CN111458382A - Room-temperature flexible graphene oxide ordered porous film sensor and preparation method and application thereof - Google Patents
Room-temperature flexible graphene oxide ordered porous film sensor and preparation method and application thereof Download PDFInfo
- Publication number
- CN111458382A CN111458382A CN202010300755.9A CN202010300755A CN111458382A CN 111458382 A CN111458382 A CN 111458382A CN 202010300755 A CN202010300755 A CN 202010300755A CN 111458382 A CN111458382 A CN 111458382A
- Authority
- CN
- China
- Prior art keywords
- graphene oxide
- room
- ordered porous
- temperature flexible
- film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000004793 Polystyrene Substances 0.000 claims abstract description 58
- 239000004005 microsphere Substances 0.000 claims abstract description 43
- 229920002223 polystyrene Polymers 0.000 claims abstract description 31
- 239000011521 glass Substances 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000001035 drying Methods 0.000 claims abstract description 26
- 239000002131 composite material Substances 0.000 claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000000725 suspension Substances 0.000 claims abstract description 9
- 239000011248 coating agent Substances 0.000 claims abstract description 8
- 238000000576 coating method Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 229920000642 polymer Polymers 0.000 claims abstract description 8
- 239000002356 single layer Substances 0.000 claims abstract description 6
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 31
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 11
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 4
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- 239000002211 L-ascorbic acid Substances 0.000 claims description 2
- 235000000069 L-ascorbic acid Nutrition 0.000 claims description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 2
- 239000004677 Nylon Substances 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 229960005070 ascorbic acid Drugs 0.000 claims description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 2
- 229910000043 hydrogen iodide Inorganic materials 0.000 claims description 2
- 229920001778 nylon Polymers 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims 3
- 239000000243 solution Substances 0.000 description 26
- 230000004044 response Effects 0.000 description 11
- 230000035945 sensitivity Effects 0.000 description 8
- 239000010410 layer Substances 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000012266 salt solution Substances 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 206010037660 Pyrexia Diseases 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical class [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000004964 aerogel Substances 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Classifications
-
- 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
- G01N27/02—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
- G01N27/121—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 for determining moisture content, e.g. humidity, of the fluid
-
- 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
- G01N27/02—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
- G01N27/126—Composition of the body, e.g. the composition of its sensitive layer comprising organic polymers
-
- 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
- G01N27/02—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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention discloses a preparation method of a room temperature flexible graphene oxide ordered porous film sensor, which comprises the steps of uniformly coating a monodisperse crosslinked polystyrene microsphere suspension on a glass slide, drying, obliquely immersing the glass slide in water, separating out a single-layer polystyrene microsphere film, transferring the obtained film onto the liquid surface of a graphene oxide solution, reacting for 20min-1h to obtain a composite film, transferring the obtained composite film onto the water surface, heating the composite film to 80-100 ℃ in an oven, dripping a 10 mu L-1 m L reducing agent, reacting for 3-10min to obtain a composite film 2, covering the composite film 2 on a high polymer flexible material, taking out, drying to obtain a high polymer flexible substrate-loaded polystyrene and graphene oxide composite gas sensor, immersing the obtained gas sensor into a solvent capable of dissolving polystyrene microspheres for 10-15s, and drying at 60 ℃ to obtain the room temperature flexible graphene oxide ordered porous gas sensor.
Description
Technical Field
The invention relates to the technical field of gas sensors, in particular to a room-temperature flexible graphene oxide ordered porous film sensor and a preparation method and application thereof.
