, then take out 120 DEG C
It is dried 10 hours, be then transferred in mortar be ground to uniformly, then weigh 0.1 gram of product and put in another container, Xiang Qi
The middle superconduction c powder adding 0.1 gram is poured in same beaker, instills 8ml ammonia thereto, and the colloid being stirred until homogeneous is
Only, it is transferred in 80 DEG C of water-bath and keeps thoroughly vaporing away to ammonia for 8 hours, then cool down under room temperature, the powder body after cooling is put
Enter in porcelain boat, be transferred in Muffle furnace 500 DEG C and be incubated 4 hours, then natural cooling, the powder after cooling is transferred in Achatess and grinds
It is milled to uniformly, is transferred in ceramic crucible, room temperature stands 8 hours, is added thereto to nation emulsion, stirs, with weighing
Spoon is uniformly applied on three waterproof ventilated membranes；Again pretreatment is carried out to nafion film, first nafion film is first placed into seething with excitement
5% h2o2Boil in solution 50 minutes, to remove contained organic impuritiess, be then dipped in the dilute sulfuric acid that temperature is 80 DEG C again
In 2 hours, carry out the protonation of nafion film, deionized water puts into deionized water after rinsing out the remaining acid solution on film surface
In, transfer to the three waterproof ventilated membrane hot pressing taking out and being coated with catalyst after keeping 1 hour in the water-bath of boiling, formed
Electrochemistry co gas sensor three-electrode system.Co gas is monitored, its response time is 9 seconds, sensitivity is 60.9na/
ppm.
Embodiment 4: weigh 7.82 grams of ce (no3)3·6h2O powder, 0.73 gram of cu (no3)2·3h2O powder pours beaker into
In, then weigh 4.03 grams of oxalic acid and pour in same beaker, transfer to ball milling 10 hours in ball mill, then take out 120 DEG C
It is dried 9 hours, be then transferred in mortar be ground to uniformly, then weigh 0.1 gram of product and put in another container, thereto
The superconduction c powder adding 0.1 gram is poured in same beaker, till instilling 8ml ammonia, the colloid being stirred until homogeneous thereto,
It is transferred in 90 DEG C of water-bath and keeps thoroughly vaporing away to ammonia for 8 hours, then cool down under room temperature, the powder body after cooling puts into porcelain
In boat, it is transferred in Muffle furnace 500 DEG C and is incubated 4 hours, then natural cooling, the powder after cooling is transferred in Achatess and is ground to
Uniformly, it is transferred in ceramic crucible, room temperature stands 8 hours, is added thereto to nation emulsion, stirs, equal with weighing scoop
Even it is applied on three waterproof ventilated membranes；Nafion film is carried out with pretreatment again, first nafion film is first placed into the 5% of boiling
H2o2Boil in solution 50 minutes, to remove contained organic impuritiess, be then dipped in again 2 in the dilute sulfuric acid that temperature is 80 DEG C
Hour, carry out the protonation of nafion film, deionized water is put in deionized water after rinsing out the remaining acid solution on film surface, then
It is transferred to the three waterproof ventilated membrane hot pressing taking out and being coated with catalyst after keeping 1 hour in the water-bath of boiling, form electrification
Learn co gas sensor three-electrode system.Co gas is monitored, its response time is 8 seconds, sensitivity is 67.1na/ppm.
Embodiment 5: weigh 9.12 grams of ce (no3)3·6h2O powder, 0.725 gram of cu (no3)2·3h2O powder pours beaker into
In, then weigh 4.41 grams of oxalic acid and pour in same beaker, transfer to ball milling 8 hours in ball mill, then take out 120 DEG C and do
Dry 8 hours, be then transferred in mortar to be ground to uniformly, then weigh 0.1 gram of product and put in another container, thereto plus
The superconduction c powder entering 0.1 gram is poured in same beaker, till instilling 7ml ammonia, the colloid being stirred until homogeneous thereto, turns
Move to and keep in 80 DEG C of water-bath thoroughly vaporing away to ammonia for 8 hours, then cool down under room temperature, the powder body after cooling puts into porcelain boat
In, it is transferred in Muffle furnace 500 DEG C and be incubated 4 hours, then natural cooling, the powder after cooling is transferred in Achatess and is ground to all
Even, it is transferred in ceramic crucible, room temperature stands 8 hours, is added thereto to nation emulsion, stirs, uniform with weighing scoop
It is applied on three waterproof ventilated membranes；Nafion film is carried out with pretreatment again, first nafion film is first placed into seething with excitement 5%
h2o2Boil in solution 50 minutes, to remove contained organic impuritiess, be then dipped in the dilute sulfuric acid that temperature is 80 DEG C 2 less
When, carry out the protonation of nafion film, deionized water is put in deionized water after rinsing out the remaining acid solution on film surface, then turns
Move to the three waterproof ventilated membrane hot pressing taking out and being coated with catalyst after keeping 1 hour in the water-bath of boiling, form electrochemistry
Co gas sensor three-electrode system.Co gas is monitored, its response time is 10 seconds, sensitivity is 65.8na/ppm.
