CN113588738A - Ultrathin all-solid-state formaldehyde electrochemical gas sensor - Google Patents
Ultrathin all-solid-state formaldehyde electrochemical gas sensor Download PDFInfo
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Images
Classifications
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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
-
- 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
-
- 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
- G01N27/301—Reference electrodes
Abstract
The invention belongs to the field of electrochemical formaldehyde detection, and particularly relates to an ultrathin all-solid-state formaldehyde electrochemical gas sensor which comprises an electrode and a solid electrolyte, wherein the electrode comprises a working electrode, a reference electrode and a counter electrode, a catalyst layer is arranged between each electrode and the solid electrolyte, the catalyst layer is made of specific slurry, and the specific slurry is slurry formed by mixing a single-wall carbon nanotube, graphene, platinum, rhodium, palladium, silver, nano tin oxide, copper oxide, titanium dioxide, cobalt oxide, nano silicon dioxide and nafion solution with a PVDF solution, and has the viscosity of 300/pa.s and the solid mass fraction of 30-45%. The invention has high anti-interference performance and is suitable for real-time detection of formaldehyde in daily life.
Description
Technical Field
The invention belongs to the field of electrochemical formaldehyde detection, and particularly relates to a selective ultrathin all-solid-state formaldehyde electrochemical gas sensor.
Background
Formaldehyde pollution has become an unavoidable reality in urban resident life all over the world. Formaldehyde has a strong three-fold effect: teratogenicity, carcinogenesis and mutagenicity, which are derived from the release of interior construction, finishing materials and the like. Investigation shows that most of indoor formaldehyde concentration exceeds the standard, and especially the formaldehyde concentration of a newly-decorated room can be dozens of times or higher than the standard, so that the research on the detection and elimination of formaldehyde in indoor air has very important practical significance on the health of modern human beings.
The electrochemical analysis method is a currently common formaldehyde detection method, namely formaldehyde content is reacted by measuring voltage and current changes after formaldehyde reacts with specified substances, and the formaldehyde concentration is further displayed by processing signals at the later stage. The method has the advantages of simple equipment, rapidness, low cost, high sensitivity, wide measurement range and the like, and has the biggest defect of weak anti-interference capability, and under the condition that multiple gases exist simultaneously, the detection method is easy to generate larger measurement errors, so that the actual content of the formaldehyde gas in the environment cannot be effectively detected.
Disclosure of Invention
The invention aims to provide an ultrathin all-solid-state formaldehyde electrochemical gas sensor, a preparation method of a solid electrolyte slurry material and an assembly process. The sensor has high anti-interference performance and is suitable for real-time detection of formaldehyde in daily life.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
an ultrathin all-solid-state formaldehyde electrochemical gas sensor comprises an electrode and a solid electrolyte, wherein the electrode comprises a working electrode, a reference electrode and a counter electrode, a catalyst layer is arranged between each electrode and the solid electrolyte, the catalyst layer is made of specific slurry, and the specific slurry is slurry formed by mixing single-walled carbon nanotube, graphene, platinum, rhodium, palladium, silver, nano tin oxide, copper oxide, titanium dioxide, cobalt oxide, nano silicon dioxide, nafion solution and PVDF solution, and has the viscosity of 300/pa.s and the solid mass fraction of 30-45%.
The ultrathin all-solid-state formaldehyde electrochemical gas sensor adopts the improved catalyst layer, and experiments prove that the improved catalyst layer can improve the selectivity of the whole sensor for formaldehyde, and has higher response value for formaldehyde under the condition of the same concentration.
Further, the air-permeable insulating substrate is used as a carrier.
Selecting a substrate of an inorganic material having a gas-permeable function, said substrate having a resistivity of 1 x 1014-1×1015The length of the omega-cm is equal to or more than omega cm,the substrate has good mechanical strength, insulating property and processability, the porosity is 30-90%, and the pore diameter is 10-100 microns. The thickness of the substrate is between 0.1 and 2 mm.
