CN113219006A - Gas sensor, preparation method thereof and wearable electronic device - Google Patents
Gas sensor, preparation method thereof and wearable electronic device Download PDFInfo
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- CN113219006A CN113219006A CN202110411662.8A CN202110411662A CN113219006A CN 113219006 A CN113219006 A CN 113219006A CN 202110411662 A CN202110411662 A CN 202110411662A CN 113219006 A CN113219006 A CN 113219006A
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- 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
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
Abstract
The invention discloses a gas sensor, comprising: a paper-based substrate; the gas induction layer is arranged on the paper-based substrate and is a composite layer consisting of rGO and ZnO nano materials; and the electrode is arranged on the gas induction layer. The gas sensor combines the excellent gas sensitivity of rGO and ZnO, can work at room temperature, avoids the high temperature on the surface when an additional heating device and the sensor work, and can be used for low-concentration NO at room temperature2The gas has higher detection sensitivity.
Description
Technical Field
The invention belongs to the technical field of gas detection, and particularly relates to a gas sensor, a preparation method of the gas sensor and wearable electronic equipment.
Background
With the continuous advance of social industrialization, the composition of the polluted gas in the air is continuously increased. Due to the demands of environmental protection and air quality monitoring in special occasions such as factories, the detection technology of toxic and harmful gases in the air attracts more and more attention and research and development, and the gas sensor is a leading-edge technology which is disputed by vast researchers to develop and research, is used for detecting the concentration and components of gases and plays an important role in the aspects of environmental protection and safety supervision.
NO2Is one of nitrogen oxide pollutants, which is one of the causes of acid rain, and can also reduce atmospheric visibility, acidify surface water, eutrophicate surface water (due to oxygen deficiency caused by massive proliferation of algae rich in nutrients such as nitrogen and phosphorus), and increase the content of toxins harmful to fish and other aquatic organisms in water, thereby treating NO2Gas detection is particularly important, but existing gas sensors are sensitive to low concentrations of NO at room temperature2Has low detection sensitivity, so that the development of a method for detecting NO at a low concentration at room temperature is urgently required2The gas sensor with higher detection sensitivity.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. To this end, the invention proposes a gas sensor which is sensitive to low concentrations of NO at room temperature2Has higher detection sensitivity.
The technical purpose of the invention is realized by the following technical scheme:
a gas sensor, comprising: a paper-based substrate; the gas induction layer is arranged on the paper-based substrate and is a composite layer consisting of rGO and ZnO nano materials; and the electrode is arranged on the gas induction layer.
Specifically, the ZnO nano material is an n-type semiconductor with the forbidden band width of 3.37eV, has a wurtzite structure, has the exciton binding energy of 60meV at room temperature, has the advantages of low cost, NO toxicity, rich content, good stability and biocompatibility, excellent electrical property and the like, and can react with NO in the air at a proper temperature2The gas undergoes electron transfer, so its resistance follows NO in the air2The concentration changes obviously, but the ZnO nano material has the defects of lower responsivity, higher working temperature and the like, and can be used for treating low-concentration NO at room temperature2The detection sensitivity of (2) is low.
The rGO is reduced graphene oxide and is obtained by reducing GO (reduced graphene), has the advantages of low density, high specific surface area, high electron mobility at room temperature and high thermal stability, and is prepared by mixing the rGO and ZnO nano-materialsThe composite layer formed by the materials is used as a gas sensing layer of the gas sensor, and the advantages of rGO and ZnO can be integrated, so that the gas sensor can be used for low-concentration NO at room temperature2Has higher detection sensitivity.
Meanwhile, the gas sensor is a paper-based substrate, so that the gas sensor has better flexibility, the convenience of the gas sensor in the field of wearable electronic equipment is greatly improved, and the gas sensor can be well attached to the wearable electronic equipment.
Preferably, the paper-based substrate is filled with a compound consisting of rGO and ZnO nano materials.
Specifically, due to the loose and porous structure of the paper-based substrate, a compound formed by the rGO and the ZnO nano material in the paper-based substrate can be in contact with detected gas to participate in the gas-sensitive process, so that the surface area of the sensing gas is increased, the electrical characteristic change range of the gas-sensitive element is increased, and the sensitivity of the gas-sensitive sensor is improved.
Preferably, the ZnO nano material is doped with Fe.
Specifically, when the gas sensing layer is composed of a composite layer formed by rGO, ZnO nano materials and Fe doping, the gas sensor can not only sense low-concentration NO at room temperature2The gas has excellent detection sensitivity, and also has excellent detection sensitivity to formaldehyde gas with low concentration at room temperature.
