CN117871615A - O 3 Sensor, preparation method thereof and O 3 Concentration detection method and detection device - Google Patents
O 3 Sensor, preparation method thereof and O 3 Concentration detection method and detection device Download PDFInfo
- Publication number
- CN117871615A CN117871615A CN202311307004.XA CN202311307004A CN117871615A CN 117871615 A CN117871615 A CN 117871615A CN 202311307004 A CN202311307004 A CN 202311307004A CN 117871615 A CN117871615 A CN 117871615A
- Authority
- CN
- China
- Prior art keywords
- sensor
- pbi
- concentration
- substrate
- resistance
- 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
- 238000001514 detection method Methods 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000758 substrate Substances 0.000 claims abstract description 80
- 239000000463 material Substances 0.000 claims abstract description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 33
- 239000010439 graphite Substances 0.000 claims abstract description 33
- 239000000919 ceramic Substances 0.000 claims abstract description 30
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical group [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims abstract description 27
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 39
- 239000002243 precursor Substances 0.000 claims description 31
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 26
- 230000035945 sensitivity Effects 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 14
- 239000003960 organic solvent Substances 0.000 claims description 12
- 238000012545 processing Methods 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 3
- 239000004065 semiconductor Substances 0.000 abstract description 11
- 229910052740 iodine Inorganic materials 0.000 abstract description 9
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 abstract description 7
- 239000011630 iodine Substances 0.000 abstract description 7
- 230000005540 biological transmission Effects 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 31
- 239000010408 film Substances 0.000 description 28
- 239000007789 gas Substances 0.000 description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- 230000004044 response Effects 0.000 description 10
- 238000012512 characterization method Methods 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 8
- 230000008859 change Effects 0.000 description 8
- 238000011084 recovery Methods 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 239000010409 thin film Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- 238000010952 in-situ formation Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- CLOMYZFHNHFSIQ-UHFFFAOYSA-N clonixin Chemical compound CC1=C(Cl)C=CC=C1NC1=NC=CC=C1C(O)=O CLOMYZFHNHFSIQ-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- LLWRXQXPJMPHLR-UHFFFAOYSA-N methylazanium;iodide Chemical compound [I-].[NH3+]C LLWRXQXPJMPHLR-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000001548 drop coating Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005802 health problem Effects 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 208000026278 immune system disease Diseases 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical group 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Landscapes
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The present application relates to O 3 Sensor, preparation method thereof and O 3 Concentration detection method and detection device. O (O) 3 The sensor comprises a substrate with interdigital electrodes and a sensitive material layer arranged on the surface of the interdigital electrodes, wherein the sensitive material layer is tetragonal CH 3 NH 3 PbI 3 The interdigital electrode is a graphite interdigital electrode, and the substrate is a ceramic substrate. Will tetragonal CH 3 NH 3 PbI 3 Preparing O with graphite interdigital electrode and ceramic substrate by using semiconductor material as sensitive material 3 Sensor, O 3 Can be adsorbed on the vacancy of iodine and is connected with tetragonal CH 3 NH 3 PbI 3 In (b) 2+ The bonding performs electron transport, thereby increasing the carrier concentration of the semiconductor material; and the carrier concentration affects the current, thereby affecting O 3 The resistance of the sensor is further used for detecting O under the room temperature condition 3 Is a concentration of (3). And tetragonal CH 3 NH 3 PbI 3 Octahedron [ PbI ] of (E) 6 ] 2‑ The skeleton provides an electron transmission channel, which can effectively promote O 3 Is provided.
Description
Technical Field
The present application relates to the field of sensors, and in particular to an O 3 Sensor, preparation method thereof and O 3 Concentration detection method and detection device.
Background
Ozone, also known as trioxygen, of the formula O 3 The product is also called triatomic oxygen and superoxide, is a photochemistry pollution product, has strong oxidizing property, and can induce haze. Within 8 h mean, the human body is exposed to O 3 The safe concentration threshold in (a) is 50 ppb if O in the environment 3 Exceeding this limit will cause a series of health problems such as asthma, cardiovascular diseases, immune system diseases, etc. Thus, for O in the atmosphere 3 Accurate monitoring of concentration in real time is of paramount importance.
At present, build O 3 The sensitive material of the sensor is Metal Oxide Semiconductor (MOSs) including ZnO and In 2 O 3 WO (WO) 3 Etc. The sensitivity of the MOSs-based gas sensor is high, but in practical applications, a high operating temperature is required, which leads to thermal growth of oxide grains, so that the stability of the sensor is poor, and the high operating temperature also increases the power consumption of the sensor.
Disclosure of Invention
Based on this, the present applicationProvides a method for detecting O under room temperature without illumination 3 Concentration, and can detect lower concentration O 3 O of (2) 3 Sensor, preparation method thereof and O 3 Concentration detection method and detection device.
The technical scheme for solving the technical problems is as follows.
The first aspect of the present application provides an O 3 The sensor comprises a substrate with interdigital electrodes and a sensitive material layer arranged on the surfaces of the interdigital electrodes, wherein the sensitive material layer is tetragonal CH 3 NH 3 PbI 3 The interdigital electrode is a graphite interdigital electrode, and the substrate is a ceramic substrate.
In some of these embodiments, O 3 In the sensor, the substrate is an alumina ceramic substrate.
In a second aspect the present application provides an O 3 The preparation method of the sensor comprises the following steps:
PbI is prepared 2 、CH 3 NH 3 I and organic solvent to obtain CH 3 NH 3 PbI 3 A precursor solution;
the CH is subjected to 3 NH 3 PbI 3 The precursor solution is arranged on the surface of an interdigital electrode on a substrate, and a tetragonal CH is formed on the surface of the interdigital electrode after drying 3 NH 3 PbI 3 The membrane layer, the interdigital electrode is graphite interdigital electrode, and the substrate is a ceramic substrate.
In some of these embodiments, O 3 In the preparation method of the sensor, the PbI 2 With the CH 3 NH 3 The molar ratio of I is (1-3): 1.