Further, the electrode is made of conductive slurry, and the conductive slurry contains one or more conductive materials of nano silver, graphene, carbon nano tubes, nano gold and nano copper.
Further, the electrodes are interdigital electrodes.
Furthermore, the solid electrolyte adopts nafion solution, PEO, nano-cellulose, nano-alumina and nano-silica to form slurry with the viscosity of 100-300/pa.S, and the solid mass fraction is between 20 and 40 percent.
Further, the substrate is made of alumina, silica, glass fiber, basalt fiber and low-temperature co-sintered ceramic.
Drawings
FIG. 1 is a schematic cross-sectional view of an embodiment of an ultra-thin all-solid formaldehyde electrochemical gas sensor of the present invention.
FIG. 2 is a schematic diagram of an all-solid-state gas sensor with a reference electrode, a working electrode and a counter electrode on the same side.
Fig. 3 is an enlarged schematic diagram of the reference electrode, the working electrode and the counter electrode of the all-solid-state gas sensor.
Fig. 4 is a diagrammatic cross-sectional view of a structural variant corresponding to fig. 1.
FIG. 5 is a graph showing the results of the response test of the present invention for formaldehyde and various concentrations of interfering gases.
FIG. 6 is a graph comparing the response of the present invention to a commercially available conventional formaldehyde sensor for 1ppm interfering gas.
Detailed Description
The following is a more detailed description of embodiments, taken in conjunction with the accompanying drawings of which:
the reference numbers in the drawings include: counter electrode 1, working electrode 2, reference electrode 3, catalysis layer 4, solid-state electrolyte 5, base plate 6, conducting electrode 7.
Examples
As shown in fig. 1 and 2, the all-solid-state formaldehyde electrochemical gas sensor of the present embodiment has a main structure of a substrate, a solid electrolyte, a catalyst layer, and an electrode, which are sequentially disposed. Wherein the electrodes comprise a counter electrode, a working electrode, a reference electrode and a conductive electrode, and all the electrodes are basically positioned on the same surface.
The substrate is an inorganic material substrate with a ventilation function, has good mechanical strength, insulation and processability, and has the porosity of 30-90% and the pore diameter of 10-100 microns. The thickness of the substrate is between 0.1 and 2 mm;
the counter electrode, the working electrode and the reference electrode of the all-solid-state formaldehyde electrochemical gas sensor of the embodiment adopt commercial conductive paste, the conductive paste may include multiple mixed conductive materials such as nano silver, graphene, carbon nanotube, nano gold and nano copper or a single conductive material, and the conductive paste is sprayed on the substrate by screen printing, spraying, spin coating, or other methods to form the shape of the interdigital electrode, or a single planar state (as shown in fig. 3), and is printed with the conductive electrode (see fig. 2), and the thickness of the printed conductive electrode is 10-200 micrometers.
The catalyst layer has a selective catalytic effect on formaldehyde, and the adopted slurry is formed by mixing a single-walled carbon nanotube, graphene, platinum Pt, rhodium Rh, palladium Pd, silver Ag, nano tin oxide, copper oxide, titanium dioxide, cobalt oxide, nano silicon dioxide, nafion solution and PVDF solution, wherein the viscosity of the slurry is 100-pa.s, and the solid content of the slurry is 30-45%. The catalytic layer is formed on the counter electrode to a thickness of 30 to 100 μm by screen printing, spray coating, spin coating, or the like. The peripheral area of the catalyst layer is larger than that of the counter electrode, and the catalyst layer is in a shape of a full-coverage circle, a square or the like.
The solid electrolyte is formed by mixing nafion, PEO, nano-cellulose, nano-alumina and nano-silica according to a certain proportion to form slurry with the viscosity of 100-300/pa.S, the solid content is 20-40%, the slurry is formed on the catalyst layer by spraying, spin coating, screen printing and other modes, and the thickness is 300-500 microns. The covered peripheral area is larger than the catalytic layer area. The shape of the solid electrolyte is a full coverage circle, square, etc.