Preferably, the paper-based substrate is filled with a compound consisting of rGO and a ZnO nano material, and the ZnO nano material is doped with Fe.
Specifically, the paper-based substrate has a loose and porous structure, so that a compound formed by doping rGO, ZnO nano materials and Fe in the paper-based substrate can be contacted with detected gas to participate in the gas-sensitive process, the surface area of the sensing gas is increased, the change range of the electrical characteristics of the gas-sensitive sensor is increased, and the sensitivity of the gas-sensitive sensor is improved.
Preferably, the paper-based substrate is aramid paper.
Specifically, the aramid paper has good thermal stability, excellent mechanical properties and strong chemical corrosion resistance, so that the application of the gas sensor in more scenes can be effectively widened.
Preferably, the electrodes include a first electrode and a second electrode, and the first electrode and the second electrode are disposed at two opposite ends of the same side of the gas sensing layer.
Another object of the present invention is to provide a method for preparing the gas sensor, comprising:
a method for preparing a gas sensor as described above, comprising the steps of:
(1) mixing paper base liner pulp with GO suspension, and performing vacuum filtration to obtain a paper base liner filled inside and exposed with GO on the surface;
(2) soaking the paper-based substrate prepared in the step (1) in a precursor solution of a ZnO nano material for hydrothermal treatment, so that a composite layer consisting of rGO and the ZnO nano material, namely a gas induction layer, is formed on the surface of the paper-based substrate;
(3) and (5) mounting an electrode on the gas induction layer to obtain the sensor.
Concretely, mix back with paper base substrate pulp and GO suspension, vacuum filtration, can prepare the inside filling one step and whole surface exposes the paper base substrate that has GO, in addition, because paper base substrate has loose porous structure, when making to soak the paper base substrate that step (1) made in the precursor liquid of ZnO nano-material and carry out hydrothermal treatment, the GO on paper base substrate surface is reduced into rGO, when forming the rGO layer, the inside GO of paper base substrate also can be reduced into rGO, also can grow out the composite bed that the rGO layer of ZnO nano-material layer and the rGO layer formation rGO of paper base substrate surface and ZnO nano-material constitute in situ in the precursor liquid of ZnO nano-material simultaneously, form gaseous response layer promptly, the inside rGO complex of ZnO nano-material and paper base substrate forms rGO and the compound that the ZnO nano-material constitutes simultaneously.
Preferably, the ZnO nanomaterial in step (2) is Fe-doped ZnO nanoparticles.
Specifically, the prepared gas sensing layer of the gas sensor is a composite layer formed by doping rGO, ZnO nanoparticles and Fe, and the paper-based substrate is filled with a composite formed by doping rGO, ZnO nanoparticles and Fe.
Preferably, the ZnO nanomaterial in step (2) is a ZnO seed layer.
Specifically, the prepared gas sensing layer of the gas sensor is a composite layer consisting of rGO and ZnO nano-rods, and the paper-based substrate is filled with a composite consisting of rGO and ZnO nano-particles.
A third object of the present invention is to provide a wearable electronic device.
A wearable electronic device comprising a gas sensor as described above.
In particular, the wearable electronic equipment can be used for low-concentration NO at room temperature2The gas has higher detection sensitivity, thereby being convenient for NO in the environment2The gas is detected and monitored.
The invention has the beneficial effects that:
(1) the gas sensor disclosed by the invention takes the paper-based substrate with good flexibility as a substrate, combines the excellent gas sensitivity of rGO and ZnO, increases the surface area of induction gas, can work at room temperature, avoids the high temperature of the surface when an additional heating device and the sensor work, and can be used for low-concentration NO at room temperature2The detection sensitivity is higher;
(2) according to the preparation method of the gas sensor, the paper-based substrate pulp and the GO suspension are mixed, the paper-based substrate with GO on the surface and in the inner part is prepared through vacuum filtration, and then the GO is reduced into rGO in the process of preparing the ZnO nano material through in-situ growth by a hydrothermal method, so that the operation steps can be effectively reduced, the production efficiency is improved, and the production cost is reduced.
(3) The wearable electronic equipment provided by the invention is provided with the gas sensor, so that the wearable electronic equipment can be used for low-concentration NO at room temperature2The gas has higher detection sensitivity, thereby being convenient for NO in the environment2The gas is detected and monitored.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is an exploded view of a gas sensor according to example 1 of the present invention;
FIG. 2 is a schematic view of a gas sensor according to example 1 of the present invention;
FIG. 3 is an exploded view of a gas sensor according to example 2 of the present invention;
FIG. 4 is a schematic view of a gas sensor according to example 2 of the present invention;
FIG. 5 is an exploded view of a gas sensor according to example 3 of the present invention;
FIG. 6 is a schematic view of a gas sensor according to example 3 of the present invention.