In some of these embodiments, O 3 In the preparation method of the sensor, the organic solvent is at least one selected from N, N-dimethylformamide and dimethyl sulfoxide.
In some of these embodiments, O 3 In the preparation method of the sensor, the CH 3 NH 3 PbI 3 PbI in precursor solution 2 The concentration of (C) is 0.5 mol/L-3 mol/L.
In a third aspect the present application provides an O 3 The concentration detection method comprises the following steps:
o is added with 3 The sensors are respectively arranged at least 3O with different standard concentrations 3 In standard environment, different O's are obtained respectively 3 At the concentration of O 3 Standard resistance R of sensor g The method comprises the steps of carrying out a first treatment on the surface of the The O is 3 The sensor comprises a substrate, an electrode arranged on the substrate and a sensitive material layer arranged on the surface of the electrode, wherein the sensitive material layer is tetragonal CH 3 NH 3 PbI 3 The substrate is a ceramic substrate, and the electrode is a graphite interdigital electrode;
according to different O 3 At the concentration of O 3 Standard resistance R of sensor g Obtaining the O 3 Resistance and O of sensor 3 Standard relationship of concentration;
acquiring the O 3 Resistance R of sensor in environment to be measured x The method comprises the steps of carrying out a first treatment on the surface of the According to the standard relation and the resistance R x Obtaining O in the environment to be tested 3 Concentration.
In some of these embodiments, O 3 In the method for detecting the concentration, the concentration is determined according to different O 3 At the concentration of O 3 Standard resistance R of sensor g Obtaining the O 3 Resistance and O of sensor 3 The standard relationship of the concentration comprises the following steps:
o is added with 3 The sensor is placed in the air to obtain the O 3 Initial resistance R of sensor a ；
According to different O 3 At the concentration of O 3 Standard resistance R of sensor g Obtaining the O 3 Sensor relative to initial resistance R a Sensitivity of said O 3 Sensitivity of sensor = Δr/R a X 100%, ΔR is R a And R is R g Absolute value of the difference;
establishing the O 3 Sensitivity of sensor and O 3 Linear relation between the concentrations of (a).
In a fourth aspect the present application provides an O 3 A concentration detection apparatus comprising:
O 3 the sensor comprises a substrate, an electrode arranged on the substrate and a sensitive material layer arranged on the surface of the electrode, wherein the sensitive material layer is tetragonal CH 3 NH 3 PbI 3 The substrate is a ceramic substrate, and the electrode is a graphite interdigital electrode; and
A resistance detection module for connecting with the O 3 Sensor connection and acquisition of the O 3 Measured resistance of the sensor.
In some of these embodiments, O 3 The concentration detection apparatus further includes:
a data processing module for processing the data according to the preset O 3 Resistance and O of sensor 3 Standard relation of concentration and the measured resistance, determining O 3 Is a concentration of (3).
The skilled person in the present application found through research that tetragonal lead methyl ammonium iodide (CH) in organic-inorganic hybrid perovskite semiconductor materials 3 NH 3 PbI 3 ) Contains abundant iodine vacancy, and tetragonal CH 3 NH 3 PbI 3 Preparing O with graphite interdigital electrode and ceramic substrate by using semiconductor material as sensitive material 3 Sensor, O 3 Can be adsorbed on the vacancy of iodine and is connected with tetragonal CH 3 NH 3 PbI 3 Pb in (B) 2+ The bonding performs electron transport, thereby increasing the carrier concentration of the semiconductor material; and the carrier concentration affects the current, thereby affecting O 3 The resistance of the sensor is further realized, and O can be detected under the room temperature condition without illumination 3 Is a concentration of (3). And tetragonal CH 3 NH 3 PbI 3 Octahedron [ PbI ] of (E) 6 ] 2- The skeleton provides an electron transmission channel, which can effectively promote O 3 Is provided. Will tetragonal CH 3 NH 3 PbI 3 Is matched with the graphite interdigital electrode and the ceramic substrate, and can be realized in O 3 At lower concentrations there is still a clear and complete response recovery signal, giving the sensor the ability to detect trace O 3 Capacity of the gas.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present application, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is O 3 Schematic diagram of gas-sensitive mechanism of sensor;
FIG. 2 is a diagram of CH in example 1 3 NH 3 PbI 3 XRD characterization of the film;
FIG. 3 is a diagram of CH in example 1 3 NH 3 PbI 3 EDX characterization of the film;
FIG. 4 is a diagram of CH in example 1 3 NH 3 PbI 3 SEM characterization of the film;
FIG. 5 is a diagram of CH in example 1 3 NH 3 PbI 3 TEM characterization of the film;
FIG. 6 is a diagram of CH in example 1 3 NH 3 PbI 3 XPS spectrum of film;
FIG. 7 is O 3 A gas-sensitive test pattern of the sensor;
FIG. 8 is a diagram of CH in example 1 3 NH 3 PbI 3 Exposure of the film to O 3 XPS spectra before and after atmosphere.
Detailed Description
Reference now will be made in detail to embodiments of the invention, one or more examples of which are described below. Each example is provided by way of explanation, not limitation, of the invention. Indeed, it will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the scope or spirit of the invention. For example, features illustrated or described as part of one embodiment can be used on another embodiment to yield still a further embodiment.
Accordingly, it is intended that the present invention cover such modifications and variations as fall within the scope of the appended claims and their equivalents. Other objects, features and aspects of the present invention will be disclosed in or be apparent from the following detailed description. It is to be understood by one of ordinary skill in the art that the present discussion is a description of exemplary embodiments only, and is not intended as limiting the broader aspects of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element. The indefinite articles "a" and "an" preceding an element or component of the invention are not limited to the requirement (i.e. the number of occurrences) of the element or component. Thus, the use of "a" or "an" should be interpreted as including one or at least one, and the singular reference of an element or component includes the plural reference unless the amount clearly dictates otherwise. The meaning of "a plurality of" means at least two, e.g., two, three, etc., unless explicitly defined otherwise.