Background
Humidity sensors have received attention because they have a wide range of applications in the fields of production, process control, environmental monitoring, storage, and the like. The graphene has a two-dimensional planar structure, and the surface of the graphene contains a large amount of grapheneGraphene humidity sensors in the prior art mainly support semiconductors (e.g., SnO) by noble metal modification (e.g., Ag nanoparticle modification), metal doping (e.g., L i, B doping), and making graphene into aerogel2) The sensitivity of the graphene is improved in a nanoparticle mode, the preparation methods are complicated in steps, dependence on high temperature and a rigid substrate cannot be removed, and the improvement of the sensitivity is not obvious; in addition, in the chemical modification process, the original perfect atomic lattice of the original graphene oxide is affected by chemical bonds, thereby seriously affecting the inherent electrical properties of the graphene.
Disclosure of Invention
The invention aims to provide a method for preparing a graphene oxide ordered porous film gas-sensitive material based on a template induction method and a flexible room-temperature graphene oxide ordered porous gas sensor prepared by the method, which are used for solving the problems that the gas sensor prepared in the prior art is low in sensitivity, poor in response and recovery performance and capable of damaging the atomic lattice of original graphene oxide.
In order to achieve the purpose, the technical scheme provided by the invention is as follows: a preparation method of a room-temperature flexible graphene oxide ordered porous film sensor comprises the following steps:
(1) uniformly coating the monodisperse crosslinked polystyrene microsphere suspension on a clean glass slide, drying, slowly and obliquely immersing the glass slide into water, and separating out a single-layer polystyrene microsphere film;
(2) transferring the polystyrene microsphere film to the liquid surface of a graphene oxide solution, and obtaining a composite film of polystyrene and graphene oxide after 20min-1 h;
(3) transferring the composite film obtained in the step (2) to a water surface, putting the composite film on an oven to heat, dripping 10 mu L-1 m L reducing agent, and reacting for 3-10min to obtain a composite film 2;
(4) covering the composite film 2 on a high polymer flexible material, fishing out, and drying to obtain a gas sensor with a high polymer flexible substrate loaded with polystyrene and graphene oxide;
(5) and (5) immersing the gas sensor obtained in the step (4) into a solvent capable of dissolving polystyrene microspheres for 10-15s, and drying at 60 ℃ to obtain the room-temperature flexible graphene oxide ordered porous gas sensor.
The size of the monodisperse crosslinked polystyrene microsphere is 500-1000 nm. Under the size, the single-layer polystyrene microsphere films separated from the water surface are uniformly, firmly and orderly arranged. The size is small, and the single-layer film is not easy to separate; the size is large, and the single-layer film is easy to loosen.
The monodisperse crosslinked polystyrene microsphere is coated on a glass slide, and the coating area is 2-3cm × 4 cm.
The solid content of the graphene oxide solution is 0.1-1mg/ml, the solid content of the graphene oxide is within the range of 0.1-1mg/m L, a GO ordered porous film with a certain uniform thickness can be obtained, if the solid content is too small, GO cannot be well adsorbed, and if the solid content is too large, the adsorption is too fast, so that the film is too thick.
The sampling amount of the graphene oxide solution in the step (2) is 20ml, and the diameter of the culture dish is 60 mm.
The reducing agent in the step (3) is one or more of hydrogen iodide, hydrazine hydrate, L-ascorbic acid and ammonia water, the reduction time is designed to be 3min-10min, because if the reduction time is too short, the film resistance is too large and exceeds the measurement range of a gas sensitive tester, and if the reduction time is too long, the sensitivity of the reduced graphene oxide film to the measured water can be greatly reduced.
The polymer flexible substrate is one of a PET interdigital electrode, a PI interdigital electrode and a nylon wire.
The solvent capable of dissolving the polystyrene microspheres is one or more of dichloromethane, chloroform, tetrahydrofuran, N-dimethylformamide, cyclohexane and toluene.
The invention also aims to provide the room-temperature flexible graphene oxide ordered porous humidity sensor prepared by the method.
The invention also aims to provide a new application of the room-temperature flexible graphene oxide ordered porous humidity-sensitive sensor in detecting different motion states and heartbeats of a human body.