When the electrode, the catalytic layer and the solid electrolyte are arranged on the substrate, the drying is carried out in a vacuum drying oven at the temperature of 60-120 ℃ for 8-24 hours.
The catalyst layer and the solid electrolyte of the all-solid-state formaldehyde electrochemical gas sensor are formed by coating slurry, the thickness can be conveniently controlled, and the total thickness of the substrate can be controlled
The preparation method comprises the following steps:
1. and preparing solid electrolyte slurry. First weigh 2-3 grams of nanocellulose (increasing specific surface area while possessing more hydroxyl and carboxyl groups favoring H+Migration of (d), 0.5 g of nano alumina, 0.25 g of nano silica, 0.25 g of citric acid, 0.5 g of PVDF powder were mixed in a ball mill for more than 2 hours to prepare a mixture S1.
2. Mixing 5% nafion117 solution, NMP, deionized water, NMP and absolute ethyl alcohol according to a certain volume ratio of 2:0.5:1:0.25:1 to form liquid Y1.
3. S1 was added to Y1 and stirred constantly to form solid electrolyte slurry J1. And the viscosity of the solution is controlled by dripping absolute ethyl alcohol, so that the solution is suitable for screen printing.
4. The solid electrolyte paste was printed on the substrate or the counter electrode on the substrate to a thickness of 50 μm.
5. And drying the printed solid electrolyte in a vacuum drying oven at 60-80 ℃ for 8 hours.
7. Preparation of catalyst layer slurry, 5g of HEC was added to deionized water, and stirred with a magnetic stirrer at 50 ℃ for 6 hours to prepare 5% HEC colloid.
8. 0.8 g of Pt black, 0.05 g of nano titanium dioxide, 0.15 g of nano tin oxide, 0.15 g of nano silicon dioxide (hydrophilic), 1.2 g of 10% commercialized Nafion emulsion (from dupont) were added, magnetic stirring was performed for 4 hours, the HEC colloidal solution prepared at the previous stage was dropped, 1ml of absolute ethanol was added, and magnetic stirring was performed at 25 ℃ for 12 hours at room temperature to prepare a screen printing paste.
9. The prepared catalyst layer slurry is printed on a solid electrolyte on a substrate according to a designed shape (circular or square), the printing thickness is 40 micrometers, and the printed solid electrolyte is dried for 8 hours at 70-80 ℃ in a vacuum drying oven.
10. And preparing a working electrode, a reference electrode and a counter electrode. Various mixed conductive materials or single conductive paste materials such as commercial conductive silver paste (sold by Shanghai Polylon electronic technology Co., Ltd.), graphene, carbon nano tubes, nano gold, nano copper and the like are adopted, the shapes of all electrodes are designed (as shown in figure 3, the electrodes can be interdigital electrodes or plane sheets), the thickness of the conductive electrodes (generally conductive carbon black or metal gold) is printed to be 30 micrometers through screen printing, the conductive electrodes are kept in a vacuum drying oven for 10 minutes after each electrode printing, and the temperature is 80-100 ℃.
And (3) interference resistance testing: the ultra-thin all-solid-state formaldehyde electrochemical gas sensor adopts a static injection device, standard air is injected into a test gas test box, and the standard air is respectively injected according to a determined volume. The gas to be tested included 10ppm of toluene, 10ppm of ammonia, 1000ppm of oxygen, 1000ppm of hydrogen, 1000ppm of methane, 1000ppm of ethanol and 1000ppm of acetone in addition to 10ppm of formaldehyde, and the test temperature was 25 ℃. The response to the interfering gas is shown in fig. 5, corresponding to the response value (unit: mA).
A commercial product comparison test is carried out, and the ultrathin all-solid-state formaldehyde electrochemical sensor manufactured by the method is used for carrying out a response comparison test on 1ppm of interference gas and a commercial traditional formaldehyde sensor. The results are shown in FIG. 6.