Reference numerals:
100. aramid paper;
200. a gas sensing layer; 200a. rgo layer; a zno nanoparticle layer 200 b; 200c. a Fe-containing doped ZnO nanoparticle layer; 200d.ZnO nanorod layer;
300. an electrode; 301. and (4) silver paste blocks.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1:
a gas sensor, as shown in fig. 1-2, comprising: aramid paper 100, a gas sensing layer 200, and an electrode 300; gaseous response layer 200 sets up on aramid paper 100, and gaseous response layer 200 is the composite bed that rGO and ZnO nanoparticle constitute, and electrode 300 sets up on gaseous response layer 200, and aramid paper 100 intussuseption is filled with the compound that comprises rGO and ZnO nanoparticle, and electrode 300 includes first electrode and second electrode, and first electrode and second electrode set up in the relative both ends of gaseous response layer 200 with one side.
The preparation method of the gas sensor comprises the following steps:
(1) 60mL of aramid pulp with the concentration of 1mg-10mg/mL is prepared and then stirred by a glass rod to be uniformly distributed.
(2) Prepare 60mL GO suspension with concentration of 0.5-20mg/mL, then stir with a glass rod to make it distribute evenly.
(3) And mixing the aramid fiber pulp suspension and the GO suspension together, and then carrying out ultrasonic treatment on the mixed solution to uniformly mix the mixed solution.
(4) Vacuum filtering the mixture of aramid fiber pulp and GO suspension in a vacuum filtering device to obtain a mixture filled with the aramid fiber pulp and with an exposed density of 1.5-240mg/mm on the whole surface2Aramid paper 100 of GO in the range.
(5) And (3) compacting the obtained aramid fiber paper 100 at the temperature of 100-140 ℃, and maintaining for 30 min.
(6) Preparing 40mL of zinc nitrate solution with the concentration of 0.05-0.5mol/L, and magnetically stirring the solution uniformly at room temperature.
(7) Preparing 40mL of HMT (C) with the concentration of 0.05-0.5mol/L6H12N4) The solution is magnetically stirred evenly at room temperature.
(8) Mixing the above zinc nitrate solution with HMT (C)6H12N4) And mixing the solutions, and magnetically stirring the mixture uniformly at room temperature to prepare the precursor solution of the ZnO nanoparticles.
(9) And (3) transferring the mixed solution into an autoclave, soaking the aramid paper 100 prepared in the step (5) in the mixed solution with the right side facing upwards, sealing the autoclave, placing the autoclave in an oven at 80-100 ℃ for 6-8h, and carrying out hydrothermal treatment.
(10) After the hydrothermal is accomplished, take out aramid paper 100, at hydrothermal in-process, inside and surperficial GO of aramid paper 100 is reduced into rGO, and form rGO layer 200a on aramid paper 100 surface, and all grow with ZnO nanoparticle on the rGO on aramid paper inside and the surface, make and form ZnO nanoparticle layer 200b on rGO layer 200a, make aramid paper 100 surface form the composite bed of constituteing by rGO and ZnO nanoparticle, gaseous induction layer 200 promptly.
(11) The obtained aramid paper 100 is subjected to cleaning, drying, and aging treatment.
(12) Two platinum wires are respectively fixed at two ends of the gas sensing layer 200 on the front surface of the aramid paper 100 by silver paste blocks 301 to be used as electrodes 300 (a first electrode and a second electrode), and then the gas sensor is manufactured.
The gas sensor can be used for low-concentration NO at room temperature2Has higher detection sensitivity.
A wearable electronic device comprising a gas sensor as described above. The wearable electronic device can be used for controlling NO at room temperature2And (5) detecting the gas.
Example 2:
a gas sensor, as shown in fig. 3-4, comprising: aramid paper 100, a gas sensing layer 200, and an electrode 300; gaseous response layer 200 sets up on aramid paper 100, and gaseous response layer 200 is the composite bed that rGO, ZnO nanoparticle and Fe are constituteed, and electrode 300 sets up on gaseous response layer 200, and aramid paper 100 intussuseption is filled with the compound of constituteing by rGO, ZnO nanoparticle and Fe, and electrode 300 includes first electrode and second electrode, and first electrode and second electrode set up in the relative both ends of gaseous response layer 200 with one side.
The preparation method of the gas sensor comprises the following steps:
(1) 60mL of aramid pulp with the concentration of 1mg-10mg/mL is prepared and then stirred by a glass rod to be uniformly distributed.