Embodiment 6: weigh 10.42 grams of ce (no3)3·6h2O powder, 0.725 gram of cu (no3)2·3h2O powder pours beaker into
In, then weigh 5.04 grams of oxalic acid and pour in same beaker, transfer to ball milling 8 hours in ball mill, then take out 120 DEG C and do
Dry 10 hours, it is then transferred in mortar be ground to uniformly, then weighs 0.1 gram of product and put in another container, thereto
The superconduction c powder adding 0.1 gram is poured in same beaker, till instilling 8ml ammonia, the colloid being stirred until homogeneous thereto,
It is transferred in 70 DEG C of water-bath and keeps thoroughly vaporing away to ammonia for 8 hours, then cool down under room temperature, the powder body after cooling puts into porcelain
In boat, it is transferred in Muffle furnace 500 DEG C and is incubated 4 hours, then natural cooling, the powder after cooling is transferred in Achatess and is ground to
Uniformly, it is transferred in ceramic crucible, room temperature stands 8 hours, is added thereto to nation emulsion, stirs, equal with weighing scoop
Even it is applied on three waterproof ventilated membranes；Nafion film is carried out with pretreatment again, first nafion film is first placed into the 5% of boiling
H2o2Boil in solution 50 minutes, to remove contained organic impuritiess, be then dipped in again 2 in the dilute sulfuric acid that temperature is 80 DEG C
Hour, carry out the protonation of nafion film, deionized water is put in deionized water after rinsing out the remaining acid solution on film surface, then
It is transferred to the three waterproof ventilated membrane hot pressing taking out and being coated with catalyst after keeping 1 hour in the water-bath of boiling, form electrification
Learn co gas sensor three-electrode system.Co gas is monitored, its response time is 7 seconds, sensitivity is 63.6na/ppm.
Claims (1)
1. a kind of preparation method of Electrochemical carbon monoxide gas sensors electrode is it is characterised in that the catalysis that used of electrode
Agent is superconduction carbon Supporting cerium oxide-copper oxide (ceo2- cuo) catalyst, base material is perfluorinated sulfonic acid ion exchange membrane (nafion
Film), its preparation process comprises step in detail below:
Step 1, weighs ce (no3)3·6h2O powder is transferred in beaker, then weighs cu (no3)2·3h2O powder is transferred to same
In individual beaker, then weigh excessive oxalic acid and be transferred in same beaker；Be then transferred to ball milling in ball mill, after taking-up
It is dried at 120 DEG C, be then transferred in mortar grind uniformly, stand-by；
Step 2, weighs the product in step 1, then weighs the superconduction carbon of equal in quality, is placed in stand-by in same beaker；
Step 3, the ammonia instilling in the beaker of step 2, after being stirred until homogeneous, it is put in water-bath, the colloid in beaker becomes dry
Take out；
Step 4, the catalyst powder that step 3 is taken out moves in pottery, is then incubated in Muffle furnace, takes after cooling
Go out, be then transferred in agate mortar be ground to uniformly, be transferred in ceramic crucible, after room temperature standing, be added thereto to 5%
Nafion solution, is stirred until homogeneous, and is just made for catalyst material, then this catalyst with weighing scoop uniform application to waterproof
On ventilated membrane；
Step 5, is placed with the nafion film processing in the beaker of deionized water, puts into insulation in water-bath, then pulls out, treat
With；
Step 6, scribbling the waterproof ventilated membrane of catalyst and adopting the reference electrode of same procedure making and to electricity in step 4
Pole is attached to hot pressing on the nafion film being formed after step 4, and room temperature decentralization after hot pressing is put, and is so just made for electrochemistry one oxygen
Change carbon gas sensors electrode；
Ce (the no weighing described in step 13)3·6h2O powder and cu (no3)2·3h2The atomic percent of o powder be 1/19～
1/4, ce (no3)3·6h2O and cu (no3)2·3h2The molal quantity sum of o is divided by h2c2o4Molal quantity value be less than 3: 4；Institute
Stating Ball-milling Time in ball mill is 6～10 hours, and drying time is dry 8～10 hours；
Ammonia volume described in step 3 is 30～40ml/g catalyst；The temperature of water-bath is constant temperature, and temperature is between 70～90
DEG C, the retention time is 6～8 hours；
The temperature of Muffle furnace described in step 4 is 500 DEG C, and temperature retention time is 3～5 hours；Described room temperature time of repose is 8～12
Hour；Described is applied in colloid catalyst on waterproof ventilated membrane, for being applied on 3 waterproof ventilated membranes, respectively as work
Make electrode, electrode and reference electrode are used, waterproof ventilated membrane used is expanded PTFE (eptfe) film；
The nafion film processing described in step 5, described process is to carry out pretreatment to nafion film, and nafion film is first
First put into the 5% of boiling h2o2Boil in solution 50 minutes, to remove contained organic impuritiess, being then dipped in temperature again is 80
DEG C dilute sulfuric acid in 2 hours, carry out the protonation of nafion film, deionized water is put into after rinsing out the remaining acid solution on film surface
In deionized water, then stand-by；The water-bath of described specified temp refers to the water-bath that temperature is 80～100 DEG C, is incubated 1 hour；
Described in step 6, the waterproof ventilated membrane being sprayed with catalyst is attached on nafion film, refers to three waterproof ventilated membranes respectively
It is attached to the both sides of nafion film, side pastes one, opposite side pastes two, form three-electrode system.
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| CN108445060B (en) * | 2018-03-19 | 2020-02-14 | 广东华晟安全职业评价有限公司 | Preparation method of sensor electrode for detecting formaldehyde content in air |
| CN111793393B (en) * | 2020-06-29 | 2022-03-08 | 重庆第二师范学院 | Nanocomposite material, glassy carbon composite electrode, manufacturing methods of nanocomposite material and glassy carbon composite electrode, and electrochemical sensor |
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| CN101435790A (en) * | 2008-12-22 | 2009-05-20 | 中国科学院长春应用化学研究所 | Method for preparing multiple-electrode electrochemical gas sensor |
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