The weights of the relevant components mentioned in the description of the embodiments of the present invention may refer not only to the specific contents of the components, but also to the proportional relationship between the weights of the components, so long as the contents of the relevant components in the description of the embodiments of the present invention are scaled up or down within the scope of the disclosure of the embodiments of the present invention. Specifically, the weight described in the specification of the embodiment of the present invention may be mass units known in the chemical industry field such as μ g, mg, g, kg.
Except where shown or otherwise indicated in the operating examples, all numbers expressing quantities of ingredients, physical and chemical properties, and so forth, used in the specification and claims are to be understood as being modified in all instances by the term "about". For example, therefore, unless indicated to the contrary, the numerical parameters set forth in the foregoing specification and attached claims are approximations that can be varied appropriately by those skilled in the art utilizing the teachings disclosed herein seeking to obtain the desired properties. The use of numerical ranges by endpoints includes all numbers subsumed within that range and any range within that range, e.g., 1 to 5 includes 1, 1.1, 1.3, 1.5, 2, 2.75, 3, 3.80, 4, 5, and the like.
One embodiment of the present application provides an O 3 The sensor comprises a substrate with interdigital electrodes and a sensitive material layer arranged on the surface of the graphite interdigital electrodes, wherein the sensitive material layer is tetragonal CH 3 NH 3 PbI 3 The interdigital electrode is a graphite interdigital electrode, and the substrate is a ceramic substrate.
The organic-inorganic hybrid perovskite semiconductor material has the characteristics of larger carrier concentration and higher mobility.
Referring to fig. 1, the skilled person of the present application found through research that tetragonal lead methyl ammonium iodide (CH) in an organic-inorganic hybrid perovskite semiconductor material 3 NH 3 PbI 3 ) Contains abundant iodine vacancy, and tetragonal CH 3 NH 3 PbI 3 Preparing O with graphite interdigital electrode and ceramic substrate by using semiconductor material as sensitive material 3 Sensor, O 3 Can be adsorbed on iodine vacancy and tetragonal CH 3 NH 3 PbI 3 Pb in (B) 2+ The bonding performs electron transport, thereby increasing the carrier concentration of the semiconductor material; and the carrier concentration affects the current, thereby affecting O 3 The resistance of the sensor is further realized, and O can be detected under the room temperature condition without illumination 3 Is a concentration of (3). And CH (CH) 3 NH 3 PbI 3 Octahedron [ PbI ] of (E) 6 ] 2- The skeleton provides an electron transmission channel, which can effectively promote O 3 Is provided. Will tetragonal CH 3 NH 3 PbI 3 Is matched with the graphite interdigital electrode and the ceramic substrate, and can be realized in O 3 At lower concentrations there is still a clear and complete response recovery signal, giving the sensor the ability to detect trace O 3 Capacity of the gas.
Above O 3 The sensor can work in room temperature environment without thermal excitation or light excitation, so that the power consumption of the sensitive element is reduced, and potential safety hazards are avoided.
It will be appreciated that when in the ambient environment O 3 By CH when the concentration varies 3 NH 3 PbI 3 The current of the semiconductor material will change, which in turn results in a change in the resistance of the sensor. By measuring the variation of the resistance, O can be calculated 3 Sensitivity of the sensor of (2) so that O can be obtained 3 Sensitivity of the sensor of (2) with O 3 Relationship between concentrations, build up of O 3 And a gas concentration detection model.
It was found that O as described above 3 The sensor is used for detecting O 3 At the concentration, the surface of the perovskite film has no color reaction.
In some of these examples, O 3 In the sensor, the substrate is an alumina ceramic substrate.
One embodiment of the present application provides an O 3 The preparation method of the concentration comprises the following steps:
step S10, pbI is processed 2 、CH 3 NH 3 I and organic solvent to obtain CH 3 NH 3 PbI 3 Precursor solution.
In some of these examples, in step S10, pbI 2 And CH (CH) 3 NH 3 The molar ratio of I is (1-3): 1.
It will be appreciated that PbI 2 And CH (CH) 3 NH 3 The molar ratio of I includes, but is not limited to, 1:1, 1.2:1, 1.5:1, 1.8:1, 2:1, 2.2:1, 2.5:1, 2.8:1, 3:1; the following holds true for the range that any two of these point values may be made up as end values in some examples.
Optionally, in step S10, pbI 2 And CH (CH) 3 NH 3 The molar ratio of I is (1-2): 1.
Further, in step S10, pbI 2 And CH (CH) 3 NH 3 The molar ratio of I is 1:1.
In some examples, in step S10, the organic solvent is selected from at least one of N, N-dimethylformamide and dimethyl sulfoxide.
Optionally, in step S10, the organic solvent is a mixture of N, N-dimethylformamide and dimethyl sulfoxide.
In some examples, in step S10, the volume ratio of N, N-dimethylformamide to dimethyl sulfoxide is (5-10): 3.
It is understood that the volume ratio of N, N-dimethylformamide to dimethylsulfoxide includes, but is not limited to, 5:3, 6:3, 7:3, 8:3, 9:3, 10:3.
Optionally, in the step S10, the volume ratio of the N, N-dimethylformamide to the dimethyl sulfoxide is (6-8): 3.
Further, in step S10, the volume ratio of N, N-dimethylformamide to dimethyl sulfoxide is 7:3.
In some of these examples, in step S10, CH 3 NH 3 PbI 3 PbI in precursor solution 2 The concentration of (C) is 0.5 mol/L-3 mol/L.
It will be appreciated that PbI 2 The concentration of (C) includes, but is not limited to, 0.5 mol/L, 0.8 mol/L, 1 mol/L, 1.2 mol/L, 1.5 mol/L, 1.8 mol/L, 2 mol/L, 2.5 mol/L, 3 mol/L.
In some of these examples, in step S10, CH 3 NH 3 PbI 3 In the precursor solution, CH 3 NH 3 The concentration of I is 0.5 mol/L to 3 mol/L.