(2) Prepare 60mL GO suspension with concentration of 0.5-20mg/mL, then stir with a glass rod to make it distribute evenly.
(3) And mixing the aramid fiber pulp suspension and the GO suspension together, and then carrying out ultrasonic treatment on the mixed solution to uniformly mix the mixed solution.
(4) Vacuum filtering the mixture of aramid fiber pulp and GO suspension in a vacuum filtering device to obtain a mixture filled with the aramid fiber pulp and with an exposed density of 1.5-240mg/mm on the whole surface2Aramid paper 100 of GO in the range.
(5) And (3) compacting the obtained aramid fiber paper 100 at the temperature of 100-140 ℃, and maintaining for 30 min.
(6) Weighing a certain amount of mixed solid of zinc sulfate and ferric chloride hexahydrate, wherein Fe3+With Zn2+Is between 1:40 and 1: 10.
(7) Dissolving the mixed solid of zinc sulfate and ferric chloride hexahydrate in 40mL of deionized water, wherein ZnSO is4The concentration of (A) is 0.05-0.5mol/L, and the mixture is magnetically stirred uniformly at room temperature.
(8) Preparing 40mL of HMT (C) with the concentration of 0.05-0.5mol/L6H12N4) The solution is magnetically stirred evenly at room temperature.
(9) Mixing the mixed solution of zinc sulfate and ferric chloride with hexamethylenetetramine HMT (C)6H12N4) And mixing the solution, and magnetically stirring the solution uniformly at room temperature to prepare the precursor solution of the ZnO nanoparticles doped with Fe.
(10) And (3) transferring the mixed solution into an autoclave, soaking the aramid paper 100 prepared in the step (5) in the mixed solution with the right side facing upwards, sealing the autoclave, placing the autoclave in an oven at 80-100 ℃ for 6-8h, and carrying out hydrothermal treatment.
(11) After the hydrothermal process, taking out the aramid paper 100, in the hydrothermal process, GO inside and on the surface of the aramid paper 100 is reduced into rGO, and an rGO layer 200a is formed on the surface of the aramid paper, ZnO nanoparticles doped with Fe with the concentration of 2.5-5.0 at% are grown on the rGO inside and on the surface of the aramid paper 100, so that a ZnO nanoparticle layer 200c doped with Fe is formed on the rGO layer 200a, and a composite layer formed by the rGO, the ZnO nanoparticles and the Fe is formed on the surface of the aramid paper 100, namely the gas induction layer 200.
(12) The obtained aramid paper 100 is subjected to cleaning, drying, and aging treatment.
(13) Two platinum wires are respectively fixed at two ends of the gas sensing layer 200 on the front surface of the aramid paper 100 by silver paste blocks 301 to be used as electrodes 300 (a first electrode and a second electrode), and then the gas sensor is manufactured.
The gas sensor can be used for low-concentration NO at room temperature2And formaldehyde gas has higher detection sensitivity.
A wearable electronic device comprising a gas sensor as described above. The wearable electronic device can be used for controlling NO at room temperature2And detecting the gas and the formaldehyde gas.
Example 3:
a gas sensor, as shown in fig. 5-6, comprising: aramid paper 100, a gas sensing layer 200, and an electrode 300; gaseous response layer 200 sets up on aramid paper 100, and gaseous response layer 200 comprises the compound that rGO and ZnO nano-rod are constituteed, and electrode 300 sets up on gaseous response layer 200, and aramid paper 100 intussuseption is filled with the compound that comprises rGO and ZnO nano-particle, and electrode 300 includes first electrode and second electrode, and first electrode and second electrode set up in the relative both ends of gaseous response layer 200 with one side.
The preparation method of the gas sensor comprises the following steps:
(1) 60mL of aramid pulp with the concentration of 1mg-10mg/mL is prepared and then stirred by a glass rod to be uniformly distributed.
(2) Prepare 60mL GO suspension with concentration of 0.5-20mg/mL, then stir with a glass rod to make it distribute evenly.
(3) And mixing the aramid fiber pulp suspension and the GO suspension together, and then carrying out ultrasonic treatment on the mixed solution to uniformly mix the mixed solution.
(4) Vacuum filtering the mixture of aramid fiber pulp and GO suspension in a vacuum filtering device to obtain a mixture filled with the aramid fiber pulp and with an exposed density of 1.5-240mg/mm on the whole surface2Aramid paper 100 of GO in the range.
(5) And (3) compacting the obtained aramid fiber paper 100 at the temperature of 100-140 ℃, and maintaining for 30 min.