Compared with the prior art, the invention has the following advantages:
according to the preparation method provided by the invention, the graphene oxide ordered porous film is formed on the lower half part of the polystyrene microsphere in a way of interaction of the polystyrene microsphere and the graphene oxide, the film can be directly fished by a high-molecular transparent flexible substrate, and after the film is removed, the gas sensor which has high sensitivity to water (such as humidity, moisture in human body exhalation gas and the like) and high response and recovery speed is obtained. The preparation method is simple, and the sensor material which is flexible, transparent and highly sensitive to water can be prepared. The manufacturing method is low in cost, easy for mass production and high in yield, overcomes the defects of multi-step operation, repeated processing and batch processing in the processing process of the conventional gas sensor, and gets rid of dependence on high temperature and a rigid substrate, so that the processing flow of the gas sensor is simplified, and the ultra-efficient gas sensor is obtained.
Drawings
FIG. 1 is a scanning electron microscope image before the spherical surface of the graphene oxide ordered porous film is removed;
FIG. 2 is a scanning electron microscope image of a process of forming a degphered graphene oxide ordered porous film;
FIG. 3 is a graph of response performance of a room-temperature flexible graphene oxide ordered porous film gas sensor prepared at different adsorption times to humidity;
FIG. 4 is a graph of humidity gradient response and a linear plot thereof;
fig. 5 is a response performance diagram of the room-temperature flexible graphene oxide ordered porous film gas sensor to moisture in exhaled air of a human body in different motion states and under heartbeat.
Detailed Description
The technical solution of the present invention will be described in further detail with reference to the following embodiments, but the present invention is not limited thereto.
Example 1
Monodisperse cross-linked polystyrene microsphere suspensions were prepared with dimensions of approximately 800 nm. Dipping the glass rod uniformlyGround coating was applied to a clean glass slide over an area of 2.54 × 4cm2And after drying, slowly and obliquely immersing the glass slide into water, and separating a layer of PS microsphere film on the water surface to prepare a graphene oxide solution, wherein the solid content of the graphene oxide solution is 0.34mg/ml, taking 20ml of GO solution into a culture dish with the diameter of 60mm, transferring the PS microsphere film onto the liquid surface of GO, acting for 30min, transferring the film onto the water surface, placing the film into an oven, heating to 90 ℃, dropping 10 mu L HI, reacting for 3min, selecting a clean PET interdigital electrode as a substrate, fishing out the film, and drying to obtain the PET PS/GO-loaded gas sensor.
Example 2
A monodisperse cross-linked polystyrene microsphere suspension was prepared, approximately 800nm in size, dipped in a glass rod and applied uniformly to a clean glass slide over an area of 2.54 × 4cm2After drying, slowly and obliquely immersing the glass slide into water, separating a layer of PS microsphere film on the water surface, preparing a graphene oxide solution, wherein the solid content of the graphene oxide solution is 0.34mg/ml, putting 20ml of GO solution into a culture dish with the diameter of 60mm, transferring the PS microsphere film onto the liquid surface of GO, acting for 10min, transferring the film onto the water surface, putting the film into an oven, heating to 90 ℃, dropping 10 mu L of HI, reacting for 3min, selecting a clean PET interdigital electrode as a substrate, taking out the film, drying to obtain the PET PS/GO-loaded gas sensor, immersing the humidity sensor into dichloromethane for about 10s to remove PS microspheres, and drying to obtain the room-temperature flexible GO ordered porous humidity sensor.
Example 3
A monodisperse cross-linked polystyrene microsphere suspension was prepared, approximately 800nm in size, dipped in a glass rod and applied uniformly to a clean glass slide over an area of 2.54 × 4cm2After drying, slowly and obliquely immersing the glass slide into water, separating a layer of PS microsphere film on the water surface, preparing graphene oxide solution, wherein the solid content is 0.34mg/ml, taking 20ml of GO solution into a culture dish with the diameter of 60mm, transferring the PS microsphere film onto the GO liquid surface, acting for 20min, transferring the film onto the water surface, placing the film into an oven, heating to 90 ℃, dropping 10 mu L HI, reacting for 3min, selecting a clean PET interdigital electrode as a substrate, fishing out the film, and taking out the filmAnd drying to obtain the PET PS/GO loaded gas sensor. And immersing the humidity sensor in dichloromethane for about 10s to remove PS microspheres, and drying to obtain the room-temperature flexible GO ordered porous humidity sensor.