It can be appreciated that CH 3 NH 3 The concentration of I includes, but is not limited to, 0.5 mol/L, 0.8 mol/L, 1 mol/L, 1.2 mol/L, 1.5 mol/L, 1.8 mol/L, 2 mol/L, 2.5 mol/L, 3 mol/L.
In some specific examples, in step S10, CH 3 NH 3 PbI 3 In the precursor solution, CH 3 NH 3 The concentration of I is 1 mol/L.
In some examples, in step S10, the mixing step is performed at 20 ℃ to 30 ℃.
In some specific examples thereof, step S10 includes:
PbI is prepared 2 And CH (CH) 3 NH 3 I is added into the mixed solution of N, N-dimethylformamide and dimethyl sulfoxide, and is stirred until dissolved, thus obtaining CH 3 NH 3 PbI 3 Precursor solution.
Step S11, CH is processed 3 NH 3 PbI 3 The precursor solution is arranged on the surface of the interdigital electrode on the substrate, and after drying, tetragonal CH is formed on the surface of the interdigital electrode 3 NH 3 PbI 3 The membrane layer, the interdigital electrode is a graphite interdigital electrode, and the substrate is a ceramic substrate.
It will be appreciated that CH 3 NH 3 PbI 3 The precursor solution is arranged on the surface of the interdigital electrode, and after drying, tetragonal CH is formed on the surface of the interdigital electrode in situ 3 NH 3 PbI 3 And (3) a film layer.
In some of these examples, in step S11, CH is set 3 NH 3 PbI 3 The manner in which the precursor solution is disposed on the surface of the interdigitated electrodes on the substrate includes, but is not limited to, drop coating, spin coating, and the like.
Optionally, in step S11, CH is set 3 NH 3 PbI 3 The precursor solution is dripped on the surfaces of the interdigital electrodes.
In some of these examples, in step S11, CH is set 3 NH 3 PbI 3 The step of disposing the precursor solution on the surface of the interdigital electrode is performed in a glove box.
In some examples, in step S11, the drying temperature is 90 ℃ to 110 ℃ and the drying time is 25 min to 30 min.
It is understood that the drying temperature includes, but is not limited to, 90 ℃, 95 ℃, 100 ℃, 105 ℃, 110 ℃, and the drying time includes, but is not limited to, 25 min, 28 min, 30 min.
Alternatively, in step S11, the temperature of drying is 100 ℃.
It will be appreciated that CH 3 NH 3 PbI 3 The precursor solution is arranged on the substrateDrying the surface of the interdigital electrode, evaporating the organic solvent, and finally forming CH on the surface of the interdigital electrode 3 NH 3 PbI 3 Film layer, and CH 3 NH 3 PbI 3 The surface of the film layer is continuous and smooth and has no fault.
In some examples, before performing step S11, the method further includes a step of pre-treating the substrate with the interdigital electrode:
and (3) sequentially placing the substrate with the interdigital electrodes in ethanol and water for cleaning, and then drying at 50-60 ℃.
Further, the ethanol is absolute ethanol, and the water is deionized water.
Above O 3 The preparation method of the sensor can form CH on the surface of the interdigital electrode on the substrate by using a simple one-step pre-mixed precursor deposition method 3 NH 3 PbI 3 The film has the advantages of simple preparation method, short preparation period and low cost, and is suitable for mass production.
One embodiment of the present application provides an O 3 The concentration detection method comprises the steps of S20-S23:
step S20: o is added with 3 The sensors are respectively arranged at least 3O with different standard concentrations 3 In standard environment, different O's are obtained respectively 3 At a concentration of O 3 Standard resistance R of sensor g ；O 3 The sensor comprises a substrate, an electrode arranged on the substrate and a sensitive material layer arranged on the surface of the electrode, wherein the sensitive material layer is tetragonal CH 3 NH 3 PbI 3 The substrate is a ceramic substrate, and the electrodes are graphite interdigital electrodes.
It will be appreciated that different standard concentrations of O 3 O in standard environment 3 The concentrations are known.
Step S21: according to different O 3 At a concentration of O 3 Standard resistance R of sensor g Obtaining O 3 Resistance and O of sensor 3 Standard relationship of concentration.
It will be appreciated that when establishing the standard curve, O of different standard concentrations 3 Standard environments include, but are not limited to, 3, 4, 56, 7, etc.
In some examples, step S21 includes steps S211 to S213:
step S211: o is added with 3 The sensor is placed in the air to obtain O 3 Initial resistance R of sensor a ；
Step S212: according to different O 3 At a concentration of O 3 Standard resistance R of sensor g Obtaining O 3 Sensor relative to initial resistance R a Sensitivity of O 3 Sensitivity of sensor = Δr/R a X 100%, ΔR is R a And R is R g Absolute value of the difference;
step S213: build O 3 Sensitivity of sensor and O 3 Linear relation between the concentrations of (a).
It can be understood that O established in step S211 to step S213 3 Sensitivity of sensor and O 3 The linear relationship between the concentrations of (2) is O in step S21 3 Resistance and O of sensor 3 Standard relationship of concentration.
Step S22: acquisition of O 3 Resistance R of sensor in environment to be measured x 。
Step S23: according to the standard relation and resistance R x Obtaining O in the environment to be tested 3 Concentration.
It will be appreciated that O 3 Sensor at different O 3 Different resistances R are obtained at the concentration g1、 R g2、 R g3 Etc.; o established in step S211-step S213 3 Sensitivity of sensor and O 3 When the linear relation between the concentrations of (a) is established, the equation DeltaR/R a X 100% = k·c+b, where Δr= |r a -R g C is O 3 Concentration; resistor R of air a Different and known O 3 Concentration and O of different concentration from the above 3 Resistance R obtained under standard environment g1、 R g2、 R g3 Respectively substituting into equation DeltaR/R a In x 100% = k.c+b, the values of k and b are derived, thus establishing O 3 Sensitivity of sensor and O 3 Linear relationship between the concentrations of (i) O 3 Sensor for detecting a position of a bodyResistance and O of (2) 3 Standard relationship of concentration.