Therefore, the ultrathin all-solid-state formaldehyde electrochemical gas sensor has very obvious selectivity on formaldehyde gas, and has the effect of effectively avoiding the interference of other gases compared with a common formaldehyde sensor (a formaldehyde gas sensor RS485 CH2O produced by Fukat technology in the embodiment) sold in the market in the prior art.
Although the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be construed as limiting the present invention, but various modifications or alterations thereof will become apparent to those skilled in the art upon reading the above description, and therefore the scope of the present invention should be defined by the appended claims. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several modifications and improvements can be made, such as changing the position structure of each layer to the structure shown in fig. 4, installing a housing for protecting each element outside the sensor, and/or changing the relative positions of each electrode on the catalytic layer (centering the counter electrode, and separating the reference electrode and the working electrode on both sides) should also be considered as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent.
The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (6)
1. The utility model provides an ultra-thin full solid-state formaldehyde electrochemical gas sensor, includes electrode and solid electrolyte, and the electrode includes working electrode, reference electrode and counter electrode, its characterized in that: a catalyst layer is arranged between each electrode and the solid electrolyte, the catalyst layer is made of specific slurry, and the specific slurry is slurry formed by mixing single-wall carbon nano-tubes, graphene, platinum, rhodium, palladium, silver, nano tin oxide, copper oxide, titanium dioxide, cobalt oxide, nano silicon dioxide, nafion solution and PVDF solution, wherein the viscosity of the slurry is 100-pa-s, and the solid mass fraction of the slurry is 30-45%.
2. The ultra-thin all-solid-state formaldehyde electrochemical gas sensor of claim 1, wherein: also includes a gas-permeable insulating substrate as a carrier.
3. The ultra-thin all-solid-state formaldehyde electrochemical gas sensor of claim 1, wherein: the electrode is made of conductive slurry, and the conductive slurry contains one or more conductive materials of nano silver, graphene, carbon nano tubes, nano gold and nano copper.
4. The ultra-thin all-solid-state formaldehyde electrochemical gas sensor of claim 1, wherein: the electrodes are interdigital electrodes.
5. The ultra-thin all-solid-state formaldehyde electrochemical gas sensor of claim 1, wherein: the solid electrolyte adopts slurry with the viscosity of 100-.
6. The ultra-thin all-solid-state formaldehyde electrochemical gas sensor of claim 2, wherein: the substrate is made of alumina, silicon dioxide, glass fiber, basalt fiber and low-temperature co-sintered ceramic.
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| CN111307914A (en) * | 2018-12-11 | 2020-06-19 | 上海苏萨电子科技有限公司 | Working electrode, preparation method thereof and formaldehyde sensor comprising working electrode |
| CN111600067A (en) * | 2020-04-10 | 2020-08-28 | 北京理工大学 | High-temperature solid electrolyte and preparation method and application thereof |
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2021
- 2021-07-29 CN CN202110866623.7A patent/CN113588738A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| TW201012292A (en) * | 2008-09-08 | 2010-03-16 | Univ Feng Chia | Electrochromic device and fabrication method thereof |
| CN105092646A (en) * | 2015-08-19 | 2015-11-25 | 电子科技大学 | Graphene/metal oxide composite film gas sensor and preparation method |
| CN106093164A (en) * | 2016-07-11 | 2016-11-09 | 郑州炜盛电子科技有限公司 | Room temperature solid electrolyte CO2 sensor and preparation method thereof |
| CN108445060A (en) * | 2018-03-19 | 2018-08-24 | 广东华晟安全职业评价有限公司 | A kind of preparation method of the sensor electrode of detection formaldehyde in air content |
| CN111307914A (en) * | 2018-12-11 | 2020-06-19 | 上海苏萨电子科技有限公司 | Working electrode, preparation method thereof and formaldehyde sensor comprising working electrode |
| CN111600067A (en) * | 2020-04-10 | 2020-08-28 | 北京理工大学 | High-temperature solid electrolyte and preparation method and application thereof |
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