Example 4
A monodisperse cross-linked polystyrene microsphere suspension was prepared, approximately 800nm in size, dipped in a glass rod and applied uniformly to a clean glass slide over an area of 2.54 × 4cm2After drying, slowly and obliquely immersing the glass slide into water, separating a layer of PS microsphere film on the water surface, preparing a graphene oxide solution, wherein the solid content of the graphene oxide solution is 0.34mg/ml, putting 20ml of GO solution into a culture dish with the diameter of 60mm, transferring the PS microsphere film onto the liquid surface of GO, acting for 30min, transferring the film onto the water surface, putting the film into an oven, heating to 90 ℃, dripping 10 mu L of HI, reacting for 3min, selecting a clean PET interdigital electrode as a substrate, taking out the film, drying to obtain the PET PS/GO-loaded gas sensor, immersing the humidity sensor into dichloromethane for about 10s to remove PS microspheres, and drying to obtain the room-temperature flexible GO ordered porous humidity sensor.
Example 5
A monodisperse cross-linked polystyrene microsphere suspension was prepared, approximately 800nm in size, dipped in a glass rod and applied uniformly to a clean glass slide over an area of 2.54 × 4cm2After drying, slowly and obliquely immersing the glass slide into water, separating a layer of PS microsphere film on the water surface, preparing a graphene oxide solution, wherein the solid content of the graphene oxide solution is 0.34mg/ml, putting 20ml of GO solution into a culture dish with the diameter of 60mm, transferring the PS microsphere film onto the liquid surface of GO, acting for 1h, transferring the film onto the water surface, putting the film into an oven, heating to 90 ℃, dripping 10 mu L of HI into the oven, reacting for 3min, selecting a clean PET interdigital electrode as a substrate, taking out the film, drying to obtain a PET PS/GO-loaded gas sensor, immersing the humidity sensor into dichloromethane for about 10s to remove PS microspheres, and drying to obtain the room-temperature flexible GO ordered porous humidity sensor.
Example 6
A monodisperse cross-linked polystyrene microsphere suspension was prepared, having a size of about 80Dipping with a glass rod at 0nm, and uniformly coating on a clean glass slide with a coating area of 2.54 × 4cm2After drying, slowly and obliquely immersing the glass slide into water, separating a layer of PS microsphere film on the water surface, preparing a graphene oxide solution, wherein the solid content of the graphene oxide solution is 0.34mg/ml, putting 20ml of GO solution into a culture dish with the diameter of 60mm, transferring the PS microsphere film onto the liquid surface of GO, acting for 2h, transferring the film onto the water surface, putting the film into an oven, heating to 90 ℃, dripping 10 mu L of HI into the oven, reacting for 3min, selecting a clean PET interdigital electrode as a substrate, taking out the film, drying to obtain a PET PS/GO-loaded gas sensor, immersing the humidity sensor into dichloromethane for about 10s to remove PS microspheres, and drying to obtain the room-temperature flexible GO ordered porous humidity sensor.
The scanning electron micrograph of the sensor obtained in example 1 is shown in FIG. 1. It can be seen that when PS is transferred to the GO liquid surface, we microscopically divide it into two parts, one the lower half in contact with the GO solution and the upper half in contact with air. The lower half part of PS microballon contacts with GO, adsorbs the lower surface at PS microballon through adsorption, and the lower surface of PS microballon is wrapped well by the GO piece, and the upper half part is because of unable and GO piece contact, consequently still is smooth spherical upper surface.