It is further understood that at different O 3 Standard relationships can be established in the concentration range in a partitioning manner.
For example, in some of these examples, O 3 In the method for detecting the concentration, O 3 Sensitivity of sensor and O 3 The linear relationship between the concentrations of (2) is:
ΔR/R a ×100%=k 1 ·C 1 +b 1 ，50 ppb≤C≤450 ppb；
ΔR/R a ×100%=k 2 ·C 2 +b 2 ，450 ppb＜C≤870 ppb。
it will be appreciated that k 1 、k 2 、b 1 、b 2 To determine the value.
Further, in some specific examples thereof, O 3 In the method for detecting the concentration, O 3 Sensitivity of sensor and O 3 The linear relationship between the concentrations of (2) is:
ΔR/R a = 0.178·C 1 ×100%-11.965，50 ppb≤C≤450 ppb。
one embodiment of the present application provides an O 3 A concentration detection apparatus comprising:
O 3 the sensor comprises a substrate, an electrode arranged on the substrate and a sensitive material layer arranged on the surface of the electrode, wherein the sensitive material layer is tetragonal CH 3 NH 3 PbI 3 The substrate is a ceramic substrate, and the electrodes are graphite interdigital electrodes; and
Resistance detection module for combining with O 3 Sensor connection and acquisition of O 3 Measured resistance of the sensor.
It will be appreciated that substituting the measured resistance into the established O 3 Resistance and O of sensor 3 In standard relation of concentration or substituted into O 3 Sensitivity of sensor and O 3 In a linear relationship between the concentrations of (2) O can be obtained 3 Is a concentration of (3). And O provided by the present application 3 Concentration detection device, need not the illumination condition, can test O under room temperature condition 3 Is a concentration of (3).
In some of these examples, O 3 The concentration detection apparatus further includes:
a data processing module for processing data according to preset O 3 Resistance and O of sensor 3 Standard relation of concentration and measured resistance, determining O 3 Is a concentration of (3).
The present application will be described in further detail with reference to the following specific embodiments, but embodiments of the present application are not limited thereto.
Example 1
(1) At room temperature (25 ℃ C.+ -. 3 ℃ C.), 0.7 mL of N, N-dimethylformamide was mixed with 0.3. 0.3 mL dimethyl sulfoxide uniformly, and 0.461 g of PbI was added 2 And 0.159 g CH 3 NH 3 PbI 3 Respectively adding into the above mixed solution, stirring to dissolve to obtain CH 3 NH 3 PbI 3 A precursor solution;
(2) Sequentially placing an alumina ceramic wafer substrate with graphite interdigital electrodes into absolute ethyl alcohol and deionized water for cleaning, and then drying at 60 ℃;
(3) In a glove box, 20. Mu.L of CH obtained in step (1) was taken 3 NH 3 PbI 3 The precursor solution is dripped on a ceramic wafer substrate with graphite interdigital electrodes to lead CH to be formed 3 NH 3 PbI 3 The precursor solution is uniformly covered on the surface of the substrate, and the substrate is subjected to heat treatment at 100 ℃ for 30 min, so that the organic solvent is evaporated and CH is promoted 3 NH 3 PbI 3 Crystallization of thin films, in situ formation of CH on the surface of ceramic substrates printed with graphite interdigital electrodes 3 NH 3 PbI 3 A film.
Will CH 3 NH 3 PbI 3 XRD characterization of the film was performed as shown in figure 2; the XRD pattern data are obtained by a RigakuD/MAX 2550 type X-ray diffractometer, and Cu is the target.
From fig. 2 it is clearly observed that the eight characteristic peaks are located at positions 14.5 °, 20.3 °, 23.8 °, 24.9 °, 28.8 °, 32.2 °, 41.0 ° and 43.6 °, respectively, corresponding to tetragonal CH 3 NH 3 PbI 3 (110), (200), (211), (2)02 (220), (310), (224) and (314) crystal planes, indicating the successful synthesis of perovskite CH by a single-step deposition process 3 NH 3 PbI 3 A film.
Will CH 3 NH 3 PbI 3 The film was subjected to EDX elemental quantification as shown in fig. 3; wherein, EDX characterization result is obtained by JEOL JSM-7500F type scanning electron microscope.
From the quantitative analysis results of the EDX element in fig. 3, C, N, I and Pb elements were present in the entire test region, and the mass percentages of I and Pb were measured to be 55.35% and 30.32%, respectively. That is, the measured atomic ratio of I to Pb was about 2.9:1, below the stoichiometric ratio 3 in the structural formula: 1, indicating CH prepared in example 1 3 NH 3 PbI 3 Iodine vacancies exist in the film.
Will CH 3 NH 3 PbI 3 The films were SEM characterized as shown in figure 4; wherein, SEM characterization results are obtained by a JEOL JSM-7500F type scanning electron microscope.
As can be seen from fig. 4, CH 3 NH 3 PbI 3 The film is continuous and free of cracking, which is advantageous for reinforcing CH 3 NH 3 PbI 3 The conductivity of the film.
Will CH 3 NH 3 PbI 3 The films were subjected to high resolution TEM characterization as shown in fig. 5; wherein, TEM characterization images are collected by a JEOL JEM-2100F type field emission transmission electron microscope.
From FIG. 5, it can be seen that the lattice fringes, with a gap of about 0.61. 0.61 nm, indicate CH 3 NH 3 PbI 3 The film has a good crystal structure.
Will CH 3 NH 3 PbI 3 XPS analysis of the film further analyzed CH 3 NH 3 PbI 3 Surface element state of the film. Wherein, the I3 d spectrum is shown in (a) of FIG. 6, the Pb 4f spectrum is shown in (b) of FIG. 6, the XPS spectrum is obtained by an ESCALAB 250 type X-ray photoelectron spectroscopy analyzer, and all peak positions are calibrated by 284.5 eV C1 s before formal measurement.