(6) Preparing 40mL of zinc acetate solution with the concentration of 0.01-0.05mol/L, and magnetically stirring the solution uniformly at room temperature.
(7) 40mL of KOH solution with the concentration of 0.01-0.05mol/L is prepared, and the mixture is magnetically stirred uniformly at room temperature.
(8) And mixing the zinc acetate solution and the KOH solution, and magnetically stirring uniformly at room temperature to prepare the precursor solution of the ZnO seed layer.
(9) And (3) transferring the mixed solution into an autoclave, soaking the aramid paper 100 prepared in the step (5) in the mixed solution with the right side facing upwards, sealing the autoclave, placing the autoclave in an oven at 80-100 ℃ for 6-8h, and carrying out hydrothermal treatment.
(10) After hydrothermal, take out aramid paper 100, wash, dry, inside and surperficial GO of aramid paper 100 has been reduced into rGO to form rGO layer 200a on aramid paper surface, and all grow the granule of ZnO on the rGO on inside and the surface of aramid paper 100, the granule of the ZnO that grows on the rGO on aramid paper 100 surface, as the seed layer of follow-up growth ZnO nano-rod.
(11) Preparing 40mL of zinc nitrate solution with the concentration of 0.05-0.5mol/L, and magnetically stirring the solution uniformly at room temperature.
(12) Preparing 40mL of HMT (C) with the concentration of 0.05-0.5mol/L6H12N4) The solution is magnetically stirred evenly at room temperature.
(13) Mixing the zinc nitrate solution of the step (11) and the HMT (C) of the hexamethylenetetramine of the step (12)6H12N4) The solution is mixed and stirred magnetically at room temperature.
(14) And (3) transferring the mixed solution obtained in the step (11) into an autoclave, soaking the aramid fiber paper 100 prepared in the step (10) in the mixed solution with the right side facing upwards, sealing the autoclave, then placing the autoclave in an oven at 80-100 ℃ for 6-8h, and carrying out hydrothermal treatment.
(15) After the hydrothermal process, the aramid paper 100 is taken out, that is, the ZnO nanorod layer 200d is formed on the rGO layer 200a to form the gas sensing layer 200.
(16) The obtained aramid paper 100 is subjected to cleaning, drying, and aging treatment.
(17) Two platinum wires are respectively fixed at two ends of the gas sensing layer 200 on the front surface of the aramid paper 100 by silver paste blocks 301 to be used as electrodes 300 (a first electrode and a second electrode), and then the gas sensor is manufactured.
The gas sensor can be used for low-concentration NO at room temperature2The gas has higher detection sensitivity.
A wearable electronic device comprising a gas sensor as described above. The wearable electronic device can be used for controlling NO at room temperature2And (5) detecting the gas.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A gas sensor, comprising:
a paper-based substrate;
the gas induction layer is arranged on the paper-based substrate and is a composite layer consisting of rGO and ZnO nano materials;
and the electrode is arranged on the gas induction layer.
2. A gas sensor as claimed in claim 1, wherein: the paper-based substrate is filled with a compound consisting of rGO and ZnO nano materials.
3. A gas sensor as claimed in claim 1, said ZnO nanomaterial being doped with Fe.
4. A gas sensor as claimed in claim 3, wherein: the paper-based substrate is filled with a compound consisting of rGO and ZnO nano materials, and the ZnO nano materials are doped with Fe.
5. A gas sensor as claimed in claim 1, wherein: the paper-based substrate is aramid paper.
6. A gas sensor as claimed in claim 1, wherein: the electrodes comprise a first electrode and a second electrode, and the first electrode and the second electrode are arranged at two opposite ends of the same side of the gas induction layer.
7. A method for producing a gas sensor as claimed in any one of claims 1 to 6, characterized in that: the method comprises the following steps:
(1) mixing paper base liner pulp with GO suspension, and performing vacuum filtration to obtain a paper base liner filled inside and exposed with GO on the surface;
(2) soaking the paper-based substrate prepared in the step (1) in a precursor solution of a ZnO nano material for hydrothermal treatment, so that a composite layer consisting of rGO and the ZnO nano material, namely a gas induction layer, is formed on the surface of the paper-based substrate;
(3) and (5) mounting an electrode on the gas induction layer to obtain the sensor.
8. The method for preparing a gas sensor according to claim 7, wherein: and (3) in the step (2), the ZnO nano material is ZnO nano particles doped with Fe.
9. The method for preparing a gas sensor according to claim 7, wherein: and (3) the ZnO nano material in the step (2) is a ZnO seed layer.
10. A wearable electronic device, characterized in that: comprising a gas sensor as claimed in any of claims 1 to 6.
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