Scanning electron micrographs of the sensors obtained in example 2, example 3, example 4, example 5 and example 6 are shown in the respective panels of FIG. 2. It can be seen that as the adsorption time increases, the GO film grows from the first bottom pit to a thin shell, followed by a growing process in which the pore walls gradually thicken.
Experimental example 1
Testing the performance of the room-temperature flexible graphene oxide ordered porous film gas sensor:
preparing saturated potassium sulfate solution with a relative humidity value of 97 percent, placing the saturated potassium sulfate solution in a closed glass bottle for one night, and generating a constant 97 percent relative humidity environment above the solution. The sensors obtained in example 3, example 4, example 5 and example 6 were connected to a test plate of a gas sensor through a connector, and the portion of the other end of the sensor, which sandwiched the gas sensor, was inserted above the liquid surface of the closed glass bottle, and the response performance at the relative humidity was measured. The obtained performance is shown in figure 3, and it can be seen that the adsorption time is 30min, the sensitivity of the obtained sensor to humidity is highest, and the response time is short.
In addition, the type of saturated salt solution and its relative humidity value at a temperature of 25 ℃ are detailed in Table 1:
experimental example 2
Testing the humidity gradient of the room-temperature flexible GO ordered porous film humidity-sensitive sensor:
saturated salt solutions with different relative humidity values are prepared and placed in a closed glass bottle for one night, so that a constant humidity environment can be generated above the solutions. The type of saturated salt solution used herein and its relative humidity value at a temperature of 25 c are given in the attached table 1. The room temperature flexible GO ordered porous humidity sensor obtained in the embodiment 4 is connected to a test board of a gas sensitive tester through a connecting device, the part of the other end of the room temperature flexible GO ordered porous humidity sensor, which clamps the gas sensor, is inserted above the liquid level of the sealed glass bottle, and the response performance of the room temperature flexible GO ordered porous humidity sensor under different relative humidity gradients is tested. The resulting performance is shown in fig. 4(a), and it can be seen that the sensitivity gradually increases with increasing humidity gradient. The sensitivity corresponding to the humidity gradient was linearly fitted as shown in FIG. 4(b), and it was found that there was a good linear relationship.
Experimental example 3
The response performance of the room-temperature flexible graphene oxide ordered porous film gas sensor to moisture in exhaled air under different motion or physiological states and heartbeats of a human body is tested:
the room temperature flexible GO ordered porous humidity sensor obtained in the embodiment 4 is connected to a test board of a gas sensitive tester through a connecting device, and the other end of the room temperature flexible GO ordered porous humidity sensor is used for measuring the response performance of moisture in exhaled air of a human body in the states of sitting still, moving, sleeping and fever. As shown in figure 5, the sensor can be seen to have obvious differences in the response of the human body in the states of sitting still, moving, sleeping and fever.
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 preparation method of a room-temperature flexible graphene oxide ordered porous film sensor is characterized by comprising the following steps:
(1) uniformly coating the monodisperse crosslinked polystyrene microsphere suspension on a glass slide, drying, obliquely immersing the glass slide in water, and separating out a single-layer polystyrene microsphere film;
(2) transferring the polystyrene microsphere film to the liquid surface of a graphene oxide solution, and obtaining a composite film of polystyrene and graphene oxide after 20min-2 h;
(3) transferring the composite membrane obtained in the step (2) to a water surface, placing the composite membrane on an oven, heating to 80-100 ℃, dropwise adding a 10 mu L-1 m L reducing agent, and reacting for 3-10min to obtain a composite membrane 2;
(4) covering the composite film 2 on a high polymer flexible material, fishing out, and drying to obtain a gas sensor with a high polymer flexible substrate loaded with polystyrene and graphene oxide;
(5) and (5) immersing the gas sensor obtained in the step (4) into a solvent capable of dissolving polystyrene microspheres for 10-15s, and drying at 60 ℃ to obtain the room-temperature flexible graphene oxide ordered porous gas sensor.