In FIG. 6 (a), at positions where the binding energies were about 618.9 eV and 630.3 eV, two sets of characteristic peaks were observed, corresponding to I3 d5/2 and I3 d3/2, respectively.
In FIG. 6 (b), the XPS spectrum of Pb 4f consists of two sets of absorption peaks, pb 4f5/2 and Pb 4f7/2, which are located at binding energies of about 142.9 eV and 138.1 eV, respectively, indicating Pb 2+ Exists in Pb-I octahedra ([ PbI) 6 ] 4- ) Is arranged in the frame of the (c). The weak peak in the figure is a characteristic peak of unsaturated Pb, compared with the strong characteristic peak of Pb-I bond, which indicates that the compound is present in CH 3 NH 3 PbI 3 Iodine vacancies exist in the crystal lattice.
Step (3) the CH thus obtained was subjected to the procedure of example 1 3 NH 3 PbI 3 The precursor solution is dripped on the surface of the graphite interdigital electrode on the ceramic wafer substrate, and CH is generated in situ on the surface of the graphite interdigital electrode after heat treatment 3 NH 3 PbI 3 Film to obtain O 3 A sensor. O is added with 3 Resistance test system is connected at both ends of graphite interdigital electrode of sensor to O 3 The sensor is tested to obtain the organic-inorganic hybridization perovskite CH 3 NH 3 PbI 3 Room temperature O of film 3 Sensor pair O 3 Is provided. Wherein the following tests were carried out under room temperature conditions (25 ℃.+ -. 3 ℃).
FIG. 7 is O 3 Gas-sensitive test chart of sensor, wherein (a) in FIG. 7 is O 3 Single-period dynamic response recovery curve of sensor, initial resistance value R a About 40M Ω. When O is 3 The sensor was shifted to 300 ppb of O 3 In the atmosphere, the resistance immediately drops until equilibrium is reached; response time (T) res ) And recovery time (T) rec ) About 68 s and 270 s. Wherein, response time (Tres) is defined as the time taken for the sensor to reach 90% of the change in resistance signal when it is transferred from air to the target gas; the recovery time (Trec) is then defined as the time it takes for the resistance signal to recover to 90% of the change value after the sensor has been diverted back to air from the target gas.
FIG. 7 (b) is O 3 O of 50 ppb-870 ppb of sensor 3 Dynamic response recovery in an atmosphereTest curves, it can be seen that at O 3 The amount of change in sensor resistance gradually decreases as the concentration gradually decreases from 870 ppb to 50 ppb. Notably, at a concentration of 50 ppb, the sensor still had a clear and complete response recovery signal, indicating that the sensor had the ability to detect trace O 3 The capacity of the gas, the lower detection limit can reach 50 ppb.
According to O 3 O of 50 ppb-870 ppb of sensor 3 Dynamic response recovery test curves in atmosphere can be plotted in FIG. 7 (c) for O at 50 ppb, 160 ppb, 300 ppb, 450 ppb, 630 ppb and 870 ppb 3 In the atmosphere, CH 3 NH 3 PbI 3 The sensitivity of the sensor was approximately 17%, 44%, 69%, 89%, 100% and 112%, respectively. Wherein the sensitivity is defined as DeltaR/R a X 100%, ΔR is R a And R is R g Absolute value of difference, R a R is the initial resistance value of the sensor in the air g Is the resistance value of the sensor in the target gas.
It can be seen that O 3 The concentration is in the range of 50 ppb to 450 ppb, the sensitivity and the concentration are approximately in a linear change relation, and the function is as follows: y=0.178 x-11.965, r 2 =0.983; with O 3 Further increase in concentration, sensitivity shows a saturation trend due to CH 3 NH 3 PbI 3 The active sites on the surface of the film are sufficiently filled to cause adsorption saturation of the sensitive layer.
FIG. 7 (d) is O 3 The selective test result of the sensor can be seen that the sensor pairs O 3 The response signal of (C) is obviously higher than that of nitrogen dioxide, acetone, trimethylamine and methanol, indicating that the catalyst is specific to O 3 Has stronger selectivity.
FIG. 7 (e) shows the sensor at 870 ppb O 3 The stability test in atmosphere, in five continuous test cycles, the resistance signal variation amplitude is similar, the sensitivity variation is smaller, the sensor has stronger stability.
FIG. 7 (f) is five lots O 3 The sensor is used for measuring O with different concentrations at room temperature 3 The response of the gases, five batches can be seen from the figureThe secondary sensor has stronger reliability and consistency.
To study CH 3 NH 3 PbI 3 At O 3 The gas-sensitive mechanism of the sensor, for exposure to O 3 CH before and after atmosphere 3 NH 3 PbI 3 The film was subjected to XPS analysis as shown in FIG. 8.
As can be seen from FIG. 8 (a), compared to the exposure to O 3 Binding energy before atmosphere, after prolonged exposure to O 3 After the atmosphere, the diffraction peak of Pb 4f was shifted by 0.2. 0.2 eV in the direction of high binding energy, indicating Pb 2+ Electrons are lost. However, as can be seen from FIG. 8 (b), the characteristic peak of I3 d is shifted by 0.1. 0.1 eV in the direction of lower binding energy, indicating that I - Electrons are trapped. This change in binding energy is due to CH 3 NH 3 PbI 3 Film and O 3 Electron transfer of molecules under strong interactions. In addition, the peak intensity of Pb 4f increases, while the peak intensity of I3 d decreases, indicating that the relative contents of these two elements change before and after the gas-sensitive reaction.
Example 2
(1) At room temperature (25 ℃ C.+ -. 3 ℃ C.), 0.7 mL of N, N-dimethylformamide was mixed with 0.3. 0.3 mL dimethyl sulfoxide uniformly, and 0.461 g of PbI was added 2 And 0.159 g CH 3 NH 3 PbI 3 Respectively adding into the above mixed solution, stirring to dissolve to obtain CH 3 NH 3 PbI 3 A precursor solution;
(2) Sequentially placing the ceramic wafer substrate with the graphite interdigital electrodes into absolute ethyl alcohol and deionized water for cleaning, and then drying at 60 ℃;
(3) In a glove box, 30. Mu.L of CH obtained in the step (1) was taken 3 NH 3 PbI 3 The precursor solution is dripped on a ceramic wafer substrate with graphite interdigital electrodes to lead CH to be formed 3 NH 3 PbI 3 The precursor solution is uniformly covered on the surface of the substrate, and the substrate is subjected to heat treatment at 100 ℃ for 30 min, so that the organic solvent is evaporated and CH is promoted 3 NH 3 PbI 3 Crystallization of thin films, in situ formation of graphite interdigital electrodes on the surface of ceramic substratesCH 3 NH 3 PbI 3 Thin film, O is produced 3 A sensor.
Example 3
(1) At room temperature (25 ℃ C.+ -. 3 ℃ C.), 0.7 mL of N, N-dimethylformamide was mixed with 0.3. 0.3 mL dimethyl sulfoxide uniformly, and 0.461 g of PbI was added 2 And 0.159 g CH 3 NH 3 PbI 3 Respectively adding into the above mixed solution, stirring to dissolve to obtain CH 3 NH 3 PbI 3 A precursor solution;
(2) Sequentially placing the ceramic wafer substrate with the graphite interdigital electrodes into absolute ethyl alcohol and deionized water for cleaning, and then drying at 60 ℃;
(3) In a glove box, 40. Mu.L of CH obtained in step (1) was taken 3 NH 3 PbI 3 The precursor solution is dripped on a ceramic wafer substrate with graphite interdigital electrodes to lead CH to be formed 3 NH 3 PbI 3 The precursor solution is uniformly covered on the surface of the substrate, and the substrate is subjected to heat treatment at 100 ℃ for 30 min, so that the organic solvent is evaporated and CH is promoted 3 NH 3 PbI 3 Crystallization of thin films, in situ formation of CH on the surface of ceramic substrates printed with graphite interdigital electrodes 3 NH 3 PbI 3 Thin film, O is produced 3 A sensor.
Example 4
(1) At room temperature (25 ℃ C.+ -. 3 ℃ C.), 0.7 mL of N, N-dimethylformamide was mixed with 0.3. 0.3 mL dimethyl sulfoxide uniformly, and 0.461 g of PbI was added 2 And 0.159 g CH 3 NH 3 PbI 3 Respectively adding into the above mixed solution, stirring to dissolve to obtain CH 3 NH 3 PbI 3 A precursor solution;
(2) Sequentially placing the ceramic wafer substrate with the Ag interdigital electrodes in absolute ethyl alcohol and deionized water for cleaning, and then drying at 60 ℃;
(3) In a glove box, 20. Mu.L of CH obtained in step (1) was taken 3 NH 3 PbI 3 The precursor solution is dripped on a ceramic wafer substrate with graphite interdigital electrodes to lead CH to be formed 3 NH 3 PbI 3 Precursor solution is uniformCovering the surface of the substrate, and heat treating the substrate at 100deg.C for 30 min to evaporate the organic solvent and promote CH 3 NH 3 PbI 3 Crystallization of thin films, in situ formation of CH on the surface of ceramic substrates printed with graphite interdigital electrodes 3 NH 3 PbI 3 Thin film, O is produced 3 A sensor.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples merely represent a few embodiments of the present application, which facilitate a specific and detailed understanding of the technical solutions of the present application, but are not to be construed as limiting the scope of the invention. It should be noted that it would be apparent to those skilled in the art that various modifications and improvements could be made without departing from the spirit of the present application, which would be within the scope of the present application. It should be understood that those skilled in the art, based on the technical solutions provided in the present application, can obtain technical solutions through logical analysis, reasoning or limited experiments, all fall within the protection scope of the claims attached in the present application. The scope of the patent application is therefore intended to be limited by the content of the appended claims, the description and drawings being presented to the extent that the claims are defined.
Claims (10)
1. O (O) 3 The sensor is characterized by comprising a substrate with interdigital electrodes and a sensitive material layer arranged on the surfaces of the interdigital electrodes, wherein the sensitive material layer is tetragonal CH 3 NH 3 PbI 3 The interdigital electrode is a graphite interdigital electrode, and the substrate is a ceramic substrate.
2. O as claimed in claim 1 3 The sensor is characterized in that the substrate is an alumina ceramic substrate.
3. O (O) 3 The preparation method of the sensor is characterized by comprising the following steps of:
PbI is prepared 2 、CH 3 NH 3 I and organic solvent to obtain CH 3 NH 3 PbI 3 A precursor solution;
the CH is subjected to 3 NH 3 PbI 3 The precursor solution is arranged on the surface of an interdigital electrode on a substrate, and a tetragonal CH is formed on the surface of the interdigital electrode after drying 3 NH 3 PbI 3 The membrane layer, the interdigital electrode is graphite interdigital electrode, and the substrate is a ceramic substrate.
4. A method of preparing as claimed in claim 3, wherein the PbI 2 With the CH 3 NH 3 The molar ratio of I is (1-3): 1.
5. The method according to claim 3, wherein the organic solvent is at least one selected from the group consisting of N, N-dimethylformamide and dimethyl sulfoxide.
6. The method according to any one of claims 3 to 5, wherein the CH 3 NH 3 PbI 3 PbI in precursor solution 2 The concentration of (C) is 0.5 mol/L-3 mol/L.