2. The method for preparing a room temperature flexible graphene oxide ordered porous film sensor according to claim 1, wherein the size of the monodisperse crosslinked polystyrene microsphere is 500-1000 nm.
3. The method for preparing the room-temperature flexible graphene oxide ordered porous film sensor according to claim 1, wherein the monodisperse crosslinked polystyrene microspheres are coated on a glass slide, and the coating area is 2-3cm × 4 cm.
4. The preparation method of the room-temperature flexible graphene oxide ordered porous film sensor according to claim 1, wherein the solid content of the graphene oxide solution is 0.1-1 mg/ml.
5. The method for preparing the room-temperature flexible graphene oxide ordered porous film sensor according to claim 1, wherein the sampling amount of the graphene oxide solution in the step (2) is 20ml, and the diameter of the culture dish is 60 mm.
6. The method for preparing the room-temperature flexible graphene oxide ordered porous film sensor according to claim 1, wherein the reducing agent in the step (3) is one or more of hydrogen iodide, hydrazine hydrate, L-ascorbic acid and ammonia water.
7. The method for preparing the room-temperature flexible graphene oxide ordered porous film sensor according to claim 1, wherein the polymer flexible substrate is one of a PET interdigital electrode, a PI interdigital electrode and a nylon wire.
8. The method for preparing the room-temperature flexible graphene oxide ordered porous film sensor according to claim 1, wherein the solvent capable of dissolving the polystyrene microspheres is one or more of dichloromethane, chloroform, tetrahydrofuran, N-dimethylformamide, cyclohexane and toluene.
9. The room-temperature flexible graphene oxide ordered porous humidity-sensitive sensor is characterized by being prepared by the method of any one of claims 1 to 8.
10. The room-temperature flexible graphene oxide ordered porous humidity-sensitive sensor as claimed in claim 9, which is used for detecting different motion states and heartbeats of a human body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010300755.9A CN111458382A (en) | 2020-04-16 | 2020-04-16 | Room-temperature flexible graphene oxide ordered porous film sensor and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010300755.9A CN111458382A (en) | 2020-04-16 | 2020-04-16 | Room-temperature flexible graphene oxide ordered porous film sensor and preparation method and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111458382A true CN111458382A (en) | 2020-07-28 |
Family
ID=71677234
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010300755.9A Pending CN111458382A (en) | 2020-04-16 | 2020-04-16 | Room-temperature flexible graphene oxide ordered porous film sensor and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111458382A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113567512A (en) * | 2021-07-20 | 2021-10-29 | 上海大学 | Carbon-based material sensor based on lithium ion doping and preparation method thereof |
| CN114751368A (en) * | 2022-04-12 | 2022-07-15 | 安徽维纳物联科技有限公司 | Preparation method of graphene oxide surface modified MEMS gas sensor chip |
| CN115716712A (en) * | 2022-11-08 | 2023-02-28 | 中国科学院合肥物质科学研究院 | Based on GO @ Ni-SnO 2 Gas sensor of micro-nano porous sensitive film, preparation method and application |
| CN116693924A (en) * | 2023-05-10 | 2023-09-05 | 华南师范大学 | Room-temperature polyaniline porous film sensor and preparation method and application thereof |
| CN115716712B (en) * | 2022-11-08 | 2024-07-09 | 中国科学院合肥物质科学研究院 | GO@Ni-SnO based2Gas sensor of micro-nano porous sensitive film, preparation method and application |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101270197A (en) * | 2008-03-12 | 2008-09-24 | 南京大学 | Method for preparing adjustable uniform hole polystyrene monolayer film |