7. O (O) 3 The concentration detection method is characterized by comprising the following steps:
o is added with 3 The sensors are respectively arranged at least 3O with different standard concentrations 3 In standard environment, different O's are obtained respectively 3 At the concentration of O 3 Standard resistance R of sensor g The method comprises the steps of carrying out a first treatment on the surface of the The O is 3 The sensor comprises a substrate, an electrode arranged on the substrate and a sensitive material layer arranged on the surface of the electrode, wherein the sensitive material layer is tetragonal CH 3 NH 3 PbI 3 The substrate is a ceramic substrate, and the electrode is a graphite interdigital electrode;
according to different O 3 At the concentration of O 3 Standard resistance R of sensor g Obtaining the O 3 Resistance and O of sensor 3 Standard relationship of concentration;
acquiring the O 3 Resistance R of sensor in environment to be measured x The method comprises the steps of carrying out a first treatment on the surface of the According to the standard relation and the resistance R x Obtaining O in the environment to be tested 3 Concentration.
8. O as claimed in claim 7 3 The method for detecting the concentration is characterized in that the method is based on different O 3 At the concentration of O 3 Standard resistance R of sensor g Obtaining the O 3 Resistance and O of sensor 3 The standard relationship of the concentration comprises the following steps:
o is added with 3 The sensor is placed in the air to obtain the O 3 Initial resistance R of sensor a ；
According to different O 3 At the concentration of O 3 Standard resistance R of sensor g Obtaining the O 3 Sensor relative to initial resistance R a Sensitivity of said O 3 Sensitivity of sensor = Δr/R a X 100%, ΔR is R a And R is R g Absolute value of the difference;
establishing the O 3 Sensitivity of sensor and O 3 Linear relation between the concentrations of (a).
9. O (O) 3 Concentration detection apparatus, characterized by comprising:
O 3 the sensor comprises a substrate, an electrode arranged on the substrate and a sensitive material layer arranged on the surface of the electrode, wherein the sensitive material layer is tetragonal CH 3 NH 3 PbI 3 The substrate is a ceramic substrate, and the electrode is a graphite interdigital electrode; and
A resistance detection module for connecting with the O 3 Sensor connection and acquisition of the O 3 Measured resistance of the sensor.
10. O as claimed in claim 9 3 Concentration detection apparatus, its characterized in that still includes:
a data processing module for processing the data according to the preset O 3 Resistance and O of sensor 3 Standard relation of concentration and the measured resistance, determining O 3 Is a concentration of (3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311307004.XA CN117871615A (en) | 2023-10-10 | 2023-10-10 | O 3 Sensor, preparation method thereof and O 3 Concentration detection method and detection device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311307004.XA CN117871615A (en) | 2023-10-10 | 2023-10-10 | O 3 Sensor, preparation method thereof and O 3 Concentration detection method and detection device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117871615A true CN117871615A (en) | 2024-04-12 |
Family
ID=90577919
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311307004.XA Pending CN117871615A (en) | 2023-10-10 | 2023-10-10 | O 3 Sensor, preparation method thereof and O 3 Concentration detection method and detection device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117871615A (en) |
-
2023
- 2023-10-10 CN CN202311307004.XA patent/CN117871615A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Wang et al. | Au-loaded mesoporous WO3: preparation and n-butanol sensing performances | |
| Chen et al. | CO sensing properties and mechanism of Pd doped SnO2 thick-films | |
| Qin et al. | Microstructure characterization and NO2-sensing properties of tungsten oxide nanostructures | |
| Rai et al. | Synthesis of flower-like ZnO microstructures for gas sensor applications | |
| Khuspe et al. | Nanostructured SnO2 thin films for NO2 gas sensing applications | |
| Qin et al. | Effect of annealing on microstructure and NO2-sensing properties of tungsten oxide nanowires synthesized by solvothermal method | |
| Wang et al. | Multi-walled carbon nanotubes and metal–organic framework nanocomposites as novel hybrid electrode materials for the determination of nano-molar levels of lead in a lab-on-valve format | |
| Chen et al. | Lanthanum dioxide carbonate La2O2CO3 nanorods as a sensing material for chemoresistive CO2 gas sensor | |
| Grigorieva et al. | Synthesis, structure, and sensor properties of vanadium pentoxide nanorods | |
| Zare-Dorabei et al. | Preparation and characterization of a novel tetrakis (4-hydroxyphenyl) porphyrin–graphene oxide nanocomposite and application in an optical sensor and determination of mercury ions | |
| Siemons et al. | Preparation and gas sensing properties of nanocrystalline La-doped CoTiO3 | |
| CN110887874A (en) | Based on perovskite Cs2PdBr6Humidity-sensitive sensor and preparation method and application thereof | |
| Hemalatha et al. | Comparison of electrical and sensing properties of pure, Sn-and Zn-doped CuO gas sensors | |
| Srivastava et al. | Study of structural and microstructural properties of SnO2 powder for LPG and CNG gas sensors | |
| Zhu et al. | Ppt-level benzene detection and gas sensing mechanism using (C 4 H 9 NH 3) 2 PbI 2 Br 2 organic–inorganic layered perovskite | |
| Hou et al. | Enhanced triethylamine-sensing properties of hierarchical molybdenum trioxide nanostructures derived by oxidizing molybdenum disulfide nanosheets | |
| Yang et al. | Electrical properties and acetone-sensing characteristics of LaNi1− xTixO3 perovskite system prepared by amorphous citrate decomposition | |
| Wang et al. | Molecular imprinting Ag-LaFeO3 spheres for highly sensitive acetone gas detection | |
| Sinha et al. | Fast response and low temperature sensing of acetone and ethanol using Al-doped ZnO microrods | |
| CN112798661B (en) | SO (SO) 2 F 2 Detection method of (2) | |
| Marikutsa et al. | Improved H2S sensitivity of nanosized BaSnO3 obtained by hydrogen peroxide assisted sol-gel processing | |
| Narwade et al. | Nanostructured hydroxyapatite biomaterial as gas sensor | |
| CN112362712B (en) | Electrochemical sensor electrode capable of simultaneously detecting heavy metal lead and cadmium ions in grains | |
| KR102474884B1 (en) | Acetone gas sensor using Nb-doped WO3 and fabrication method thereof | |
| CN117871615A (en) | O 3 Sensor, preparation method thereof and O 3 Concentration detection method and detection device |
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 |