| CN101672847A (en) * | 2009-09-30 | 2010-03-17 | 青岛科技大学 | Preparation method of protein chip glass carrier |
| CN102486967A (en) * | 2010-12-06 | 2012-06-06 | 长沙理工大学 | Preparation method of composite ordered porous nanometer titanium dioxide (TiO2) film |
| CN103145118A (en) * | 2013-03-04 | 2013-06-12 | 哈尔滨工业大学 | Preparation method of three-dimensional interpenetrating macroporous graphene high-efficiency oil absorption material |
| CN105932258A (en) * | 2016-06-27 | 2016-09-07 | 天津工业大学 | Preparation method for inorganic nanoparticle/graphene three-dimensional porous composite material |
| US20160377611A1 (en) * | 2015-06-29 | 2016-12-29 | Polestar Technologies, Inc. | Chemical sensor using molecularly-imprinted single layer graphene |
| US20180059041A1 (en) * | 2016-08-08 | 2018-03-01 | B.G. Negev Technologies & Applications Ltd. At Ben-Gurion University | High sensitivity broad-target porous graphene oxide capacitive vapor sensor |
| CN110104640A (en) * | 2019-05-16 | 2019-08-09 | 宁波石墨烯创新中心有限公司 | Composite air-sensitive material, gas sensor and preparation method thereof |
| KR20190094010A (en) * | 2018-02-02 | 2019-08-12 | 가천대학교 산학협력단 | Stretchable gas sensors using elastomeric sponge structures and fabrication method thereof |
| CN110208334A (en) * | 2019-05-13 | 2019-09-06 | 中国石油大学(华东) | For the humidity transducer production method and its detection system of expiratory air |
-
2020
- 2020-04-16 CN CN202010300755.9A patent/CN111458382A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101270197A (en) * | 2008-03-12 | 2008-09-24 | 南京大学 | Method for preparing adjustable uniform hole polystyrene monolayer film |
| CN101672847A (en) * | 2009-09-30 | 2010-03-17 | 青岛科技大学 | Preparation method of protein chip glass carrier |
| CN102486967A (en) * | 2010-12-06 | 2012-06-06 | 长沙理工大学 | Preparation method of composite ordered porous nanometer titanium dioxide (TiO2) film |
| CN103145118A (en) * | 2013-03-04 | 2013-06-12 | 哈尔滨工业大学 | Preparation method of three-dimensional interpenetrating macroporous graphene high-efficiency oil absorption material |
| US20160377611A1 (en) * | 2015-06-29 | 2016-12-29 | Polestar Technologies, Inc. | Chemical sensor using molecularly-imprinted single layer graphene |
| CN105932258A (en) * | 2016-06-27 | 2016-09-07 | 天津工业大学 | Preparation method for inorganic nanoparticle/graphene three-dimensional porous composite material |
| US20180059041A1 (en) * | 2016-08-08 | 2018-03-01 | B.G. Negev Technologies & Applications Ltd. At Ben-Gurion University | High sensitivity broad-target porous graphene oxide capacitive vapor sensor |
| KR20190094010A (en) * | 2018-02-02 | 2019-08-12 | 가천대학교 산학협력단 | Stretchable gas sensors using elastomeric sponge structures and fabrication method thereof |
| CN110208334A (en) * | 2019-05-13 | 2019-09-06 | 中国石油大学(华东) | For the humidity transducer production method and its detection system of expiratory air |
| CN110104640A (en) * | 2019-05-16 | 2019-08-09 | 宁波石墨烯创新中心有限公司 | Composite air-sensitive material, gas sensor and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 侯朝霞等: "聚苯乙烯微球的制备及构筑三维多孔石墨烯", 《沈阳大学学报(自然科学版)》 * |
| 赵振兵: "有序多孔氧化锌石墨烯复合膜制备及性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113567512A (en) * | 2021-07-20 | 2021-10-29 | 上海大学 | Carbon-based material sensor based on lithium ion doping and preparation method thereof |
| CN113567512B (en) * | 2021-07-20 | 2024-05-14 | 上海大学 | Carbon-based material sensor based on lithium ion doping and preparation method thereof |
| CN114751368A (en) * | 2022-04-12 | 2022-07-15 | 安徽维纳物联科技有限公司 | Preparation method of graphene oxide surface modified MEMS gas sensor chip |
| CN115716712A (en) * | 2022-11-08 | 2023-02-28 | 中国科学院合肥物质科学研究院 | Based on GO @ Ni-SnO 2 Gas sensor of micro-nano porous sensitive film, preparation method and application |
| CN115716712B (en) * | 2022-11-08 | 2024-07-09 | 中国科学院合肥物质科学研究院 | GO@Ni-SnO based2Gas sensor of micro-nano porous sensitive film, preparation method and application |
| CN116693924A (en) * | 2023-05-10 | 2023-09-05 | 华南师范大学 | Room-temperature polyaniline porous film sensor and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111458382A (en) | Room-temperature flexible graphene oxide ordered porous film sensor and preparation method and application thereof | |
| Zhang et al. | Graphene‐based electrochemical glucose sensors: Fabrication and sensing properties | |
| CN100523799C (en) | Polyelectrolyte / intrinsic conducting polymer composite humidity sensor and its production method | |
| CN108414583A (en) | Humidity sensor and the improvement based on graphene oxide humidity sensor and preparation | |
| WO2021228016A1 (en) | Nonenzymatic biosensor based on metal-modified porous boron-doped diamond electrode, and preparation method therefor and use thereof | |
| Wu et al. | Double signal ratiometric electrochemical riboflavin sensor based on macroporous carbon/electroactive thionine-contained covalent organic framework | |
| CN101799441A (en) | Polymer resistor type humidity element of water dispersion nano-polyaniline and manufacturing method thereof | |
| Dai et al. | Morphology-dependent electrochemical behavior of 18-facet Cu7S4 nanocrystals based electrochemical sensing platform for hydrogen peroxide and prostate specific antigen | |
| Nie et al. | Improved dielectricity of anisotropic wood slices and bioinspired micropatterned film electrodes for highly sensitive flexible electronic sensors | |
| Khalifa et al. | Highly sensitive and wearable NO2 gas sensor based on PVDF nanofabric containing embedded polyaniline/g-C3N4 nanosheet composites | |
| CN111855749A (en) | Porous TiO2Preparation method of NaPSS composite sensitive material and product thereof | |
| CN109324091B (en) | Preparation method of intelligent material suitable for sensing humid environment | |
| CN115219575B (en) | Stretchable electrochemical three-dimensional microelectrode and application thereof in biomolecule detection | |
| CN116148328A (en) | Flexible reference electrode and preparation method thereof | |
| CN109459474A (en) | A kind of preparation and application of gold nanoparticle/three-dimensional graphene composite material | |
| CN113292041B (en) | SnSe-based 2 Multifunctional intelligent semiconductor sensor and preparation method thereof | |
| Ren et al. | ZIF-derived nanoparticles modified ZnO nanorods hierarchical structure for conductometric NO2 gas sensor | |
| CN110243909B (en) | Fixed connection type self-plasticizing polymer film lead ion selective electrode based on multi-wall carbon nano tube | |
| CN201340405Y (en) | Macromolecule resistive-type humidity sensitive element with hyperbranched structure | |
| CN110907503A (en) | Manufacturing method of hierarchical porous structure metal oxide and metal oxide semiconductor gas sensor | |
| CN111929350A (en) | Hydrogen sulfide gas detection method and sensor based on hollow microsphere composite membrane | |
| CN112255277B (en) | Acetone gas sensor based on branched heterojunction array, preparation method and application | |
| CN112782241A (en) | Nano silicon sensor applicable to room temperature and high humidity environment and preparation method thereof | |
| CN115716712B (en) | GO@Ni-SnO based2Gas sensor of micro-nano porous sensitive film, preparation method and application | |
| CN115991892B (en) | Humidity pressure sensor based on composite flexible material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200728 |
|
| RJ01 | Rejection of invention patent application after publication |